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CN118006274B - A preparation method of epoxy resin modified asparagus polyurea seam beautifying agent - Google Patents

A preparation method of epoxy resin modified asparagus polyurea seam beautifying agent Download PDF

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Publication number
CN118006274B
CN118006274B CN202410159834.0A CN202410159834A CN118006274B CN 118006274 B CN118006274 B CN 118006274B CN 202410159834 A CN202410159834 A CN 202410159834A CN 118006274 B CN118006274 B CN 118006274B
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reaction
agent
parts
microwave
epoxy resin
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CN118006274A (en
Inventor
刘晟
王检
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Zhejiang Peak New Materials Co ltd
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Zhejiang Fengfeng Building Materials Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J175/00—Adhesives based on polyureas or polyurethanes; Adhesives based on derivatives of such polymers
    • C09J175/02—Polyureas
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/48—Polyethers
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40—High-molecular-weight compounds
    • C08G18/58—Epoxy resins
    • C08G18/584—Epoxy resins having nitrogen
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00—Polymeric products of isocyanates or isothiocyanates
    • C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/67—Unsaturated compounds having active hydrogen
    • C08G18/675—Low-molecular-weight compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02—Non-macromolecular additives
    • C09J11/04—Non-macromolecular additives inorganic

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Epoxy Resins (AREA)

Abstract

本发明公开了一种环氧树脂改性天冬聚脲美缝剂的制备方法，涉及环氧树脂技术领域，通过开环反应将脂肪族伯胺和脂环族伯胺与氢化双酚A型环氧树脂进行化学反应生成，并通过微波化学系统控制反应程度，均匀生成环氧树脂改性脂肪族或脂环族伯二胺，提高生产效率；通过加成反应生成改性的聚脲树脂A，降低脂肪族伯胺和脂环族伯胺的活性；通过添加稳定剂与异氰酸酯发生加成反应，生成稳定的有机异氰酸酯化合物，并将有机异氰酸酯化合物与聚醚多元醇混合反应生成改性聚脲固化剂B，降低异氰酸酯的活性，延长施工时间。

The invention discloses a preparation method of an epoxy resin modified asparagus polyurea seam beautifying agent, and relates to the technical field of epoxy resins. The invention comprises the following steps: chemically reacting aliphatic primary amines and alicyclic primary amines with hydrogenated bisphenol A type epoxy resins through a ring-opening reaction, and controlling the reaction degree through a microwave chemical system to uniformly generate epoxy resin modified aliphatic or alicyclic primary diamines, thereby improving production efficiency; generating a modified polyurea resin A through an addition reaction, thereby reducing the activity of aliphatic primary amines and alicyclic primary amines; adding a stabilizer to react with isocyanate to generate a stable organic isocyanate compound, and mixing the organic isocyanate compound with a polyether polyol to generate a modified polyurea curing agent B, thereby reducing the activity of isocyanate and extending the construction time.

Description

Preparation method of epoxy resin modified asparagus polyurea joint beautifying agent
Technical Field
The invention relates to the technical field of epoxy resin, and in particular relates to a preparation method of an epoxy resin modified asparagus polyurea joint beautifying agent.
Background
The epoxy-based joint beautifying agent is a special hardening joint beautifying material, and is mainly formed by mixing various raw materials such as epoxy resin, curing agent, filler and the like. Compared with the traditional cement caulking material, the epoxy-based joint compound has the advantages of remarkably improving and improving the strength, toughness, water resistance, chemical corrosion resistance and the like, but the conventional epoxy-based joint compound has poor resistance Huang Xingbian due to the benzene ring structure of bisphenol A epoxy resin, and the polyurea joint compound is increasingly favored by consumers due to the good yellowing resistance effect.
In the prior art, the traditional polyurea joint beautifying agent has a plurality of defects, on one hand, the traditional polyurea joint beautifying agent has high reactant activity, so that constructors are easy to skin allergy, the construction time is short, the bulge is easy to occur, and the bonding strength is low after the solidified matters in the construction process are mixed, and the bonding strength is easy to fall off.
Disclosure of Invention
Aiming at the defects of the prior art, the invention discloses a preparation method of an epoxy resin modified asparagus polyurea joint beautifying agent, which can reduce the activity of reactants, prolong the construction time and improve the preparation speed, wherein aliphatic primary amine and alicyclic primary amine are subjected to chemical reaction with hydrogenated bisphenol A epoxy resin to generate aliphatic or alicyclic primary diamine through ring opening reaction, the reaction degree is controlled through a microwave chemical system, the production efficiency is improved, the aliphatic or alicyclic primary diamine is subjected to reaction with alkylated maleate through addition reaction to generate modified polyurea resin A, the activity of the aliphatic primary amine and alicyclic primary amine is reduced, the addition reaction of stabilizer and isocyanate is carried out to generate stable organic isocyanate compound, the organic isocyanate compound and polyether polyol are mixed to generate modified polyurea curing agent B, the activity of isocyanate is reduced, and the construction time is prolonged.
The invention adopts the following technical scheme:
The preparation method of the epoxy resin modified asparagus polyurea joint beautifying agent comprises the following steps:
step one, preparing raw materials;
The raw materials comprise, by weight, 3-4 parts of aliphatic primary amine, 3-4 parts of alicyclic primary amine, 1.6-2 parts of hydrogenated bisphenol A epoxy resin, 0.4-0.5 part of diethyl maleate, 0.4-0.5 part of dibutyl maleate, 4-5 parts of isocyanate, 2-3 parts of polyether polyol and 0.9-1 part of stabilizer;
Step two, performing ring-opening reaction to generate aliphatic or alicyclic primary diamine;
Performing chemical reaction on aliphatic primary amine and alicyclic primary amine and hydrogenated bisphenol A epoxy resin through a ring-opening reaction to generate aliphatic or alicyclic primary diamine, wherein the ring-opening reaction controls the reaction process through a microwave chemical system;
Step three, obtaining modified polyurea resin A;
Reacting an aliphatic or cycloaliphatic primary diamine with an alkylated maleate to form a modified polyurea resin A by an addition reaction having the chemical reaction formula:
In the reaction scheme (1) of the present invention, Represents an alkylated maleate ester of a carboxylic acid,Represents an aliphatic or cycloaliphatic primary diamine,Represents a modified polyurea resin A;
Step four, obtaining a modified polyurea curing agent B;
Adding a stabilizer to react with isocyanate HDI to generate a stable organic isocyanate compound so as to achieve the purpose of reducing the reactivity of isocyanate, and mixing the organic isocyanate compound with polyether polyol to react to generate a modified polyurea curing agent B, wherein the chemical reaction formula of the addition reaction is as follows:
In the reaction scheme (2) of the present invention, It is meant that the stabilizer is present in the composition,Represents the terminal groups of the isocyanate polymer chain,Represents an organic isocyanate compound which is used as a reactive component,Represents carbon dioxide and is used to produce a carbon dioxide gas,Represents the carbon monoxide content of the gas,Represents the ammonia gas, and the ammonia gas,Represents water;
Step five, preparing a seam beautifying agent A and a seam beautifying agent B;
Firstly, obtaining modified polyurea resin A through the second step and the third step, obtaining modified polyurea curing agent B through the fourth step, wherein hydrophobic fumed silica, filling powder, molecular sieve, defoaming agent and toner are purchased from the chemical market, preparing seam beautifying agent A according to the proportion of the modified polyurea resin A to the hydrophobic fumed silica to the filling powder to the molecular sieve=25:3:15:1:1, and preparing seam beautifying agent B according to the proportion of the modified polyurea curing agent B to the hydrophobic fumed silica to the filling powder to the molecular sieve to the defoaming agent to the toner=29:3:15:1:1.
As a further technical scheme of the present invention, the aliphatic primary amine and the alicyclic primary amine are obtained by chemically reacting aliphatic alcohol and alicyclic compound with hydrogen by an aliphatic alcohol amination method and a thermal condensation method, the hydrogenated bisphenol a type epoxy resin and the special alicyclic epoxy resin are obtained by an epoxidation reaction of bisphenol a and alicyclic compound with an epoxidizing agent, the diethyl maleate and dibutyl maleate are obtained by an esterification reaction of maleic acid with ethanol and n-butanol, and the isocyanate, polyether polyol and stabilizer are purchased from chemical markets.
As a further technical scheme of the invention, the specific steps of the ring-opening reaction are as follows:
step1, preparing aliphatic primary amine and alicyclic primary amine;
weighing 8 parts of aliphatic primary amine and alicyclic primary amine according to the ratio of 1:1, putting the mixture into a reaction kettle, uniformly mixing the mixture by adopting a paddle stirrer to obtain a primary amine mixture, and heating the primary amine mixture to 70-80 ℃ by a heater;
step 2, preparing hydrogenated bisphenol A epoxy resin;
2 parts of hydrogenated bisphenol A epoxy resin is weighed and added into a reaction kettle dropwise adding device, and the hydrogenated bisphenol A epoxy resin is heated to 70-80 ℃ through a heater;
Step 3, dropwise adding hydrogenated bisphenol A epoxy resin;
Controlling the temperature in the reaction kettle to be within 50 ℃ through a microwave chemical system, slowly dropwise adding hydrogenated bisphenol A epoxy resin into the primary amine mixture for 1-2 hours, and controlling the dropwise adding speed of a reaction kettle dropwise adding device through a valve in the dropwise adding process;
Step 4, vacuumizing to start reaction;
After the dripping process is finished, firstly, closing the reaction kettle to form a closed space, pumping air or gas from the reaction kettle through a vacuum pump to form a vacuum environment, secondly, adding a catalyst to start the reaction, and in the reaction process, reducing the activation energy of the reaction through a microwave chemical system to improve the reaction rate, wherein the chemical reaction formula of the ring-opening reaction is as follows:
in the reaction scheme (3) of the present invention, Represents a hydrogenated bisphenol A type epoxy resin,Represents primary amine mixture molecules, whereinRepresents an alkyl group of an aliphatic primary amine or an aromatic ring group of an alicyclic primary amine,Represents an aliphatic or cycloaliphatic primary diamine,Represents water;
Step 5, obtaining aliphatic or alicyclic primary diamine;
After the reaction is finished, the mixture is treated by an organic solvent extraction mode, and aliphatic or alicyclic primary di-solvent is dissolved in the organic solvent to obtain aliphatic or alicyclic primary diamine.
As a further technical scheme of the present invention, the microwave chemical system includes a microwave generator, a microwave reflector, a temperature control device and a visualization module, the microwave generator is used for generating microwaves, the microwave reflector is used for generating microwave radiation fields, the temperature control device is used for adjusting the temperature in the reaction kettle, the visualization module is used for displaying microwave data, microwave radiation energy, temperature data and reaction rate data in real time, and the working mode of the microwave chemical system includes the following steps:
s1, generating microwaves;
The microwave generator generates microwaves through a solid-state oscillation method, and calculates the generated microwave radiation energy through a microwave energy function, wherein the formula of the microwave energy function is as follows:
in the formula (4) of the present invention, In order to radiate energy of the microwaves,Is a constant of planck, which is set to be the planck's constant,The value of (2) isIn order to achieve the light velocity, the light beam is,The value of (2) is,Is the wavelength of the microwave;
S2, forming a uniform microwave radiation field;
the microwave reflector is made into a closed space through a metal material and is arranged at the outer side of the reaction kettle, and the microwave reflector forms a stable and uniform radiation field for microwaves in the microwave reflector based on the interaction of electromagnetic waves and free electrons in the metal;
S3, obtaining and controlling the temperature in the reaction kettle;
The temperature control device collects temperature data in the reaction kettle through an infrared thermometer, the temperature data are transmitted to an RK3288 chip through an RS485 communication protocol, the RK3288 chip outputs a temperature control instruction according to a set reaction temperature threshold value and transmits the temperature control instruction to an actuator, and the actuator controls the operation of a heater or a refrigerator according to the temperature control instruction;
s4, obtaining the reaction rate of the chemical reaction;
The microwave chemical system calculates the reaction rate of chemical reaction in a microwave radiation field through a reaction rate function embedded in an RK3288 chip, and the reaction rate function has the formula:
In the formula (5) of the present invention, For the reaction rate of the chemical reaction,For the activation energy of the chemical reaction,In order to radiate energy of the microwaves,In order to react the energy required for the reaction,As a factor of the frequency of the signal,Is a gas constant which is a function of the gas,Is the temperature in the reaction kettle;
S5, displaying in real time;
The visualization module displays the generated microwave data, microwave radiation energy, temperature data and reaction rate data in real time through the Internet of things platform.
As a further technical scheme of the invention, the seam-beautifying agent A comprises, by weight, 60-80 parts of modified polyurea resin A, 4-6 parts of hydrophobic fumed silica, 1-3 parts of molecular sieve, 20-40 parts of filling powder and 1-3 parts of defoamer, and the seam-beautifying agent B comprises, by weight, 50-70 parts of modified polyurea curing agent B, 3-6 parts of hydrophobic fumed silica, 1-3 parts of molecular sieve, 30-50 parts of filling powder, 3-5 parts of toner and 1-3 parts of defoamer.
As a further technical scheme of the invention, the hydrophobic fumed silica increases the dispersity of raw materials in the modified polyurea resin A through a dispersing effect, increases the rheological property of the modified polyurea resin A, the filling powder increases the density and durability of the modified polyurea resin A through filling gaps, the molecular sieve adsorbs impurities and moisture in the joint beautifying agent A in a physical adsorption and chemical adsorption combined mode so as to achieve the purpose of purifying the joint beautifying agent A, and the defoaming agent eliminates or prevents the formation of bubbles by reducing the surface tension between the joint beautifying agent A and air, and the color of the joint beautifying agent B is changed by the toner.
As a further technical scheme of the invention, the construction steps of the epoxy resin modified asparagus polyurea joint beautifying agent are as follows:
S01, cleaning gaps;
Firstly, cleaning cement dust in the gap by using an art designer knife at an angle of 45 degrees, sucking dust impurities by using a dust collector, cleaning black edges of the ceramic tile by using a multifunctional decontamination paste, and wiping the gap and the surface of the tile by using a dry towel to ensure that the construction environment is clean and dry;
S02, waxing the periphery of the gap;
A proper amount of seam wax is dipped by sponge and beaten on the surfaces of the ceramic tiles at two sides of the seam, so that the residual materials can be conveniently shoveled off at the back;
S03, driving the seam beautifying agent into the seam;
Firstly, a 40cm seam beautifying agent is punched out without being used, so that uneven mixing of the seam beautifying agent A and the seam beautifying agent B is avoided, then a glue nozzle is attached to a seam, the included angle between a glue gun and the seam is larger than 60 degrees, glue is punched vertically at a uniform speed, and the tip of the glue gun is enabled to fully inject the seam beautifying agent into the seam, and the seam is fully punched and compacted;
S04, caulking;
after the sizing is finished, starting to press the sizing, firstly adopting a metal groove pressing cutter to test pressure, confirming the fluidity and the adhesive force of the joint beautifying agent, then keeping stable force application, and dragging a silica gel rod at uniform speed to finish the sizing;
s05, cleaning the residue;
After the seam beautifying agent is solidified, the residual materials are shoveled by a shovel blade, and the seam beautifying operation is completed.
The invention has positive and beneficial effects different from the prior art:
The invention discloses a preparation method of an epoxy resin modified asparagus polyurea joint beautifying agent, which can reduce the activity of reactants, prolong the construction time and improve the preparation speed, chemically react aliphatic primary amine and alicyclic primary amine with hydrogenated bisphenol A epoxy resin to generate aliphatic or alicyclic primary diamine through ring opening reaction, control the reaction degree through a microwave chemical system, improve the production efficiency, react the aliphatic or alicyclic primary diamine with alkylated maleate through addition reaction to generate modified polyurea resin A, reduce the activity of the aliphatic primary amine and the alicyclic primary amine, generate stable organic isocyanate compound through addition reaction of a stabilizer and isocyanate, and mix the organic isocyanate compound with polyether polyol to generate modified polyurea curing agent B, reduce the activity of isocyanate and prolong the construction time.
Drawings
FIG. 1 is a schematic overall flow diagram of a method for preparing an epoxy resin modified asparagus polyurea seam sealer of the present invention;
FIG. 2 is a schematic diagram of a specific flow chart of a ring-opening reaction in a preparation method of an epoxy resin modified asparagus polyurea joint beautifying agent;
FIG. 3 is a schematic diagram of the workflow of a microwave chemical system in a method for preparing an epoxy resin modified asparagus polyurea joint compound according to the present invention;
FIG. 4 is a schematic diagram showing the contents of the agent A and the agent B in the preparation method of the epoxy resin modified asparagus polyurea joint beautifying agent;
FIG. 5 is a schematic view of a construction flow in a method for preparing an epoxy resin modified asparagus polyurea joint beautifying agent of the invention.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Examples
The preparation method of the epoxy resin modified asparagus polyurea joint beautifying agent comprises the following steps:
step one, preparing raw materials;
The raw materials comprise, by weight, 3 parts of aliphatic primary amine, 3 parts of alicyclic primary amine, 1.6 parts of hydrogenated bisphenol A epoxy resin, 0.4 part of diethyl maleate, 0.4 part of dibutyl maleate, 4 parts of isocyanate, 2 parts of polyether polyol and 0.9 part of stabilizer;
Step two, performing ring-opening reaction to generate aliphatic or alicyclic primary diamine;
Performing chemical reaction on aliphatic primary amine and alicyclic primary amine and hydrogenated bisphenol A epoxy resin through a ring-opening reaction to generate aliphatic or alicyclic primary diamine, wherein the ring-opening reaction controls the reaction process through a microwave chemical system;
Step three, obtaining modified polyurea resin A;
Reacting an aliphatic or cycloaliphatic primary diamine with an alkylated maleate to form a modified polyurea resin A by an addition reaction having the chemical reaction formula:
In the reaction scheme (1) of the present invention, Represents an alkylated maleate ester of a carboxylic acid,Represents an aliphatic or cycloaliphatic primary diamine,Represents a modified polyurea resin A;
Step four, obtaining a modified polyurea curing agent B;
Adding a stabilizer to react with isocyanate HDI to generate a stable organic isocyanate compound so as to achieve the purpose of reducing the reactivity of isocyanate, and mixing the organic isocyanate compound with polyether polyol to react to generate a modified polyurea curing agent B, wherein the chemical reaction formula of the addition reaction is as follows:
In the reaction scheme (2) of the present invention, It is meant that the stabilizer is present in the composition,Represents the terminal groups of the isocyanate polymer chain,Represents an organic isocyanate compound which is used as a reactive component,Represents carbon dioxide and is used to produce a carbon dioxide gas,Represents the carbon monoxide content of the gas,Represents the ammonia gas, and the ammonia gas,Represents water;
Step five, preparing a seam beautifying agent A and a seam beautifying agent B;
Firstly, obtaining modified polyurea resin A through the second step and the third step, obtaining modified polyurea curing agent B through the fourth step, wherein hydrophobic fumed silica, filling powder, molecular sieve, defoaming agent and toner are purchased from the chemical market, preparing seam beautifying agent A according to the proportion of the modified polyurea resin A to the hydrophobic fumed silica to the filling powder to the molecular sieve=25:3:15:1:1, and preparing seam beautifying agent B according to the proportion of the modified polyurea curing agent B to the hydrophobic fumed silica to the filling powder to the molecular sieve to the defoaming agent to the toner=29:3:15:1:1.
The mass percentages of the raw materials in the steps are shown in table 1:
the embodiment of the invention is now illustrated, wherein 2 groups of examples are compared, 4 pieces of to-be-stitched areas with the same material and position are adopted for testing in the comparison process, the test times are 3 times, wherein when 4 pieces of to-be-stitched areas with the same material and position are tested, 2 pieces of to-be-stitched areas are adopted for testing, polyurea stitching agent is recorded as a comparison area 1 and a comparison area 2, the stitching agent with the formula is adopted as a test area 1 and a test area 2, the to-be-stitched areas are treated by using different types of stitching agents, and the results after the treatment are observed and recorded are shown in a comparison meaning table as shown in table 2:
The bonding strength and yellowing time of the joint beautifying agent directly influence the performance of the joint beautifying agent, and the drying time of the joint beautifying agent directly influences the construction time of the joint beautifying agent, so that performance indexes such as the drying time, the bonding strength, the yellowing time and the like are extremely important for the formula of the joint beautifying agent.
Examples
The preparation method of the epoxy resin modified asparagus polyurea joint beautifying agent comprises the following steps:
step one, preparing raw materials;
The raw materials comprise, by weight, 4 parts of aliphatic primary amine, 4 parts of alicyclic primary amine, 2 parts of hydrogenated bisphenol A epoxy resin, 0.5 part of diethyl maleate, 0.5 part of dibutyl maleate, 5 parts of isocyanate, 3 parts of polyether polyol and 1 part of stabilizer;
Step two, performing ring-opening reaction to generate aliphatic or alicyclic primary diamine;
Performing chemical reaction on aliphatic primary amine and alicyclic primary amine and hydrogenated bisphenol A epoxy resin through a ring-opening reaction to generate aliphatic or alicyclic primary diamine, wherein the ring-opening reaction controls the reaction process through a microwave chemical system;
Step three, obtaining modified polyurea resin A;
Reacting an aliphatic or cycloaliphatic primary diamine with an alkylated maleate to form a modified polyurea resin A by an addition reaction having the chemical reaction formula:
In the reaction scheme (1) of the present invention, Represents an alkylated maleate ester of a carboxylic acid,Represents an aliphatic or cycloaliphatic primary diamine,Represents a modified polyurea resin A;
Step four, obtaining a modified polyurea curing agent B;
Adding a stabilizer to react with isocyanate HDI to generate a stable organic isocyanate compound so as to achieve the purpose of reducing the reactivity of isocyanate, and mixing the organic isocyanate compound with polyether polyol to react to generate a modified polyurea curing agent B, wherein the chemical reaction formula of the addition reaction is as follows:
In the reaction scheme (2) of the present invention, It is meant that the stabilizer is present in the composition,Represents the terminal groups of the isocyanate polymer chain,Represents an organic isocyanate compound which is used as a reactive component,Represents carbon dioxide and is used to produce a carbon dioxide gas,Represents the carbon monoxide content of the gas,Represents the ammonia gas, and the ammonia gas,Represents water;
Step five, preparing a seam beautifying agent A and a seam beautifying agent B;
Firstly, obtaining modified polyurea resin A through the second step and the third step, obtaining modified polyurea curing agent B through the fourth step, wherein hydrophobic fumed silica, filling powder, molecular sieve, defoaming agent and toner are purchased from the chemical market, preparing seam beautifying agent A according to the proportion of the modified polyurea resin A to the hydrophobic fumed silica to the filling powder to the molecular sieve=25:3:15:1:1, and preparing seam beautifying agent B according to the proportion of the modified polyurea curing agent B to the hydrophobic fumed silica to the filling powder to the molecular sieve to the defoaming agent to the toner=29:3:15:1:1.
The mass percentages of the raw materials in the steps are shown in Table 3:
The embodiment of the invention is now illustrated, wherein 2 groups of examples are compared, 4 pieces of to-be-stitched areas with the same material and position are adopted for testing in the comparison process, the test times are 3 times, wherein when 4 pieces of to-be-stitched areas with the same material and position are tested, 2 pieces of to-be-stitched areas are adopted for testing, polyurea stitching agent is recorded as a comparison area 1 and a comparison area 2, the stitching agent with the formula is adopted as a test area 1 and a test area 2, the to-be-stitched areas are treated by using different types of stitching agents, the results after the treatment are observed and recorded are shown in a comparison meaning table 4:
through experiments, the structural modification is carried out on the polyurea joint beautifying agent through the epoxy resin, so that the structural introduction of the epoxy resin prolongs the construction time while the excellent yellowing resistance is maintained, and the structural modification has the characteristics of excellent bonding strength and hardness of the epoxy resin.
In the above examples, the aliphatic primary amine and the alicyclic primary amine are obtained by chemically reacting an aliphatic alcohol and an alicyclic compound with hydrogen by an aliphatic alcohol amination method and a thermal condensation method, the hydrogenated bisphenol a type epoxy resin and the special alicyclic epoxy resin are obtained by epoxidizing bisphenol a and an alicyclic compound with an epoxidizing agent, the diethyl maleate and dibutyl maleate are obtained by esterifying maleic acid with ethanol and n-butanol, and isocyanate, polyether polyol and stabilizer are purchased from chemical markets.
In the specific embodiment, the principle of the aliphatic alcohol amination method is that hydroxyl and amino in aliphatic alcohol are subjected to chemical reaction under the action of a catalyst to generate an intermediate-hydroxylamine salt, then the hydroxylamine salt is reduced in the presence of hydrogen to generate corresponding aliphatic primary amine, the principle of the heating condensation method is that an alicyclic compound and hydrogen are subjected to condensation reaction under the heating condition to generate an alicyclic amide intermediate, then the alicyclic amide is subjected to saturated reduction reaction to generate corresponding alicyclic primary amine, the process of preparing hydrogenated bisphenol A epoxy resin through epoxidation reaction is that firstly bisphenol A is reacted with hydrogen at high temperature to generate hydrogenated bisphenol A, secondly hydrogenated bisphenol A is reacted with an epoxidizing agent such as propylene oxide to generate epoxidized bisphenol A, then the epoxidized bisphenol A is subjected to addition reaction with a compound with amine at the tail end, such as polyamide amine, to generate the alicyclic epoxy resin, firstly the appropriate epoxidizing agent is required to be determined before the alicyclic epoxy resin is prepared, secondly the alicyclic epoxy resin is subjected to the appropriate epoxidizing reaction with the catalyst, and finally the alicyclic compound is subjected to the esterification reaction with the epoxy compound under the existence of the catalyst to generate the alicyclic epoxy resin, and finally the alicyclic epoxy resin is subjected to the esterification reaction with the specific epoxy resin.
In the above embodiment, the specific steps of the ring-opening reaction are as follows:
step1, preparing aliphatic primary amine and alicyclic primary amine;
weighing 8 parts of aliphatic primary amine and alicyclic primary amine according to the ratio of 1:1, putting the mixture into a reaction kettle, uniformly mixing the mixture by adopting a paddle stirrer to obtain a primary amine mixture, and heating the primary amine mixture to 70-80 ℃ by a heater;
step 2, preparing hydrogenated bisphenol A epoxy resin;
2 parts of hydrogenated bisphenol A epoxy resin is weighed and added into a reaction kettle dropwise adding device, and the hydrogenated bisphenol A epoxy resin is heated to 70-80 ℃ through a heater;
Step 3, dropwise adding hydrogenated bisphenol A epoxy resin;
Controlling the temperature in the reaction kettle to be within 50 ℃ through a microwave chemical system, slowly dropwise adding hydrogenated bisphenol A epoxy resin into the primary amine mixture for 1-2 hours, and controlling the dropwise adding speed of a reaction kettle dropwise adding device through a valve in the dropwise adding process;
Step 4, vacuumizing to start reaction;
After the dripping process is finished, firstly, closing the reaction kettle to form a closed space, pumping air or gas from the reaction kettle through a vacuum pump to form a vacuum environment, secondly, adding a catalyst to start the reaction, and in the reaction process, reducing the activation energy of the reaction through a microwave chemical system to improve the reaction rate, wherein the chemical reaction formula of the ring-opening reaction is as follows:
in the reaction scheme (3) of the present invention, Represents a hydrogenated bisphenol A type epoxy resin,Represents primary amine mixture molecules, whereinRepresents an alkyl group of an aliphatic primary amine or an aromatic ring group of an alicyclic primary amine,Represents an aliphatic or cycloaliphatic primary diamine,Represents water;
Step 5, obtaining aliphatic or alicyclic primary diamine;
After the reaction is finished, the mixture is treated by an organic solvent extraction mode, and aliphatic or alicyclic primary di-solvent is dissolved in the organic solvent to obtain aliphatic or alicyclic primary diamine.
In particular embodiments, the ring opening reaction is a type of chemical reaction that is commonly used, and generally refers to the acid catalyzed partial acidolysis of a heterocyclic compound within the ring to form a byproduct without a ring. The principle involves activation of electrophilic or nucleophilic centers inside the heterocyclic compounds under acid (or base) catalysis, thereby undergoing a reaction process of breaking ring bonds, forming side reaction products without rings. The reaction kettle is a device for carrying out chemical reaction, and mainly has the function of promoting chemical reaction between reactants under certain temperature, pressure and other conditions to produce required chemical products, and comprises a reaction container, a paddle stirrer, a heating or cooling device and other components. Wherein the reaction vessel is the main body for reaction and provides the chemical environment needed by chemical reaction in the reaction, and the paddle stirrer is used for uniformly mixing the components and promoting the interaction of reactants so as to accelerate the chemical reaction. The paddle stirrer has the principle that a motor drives a rotary knife to more uniformly distribute the energy of each molecule in a reaction system, so that reaction substances are further and completely mixed, and a heating or cooling device is used for adjusting the temperature in the reaction process. The heating or cooling device provides or absorbs energy to regulate and control the reaction temperature. A vacuum pump is a device for sucking gas and generating vacuum, the principle of which is to suck the gas into the pump by mechanical movement and then to discharge the gas through a connection port with an isolating medium. In the pump, the gas molecules are mechanically squeezed together, increasing the probability of collisions between the gas molecules, which are then sucked into the exhaust channel, creating a vacuum. The oven is used for heating the object to achieve the purposes of drying, baking, sterilizing or baking. The principle is to use a heating element to generate heat, and then transfer the heat to the box and heat the placed object.
In the above embodiment, the microwave chemical system includes a microwave generator, a microwave reflector, a temperature control device and a visualization module, wherein the microwave generator is used for generating microwaves, the microwave reflector is used for generating a microwave radiation field, the temperature control device is used for adjusting the temperature in the reaction kettle, and the visualization module is used for displaying microwave data, microwave radiation energy, temperature data and reaction rate data in real time, and the working mode of the microwave chemical system includes the following steps:
s1, generating microwaves;
The microwave generator generates microwaves through a solid-state oscillation method, and calculates the generated microwave radiation energy through a microwave energy function, wherein the formula of the microwave energy function is as follows:
in the formula (4) of the present invention, In order to radiate energy of the microwaves,Is a constant of planck, which is set to be the planck's constant,The value of (2) isIn order to achieve the light velocity, the light beam is,The value of (2) is,Is the wavelength of the microwave;
S2, forming a uniform microwave radiation field;
the microwave reflector is made into a closed space through a metal material and is arranged at the outer side of the reaction kettle, and the microwave reflector forms a stable and uniform radiation field for microwaves in the microwave reflector based on the interaction of electromagnetic waves and free electrons in the metal;
S3, obtaining and controlling the temperature in the reaction kettle;
The temperature control device collects temperature data in the reaction kettle through an infrared thermometer, the temperature data are transmitted to an RK3288 chip through an RS485 communication protocol, the RK3288 chip outputs a temperature control instruction according to a set reaction temperature threshold value and transmits the temperature control instruction to an actuator, and the actuator controls the operation of a heater or a refrigerator according to the temperature control instruction;
s4, obtaining the reaction rate of the chemical reaction;
The microwave chemical system calculates the reaction rate of chemical reaction in a microwave radiation field through a reaction rate function embedded in an RK3288 chip, and the reaction rate function has the formula:
In the formula (5) of the present invention, For the reaction rate of the chemical reaction,For the activation energy of the chemical reaction,In order to radiate energy of the microwaves,In order to react the energy required for the reaction,As a factor of the frequency of the signal,Is a gas constant which is a function of the gas,Is the temperature in the reaction kettle;
S5, displaying in real time;
The visualization module displays the generated microwave data, microwave radiation energy, temperature data and reaction rate data in real time through the Internet of things platform.
In a specific embodiment, an application platform of the microwave chemical system may be constructed, and during operation of the platform, a hardware platform may be constructed, such as by constructing a programmable controller, a storage device, a microwave generator, an infrared thermometer, a heater, a refrigerator, a bus, and a display, as described in more detail below:
The programmable controller can realize the basic operations of carrying out arithmetic and logic operation on data and reading and storing the data in the memory.
Storage devices-microwave chemical systems need to store large amounts of data, and data needs to be read and written quickly during operation, so that high-speed storage devices such as SSD (solid state drive) or NVMe (nonvolatile memory extension) need to be used.
The microwave generator is used for generating microwave signals.
Infrared thermometer the infrared thermometer is used to measure the infrared energy radiated from the surface of the reactor to determine the temperature of the reactor.
The heater is used for providing heat for the reaction kettle so as to increase the temperature of the reaction kettle.
And the refrigerator absorbs heat from the air or the reaction kettle by utilizing the process of compression and expansion of the refrigerant and discharges the heat outside the reaction kettle, so that the temperature of the reaction kettle is reduced.
The bus is used for connecting all the components of the equipment, and the communication and coordination among all the components are realized through data, control and address information transmission.
The display is used for displaying the running state and parameters of the system and providing a window for a user to observe and adjust the parameters in time.
Under the cooperation of the hardware components, the operation of the microwave chemical system can be realized according to specific application requirements and system requirements, and the working state of the plasma purifier is controlled by outputting a control instruction according to current air quality data in practical application, so that the use energy consumption of the plasma purifier is reduced, the total use energy consumption of a commercial refrigerator is further reduced, and the use cost is reduced.
In a specific embodiment, the microwave generator is used to generate a high frequency microwave signal. The main principle is that the feedback function in the microwave oscillating circuit is utilized to make the resonant circuit in the circuit produce self-oscillation, so as to produce stable high-frequency microwave signal. The method comprises the following steps of 1. Generating an excitation signal, wherein an excitation signal generator is arranged in a microwave generator, and a stable high-frequency excitation signal is generated through an oscillator or other electronic components. 2. Signal amplification, namely, the excitation signal is passed through an amplifier to reach enough amplitude. 3. Generating a resonant tank in a microwave generator, a resonant tank is generated using a resonant cavity in a microwave circuit. 4. The oscillation circuit is self-excited, the amplified excitation signal is connected with the resonance circuit through a coupler, and a feedback effect is generated. If the output energy is enough, the feedback signal will repeatedly jump in the resonant circuit and form a stable microwave resonant circuit. In this oscillator, the frequency of the resonator is matched to the time step of the feedback loop, thereby generating a microwave signal. 5. And outputting a microwave signal, namely outputting the microwave signal generated by the resonant circuit in the circuit from an output interface, so that the microwave generator can realize the required microwave power output, and measuring by using the characteristic of infrared radiation energy by using the infrared thermometer. The infrared sensor consists of one photosensitive element and one optical system and has the temperature measuring principle that the surface of the object emits infrared radiation outwards when the temperature is higher than absolute zero, the infrared sensor captures the radiation energy and converts it into electric signal, the infrared sensor quantizes the radiation energy to convert it into voltage signal and output it in certain proportion, and the infrared thermometer converts the output voltage signal into the temperature of the surface of the object via internal algorithm and calibration parameters. The principle of the heater is to convert electric energy or other energy into heat energy to raise the temperature of the heated object. The commonly used heater is an electric heater, which generates heat energy by means of resistive heating. The principle of the refrigerator is to lower the temperature of an object using a refrigerating cycle of a refrigerant. The refrigeration cycle generally includes four basic components, a compressor, a condenser, an expansion valve, and an evaporator. Wherein the compressor in charge of pressurizing the refrigerant compresses the low-temperature and low-pressure gas to raise its temperature and pressure. The condenser cools the compressed gas by discharging the heat of the refrigerant and converts the compressed gas into a high-pressure high-temperature liquid. The liquid refrigerant is then throttled by the expansion valve, causing its pressure to drop and the temperature to drop. Finally, the refrigerant flows through the evaporator to absorb heat on the surface of the object to be refrigerated, so that the aim of refrigeration is fulfilled.
Examples
In the embodiment, the composition parts by weight of the seam beautifying agent A comprises 60 parts of modified polyurea resin A, 4 parts of hydrophobic fumed silica, 1 part of molecular sieve, 20 parts of filling powder and 1 part of defoaming agent, and the composition parts by weight of the seam beautifying agent B comprises 50 parts of modified polyurea curing agent B, 3 parts of hydrophobic fumed silica, 1 part of molecular sieve, 30 parts of filling powder, 3 parts of toner and 1 part of defoaming agent.
The mass percentages of the raw materials in the steps are shown in Table 5:
the embodiment of the invention is now illustrated, wherein 2 groups of examples are compared, 4 pieces of to-be-stitched areas with the same material and position are adopted for testing in the comparison process, the test times are 4 times, wherein when 4 pieces of to-be-stitched areas with the same material and position are tested, 2 pieces of to-be-stitched areas are adopted for testing, polyurea stitching agent is recorded as a comparison area 1 and a comparison area 2, the stitching agent with the formula is adopted as a test area 1 and a test area 2, the to-be-stitched areas are treated by using different types of stitching agents, the results after the treatment are observed and recorded are shown in a comparison meaning table 6:
the dispersity, impurity content and moisture content of the joint beautifying agent directly influence the performance of the joint beautifying agent, and the Shore hardness of the joint beautifying agent reflects the wear resistance, pressure resistance and durability of the joint beautifying agent, so that the performance indexes such as the Shore hardness, the dispersity, the impurity content and the moisture content are extremely important for the formula of the joint beautifying agent.
Examples
In the embodiment, the composition parts by weight of the seam beautifying agent A comprises 80 parts of modified polyurea resin A, 6 parts of hydrophobic fumed silica, 3 parts of molecular sieve, 40 parts of filling powder and 3 parts of defoamer, and the composition parts by weight of the seam beautifying agent B comprises 70 parts of modified polyurea curing agent B, 6 parts of hydrophobic fumed silica, 3 parts of molecular sieve, 50 parts of filling powder, 5 parts of toner and 3 parts of defoamer.
The mass percentages of the raw materials in the steps are shown in Table 7:
The embodiment of the invention is now illustrated, wherein 2 groups of examples are compared, 4 pieces of to-be-stitched areas with the same material and position are adopted for testing in the comparison process, the test times are 4 times, wherein when 4 pieces of to-be-stitched areas with the same material and position are tested, 2 pieces of to-be-stitched areas are adopted for testing, polyurea stitching agent is recorded as a comparison area 1 and a comparison area 2, the stitching agent with the formula is adopted as a test area 1 and a test area 2, the to-be-stitched areas are treated by using different types of stitching agents, the results after the treatment are observed and recorded are shown in a comparison meaning table 8:
through experiments, in the scheme of the invention, the performance index of the seam beautifying agent adopted by the invention is obviously higher than that of the polyurea seam beautifying agent, and the invention has outstanding technical effects and obvious technical progress.
In the above embodiment, the hydrophobic fumed silica increases the dispersity of the raw materials in the modified polyurea resin a by dispersing action, increases the rheological property of the modified polyurea resin a, the filler powder increases the density and durability of the modified polyurea resin a by filling voids, the molecular sieve adsorbs impurities and moisture in the agent a by means of combination of physical adsorption and chemical adsorption, so as to achieve the purpose of purifying the agent a, the defoamer eliminates or prevents the formation of bubbles by reducing the surface tension between the agent a and air, and the toner changes the color of the agent B by means of the colorant.
In the specific embodiment, after the hydrophobic fumed silica is added into the modified polyurea resin A, particles in the modified polyurea resin A are more uniformly distributed in the whole system through the dispersion effect, so that the accumulation among the particles is avoided, the dispersion degree of raw materials is improved, and the hydrophobic fumed silica has a certain surface area and pore structure on the basis of the dispersion effect, so that the surface area and the gap of the modified polyurea resin A can be increased, and the rheological property of the coating is improved; the filling powder fills the gaps in the modified polyurea resin A to increase the density of the material, so as to improve the mechanical property and the compressive strength of the material, and simultaneously, the filling powder can increase the thickness of the coating, isolate the entry of external substances such as air, water and the like, and improve the quality and the durability of the coating, the physical adsorption is that the lattice structure of the molecular sieve has porosity and can form a large number of micropores and mesopores, impurities and moisture in target molecules are adsorbed into pore channels through the physical adsorption actions such as electrostatic interaction, van der Waals force, hydrogen bond and the like to reduce the impurity and the moisture content in the agent A, the chemical adsorption is that the surface of the molecular sieve is provided with a plurality of active centers, namely chemical functional groups, which can react with some molecules in the impurity and the moisture in the agent A to form chemical bonds or ionic bonds, so as to reduce the impurity and the moisture content in the agent A, the action principle of the defoamer is that the surface tension is changed through the molecular structure of the self and the adsorption action on the surface of the material, so that bubbles are broken, vanished or the residual light of the color powder is prevented from forming the residual light of the specific wavelength by the color powder, thereby changing the color of the seam beautifying agent B.
In the above embodiment, the construction steps of the epoxy resin modified aspen polyurea joint beautifying agent are as follows:
S01, cleaning gaps;
Firstly, cleaning cement dust in the gap by using an art designer knife at an angle of 45 degrees, sucking dust impurities by using a dust collector, cleaning black edges of the ceramic tile by using a multifunctional decontamination paste, and wiping the gap and the surface of the tile by using a dry towel to ensure that the construction environment is clean and dry;
S02, waxing the periphery of the gap;
A proper amount of seam wax is dipped by sponge and beaten on the surfaces of the ceramic tiles at two sides of the seam, so that the residual materials can be conveniently shoveled off at the back;
S03, driving the seam beautifying agent into the seam;
Firstly, a 40cm seam beautifying agent is punched out without being used, so that uneven mixing of the seam beautifying agent A and the seam beautifying agent B is avoided, then a glue nozzle is attached to a seam, the included angle between a glue gun and the seam is larger than 60 degrees, glue is punched vertically at a uniform speed, and the tip of the glue gun is enabled to fully inject the seam beautifying agent into the seam, and the seam is fully punched and compacted;
S04, caulking;
after the sizing is finished, starting to press the sizing, firstly adopting a metal groove pressing cutter to test pressure, confirming the fluidity and the adhesive force of the joint beautifying agent, then keeping stable force application, and dragging a silica gel rod at uniform speed to finish the sizing;
s05, cleaning the residue;
After the seam beautifying agent is solidified, the residual materials are shoveled by a shovel blade, and the seam beautifying operation is completed.
In the specific embodiment, in the first step, the gap is cleaned, and the reason that the gap needs to be cleaned before the glue is applied is that if the surface of the ceramic tile and the gap are not cleaned, and the environment is moist, a large amount of dust and impurities exist in the air, which will affect the adhesive force and the gap-beautifying effect of the gap-beautifying agent. Therefore, the construction environment is thoroughly cleaned, the drying and the cleaning of the construction environment are ensured, the quality and the effect of the beautiful joint are improved, and the concrete operation is that firstly, cement dust in the joint is cleaned by using an art designing knife, and then, the dust and impurities in the joint are sucked by using a dust collector. Next, the black edges of the tiles can be cleaned with a multifunctional cleaning paste. The multifunctional decontamination paste has multiple functions of decontamination, wiping, polishing and the like, can effectively remove dirt and black edges, and needs to wipe gaps and brick surfaces with a dry towel after the cleaning work is completed so as to ensure that the construction environment is clean and dry.
And secondly, waxing, wherein the waxing effect is beneficial to the subsequent shoveling and cleaning of the redundant seam beautifying agent, and the method comprises the specific steps of dipping a proper amount of seam beautifying wax by using a clean sponge, then placing the sponge dipped with the seam beautifying wax on a slit, and forcefully extruding the seam beautifying wax into the slit. In the process, the consumption of the seam-beautifying wax is controlled, so that waste and construction non-uniformity are avoided. At the same time of extruding the seam wax, the surface of the ceramic tile is also coated, so that the residual materials are easy to be shoveled off in the subsequent cleaning.
Thirdly, the glue is beaten, the seam beautifying agent A and the seam beautifying agent B are required to be mixed before use, so that the seam beautifying agent of about 40cm is required to be beaten before glue is beaten, and the mixture is placed aside for standby, the seam-beautifying agent A and the seam-beautifying agent B are prevented from being mixed unevenly, the glue nozzle can be attached to the seam, the included angle between the glue gun and the seam is larger than 60 degrees, uniform force is kept to vertically glue, and the seam-beautifying agent is guaranteed to be fully filled in the seam.
And fourthly, pressing glue, namely firstly using a metal groove pressing knife to test pressure, confirming the fluidity and the adhesive force of the joint beautifying agent, judging whether the glue pressing of the whole joint beautifying agent achieves the expected effect, if the fluidity of the joint beautifying agent is poor, the adhesive force is not strong, or the expected glue pressing effect is not achieved, adjusting the application amount of the construction method or the joint beautifying agent in time, and after confirming the fluidity and the adhesive force of the joint beautifying agent, performing formal glue pressing. And (5) keeping stable force application, and dragging the metal grooving cutter at uniform speed to finish the glue pressing. When the glue is pressed, a glue pressing mode from the center to the two sides and then from the two sides to the center is adopted, so that the construction quality of the joint beautifying agent is prevented from being influenced. Meanwhile, the size and the uniformity of the applied force are controlled, the principles of uniform force and moderate force are maintained, the gap filling agent is ensured to fully fill the gap, the compaction is firm, and meanwhile, the neatness and smoothness of the surface of the ceramic tile are ensured.
And fifthly, cleaning the excess materials, and cleaning the excess seam-beautifying agent in time after the seam-beautifying agent is solidified so as to ensure the quality and the attractiveness of the seam-beautifying engineering. Specifically, the extra seam beautifying agent is shoveled off by a shovel blade so as to facilitate the subsequent cleaning operation. When the excess seam-beautifying agent is shoveled, the quality and the effect of the seam-beautifying agent are checked, and if the conditions of foaming, cracking, falling and the like of the seam-beautifying agent are found, the seam-beautifying agent needs to be repaired and treated in time so as to ensure that the seam-beautifying effect meets the expected requirement.
While specific embodiments of the present invention have been described above, it will be understood by those skilled in the art that these specific embodiments are by way of example only, and that various omissions, substitutions, and changes in the form and details of the methods and systems described above may be made by those skilled in the art without departing from the spirit and scope of the invention. For example, it is within the scope of the present invention to combine the above-described method steps to perform substantially the same function in substantially the same way to achieve substantially the same result. Accordingly, the scope of the invention is limited only by the following claims.

Claims (5)

1.一种环氧树脂改性天冬聚脲美缝剂的制备方法，其特征在于：包括以下步骤：1. A method for preparing an epoxy resin modified asparagine polyurea seam beautifying agent, characterized in that it comprises the following steps: 步骤一、准备原材料；Step 1: Prepare raw materials; 所述原材料的组分重量份数包括脂肪族伯胺3-4份、脂环族伯胺3-4份、氢化双酚A型环氧树脂1.6-2份、马来酸二乙酯0.4-0.5份、马来酸二丁酯0.4-0.5份、异氰酸酯4-5份、聚醚多元醇2-3份和稳定剂0.9-1份；The components of the raw materials include 3-4 parts of aliphatic primary amine, 3-4 parts of alicyclic primary amine, 1.6-2 parts of hydrogenated bisphenol A epoxy resin, 0.4-0.5 parts of diethyl maleate, 0.4-0.5 parts of dibutyl maleate, 4-5 parts of isocyanate, 2-3 parts of polyether polyol and 0.9-1 parts of stabilizer by weight; 步骤二、进行开环反应生成脂肪族和脂环族伯二胺；Step 2: performing a ring-opening reaction to generate aliphatic and alicyclic primary diamines; 通过开环反应将脂肪族伯胺和脂环族伯胺与氢化双酚A型环氧树脂进行化学反应生成脂肪族和脂环族伯二胺，所述开环反应通过微波化学系统控制反应过程；The aliphatic primary amine and the alicyclic primary amine are chemically reacted with the hydrogenated bisphenol A type epoxy resin to generate aliphatic and alicyclic primary diamines through a ring-opening reaction, wherein the ring-opening reaction is controlled by a microwave chemical system; 步骤三、获得改性聚脲树脂A；Step 3, obtaining modified polyurea resin A; 通过加成反应将脂肪族和脂环族伯二胺与马来酸二乙酯和马来酸二丁酯进行反应，生成改性聚脲树脂A，所述加成反应的化学反应示意图为:Aliphatic and alicyclic primary diamines are reacted with diethyl maleate and dibutyl maleate by addition reaction to generate modified polyurea resin A. The chemical reaction diagram of the addition reaction is as follows: 在反应式（1）中，表示马来酸二乙酯和马来酸二丁酯，表示脂肪族和脂环族伯二胺，表示改性聚脲树脂A；In reaction formula (1), represents diethyl maleate and dibutyl maleate, denotes aliphatic and alicyclic primary diamines, Represents modified polyurea resin A; 步骤四、获得改性聚脲固化剂B；Step 4, obtaining modified polyurea curing agent B; 通过添加稳定剂H3PO3与异氰酸酯HDI发生加成反应，生成稳定的有机异氰酸酯化合物，以实现降低异氰酸酯反应活性的目的，并将有机异氰酸酯化合物与聚醚多元醇混合反应生成改性聚脲固化剂B，所述加成反应的化学反应示意图为：By adding stabilizer H 3 PO 3 to react with isocyanate HDI, a stable organic isocyanate compound is generated to achieve the purpose of reducing the reactivity of isocyanate, and the organic isocyanate compound is mixed with polyether polyol to react to generate modified polyurea curing agent B. The chemical reaction diagram of the addition reaction is as follows: 在反应式（2）中，表示稳定剂，表示异氰酸酯聚合物链的末端基团，表示有机异氰酸酯化合物，In reaction (2), Indicates stabilizer, represents the terminal group of the isocyanate polymer chain, represents an organic isocyanate compound, 步骤五、制备美缝剂A剂和美缝剂B剂；Step 5, preparing seam beautifying agent A and seam beautifying agent B; 首先，通过步骤二和步骤三获得改性聚脲树脂A，通过步骤四获得改性聚脲固化剂B，美缝剂A剂的组分重量份数包括改性聚脲树脂A60-80份、疏水气相二氧化硅4-6份、分子筛1-3份、填充粉20-40份和消泡剂1-3份，美缝剂B剂的组分重量份数包括改性聚脲固化剂B50-70份、疏水气相二氧化硅3-6份、分子筛1-3份、填充粉30-50份、色粉3-5份和消泡剂1-3份，分别获得美缝剂A剂和美缝剂B剂，其中疏水气相二氧化硅、填充粉、分子筛、消泡剂和色粉从化工市场购买获得。First, a modified polyurea resin A is obtained through steps two and three, and a modified polyurea curing agent B is obtained through step four. The components of the caulking agent A include 60-80 parts of modified polyurea resin A, 4-6 parts of hydrophobic fumed silica, 1-3 parts of molecular sieves, 20-40 parts of filler powder and 1-3 parts of defoaming agent in weight parts, and the components of the caulking agent B include 50-70 parts of modified polyurea curing agent B, 3-6 parts of hydrophobic fumed silica, 1-3 parts of molecular sieves, 30-50 parts of filler powder, 3-5 parts of color powder and 1-3 parts of defoaming agent in weight parts, to obtain caulking agent A and caulking agent B respectively, wherein the hydrophobic fumed silica, filler powder, molecular sieve, defoaming agent and color powder are purchased from the chemical market. 2.根据权利要求1所述的一种环氧树脂改性天冬聚脲美缝剂的制备方法，其特征在于：所述开环反应的具体步骤如下：2. The method for preparing an epoxy resin modified asparagine polyurea seam beautifying agent according to claim 1, characterized in that the specific steps of the ring-opening reaction are as follows: 步骤1、准备脂肪族伯胺和脂环族伯胺；Step 1, preparing aliphatic primary amine and alicyclic primary amine; 按照脂肪族伯胺：脂环族伯胺=1：1的比例称取8份投入反应釜中，采用桨式搅拌器将混合物混合均匀，获得伯胺混合物；8 parts of aliphatic primary amine and alicyclic primary amine were weighed and put into a reaction kettle in a ratio of 1:1, and the mixture was mixed evenly with a paddle stirrer to obtain a primary amine mixture; 步骤2、准备氢化双酚A型环氧树脂；Step 2, preparing hydrogenated bisphenol A epoxy resin; 称取氢化双酚A型环氧树脂2份加入反应釜滴加器中；Weigh 2 parts of hydrogenated bisphenol A epoxy resin and add it into the reactor dropper; 步骤3、滴加氢化双酚A型环氧树脂；Step 3, adding hydrogenated bisphenol A epoxy resin dropwise; 通过微波化学系统将反应釜内的温度控制在50℃以内，并将氢化双酚A型环氧树脂缓慢滴加入伯胺混合物中，滴加时间持续1-2个小时，在滴加过程中，通过阀门控制反应釜滴加器滴加的速度；The temperature in the reactor is controlled within 50° C. by a microwave chemical system, and the hydrogenated bisphenol A epoxy resin is slowly added dropwise to the primary amine mixture for 1-2 hours. During the addition process, the speed of the reactor dropper is controlled by a valve; 步骤4、抽真空开始反应；Step 4, vacuumize and start the reaction; 滴加过程完成后，首先，闭合反应釜形成密闭空间，通过真空泵将空气或气体从反应釜中抽出，形成真空环境，其次，加入催化剂开始反应，在反应过程中，通过微波化学系统降低反应的活化能，提高反应速率，After the dropwise addition process is completed, first, the reactor is closed to form a closed space, and the air or gas is pumped out of the reactor through a vacuum pump to form a vacuum environment. Secondly, the catalyst is added to start the reaction. During the reaction, the microwave chemical system is used to reduce the activation energy of the reaction and increase the reaction rate. 步骤5、获得环氧树脂改性脂肪族和脂环族伯二胺；Step 5, obtaining epoxy resin modified aliphatic and alicyclic primary diamines; 反应完成后，通过有机溶剂萃取的方式对混合物进行处理，将脂肪族和脂环族伯二溶于有机溶剂中，获得脂肪族和脂环族伯二胺。After the reaction is completed, the mixture is treated by extraction with an organic solvent, and the aliphatic and alicyclic primary diamines are dissolved in the organic solvent to obtain the aliphatic and alicyclic primary diamines. 3.根据权利要求2所述的一种环氧树脂改性天冬聚脲美缝剂的制备方法，其特征在于：所述微波化学系统包括微波发生器、微波反射体、温度控制装置和可视化模块，所述微波发生器用于产生微波，所述微波反射体用于产生微波辐射场，所述温度控制装置用于调节反应釜中的温度，所述可视化模块用于实时展示微波数据、微波辐射能量、温度数据和反应速率数据，所述微波化学系统的工作方式包括以下步骤：3. The method for preparing an epoxy resin modified asparagine polyurea seam beautifying agent according to claim 2, characterized in that: the microwave chemical system comprises a microwave generator, a microwave reflector, a temperature control device and a visualization module, the microwave generator is used to generate microwaves, the microwave reflector is used to generate a microwave radiation field, the temperature control device is used to adjust the temperature in the reactor, and the visualization module is used to display microwave data, microwave radiation energy, temperature data and reaction rate data in real time, and the working mode of the microwave chemical system comprises the following steps: S1产生微波；S1 generates microwaves; 所述微波发生器通过固态振荡法产生微波，并通过微波能量函数计算出产生的微波辐射能量，所述微波能量函数的公式为：The microwave generator generates microwaves by a solid-state oscillation method, and calculates the generated microwave radiation energy by a microwave energy function. The formula of the microwave energy function is: 在公式（4）中，为微波辐射能量，为普朗克常数，的值为6.626×10-34J·s， 为光速，的值为2.99792458×108m/s，为微波的波长；In formula (4), is the microwave radiation energy, is Planck's constant, The value of is 6.626×10 -34 J·s, is the speed of light, The value of is 2.99792458×10 8 m/s, is the wavelength of microwaves; S2形成均匀的微波辐射场；S2 forms a uniform microwave radiation field; 所述微波反射体通过金属材料制成密闭空间，安置在反应釜的外侧，所述微波反射体基于电磁波与金属中自由电子的相互作用将微波反射体内的微波形成一个稳定、均匀的辐射场；The microwave reflector is made of metal material to form a closed space and is placed outside the reactor. The microwave reflector forms a stable and uniform radiation field based on the interaction between electromagnetic waves and free electrons in the metal. S3获得并控制反应釜中的温度；S3 obtains and controls the temperature in the reactor; 所述温度控制装置通过红外线温度计采集反应釜中的温度数据，并通过RS485通信协议将温度数据传输至RK3288芯片，所述RK3288芯片根据设定的反应温度阈值输出温度控制指令，并将温度控制指令传输至执行器，所述执行器根据温度控制指令控制加热器或制冷器的运行；The temperature control device collects temperature data in the reactor through an infrared thermometer, and transmits the temperature data to the RK3288 chip through the RS485 communication protocol. The RK3288 chip outputs a temperature control instruction according to a set reaction temperature threshold, and transmits the temperature control instruction to the actuator. The actuator controls the operation of the heater or refrigerator according to the temperature control instruction; S4获得化学反应的反应速率；S4 obtains the reaction rate of a chemical reaction; 所述微波化学系统通过嵌入RK3288芯片的反应速率函数计算出微波辐射场中化学反应的反应速率，所述反应速率函数的公式为：The microwave chemical system calculates the reaction rate of the chemical reaction in the microwave radiation field through the reaction rate function embedded in the RK3288 chip. The formula of the reaction rate function is: 在公式（5）中，为化学反应的反应速率，为化学反应的活化能，为微波辐射能量，为反应需要的能量，为频率因子，为气体常数，为反应釜中的温度；In formula (5), is the reaction rate of the chemical reaction, is the activation energy of the chemical reaction, is the microwave radiation energy, The energy required for the reaction, is the frequency factor, is the gas constant, is the temperature in the reactor; S5进行实时显示；S5 for real-time display; 所述可视化模块通过物联网平台将产生的微波数据、微波辐射能量、温度数据和反应速率数据进行实时显示。The visualization module displays the generated microwave data, microwave radiation energy, temperature data and reaction rate data in real time through the Internet of Things platform. 4.根据权利要求1所述的一种环氧树脂改性天冬聚脲美缝剂的制备方法，其特征在于：所述疏水气相二氧化硅通过分散作用增加改性聚脲树脂A中原料的分散度，增加改性聚脲树脂A的流变性能，所述填充粉通过填充空隙增加改性聚脲树脂A的密度和耐久性，所述分子筛采用物理吸附和化学吸附结合的方式吸附美缝剂A剂中的杂质和水分，以实现净化美缝剂A剂的目的，所述消泡剂通过降低美缝剂A剂与空气之间的表面张力，消除或预防气泡的形成，所述色粉通过着色剂改变美缝剂B剂的颜色。4. The method for preparing an epoxy resin modified asparagus polyurea seam beautifying agent according to claim 1, characterized in that: the hydrophobic fumed silica increases the dispersion of raw materials in the modified polyurea resin A by dispersing action, and increases the rheological properties of the modified polyurea resin A; the filling powder increases the density and durability of the modified polyurea resin A by filling gaps; the molecular sieve adsorbs impurities and moisture in the seam beautifying agent A by combining physical adsorption and chemical adsorption to achieve the purpose of purifying the seam beautifying agent A; the defoaming agent eliminates or prevents the formation of bubbles by reducing the surface tension between the seam beautifying agent A and the air; and the color powder changes the color of the seam beautifying agent B by a colorant. 5.根据权利要求1所述的一种环氧树脂改性天冬聚脲美缝剂的制备方法，其特征在于：所述环氧树脂改性天冬聚脲美缝剂的施工步骤如下：5. The method for preparing an epoxy resin modified asparagine polyurea seam beautifying agent according to claim 1, characterized in that the construction steps of the epoxy resin modified asparagine polyurea seam beautifying agent are as follows: S01清理缝隙；S01 Clean the gap; 先用美工刀斜45度清理缝隙中的水泥灰尘，并借助吸尘器吸净灰尘杂质，然后用多功能去污膏清理瓷砖黑边，再使用干燥的毛巾擦拭缝隙及砖面，保证施工环境干净干燥；First, use a utility knife to clean the cement dust in the gap at a 45-degree angle, and use a vacuum cleaner to remove dust and impurities. Then use a multi-functional decontamination paste to clean the black edges of the tiles, and then use a dry towel to wipe the gaps and brick surfaces to ensure that the construction environment is clean and dry. S02在缝隙周边打蜡；S02 waxes around the gap; 用海绵蘸取适量美缝蜡，打在缝隙两侧的瓷砖表面，便于后面铲除余料；Dip a sponge in a proper amount of caulking wax and apply it on the tile surfaces on both sides of the gap to facilitate the removal of excess material later; S03将美缝剂打入缝隙中；S03 inject the caulking agent into the gap; 先打出40cm美缝剂不用，避免美缝剂A剂与B剂混合不均匀，再把胶嘴贴合缝隙，胶枪与缝隙夹角大于60度，直立匀速打胶，使胶枪尖嘴充分把美缝剂注入到缝隙里面，打满打实；First, apply 40cm of caulking agent to avoid uneven mixing of caulking agent A and agent B. Then, fit the glue nozzle to the gap. The angle between the glue gun and the gap should be greater than 60 degrees. Apply glue at a constant speed in an upright position. Make sure the glue gun tip fully injects the caulking agent into the gap and fills it up. S04压缝；S04 press seam; 在打胶完成后开始压胶，先采用金属压槽刀进行试压，确认美缝剂的流动性和粘附力，然后保持稳定的施力，均速拖动硅胶棒完成压胶；After the glue is applied, start pressing the glue. First, use a metal groove knife to test the pressure to confirm the fluidity and adhesion of the caulking agent. Then maintain a stable force and drag the silicone rod at a constant speed to complete the pressing. S05清理余料；S05 clean up the remaining materials; 待美缝剂固化后，用铲刀铲除余料，完成美缝操作。After the caulking agent solidifies, use a spatula to remove the remaining material to complete the caulking operation.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101817924A (en) * 2010-03-19 2010-09-01 上海市建筑科学研究院(集团)有限公司 Method for preparing novel polyaspartic ester and application thereof
CN109999009A (en) * 2019-03-14 2019-07-12 重庆医药高等专科学校 A kind of anti-tumor drug oral slow-releasing preparation and preparation method thereof

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2095832A1 (en) * 2008-02-28 2009-09-02 Bayer MaterialScience AG Post-operative adhesion barriers
JP2010248303A (en) * 2009-04-13 2010-11-04 Aica Kogyo Co Ltd Polyurea urethane adhesive composition and film laminate
KR102662508B1 (en) * 2021-04-20 2024-05-02 애경케미칼주식회사 Pot life and hardness adjustable polyol modified aspartic two components type poly urea resin composition and the manufacturing method thereof
KR102520941B1 (en) * 2021-04-28 2023-04-13 애경케미칼주식회사 Room temperature curing and hardness adjustable polyol modified aspartic two components type poly urea heat dissipation adhesive composition

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101817924A (en) * 2010-03-19 2010-09-01 上海市建筑科学研究院(集团)有限公司 Method for preparing novel polyaspartic ester and application thereof
CN109999009A (en) * 2019-03-14 2019-07-12 重庆医药高等专科学校 A kind of anti-tumor drug oral slow-releasing preparation and preparation method thereof

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