Waterproof redispersible latex powder based on modified tertiary carboxylic acid emulsion and preparation method thereof
Through the waterproof redispersible latex powder based on modified tertiary carbonic acid emulsion, the lack of performance of traditional latex powder under high waterproof requirements is solved, and the significant impermeability and water resistance of building materials are improved.
Patent Information
- Application Number
- CN202510596354.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-05-09
- Publication Date
- 2025-06-06
- Estimated Expiration
- 2045-05-09
AI Technical Summary
The existing redispersible latex powder still needs to be improved in waterproof performance, especially in construction projects with humid environments or high waterproof requirements, the modified building materials of traditional latex powder are prone to problems such as water seepage and powdering.
Waterproof redispersible latex powder based on modified tertiary carbonic acid emulsion is used to prepare waterproof latex powder by spray drying by a combination of modified tertiary carbonic acid emulsion, polyvinyl alcohol, anti-caking agent and defoaming agent.
It significantly improves the permeability and water resistance of building materials, prevents moisture penetration, and improves adhesion, flexibility and mechanical properties, extending the service life of building materials.
Abstract
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 latex powder is a polymer powder prepared by spray drying of emulsion. The product has good fluidity, dispersibility and storage stability. Redispersible latex powder can be dispersed in water to regenerate a stable polymer emulsion with similar properties to the original emulsion. Using redispersible latex powder as a modifier for building materials can significantly improve the adhesion, flexibility, mechanical strength and other properties of building materials.
[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: The waterproof redispersible latex powder based on modified versatile carbonic acid emulsion 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: adding tert-butyl carbonate, 3-butene-1-ol and stannous octoate into a three-necked flask equipped with a stirrer and a thermometer, stirring the mixture for 20-30 min at a temperature of 25-30° C. and a stirring rate of 200-300 r / min, then heating the mixture to 120-130° C. and continuing to stir the mixture for 2-4 h. After the reaction is completed, the reaction product is cooled to room temperature to obtain a tert-butyl carbonate monomer; Step s2: adding tert-butyl carbonate monomer, perfluorobutyric acid, 4-dimethylaminopyridine, N,N'-dicyclohexylcarbodiimide and dichloromethane to a three-necked flask equipped with a stirrer, a thermometer and an air duct, introducing nitrogen protection, stirring the reaction at a temperature of 0-5°C and a stirring rate of 200-300 r / min for 20-30 min, then heating to 45-50°C and continuing to stir the reaction for 6-8 h, after the reaction is completed, cooling the reaction product to room temperature, then rotary evaporating to remove the solvent, then adding it to ethyl acetate, then vacuum filtering, rotary evaporating the filtrate to remove the solvent, and obtaining a fluorine-containing tert-butyl carbonate monomer; 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 200-300r / min, then heat to 80-85°C and continue to stir and react for 10-15 minutes, then add ammonium persulfate solution dropwise while stirring, control the dropping rate to 1-2 drops / s, continue to stir and react for 2-4 hours after the dropwise addition is completed, and after the reaction is completed, cool the reaction product to room temperature, and then pass through a 200-300 mesh sieve to obtain a modified versatile carbonic acid emulsion.
[0007] 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.
[0008] As a further embodiment of the present invention: the tert-butyl glycidyl carbonate is tert-butyl glycidyl carbonate E10P.
[0009] As a further solution of the present invention: the usage ratio of the tert-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.
[0010] As a further scheme 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.
[0011] As a further solution of the present invention: the cross-linking modification monomer is a polyunsaturated fatty acid.
[0012] As a further embodiment of the present invention: the polyunsaturated fatty acid is one of linoleic acid, α-linolenic acid and arachidonic acid.
[0013] As a further solution of the present invention: the mass fraction of the ammonium persulfate solution is 2-3%.
[0014] 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.
[0015] 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: 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 kettle, 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.
[0016] As a further solution of the present invention: the polyvinyl alcohol is PVA-1788.
[0017] As a further solution of the present invention: the anti-caking agent is white carbon black TH-2000.
[0018] As a further solution of the present invention: the defoamer is BYK-028 aqueous defoamer.
[0019] Beneficial effects of the present invention: The invention discloses a waterproof redispersible latex powder based on modified versatate carbonate emulsion and a preparation method thereof. The modified versatate carbonate emulsion, polyvinyl alcohol, an anti-caking agent and a defoaming agent are added into 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 carbonate emulsion as a main raw material, and is endowed with good waterproof performance. When the modified versatate carbonate emulsion is added into building materials, the impermeability and water resistance of the building materials can be significantly improved, and water penetration can be effectively prevented. The waterproof redispersible latex powder has good adhesion and flexibility, and can improve the internal bonding strength of the building materials. At the same time, the building materials are endowed with a certain impact resistance, and the mechanical properties of the building materials can be improved, and the comprehensive performance and service life of the building materials can be significantly improved, and the demand of modern buildings for high-performance waterproof materials can be met.
[0020] In the process of preparing waterproof redispersible latex powder, a modified versatile carbonic acid emulsion is first prepared. First, versatile carbonic acid glycidyl ester and 3-butene-1-ol are reacted, and the epoxy group on versatile carbonic acid glycidyl ester and the hydroxyl group on 3-butene-1-ol undergo a ring-opening reaction, and an olefin group is introduced and a hydroxyl group is re-formed to obtain a versatile carbonic acid monomer. Then, the versatile carbonic acid monomer and perfluorobutyric acid are reacted, and the hydroxyl group on the versatile carbonic acid monomer and the carboxyl group on the perfluorobutyric acid undergo an esterification reaction, and a fluorine atom is introduced to obtain a fluorine-containing versatile carbonic acid monomer. Finally, the fluorine-containing versatile 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 versatile carbonic acid emulsion. The polymer molecular chain in the modified versatile carbonic acid emulsion contains a versatile carbonic acid structure, and the shield effect brought by the large steric hindrance of the versatile carbonic acid structure can make the ester group on the polymer side chain and other groups on the polymer main chain not easy to hydrolyze, 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 a 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, thereby 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 water penetration and thereby improves the comprehensive performance of the building material. DETAILED DESCRIPTION
[0021] 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.
[0022] Embodiment 1, this embodiment is a method for preparing a waterproof redispersible latex powder based on modified versatile carbonic acid emulsion, comprising the following steps: Step S1: 0.1 mmol tert-butyl carbonate E10P, 0.1 mmol 3-butene-1-ol and 0.1 g stannous octoate are added to a three-necked flask equipped with a stirrer and a thermometer, and stirred for reaction at a temperature of 25° C. and a stirring rate of 200 r / min for 20 min, and then the temperature is raised to 120° C. and the stirring reaction is continued for 2 h. After the reaction is completed, the reaction product is cooled to room temperature to obtain a tert-butyl carbonate monomer; Step S2: 10 mmol tert-carbonic acid monomer, 10 mmol perfluorobutyric acid, 0.1 g 4-dimethylaminopyridine, 12 mmol N, N'-dicyclohexylcarbodiimide and 80 mL dichloromethane are added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen is introduced for protection. The mixture is stirred for reaction at a temperature of 0° C. and a stirring rate of 200 r / min for 20 min, and then the mixture is heated to 45° C. and stirred for reaction for 6 h. After the reaction is completed, the reaction product is cooled to room temperature, and then the solvent is removed by rotary evaporation, and then the mixture is added to ethyl acetate, and then vacuum filtered, and the filtrate is rotary evaporated to remove the solvent to obtain a fluorine-containing tert-carbonic acid monomer; Step S3: 10 g of fluorinated tert-butyl carbonate monomer, 40 g of methyl methacrylate, 20 g of butyl acrylate, 2.5 g of glycidyl methacrylate, 3.3 g of cross-linked 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 min, and then the mixture was heated to 80° C. and stirred for 20 min. The mixture was stirred for 10 minutes, and then 10 g of ammonium persulfate solution was added dropwise while stirring, and the drop rate was controlled to be 1 drop / s. After the dropwise 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 modified monomer was a polyunsaturated fatty acid; the polyunsaturated fatty acid was linoleic acid; the mass fraction of the ammonium persulfate solution was 2%; the composite emulsifier was a mixture of OP-10 emulsifier and SDS emulsifier in a mass ratio of 1:1; 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 according to weight parts for standby use; the polyvinyl alcohol is PVA-1788; the anti-caking agent is white carbon black TH-2000; the defoaming agent is BYK-028 water-based defoaming agent; Step S5: Add modified versatile carbonic acid emulsion, polyvinyl alcohol, anti-caking agent and defoaming agent into 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.
[0023] Embodiment 2: This embodiment is a method for preparing a waterproof redispersible latex powder based on a modified versatile carbonic acid emulsion, comprising the following steps: Step S1: 0.1 mmol tert-butyl carbonate E10P, 0.1 mmol 3-butene-1-ol and 0.12 g stannous octoate are added to a three-necked flask equipped with a stirrer and a thermometer, and stirred for reaction at a temperature of 28° C. and a stirring rate of 250 r / min for 25 min, and then the temperature is raised to 125° C. and the stirring reaction is continued for 3 h. After the reaction is completed, the reaction product is cooled to room temperature to obtain a tert-butyl carbonate monomer; Step S2: 10 mmol tert-carbonic acid monomer, 10 mmol perfluorobutyric acid, 0.11 g 4-dimethylaminopyridine, 14 mmol N, N'-dicyclohexylcarbodiimide and 90 mL dichloromethane are added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen is introduced for protection. The mixture is stirred for reaction at a temperature of 3° C. and a stirring rate of 250 r / min for 25 min, and then the mixture is heated to 48° C. and stirred for reaction for 7 h. After the reaction is completed, the reaction product is cooled to room temperature, and then the solvent is removed by rotary evaporation, and then the mixture is added to ethyl acetate, and then vacuum filtered, and the filtrate is rotary evaporated to remove the solvent to obtain a fluorine-containing tert-carbonic acid monomer; Step S3: 20 g of fluorinated tert-butyl carbonate monomer, 42 g of methyl methacrylate, 22 g of butyl acrylate, 4.5 g of glycidyl methacrylate, 5.4 g of cross-linked 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 11g of ammonium persulfate solution dropwise while stirring, control the drop rate to be 1 drop / s, continue stirring and reacting for 3h after the drop addition is completed, 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 modified 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%; the composite emulsifier is a mixture of OP-10 emulsifier and SDS emulsifier in a mass ratio of 1:1.2; 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 for later use; the polyvinyl alcohol is PVA-1788; the anti-caking agent is white carbon black TH-2000; the defoaming agent is BYK-028 water-based defoaming agent; Step S5: Add modified versatile carbonic acid emulsion, polyvinyl alcohol, anti-caking agent and defoaming agent into 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.
[0024] Embodiment 3, this embodiment is a method for preparing a waterproof redispersible latex powder based on modified versatile carbonic acid emulsion, comprising the following steps: Step S1: 0.1 mmol tert-butyl carbonate E10P, 0.1 mmol 3-butene-1-ol and 0.15 g stannous octoate were added into a three-necked flask equipped with a stirrer and a thermometer, and stirred for reaction at 30° C. and a stirring rate of 300 r / min for 30 min, and then heated to 130° C. and continued to stir for reaction for 4 h. After the reaction was completed, the reaction product was cooled to room temperature to obtain tert-butyl carbonate monomer; Step S2: 10 mmol tert-carbonic acid monomer, 10 mmol perfluorobutyric acid, 0.12 g 4-dimethylaminopyridine, 15 mmol N, N'-dicyclohexylcarbodiimide and 100 mL dichloromethane are added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen is introduced for protection. The mixture is stirred for reaction at a temperature of 5° C. and a stirring rate of 300 r / min for 30 min, and then the mixture is heated to 50° C. and stirred for reaction for 8 h. After the reaction is completed, the reaction product is cooled to room temperature, and then the solvent is removed by rotary evaporation, and then the mixture is added to ethyl acetate, and then vacuum filtered, and the filtrate is rotary evaporated to remove the solvent to obtain a fluorine-containing tert-carbonic acid monomer; Step S3: 30 g of fluorinated tert-butyl carbonate monomer, 45 g of methyl methacrylate, 25 g of butyl acrylate, 6.5 g of glycidyl methacrylate, 7.5 g of cross-linked 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 5min, then add 12g of ammonium persulfate solution dropwise while stirring, control the drop rate to 2 drops / s, continue stirring and reacting for 4h after the dropwise addition is completed, cool the reaction product to room temperature after the reaction is completed, and then pass through a 300-mesh sieve to obtain a modified versatile carbonic acid emulsion; the cross-linking modified 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; 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 according to weight parts for standby use; the polyvinyl alcohol is PVA-1788; the anti-caking agent is white carbon black TH-2000; the defoaming agent is BYK-028 water-based defoaming agent; Step S5: Add modified versatile carbonic acid emulsion, polyvinyl alcohol, anti-caking agent and defoaming agent into a stirring tank, stir and mix for 30 minutes at a temperature of 75°C and a stirring rate of 300r / 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.
[0025] Comparative Example 1: 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: 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 is introduced for protection. The mixture is stirred and reacted for 30min at a temperature of 30°C and a stirring rate of 300r / min, and then the mixture is heated to 85°C and stirred and reacted 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 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 sieved 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; 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 according to weight parts for use; the polyvinyl alcohol is PVA-1788; the anti-caking agent is white carbon black TH-2000; the defoaming agent is BYK-028 water-based defoaming agent; Step S3: Add acrylic emulsion, polyvinyl alcohol, anti-caking agent and defoaming agent into 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.
[0026] Comparative Example 2: 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: Step S1: 0.1 mmol tert-butyl carbonate E10P, 0.1 mmol 3-butene-1-ol and 0.15 g stannous octoate were added into a three-necked flask equipped with a stirrer and a thermometer, and stirred for reaction at 30° C. and a stirring rate of 300 r / min for 30 min, and then heated to 130° C. and continued to stir for reaction for 4 h. After the reaction was completed, the reaction product was cooled to room temperature to obtain tert-butyl carbonate monomer; 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 is introduced for protection. The mixture is stirred and reacted for 30min at a temperature of 30°C and a stirring rate of 300r / min, and then the mixture is heated to 85°C and stirred and reacted for 15min. Then, 12g of ammonium persulfate solution is added dropwise while stirring, and the dropping rate is controlled to be 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 sieved 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; 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 in parts by weight for later use; the polyvinyl alcohol is PVA-1788; the anti-caking agent is white carbon black TH-2000; the defoaming agent is BYK-028 water-based defoaming agent; Step S4: Add versatile carbonic acid emulsion, polyvinyl alcohol, anti-caking agent and defoaming agent into a stirring tank, stir and mix for 30 minutes at a temperature of 75°C and a stirring rate of 300r / 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.
[0027] Comparative Example 3: 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: Step S1: 0.1 mmol tert-butyl carbonate E10P, 0.1 mmol 3-butene-1-ol and 0.15 g stannous octoate were added into a three-necked flask equipped with a stirrer and a thermometer, and stirred for reaction at 30° C. and a stirring rate of 300 r / min for 30 min, and then heated to 130° C. and continued to stir for reaction for 4 h. After the reaction was completed, the reaction product was cooled to room temperature to obtain tert-butyl carbonate monomer; Step S2: 10 mmol tert-carbonic acid monomer, 10 mmol perfluorobutyric acid, 0.12 g 4-dimethylaminopyridine, 15 mmol N, N'-dicyclohexylcarbodiimide and 100 mL dichloromethane are added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen is introduced for protection. The mixture is stirred for reaction at a temperature of 5° C. and a stirring rate of 300 r / min for 30 min, and then the mixture is heated to 50° C. and stirred for reaction for 8 h. After the reaction is completed, the reaction product is cooled to room temperature, and then the solvent is removed by rotary evaporation, and then the mixture is added to ethyl acetate, and then vacuum filtered, and the filtrate is rotary evaporated to remove the solvent to obtain a fluorine-containing tert-carbonic acid monomer; 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 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 is introduced for protection. The mixture is stirred and reacted for 30min at a temperature of 30°C and a stirring rate of 300r / min, and then the mixture is heated to 85°C and stirred and reacted for 15min. Then, 12g of ammonium persulfate solution is added dropwise while stirring, and the dropping rate is controlled to be 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 sieved through a 300-mesh sieve to obtain a modified 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; 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 according to weight parts for standby use; the polyvinyl alcohol is PVA-1788; the anti-caking agent is white carbon black TH-2000; the defoaming agent is BYK-028 water-based defoaming agent; Step S5: Add modified versatile carbonic acid emulsion, polyvinyl alcohol, anti-caking agent and defoaming agent into a stirring tank, stir and mix for 30 minutes at a temperature of 75°C and a stirring rate of 300r / 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.
[0028] Comparative Example 4: 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: Step S1: 0.1 mmol tert-butyl carbonate E10P, 0.1 mmol 3-butene-1-ol and 0.15 g stannous octoate were added into a three-necked flask equipped with a stirrer and a thermometer, and stirred for reaction at 30° C. and a stirring rate of 300 r / min for 30 min, and then heated to 130° C. and continued to stir for reaction for 4 h. After the reaction was completed, the reaction product was cooled to room temperature to obtain tert-butyl carbonate monomer; Step S2: 10 mmol tert-carbonic acid monomer, 10 mmol perfluorobutyric acid, 0.12 g 4-dimethylaminopyridine, 15 mmol N, N'-dicyclohexylcarbodiimide and 100 mL dichloromethane are added to a three-necked flask equipped with a stirrer, a thermometer and an air guide tube, and nitrogen is introduced for protection. The mixture is stirred for reaction at a temperature of 5° C. and a stirring rate of 300 r / min for 30 min, and then the mixture is heated to 50° C. and stirred for reaction for 8 h. After the reaction is completed, the reaction product is cooled to room temperature, and then the solvent is removed by rotary evaporation, and then the mixture is added to ethyl acetate, and then vacuum filtered, and the filtrate is rotary evaporated to remove the solvent to obtain a fluorine-containing tert-carbonic acid monomer; 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 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 is introduced for protection. The mixture is stirred and reacted for 30min at a temperature of 30°C and a stirring rate of 300r / min, and then the mixture is heated to 85°C and stirred and reacted for 15min. Then, 12g of ammonium persulfate solution is added dropwise while stirring, and the dropping rate is controlled to be 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 sieved through a 300-mesh sieve to obtain a modified 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; 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 according to weight parts for standby use; the polyvinyl alcohol is PVA-1788; the anti-caking agent is white carbon black TH-2000; the defoaming agent is BYK-028 water-based defoaming agent; Step S5: Add modified versatile carbonic acid emulsion, polyvinyl alcohol, anti-caking agent and defoaming agent into a stirring tank, stir and mix for 30 minutes at a temperature of 75°C and a stirring rate of 300r / 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.
[0029] Comparative Example 5: 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: Step S1: 0.1 mmol tert-butyl carbonate E10P, 0.1 mmol 3-butene-1-ol and 0.15 g stannous octoate were added into a three-necked flask equipped with a stirrer and a thermometer, and stirred for reaction at 30° C. and a stirring rate of 300 r / min for 30 min, and then heated to 130° C. and continued to stir for reaction for 4 h. After the reaction was completed, the reaction product was cooled to room temperature to obtain tert-butyl carbonate monomer; Step S2: 30 g of tert-butyl carbonate 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 12g of ammonium persulfate solution dropwise while stirring, control the drop rate to 2 drops / s, continue stirring and reacting for 4h after the drop addition is completed, 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 modified 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; 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 in parts by weight for later use; the polyvinyl alcohol is PVA-1788; the anti-caking agent is white carbon black TH-2000; the defoaming agent is BYK-028 water-based defoaming agent; Step S4: Add modified versatile carbonic acid emulsion, polyvinyl alcohol, anti-caking agent and defoaming agent into a stirring tank, stir and mix for 30 minutes at a temperature of 75°C and a stirring rate of 300r / 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.
[0030] The waterproof redispersible latex powder from Examples 1-3 and Comparative Examples 1-5 was mixed into the water-permeable mortar at a ratio of 2 wt %, and the performance of the water-permeable mortar was tested. The test results are shown in the following table: .
[0031] 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 known that adding the waterproof redispersible latex powder of the present application can greatly improve the mechanical properties and waterproof properties of the permeable mortar.
[0032] Among them, the blank example is a permeable mortar without adding waterproof redispersible latex powder.
[0033] The permeable mortar is mixed with 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 1-3mm; and the water reducing agent is PC-1006 polycarboxylate water reducing agent.
[0034] Among them, the 7d compressive strength is tested in accordance with JGJ / T 70-2009 "Standard Test Method 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".
[0035] In the description of this 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.
[0036] 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 in this application, they shall all fall within the protection scope 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 tert-butyl carbonate, 3-butene-1-ol and stannous octoate to react, and cooling the reaction product after the reaction is completed to obtain tert-butyl carbonate monomer; Step s2: stirring a tert-butyl carbonate monomer, perfluorobutyric acid, 4-dimethylaminopyridine, N,N'-dicyclohexylcarbodiimide and dichloromethane for reaction, cooling the reaction product after the reaction is completed, then rotary evaporating the reaction product, then adding the product to ethyl acetate, then vacuum filtering the product, and rotary evaporating the filtrate to obtain a fluorine-containing tert-butyl carbonate monomer; Step s3: stirring the fluorinated versatile carbonic acid monomer, methyl methacrylate, butyl acrylate, glycidyl methacrylate, cross-linking modified monomer, composite emulsifier and deionized water for reaction, then adding ammonium persulfate solution dropwise while stirring, and continuing to stir the reaction after the addition is completed. After the reaction is completed, the reaction product is cooled and then sieved to obtain a modified versatile carbonic acid emulsion.
2. The waterproof redispersible latex powder based on modified versatile carbonic acid emulsion according to claim 1, characterized in that: 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.
3. The waterproof redispersible latex powder based on modified versatile carbonic acid emulsion according to claim 2, characterized in that: The tert-butyl glycidyl carbonate is tert-butyl glycidyl carbonate E10P.
4. The waterproof redispersible latex powder based on modified versatile carbonic acid emulsion according to claim 1, characterized in that: The usage ratio of the tert-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.
5. The waterproof redispersible latex powder based on modified versatile carbonic acid emulsion according to claim 1, characterized in that: 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.
6. The waterproof redispersible latex powder based on modified versatile carbonic acid emulsion according to claim 5, characterized in that: The cross-linking modification monomer is a polyunsaturated fatty acid; the polyunsaturated fatty acid is one of linoleic acid, α-linolenic acid and arachidonic acid.
7. The waterproof redispersible latex powder based on modified versatile carbonic acid emulsion according to claim 5, characterized in that: The mass fraction of the ammonium persulfate solution is 2-3%.
8. The waterproof redispersible latex powder based on modified versatile carbonic acid emulsion according to claim 5, 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.
9. A method for preparing a waterproof redispersible latex powder based on a modified versatile carbonic acid emulsion, 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 kettle, 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.
10. The method for preparing a waterproof redispersible latex powder based on modified versatile carbonic acid emulsion according to claim 9, 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.
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