Waterproof redispersible latex powder based on modified versatile carbonic acid emulsion and preparation method

Abstract

The invention relates to the field of redispersible latex powder, and in particular to a waterproof redispersible latex powder based on modified versatate carbonic acid emulsion and a preparation method thereof, and is used to solve the problem of poor waterproof performance of existing redispersible latex powders. The waterproof redispersible latex powder uses modified versatate carbonic acid emulsion as a main raw material, and is endowed with good waterproof performance. When added to building materials, the waterproof redispersible latex powder can significantly improve the impermeability and water resistance of the building materials, effectively preventing moisture penetration. The redispersible latex powder has good adhesion and flexibility, and can improve the internal bonding strength of the building materials. At the same time, it endows the building materials with a certain impact resistance, and can improve the mechanical properties of the building materials, thereby significantly improving the comprehensive performance and service life of the building materials, and meeting the demand of modern buildings for high-performance waterproof materials.

Description

Technical Field

[0001] The invention relates to the field of redispersible latex powder, in particular to waterproof redispersible latex powder based on modified versatile carbonic acid emulsion and a preparation method thereof. Background Art

[0002] Redispersible polymer powder is a polymer powder produced by spray-drying an emulsion. This product exhibits excellent fluidity, dispersibility, and storage stability. When dispersed in water, the redispersible polymer powder regenerates into a stable polymer emulsion with properties similar to the original emulsion. Using redispersible polymer powder as a modifier for building materials can significantly improve their adhesion, flexibility, and mechanical strength.

[0003] However, the waterproof performance of existing redispersible latex powders still needs to be improved, especially in some humid environments or construction projects with high waterproofing requirements. Building materials modified with traditional redispersible latex powders are prone to problems such as water seepage and powdering, which affect the service life and appearance quality of the building and limit its widespread application in high-requirement construction projects.

[0004] Therefore, it is of great significance to develop a waterproof redispersible latex powder based on modified versatile carbonic acid emulsion and a preparation method. Summary of the Invention

[0005] In order to overcome the above technical problems, the purpose of the present invention is to provide a waterproof redispersible latex powder based on modified versatile carbonic acid emulsion and a preparation method, which solves the problem of poor waterproof performance of existing redispersible latex powder.

[0006] The purpose of the present invention can be achieved through the following technical solutions:

[0007] The waterproof redispersible latex powder based on modified versatile carbonic acid emulsion comprises the following components in parts by weight:

[0008] 80-85 parts of modified versatile carbonic acid emulsion, 6-10 parts of polyvinyl alcohol, 3-7 parts of anti-caking agent and 1-3 parts of defoaming agent;

[0009] Wherein, the modified versatile carbonic acid emulsion is prepared by the following steps:

[0010] Step s1: adding tert-butyl carbonate, 3-butene-1-ol, and stannous octoate to a three-necked flask equipped with a stirrer and a thermometer, stirring the mixture at a temperature of 25-30° C. and a stirring rate of 200-300 r / min for 20-30 minutes, then heating the mixture to 120-130° C. and continuing stirring the mixture for 2-4 hours. After the reaction is completed, the reaction product is cooled to room temperature to obtain a tert-butyl carbonate monomer;

[0011] Step s2: adding versatile carbonic acid monomer, perfluorobutyric acid, 4-dimethylaminopyridine, N,N'-dicyclohexylcarbodiimide and dichloromethane to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, introducing nitrogen protection, stirring and reacting at a temperature of 0-5°C and a stirring rate of 200-300 r / min for 20-30 minutes, then heating to 45-50°C and continuing to stir and react for 6-8 hours. After the reaction is completed, the reaction product is cooled to room temperature, then rotary evaporated to remove the solvent, then added to ethyl acetate, and then vacuum filtered, and the filtrate is rotary evaporated to remove the solvent to obtain a fluorine-containing versatile carbonic acid monomer;

[0012] Step s3: Add fluorinated versatile carbonic acid monomer, methyl methacrylate, butyl acrylate, glycidyl methacrylate, cross-linking modified monomer, composite emulsifier and deionized water into a three-necked flask equipped with a stirrer, a thermometer, an air guide tube and a constant pressure dropping funnel, introduce nitrogen protection, stir and react for 20-30 minutes at a temperature of 25-30°C and a stirring rate of 200-300 r / min, then heat to 80-85°C and continue stirring and reacting for 10-15 minutes, then add ammonium persulfate solution dropwise while stirring, controlling the dropping rate to 1-2 drops / s, and continue stirring and reacting for 2-4 hours after the addition is completed. After the reaction is completed, the reaction product is cooled to room temperature and then passed through a 200-300 mesh sieve to obtain a modified versatile carbonic acid emulsion.

[0013] As a further solution of the present invention: the usage ratio of the tert-butyl carbonate, 3-butene-1-ol and stannous octoate in step s1 is 0.1 mmol: 0.1 mmol: 0.1-0.15 g.

[0014] As a further embodiment of the present invention: the tertiary glycidyl carbonate is tertiary glycidyl carbonate E10P.

[0015] As a further solution of the present invention: the usage ratio of the versatile carbonic acid monomer, perfluorobutyric acid, 4-dimethylaminopyridine, N,N'-dicyclohexylcarbodiimide and dichloromethane in step s2 is 10 mmol: 10 mmol: 0.1-0.12 g: 12-15 mmol: 80-100 mL.

[0016] As a further solution of the present invention: the usage ratio of the fluorinated versatile carbonic acid monomer, methyl methacrylate, butyl acrylate, glycidyl methacrylate, cross-linking modified monomer, composite emulsifier, ammonium persulfate solution and deionized water in step s3 is 10-30g:40-45g:20-25g:2.5-6.5g:3.3-7.5g:2.8-3.6g:10-12g:90-100g.

[0017] As a further solution of the present invention: the cross-linking modification monomer is a polyunsaturated fatty acid.

[0018] As a further embodiment of the present invention: the polyunsaturated fatty acid is one of linoleic acid, α-linolenic acid, and arachidonic acid.

[0019] As a further solution of the present invention: the mass fraction of the ammonium persulfate solution is 2-3%.

[0020] As a further solution of the present invention: the composite emulsifier is a mixture of OP-10 emulsifier and SDS emulsifier in a mass ratio of 1:1-1.5.

[0021] As a further solution of the present invention: a method for preparing a waterproof redispersible latex powder based on a modified versatile carbonic acid emulsion comprises the following steps:

[0022] Step 1: Weigh 80-85 parts of modified versatile carbonic acid emulsion, 6-10 parts of polyvinyl alcohol, 3-7 parts of anti-caking agent and 1-3 parts of defoaming agent according to weight parts and set aside;

[0023] Step 2: Add modified versatile carbonic acid emulsion, polyvinyl alcohol, anti-caking agent and defoaming agent into a stirring tank, stir and mix for 20-30 minutes at a temperature of 70-75°C and a stirring rate of 200-300r / min, and then spray dry in a spray dryer at an inlet temperature of 180-185°C and an outlet temperature of 85-89°C to obtain a waterproof redispersible latex powder.

[0024] As a further embodiment of the present invention: the polyvinyl alcohol is PVA-1788.

[0025] As a further solution of the present invention: the anti-caking agent is white carbon black TH-2000.

[0026] As a further solution of the present invention: the defoamer is BYK-028 water-based defoamer.

[0027] Beneficial effects of the present invention:

[0028] The present invention discloses a waterproof redispersible latex powder based on modified versatate carbonic acid emulsion and a preparation method thereof. The modified versatate carbonic acid emulsion, polyvinyl alcohol, an anti-caking agent and a defoaming agent are added to a stirring kettle, stirred and mixed, and then spray-dried in a spray dryer to obtain the waterproof redispersible latex powder. The waterproof redispersible latex powder uses the modified versatate carbonic acid emulsion as a main raw material and is endowed with good waterproof performance. When added to building materials, the waterproof redispersible latex powder can significantly improve the impermeability and water resistance of the building materials and effectively prevent moisture penetration. The waterproof redispersible latex powder has good adhesion and flexibility, can improve the internal bonding strength of the building materials, and at the same time endows the building materials with a certain impact resistance, can improve the mechanical properties of the building materials, significantly improve the comprehensive performance and service life of the building materials, and meet the demand of modern buildings for high-performance waterproof materials.

[0029] In the process of preparing waterproof redispersible latex powder, a modified versatate carbonic acid emulsion is first prepared. First, versatate carbonic acid glycidyl ester and 3-butene-1-ol are reacted, and the epoxy group on versatate carbonic acid glycidyl ester undergoes a ring-opening reaction with the hydroxyl group on 3-butene-1-ol, and an alkenyl group is introduced and a hydroxyl group is re-formed to obtain a versatate carbonic acid monomer. Then, the versatate carbonic acid monomer and perfluorobutyric acid are reacted, and the hydroxyl group on the versatate carbonic acid monomer undergoes an esterification reaction with the carboxyl group on the perfluorobutyric acid, and a fluorine atom is introduced to obtain a fluorine-containing versatate carbonic acid monomer. Finally, the fluorine-containing versatate carbonic acid monomer, methyl methacrylate, butyl acrylate, glycidyl methacrylate, and a cross-linking modified monomer are used as polymerization monomers to form a polymer to obtain a modified versatate carbonic acid emulsion. The polymer molecular chain in the modified versatate carbonic acid emulsion contains a versatate carbonic acid structure, and the shield effect brought about by the large steric hindrance of the versatate carbonic acid structure can make the ester group on the polymer side chain and other groups on the polymer main chain not easily hydrolyzed, and has good The flexibility of the cross-linking monomer gives the polymer good anti-cracking properties. The introduced fluorine atoms can reduce the surface energy of the polymer and effectively prevent the adsorption and penetration of water molecules, thereby forming a dense waterproof layer, which has excellent hydrophobic and waterproof properties. Among them, the epoxy group provided by glycidyl methacrylate can not only chemically react with the components in the building materials to connect, thereby improving the tightness of the internal structure of the building materials and improving their mechanical strength, but also react with the carboxyl group provided by the cross-linking modified monomer to achieve self-cross-linking effect. Moreover, the cross-linking modified monomer provides multiple olefinic groups, which can further enhance the cross-linking effect and form a dense polymer network structure, thereby enhancing the density of the film formed by the waterproof redispersible latex powder and enhancing its water resistance and waterproofness. Therefore, after the waterproof redispersible latex powder is added to the building material, a stable and dense waterproof film can be formed on its surface, which effectively prevents moisture penetration and thus improves the comprehensive performance of the building material. 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 embodiments described 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 making any creative efforts shall fall within the scope of protection of the present invention.

[0031] Example 1: This example is a method for preparing a waterproof redispersible latex powder based on a modified versatile carbonic acid emulsion, comprising the following steps:

[0032] Step S1: 0.1 mmol of versatate glycidyl carbonate E10P, 0.1 mmol of 3-butene-1-ol, and 0.1 g of stannous octoate were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at 25° C. and a stirring rate of 200 r / min for 20 minutes, then heated to 120° C. and continued to stir for 2 hours. After the reaction was completed, the reaction product was cooled to room temperature to obtain versatate carbonic acid monomer;

[0033] Step S2: 10 mmol of versatile carbonic acid monomer, 10 mmol of perfluorobutyric acid, 0.1 g of 4-dimethylaminopyridine, 12 mmol of N,N'-dicyclohexylcarbodiimide and 80 mL of dichloromethane were added to a three-necked flask equipped with a stirrer, a thermometer and a gas guide tube, and nitrogen was introduced for protection. The mixture was stirred at 0°C and a stirring rate of 200 r / min for 20 minutes, and then the temperature was raised to 45°C and the stirring reaction was continued for 6 hours. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation. The product was then added to ethyl acetate, and then vacuum filtered. The filtrate was rotary evaporated to remove the solvent to obtain a fluorine-containing versatile carbonic acid monomer;

[0034] Step S3: 10 g of fluorinated versatile carbonic acid monomer, 40 g of methyl methacrylate, 20 g of butyl acrylate, 2.5 g of glycidyl methacrylate, 3.3 g of cross-linking modified monomer, 2.8 g of composite emulsifier and 90 g of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer, an air guide tube and a constant pressure dropping funnel, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 25 ° C and a stirring rate of 200 r / min for 20 minutes, and then the mixture was heated to 80 ° C and continued to stir and react. The mixture was stirred for 10 minutes, and then 10 g of ammonium persulfate solution was added dropwise while stirring at a rate of 1 drop / s. After the addition was completed, the stirring reaction was continued for 2 hours. After the reaction was completed, the reaction product was cooled to room temperature and then passed through a 200-mesh sieve to obtain a modified versatile carbonic acid emulsion; the cross-linking modification monomer was a polyunsaturated fatty acid; the polyunsaturated fatty acid was linoleic acid; the mass fraction of the ammonium persulfate solution was 2%; and the composite emulsifier was a mixture of OP-10 emulsifier and SDS emulsifier in a mass ratio of 1:1;

[0035] Step S4: 80 parts of modified versatile carbonic acid emulsion, 6 parts of polyvinyl alcohol, 3 parts of anti-caking agent and 1 part of defoaming agent are weighed and set aside according to weight; the polyvinyl alcohol is PVA-1788; the anti-caking agent is white carbon black TH-2000; and the defoaming agent is BYK-028 water-based defoaming agent;

[0036] Step S5: Add modified versatile carbonic acid emulsion, polyvinyl alcohol, anti-caking agent and defoaming agent to a stirring tank, stir and mix for 20 minutes at a temperature of 70°C and a stirring rate of 200 r / min, and then spray dry in a spray dryer at an inlet temperature of 180°C and an outlet temperature of 85°C to obtain a waterproof redispersible latex powder.

[0037] Example 2: This example is a method for preparing a waterproof redispersible latex powder based on a modified versatile carbonic acid emulsion, comprising the following steps:

[0038] Step S1: 0.1 mmol of versatate glycidyl carbonate E10P, 0.1 mmol of 3-butene-1-ol, and 0.12 g of stannous octoate were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at 28° C. and a stirring rate of 250 r / min for 25 minutes. The mixture was then heated to 125° C. and stirred for 3 hours. After the reaction was completed, the reaction product was cooled to room temperature to obtain a versatate carbonic acid monomer.

[0039] Step S2: 10 mmol of versatile carbonic acid monomer, 10 mmol of perfluorobutyric acid, 0.11 g of 4-dimethylaminopyridine, 14 mmol of N,N'-dicyclohexylcarbodiimide and 90 mL of dichloromethane were added to a three-necked flask equipped with a stirrer, a thermometer and a gas guide tube, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 3°C and a stirring rate of 250 r / min for 25 minutes, and then the temperature was raised to 48°C and the stirring reaction was continued for 7 hours. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation. The product was then added to ethyl acetate, and then vacuum filtered. The filtrate was rotary evaporated to remove the solvent to obtain a fluorine-containing versatile carbonic acid monomer;

[0040] Step S3: 20 g of fluorinated versatile carbonic acid monomer, 42 g of methyl methacrylate, 22 g of butyl acrylate, 4.5 g of glycidyl methacrylate, 5.4 g of cross-linking modified monomer, 3.2 g of composite emulsifier and 95 g of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer, an air guide tube and a constant pressure dropping funnel, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 28 ° C and a stirring rate of 250 r / min for 25 min, and then the mixture was heated to 82 ° C and stirred for 12 min. min, then add 11 g of ammonium persulfate solution dropwise while stirring, controlling the drop rate to 1 drop / s, continue stirring and reacting for 3 hours after the dropwise addition is completed, and cool the reaction product to room temperature after the reaction is completed, and then pass it through a 250-mesh sieve to obtain a modified versatile carbonic acid emulsion; the cross-linking modification monomer is a polyunsaturated fatty acid; the polyunsaturated fatty acid is α-linolenic acid; the mass fraction of the ammonium persulfate solution is 2.5%; and the composite emulsifier is a mixture of OP-10 emulsifier and SDS emulsifier in a mass ratio of 1:1.2;

[0041] Step S4: 82 parts of modified versatile carbonic acid emulsion, 8 parts of polyvinyl alcohol, 5 parts of anti-caking agent, and 2 parts of defoaming agent are weighed in parts by weight and set aside; the polyvinyl alcohol is PVA-1788; the anti-caking agent is white carbon black TH-2000; and the defoaming agent is BYK-028 water-based defoaming agent;

[0042] Step S5: Add modified versatile carbonic acid emulsion, polyvinyl alcohol, anti-caking agent and defoaming agent to a stirring tank, stir and mix for 25 minutes at a temperature of 72°C and a stirring rate of 250r / min, and then spray dry in a spray dryer at an inlet temperature of 182°C and an outlet temperature of 87°C to obtain a waterproof redispersible latex powder.

[0043] Example 3: This example is a method for preparing a waterproof redispersible latex powder based on a modified versatile carbonic acid emulsion, comprising the following steps:

[0044] Step S1: 0.1 mmol of versatate glycidyl carbonate E10P, 0.1 mmol of 3-butene-1-ol, and 0.15 g of stannous octoate were added to a three-necked flask equipped with a stirrer and a thermometer, and the mixture was stirred at 30° C. and a stirring rate of 300 r / min for 30 minutes. The mixture was then heated to 130° C. and stirred for 4 hours. After the reaction was completed, the reaction product was cooled to room temperature to obtain a versatate carbonic acid monomer.

[0045] Step S2: 10 mmol of versatile carbonic acid monomer, 10 mmol of perfluorobutyric acid, 0.12 g of 4-dimethylaminopyridine, 15 mmol of N,N'-dicyclohexylcarbodiimide and 100 mL of dichloromethane were added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 5°C and a stirring rate of 300 r / min for 30 minutes, and then the temperature was raised to 50°C and the stirring reaction was continued for 8 hours. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation. The product was then added to ethyl acetate, and then vacuum filtered. The filtrate was rotary evaporated to remove the solvent to obtain a fluorine-containing versatile carbonic acid monomer;

[0046] Step S3: 30 g of fluorinated versatile carbonic acid monomer, 45 g of methyl methacrylate, 25 g of butyl acrylate, 6.5 g of glycidyl methacrylate, 7.5 g of cross-linking modified monomer, 3.6 g of composite emulsifier and 100 g of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer, an air guide tube and a constant pressure dropping funnel, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 30 ° C and a stirring rate of 300 r / min for 30 min, and then the temperature was raised to 85 ° C and the stirring reaction was continued for 1 min. 5 minutes, then 12g of ammonium persulfate solution was added dropwise while stirring, and the drop rate was controlled to be 2 drops / s. After the dropwise addition was completed, the stirring reaction was continued for 4 hours. After the reaction was completed, the reaction product was cooled to room temperature and then passed through a 300-mesh sieve to obtain a modified versatile carbonic acid emulsion; the cross-linking modification monomer was a polyunsaturated fatty acid; the polyunsaturated fatty acid was arachidonic acid; the mass fraction of the ammonium persulfate solution was 3%; and the composite emulsifier was a mixture of OP-10 emulsifier and SDS emulsifier in a mass ratio of 1:1.5;

[0047] Step S4: 85 parts of modified versatile carbonic acid emulsion, 10 parts of polyvinyl alcohol, 7 parts of anti-caking agent, and 3 parts of defoaming agent are weighed and set aside according to weight; the polyvinyl alcohol is PVA-1788; the anti-caking agent is white carbon black TH-2000; and the defoaming agent is BYK-028 water-based defoaming agent;

[0048] Step S5: Add modified versatile carbonic acid emulsion, polyvinyl alcohol, anti-caking agent and defoaming agent to a stirring tank, stir and mix for 30 minutes at a temperature of 75°C and a stirring rate of 300 r / min, and then spray dry in a spray dryer at an inlet temperature of 185°C and an outlet temperature of 89°C to obtain a waterproof redispersible latex powder.

[0049] Comparative Example 1:

[0050] This comparative example is a method for preparing a waterproof redispersible latex powder based on a modified versatile carbonic acid emulsion, comprising the following steps:

[0051] Step S1: 45g of methyl methacrylate, 25g of butyl acrylate, 3.6g of a composite emulsifier and 100g of deionized water are added to a three-necked flask equipped with a stirrer, a thermometer, an air guide tube and a constant pressure dropping funnel, and nitrogen protection is introduced. The mixture is stirred and reacted for 30 minutes at a temperature of 30°C and a stirring rate of 300r / min. The mixture is then heated to 85°C and stirred for 15 minutes. 12g of ammonium persulfate solution is then added dropwise while stirring, and the dropping rate is controlled to 2 drops / s. After the addition is completed, the stirring reaction is continued for 4 hours. After the reaction is completed, the reaction product is cooled to room temperature and then passed through a 300-mesh sieve to obtain an acrylate emulsion; the mass fraction of the ammonium persulfate solution is 3%; the composite emulsifier is a mixture of OP-10 emulsifier and SDS emulsifier in a mass ratio of 1:1.5;

[0052] Step S2: 85 parts of acrylic emulsion, 10 parts of polyvinyl alcohol, 7 parts of anti-caking agent, and 3 parts of defoaming agent are weighed and set aside according to weight; the polyvinyl alcohol is PVA-1788; the anti-caking agent is white carbon black TH-2000; and the defoaming agent is BYK-028 water-based defoaming agent;

[0053] Step S3: Add acrylic emulsion, polyvinyl alcohol, anti-caking agent and defoaming agent to a stirring tank, stir and mix for 30 minutes at a temperature of 75°C and a stirring rate of 300 r / min, and then spray dry in a spray dryer at an inlet temperature of 185°C and an outlet temperature of 89°C to obtain a waterproof redispersible latex powder.

[0054] Comparative Example 2:

[0055] This comparative example is a method for preparing a waterproof redispersible latex powder based on a modified versatile carbonic acid emulsion, comprising the following steps:

[0056] Step S1: 0.1 mmol of versatate glycidyl carbonate E10P, 0.1 mmol of 3-butene-1-ol, and 0.15 g of stannous octoate were added to a three-necked flask equipped with a stirrer and a thermometer, and the mixture was stirred at 30° C. and a stirring rate of 300 r / min for 30 minutes. The mixture was then heated to 130° C. and stirred for 4 hours. After the reaction was completed, the reaction product was cooled to room temperature to obtain a versatate carbonic acid monomer.

[0057] Step S2: 30g of versatile carbonic acid monomer, 45g of methyl methacrylate, 25g of butyl acrylate, 3.6g of composite emulsifier and 100g of deionized water are added to a three-necked flask equipped with a stirrer, a thermometer, an air guide tube and a constant pressure dropping funnel, and nitrogen protection is introduced. The mixture is stirred and reacted for 30min at a temperature of 30°C and a stirring rate of 300r / min. After that, the mixture is heated to 85°C and the stirring reaction is continued for 15min. Then, 12g of ammonium persulfate solution is added dropwise while stirring, and the dropping rate is controlled to 2 drops / s. After the dropwise addition is completed, the stirring reaction is continued for 4h. After the reaction is completed, the reaction product is cooled to room temperature and then passed through a 300-mesh sieve to obtain a versatile carbonic acid emulsion; the mass fraction of the ammonium persulfate solution is 3%; the composite emulsifier is a mixture of OP-10 emulsifier and SDS emulsifier in a mass ratio of 1:1.5;

[0058] Step S3: 85 parts of versatile carbonic acid emulsion, 10 parts of polyvinyl alcohol, 7 parts of anti-caking agent and 3 parts of defoaming agent are weighed and set aside according to weight; the polyvinyl alcohol is PVA-1788; the anti-caking agent is white carbon black TH-2000; and the defoaming agent is BYK-028 water-based defoaming agent;

[0059] Step S4: Add versatile carbonic acid emulsion, polyvinyl alcohol, anti-caking agent and defoaming agent to a stirring tank, stir and mix for 30 minutes at a temperature of 75°C and a stirring rate of 300 r / min, and then spray dry in a spray dryer at an inlet temperature of 185°C and an outlet temperature of 89°C to obtain a waterproof redispersible latex powder.

[0060] Comparative Example 3:

[0061] This comparative example is a method for preparing a waterproof redispersible latex powder based on a modified versatile carbonic acid emulsion, comprising the following steps:

[0062] Step S1: 0.1 mmol of versatate glycidyl carbonate E10P, 0.1 mmol of 3-butene-1-ol, and 0.15 g of stannous octoate were added to a three-necked flask equipped with a stirrer and a thermometer, and the mixture was stirred at 30° C. and a stirring rate of 300 r / min for 30 minutes. The mixture was then heated to 130° C. and stirred for 4 hours. After the reaction was completed, the reaction product was cooled to room temperature to obtain a versatate carbonic acid monomer.

[0063] Step S2: 10 mmol of versatile carbonic acid monomer, 10 mmol of perfluorobutyric acid, 0.12 g of 4-dimethylaminopyridine, 15 mmol of N,N'-dicyclohexylcarbodiimide and 100 mL of dichloromethane were added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 5°C and a stirring rate of 300 r / min for 30 minutes, and then the temperature was raised to 50°C and the stirring reaction was continued for 8 hours. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation. The product was then added to ethyl acetate, and then vacuum filtered. The filtrate was rotary evaporated to remove the solvent to obtain a fluorine-containing versatile carbonic acid monomer;

[0064] Step S3: 30g of fluorinated versatile carbonic acid monomer, 45g of methyl methacrylate, 25g of butyl acrylate, 3.6g of composite emulsifier and 100g of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer, an air guide tube and a constant pressure dropping funnel, and nitrogen was introduced for protection. The mixture was stirred and reacted for 30min at a temperature of 30°C and a stirring rate of 300r / min. The mixture was then heated to 85°C and stirred for 15min. Then, 12g of ammonium persulfate solution was added dropwise while stirring, and the dropping rate was controlled to 2 drops / s. After the addition was completed, the stirring reaction was continued for 4h. After the reaction was completed, the reaction product was cooled to room temperature and then passed through a 300-mesh sieve to obtain a modified versatile carbonic acid emulsion; the mass fraction of the ammonium persulfate solution was 3%; the composite emulsifier was a mixture of OP-10 emulsifier and SDS emulsifier in a mass ratio of 1:1.5;

[0065] Step S4: 85 parts of modified versatile carbonic acid emulsion, 10 parts of polyvinyl alcohol, 7 parts of anti-caking agent, and 3 parts of defoaming agent are weighed and set aside according to weight; the polyvinyl alcohol is PVA-1788; the anti-caking agent is white carbon black TH-2000; and the defoaming agent is BYK-028 water-based defoaming agent;

[0066] Step S5: Add modified versatile carbonic acid emulsion, polyvinyl alcohol, anti-caking agent and defoaming agent to a stirring tank, stir and mix for 30 minutes at a temperature of 75°C and a stirring rate of 300 r / min, and then spray dry in a spray dryer at an inlet temperature of 185°C and an outlet temperature of 89°C to obtain a waterproof redispersible latex powder.

[0067] Comparative Example 4:

[0068] This comparative example is a method for preparing a waterproof redispersible latex powder based on a modified versatile carbonic acid emulsion, comprising the following steps:

[0069] Step S1: 0.1 mmol of versatate glycidyl carbonate E10P, 0.1 mmol of 3-butene-1-ol, and 0.15 g of stannous octoate were added to a three-necked flask equipped with a stirrer and a thermometer, and the mixture was stirred at 30° C. and a stirring rate of 300 r / min for 30 minutes. The mixture was then heated to 130° C. and stirred for 4 hours. After the reaction was completed, the reaction product was cooled to room temperature to obtain a versatate carbonic acid monomer.

[0070] Step S2: 10 mmol of versatile carbonic acid monomer, 10 mmol of perfluorobutyric acid, 0.12 g of 4-dimethylaminopyridine, 15 mmol of N,N'-dicyclohexylcarbodiimide and 100 mL of dichloromethane were added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 5°C and a stirring rate of 300 r / min for 30 minutes, and then the temperature was raised to 50°C and the stirring reaction was continued for 8 hours. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation. The product was then added to ethyl acetate, and then vacuum filtered. The filtrate was rotary evaporated to remove the solvent to obtain a fluorine-containing versatile carbonic acid monomer;

[0071] Step S3: 30g of fluorinated versatile carbonic acid monomer, 45g of methyl methacrylate, 25g of butyl acrylate, 6.5g of glycidyl methacrylate, 3.6g of composite emulsifier and 100g of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer, an air guide tube and a constant pressure dropping funnel, and nitrogen was introduced for protection. The mixture was stirred and reacted for 30min at a temperature of 30°C and a stirring rate of 300r / min. The mixture was then heated to 85°C and stirred for 15min. Then, 12g of ammonium persulfate solution was added dropwise while stirring, and the dropping rate was controlled to 2 drops / s. After the addition was completed, the stirring reaction was continued for 4h. After the reaction was completed, the reaction product was cooled to room temperature and then passed through a 300-mesh sieve to obtain a modified versatile carbonic acid emulsion; the mass fraction of the ammonium persulfate solution was 3%; and the composite emulsifier was a mixture of OP-10 emulsifier and SDS emulsifier in a mass ratio of 1:1.5;

[0072] Step S4: 85 parts of modified versatile carbonic acid emulsion, 10 parts of polyvinyl alcohol, 7 parts of anti-caking agent, and 3 parts of defoaming agent are weighed and set aside according to weight; the polyvinyl alcohol is PVA-1788; the anti-caking agent is white carbon black TH-2000; and the defoaming agent is BYK-028 water-based defoaming agent;

[0073] Step S5: Add modified versatile carbonic acid emulsion, polyvinyl alcohol, anti-caking agent and defoaming agent to a stirring tank, stir and mix for 30 minutes at a temperature of 75°C and a stirring rate of 300 r / min, and then spray dry in a spray dryer at an inlet temperature of 185°C and an outlet temperature of 89°C to obtain a waterproof redispersible latex powder.

[0074] Comparative Example 5:

[0075] This comparative example is a method for preparing a waterproof redispersible latex powder based on a modified versatile carbonic acid emulsion, comprising the following steps:

[0076] Step S1: 0.1 mmol of versatate glycidyl carbonate E10P, 0.1 mmol of 3-butene-1-ol, and 0.15 g of stannous octoate were added to a three-necked flask equipped with a stirrer and a thermometer, and the mixture was stirred at 30° C. and a stirring rate of 300 r / min for 30 minutes. The mixture was then heated to 130° C. and stirred for 4 hours. After the reaction was completed, the reaction product was cooled to room temperature to obtain a versatate carbonic acid monomer.

[0077] Step S2: 30 g of versatile carbonic acid monomer, 45 g of methyl methacrylate, 25 g of butyl acrylate, 6.5 g of glycidyl methacrylate, 7.5 g of cross-linking modified monomer, 3.6 g of composite emulsifier and 100 g of deionized water were added to a three-necked flask equipped with a stirrer, a thermometer, an air guide tube and a constant pressure dropping funnel, and nitrogen was introduced for protection. The mixture was stirred at a temperature of 30 ° C and a stirring rate of 300 r / min for 30 min, and then the temperature was raised to 85 ° C and the stirring reaction was continued for 15 min. min, then add 12 g of ammonium persulfate solution dropwise while stirring, controlling the drop rate to 2 drops / s, continue stirring and reacting for 4 hours after the dropwise addition is completed, and cool the reaction product to room temperature after the reaction is completed, and then pass it through a 300-mesh sieve to obtain a modified versatile carbonic acid emulsion; the cross-linking modification monomer is a polyunsaturated fatty acid; the polyunsaturated fatty acid is arachidonic acid; the mass fraction of the ammonium persulfate solution is 3%; the composite emulsifier is a mixture of OP-10 emulsifier and SDS emulsifier in a mass ratio of 1:1.5;

[0078] Step S3: 85 parts of modified versatile carbonic acid emulsion, 10 parts of polyvinyl alcohol, 7 parts of anti-caking agent, and 3 parts of defoaming agent are weighed and set aside according to weight; the polyvinyl alcohol is PVA-1788; the anti-caking agent is white carbon black TH-2000; and the defoaming agent is BYK-028 water-based defoaming agent;

[0079] Step S4: Add modified versatile carbonic acid emulsion, polyvinyl alcohol, anti-caking agent and defoaming agent to a stirring tank, stir and mix for 30 minutes at a temperature of 75°C and a stirring rate of 300 r / min, and then spray dry in a spray dryer at an inlet temperature of 185°C and an outlet temperature of 89°C to obtain a waterproof redispersible latex powder.

[0080] The waterproof redispersible latex powders from Examples 1-3 and Comparative Examples 1-5 were added to the permeable mortar at a ratio of 2 wt %, and the performance of the permeable mortar was tested. The test results are shown in the following table:

[0081] .

[0082] Referring to the data in the above table, based on the comparison between Examples 1-3, Comparative Examples 1-5 and the blank example, it can be seen that adding the waterproof redispersible latex powder of the present application can greatly improve the mechanical properties and waterproof properties of the permeable mortar.

[0083] Among them, the blank example is a permeable mortar without the addition of waterproof redispersible latex powder.

[0084] The permeable mortar is made by mixing cement, fine aggregate, water and water reducing agent in a mass ratio of 365:1600:110:7. The cement is Jidong Cement P·O 42.5 ordinary Portland cement; the fine aggregate is river sand with a particle size of 1-3 mm; and the water reducing agent is PC-1006 polycarboxylate water reducing agent.

[0085] Among them, the 7d compressive strength is tested in accordance with JGJ / T 70-2009 "Standard for Test Methods for Basic Properties of Building Mortar"; the 7d flexural strength is tested in accordance with GB / T 17671-2021 "Test Method for Strength of Cement Mortar (ISO Method)"; and the 48h water absorption is tested in accordance with JC 474-2008 "Mortar and Concrete Waterproofing Agent".

[0086] Throughout this specification, references to terms such as "one embodiment," "example," or "specific example" indicate that the specific features, structures, materials, or characteristics described in conjunction with that embodiment or example are included in at least one embodiment or example of the present invention. In this specification, schematic representations of these terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.

[0087] 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 described specific embodiments or replace them in similar ways. As long as they do not deviate from the invention or exceed the scope defined in this application, they should all fall within the scope of protection of the present invention.

Claims

1. A waterproof redispersible latex powder based on modified versatile carbonic acid emulsion, characterized in that: It comprises the following components in parts by weight: 80-85 parts of modified versatile carbonic acid emulsion, 6-10 parts of polyvinyl alcohol, 3-7 parts of anti-caking agent and 1-3 parts of defoaming agent; Wherein, the modified versatile carbonic acid emulsion is prepared by the following steps: Step s1: stirring and reacting versatile glycidyl carbonate, 3-butene-1-ol, and stannous octoate, and cooling the reaction product after the reaction to obtain versatile carbonic acid monomer; the amount ratio of versatile glycidyl carbonate, 3-butene-1-ol, and stannous octoate is 0.1 mmol:0.1 mmol:0.1-0.15 g; the versatile glycidyl carbonate is versatile glycidyl carbonate E10P; Step s2: stirring a versatile carbonic acid monomer, perfluorobutyric acid, 4-dimethylaminopyridine, N,N'-dicyclohexylcarbodiimide, and dichloromethane to react. After the reaction, the reaction product is cooled, rotary evaporated, and then added to ethyl acetate. The product is then vacuum filtered and the filtrate is rotary evaporated to obtain a fluorine-containing versatile carbonic acid monomer. The amount ratio of the versatile carbonic acid monomer, perfluorobutyric acid, 4-dimethylaminopyridine, N,N'-dicyclohexylcarbodiimide, and dichloromethane is 10 mmol: 10 mmol: 0.1-0.12 g: 12-15 mmol: 80-100 mL. Step s3: stirring a fluorinated versatile carbonic acid monomer, methyl methacrylate, butyl acrylate, glycidyl methacrylate, a cross-linking modified monomer, a composite emulsifier and deionized water for reaction, then adding an ammonium persulfate solution dropwise while stirring, continuing to stir and react after the addition is complete, cooling the reaction product after the reaction is complete, and then sieving to obtain a modified versatile carbonic acid emulsion; the amount ratio of the fluorinated versatile carbonic acid monomer, methyl methacrylate, butyl acrylate, glycidyl methacrylate, cross-linking modified monomer, composite emulsifier, ammonium persulfate solution and deionized water is 10-30g:40-45g:20-25g:2.5-6.5g:3.3-7.5g:2.8-3.6g:10-12g:90-100g; the cross-linking modified monomer is a polyunsaturated fatty acid; the polyunsaturated fatty acid is one of linoleic acid, α-linolenic acid and arachidonic acid.

2. The waterproof redispersible latex powder based on modified versatile carbonic acid emulsion according to claim 1, characterized in that: The mass fraction of the ammonium persulfate solution is 2-3%.

3. The waterproof redispersible latex powder based on modified versatile carbonic acid emulsion according to claim 1, characterized in that: The composite emulsifier is a mixture of OP-10 emulsifier and SDS emulsifier in a mass ratio of 1:1-1.

5.

4. The method for preparing a waterproof redispersible latex powder based on a modified versatile carbonic acid emulsion according to any one of claims 1 to 3, characterized in that: The following steps are involved: Step 1: Weigh 80-85 parts of modified versatile carbonic acid emulsion, 6-10 parts of polyvinyl alcohol, 3-7 parts of anti-caking agent and 1-3 parts of defoaming agent according to weight parts and set aside; Step 2: Add modified versatile carbonic acid emulsion, polyvinyl alcohol, anti-caking agent and defoaming agent into a stirring tank, stir and mix for 20-30 minutes at a temperature of 70-75°C and a stirring rate of 200-300r / min, and then spray dry in a spray dryer at an inlet temperature of 180-185°C and an outlet temperature of 85-89°C to obtain a waterproof redispersible latex powder.

5. The method for preparing a waterproof redispersible latex powder based on a modified versatile carbonic acid emulsion according to claim 4, characterized in that: The polyvinyl alcohol is PVA-1788; the anti-caking agent is white carbon black TH-2000; and the defoaming agent is BYK-028 water-based defoaming agent.