Heat shrinkage resistant asphalt waterproof coating and preparation method thereof
By pretreating the asphalt raw materials and polymerizing with heat-shrinkage resin additives, combining with the addition of plasticizers, leveling agents, light stabilizers and adsorbents, and ultrasonic treatment and maturation, the existing asphalt waterproof coatings have poor heat-shrinkage resistance and poor environmental protection performance, and a heat-shrinkage resistance asphalt waterproof coating with excellent heat-shrinkage resistance and good environmental protection performance has been prepared.
Patent Information
- Application Number
- CN202510300584.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-14
- Publication Date
- 2025-05-16
- Estimated Expiration
- 2045-03-14
AI Technical Summary
The existing asphalt waterproof coatings have excellent waterproofing effects, poor heat shrinkage resistance and easy release of harmful substances, resulting in poor environmental protection performance.
By pretreating the asphalt raw material, refined asphalt is obtained; grafted polyphenylene sulfide and polyether ether ketone are mixed to obtain heat-shrinkage resin additives; polymerization of heat-shrinkage resin additives with refined asphalt is carried out to form heat-shrinkage asphalt substrates; plasticizers, leveling agents, light stabilizers and adsorbents are added to the coating, and after sonication and maturation, heat-shrinkage asphalt waterproof coatings are finally produced.
While maintaining waterproof performance, the heat shrinkage resistance of the coating is significantly improved, VOC emissions are reduced, and it has good environmental protection performance.
Smart Images

Figure CN119823652B_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of coating compositions and relates to a heat shrinkage resistant asphalt waterproof coating and a preparation method thereof. Background Art
[0002] The application of waterproof materials in human society has a long history. With the development of human industry, people have more and more diverse performance requirements for waterproof materials, giving rise to various types of waterproof materials. Traditional waterproof materials such as rubber have begun to be used in various fields, and with the increasing demand for functional waterproof materials in more and more application fields, various composite materials have also received more and more attention. Among them, asphalt waterproof coating is an important functional waterproof material. It has been widely used in building waterproofing, road and bridge engineering and other fields due to its good adhesion, ductility and self-healing properties. However, while asphalt waterproof coating has excellent waterproof effect, it also has disadvantages such as poor heat shrinkage resistance and easy release of harmful substances. In order to solve these problems, people have made many improvements to asphalt waterproof coating.
[0003] For example, Chinese patent CN116333596B proposes a modified asphalt waterproof coating and a preparation method thereof. By compounding effective components such as emulsified asphalt and emulsified thick oil, the asphalt waterproof coating provided by the invention has a certain fluidity at high temperature, and can provide a better bonding interface for the composite of asphalt coating and coiled material. The problem with this invention is that while improving the high temperature resistance, it produces exudative oil, and the environmental protection performance is poor. Chinese patent CN114133872B proposes a rubber asphalt waterproof coating and a preparation method thereof. Asphalt is modified by end-epoxy liquid nitrile rubber. The prepared rubber asphalt waterproof coating not only has good storage stability before use, but also can maintain creep and good bonding performance for a long time during application. The problem with this invention is that it does not have significant heat shrinkage resistance and has poor weather resistance under high temperature environment. Chinese patent CN117625044B proposes a high heat-resistant non-curing rubber asphalt waterproof coating and a preparation method thereof. It uses silica ash and SBS composite modified asphalt as the main body to improve the compatibility of rubber and asphalt, thereby improving the high temperature stability of the coating. The problem with this invention is that although it has good high and low temperature mechanical properties, its environmental performance has not been improved.
[0004] At present, the existing asphalt waterproof coatings have poor heat shrinkage resistance and are prone to release harmful substances, which are still major problems facing the industry.
[0005] To this end, a heat shrinkage resistant asphalt waterproof coating and a preparation method thereof are proposed. Summary of the invention
[0006] The object of the present invention is to provide a heat-shrinkage-resistant asphalt waterproof coating and a preparation method thereof. The heat-shrinkage-resistant asphalt waterproof coating is prepared by pre-treating asphalt raw materials to obtain refined asphalt; mixing grafted polyphenylene sulfide and polyetheretherketone to obtain a heat-shrinkage-resistant resin additive; polymerizing the heat-shrinkage-resistant resin additive with refined asphalt to obtain a heat-shrinkage-resistant asphalt base material; mixing the heat-shrinkage-resistant asphalt base material with a plasticizer and a leveling agent and then ultrasonically treating the mixture to obtain a coating base material; dispersing a light stabilizer and an adsorbent in an aqueous solvent to obtain a coating additive; and mixing the coating base material with the coating additive and subjecting the mixture to a aging treatment. The heat-shrinkage-resistant asphalt waterproof coating prepared by the present invention has excellent heat-shrinkage resistance while maintaining waterproof performance, and has low VOC emissions and good environmental performance.
[0007] To achieve the above object, the present invention provides the following technical solutions:
[0008] A method for preparing a heat shrinkage resistant asphalt waterproof coating comprises the following steps:
[0009] Mix 70# asphalt, 100# asphalt and mastic asphalt in a mass ratio of 1:2:0.5, heat to 130-180°C at a heating rate of 10°C / min, and heat at a rotation speed of 200 rpm for 5-8 hours to obtain a matured asphalt raw material;
[0010] The matured asphalt raw material is cooled to 25°C, vacuum dried for 2-3 hours, heated to 150°C at a heating rate of 10°C / min, and kept warm for 2 hours to obtain refined asphalt;
[0011] The grafted polyphenylene sulfide and polyetheretherketone are dissolved in an organic solvent A at a mass ratio of 1:1, heated to 50°C, and stirred at a speed of 500-700 rpm for 2 hours, and the organic solvent A is removed to obtain an anti-heat shrinkage resin additive; wherein the organic solvent A is obtained by mixing N-methylpyrrolidone, chloroform and N,N-dimethylacetamide at a volume ratio of 3:1:1;
[0012] 100 parts of refined asphalt and 25 parts of heat-resistant resin additive are dissolved in 300 parts of organic solvent B, and the mixture is fully mixed to obtain heat-resistant asphalt stock solution; wherein the organic solvent B is obtained by mixing N-methylpyrrolidone, tetrahydrofuran and dimethyl sulfoxide in a volume ratio of 2:1:1; 100 parts of the heat-resistant asphalt stock solution are heated to 50°C, 1 part of initiator and 2 parts of phase transfer catalyst are added, the mixture is mixed evenly, the temperature is raised to 70°C, the mixture is reacted at a speed of 500 rpm for 12 hours, the temperature is then lowered to 50°C and the mixture is allowed to stand for 2 hours, the solvent is removed, and the mixture is washed and dried to obtain the heat-resistant asphalt substrate;
[0013] 100 parts of heat-shrinkage-resistant asphalt base material, 3-5 parts of plasticizer, and 2-3 parts of leveling agent are mixed and dissolved in an aqueous solvent, mixed evenly, and then ultrasonically treated for 3-5 hours to obtain a coating base material;
[0014] Dispersing 2 parts of a light stabilizer and 5 parts of an adsorbent in 20 parts of an aqueous solvent, stirring at 300-500 rpm at 40°C for 2 hours, standing for 30 minutes, and removing the precipitate to obtain a coating additive;
[0015] 20 parts of coating additives are mixed with 200 parts of coating base material, and the mixture is cured at 50-70° C. for 24 hours to obtain a heat shrinkage resistant asphalt waterproof coating.
[0016] Preferably, the preparation method of grafted polyphenylene sulfide is as follows: 50 parts of p-dichlorobenzene and 20 parts of anhydrous sodium sulfide are dissolved in 200 parts of N-methylpyrrolidone, heated to 170°C and mixed at a speed of 200 rpm for 30 minutes to obtain a pre-condensation solution; 1 part of anhydrous lithium chloride and 5 parts of sodium hydroxide are added to the pre-condensation solution, nitrogen is passed through and pressurized to 2 bar, the temperature is raised to 240°C and the speed is maintained at 200 rpm for reaction for 2 hours, the temperature is lowered to 130°C and 30 parts of styrene, 1 part of azobisisobutyronitrile and 1 part of benzoyl peroxide are added, the reaction is continued for 8 hours, the solvent is removed, and the grafted polyphenylene sulfide is obtained after washing and drying.
[0017] Preferably, the initiator is azobisisoheptanitrile; and the phase transfer catalyst is tetrabutylammonium bromide.
[0018] Preferably, the plasticizer is dibutyl phthalate (DBP for short, the same below); the leveling agent is organic bentonite; the organic bentonite is obtained by the following steps: 20 parts of sodium bentonite are crushed and mixed with 5 parts of hexadecyltrimethylammonium bromide, stirred and reacted at 300°C at a speed of 100 rpm for 2 hours, and then ground and passed through a 100-mesh sieve to obtain organic bentonite.
[0019] Preferably, the light stabilizer is 2'-(2'-hydroxy-3'-tert-butyl-5'-methylphenyl)-5-chlorobenzotriazole (abbreviated as UV-326, the same below); the adsorbent is diatomaceous earth; the aqueous solvent includes: deionized water, isopropanol, sorbitan oleate and sodium dodecyl sulfate, wherein the amount of deionized water added is 50 parts, the amount of isopropanol added is 20 parts, the amount of sorbitan oleate added is 3 parts, and the amount of sodium dodecyl sulfate added is 2 parts; the aging treatment is: 20 parts of the coating additive are mixed with 200 parts of the coating base material, heated to 50-70°C, stirred at a speed of 20 rpm for 2 hours, stopped stirring, and kept warm for 22 hours to obtain a heat shrinkage resistant asphalt waterproof coating.
[0020] A heat shrinkage resistant asphalt waterproof coating, the main components of which include: refined asphalt, heat shrinkage resistant resin additives, coating additives and aqueous solvents; wherein the heat shrinkage resistant asphalt waterproof coating has the following physical parameters: appearance is a dark brown viscous liquid, density is 1.26-1.31g / mL, surface drying time is 2.2-3.5 hours, and actual drying time is 14.5-16.7 hours.
[0021] Compared with the prior art, the present invention has the following beneficial effects:
[0022] 1. Pre-treat the mixture of 70# asphalt, 100# asphalt and mastic asphalt to remove most of the VOC and moisture in the asphalt, and fully mix the asphalts of different grades, which not only enhances the compatibility of asphalt with various additives, but also ensures that the final asphalt coating has good waterproof performance. At the same time, water-based solvents are used as the base solvent of the coating, which avoids the problem of VOC emissions caused by the use of organic solvents while ensuring good dispersibility of the coating.
[0023] 2. The use of grafted polyphenylene sulfide and polyetheretherketone composed of heat-resistant resin additives and refined asphalt forms a polymer network, which significantly enhances the toughness and adhesion of the asphalt waterproof coating. While improving the waterproofness, it also significantly improves the coating's heat-resistant performance.
[0024] 3. By adding dibutyl phthalate and organic bentonite to the paint, the compatibility of asphalt and aqueous solvents is significantly improved. While introducing high-strength resin additives, it is ensured that the finished paint still has good construction performance, certain fluidity and good adhesion.
[0025] 4. Introducing light stabilizers and adsorbents into the coating significantly improves the light stability of the coating in application scenarios, maintains basic chemical stability under long-term direct sunlight, ensures that organic components are not easily decomposed to produce VOCs, and most of the trace VOCs produced by direct volatilization of organic matter are adsorbed by the adsorbent, so that the waterproof coating prepared by the present invention has excellent weather resistance and environmental protection performance.
[0026] 5. The aging treatment is carried out during the mixing process of the coating to release the internal stress of the polymer structure in the coating, improve the compatibility of asphalt and other functional components, and make the coating product have excellent resistance to heat shrinkage while maintaining excellent waterproof performance. Furthermore, the aging treatment can significantly inhibit the phase separation caused by the aqueous solvent, effectively prolong the storage time of the asphalt waterproof coating, and improve its practical value. BRIEF DESCRIPTION OF THE DRAWINGS
[0027] Figure 1 The present invention is a process flow chart of the preparation method of the heat shrinkage resistant asphalt waterproof coating. DETAILED DESCRIPTION
[0028] The technical solution of the present invention will be clearly and completely described below through some embodiments and experimental examples. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. 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.
[0029] Reference Figure 1 The preparation flow chart shown in the figure, the present invention provides a heat shrinkage resistant asphalt waterproof coating and a preparation method thereof, and the technical scheme is as follows:
[0030] The substance information involved in the present invention is as follows:
[0031] Polyetheretherketone: CAS: 29658-26-2; 70# asphalt: purchased from Shandong Jincheng Petrochemical Group Co., Ltd.; 100# asphalt: purchased from Luoyang Petrochemical; asphalt mastic: purchased from Hejian Wuhu Waterproof Material Factory; p-dichlorobenzene: CAS: 106-46-7; anhydrous sodium sulfide: CAS: 1313-82-2; N-methylpyrrolidone: CAS: 872-50-4; anhydrous lithium chloride: CAS: 7447-41-8; Sodium hydroxide: CAS: 1310-73-2; Styrene: CAS: 100-42-5; Azobisisobutyronitrile: CAS: 78-67-1; Benzoyl peroxide: CAS: 94-36-0; Chloroform: CAS: 67-66-3; N,N-dimethylacetamide: CAS: 127-19-5; Tetrahydrofuran: CAS: 109-99-9; Dimethyl sulfoxide: CAS: 67-68 ... Heptanenitrile: CAS: 4419-11-8; Tetrabutylammonium bromide: CAS: 1643-19-2; Dibutyl phthalate: CAS: 84-74-2; Sodium bentonite: CAS: 85049-30-5; Hexadecyltrimethylammonium bromide: CAS: 57-09-0; UV-326 (i.e. 2'-(2'-hydroxy-3'-tert-butyl-5'-methylphenyl)-5-chlorobenzotriazole): CAS: 3896 -11-5; diatomaceous earth: CAS: 61790-53-2; isopropanol: CAS: 67-63-0; sorbitan oleate: CAS: 1338-43-8; sodium lauryl sulfate: CAS: 151-21-3; acetone: CAS: 67-64-1; ethyl acetate: CAS: 141-78-6; n-hexane: CAS: 110-54-3; polyphenylene sulfide: CAS: 26125-40-6.
[0032] Example 1
[0033] 70# asphalt, 100# asphalt and mastic asphalt were mixed in a mass ratio of 1:2:0.5, heated to 130°C at a heating rate of 10°C / min, and heated at a rotation speed of 200 rpm for 8 hours to obtain a matured asphalt raw material;
[0034] 100 parts of mature asphalt raw material were cooled to 25°C, vacuum dried for 2 hours, heated to 150°C at a heating rate of 10°C / min, and kept warm for 2 hours to obtain refined asphalt;
[0035] 50 parts of p-dichlorobenzene and 20 parts of anhydrous sodium sulfide are dissolved in 200 parts of N-methylpyrrolidone, heated to 170°C and mixed at a speed of 200 rpm for 30 minutes to obtain a pre-condensation solution; 1 part of anhydrous lithium chloride and 5 parts of sodium hydroxide are added to the pre-condensation solution, nitrogen is passed through and pressurized to 2 bar, the temperature is raised to 240°C and the speed is maintained at 200 rpm for reaction for 2 hours, the temperature is lowered to 130°C and 30 parts of styrene, 1 part of azobisisobutyronitrile and 1 part of benzoyl peroxide are added, the reaction is continued for 8 hours, the solvent is removed, and the grafted polyphenylene sulfide is obtained after washing and drying;
[0036] Grafted polyphenylene sulfide and polyetheretherketone are dissolved in an organic solvent A at a mass ratio of 1:1, heated to 50°C, stirred at a speed of 500 rpm for 2 hours, and the organic solvent A is removed to obtain an anti-heat shrinkage resin additive; wherein the organic solvent A is obtained by mixing N-methylpyrrolidone, chloroform and N,N-dimethylacetamide at a volume ratio of 3:1:1;
[0037] 100 parts of refined asphalt and 25 parts of heat-resistant resin additive are dissolved in 300 parts of organic solvent B, and the mixture is fully mixed to obtain heat-resistant asphalt stock solution; wherein the organic solvent B is obtained by mixing N-methylpyrrolidone, tetrahydrofuran and dimethyl sulfoxide in a volume ratio of 2:1:1; 100 parts of the heat-resistant asphalt stock solution are heated to 50°C, 1 part of azobisisoheptanenitrile and 2 parts of tetrabutylammonium bromide are added, the mixture is mixed evenly, the mixture is heated to 70°C, the mixture is reacted at a speed of 500 rpm for 12 hours, the mixture is then cooled to 50°C and allowed to stand for 2 hours, the solvent is removed, and the mixture is washed and dried to obtain the heat-resistant asphalt substrate;
[0038] 20 parts of sodium bentonite were crushed and mixed with 5 parts of hexadecyltrimethylammonium bromide, stirred at 300°C and 100 rpm for 2 hours, and then ground and passed through a 100 mesh sieve to obtain organic bentonite;
[0039] 100 parts of heat shrinkage resistant asphalt base material, 3 parts of DBP and 2 parts of organic bentonite are mixed and dissolved in an aqueous solvent, mixed evenly and then subjected to ultrasonic treatment for 3 hours to obtain a coating base material;
[0040] Dispersing 2 parts of UV-326 and 5 parts of diatomaceous earth in 20 parts of an aqueous solvent, stirring at 300 rpm for 2 hours at 40°C, standing for 30 minutes, and removing the precipitate to obtain a coating additive; the aqueous solvent is obtained by mixing deionized water, isopropanol, sorbitan oleate and sodium lauryl sulfate, wherein the amount of deionized water added is 50 parts, the amount of isopropanol added is 20 parts, the amount of sorbitan oleate added is 3 parts, and the amount of sodium lauryl sulfate added is 2 parts;
[0041] 20 parts of coating additives were mixed with 200 parts of coating base material, heated to 50°C, stirred at 20 rpm for 2 hours, then the stirring was stopped and kept warm for 22 hours to obtain a heat shrinkage resistant asphalt waterproof coating.
[0042] The obtained heat shrinkage resistant asphalt waterproof coating has the following physical parameters: appearance is dark brown viscous liquid, density is 1.26g / mL, surface drying time is 2.2 hours, and actual drying time is 14.5 hours.
[0043] Example 2
[0044] The difference from Example 1 is that the vacuum drying time of the matured asphalt raw material is 3 hours, and the other process parameters are the same.
[0045] Example 3
[0046] Different from Example 1, during the preparation of the matured asphalt raw material, the heating temperature was 140° C., the heating time was 6 hours, and the other process parameters were the same.
[0047] Example 4
[0048] Different from Example 1, during the preparation of the matured asphalt raw material, the heating temperature was 155° C., the heating time was 7 hours, and the other process parameters were the same.
[0049] Example 5
[0050] Different from Example 1, during the preparation of the matured asphalt raw material, the heating temperature was 170° C., the heating time was 5.5 hours, and the other process parameters were the same.
[0051] Example 6
[0052] Different from Example 1, during the preparation of the matured asphalt raw material, the heating temperature was 180° C., the heating time was 5 hours, and the other process parameters were the same.
[0053] Comparative Example 1
[0054] Different from Example 1, the mixture of asphalt raw materials is not pretreated, and other process parameters are the same.
[0055] Comparative Example 2
[0056] Different from Example 1, the aqueous solvent is replaced by an equal number of mixed organic solvents, wherein the mixed organic solvent is obtained by mixing acetone, ethyl acetate and n-hexane in a volume ratio of 1:1:1, and other process parameters are the same.
[0057] Experimental Example 1
[0058] According to the relevant method of GB 30981-2020 standard, the VOC emission of the asphalt waterproof coatings prepared in Examples 1-6 and Comparative Examples 1-2 was measured.
[0059] The VOC emissions corresponding to the asphalt waterproof coatings prepared in Examples 1-6 and Comparative Examples 1-2 are recorded and summarized in Table 1.
[0060] Table 1 Effects of asphalt pretreatment and solvent selection on coating VOC
[0061]
[0062] As shown in the VOC test data of Table 1, the pretreatment of the asphalt raw material significantly reduces the VOC content in the finished coating. The different pretreatment conditions in Examples 1-6 have little effect on the final VOC content. Due to the lack of pretreatment, the VOC value of the final coating obtained in Comparative Example 1 is relatively high, which only meets the general standards of GB 30981-2020 for building protective coatings, and cannot meet the requirements of environmentally friendly coatings. For Comparative Example 2, the replacement of the aqueous solvent with an organic solvent causes the VOC measurement value of the coating to increase significantly, and it does not have environmental protection performance. The vacuum drying and heating treatment in the pretreatment can effectively remove the volatile organic matter and moisture present in the asphalt raw material, while facilitating the subsequent process and reducing the initial VOC content of the raw material; further, replacing the organic solvent with an aqueous solvent can effectively reduce the VOC content of the coating, so that the asphalt waterproof coating prepared by the present invention has excellent environmental protection performance.
[0063] Example 7
[0064] Mix 70# asphalt, 100# asphalt and mastic asphalt in a mass ratio of 1:2:0.5, heat to 150°C at a heating rate of 10°C / min, and heat at a rotation speed of 200 rpm for 7 hours to obtain a matured asphalt raw material;
[0065] 100 parts of mature asphalt raw material were cooled to 25°C, vacuum dried for 2 hours, heated to 150°C at a heating rate of 10°C / min, and kept warm for 2 hours to obtain refined asphalt;
[0066] 50 parts of p-dichlorobenzene and 20 parts of anhydrous sodium sulfide are dissolved in 200 parts of N-methylpyrrolidone, heated to 170°C and mixed at a speed of 200 rpm for 30 minutes to obtain a pre-condensation solution; 1 part of anhydrous lithium chloride and 5 parts of sodium hydroxide are added to the pre-condensation solution, nitrogen is passed through and pressurized to 2 bar, the temperature is raised to 240°C and the speed is maintained at 200 rpm for reaction for 2 hours, the temperature is lowered to 130°C and 30 parts of styrene, 1 part of azobisisobutyronitrile and 1 part of benzoyl peroxide are added, the reaction is continued for 8 hours, the solvent is removed, and the grafted polyphenylene sulfide is obtained after washing and drying;
[0067] Grafted polyphenylene sulfide and polyetheretherketone are dissolved in an organic solvent A at a mass ratio of 1:1, heated to 50°C, stirred at a speed of 700 rpm for 2 hours, and the organic solvent A is removed to obtain an anti-heat shrinkage resin additive; wherein the organic solvent A is obtained by mixing N-methylpyrrolidone, chloroform and N,N-dimethylacetamide at a volume ratio of 3:1:1;
[0068] 100 parts of refined asphalt and 25 parts of heat-resistant resin additive are dissolved in 300 parts of organic solvent B, and the mixture is fully mixed to obtain heat-resistant asphalt stock solution; wherein the organic solvent B is obtained by mixing N-methylpyrrolidone, tetrahydrofuran and dimethyl sulfoxide in a volume ratio of 2:1:1; 100 parts of the heat-resistant asphalt stock solution are heated to 50°C, 1 part of azobisisoheptanenitrile and 2 parts of tetrabutylammonium bromide are added, the mixture is mixed evenly, the mixture is heated to 70°C, the mixture is reacted at a speed of 500 rpm for 12 hours, the mixture is then cooled to 50°C and allowed to stand for 2 hours, the solvent is removed, and the mixture is washed and dried to obtain the heat-resistant asphalt substrate;
[0069] 20 parts of sodium bentonite were crushed and mixed with 5 parts of hexadecyltrimethylammonium bromide, stirred at 300°C and 100 rpm for 2 hours, and then ground and passed through a 100 mesh sieve to obtain organic bentonite;
[0070] 100 parts of heat shrinkage resistant asphalt base material, 5 parts of DBP and 3 parts of organic bentonite are mixed and dissolved in an aqueous solvent, mixed evenly and then subjected to ultrasonic treatment for 3 hours to obtain a coating base material;
[0071] Dispersing 2 parts of UV-326 and 5 parts of diatomaceous earth in 20 parts of an aqueous solvent, stirring at 500 rpm for 2 hours at 40°C, standing for 30 minutes, and removing the precipitate to obtain a coating additive; the aqueous solvent is obtained by mixing water, isopropanol, sorbitan oleate and sodium lauryl sulfate, wherein the amount of water added is 50 parts, the amount of isopropanol added is 20 parts, the amount of sorbitan oleate added is 3 parts, and the amount of sodium lauryl sulfate added is 2 parts;
[0072] 20 parts of coating additives were mixed with 200 parts of coating base material, heated to 60°C, stirred at 20 rpm for 2 hours, then the stirring was stopped and kept warm for 22 hours to obtain a heat shrinkage resistant asphalt waterproof coating.
[0073] The obtained heat shrinkage resistant asphalt waterproof coating has the following physical parameters: appearance is dark brown viscous liquid, density is 1.31g / mL, surface drying time is 3.5 hours, and actual drying time is 16.7 hours.
[0074] Example 8
[0075] The difference from Example 7 is that during the mixing process of grafted polyphenylene sulfide and polyetheretherketone, the stirring speed is 600 rpm, and the other process parameters are the same.
[0076] Example 9
[0077] The difference from Example 7 is that during the mixing process of grafted polyphenylene sulfide and polyetheretherketone, the stirring speed is 500 rpm, and the other process parameters are the same.
[0078] Comparative Example 3
[0079] The difference from Example 7 is that an equal amount of polyphenylene sulfide is used to replace the grafted polyphenylene sulfide, and the other process parameters are the same.
[0080] Comparative Example 4
[0081] The difference from Example 7 is that the grafted polyphenylene sulfide and polyetheretherketone are not dissolved and mixed, and a simple mixture of equal parts of grafted polyphenylene sulfide and polyetheretherketone in a ratio of 1:1 is used to replace the anti-heat shrinkage resin additive, and other process parameters are the same.
[0082] Comparative Example 5
[0083] The difference from Example 7 is that the refined asphalt and the anti-heat shrinkage resin additive are not polymerized, the anti-heat shrinkage asphalt stock solution is used to replace the anti-heat shrinkage asphalt substrate for subsequent processes after the solvent is removed, and other process parameters are the same.
[0084] Comparative Example 6
[0085] The difference from Example 7 is that no anti-heat shrinkage resin additive is added, and an equal amount of refined asphalt is used to replace the anti-heat shrinkage resin additive. Other process parameters are the same.
[0086] Experimental Example 2
[0087] The asphalt waterproof coatings prepared in Examples 7-9 and Comparative Examples 3-6 were subjected to contact angle measurement and water permeability test to characterize their waterproof properties; static thermomechanical analysis was performed to test the heat shrinkage rate of each coating to characterize its heat shrinkage resistance. The relevant test results are summarized in Table 2.
[0088] The specific test method is as follows:
[0089] Contact angle measurement: Apply the asphalt waterproof coating on the cement substrate to a thickness of about 1-2 mm after drying. Use the sessile drop method to measure the static contact angle between the corresponding coating and the water drop.
[0090] Water permeability test: Apply asphalt waterproof coating on the bottom and sides of a cement container with a height of 50 cm, a bottom size of 20×20 cm, and a thickness of 1 cm. Make the thickness of the coating about 2 mm after drying. Inject 12 kg of water and seal the container. After 24 hours, weigh the remaining water. The water permeability is 2800 cm. 2 The corresponding water permeability and permeability coefficient are calculated based on the reference.
[0091] Static thermomechanical analysis: HITACHI TMA7100 was used to test the heat shrinkage of a Φ8×L20mm solid dry paint sample, wherein the test temperature range was 25-200°C. The smaller the heat shrinkage of the paint, the stronger the corresponding heat shrinkage resistance.
[0092] Table 2 Waterproofness and heat shrinkage resistance of coatings prepared in Examples 7-9 and Comparative Examples 3-6
[0093]
[0094] As shown in the water resistance and heat shrinkage resistance data of Table 2, Examples 7-9 all have good water resistance and heat shrinkage resistance, and the change in stirring speed has little effect on the final performance of the coating. For Comparative Example 3, the lack of grafting treatment of polyphenylene sulfide affects the compatibility of the heat shrinkage-resistant resin additive with refined asphalt, resulting in a decrease in the water resistance of the coating product and a weakening of the heat shrinkage resistance. For Comparative Example 4, the two thermoplastic resins that are not fully mixed in advance affect the effects of other processes in subsequent steps, and also reduce the water resistance and heat shrinkage resistance of the coating product. In Comparative Example 5, the lack of polymerization reaction makes it impossible for the asphalt matrix to form a composite polymer network with the resin additive, and the water resistance is significantly reduced, and the heat shrinkage resistance is also greatly reduced. Due to the lack of the heat shrinkage-resistant resin additive in Comparative Example 6, it only relies on the waterproof effect of the asphalt matrix itself, and its water resistance is similar to that of Comparative Example 5, which proves the importance of polymerization reaction in improving water resistance. At the same time, the disadvantage of poor heat shrinkage resistance of the asphalt coating itself is very obvious. The main purpose of the grafting treatment of polyphenylene sulfide and the dissolving and mixing with polyetheretherketone is to improve the compatibility of thermoplastic resin with asphalt matrix and other components, so as to achieve a strong composite of the functionalities of various components. The lack of this step will cause a significant reduction in the overall performance of the coating. The polymerization reaction of the anti-heat shrinkage resin additive and refined asphalt effectively forms a polymer network between the two components, improving the toughness and stability of the finished coating, while improving the original waterproofness of the asphalt coating and improving its poor heat shrinkage resistance. If the polymerization reaction is not carried out, the addition of the anti-heat shrinkage resin additive can hardly improve the waterproofness of the coating, and the improvement of the heat shrinkage resistance of the coating is small, and it has no use value.
[0095] Example 10
[0096] 70# asphalt, 100# asphalt and mastic asphalt were mixed in a mass ratio of 1:2:0.5, heated to 160°C at a heating rate of 10°C / min, and heated at a rotation speed of 200 rpm for 7 hours to obtain a matured asphalt raw material;
[0097] 100 parts of mature asphalt raw material were cooled to 25°C, vacuum dried for 2.5 hours, heated to 150°C at a heating rate of 10°C / min, and kept warm for 2 hours to obtain refined asphalt;
[0098] 50 parts of p-dichlorobenzene and 20 parts of anhydrous sodium sulfide are dissolved in 200 parts of N-methylpyrrolidone, heated to 170°C and mixed at a speed of 200 rpm for 30 minutes to obtain a pre-condensation solution; 1 part of anhydrous lithium chloride and 5 parts of sodium hydroxide are added to the pre-condensation solution, nitrogen is passed through and pressurized to 2 bar, the temperature is raised to 240°C and the speed is maintained at 200 rpm for reaction for 2 hours, the temperature is lowered to 130°C and 30 parts of styrene, 1 part of azobisisobutyronitrile and 1 part of benzoyl peroxide are added, the reaction is continued for 8 hours, the solvent is removed, and the grafted polyphenylene sulfide is obtained after washing and drying;
[0099] Grafted polyphenylene sulfide and polyetheretherketone are dissolved in an organic solvent A at a mass ratio of 1:1, heated to 50°C, stirred at a speed of 700 rpm for 2 hours, and the organic solvent A is removed to obtain an anti-heat shrinkage resin additive; wherein the organic solvent A is obtained by mixing N-methylpyrrolidone, chloroform and N,N-dimethylacetamide at a volume ratio of 3:1:1;
[0100] 100 parts of refined asphalt and 25 parts of heat-resistant resin additive are dissolved in 300 parts of organic solvent B, and the mixture is fully mixed to obtain heat-resistant asphalt stock solution; wherein the organic solvent B is obtained by mixing N-methylpyrrolidone, tetrahydrofuran and dimethyl sulfoxide in a volume ratio of 2:1:1; 100 parts of the heat-resistant asphalt stock solution are heated to 50°C, 1 part of azobisisoheptanenitrile and 2 parts of tetrabutylammonium bromide are added, the mixture is mixed evenly, the mixture is heated to 70°C, the mixture is reacted at a speed of 500 rpm for 12 hours, the mixture is then cooled to 50°C and allowed to stand for 2 hours, the solvent is removed, and the mixture is washed and dried to obtain the heat-resistant asphalt substrate;
[0101] 20 parts of sodium bentonite were crushed and mixed with 5 parts of hexadecyltrimethylammonium bromide, stirred at 300°C and 100 rpm for 2 hours, and then ground and passed through a 100 mesh sieve to obtain organic bentonite;
[0102] 100 parts of heat shrinkage resistant asphalt base material, 5 parts of DBP and 3 parts of organic bentonite are mixed and dissolved in an aqueous solvent, mixed evenly and then subjected to ultrasonic treatment for 4 hours to obtain a coating base material;
[0103] Dispersing 2 parts of UV-326 and 5 parts of diatomaceous earth in 20 parts of an aqueous solvent, stirring at 300 rpm for 2 hours at 40°C, standing for 30 minutes, and removing the precipitate to obtain a coating additive; the aqueous solvent is obtained by mixing deionized water, isopropanol, sorbitan oleate and sodium lauryl sulfate, wherein the amount of deionized water added is 50 parts, the amount of isopropanol added is 20 parts, the amount of sorbitan oleate added is 3 parts, and the amount of sodium lauryl sulfate added is 2 parts;
[0104] 20 parts of coating additives were mixed with 200 parts of coating base material, heated to 70°C, stirred at 20 rpm for 2 hours, then the stirring was stopped and kept warm for 22 hours to obtain a heat shrinkage resistant asphalt waterproof coating.
[0105] The obtained heat shrinkage resistant asphalt waterproof coating has the following physical parameters: appearance is dark brown viscous liquid, density is 1.29g / mL, surface drying time is 3.1 hours, and actual drying time is 15.3 hours.
[0106] Embodiment 11
[0107] The difference from Example 10 is that the added amount of DBP is 3 parts, the added amount of organic bentonite is 2 parts, and the other process parameters are the same.
[0108] Example 12
[0109] The difference from Example 10 is that the added amount of DBP is 4 parts, the added amount of organic bentonite is 2 parts, and the other process parameters are the same.
[0110] Embodiment 13
[0111] The difference from Example 10 is that the amount of organic bentonite added is 2 parts, and the other process parameters are the same.
[0112] Comparative Example 7
[0113] The difference from Example 10 is that DBP is not added, and other process parameters are the same.
[0114] Comparative Example 8
[0115] The difference from Example 10 is that no organic bentonite is added, and other process parameters are the same.
[0116] Comparative Example 9
[0117] The difference from Example 10 is that an equal amount of sodium bentonite is used to replace the organic bentonite, and the other process parameters are the same.
[0118] Experimental Example 3
[0119] The viscosity of the asphalt waterproof coatings prepared in Examples 10-13 and Comparative Examples 7-9 was measured using a rotational viscometer to characterize the workability of the coatings. The results are summarized in Table 3.
[0120] The asphalt waterproof coatings prepared in Examples 10-13 and Comparative Examples 7-9 were placed in an acrylic cylinder with a diameter of 20 cm and a height of 30 cm for 96 hours to observe whether stratification and agglomeration occurred. The results are summarized in Table 3.
[0121] Table 3 Workability of coatings prepared in Examples 10-13 and Comparative Examples 7-9
[0122]
[0123] As shown in the construction-related data of Table 3, DBP and organic bentonite significantly improve the construction performance of the coating. For Examples 10-13, different amounts of plasticizers and leveling agents have little effect on the construction performance of the coating, and the coating has better preservation. For Comparative Example 7, the lack of plasticizer DBP significantly reduces the compatibility between the asphalt component and the aqueous solvent, and the coating is stratified after being placed for a long time. Due to the introduction of polyphenylene sulfide and polyetheretherketone, the entire coating system has a higher viscosity than ordinary modified asphalt, and the coating substrate needs to be better soluble in the aqueous solvent to maintain good construction performance. For Comparative Example 8, the lack of organic bentonite makes it easy for the coating components to agglomerate. After standing, the coating will be stratified and the polymer component will agglomerate at the same time, and the overall construction performance will deteriorate. If sodium bentonite is used directly, because it does not have amphiphilicity, it is reflected in Comparative Example 9 as a construction performance worse than that of Comparative Example 8, and stratification and coating agglomeration usually occur. Therefore, the addition of DBP and organic bentonite is necessary to maintain the good construction performance and stability of asphalt waterproof coatings. These two additives can effectively disperse the polymer components in the aqueous solvent and stably maintain the dispersed state. Even with the addition of thermosetting resin additives, the coating can still maintain good construction performance. At the same time, organic bentonite can disperse the organic components that are prone to agglomeration, thereby inhibiting the agglomeration phenomenon of the coating and helping to extend the shelf life of the coating.
[0124] Embodiment 14
[0125] 70# asphalt, 100# asphalt and mastic asphalt were mixed in a mass ratio of 1:2:0.5, heated to 130°C at a heating rate of 10°C / min, and heated at a rotation speed of 200 rpm for 8 hours to obtain a matured asphalt raw material;
[0126] 100 parts of mature asphalt raw material were cooled to 25°C, vacuum dried for 2 hours, heated to 150°C at a heating rate of 10°C / min, and kept warm for 2 hours to obtain refined asphalt;
[0127] 50 parts of p-dichlorobenzene and 20 parts of anhydrous sodium sulfide are dissolved in 200 parts of N-methylpyrrolidone, heated to 170°C and mixed at a speed of 200 rpm for 30 minutes to obtain a pre-condensation solution; 1 part of anhydrous lithium chloride and 5 parts of sodium hydroxide are added to the pre-condensation solution, nitrogen is passed through and pressurized to 2 bar, the temperature is raised to 240°C and the speed is maintained at 200 rpm for reaction for 2 hours, the temperature is lowered to 130°C and 30 parts of styrene, 1 part of azobisisobutyronitrile and 1 part of benzoyl peroxide are added, the reaction is continued for 8 hours, the solvent is removed, and the grafted polyphenylene sulfide is obtained after washing and drying;
[0128] Grafted polyphenylene sulfide and polyetheretherketone are dissolved in an organic solvent A at a mass ratio of 1:1, heated to 50°C, stirred at a speed of 500 rpm for 2 hours, and the organic solvent A is removed to obtain an anti-heat shrinkage resin additive; wherein the organic solvent A is obtained by mixing N-methylpyrrolidone, chloroform and N,N-dimethylacetamide at a volume ratio of 3:1:1;
[0129] 100 parts of refined asphalt and 25 parts of heat-resistant resin additive are dissolved in 300 parts of organic solvent B, and the mixture is fully mixed to obtain heat-resistant asphalt stock solution; wherein the organic solvent B is obtained by mixing N-methylpyrrolidone, tetrahydrofuran and dimethyl sulfoxide in a volume ratio of 2:1:1; 100 parts of the heat-resistant asphalt stock solution are heated to 50°C, 1 part of azobisisoheptanenitrile and 2 parts of tetrabutylammonium bromide are added, the mixture is mixed evenly, the mixture is heated to 70°C, the mixture is reacted at a speed of 500 rpm for 12 hours, the mixture is then cooled to 50°C and allowed to stand for 2 hours, the solvent is removed, and the mixture is washed and dried to obtain the heat-resistant asphalt substrate;
[0130] 20 parts of sodium bentonite were crushed and mixed with 5 parts of hexadecyltrimethylammonium bromide, stirred at 300°C and 100 rpm for 2 hours, and then ground and passed through a 100 mesh sieve to obtain organic bentonite;
[0131] 100 parts of heat shrinkage resistant asphalt base material, 5 parts of DBP and 3 parts of organic bentonite are mixed and dissolved in an aqueous solvent, mixed evenly and then subjected to ultrasonic treatment for 5 hours to obtain a coating base material;
[0132] Dispersing 2 parts of UV-326 and 5 parts of diatomaceous earth in 20 parts of an aqueous solvent, stirring at 300 rpm for 2 hours at 40°C, standing for 30 minutes, and removing the precipitate to obtain a coating additive; the aqueous solvent is obtained by mixing deionized water, isopropanol, sorbitan oleate and sodium lauryl sulfate, wherein the amount of deionized water added is 50 parts, the amount of isopropanol added is 20 parts, the amount of sorbitan oleate added is 3 parts, and the amount of sodium lauryl sulfate added is 2 parts;
[0133] 20 parts of coating additives were mixed with 200 parts of coating base material, heated to 60°C, stirred at 20 rpm for 2 hours, then the stirring was stopped and kept warm for 22 hours to obtain a heat shrinkage resistant asphalt waterproof coating.
[0134] The obtained heat shrinkage resistant asphalt waterproof coating has the following physical parameters: appearance is dark brown viscous liquid, density is 1.30g / mL, surface drying time is 2.9 hours, and actual drying time is 14.8 hours.
[0135] Comparative Example 10
[0136] The difference from Example 14 is that UV-326 is not added, and other process parameters are the same.
[0137] Comparative Example 11
[0138] The difference from Example 14 is that diatomaceous earth is not added, and other process parameters are the same.
[0139] Comparative Example 12
[0140] The difference from Example 14 is that UV-326 and diatomaceous earth are not added, and other process parameters are the same.
[0141] Experimental Example 4
[0142] The coatings prepared in Example 14 and Comparative Examples 10-12 were respectively coated on a cement substrate with a side length of 20 cm, and after drying, placed in a 0.5 m 3 The samples were placed in transparent acrylic jars and sealed in the open air for 72 hours, with an average sunshine duration of 12.3 h / day.
[0143] The air samples in the tanks corresponding to each paint sample were tested by gas chromatography to obtain VOC concentration data.
[0144] The test results are as follows:
[0145] Example 14: paint sample, VOC concentration: 3.7 mg / m 3 ;
[0146] Comparative Example 10 corresponds to the paint sample, VOC concentration: 165.2 mg / m 3 ;
[0147] Comparative Example 11 corresponds to the paint sample, VOC concentration: 51.3 mg / m 3 ;
[0148] Comparative Example 12 corresponds to the paint sample, VOC concentration: 329.1 mg / m 3 .
[0149] According to the VOC concentration data obtained in Experimental Example 4, it can be seen that under the condition of direct sunlight in the open air, UV-326 can effectively inhibit the decomposition of organic matter in the coating, thereby significantly reducing the amount of VOC generated. For Comparative Example 10, due to the lack of light stabilizer, under direct sunlight, some non-volatile organic molecules in the coating decompose under the action of ultraviolet rays, produce volatile organic matter and evaporate into the air, causing certain pollution. For Comparative Example 11, the light stabilizer inhibits the decomposition of non-volatile organic matter, but due to the lack of adsorbent, part of the volatile organic matter originally present in the coating escapes, causing an increase in the VOC concentration, but compared to Comparative Example 10 without adding light stabilizer, its concentration is relatively low. For Comparative Example 12, due to the simultaneous lack of light stabilizer and adsorbent, the decomposition of non-volatile organic matter and the partial escape of volatile organic matter are not inhibited, so the VOC concentration is very high and has certain pollution. UV-326 and diatomaceous earth have a key synergistic effect in inhibiting the generation of VOCs in asphalt waterproof coatings under light: UV-326 can absorb energy from ultraviolet rays, avoid the decomposition of unstable non-volatile organic compounds, and reduce the generation of volatile organic compounds; diatomaceous earth can adsorb free volatile organic compounds and reduce the total amount of VOCs released by the coating. Therefore, the effects of the two complement each other and significantly reduce the generation of VOCs in the finished coating under light.
[0150] Embodiment 15
[0151] 70# asphalt, 100# asphalt and mastic asphalt were mixed in a mass ratio of 1:2:0.5, heated to 145°C at a heating rate of 10°C / min, and heated at a rotation speed of 200 rpm for 6 hours to obtain a matured asphalt raw material;
[0152] 100 parts of mature asphalt raw materials were cooled to 25°C, vacuum dried for 3 hours, heated to 150°C at a heating rate of 10°C / min, and kept warm for 2 hours to obtain refined asphalt;
[0153] 50 parts of p-dichlorobenzene and 20 parts of anhydrous sodium sulfide are dissolved in 200 parts of N-methylpyrrolidone, heated to 170°C and mixed at a speed of 200 rpm for 30 minutes to obtain a pre-condensation solution; 1 part of anhydrous lithium chloride and 5 parts of sodium hydroxide are added to the pre-condensation solution, nitrogen is passed through and pressurized to 2 bar, the temperature is raised to 240°C and the speed is maintained at 200 rpm for reaction for 2 hours, the temperature is lowered to 130°C and 30 parts of styrene, 1 part of azobisisobutyronitrile and 1 part of benzoyl peroxide are added, the reaction is continued for 8 hours, the solvent is removed, and the grafted polyphenylene sulfide is obtained after washing and drying;
[0154] Grafted polyphenylene sulfide and polyetheretherketone are dissolved in an organic solvent A at a mass ratio of 1:1, heated to 50°C, stirred at a speed of 500 rpm for 2 hours, and the organic solvent A is removed to obtain an anti-heat shrinkage resin additive; wherein the organic solvent A is obtained by mixing N-methylpyrrolidone, chloroform and N,N-dimethylacetamide at a volume ratio of 3:1:1;
[0155] 100 parts of refined asphalt and 25 parts of heat-resistant resin additive are dissolved in 300 parts of organic solvent B, and the mixture is fully mixed to obtain heat-resistant asphalt stock solution; wherein the organic solvent B is obtained by mixing N-methylpyrrolidone, tetrahydrofuran and dimethyl sulfoxide in a volume ratio of 2:1:1; 100 parts of the heat-resistant asphalt stock solution are heated to 50°C, 1 part of azobisisoheptanenitrile and 2 parts of tetrabutylammonium bromide are added, the mixture is mixed evenly, the mixture is heated to 70°C, the mixture is reacted at a speed of 500 rpm for 12 hours, the mixture is then cooled to 50°C and allowed to stand for 2 hours, the solvent is removed, and the mixture is washed and dried to obtain the heat-resistant asphalt substrate;
[0156] 20 parts of sodium bentonite were crushed and mixed with 5 parts of hexadecyltrimethylammonium bromide, stirred at 300°C and 100 rpm for 2 hours, and then ground and passed through a 100 mesh sieve to obtain organic bentonite;
[0157] 100 parts of heat shrinkage resistant asphalt base material, 4 parts of DBP and 3 parts of organic bentonite are mixed and dissolved in an aqueous solvent, mixed evenly and then subjected to ultrasonic treatment for 5 hours to obtain a coating base material;
[0158] Dispersing 2 parts of UV-326 and 5 parts of diatomaceous earth in 20 parts of an aqueous solvent, stirring at 300 rpm for 2 hours at 40°C, standing for 30 minutes, and removing the precipitate to obtain a coating additive; the aqueous solvent is obtained by mixing deionized water, isopropanol, sorbitan oleate and sodium lauryl sulfate, wherein the amount of deionized water added is 50 parts, the amount of isopropanol added is 20 parts, the amount of sorbitan oleate added is 3 parts, and the amount of sodium lauryl sulfate added is 2 parts;
[0159] 20 parts of coating additives were mixed with 200 parts of coating base material, heated to 70°C, stirred at 20 rpm for 2 hours, then the stirring was stopped and kept warm for 22 hours to obtain a heat shrinkage resistant asphalt waterproof coating.
[0160] The obtained heat shrinkage resistant asphalt waterproof coating has the following physical parameters: appearance is dark brown viscous liquid, density is 1.27g / mL, surface drying time is 3.1 hours, and actual drying time is 15.5 hours.
[0161] Example 16
[0162] The difference from Example 15 is that the aging temperature is 60° C., and the other process parameters are the same.
[0163] Embodiment 17
[0164] The difference from Example 15 is that the aging temperature is 50° C. and the other process parameters are the same.
[0165] Comparative Example 13
[0166] The difference from Example 15 is that no aging treatment is performed, and other process parameters are the same.
[0167] Comparative Example 14
[0168] The difference from Example 15 is that during the aging process, no stirring is performed and the mixture is kept warm for 24 hours. Other process parameters are the same.
[0169] Comparative Example 15
[0170] The difference from Example 15 is that during the aging process, stirring is not stopped and stirring is continued at a rotation speed of 20 rpm for 24 hours, and other process parameters are the same.
[0171] Experimental Example 5
[0172] Referring to the methods in Experimental Examples 2 and 3, the asphalt waterproof coatings prepared in Examples 15-17 and Comparative Examples 13-15 were tested for waterproofness and heat shrinkage resistance, and their viscosity was tested, and the stratification and the occurrence of lumps were observed. The results are summarized in Table 4.
[0173] Table 4 Effect of aging treatment on comprehensive performance of coatings
[0174]
[0175] As shown in the comprehensive performance data of the coating in Table 4, different steps of the aging treatment have different effects on the performance of the coating. For Examples 15-17, different aging temperatures have no obvious effect on the water resistance and workability of the coating, and the coatings prepared within the aging temperature range of 50-70°C have good water resistance and heat shrinkage resistance, and good workability. For Comparative Example 13, the lack of the aging process does not release the internal stress of the polymer structure in the coating, and the compatibility of asphalt with other components deteriorates, so it is difficult to fully exert the synergistic effect of various functional components, and at the same time causes the storage resistance of the coating to decrease. For Comparative Example 14, the lack of stirring causes the dispersibility of the asphalt component in the aqueous solvent to deteriorate, and the overall uniformity of the coating is reduced, but it still has certain water resistance and heat shrinkage resistance, but the workability and storage resistance have been greatly reduced. For Comparative Example 15, continuous stirring causes agglomeration between some organic components, which reduces the workability of the coating to a certain extent, but the water resistance and heat shrinkage resistance are not greatly affected. Therefore, the aging process effectively reduces the internal stress of the polymer structure in the coating, improves the compatibility of the components, helps the functional components to play a synergistic role, and obtains a coating product with excellent construction performance, storage resistance, waterproofness, and heat shrinkage resistance.
[0176] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.
Claims
1. A method for preparing a heat shrinkage resistant asphalt waterproof coating, characterized in that: The preparation method is as follows: Pre-treating the asphalt raw material to obtain refined asphalt; The grafted polyphenylene sulfide and polyetheretherketone are dissolved in an organic solvent A at a mass ratio of 1:1, heated to 50° C., stirred at a speed of 500-700 rpm, and the organic solvent A is removed to obtain an anti-heat shrinkage resin additive; The refined asphalt and the anti-heat shrinkage resin additive are dissolved in an organic solvent B, and the mixture is fully mixed to obtain an anti-heat shrinkage asphalt stock solution; the anti-heat shrinkage asphalt stock solution is heated to 50° C., an initiator and a phase transfer catalyst are added, and a polymerization reaction is performed to obtain an anti-heat shrinkage asphalt substrate; 100 parts of the heat-resistant asphalt base material are mixed with 3-5 parts of a plasticizer and 2-3 parts of a leveling agent, and then dissolved in an aqueous solvent, mixed evenly, and then subjected to ultrasonic treatment for 3-5 hours to obtain a coating base material; Dispersing the light stabilizer and the adsorbent in the aqueous solvent, stirring at 300-500 rpm at 40° C. for 2 hours, standing for 30 minutes, and removing the precipitate to obtain a coating additive; The coating additive is mixed with the coating base material, and subjected to aging treatment at 50-70° C. for 24 hours to obtain a heat shrinkage resistant asphalt waterproof coating.
2. The method for preparing a heat shrinkage resistant asphalt waterproof coating according to claim 1, characterized in that: The asphalt raw material is a mixture of 70# asphalt, 100# asphalt and mastic asphalt; the mass ratio of the 70# asphalt, 100# asphalt and mastic asphalt is 1:2:0.
5.
3. The method for preparing a heat shrinkage resistant asphalt waterproof coating according to claim 1, characterized in that: The pretreatment is as follows: heating the asphalt raw material to 130-180°C at a heating rate of 10°C / min, stirring and heating for 5-8 hours to obtain a matured asphalt raw material; cooling the matured asphalt raw material, vacuum drying for 2-3 hours, heating to 150°C at a heating rate of 10°C / min, and obtaining the refined asphalt after heat preservation.
4. The method for preparing a heat shrinkage resistant asphalt waterproof coating according to claim 1, characterized in that: The preparation method of the grafted polyphenylene sulfide is as follows: dissolving p-dichlorobenzene and anhydrous sodium sulfide in N-methylpyrrolidone, heating to 170°C and stirring and mixing to obtain a pre-condensation solution; adding anhydrous lithium chloride and sodium hydroxide to the pre-condensation solution, passing nitrogen gas to pressurize to 2 bar, heating to 240°C and stirring to react for 2 hours, cooling to 130°C and adding styrene, azobisisobutyronitrile and benzoyl peroxide, continuing to react for 8 hours, removing the solvent and washing and drying to obtain the grafted polyphenylene sulfide.
5. The method for preparing a heat shrinkage resistant asphalt waterproof coating according to claim 1, characterized in that: The organic solvent A is a mixture of N-methylpyrrolidone, chloroform and N,N-dimethylacetamide; the volume ratio of the N-methylpyrrolidone, the chloroform and the N,N-dimethylacetamide is 3:1:
1.
6. The method for preparing a heat shrinkage resistant asphalt waterproof coating according to claim 1, characterized in that: The organic solvent B is a mixture of N-methylpyrrolidone, tetrahydrofuran and dimethyl sulfoxide; the volume ratio of the N-methylpyrrolidone, the tetrahydrofuran and the dimethyl sulfoxide is 2:1:
1.
7. The method for preparing a heat shrinkage resistant asphalt waterproof coating according to claim 1, characterized in that: The steps of the polymerization reaction are: heating the anti-heat shrinkage asphalt stock solution to 50°C, adding the initiator and the phase transfer catalyst, mixing evenly and heating to 70°C, stirring for reaction for 12 hours, then cooling to 50°C and standing, removing the solvent and washing and drying to obtain the anti-heat shrinkage asphalt substrate; the initiator is azobisisoheptanonitrile; and the phase transfer catalyst is tetrabutylammonium bromide.
8. The method for preparing a heat shrinkage resistant asphalt waterproof coating according to claim 1, characterized in that: The plasticizer is dibutyl phthalate; the leveling agent is organic bentonite; the organic bentonite is obtained by the following steps: crushing sodium bentonite and mixing it with hexadecyltrimethylammonium bromide, heating and stirring the mixture, grinding the obtained product and passing it through a 100-mesh sieve to obtain the organic bentonite.
9. The method for preparing a heat shrinkage resistant asphalt waterproof coating according to claim 1, characterized in that: The light stabilizer is 2'-(2'-hydroxy-3'-tert-butyl-5'-methylphenyl)-5-chlorobenzotriazole; the adsorbent is diatomaceous earth; the aqueous solvent includes: deionized water, isopropanol, sorbitan oleate and sodium dodecyl sulfate; the aging treatment step is: mixing the coating additive with the coating substrate, heating to 50-70°C and stirring for 2 hours, then stopping stirring and keeping warm for 22 hours to obtain the heat shrinkage resistant asphalt waterproof coating.
10. A heat shrinkage resistant asphalt waterproof coating, characterized in that: The heat-shrinkage-resistant asphalt waterproof coating comprises: refined asphalt, heat-shrinkage-resistant resin additive, coating additive and aqueous solvent; the heat-shrinkage-resistant asphalt waterproof coating is prepared by the preparation method described in any one of claims 1-9.
Citation Information
Patent Citations
Rubber Asphalt Waterproof Coating and its Preparation Method
CN114133872B
A modified asphalt waterproof coating and preparation method thereof
CN116333596B
High heat-resistant non-curing rubber asphalt waterproof coating and preparation method thereof
CN117625044B
High-performance polyether-ether-ketone plastic alloy and preparation method thereof
CN103059507A
Preparation method of building waterproofing materials
CN108859288A