WO2017005072A1

WO2017005072A1 - Flame-retardant heat-insulated coating for curtain wall and preparation method therefor

Info

Publication number: WO2017005072A1
Application number: PCT/CN2016/084897
Authority: WO
Inventors: 梁怡芃
Original assignee: 梁怡芃
Priority date: 2015-07-06
Filing date: 2016-06-06
Publication date: 2017-01-12
Also published as: CN104987795A

Abstract

A flame-retardant heat-insulated coating for a curtain wall consists of the of the following raw materials in parts by weight: 100 to 115 parts of modified acrylic resin, 1 to 1.6 parts of a leveling agent, 3 to 4 parts of (1S,3S,5S)-3-(amino carbonyl)-2-azabycialo[3.1.0]hexane-2-Tert-Butyl formate, 0.8 to 1.6 parts of guanidine carbonate, 1 to 1.5 parts of zinc molybdate, and 10 to 15 parts of bis(3,4-diphenylmethylene)sorbitol.

Description

Flame-retardant heat-insulating coating for curtain wall and preparation method thereof

Technical field

The invention relates to the technical field of coatings, in particular to a flame-retardant heat-insulating coating for curtain wall and a preparation method thereof.

Background technique

Curtain wall spraying functional coating is an important means of building energy saving, and its cost is low and construction is convenient. Although the existing performance index of the existing thermal insulation coatings has reached a high level, comprehensive indicators such as comprehensive temperature resistance, flame retardant, heat insulation, waterproof and adhesion are still difficult to meet the requirements. The large amount of flame retardant added to the existing coatings leads to a decrease in heat insulation efficiency, which affects the overall performance of the coating. Some paint coatings are thick and uneconomical to apply. Other coatings contain a large amount of organic solvents, and VOC volatilization is high, which is not conducive to use in environmentally friendly building materials. Commonly used thermal insulation coatings have a reduced thermal insulation effect over time. The development of curtain wall with high flame retardant efficiency, high heat insulation efficiency, low cost, and small pollution coating is a big problem in front of people.

Summary of the invention

In order to meet the needs of the current curtain wall coating, the embodiment of the invention provides a flame-retardant heat-insulating coating for a curtain wall and a preparation method thereof.

In order to achieve the above object, the present invention provides a flame-retardant heat-insulating coating for a curtain wall, which is composed of the following raw materials by weight: 100-115 parts of modified acrylic resin, 1-1.6 parts of leveling agent, (1S, 3S, 5S) 3-(aminocarbonyl)-2-azabicyclo[3.1.0]hexane-2-carboxylic acid tert-butyl ester 3-4 parts, cesium carbonate 0.8-1.6 parts, zinc molybdate 1-1.5 parts and double (3,4-Dimethylbenzylidene) sorbitol 10-15 parts.

The method for preparing the modified acrylic resin comprises the following steps:

Mixing nano boron oxide, 1,1,1-trimethylolpropane, aluminum sulfate and deionized water with a mass ratio of 8-9:1-2:60-70:200-220, stirring evenly, stirring speed 120-160r/min, adjust the pH value of 8.2-8.5, stir for 2-3 hours, reduce the stirring speed to 20-50r / min, continue to stir for 1-2 hours, then dry at 60-80 ° C to obtain powder A;

Mix and mix acrylic acid, dimethyldiethylsilane, epoxy succinic acid, powder A and deionized water with a mass ratio of 3-5:0.5-1:2-3:0.04-0.09:18-27 , stirring speed 90-110r/min, Adding ammonia water under stirring to adjust the PH value to 8-8.5 to obtain a mixture 1;

Mixing a mixture of dicumyl hydroperoxide, N,N-methylenebisacrylamide, sodium hydrogen sulfite and deionized with a mass ratio of 6:3:5:100 to obtain a mixture of two;

Add the mixture to the mixture 1 and continue to stir the mixture for 8-10 minutes, the temperature is controlled at 60-65 ° C, keep warm for 20-30 minutes, add the hollow glass beads to adjust the stirring speed to 180-240r / min to the stirring equipment Filling with nitrogen to replace the oxygen in the stirring device, after stirring for 5-8 minutes, the stirring speed is reduced to 60-70r/min; the mixture 1: the mass ratio of the mixture 2 is 1000: 1-2; the hollow The glass microbeads account for 2-5% of the three masses of the mixture;

Then, a mixture of triammonium hydrogen carbonate and 4,4'-oxybisbenzenesulfonyl hydrazide, which is a mixture of three to two parts by mass, is quickly added, and then potassium persulfate is added in an amount of 0.08 to 0.12% by weight of the mixture, and stirring is continued. 0.5-1min, the stirring is stopped, after leaving for 60-120 minutes, the temperature is lowered to 20-25 ° C to obtain a modified acrylic resin;

The mass ratio of the ammonium hydrogencarbonate to the 4,4'-oxobisbenzenesulfonylhydrazide was 28:5.

The hollow glass microbeads have a particle size of 10-30 μm.

The leveling agent is PV88.

The preparation method of the coating material comprises the following steps: mixing the raw materials in proportion according to the ratio.

The beneficial effects brought by the technical solutions provided by the embodiments of the present invention are:

1. The flame retardant effect and heat insulation effect of the coating are excellent;

2. The environmental pollution is small, the processing technology is simple, and it is easy to operate.

3. Long-term use of glass beads will not precipitate.

4, the coating weather resistance is good, and the coating components will not precipitate.

detailed description

The invention provides a flame-retardant heat-insulating coating for a curtain wall and a preparation method thereof for the problem that the comprehensive performance of the curtain wall coating is poor.

The embodiments of the present invention will be described in detail below by way of examples, by which the present invention can be applied to the technical problems, and the implementation of the technical effects can be fully understood and implemented.

(1S,3S,5S)-3-(Aminocarbonyl)-2-azabicyclo[3.1.0]hexane-2-carboxylic acid tert-butyl ester: CAS No.: 361440-67-7

4,4'-oxobisbenzenesulfonyl hydrazide: CAS No. 80-51-3

Bis(3,4-dimethylbenzylidene) sorbitol: CAS No. 135861-56-2

1,1,1-trimethylolpropane: CAS No. 77-99-6

Dimethyldiethylsilane: CAS No. 756-81-0

Epoxy succinic acid: CAS No. 16533-72-5

Diisopropylbenzene hydrogen peroxide: CAS No. 26762-93-6

N,N-methylenebisacrylamide: CAS No. 110-26-9

Barium carbonate CAS number 593-85-1

Example 1

Step 1. The preparation method of the modified acrylic resin comprises the following steps:

Nano-boron oxide: 1,1,1-trimethylolpropane: aluminum sulfate (ie Al ₂ (SO ₄ ) ₃ ): mixed with deionized water at a mass ratio of 8.5:1:60:200, stirred evenly, stirring speed 120r / min, adjust the pH value of 8.5, after stirring for 3 hours, reduce the stirring speed to 50r / min, continue to stir for 1 hour, 80 ° C to dry to obtain a powder A;

Acrylic acid, dimethyldiethylsilane, epoxy succinic acid: powder A: deionized water with a mass ratio of 5:1:3:0.06:27, stirred and mixed uniformly, stirring speed 110r/min, under stirring Adding ammonia water to adjust the pH to 8.5 to obtain a mixture 1;

Diisopropylbenzene hydrogen peroxide: N, N-methylene bis acrylamide: sodium hydrogen sulfite: deionized water mass ratio of 6:3:5:100 mixed to obtain a mixture of two;

Add the mixture 2 to the mixture 1 and continue to stir the mixture for 9 minutes for 3 minutes, control the temperature at 65 ° C, keep for 25 minutes, add the hollow glass beads to adjust the stirring speed to 240 r / min, and fill the stirring equipment with nitrogen to replace the stirring equipment. Oxygen in the mixture, after stirring for 5 minutes, the stirring speed is reduced to 70r/min; the mixture one: the mixture has a mass ratio of 1000:1; the hollow glass microbeads account for 2% of the mass of the mixture; the hollow glass The bead size was 10 μm.

Then, a mixture of 3% by mass of ammonium hydrogencarbonate and 4,4'-oxobisbenzenesulfonyl hydrazide in the mixture was quickly added, and then 0.5% potassium persulfate was added to the mixture at a mass of 0.1%, stirring was continued for 1 min, and stirring was stopped. After standing for 100 minutes, the temperature was lowered to 25 ° C to obtain a modified acrylic resin;

Step 2: Preparation of flame retardant thermal insulation coating for curtain wall: 100 parts of modified acrylic resin, leveling agent PV881.2 parts, (1S, 3S, 5S)-3-(aminocarbonyl)-2-azabicyclo[3.1 .0] 3 parts of hexane-2-carboxylic acid tert-butyl ester, 1 part of cesium carbonate, 1.5 parts of zinc molybdate, and 12 parts of bis(3,4-dimethylbenzylidene) sorbitol may be uniformly mixed.

The thermal conductivity of the coating is 0.0104 W/(m·K); the visible light reflectance is 94%, the near-infrared light blocking rate is 90%, and the ultraviolet light absorption rate is 99.5%.

The curtain wall coating is coated on the glass plate, and after drying, a coating film of about 2 mm thick is obtained, and the coating film is removed from the glass plate, and the oxygen index is measured according to the national standard GB/T2406, and the oxygen index is 34.4%.

Example 2

Nano-boron oxide: 1,1,1-trimethylolpropane: aluminum sulfate (ie Al ₂ (SO ₄ ) ₃ ): mixed with deionized water at a mass ratio of 8:1:70:220, stirred evenly, stirring speed 160r / min, adjust the pH value of 8.2, after stirring for 2 hours, reduce the stirring speed to 20r / min, continue to stir for 2 hours, then dry at 60 ° C to obtain a powder A;

Acrylic acid, dimethyldiethylsilane, epoxy succinic acid: powder A: deionized water with a mass ratio of 3:0.5:2:0.04:18, stirred and mixed uniformly, stirring speed 100r/min, under stirring Adding ammonia water to adjust the pH value to 8 to obtain a mixture 1;

Diisopropylbenzene hydrogen peroxide: N, N-methylene bis acrylamide: sodium hydrogen sulfite: deionized mass ratio of 6:3:5:100 mixed uniformly to obtain a mixture of two;

Add the mixture 2 to the mixture 1 and continue to stir the mixture for 8 minutes for 8 minutes. The temperature is controlled at 60 ° C, and the temperature is kept for 20 minutes. The stirring speed is adjusted to 180 r / min by adding hollow glass beads. The stirring equipment is filled with nitrogen to replace the stirring equipment. Oxygen in the mixture, after stirring for 6 minutes, the stirring speed is reduced to 60r/min; the mixture one: the mixture has a mass ratio of 1000:2; the glass microbeads account for 3% of the three masses of the mixture; the hollow glass micro The bead size was 30 μm.

Then rapidly add a mixture of 3% by mass of ammonium hydrogencarbonate and 4,4'-oxybisbenzenesulfonyl hydrazide, and then immediately add 0.12% of potassium persulfate to the mixture, continue stirring for 0.5 min, stop After stirring for 60 minutes, the temperature was lowered to 20 ° C to obtain a modified acrylic resin;

Step 2: Preparation of flame retardant thermal insulation coating for curtain wall: 105 parts of modified acrylic resin, leveling agent PV881.6 parts, (1S, 3S, 5S)-3-(aminocarbonyl)-2-azabicyclo[3.1 .0] 4 parts of hexane-2-carboxylic acid tert-butyl ester, 0.8 parts of cesium carbonate, 1 part of zinc molybdate, and 10 parts of bis(3,4-dimethylbenzylidene) sorbitol may be uniformly mixed.

The thermal conductivity of the coating is 0.0126 W/(m·K); the visible light reflectance is 95%, and the near-infrared light blocking ratio is 92. %, the ultraviolet light absorption rate is 99.1%.

The curtain wall coating is coated on the glass plate, and after drying, a coating film of about 2 mm thick is obtained, and the coating film is removed from the glass plate, and the oxygen index is measured according to the national standard GB/T2406, and the oxygen index is 36.4%.

Example 3

Nano-boron oxide: 1,1,1-trimethylolpropane: aluminum sulfate (ie, Al ₂ (SO ₄ ) ₃ ): mixed with deionized water at a mass ratio of 9:2:65:210, stirred evenly, stirring speed 140r / min, adjust the pH value of 8.5, after stirring for 3 hours, reduce the stirring speed to 30r / min, continue to stir for 1 hour, then dry at 70 ° C to obtain a powder A;

Acrylic acid, dimethyldiethylsilane, epoxy succinic acid: powder A: deionized water with a mass ratio of 4:0.8:3:0.09:24, stirred and mixed uniformly, stirring speed 90r/min, under stirring Adding ammonia water to adjust the pH to 8.5 to obtain a mixture 1;

Add the mixture 2 to the mixture 1 and continue to stir the mixture for 10 minutes for 10 minutes, control the temperature at 65 ° C, keep for 30 minutes, add the hollow glass beads to adjust the stirring speed to 200 r / min, and fill the stirring equipment with nitrogen to replace the stirring equipment. Oxygen in the mixture, after stirring for 8 minutes, the stirring speed is reduced to 70r/min; the mixture one: the mixture mass ratio is 1000:1; the glass microbeads account for 5% of the mixture of three mass; the hollow glass micro The bead size was 20 μm.

Then, a mixture of 3% by mass of ammonium hydrogencarbonate and 4,4'-oxybisbenzenesulfonyl hydrazide in the mixture was quickly added, and then potassium persulfate which was 0.08% by mass of the mixture was added immediately, stirring was continued for 1 min, and stirring was stopped. After standing for 120 minutes, the temperature was lowered to 25 ° C to obtain a modified acrylic resin;

Step 2: Preparation of flame retardant thermal insulation coating for curtain wall: 115 parts of modified acrylic resin, PV881 part of leveling agent, (1S, 3S, 5S)-3-(aminocarbonyl)-2-azabicyclo[3.1.0 3 parts of hexane-2-carboxylic acid tert-butyl ester, 1.6 parts of cesium carbonate, 1.2 parts of zinc molybdate, and 15 parts of bis(3,4-dimethylbenzylidene) sorbitol may be uniformly mixed.

The thermal conductivity of the coating is 0.0113 W/(m·K); the visible light reflectance is 96%, the near-infrared light blocking rate is 92%, and the ultraviolet light absorption rate is 99.2%.

The curtain wall coating is coated on the glass plate, and after drying, a coating film of about 2 mm thick is obtained, and the coating film is removed from the glass plate, and the oxygen index is measured according to the national standard GB/T2406, and the oxygen index is 40.4%.

In summary, the coatings of Examples 1-3 of the present invention have excellent comprehensive performance, and have not only good thermal insulation properties, but also high visible light reflectance, near-infrared light blocking ratio, and ultraviolet light absorption rate, and Has a good flame retardant properties.

The above are only the preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalents, improvements, etc., which are within the spirit and scope of the present invention, should be included in the protection of the present invention. Within the scope.

Claims

A flame-retardant heat-insulating coating for curtain wall, characterized in that it is composed of the following raw materials by weight: 100-115 parts of modified acrylic resin, 1-1.6 parts of leveling agent, (1S, 3S, 5S)-3-( 3-4 parts of aminocarbonyl)-2-azabicyclo[3.1.0]hexane-2-carboxylic acid tert-butyl ester, 0.8-1.6 parts of cesium carbonate, 1-1.5 parts of zinc molybdate and bis (3,4-di) Methylbenzylidene) sorbitol 10-15 parts.
The flame-retardant heat-insulating paint for curtain wall according to claim 1, wherein the method for preparing the modified acrylic resin comprises the following steps:

Mixing nano boron oxide, 1,1,1-trimethylolpropane, aluminum sulfate and deionized water with a mass ratio of 8-9:1-2:60-70:200-220, stirring evenly, stirring speed 120-160r/min, adjust the pH value of 8.2-8.5, stir for 2-3 hours, reduce the stirring speed to 20-50r / min, continue to stir for 1-2 hours, then dry at 60-80 ° C to obtain powder A;

Mix and mix acrylic acid, dimethyldiethylsilane, epoxy succinic acid, powder A and deionized water with a mass ratio of 3-5:0.5-1:2-3:0.04-0.09:18-27 , stirring speed 90-110r / min, adding ammonia water under stirring to adjust the PH value of 8-8.5 to obtain a mixture 1;

Mixing a mixture of dicumyl hydroperoxide, N,N-methylenebisacrylamide, sodium hydrogen sulfite and deionized with a mass ratio of 6:3:5:100 to obtain a mixture of two;

Add the mixture to the mixture 1 and continue to stir the mixture for 8-10 minutes, the temperature is controlled at 60-65 ° C, keep warm for 20-30 minutes, add the hollow glass beads to adjust the stirring speed to 180-240r / min to the stirring equipment Filling with nitrogen to replace the oxygen in the stirring device, after stirring for 5-8 minutes, the stirring speed is reduced to 60-70r/min; the mixture 1: the mass ratio of the mixture 2 is 1000: 1-2; the hollow The glass microbeads account for 2-5% of the three masses of the mixture;

Then, a mixture of triammonium hydrogen carbonate and 4,4'-oxybisbenzenesulfonyl hydrazide, which is a mixture of three to two parts by mass, is quickly added, and then potassium persulfate is added in an amount of 0.08 to 0.12% by weight of the mixture, and stirring is continued. 0.5-1min, the stirring is stopped, after leaving for 60-120 minutes, the temperature is lowered to 20-25 ° C to obtain a modified acrylic resin;

The mass ratio of the ammonium hydrogencarbonate to the 4,4'-oxobisbenzenesulfonylhydrazide was 28:5.
The flame-retardant heat-insulating coating for curtain wall according to claim 1, wherein the hollow glass microspheres have a particle diameter of 10 to 30 μm.
The flame-retardant heat-insulating paint for curtain wall according to claim 1, wherein the leveling agent For PV88.
The flame-retardant heat-insulating paint for curtain wall according to any one of claims 1 to 4, wherein the method for preparing the paint comprises the following steps: mixing the raw materials uniformly according to the ratio.