CN116769393A - An environmentally friendly high elongation two-component polyurethane waterproof coating and its preparation method - Google Patents

Abstract

The invention relates to an environmentally friendly high-elongation two-component polyurethane waterproof coating and a preparation method. It is mainly prepared from the following components according to the following weight parts ratio. Group A: 67-73 parts of polyether resin, isocyanate 26-32 parts of curing agent, 1-4 parts of solvent. Group B: 20-25 parts of polyether resin, 22-28 parts of plasticizer, 0.2-0.4 parts of dispersant, 35-45 parts of inorganic filler, 0.4-0.6 parts of anti-settling agent, 10-12 parts of curing agent, 0.1 catalyst -0.2 parts, 6-8 parts of solvent, 0.3-0.5 parts of defoaming agent. The environmentally friendly high-elongation two-component polyurethane waterproof coating applied in this application not only ensures a healthy environment for construction workers (low odor, no MOCA), but also ensures the smooth construction of the coating, and also ensures that the coating can be used in low-temperature environments. The stability of physical properties.

Description

An environmentally friendly high elongation two-component polyurethane waterproof coating and its preparation method

Technical field

The invention relates to the field of waterproof coatings, and in particular to an environmentally friendly high elongation two-component polyurethane waterproof coating and a preparation method thereof.

Background technique

In the modern waterproofing industry, polyurethane waterproof coatings are widely used in the waterproofing industry and are used in various large-scale projects, such as high-speed railways, subways, tunnels, underground pipelines of buildings, basements, etc. It is precisely because of such a diverse and complex environment that we will encounter various construction base surfaces or construction environments.

As a star product in waterproof coatings, two-component polyurethane has the characteristics of fast reaction speed, coupled with the modification of curing agent MOCA (Moca), which makes the coating film performance excellent, and is favored by the majority of waterproof construction workers. However, MOCA is not an environmentally friendly curing agent, and reports have shown that it may cause cancer. At the same time, the B component of high-performance two-component polyurethane waterproof coating has a high MOCA (melting point 102-107°C) content, which is easy to precipitate at low temperatures, resulting in performance fluctuations or even failure. In addition, the common solvent contained in two-component polyurethane waterproof coatings is 100# or 150# solvent oil with a strong smell, which will affect the health of workers and the progress of construction, especially in confined spaces. Therefore, it is urgent to develop a low-odor and environmentally friendly two-component polyurethane waterproof coating.

With the development of the industry in recent years, most methods for low-flavor projects are to reduce the solvent content or use solvent-free methods to achieve it. Although this reduces the taste in the paint, in order to make the viscosity of the formula normal (<10000mpa.s), the liquid raw materials (resin or plasticizer) are increased, resulting in an increase in the viscosity of the paint (more resin and plasticizer, surface tension Large), so the mechanical bubbles are not easy to eliminate (stir the two-component AB material before construction), and finally there are many bubbles or even holes in the coating film, which greatly reduces the waterproof performance of the coating.

Contents of the invention

The invention provides an environmentally friendly high elongation two-component polyurethane waterproof coating and a preparation method thereof. The environmentally friendly high elongation two-component polyurethane waterproof coating adopts a reasonable formula and does not use MOCA curing agent, so it reduces It not only eliminates the smell of paint, but also ensures good construction performance, good waterproof performance and high elongation of the paint.

The technical solution of the present invention is as follows:

An environmentally friendly two-component polyurethane waterproof coating with high elongation, which is characterized in that: it is composed of component A and component B mixed according to a mass ratio of 1:2

The A component is mainly prepared from the following components according to the following weight parts ratio:

Polyether resin 67-73

Isocyanate curing agent 26-32

High boiling point organic solvents 1-4

The B component is mainly prepared from the following components according to the following weight parts ratio:

The chain extender is TDMA-02.

Preferably, the polyether resin is one of polyether 2000D, polyether 1000D, polyether 330N, polyether M500, or a mixture of any two of them in any proportion. The preferred polyether resin can greatly improve the physical properties of the product's resin structure, improve the physical properties such as the tensile strength and elongation at break of the coating film, and also improve the high temperature resistance of the coating film.

Preferably, the plasticizer is one or a mixture of any two of dioctyl terephthalate, chlorinated paraffin, dioctyl adipate, and dioctyl phthalate in any proportion. The preferred plasticizer type can greatly increase the elongation at break of the product, reduce the overall viscosity of the coating, and improve the workability.

Preferably, the dispersant is one or a mixture of any two of branched polycarboxylic acids, linear alkyl amides, grafted acrylic copolymers or long-chain polyurethane dispersants in any proportion. The preferred type of dispersant can greatly improve the compatibility of resin and powder, improve the appearance of the coating film and the uniformity of the coating film performance, while also reducing a certain viscosity of the coating and improving the workability of the coating.

Preferably, the inorganic filler is one or a mixture of any two of talc powder, metakaolin, calcium powder or mica powder in any proportion. Preferring the type of inorganic filler can greatly improve the tensile strength of the product, reduce the viscosity of the product, and thus improve the construction performance.

Preferably, the anti-settling agent is one or a mixture of any two of bentonite, magnesium aluminum silicate, polyurea rheology agent, and polyamide wax in any proportion. The preferred type of anti-settling agent can improve the dispersibility of the filler in the coating and improve the performance and storage stability of the coating.

The chain extender TDMA-02 does not contain cancer-causing drugs (MOCA) and will not precipitate in low-temperature environments, ensuring the performance stability of the coating.

Preferably, the isocyanate curing agent is T-80 (2,4-toluene diisocyanate-80%), T-100 (2,4-toluene diisocyanate-100%), MDI-50 (2,4-toluene diisocyanate-100%), -Diphenylmethane diisocyanate-50%) or a mixture of any two in any proportion. The preferred type of isocyanate curing agent can improve the physical properties of the product (tensile strength, elongation at break, etc.), improve the surface drying time of the coating film, and the appearance of the coating film.

Preferably, the catalyst is one or a mixture of two of organic bismuth and organic zinc in any proportion. The preferred catalyst type can improve the surface drying time of the coating film and the performance of the coating.

Preferably, the high boiling point organic solvent is one of isoparaffins, dearomatized hydrocarbons, naphthenic solvents or a mixture of any two of them in any proportion. The preferred solvent type can increase the surface drying time of the coating film, reduce the viscosity and odor of the coating, and improve the workability of the coating.

Preferably, the defoaming agent is one or a mixture of any two of silicone defoaming agents, polyether defoaming agents, amide defoaming agents, and phosphate ester defoaming agents in any proportion. The preferred type of defoaming agent gives the coating the ability to quickly suppress and break foam, improving the appearance and physical properties of the coating film.

A method for preparing environmentally friendly high-elongation two-component polyurethane waterproof coating, including the following steps:

The A component is mainly prepared by the following methods:

Add the polyether resin into the reaction kettle, and dehydrate under vacuum for more than 4 hours at a stirring speed of 200-300r/min, a temperature of 112-118°C, and a pressure of -0.095MPa or above until the moisture content is ≤0.3‰.

Then close the vacuum valve on the reaction kettle, open the nitrogen valve, then close the vacuum pump, and after the nitrogen pressure reaches 0.02Mpa, open the cooling system until the temperature cools to 80-84°C, then maintain this temperature and add isocyanate curing agent for reaction 2.5- 3h;

Then cool and lower the temperature to 55-60°C, add a high-boiling point organic solvent, and finally control the temperature at 50-55°C for vacuum degassing for more than 30 minutes to obtain the component A;

The B component is mainly prepared by the following methods:

Add the polyether resin, plasticizer, dispersant, defoaming agent and TDMA-02 into the reactor, then add the inorganic filler and anti-settling agent in sequence at a stirring speed of 200r-300r/min and a temperature of 80-85°C. , then increase the rotation speed to 400-450r/min and stir for about 10-15min; then increase the temperature to 112-118℃, maintain this temperature at -0.095±0.005MPa, and vacuum dehydrate for more than 4h until the moisture content requirement is ≤0.3‰ ;

Then cool down to 55-60°C, add catalyst and high-boiling point organic solvent, stir for 10-15 minutes and then degas at negative pressure -0.095±0.005Mpa for more than 30 minutes;

Gradually reduce the stirring speed to stop, turn off the vacuum pump, open the vent valve, and remove the negative pressure in the equipment to obtain the component B.

The preparation method of the environmentally friendly high-elongation two-component polyurethane waterproof coating has a simple process, is consistent with the conventional two-component polyurethane waterproof coating, and is easy to promote.

The optimal limitation of each parameter in the preparation process makes the prepared environmentally friendly high-elongation two-component polyurethane waterproof coating have better performance.

Compared with the existing technology, the application of the present invention has the following advantages:

By replacing the curing agent with a MOCA-free low-odor liquid environmentally friendly curing agent (TDMA-02), not only the carcinogenic risk of the paint is avoided, but its liquid state at room temperature also ensures that the paint will not precipitate at low temperatures (winter). .

TDMA-02 is a monophenyl ring secondary amine chemical material. Compared with moka (traditional chain extender) of diphenyl ring primary amine, it has higher activity (the diphenyl ring steric hindrance effect is larger) and is compatible with isocyanine. The chemical structure after the acid radical reaction is more stable (one molecule will not react with two isocyanate radicals), that is, a single chain is formed after the reaction (high degree of freedom), which makes the performance of the coating film more stable and has a higher elongation at break.

The taste in paint mainly comes from solvents. By replacing the commonly used low-boiling point solvents with pungent odor (100# (boiling point - 163°C), 150# (boiling point - 176°C) solvents) with high-boiling point, low-odor solvents (Complex saturated hydrocarbon (boiling point - 260-280°C)) not only prepares low-odor polyurethane waterproof coatings, but also ensures the construction properties of the coatings (the conventional method is to reduce the amount of solvent added or eliminate the addition of solvent).

Detailed ways

The technical solution of the present invention will be described in detail below with reference to examples.

Example 1

The environmentally friendly high-elongation two-component polyurethane waterproof coating of the present invention is mainly prepared from the following components according to the weight parts ratio in the following table:

Group A

Polyether resin 67

Isocyanate curing agent 32

Saturated hydrocarbons 4

Group B

Polyether resin 20

Plasticizer 28

Dispersant 0.2

Inorganic filler 45

Anti-settling agent 0.6

TDMA-02 12

Catalyst 0.1

Saturated hydrocarbon 6

Defoaming agent 0.3

The preparation method of the environmentally friendly high elongation two-component polyurethane waterproof coating includes the following steps:

Z1. Preparation of component A

Add the measured polyether into the reaction kettle, turn on stirring (200r/min), turn on the heat source and set the temperature to 115°C.

Turn on the vacuum pump, keep it above -0.095MPa, vacuum dehydrate for 4 hours, and control the temperature within the range of 115±3°C.

Turn off the vacuum system, turn on the nitrogen protection system, take a sample to detect the moisture content in the system, the moisture content requirement is ≤0.3‰, if the moisture is >0.3%, turn on the vacuum system, turn off the nitrogen protection system, keep it above -0.095MPa, vacuum dehydrate for 1 hour, and then Carry out sampling and retesting until the moisture content is ≤0.3‰.

After dehydration is completed, first close the vacuum valve on the reaction kettle, open the nitrogen valve, then close the vacuum pump, set the nitrogen pressure to 0.02MPa, and open the cooling system.

Cool to 80°C, add the measured isocyanate curing agent and react for 2.5-3h, and control the temperature within the range of 80-84°C.

Cool to 60°C, add complex saturated hydrocarbon solvent, then control the temperature at 50-55°C, and vacuum deaeration for 30 minutes.

Unloading materials, washing cans, labeling, and placing them in designated positions.

Z2. Preparation of component B

Add the measured polyether, plasticizer, dispersant, defoaming agent and curing agent (TDMA-02) into the reaction kettle, turn on stirring (200r/min), turn on the heat source and set the temperature to 85°C.

When the temperature rises to 85°C, start adding the measured inorganic filler and anti-settling agent in sequence, increase the rotation speed to 400r/min, and stir for about 10 minutes. Raise the temperature to 115°C, turn on the vacuum pump, keep it above -0.095MPa, vacuum dehydrate for 4 hours, and control the temperature within the range of 115±3°C.

Turn off the vacuum system, turn on the nitrogen protection system, take a sample to detect the moisture content in the system, the moisture content requirement is ≤0.3‰, if the moisture is >0.3%, turn on the vacuum system, turn off the nitrogen protection system, keep it above -0.095MPa, vacuum dehydrate for 1 hour, and then Carry out sampling and retesting until the moisture content is ≤0.3‰.

Then cool down to 60°C. Add the measured catalyst and solvent, stir for 15 minutes, then turn on the vacuum pump, close the nitrogen valve, maintain -0.095MPa, and degas for more than 30 minutes.

Gradually reduce the stirring speed to stop, turn off the vacuum pump, open the air release valve, and remove the negative pressure in the equipment.

Unloading materials, washing cans, labeling, and placing them in designated positions.

Example 2

The environmentally friendly high-elongation two-component polyurethane waterproof coating of the present invention is mainly prepared from the following components according to the weight parts ratio in the following table:

Group A

Polyether resin 70

Isocyanate curing agent 28

Saturated hydrocarbon 2

Group B

Polyether resin 23

Plasticizer 25

Dispersant 0.3

Inorganic filler 40

Anti-settling agent 0.5

TDMA-02 11

Catalyst 0.15

Saturated hydrocarbon 7

Defoaming agent 0.4

The preparation method of the environmentally friendly high elongation two-component polyurethane waterproof coating includes the following steps:

Z1. Preparation of component A

Add the measured polyether into the reaction kettle, turn on stirring (200r/min), turn on the heat source and set the temperature to 115°C.

Turn on the vacuum pump, keep it above -0.095MPa, vacuum dehydrate for 4 hours, and control the temperature within the range of 115±3°C.

Turn off the vacuum system, turn on the nitrogen protection system, take a sample to detect the moisture content in the system, the moisture content requirement is ≤0.3‰, if the moisture is >0.3%, turn on the vacuum system, turn off the nitrogen protection system, keep it above -0.095MPa, vacuum dehydrate for 1 hour, and then Carry out sampling and retesting until the moisture content is ≤0.3‰.

After dehydration is completed, first close the vacuum valve on the reaction kettle, open the nitrogen valve, then close the vacuum pump, set the nitrogen pressure to 0.02MPa, and open the cooling system.

Cool to 80°C, add the measured isocyanate curing agent and react for 2.5-3h, and control the temperature within the range of 80-84°C.

Cool to 60°C, add complex saturated hydrocarbon solvent, then control the temperature at 50-55°C, and vacuum deaeration for 30 minutes.

Unloading materials, washing cans, labeling, and placing them in designated positions.

Z2. Preparation of component B

Add the measured polyether, plasticizer, dispersant, defoaming agent and curing agent (TDMA-02) into the reaction kettle, turn on stirring (200r/min), turn on the heat source and set the temperature to 85°C.

When the temperature rises to 85°C, start adding the measured inorganic filler and anti-settling agent in sequence, increase the rotation speed to 400r/min, and stir for about 10 minutes. Raise the temperature to 115°C, turn on the vacuum pump, keep it above -0.095MPa, vacuum dehydrate for 4 hours, and control the temperature within the range of 115±3°C.

Turn off the vacuum system, turn on the nitrogen protection system, take a sample to detect the moisture content in the system, the moisture content requirement is ≤0.3‰, if the moisture is >0.3%, turn on the vacuum system, turn off the nitrogen protection system, keep it above -0.095MPa, vacuum dehydrate for 1 hour, and then Carry out sampling and retesting until the moisture content is ≤0.3‰.

Then cool down to 60°C. Add the measured catalyst and solvent, stir for 15 minutes, then turn on the vacuum pump, close the nitrogen valve, maintain -0.095MPa, and degas for more than 30 minutes.

Gradually reduce the stirring speed to stop, turn off the vacuum pump, open the air release valve, and remove the negative pressure in the equipment.

Unloading materials, washing cans, labeling, and placing them in designated positions.

Example 3

The environmentally friendly high-elongation two-component polyurethane waterproof coating of the present invention is mainly prepared from the following components according to the weight parts ratio in the following table:

Group A

Polyether resin 73

Isocyanate curing agent 26

Saturated hydrocarbon 1

Group B

Polyether resin 25.0

Plasticizer 22.0

Dispersant 0.4

Inorganic filler 35.0

Anti-settling agent 0.4

TDMA-02 10.0

Catalyst 0.2

Saturated Hydrocarbon 8.0

Defoaming agent 0.5

The preparation method of the environmentally friendly high elongation two-component polyurethane waterproof coating includes the following steps:

Z1. Preparation of component A

Add the measured polyether into the reaction kettle, turn on stirring (200r/min), turn on the heat source and set the temperature to 115°C.

Turn on the vacuum pump, keep it above -0.095MPa, vacuum dehydrate for 4 hours, and control the temperature within the range of 115±3°C.

Turn off the vacuum system, turn on the nitrogen protection system, take a sample to detect the moisture content in the system, the moisture content requirement is ≤0.3‰, if the moisture is >0.3%, turn on the vacuum system, turn off the nitrogen protection system, keep it above -0.095MPa, vacuum dehydrate for 1 hour, and then Carry out sampling and retesting until the moisture content is ≤0.3‰.

After dehydration is completed, first close the vacuum valve on the reaction kettle, open the nitrogen valve, then close the vacuum pump, set the nitrogen pressure to 0.02MPa, and open the cooling system.

Cool to 80°C, add the measured isocyanate curing agent and react for 2.5-3h, and control the temperature within the range of 80-84°C.

Cool to 60°C, add complex saturated hydrocarbon solvent, then control the temperature at 50-55°C, and vacuum deaeration for 30 minutes.

Unloading materials, washing cans, labeling, and placing them in designated positions.

Z2. Preparation of component B

Add the measured polyether, plasticizer, dispersant, defoaming agent and curing agent (TDMA-02) into the reaction kettle, turn on stirring (200r/min), turn on the heat source and set the temperature to 85°C.

When the temperature rises to 85°C, start adding the measured inorganic filler and anti-settling agent in sequence, increase the rotation speed to 400r/min, and stir for about 10 minutes. Raise the temperature to 115°C, turn on the vacuum pump, keep it above -0.095MPa, vacuum dehydrate for 4 hours, and control the temperature within the range of 115±3°C.

Turn off the vacuum system, turn on the nitrogen protection system, take a sample to detect the moisture content in the system, the moisture content requirement is ≤0.3‰, if the moisture is >0.3%, turn on the vacuum system, turn off the nitrogen protection system, keep it above -0.095MPa, vacuum dehydrate for 1 hour, and then Carry out sampling and retesting until the moisture content is ≤0.3‰.

Then cool down to 60°C. Add the measured catalyst and solvent, stir for 15 minutes, then turn on the vacuum pump, close the nitrogen valve, maintain -0.095MPa, and degas for more than 30 minutes.

Gradually reduce the stirring speed to stop, turn off the vacuum pump, open the air release valve, and remove the negative pressure in the equipment.

Unloading materials, washing cans, labeling, and placing them in designated positions.

Advantage:

Examples 1-3 use a low-odor liquid curing agent (TDMA-02) to achieve a MOCA-free paint system, which avoids the risk of cancer and does not increase the taste of the paint.

In the embodiment, a low-odor liquid curing agent (TDMA-02) is first used, so that the coating film has a higher elongation at break.

The solvent uses a saturated hydrocarbon solvent with low taste and high boiling point (the smell of the solvent mainly comes from the solvent), which improves the quality of the construction environment for construction workers and reduces the harm to human health.

The viscosity of the coating is the conventional construction viscosity (5000-9000mpa.s), which can be applied smoothly, and the coating will not be sticky (low surface tension - solvent exists), the bubbles are easy to remove, and there are no bubbles on the surface of the coating film.

There is no risk of curing agent (high freezing point) precipitation in winter, ensuring stable performance of the paint.

Comparison case 1

The environmentally friendly high-elongation two-component polyurethane waterproof coating of the present invention is mainly prepared from the following components according to the weight parts ratio in the following table:

Group A

Polyether resin 70

Isocyanate curing agent 28

Saturated hydrocarbon 2

Group B

Polyether resin 23

Plasticizer 25

Dispersant 0.3

Inorganic filler 40

Anti-settling agent 0.5

TDMA-02 11

Catalyst 0.15

Solvent oil 1.5

Defoaming agent 0.4

The preparation method of the environmentally friendly high elongation two-component polyurethane waterproof coating includes the following steps:

Z1. Preparation of component A

Add the measured polyether into the reaction kettle, turn on stirring (200r/min), turn on the heat source and set the temperature to 115°C.

Turn on the vacuum pump, keep it above -0.095MPa, vacuum dehydrate for 4 hours, and control the temperature within the range of 115±3°C.

Turn off the vacuum system, turn on the nitrogen protection system, take a sample to detect the moisture content in the system, the moisture content requirement is ≤0.3‰, if the moisture is >0.3%, turn on the vacuum system, turn off the nitrogen protection system, keep it above -0.095MPa, vacuum dehydrate for 1 hour, and then Carry out sampling and retesting until the moisture content is ≤0.3‰.

After dehydration is completed, first close the vacuum valve on the reaction kettle, open the nitrogen valve, then close the vacuum pump, set the nitrogen pressure to 0.02MPa, and open the cooling system.

Cool to 80°C, add the measured isocyanate curing agent and react for 2.5-3h, and control the temperature within the range of 80-84°C.

Cool to 60°C, add complex saturated hydrocarbon solvent, then control the temperature at 50-55°C, and vacuum deaeration for 30 minutes.

Unloading materials, washing cans, labeling, and placing them in designated positions.

Z2. Preparation of component B

Add the measured polyether, plasticizer, dispersant, defoaming agent and curing agent (TDMA-02) into the reaction kettle, turn on stirring (200r/min), turn on the heat source and set the temperature to 85°C.

When the temperature rises to 85°C, start adding the measured inorganic filler and anti-settling agent in sequence, increase the rotation speed to 400r/min, and stir for about 10 minutes. Raise the temperature to 115°C, turn on the vacuum pump, keep it above -0.095MPa, vacuum dehydrate for 4 hours, and control the temperature within the range of 115±3°C.

Turn off the vacuum system, turn on the nitrogen protection system, take a sample to detect the moisture content in the system, the moisture content requirement is ≤0.3‰, if the moisture is >0.3%, turn on the vacuum system, turn off the nitrogen protection system, keep it above -0.095MPa, vacuum dehydrate for 1 hour, and then Carry out sampling and retesting until the moisture content is ≤0.3‰.

Then cool down to 60°C. Add the measured catalyst and solvent, stir for 15 minutes, then turn on the vacuum pump, close the nitrogen valve, maintain -0.095MPa, and degas for more than 30 minutes.

Gradually reduce the stirring speed to stop, turn off the vacuum pump, open the air release valve, and remove the negative pressure in the equipment.

Unloading materials, washing cans, labeling, and placing them in designated positions.

Disadvantages:

1. A low-solvent method is used in the paint to reduce the smell of the paint, but there is still some pungent smell.

2. Although there is a certain amount of solvent in the formula, the viscosity of the paint is still high and the viscosity of the paint is still strong (high surface tension). A large number of mechanical bubbles cannot escape after the AB component coating is stirred, resulting in a large number of bubbles in the film layer, resulting in a low elongation at break.

Comparative case 2

The environmentally friendly high-elongation two-component polyurethane waterproof coating of the present invention is mainly prepared from the following components according to the weight parts ratio in the following table:

Group A

Polyether resin 70

Isocyanate curing agent 28

Saturated hydrocarbon 2

Group B

Polyether resin 23

Plasticizer 25

Dispersant 0.3

Inorganic filler 40

Anti-settling agent 0.5

TDMA-02 11

Catalyst 0.15

Saturated hydrocarbon 0

Defoaming agent 0.4

The preparation method of the environmentally friendly high elongation two-component polyurethane waterproof coating includes the following steps:

Z1. Preparation of component A

Add the measured polyether into the reaction kettle, turn on stirring (200r/min), turn on the heat source and set the temperature to 115°C.

Turn on the vacuum pump, keep it above -0.095MPa, vacuum dehydrate for 4 hours, and control the temperature within the range of 115±3°C.

Turn off the vacuum system, turn on the nitrogen protection system, take a sample to detect the moisture content in the system, the moisture content requirement is ≤0.3‰, if the moisture is >0.3%, turn on the vacuum system, turn off the nitrogen protection system, keep it above -0.095MPa, vacuum dehydrate for 1 hour, and then Carry out sampling and retesting until the moisture content is ≤0.3‰.

After dehydration is completed, first close the vacuum valve on the reaction kettle, open the nitrogen valve, then close the vacuum pump, set the nitrogen pressure to 0.02MPa, and open the cooling system.

Cool to 80°C, add the measured isocyanate curing agent and react for 2.5-3h, and control the temperature within the range of 80-84°C.

Cool to 60°C, add complex saturated hydrocarbon solvent, then control the temperature at 50-55°C, and vacuum deaeration for 30 minutes.

Unloading materials, washing cans, labeling, and placing them in designated positions.

Z2. Preparation of component B

Add the measured polyether, plasticizer, dispersant, defoaming agent and curing agent (TDMA-02) into the reaction kettle, turn on stirring (200r/min), turn on the heat source and set the temperature to 85°C.

When the temperature rises to 85°C, start adding the measured inorganic filler and anti-settling agent in sequence, increase the rotation speed to 400r/min, and stir for about 10 minutes. Raise the temperature to 115°C, turn on the vacuum pump, keep it above -0.095MPa, vacuum dehydrate for 4 hours, and control the temperature within the range of 115±3°C.

Turn off the vacuum system, turn on the nitrogen protection system, take a sample to detect the moisture content in the system, the moisture content requirement is ≤0.3‰, if the moisture is >0.3%, turn on the vacuum system, turn off the nitrogen protection system, keep it above -0.095MPa, vacuum dehydrate for 1 hour, and then Carry out sampling and retesting until the moisture content is ≤0.3‰.

Then cool down to 60°C. Add the measured catalyst and solvent, stir for 15 minutes, then turn on the vacuum pump, close the nitrogen valve, maintain -0.095MPa, and degas for more than 30 minutes.

Gradually reduce the stirring speed to stop, turn off the vacuum pump, open the air release valve, and remove the negative pressure in the equipment.

Unloading materials, washing cans, labeling, and placing them in designated positions.

Disadvantages:

Compared with Example 2, this comparative example has: 1. The viscosity of the paint is relatively large and the viscosity of the paint is strong (large surface tension). A large number of mechanical bubbles cannot escape after the AB component paint is applied and stirred, resulting in the existence of A large number of bubbles, resulting in low elongation at break.

Comparative case 3

The environmentally friendly high-elongation two-component polyurethane waterproof coating of the present invention is mainly prepared from the following components according to the weight parts ratio in the following table:

Group A

Polyether resin 70

Isocyanate curing agent 28

Saturated hydrocarbon 2

Group B

Polyether resin 23

Plasticizer 25

Dispersant 0.3

Inorganic filler 40

Anti-settling agent 0.5

MOCA 11

Catalyst 0.15

Saturated hydrocarbon 7

Defoaming agent 0.4

The preparation method of the environmentally friendly high elongation two-component polyurethane waterproof coating includes the following steps:

Z1. Preparation of component A

Add the measured polyether into the reaction kettle, turn on stirring (200r/min), turn on the heat source and set the temperature to 115°C.

Turn on the vacuum pump, keep it above -0.095MPa, vacuum dehydrate for 4 hours, and control the temperature within the range of 115±3°C.

Turn off the vacuum system, turn on the nitrogen protection system, take a sample to detect the moisture content in the system, the moisture content requirement is ≤0.3‰, if the moisture is >0.3%, turn on the vacuum system, turn off the nitrogen protection system, keep it above -0.095MPa, vacuum dehydrate for 1 hour, and then Carry out sampling and retesting until the moisture content is ≤0.3‰.

After dehydration is completed, first close the vacuum valve on the reaction kettle, open the nitrogen valve, then close the vacuum pump, set the nitrogen pressure to 0.02MPa, and open the cooling system.

Cool to 80°C, add the measured isocyanate curing agent and react for 2.5-3h, and control the temperature within the range of 80-84°C.

Cool to 60°C, add solvent, then control the temperature at 50-55°C, and vacuum deaeration for 30 minutes.

Unloading materials, washing cans, labeling, and placing them in designated positions.

Z2. Preparation of component B

Add the measured polyether, plasticizer, dispersant, defoaming agent and curing agent (MOCA) into the reactor, turn on stirring (200r/min), turn on the heat source and set the temperature to 85°C.

When the temperature rises to 85°C, start adding the measured inorganic filler and anti-settling agent in sequence, increase the rotation speed to 400r/min, and stir for about 10 minutes. Raise the temperature to 115°C, turn on the vacuum pump, keep it above -0.095MPa, vacuum dehydrate for 4 hours, and control the temperature within the range of 115±3°C.

Turn off the vacuum system, turn on the nitrogen protection system, take a sample to detect the moisture content in the system, the moisture content requirement is ≤0.3‰, if the moisture is >0.3%, turn on the vacuum system, turn off the nitrogen protection system, keep it above -0.095MPa, vacuum dehydrate for 1 hour, and then Carry out sampling and retesting until the moisture content is ≤0.3‰.

Then cool down to 60°C. Add the measured catalyst and solvent, stir for 15 minutes, then turn on the vacuum pump, close the nitrogen valve, maintain -0.095MPa, and degas for more than 30 minutes.

Gradually reduce the stirring speed to stop, turn off the vacuum pump, open the air release valve, and remove the negative pressure in the equipment.

Unloading materials, washing cans, labeling, and placing them in designated positions.

Disadvantages:

Compared with Example 2 in this comparative example, TDMA-02 in component B is replaced by MOCA.

1. There are a large number of mechanical bubbles in coated instant noodles

2. When the coating is at low temperature, the curing agent will precipitate.

Comparative case 4

The environmentally friendly high-elongation two-component polyurethane waterproof coating of the present invention is mainly prepared from the following components according to the weight parts ratio in the following table:

Group A

Polyether resin 70

Isocyanate curing agent 28

Saturated hydrocarbon 2

Group B

Polyether resin 23

Plasticizer 25

Dispersant 0.3

Inorganic filler 40

Anti-settling agent 0.5

DMTDA 11

Catalyst 0.15

Saturated hydrocarbon 7

Defoaming agent 0.4

The preparation method of the environmentally friendly high elongation two-component polyurethane waterproof coating includes the following steps:

Z1. Preparation of component A

Add the measured polyether into the reaction kettle, turn on stirring (200r/min), turn on the heat source and set the temperature to 115°C.

Turn on the vacuum pump, keep it above -0.095MPa, vacuum dehydrate for 4 hours, and control the temperature within the range of 115±3°C.

Turn off the vacuum system, turn on the nitrogen protection system, take a sample to detect the moisture content in the system, the moisture content requirement is ≤0.3‰, if the moisture is >0.3%, turn on the vacuum system, turn off the nitrogen protection system, keep it above -0.095MPa, vacuum dehydrate for 1 hour, and then Carry out sampling and retesting until the moisture content is ≤0.3‰.

After dehydration is completed, first close the vacuum valve on the reaction kettle, open the nitrogen valve, then close the vacuum pump, set the nitrogen pressure to 0.02MPa, and open the cooling system.

Cool to 80°C, add the measured isocyanate curing agent and react for 2.5-3h, and control the temperature within the range of 80-84°C.

Cool to 60°C, add solvent, then control the temperature at 50-55°C, and vacuum deaeration for 30 minutes.

Unloading materials, washing cans, labeling, and placing them in designated positions.

Z2. Preparation of component B

Add the measured polyether, plasticizer, dispersant, defoaming agent and curing agent (DMTDA) into the reactor, turn on stirring (200r/min), turn on the heat source and set the temperature to 85°C.

When the temperature rises to 85°C, start adding the measured inorganic filler and anti-settling agent in sequence, increase the rotation speed to 400r/min, and stir for about 10 minutes. Raise the temperature to 115°C, turn on the vacuum pump, keep it above -0.095MPa, vacuum dehydrate for 4 hours, and control the temperature within the range of 115±3°C.

Turn off the vacuum system, turn on the nitrogen protection system, take a sample to detect the moisture content in the system, the moisture content requirement is ≤0.3‰, if the moisture is >0.3%, turn on the vacuum system, turn off the nitrogen protection system, keep it above -0.095MPa, vacuum dehydrate for 1 hour, and then Carry out sampling and retesting until the moisture content is ≤0.3‰.

Then cool down to 60°C. Add the measured catalyst and solvent, stir for 15 minutes, then turn on the vacuum pump, close the nitrogen valve, maintain -0.095MPa, and degas for more than 30 minutes.

Gradually reduce the stirring speed to stop, turn off the vacuum pump, open the air release valve, and remove the negative pressure in the equipment.

Unloading materials, washing cans, labeling, and placing them in designated positions.

Disadvantages:

Comparing this comparative example with Example 2, TDMA-02 in component B is replaced by DMTDA, and there is an obvious sulfide odor in the paint.

Comparative case 5

The environmentally friendly high-elongation two-component polyurethane waterproof coating of the present invention is mainly prepared from the following components according to the weight parts ratio in the following table:

Group A

Polyether resin 70

Isocyanate curing agent 28

Saturated hydrocarbon 2

Group B

Polyether resin 23

Plasticizer 25

Dispersant 0.3

Inorganic filler 40

Anti-settling agent 0.5

TDMA-02 11

Catalyst 0.15

solvent oil 7

Defoaming agent 0.4

The preparation method of the environmentally friendly high elongation two-component polyurethane waterproof coating includes the following steps:

Z1. Preparation of component A

Add the measured polyether into the reaction kettle, turn on stirring (200r/min), turn on the heat source and set the temperature to 115°C.

Turn on the vacuum pump, keep it above -0.095MPa, vacuum dehydrate for 4 hours, and control the temperature within the range of 115±3°C.

Turn off the vacuum system, turn on the nitrogen protection system, take a sample to detect the moisture content in the system, the moisture content requirement is ≤0.3‰, if the moisture is >0.3%, turn on the vacuum system, turn off the nitrogen protection system, keep it above -0.095MPa, vacuum dehydrate for 1 hour, and then Carry out sampling and retesting until the moisture content is ≤0.3‰.

After dehydration is completed, first close the vacuum valve on the reaction kettle, open the nitrogen valve, then close the vacuum pump, set the nitrogen pressure to 0.02MPa, and open the cooling system.

Cool to 80°C, add the measured isocyanate curing agent and react for 2.5-3h, and control the temperature within the range of 80-84°C.

Cool to 60°C, add solvent, then control the temperature at 50-55°C, and vacuum deaeration for 30 minutes.

Unloading materials, washing cans, labeling, and placing them in designated positions.

Z2. Preparation of component B

Add the measured polyether, plasticizer, dispersant, defoaming agent and curing agent (TDMA-02) into the reaction kettle, turn on stirring (200r/min), turn on the heat source and set the temperature to 85°C.

When the temperature rises to 85°C, start adding the measured inorganic filler and anti-settling agent in sequence, increase the rotation speed to 400r/min, and stir for about 10 minutes. Raise the temperature to 115°C, turn on the vacuum pump, keep it above -0.095MPa, vacuum dehydrate for 4 hours, and control the temperature within the range of 115±3°C.

Turn off the vacuum system, turn on the nitrogen protection system, take a sample to detect the moisture content in the system, the moisture content requirement is ≤0.3‰, if the moisture is >0.3%, turn on the vacuum system, turn off the nitrogen protection system, keep it above -0.095MPa, vacuum dehydrate for 1 hour, and then Carry out sampling and retesting until the moisture content is ≤0.3‰.

Then cool down to 60°C. Add the measured catalyst and solvent, stir for 15 minutes, then turn on the vacuum pump, close the nitrogen valve, maintain -0.095MPa, and degas for more than 30 minutes.

Gradually reduce the stirring speed to stop, turn off the vacuum pump, open the air release valve, and remove the negative pressure in the equipment.

Unloading materials, washing cans, labeling, and placing them in designated positions.

Disadvantages:

Comparing this comparative example with Example 2, there is a strong pungent smell in the paint.

Performance test experimental data:

According to the standard GB/T 19250-2013 "Polyurethane Waterproof Coating" and T/CBMF XX-2020 "Coating Product Odor Evaluation Method", the environmentally friendly high elongation two-component polyurethane waterproof coating in each embodiment was tested for indicators. The results are shown in Table 1:

Table 1 Performance test results of environmentally friendly high elongation two-component polyurethane waterproof coating (A:B＝1:2)

It can be seen from Table 1 that in each embodiment, the two-component polyurethane waterproof coating has excellent physical properties and meets the requirements of the high-performance standard (GB/T 19250 Type II). However, other indicators in each embodiment are different: First, in Examples 1-3, TDMA-02 was used as the curing agent, which not only eliminated the risk of cancer, but also showed no precipitation (no particles) when tested at low temperatures.

Second, in Implementation Cases 1-3, the viscosity of the paint was low, it could be applied smoothly, and no bubbles were found on the surface of the coating film.

Third: In implementation cases 1-3, the taste of the paint is weak (level 2) and the elongation rate is high.

Fourth: In Comparative Cases 1 and 2, the method of reducing the solvent or removing the solvent was used to prepare low-odor paint, but this not only increased the viscosity of the paint (unfavorable to construction), but also caused bubbles to appear on the surface of the coating film (the surface tension of the paint was high) , reduce the waterproof performance of the coating.

Fifth, MOCA was used as the curing agent in Comparative Case 3, which poses a risk of cancer. Moreover, MOCA precipitated under low-temperature testing and particles appeared in the paint. There is a risk of this phenomenon during the transportation or storage of the paint, which not only reduces the physical properties, but also causes particles to appear in the paint, which affects the construction of the paint and the appearance of the coating film.

Sixth, in Comparative Case 4, the curing agent in the paint is DMTDA (monophenyl primary amine). Since this curing agent has a sulfide odor, there is an obvious sulfide smell in the paint, and its monophenyl primary amine The amine structure gives it slightly higher elongation.

Seventh, in Comparative Case 5, the paint has a strong pungent smell because conventional solvent oil is used in the paint. Preparation of paint with pungent odor.

Eighth, from the formula point of view, the elongation of coating films using TDMA-02 is above 1000% or even more than 1200%.

Therefore, what is prepared in the implementation case is an environmentally friendly high-elongation two-component polyurethane waterproof coating. While ensuring physical properties and construction performance, it has low taste, environmentally friendly and high-elongation physical and chemical properties, and this coating can be stored in the winter. more stable.

Raw material information:

The environmentally friendly high-elongation two-component polyurethane waterproof coating and preparation method of the present invention are not limited to the above embodiments. Any improvements or replacements based on the principles of the present invention should be within the scope of the present invention. .

Claims (10)

1. An environmentally friendly high-elongation two-component polyurethane waterproof coating, which is characterized in that: it is composed of component A and component B mixed according to a mass ratio of 1:2; The A component is mainly prepared from the following components according to the following weight parts ratio: Polyether resin 67-73 Isocyanate curing agent 26-32 High boiling point organic solvents 1-4 The B component is mainly prepared from the following components according to the following weight parts ratio: The chain extender is TDMA-02. 2. An environmentally friendly high-elongation two-component polyurethane waterproof coating according to claim 1, characterized in that: the polyether resin is polyether 2000D, polyether 1000D, polyether 330N, or polyether M500. One or a mixture of any two in any proportion. 3. A kind of environment-friendly high elongation two-component polyurethane waterproof coating according to claim 1, characterized in that: the plasticizer is dioctyl terephthalate, chlorinated paraffin, diacetyl adipate. One or a mixture of any two of octyl fat, dioctyl phthalate in any proportion. 4. An environmentally friendly high-elongation two-component polyurethane waterproof coating according to claim 1, characterized in that: the dispersant is branched polycarboxylic acid, linear alkyl amide, grafted acrylic acid One or a mixture of any two of copolymers or long-chain polyurethane dispersants in any proportion. 5. An environmentally friendly high-elongation two-component polyurethane waterproof coating according to claim 1, characterized in that: the inorganic filler is one or any of talc powder, metakaolin, calcium powder or mica powder. A mixture of two mixtures in any proportion. 6. An environmentally friendly high-elongation two-component polyurethane waterproof coating according to claim 1, characterized in that: the anti-settling agent is bentonite, magnesium aluminum silicate, polyurea rheology agent, polyamide wax One or a mixture of any two in any proportion. 7. An environmentally friendly high-elongation two-component polyurethane waterproof coating according to claim 1, characterized in that: the isocyanate curing agent is 2,4-toluene diisocyanate, 2,4-toluene diisocyanate. One or a mixture of any two of isocyanate, 2,4-diphenylmethane diisocyanate in any proportion. 8. An environmentally friendly high-elongation two-component polyurethane waterproof coating according to claim 1, characterized in that: the catalyst is one or two of organic bismuth and organic zinc mixed in any proportion. mixture. 9. An environmentally friendly high-elongation two-component polyurethane waterproof coating according to claim 1, characterized in that: the high boiling point organic solvent is one of isoparaffin, dearomatized hydrocarbon, and naphthenic solvent. or a mixture of any two in any proportion; The defoaming agent is one of a silicone defoaming agent, a polyether defoaming agent, an amide defoaming agent, a phosphate defoaming agent, or a mixture of any two of them in any proportion. 10. The preparation method of the environmentally friendly high elongation two-component polyurethane waterproof coating according to any one of claims 1 to 9, characterized in that it includes the following steps: The A component is mainly prepared by the following methods: Add the polyether resin into the reaction kettle, and dehydrate under vacuum for more than 4 hours at a stirring speed of 200-300r/min, a temperature of 112-118°C, and a pressure of -0.095Mpa or more until the moisture content is ≤0.3‰. Then close the vacuum valve on the reaction kettle, open the nitrogen valve, then close the vacuum pump, and after the nitrogen pressure reaches 0.02Mpa, open the cooling system until the temperature cools to 80-84°C, then maintain this temperature and add isocyanate curing agent for reaction 2.5 -3h; Then cool and lower the temperature to 55-60°C, add a high-boiling point organic solvent, and finally control the temperature at 50-55°C for vacuum degassing for more than 30 minutes to obtain the component A; The B component is mainly prepared by the following methods: Add the polyether resin, plasticizer, dispersant, defoaming agent and TDMA-02 into the reactor, then add the inorganic filler and anti-settling agent in sequence at a stirring speed of 200r-300r/min and a temperature of 80-85°C. , then increase the rotation speed to 400-450r/min and stir for about 10-15min; then increase the temperature to 112-118℃, maintain this temperature at -0.095±0.005MPa, and vacuum dehydrate for more than 4h until the moisture content requirement is ≤0.3‰ ; Then cool down to 55-60°C, add catalyst and high-boiling point organic solvent, stir for 10-15 minutes and then degas at negative pressure -0.095±0.005Mpa for more than 30 minutes; Gradually reduce the stirring speed to stop, turn off the vacuum pump, open the vent valve, and remove the negative pressure in the equipment to obtain the component B.