CN111646909A - Preparation method and application of alcohol amine compound capable of improving early strength of cement - Google Patents
Preparation method and application of alcohol amine compound capable of improving early strength of cement Download PDFInfo
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- CN111646909A CN111646909A CN202010327064.8A CN202010327064A CN111646909A CN 111646909 A CN111646909 A CN 111646909A CN 202010327064 A CN202010327064 A CN 202010327064A CN 111646909 A CN111646909 A CN 111646909A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/04—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reaction of ammonia or amines with olefin oxides or halohydrins
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/12—Nitrogen containing compounds organic derivatives of hydrazine
- C04B24/122—Hydroxy amines
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/10—Accelerators; Activators
- C04B2103/12—Set accelerators
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/52—Grinding aids; Additives added during grinding
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
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- Chemical Kinetics & Catalysis (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a preparation method and application of an alcohol amine compound for improving early strength of cement, wherein the prepared alcohol amine compound is monoethanol dipropyleneglycol amine, and the preparation method specifically comprises the following steps: s1, adding monoethanolamine, a small amount of water and a catalyst into a reactor in sequence, heating to 30-55 ℃ in an inert gas atmosphere, S2, continuously dropwise adding epoxy propanol within 1-4 hours, and S3, adding water to adjust the water content to 14-16% to obtain the monoethanol dipropyleneglycol amine. The alcohol amine compound capable of improving the early strength of the cement is mainly used as a cement grinding aid, can provide higher early strength of the cement, and has a more obvious effect under the condition of less addition amount. The invention is prepared by taking monoethanolamine and epoxypropanol as raw materials and water as a catalyst through reaction, and the preparation conditions are simple and mild.
Description
Technical Field
The invention relates to the technical field of chemical building materials, in particular to a preparation method and application of an alcohol amine compound for improving the early strength of cement.
Background
The cement grinding aid is an additive used in the cement grinding process, can obviously improve the grinding efficiency, reduces the power consumption in the cement grinding process, and is beneficial to the cost management of cement enterprises. The cement grinding aid mainly comprises alcamines, representative alcamine compounds with enhanced grinding aid performance mainly comprise triethanolamine, triisopropanolamine, diethanol monoisopropanolamine, monoethanoldiisopropanolamine, methyldiethanolamine, tetrahydroxyethylethylenediamine and the like, and the most commonly used compounds comprise triethanolamine, triisopropanolamine and diethanol monoisopropanolamine.
The early performance is an important index performance requirement in many cement/concrete projects such as precast concrete frameworks, reinforced concrete, roads and bridges, renovation and reinforcement thereof and the like. The early strength agent is used, so that the production period can be obviously shortened for the precast concrete member and the steam-cured concrete, and the production efficiency is improved; the early strength agent is applied to road and bridge and renovating and reinforcing engineering, so that the construction period can be shortened, and the road and the bridge can be opened as soon as possible.
Commonly used early strength agents include both inorganic and organic classes. The existing organic early strength agents are represented by organic alcohol amine and calcium formate, wherein the organic alcohol amine early strength agents are most commonly used, and have the advantages of small dosage (usually ten-thousandth of ten minutes) and wide adaptive temperature range (from-5 ℃ to 90 ℃) which can play an early strength role, no corrosion to reinforcing steel bars and no influence on later strength compared with inorganic early strength agents (sodium sulfate, sodium nitrate, sodium carbonate, sodium sulfite, sodium nitrite, potassium sulfate, potassium nitrate, potassium carbonate and other alkali metal or alkaline earth metal strong electrolyte inorganic salts).
Currently, the most commonly used organic alkanolamines as early strength agents include triethanolamine, diethanol monoisopropanolamine, and monoethanol diisopropanolamine.
Patent CN201610392181 discloses a cement/concrete early strength agent which is prepared by taking diethanolamine and epoxypropanol as raw materials and isopropanol as a solvent, and reacting to obtain a product, diethanol mono-dipropanolamine. The alcohol amine compound is used as an early strength agent, has excellent early strength performance, has good adaptability with a polycarboxylic acid water reducing agent and an inorganic salt early strength agent, and has early strength performance superior to organic early strength agents such as triethanolamine, diethanol monoisopropanolamine and the like. However, the problem that the early strength of cement is too low when the traditional grinding aid is used is still not solved by trying the alcohol amine compound, and the development of a stronger polar alcohol amine compound as an early strength agent is urgently needed.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a preparation method and application of an alcohol amine compound for improving the early strength of cement, which have a more obvious effect under the condition of less addition of an early strength agent, and further, the compound can well solve the problem that the increase value of the early strength of the cement is too low when a traditional grinding aid is used.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme: the preparation method of the alcohol amine compound for improving the early strength of the cement comprises the following steps:
the preparation method of the alcohol amine compound provided by the invention is prepared by the reaction of monoethanolamine and epoxypropanol in the presence of a catalyst, and the basic reaction can be schematically shown as follows:
the preparation method of the alcohol amine compound-ethanol dipropanediol amine specifically comprises the following steps:
s1, sequentially adding monoethanolamine, a small amount of water and a catalyst into a reactor, and heating to 30-55 ℃ in an inert gas atmosphere;
s2, continuously dripping epoxypropanol within 1-4 hours, controlling the reaction temperature within the range of 40-65 ℃, and continuously preserving heat for 1-1.5 hours after finishing dripping the epoxypropanol;
s3, adding water to adjust the water content to 14-16% to obtain the monoethanol dipropyleneglycol amine.
Preferably, in the step S1, the content of monoethanolamine is 65.00% to 99.99% by mass, the content of water in monoethanolamine is 0.01% to 35.00% by mass, and the balance is mainly water.
Preferably, the catalyst in step S1 is an organic weak acid, and the organic weak acid is one of formic acid, acetic acid, propionic acid or lactic acid, preferably formic acid, and the organic acid catalyst is favorable for accelerating the reaction speed, improving the reaction selectivity, and reducing the content of alcohol ether by-products in the product.
Preferably, the molar ratio of the organic weak acid to the monoethanolamine in the catalyst is 0.0001-0.03: 1, the catalytic effect is not obvious when the catalyst is less than the range, and the problem of excessive by-product of alcohol ether is caused when the catalyst is beyond the range.
Preferably, in step S2, the molar ratio of monoethanolamine to glycidol is 1: 1.98-2.05, the amount of glycidol added is less than this range, the amount of monoethanolamine is more than this range, the amount of monoethanolamine remaining is more than this range, monoethanolamine is preferred, glycidol is 1:2.02, and the amount of monoethanolamine remaining is controlled to be less than 1%.
Preferably, the preparation method comprises the following steps:
t1, placing monoethanolamine in a reaction container, dropwise adding epoxypropanol according to a certain proportion under the stirring condition in an inert gas atmosphere, and controlling the dropwise adding speed of the epoxypropanol to enable the reaction temperature to be in the range of 40-75 ℃;
t2, after the epoxy propanol is dripped, continuously reacting for 1-1.5 hours at the temperature of 40-75 ℃;
t3, adding water to adjust the water content to 14-16% to obtain the monoethanol dipropyleneglycol amine.
Preferably, the control of the reaction temperature in step S2 is controlled by the dropping speed of the epoxypropanol.
Preferably, the inert gas in step S2 is one of nitrogen, argon or helium, preferably nitrogen.
Preferably, in view of the good water solubility of the monoethanolamine and the glycidol in the preparation method of the present invention, the reactor used is a low pressure reactor with a stirrer (mechanical seal), and the method has the advantages of simple industrialization and low investment.
The invention also discloses application of the ethanol dipropyl glycol amine prepared by the preparation method of the alcohol amine compound for improving the early strength of cement as an early strength agent of cement or concrete, blank cement is added, and compared with triethanolamine and diethanol monoisopropanolamine, the ethanol dipropyl glycol amine has more excellent performance of enhancing performance, and meanwhile, when the compound is used as a cement grinding aid, the compound has good adaptability.
(III) advantageous effects
The invention provides a preparation method and application of an alcohol amine compound for improving early strength of cement. Compared with the prior art, the method has the following beneficial effects:
(1) the preparation method and the application of the alcohol amine compound for improving the early strength of the cement specifically comprise the following steps: s1, adding monoethanolamine, a small amount of water and a catalyst into a reactor in sequence, heating to 30-55 ℃ in an inert gas atmosphere, S2, continuously dropwise adding epoxypropanol within 1-4 hours, controlling the reaction temperature to be within a range of 40-65 ℃, after the dropwise addition of the epoxypropanol is finished, keeping the temperature for 1 to 1.5 hours, S3, adding water to adjust the water content to be 14 to 16 percent, the prepared novel alcohol amine compound type early strength agent can obviously improve the early strength performance of cement or concrete, and has reasonable molecular design.
(2) According to the preparation method of the alcohol amine compound-ethanol dipropyleneglycol amine provided by the invention, an organic early strength agent with more excellent early strength performance is successfully prepared, so that the requirements of cement factories in different regions on the early strength performance of cement are met, and the method has the characteristics of simple raw materials and mild preparation conditions.
Drawings
FIG. 1 is a flow chart of the preparation method of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the embodiment of the present invention provides three technical solutions: the preparation method and the application of the alcohol amine compound for improving the early strength of the cement specifically comprise the following embodiments:
example 1
122.16g (2mol) of monoethanolamine (purity 99.90%), 25g of water and 1.84g of formic acid are added into a 2L low-pressure reaction kettle with a stirrer (mechanical seal), nitrogen is filled into the reaction kettle to 0.3MPa, the reaction kettle is continuously filled and emptied for 3 times, so that the oxygen content in the reaction kettle is less than 1%, circulating hot water is filled into a coil pipe in the reaction kettle until the material temperature reaches 35 ℃, and heating is stopped. The reaction is exothermic reaction, 299.28g (4.04mol) of epoxy propanol is dripped through a plunger pump, the dripping speed is controlled to enable the reaction temperature to be between 40 and 65 ℃, heat preservation is continued below 65 ℃ for 1 hour after the dripping of the epoxy propanol is finished, 47.50g of water is added to obtain 495.81g of monoethanol dipropylene glycol amine with the solid content of 85 percent, and the content of the product monoethanol dipropylene glycol amine is 97.5 percent, the content of the epoxy propanol is 0.69 percent, the content of the diethanol amine is 0.95 percent and the content of other impurities is 0.86 percent through gas chromatography analysis.
Example 2
122.16g (2mol) of monoethanolamine (purity 99.90%), 20g of water and 2.76g of formic acid are added into a 2L low-pressure reaction kettle with a stirrer (mechanical seal), nitrogen is filled into the reaction kettle to 0.3MPa, the reaction kettle is continuously filled and emptied for 3 times, so that the oxygen content in the reaction kettle is less than 1%, circulating hot water is filled into a coil pipe in the reaction kettle until the material temperature reaches 35 ℃, and heating is stopped. The reaction is an exothermic reaction, 293.35g (3.96mol) of epoxy propanol is dripped through a plunger pump, the dripping speed is controlled to enable the reaction temperature to be between 40 and 65 ℃, heat preservation is continued below 65 ℃ for 1 hour after the epoxy propanol is dripped, 40.60g of water is added to obtain 488.83g of monoethanol dipropylene glycol amine with the solid content of 85 percent, and the content of the product monoethanol dipropylene glycol amine is 97.1 percent, the content of epoxy propanol is 0.23 percent, the content of diethanol amine is 1.35 percent and the content of other impurities is 1.32 percent through gas chromatography analysis.
Example 3
122.16g (2mol) of monoethanolamine (purity 99.90%), 30g of water and 1.50g of formic acid are added into a 2L low-pressure reaction kettle with a stirrer (mechanical seal), nitrogen is filled into the reaction kettle to 0.3MPa, the reaction kettle is continuously filled and emptied for 3 times, so that the oxygen content in the reaction kettle is less than 1%, circulating hot water is filled into a coil pipe in the reaction kettle until the material temperature reaches 35 ℃, and heating is stopped. The reaction is an exothermic reaction, 303.73g (4.10mol) of epoxy propanol is dripped through a plunger pump, the dripping speed is controlled to enable the reaction temperature to be between 40 and 65 ℃, heat preservation is continued below 65 ℃ for 1 hour after the epoxy propanol is dripped, 43.65g of water is added to obtain 501.05g of monoethanol dipropylene glycol amine with the solid content of 85 percent, and the content of the product monoethanol dipropylene glycol amine is 97.4 percent, the content of epoxy propanol is 0.97 percent, the content of diethanol amine is 0.41 percent and the content of other impurities is 1.22 percent through gas chromatography analysis.
When the epoxy propanol-diethanolamine cement grinding aid is used as a cement grinding aid, the epoxy propanol, the diethanolamine which are not completely reacted in reaction products and alcohol ether impurities generated by the reaction do not need to be separated.
To further illustrate the advantage of monoethanol diisopropanolamine as an early strength agent for cement or concrete in the present invention, the early strength agent obtained in any of examples 1, 2 or 3 was compared with commercially available conventional early strength agents, diethanol monoisopropanolamine and triethanolamine, to prepare a mortar.
Comparative example 1
Triethanolamine: the water content is 15.5%, the chromatographic content of triethanolamine is 99.90%, and the triethanolamine is diluted with water to a content of 85.0%.
Comparative example 2
Diethanolisopropanolamine: the water content is 85.3%, the main content of diethanolisopropanolamine is 98.8%, and the content of diethanolisopropanolamine diluted by water is 85.0%.
The mortar comparison test adopts a laboratory module test, specifically referring to GB/T17671-1999 Cement mortar Strength test method, three different P.O42R cements are selected to perform the compression strength comparison test with and without adding alcohol amine compound (fracture fixation), and the specific results are as shown in the following table 1.
TABLE 1 compression Strength comparison results
As can be seen from Table 1, the 3D compressive strength of the formed monoethanol dipropyleneglycol amine as the early strength agent is obviously higher than that of triethanolamine or diethanol monoisopropanolamine, and the formed monoethanol dipropyleneglycol amine has a certain 28D compressive strength increasing effect.
In conclusion, the preparation method and the application of the compound ethanol dipropyleneglycol amine capable of improving the early strength of the cement provided by the invention successfully solve the problem that the early strength of the cement in a cement plant in part of regions is not ideal in value increase after the traditional grinding aid mainly comprising triethanolamine or diethanol monoisopropanolamine is used when the compound ethanol dipropyleneglycol amine is used as the cement grinding aid, and have high application value.
And those not described in detail in this specification are well within the skill of those in the art.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. The preparation method of the alcohol amine compound for improving the early strength of the cement is characterized in that the prepared alcohol amine compound is oneThe molecular structural formula of the ethanol dipropyleneglycol amine is as follows:
the preparation method of the alcohol amine compound-ethanol dipropanediol amine specifically comprises the following steps:
s1, sequentially adding monoethanolamine, a small amount of water and a catalyst into a reactor, and heating to 30-55 ℃ in an inert gas atmosphere;
s2, continuously dripping epoxypropanol within 1-4 hours, controlling the reaction temperature within the range of 40-65 ℃, and continuously preserving heat for 1-1.5 hours after finishing dripping the epoxypropanol;
s3, adding water to adjust the water content to 14-16% to obtain the monoethanol dipropyleneglycol amine.
2. The method of preparing an alcohol amine compound having an improved early strength of cement according to claim 1, wherein: in the step S1, the content of monoethanolamine is 65.00-99.99% by mass, and the content of water in monoethanolamine is 0.01-35.00% by mass.
3. The method of preparing an alcohol amine compound having an improved early strength of cement according to claim 1, wherein: in the step S1, the catalyst is an organic weak acid, and the organic weak acid is one of formic acid, acetic acid, propionic acid or lactic acid.
4. The method of preparing the alcohol amine compound having an improved early strength of cement according to claim 3, wherein: the molar ratio of the organic weak acid to the monoethanolamine of the catalyst is 0.0001-0.03: 1.
5. the method of preparing an alcohol amine compound having an improved early strength of cement according to claim 1, wherein: in the step S2, the molar ratio of monoethanolamine to epoxypropanol is 1: 1.98-2.05.
6. The method for preparing the alcohol amine compound for improving the early strength of cement according to claim 1, wherein the method comprises the following steps:
t1, placing monoethanolamine in a reaction container, dropwise adding epoxypropanol according to a certain proportion under the stirring condition in an inert gas atmosphere, and controlling the dropwise adding speed of the epoxypropanol to enable the reaction temperature to be in the range of 40-75 ℃;
t2, after the epoxy propanol is dripped, continuously reacting for 1-1.5 hours at the temperature of 40-75 ℃;
t3, adding water to adjust the water content to 14-16% to obtain the monoethanol dipropyleneglycol amine.
7. The method of preparing an alcohol amine compound having an improved early strength of cement according to claim 1, wherein: the control of the reaction temperature in the step S2 is controlled by the dropping speed of the epoxypropanol.
8. The method of preparing an alcohol amine compound having an improved early strength of cement according to claim 1, wherein: the inert gas in step S2 is one of nitrogen, argon or helium, preferably nitrogen.
9. The method of claim 1, wherein the alcohol amine compound for increasing early strength of cement comprises: the reactor used is a low-pressure reactor with a stirrer.
10. The application of the monoethanol dipropyleneglycol amine prepared by the preparation method of any one of claims 2-9 as an early strength agent for cement or concrete.
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