A method for preparing a water-based constant temperature heat insulation and waterproof coating

Abstract

The invention discloses a method for preparing a water-based constant temperature heat insulation waterproof coating, and belongs to the technical field of building coatings. 20-25 parts of water, 2-3 parts of propylene glycol, 0.3-0.7 parts of dispersant and 0.1-0.5 parts of defoamer are added to a reactor and stirred, followed by adding 15-20 parts of inorganic fillers, 10-15 parts of auxiliary agents and 5-10 parts of hollow glass microspheres and stirring, then adding 35-40 parts of polymer emulsion, 0.1-0.5 parts of preservatives and 8-10 parts of film-forming aids, stirring and adjusting the pH value to 8.5, and finally adding 0.3-0.6 parts of thickeners to adjust the viscosity to obtain a coating; the silane alkoxy groups on the auxiliary agents make the nitrogen, phosphorus and silicon synergistic flame retardant auxiliary agents uniformly dispersed in the coating, and then the coating of the invention has excellent and stable flame retardant effect and waterproof and water resistance, and the high dispersion of inorganic fillers and the like makes the coating have excellent adhesion, waterproofness and thermal insulation performance.

Description

Technical Field

[0001] The invention belongs to the technical field of building coatings, and in particular relates to a method for preparing a water-based constant temperature heat insulating and waterproof coating. Background Art

[0002] Building thermal insulation is an important aspect of saving energy and improving the living and use functions of buildings. Building energy consumption generally accounts for 30-40% of the total energy consumption, most of which is energy consumption for heating and cooling. Building material insulation and energy-saving measures include the use of energy-saving insulation materials and building insulation coatings. At present, more than 90% of building design and construction use organic insulation materials such as extruded polystyrene foam (XPS), molded polystyrene foam (EPS), and rigid polyurethane foam (PU) as exterior wall insulation materials, but these insulation materials have extremely poor fire resistance and will melt, deform, and drip at 80°C, making them flammable building materials.

[0003] Spraying thermal insulation paint on the exterior walls of buildings is another means of building energy conservation. It has low cost, convenient construction, and good thermal insulation effects. However, current building thermal insulation paints also generally have poor fire retardant effects. Since the base materials are all made of polymers, which are flammable, the coatings cannot achieve the fire retardant effects, posing a safety hazard. Summary of the invention

[0004] The purpose of the present invention is to overcome the defects of the prior art and provide a method for preparing a water-based constant temperature heat-insulating and waterproof coating.

[0005] The purpose of the present invention can be achieved through the following technical solutions:

[0006] A method for preparing a water-based constant temperature heat insulation and waterproof coating comprises the following steps:

[0007] First, 20-25 parts of water, 2-3 parts of propylene glycol, 0.3-0.7 parts of dispersant and 0.1-0.5 parts of defoaming agent are added into a reaction kettle, stirred, then 15-20 parts of inorganic filler, 10-15 parts of auxiliary agent and 5-10 parts of hollow glass microspheres are added, stirred and mixed to obtain a slurry of water-based flame retardant heat insulation coating; subsequently, 35-40 parts of polymer emulsion, 0.1-0.5 parts of preservative and 8-10 parts of film-forming aid are added into the slurry, stirred, and the pH value is adjusted to 8.5; finally, 0.3-0.6 parts of thickener are added to adjust the viscosity of the coating to prepare a water-based constant temperature heat insulation waterproof coating.

[0008] Furthermore, the dispersant is one of sodium polyphosphate, dispersant 5040, and Dispex N40.

[0009] Furthermore, the defoaming agent is tributyl phosphate.

[0010] Furthermore, the inorganic filler is one or more of nano zinc oxide, nano titanium dioxide, nano silicon dioxide, nano aluminum oxide, nano magnesium oxide, and nano calcium carbonate.

[0011] Nano inorganic fillers, due to their nano-scale size and good surface effect, can be added to coatings to improve the physical and chemical properties of the coatings, thereby improving the hardness, gloss, waterproofness, durability, adhesion and weather resistance of the coatings.

[0012] Furthermore, the auxiliary agent is prepared by the following steps:

[0013] S1. A fully dried four-necked flask was purged with nitrogen for 30 min, and then chloroform, 4-chloro-1-butene and triethylamine were added, and the mixture was stirred until uniformly mixed. Then, N-methyl-2-hydroxyethylamine was slowly added while stirring. After the addition was completed, the mixture was heated to 90° C. and stirred for reaction at 90° C. for 6 h. After the reaction was completed, the mixture was cooled to room temperature and distilled under reduced pressure to obtain intermediate 1; the amount ratio of N-methyl-2-hydroxyethylamine, 4-chloro-1-butene, triethylamine and chloroform was 9.5 mL:10 mL:16 mL:110 mL;

[0014] Under base catalysis, -NH- of N-methyl-2-hydroxyethylamine and -Cl of 4-chloro-1-butene undergo nucleophilic substitution reaction. The reaction process is as follows:

[0015]

[0016] S2, blow nitrogen gas into a dry three-necked flask for 30 minutes, add intermediate 1 and N,N-methylenediamide (DMF) into the flask, stir well, then slowly add a mixed solution of tripolychlorophosphazene and DMF, evacuate the system after the addition, react at room temperature for 1.5 hours, heat to 50°C for 2 hours, and then heat to 90°C for 2 hours, remove the tail gas absorption part of hydrogen chloride, and distill under reduced pressure after the reaction to obtain intermediate 2; the amount ratio of intermediate 1 to tripolychlorophosphazene is 6.95g:15.5g;

[0017] The molar ratio of tripolyphosphazene chloride and intermediate 1 is controlled to be 1:6, and the -Cl of tripolyphosphazene chloride and the -OH of intermediate 1 can undergo the following chemical reaction, and the reaction process is as follows:

[0018]

[0019] S3. Blow nitrogen gas into a dry single-necked flask for 30 minutes, dissolve the intermediates 2, 3-mercaptopropyltriethoxysilane and benzoin dimethyl ether in DMF at room temperature, then pour them into a single-necked flask, place it under a 365nm ultraviolet lamp, irradiate it with stirring for 20 minutes, and dry it for 12 hours. The whole process is carried out under nitrogen protection to obtain an auxiliary agent; the dosage ratio of the intermediates 2, 3-mercaptopropyltriethoxysilane, benzoin dimethyl ether and DMF is 9g:14.5mL:0.18g:50mL.

[0020] The molar ratio of intermediate 2 to 3-mercaptopropyltriethoxysilane is controlled to be 1:6, and the carbon-carbon double bond of intermediate 2 undergoes a mercapto-ene click reaction with the -SH of 3-mercaptopropyltriethoxysilane. The reaction process is as follows:

[0021]

[0022] The additive of the present invention contains halogen-free flame retardant elements of nitrogen, phosphorus and silicon, wherein the nitrogen and phosphorus elements have gas phase and condensed phase flame retardant mechanisms, and belong to nitrogen-phosphorus flame retardant components. The organic silicon halogen-free flame retardant component is a carbon-forming smoke suppressant, which synergistically flame retards with the nitrogen-phosphorus flame retardant, and therefore belongs to the nitrogen-phosphorus-silicon synergistic flame retardant component. In addition, the density of each element on a single flame retardant molecule is high, so that the additive has efficient and safe flame retardant properties, thereby making the water-based constant temperature heat insulation and waterproof coating have excellent flame retardant effect; the additive of the present invention contains high-density silaneoxy Siloxy groups will hydrolyze and polycondense, and then cross-link with polymer emulsion, inorganic filler and hollow glass microspheres. On the one hand, this makes the additive itself evenly dispersed and stably present in the coating, giving full play to the flame retardant effect. At the same time, the Si-O-Si bonds produced by polycondensation increase the coating density of the coating, making the coating more waterproof and water-resistant. On the other hand, it can also increase the dispersion uniformity of inorganic fillers and hollow glass microspheres in the coating, thereby further improving the adhesion, waterproofness, thermal insulation, impact resistance and weather resistance of the coating.

[0023] Furthermore, the particle size of the hollow glass microspheres is less than 180 μm.

[0024] Hollow glass microspheres are closed hollow spheres. When added to the paint, they can form many microscopic independent insulation cavities, which greatly improve the insulation of the coating against heat and sound, thereby playing a good role in thermal insulation and noise reduction; the spherical structure of the hollow glass microspheres enables them to have a good dispersion effect on impact force and stress. Adding them to the paint can greatly improve the coating's resistance to external impact and reduce stress cracking caused by thermal expansion and contraction; the low oil absorption characteristics of the hollow glass microspheres allow more resin to participate in film formation, thereby increasing the adhesion of the coating by 3-4 times, effectively enhancing the adhesion of the coating; adding hollow glass microspheres can greatly reduce the weight of the coating and avoid the occurrence of wall coating shedding; hollow glass microspheres also have a good reflective effect on ultraviolet rays, which can prevent the coating from yellowing and aging to a certain extent.

[0025] Furthermore, the polymer emulsion is one or more of styrene-acrylic emulsion, pure acrylic emulsion, silicone-acrylic emulsion, and acetate-acrylic emulsion.

[0026] Furthermore, the preservative is an isothiazolinone preservative.

[0027] Furthermore, the film-forming aid is 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate.

[0028] Furthermore, the thickener is one or more of hydroxymethyl cellulose, hydroxyethyl cellulose, methyl cellulose, hydroxypropyl methyl cellulose, sodium polyacrylate, organic bentonite, guar gum or xanthan gum.

[0029] Beneficial effects of the present invention: the synergistic flame-retardant additives of nitrogen, phosphorus and silicon make the water-based constant temperature heat-insulating and waterproof coating of the present invention have efficient and safe flame-retardant properties, the silaneoxy groups on the additives make the additives dispersed evenly in the coating for a long time, and thus the coating of the present invention has excellent and stable flame-retardant effects and waterproof and water-resistant properties for a long time, the silaneoxy groups on the additives also increase the dispersion uniformity of inorganic fillers and hollow glass microspheres in the coating, and thus the coating of the present invention has excellent adhesion, waterproofness and thermal insulation properties, etc. DETAILED DESCRIPTION

[0030] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention. Example 1

[0031] Preparation of auxiliary agent, the specific steps are as follows:

[0032] S1. A dry 250 mL four-necked flask was purged with nitrogen for 30 min, and then 110 mL of chloroform, 10 mL of 4-chloro-1-butene and 16 mL of triethylamine were added, and the mixture was stirred until uniformly mixed. Then, 9.5 mL of N-methyl-2-hydroxyethylamine was slowly added while stirring. After the addition was completed, the temperature was raised to 90° C., and the reaction was stirred at 90° C. for 6 h. After the reaction was completed, the mixture was cooled to room temperature and distilled under reduced pressure to obtain intermediate 1;

[0033] S2, purging a dry 250mL three-necked flask with nitrogen for 30min, adding 6.95g of intermediate 1 and 50mL of DMF to the flask, stirring thoroughly, then slowly adding a mixed solution of 15.5g of tripolyphosphazene chloride and 100mL of DMF, evacuating the system after the addition, reacting at room temperature for 1.5h, heating to 50°C for 2h, and then heating to 90°C for 2h, removing the tail gas absorption part of hydrogen chloride, and distilling under reduced pressure after the reaction to obtain intermediate 2;

[0034] S3. Blow nitrogen gas into a dry 100 mL single-necked flask for 30 min, dissolve 9 g of intermediate 2, 14.5 mL of 3-mercaptopropyltriethoxysilane and 0.18 g of benzoin dimethyl ether in 50 mL of DMF at room temperature, then pour the mixture into the single-necked flask, place the mixture under a 365 nm ultraviolet lamp, irradiate the mixture with stirring for 20 min, and then dry the mixture for 12 h. The entire process is carried out under nitrogen protection to obtain an auxiliary agent. Example 2

[0035] Preparation of auxiliary agent, the specific steps are as follows:

[0036] The remaining steps remain unchanged, and step S3 of Example 1 is removed to prepare the auxiliary agent. Example 3

[0037] The specific steps for preparing the coating are as follows:

[0038] First, 20 parts of water, 2 parts of propylene glycol, 0.3 parts of sodium polyphosphate and 0.1 parts of tributyl phosphate are added to a reactor and stirred, and then 4 parts of nano zinc oxide, 3 parts of nano titanium dioxide, 3 parts of nano silicon dioxide, 3 parts of nano magnesium oxide, 2 parts of nano calcium carbonate, 10 parts of the additives of Example 1 and 5 parts of hollow glass microspheres are added, and stirred and mixed to obtain a slurry of a water-based flame retardant heat-insulating and thermal insulation coating; then 35 parts of pure acrylic emulsion, 0.1 parts of 1,2-benzisothiazol-3-one and 8 parts of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate are added to the slurry, stirred, and the pH value is adjusted to 8.5; finally, 0.3 parts of hydroxymethyl cellulose are added to adjust the viscosity of the coating to prepare a water-based constant temperature heat-insulating and waterproof coating. Example 4

[0039] The specific steps for preparing the coating are as follows:

[0040] First, 23 parts of water, 2.5 parts of propylene glycol, 0.5 parts of dispersant 5040 and 0.4 parts of tributyl phosphate are added to a reaction kettle and stirred, and then 5 parts of nano zinc oxide, 4 parts of nano silicon dioxide, 3 parts of nano titanium dioxide, 3 parts of nano aluminum oxide, 3 parts of nano calcium carbonate, 14 parts of the additives of Example 1 and 8 parts of hollow glass microspheres are added, and stirred and mixed to obtain a slurry of a water-based flame-retardant heat-insulating and thermal-insulating coating; then 17 parts of styrene-acrylic emulsion, 20 parts of pure acrylic emulsion, 0.4 parts of 5-chloro-2-methyl-4-isothiazoline-3-one and 9 parts of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate are added to the slurry, stirred, and the pH value is adjusted to 8.5; finally, 0.5 parts of organic bentonite are added to adjust the viscosity of the coating to prepare a water-based constant temperature heat-insulating and thermal-insulating waterproof coating. Example 5

[0041] The specific steps for preparing the coating are as follows:

[0042] First, 25 parts of water, 3 parts of propylene glycol, 0.7 parts of dispersant DispexN40 and 0.5 parts of tributyl phosphate are added to a reactor and stirred, and then 6 parts of nano zinc oxide, 5 parts of nano silicon dioxide, 3 parts of nano titanium dioxide, 3 parts of nano aluminum oxide, 3 parts of nano calcium carbonate, 15 parts of the additives of Example 1 and 10 parts of hollow glass microspheres are added, and stirred and mixed to obtain a slurry of a water-based flame retardant heat-insulating and thermal insulation coating; then 20 parts of silicone-acrylic emulsion, 20 parts of acetic acid-acrylic emulsion, 0.5 parts of preservative Huake-981 and 10 parts of 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate are added to the slurry, stirred, and the pH value is adjusted to 8.5; finally, 0.6 parts of sodium polyacrylate are added to adjust the viscosity of the coating to prepare a water-based constant temperature heat-insulating and waterproof coating.

[0043] Comparative Example 1

[0044] The specific steps for preparing the coating are as follows:

[0045] The remaining steps remain unchanged, and the auxiliary agent in Example 5 is replaced by the auxiliary agent in Example 2 to prepare the coating.

[0046] Comparative Example 2

[0047] The specific steps for preparing the coating are as follows:

[0048] The remaining steps remain unchanged, and the additives in Example 5 are removed to prepare the coating.

[0049] Comparative Example 3

[0050] The specific steps for preparing the coating are as follows:

[0051] The remaining steps remain unchanged, and the auxiliary agent in Example 5 is replaced by melamine phosphate to prepare the coating.

[0052] Performance Testing

[0053] The limiting oxygen index of the coatings prepared in Examples 3-5 and Comparative Examples 1-3 was determined according to GB / T2406.2-2009 "Determination of Combustion Behavior by Oxygen Index Method for Plastics Part 2: Room Temperature Test";

[0054] The thermal conductivity of the coatings prepared in Examples 3-5 and Comparative Examples 1-3 was measured using the GB / T10294-2008 method;

[0055] The dry adhesion of the coatings prepared in Examples 3-5 and Comparative Examples 1-3 was measured according to the GB / T9286-1998 method;

[0056] The national standard GB / T9755-2001 "Synthetic resin emulsion exterior wall coating" was used to test various technical performance indicators of the coatings prepared in Examples 3-5 and Comparative Examples 1-3;

[0057] The test results of all items are shown in the table below:

[0058]

[0059] It can be seen from the above table that the coating prepared in the embodiment of the present invention has excellent flame retardant effect, waterproof and water-resistant and thermal insulation effect.

[0060] In the description of the specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[0061] The above contents are merely examples and explanations of the present invention. Those skilled in the art may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the invention or exceed the scope defined by the claims, they shall all fall within the protection scope of the present invention.

Claims

1. A method for preparing a water-based constant temperature heat insulation and waterproof coating, characterized in that: The steps include: 20-25 parts of water, 2-3 parts of propylene glycol, 0.3-0.7 parts of dispersant and 0.1-0.5 parts of defoamer are added to a reaction kettle and stirred, and then 15-20 parts of inorganic filler, 10-15 parts of auxiliary agent and 5-10 parts of hollow glass microspheres are added and stirred to obtain slurry; 35-40 parts of polymer emulsion, 0.1-0.5 parts of preservative and 8-10 parts of film-forming aid are added to the slurry, stirred, and the pH value is adjusted to 8.5; finally, 0.3-0.6 parts of thickener are added to adjust the viscosity of the coating to prepare a water-based constant temperature heat insulation and waterproof coating; Wherein, the auxiliary agent is prepared by the following steps: S1. Add chloroform, 4-chloro-1-butene and triethylamine into a flask, stir and add N-methyl-2-hydroxyethylamine, heat to 90°C for 6h, cool and distill under reduced pressure to obtain intermediate 1; the dosage ratio of N-methyl-2-hydroxyethylamine, 4-chloro-1-butene, triethylamine and chloroform is 9.5mL:10mL:16mL:110mL; S2, add intermediate 1 and DMF into a flask, stir, then add tripolyphosphazene chloride and DMF, evacuate the system, react at room temperature for 1.5h, heat to 50°C for 2h, then heat to 90°C for 2h, remove the tail gas absorption part of hydrogen chloride, and distill under reduced pressure to obtain intermediate 2; the usage ratio of intermediate 1 and tripolyphosphazene chloride is 6.95g:15.5g; S3, add intermediate 2, 3-mercaptopropyl triethoxysilane, benzoin dimethyl ether and DMF into a flask, place it under 365nm ultraviolet lamp for 20min, and dry it for 12h to obtain an auxiliary agent; the amount ratio of intermediate 2, 3-mercaptopropyl triethoxysilane, benzoin dimethyl ether and DMF is 9g:14.5mL:0.18g:50mL; The inorganic filler is one or more of nano zinc oxide, nano titanium dioxide, nano silicon dioxide, nano aluminum oxide, nano magnesium oxide and nano calcium carbonate.

2. The method for preparing a water-based constant temperature heat insulation and waterproof coating according to claim 1, characterized in that: The dispersant is one of sodium polyphosphate, dispersant 5040 and Dispex N40.

3. The method for preparing a water-based constant temperature heat insulation and waterproof coating according to claim 1, characterized in that: The defoaming agent is tributyl phosphate.

4. The method for preparing a water-based constant temperature heat insulation and waterproof coating according to claim 1, characterized in that: The particle size of the hollow glass microspheres is less than 180 μm.

5. The method for preparing a water-based constant temperature heat insulation and waterproof coating according to claim 1, characterized in that: The polymer emulsion is one or more of styrene-acrylic emulsion, pure acrylic emulsion, silicone-acrylic emulsion and acetate-acrylic emulsion.

6. The method for preparing a water-based constant temperature heat insulation and waterproof coating according to claim 1, characterized in that: The preservative is an isothiazolinone preservative.

7. The method for preparing a water-based constant temperature heat insulation and waterproof coating according to claim 1, characterized in that: The film-forming aid is 2,2,4-trimethyl-1,3-pentanediol monoisobutyrate.

8. The method for preparing a water-based constant temperature heat insulation and waterproof coating according to claim 1, characterized in that: The thickener is one or more of hydroxymethyl cellulose, hydroxyethyl cellulose, methyl cellulose, hydroxypropyl methyl cellulose, sodium polyacrylate, organic bentonite, guar gum or xanthan gum.

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