Production process of high-viscosity self-adhesive waterproof coiled material for wall surface

Abstract

The application discloses a production process of a high-adhesion self-adhesive waterproof coiled material for wall surfaces and belongs to the technical field of waterproof coiled material production processes. Hot melt glue melt is coated on the surface of an HDPE film, and then reaction sand is paved on the surface of the hot melt glue melt. After rolling and bonding, the sand belt with a sand layer and a hot melt glue layer is prepared by using ultraviolet light curing. The self-adhesive glue is coated on one side of the sand layer of the HDPE film raw material, and the processing of the self-adhesive glue layer is completed. Then, the release paper is covered on the side of the self-adhesive glue layer away from the HDPE film, so that the high-adhesion self-adhesive waterproof coiled material for wall surfaces is obtained. The reaction type polyurethane elastomer is beneficial to increasing the initial adhesion of the hot melt glue melt, and can further bond the reaction sand firmly after cooling and solidification. The quaternary ammonium polyphenyl ether can increase the hydrophilicity of the hot melt glue layer, is beneficial to combining the moisture in the air, and is beneficial to improving the cohesive force, firmly bonding the reaction sand and preventing the sand layer from falling off during use.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of waterproofing membrane production process, and particularly relates to a production process of a high-adhesion self-adhesive waterproofing membrane for wall surfaces. BACKGROUND

[0002] In engineering construction, waterproofing membranes play an increasingly important role as a kind of roofing material. Waterproofing membranes are mainly applied to building walls, roofs, tunnels and roads, etc., and serve as a flexible building material that can be curled into a roll to resist the infiltration of external rainwater and groundwater. As a leak-proof connection between the engineering foundation and the building, the waterproofing membrane is the first barrier of the entire engineering waterproofing and plays a crucial role in the entire project.

[0003] Self-adhesive waterproofing membranes are generally prepared from SBS and other synthetic rubbers, tackifiers and high-quality road asphalt as a base material, high-density polyethylene film or aluminum foil as the upper surface material, and peelable silicon-coated release paper as the lower surface anti-adhesion release layer. The self-adhesive waterproofing membrane has the elasticity of rubber, good elongation, excellent adhesion to the base layer, and can well adapt to the deformation and cracking of the base layer. It has good acid, alkali and chemical corrosion resistance and is a new type of waterproofing membrane. In engineering construction, the self-adhesive waterproofing membrane meets the requirements of modern safety and environmental protection. When used, it does not need to be heated, has no odor, no volatile organic substances, no pollution to the environment, and does not require special equipment, is easy to use, has less labor intensity compared with other roofing waterproofing materials, and only needs to be laid on the treated base surface, the release film is then torn off, and the self-adhesive waterproofing membrane is then adhered to the base surface. Then, the same method is used for laying, end lapping and jointing according to the product requirements.

[0004] In the construction process of self-adhesive waterproofing membranes for external walls, a layer of mortar needs to be coated on the outside of the self-adhesive waterproofing membrane after it is laid on the wall surface to prevent damage caused by external forces and affect the waterproofing effect. In order to reduce the construction difficulty and the overall aesthetic appearance of the building, a sand-faced self-adhesive waterproofing membrane is generally used. Patent No. CN107642172B discloses a self-adhesive waterproofing membrane. The patent mentions that the adhesive surface of the self-adhesive waterproofing membrane has reduced cohesion under solar radiation, and the peel strength of the cement mortar is reduced, which cannot achieve the waterproofing effect required by the national standard. Therefore, the self-adhesive waterproofing membrane is provided with a light-cured hot melt adhesive layer. The light-cured hot melt adhesive layer can absorb ultraviolet rays from sunlight during use, causing the components in the light-cured hot melt adhesive layer to undergo crosslinking reactions, thereby improving the cohesion.

[0005] However, in some cold regions, the presence of the light-cured hot melt adhesive layer can reduce the elasticity and softness of the self-adhesive waterproofing membrane, which is not conducive to the spreading of the self-adhesive waterproofing membrane. In addition, the light-cured hot melt adhesive can be hardened quickly during the bonding process due to the cold, which ultimately reduces the peel strength of the self-adhesive waterproofing membrane. SUMMARY

[0006] The application aims to provide a production process of a high-adhesion self-adhesive waterproof roll for wall surfaces to solve the problems in the background art.

[0007] The application can achieve the above-mentioned purpose by the following technical scheme.

[0008] The production process of the high-adhesion self-adhesive waterproof roll for wall surfaces comprises the following steps,

[0009] Step 1: Unwind the HDPE film, then coat the hot melt adhesive melt on the surface of the HDPE film, spread the reactive sand on the surface of the hot melt adhesive melt, roll and bond, then solidify with ultraviolet light to prepare a sand belt with a sand layer and a hot melt adhesive layer, and wind up for standby;

[0010] Step 2: Unwind the sand belt, coat the self-adhesive glue on one side of the sand layer of the HDPE film raw material, complete the processing of the self-adhesive glue layer, then cover the release paper on the side of the self-adhesive glue layer away from the HDPE film to obtain the high-adhesion self-adhesive waterproof roll for wall surfaces.

[0011] Further, the thickness of the sand layer is 0.5-2 mm; the thickness of the hot melt adhesive layer is 0.5-2 mm; the thickness of the HDPE film is 0.5-1 mm; and the thickness of the self-adhesive glue layer is 0.1-1.5 mm.

[0012] The hot melt adhesive melt is prepared by the following steps:

[0013] Step 1: Put polybutylene glycol with a molecular weight of 2000 into a flask, heat to completely melt, vacuum dry at 120℃ for 30 min, then add isophorone diisocyanate, toluene diisocyanate and dibutyltin dilaurate into the flask, react under nitrogen protection and at 80-90℃ for 1.5-2 h, reduce the temperature of the reaction system to 75℃, add ethylene glycol into the reaction system and stir quickly for 15-20 min, then add calcium carbonate powder and stir for 15-30 min to obtain a reaction type polyurethane elastomer;

[0014] Step 2: Add polyphenyl ether and chlorobenzene into the flask, stir until the polyphenyl ether is completely dissolved, then add azobisisobutyronitrile and N-bromosuccinimide into the flask, reflux under nitrogen protection for 4 h, after the reaction is completed, the product is precipitated with anhydrous ethanol, then the product is dried and crushed, dissolved with chloroform and filtered, remove the insoluble impurities, then precipitate with anhydrous ethanol again, dry, and after the purification operation is completed, brominated polyphenyl ether is obtained; the brominated polyphenyl ether is dissolved with N-methylpyrrolidone, then trimethylamine is added and reacted at 60℃ for 12 h to obtain quaternary ammonium polyphenyl ether.

[0015] Step 3: melt blend styrene-isoprene-styrene block copolymer, quaternary ammonium polyphenyl ether, reactive polyurethane elastomer, copolyether elastomer, hydrogenated petroleum resin, photoinitiator and antioxidant in a mixing machine to obtain a hot melt adhesive melt.

[0016] Further, the amount ratio of polybutylene glycol, isophorone diisocyanate, toluene diisocyanate, dibutyl tin dilaurate, ethylene glycol and calcium carbonate powder is 100g:40-45g:30-35g:0.1-0.3g:6-8mL:1.5-3.2g.

[0017] Further, the amount ratio of polyphenyl ether, chlorobenzene, azobis isobutyronitrile and N-bromosuccinimide is 6g:60mL:0.25g:9.8g.

[0018] Further, the amount ratio of brominated polyphenyl ether, N-methyl pyrrolidone and trimethylamine is 3g:10mL:6mL.

[0019] Further, the type of photoinitiator is 1173 or 2595.

[0020] Further, the antioxidant is one or more of antioxidant 801, antioxidant 1010 and antioxidant 1330 mixed in any ratio.

[0021] Further, the amount ratio of styrene-isoprene-styrene block copolymer, quaternary ammonium polyphenyl ether, reactive polyurethane elastomer, copolyether elastomer, hydrogenated petroleum resin, photoinitiator and antioxidant is 4-4.5kg:0.25-0.5kg:2-4kg:0.2-0.5kg:1-1.8kg:0.03-0.1kg:0.05-0.1kg.

[0022] Further, the copolyether elastomer is prepared by the following steps:

[0023] Step 1) add toluene and diphenyl sulfoxide to a flask at 20-30℃, stir at 300-500r / min until the dimethyl sulfoxide is dissolved, then add a 10% mass fraction of boron trifluoride ether solution to the flask, continue stirring for 30-40min, extract with n-hexane 2-3 times to obtain a dark brown complex as an initiator;

[0024] Step 2) add tetrahydrofuran, epichlorohydrin and glycidyl methyl ether to the flask, stir at 200-300r / min for 2-5min, then slowly add the initiator to the flask, react at 25℃ for 7-9h, then add a 1% mass fraction of potassium hydroxide solution and acetone to the flask, heat to 50℃ and react for 30min, then extract the reaction product with deionized water to obtain the copolyether elastomer.

[0025] Further, the toluene, diphenyl sulfoxide and boron trifluoride diethyl ether solution are used in a ratio of 20 mL:2 g:45 mL.

[0026] Further, the tetrahydrofuran, epichlorohydrin, glycidyl methyl ether, initiator, potassium hydroxide solution and acetone are used in a ratio of 50 g:40 g:10 g:1 g.

[0027] Advantages of the present application:

[0028] The wall high-adhesion self-adhesive waterproof roll material comprises a sand layer, a hot melt adhesive layer, an HDPE film, a self-adhesive layer and a release paper. In production, the hot melt adhesive melt is coated on the HDPE film, and then the sand belt is prepared by laying the reaction sand, so as to avoid overflow of the self-adhesive in the roll pressing process, embed the reaction sand in the hot melt adhesive layer, and facilitate the smooth production.

[0029] Under the ultraviolet light irradiation, the photoinitiator releases free radicals, the styrene-isoprene-styrene block copolymer in the hot melt adhesive melt is cross-linked and polymerized, and the cohesive force is enhanced, which is beneficial to increase the peel strength of the hot melt adhesive layer and the reaction sand. The styrene-isoprene-styrene block copolymer can fuse the copolyether elastomer and the reactive polyurethane elastomer. The copolyether elastomer and the reactive polyurethane elastomer are beneficial to increase the softness of the hot melt adhesive melt and reduce the glass transition temperature, which is beneficial to reduce the construction temperature of the hot melt adhesive melt, save energy consumption, speed up the production, and facilitate the use in cold environment. The reactive polyurethane elastomer is beneficial to increase the initial adhesion of the hot melt adhesive melt, and can further bond the reaction sand firmly after cooling and solidification. The quaternary ammonium polyphenyl ether can increase the hydrophilicity of the hot melt adhesive layer, and is beneficial to combine the moisture in the air. In the use process of the wall high-adhesion self-adhesive waterproof roll material, the quaternary ammonium polyphenyl ether can quickly capture the moisture in the air, the isocyanate groups in the hot melt adhesive layer combine with the moisture in the air to produce cross-linking and solidification, which is beneficial to increase the cohesive force and firmly bond the reaction sand, and prevent the sand layer from falling off in the use process. DETAILED DESCRIPTION

[0030] The technical solutions in the embodiments of the present application will be clearly and completely described below in combination with the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0031] Embodiment 1

[0032] The hot melt adhesive melt is prepared, including the following steps:

[0033] Step 1: 200 mL of toluene and 20 g of diphenyl sulfoxide were added to a flask, and stirred at 300 r / min until the dimethyl sulfoxide was dissolved. Then 450 mL of 10% by mass of boron trifluoride ether solution was added to the flask, and stirring was continued for 30 min. The product was extracted with n-hexane twice to obtain a dark brown complex as an initiator.

[0034] Step 2: 500 g of tetrahydrofuran, 400 g of epichlorohydrin, and 100 g of glycidyl methyl ether were added to a flask, and stirred at 200 r / min for 2 min. Then 10 g of the initiator was slowly added to the flask, and reacted at 25°C for 7 h. After that, 1% by mass of potassium hydroxide solution and acetone were added to the flask, and the temperature was raised to 50°C for 30 min. The reaction product was extracted with deionized water to obtain a copolyether elastomer.

[0035] Step 3: 10 kg of polybutylene glycol with a molecular weight of 2000 was added to a flask and heated to completely melt. Then the flask was vacuum dried at 120°C for 30 min. After that, 4 kg of isophorone diisocyanate, 3 kg of toluene diisocyanate, and 10 g of dibutyltin dilaurate were added to the flask, and reacted at 80°C for 1.5 h under nitrogen protection. The temperature of the reaction system was reduced to 75°C, 600 mL of ethylene glycol was added to the reaction system, and stirred quickly for 15 min. Then 150 g of calcium carbonate powder was added and stirred for 15 min to obtain a reaction-type polyurethane elastomer.

[0036] Step 4: 6 kg of polyphenyl ether and 60 L of chlorobenzene were added to a flask, and stirred until the polyphenyl ether was completely dissolved. Then 0.25 kg of azobisisobutyronitrile and 9.8 kg of N-bromosuccinimide were added to the flask, and refluxed for 4 h under nitrogen protection. After the reaction was completed, the product was precipitated with anhydrous ethanol, and then dried, crushed, dissolved with chloroform, and filtered. The insoluble impurities were removed, and then the product was precipitated with anhydrous ethanol again, and dried to obtain brominated polyphenyl ether. 3 kg of the brominated polyphenyl ether was dissolved with 10 L of N-methyl pyrrolidone, and then 6 L of trimethylamine was added and reacted at 60°C for 12 h to obtain a quaternary ammonium polyphenyl ether.

[0037] Step 5: 4 kg of styrene-isoprene-styrene block copolymer, 0.25 kg of quaternary ammonium polyphenyl ether, 2-4 kg of reaction-type polyurethane elastomer, 0.2 kg of copolyether elastomer, 1 kg of hydrogenated petroleum resin, 0.03 kg of photoinitiator 2595, and 0.05 kg of antioxidant 801 were added to a mixing machine for melt blending to obtain a hot melt adhesive melt.

[0038] Example 2

[0039] The hot melt adhesive melt was prepared, including the following steps:

[0040] Step 1: 200 mL of toluene and 20 g of diphenyl sulfoxide were added to a flask, and stirred at 300-500 r / min until the dimethyl sulfoxide was dissolved. Then 450 mL of 10% by mass of boron trifluoride ether solution was added to the flask, and stirring was continued for 35 min. The dark brown complex was extracted with n-hexane twice to obtain an initiator.

[0041] Step 2: 500 g of tetrahydrofuran, 400 g of epichlorohydrin and 100 g of glycidyl methyl ether were added to a flask, and stirred at 250 r / min for 3 min. Then 10 g of the initiator was slowly added to the flask, and reacted at 25°C for 8 h. After that, 1% by mass of potassium hydroxide solution and acetone were added to the flask, and the temperature was raised to 50°C for 30 min. The reaction product was extracted with deionized water to obtain a copolyether elastomer.

[0042] Step 3: 10 kg of polybutylene glycol with a molecular weight of 2000 was added to a flask and heated to completely melt. Then the flask was vacuum dried at 120°C for 30 min. After that, 4-4.5 kg of isophorone diisocyanate, 3.2 kg of toluene diisocyanate and 20 g of dibutyltin dilaurate were added to the flask, and reacted at 85°C for 1.5-2 h under nitrogen protection. The temperature of the reaction system was reduced to 75°C, 700 mL of ethylene glycol was added to the reaction system and stirred rapidly for 18 min. Then 220 g of calcium carbonate powder was added and stirred for 20 min to obtain a reaction-type polyurethane elastomer.

[0043] Step 4: 6 kg of polyphenyl ether and 60 L of chlorobenzene were added to a flask, and stirred until the polyphenyl ether was completely dissolved. Then 0.25 kg of azobisisobutyronitrile and 9.8 kg of N-bromosuccinimide were added to the flask, and refluxed for 4 h under nitrogen protection. After the reaction was completed, the product was precipitated with anhydrous ethanol, and then dried, crushed, dissolved with chloroform and filtered. The insoluble impurities were removed, and then the product was precipitated with anhydrous ethanol again, and dried to obtain brominated polyphenyl ether. 3 kg of the brominated polyphenyl ether was dissolved in 10 L of N-methyl pyrrolidone, and then 6 L of trimethylamine was added and reacted at 60°C for 12 h to obtain a quaternary ammonium polyphenyl ether.

[0044] Step 5: 4.2 kg of styrene-isoprene-styrene block copolymer, 0.35 kg of quaternary ammonium polyphenyl ether, 3 kg of reaction-type polyurethane elastomer, 0.3 kg of copolyether elastomer, 1.4 kg of hydrogenated petroleum resin, 0.06 kg of photoinitiator 1173 and 0.08 kg of antioxidant 1010 were added to a mixing machine for melt blending to obtain a hot melt adhesive melt.

[0045] Example 3

[0046] The hot melt adhesive melt was prepared, including the following steps:

[0047] Step 1: 200 mL of toluene and 20 g of diphenyl sulfoxide were added to a flask, and stirred at 300-500 r / min until the dimethyl sulfoxide was dissolved. Then 450 mL of 10% by mass boron trifluoride ether solution was added to the flask, and stirring was continued for 40 min. The dark brown complex was extracted with n-hexane three times to obtain an initiator.

[0048] Step 2: 500 g of tetrahydrofuran, 400 g of epichlorohydrin and 100 g of glycidyl methyl ether were added to a flask, and stirred at 300 r / min for 5 min. Then 10 g of initiator was slowly added to the flask, and reacted at 25°C for 9 h. After that, 1% by mass potassium hydroxide solution and acetone were added to the flask, and the temperature was raised to 50°C for 30 min. The reaction product was extracted with deionized water to obtain a copolyether elastomer.

[0049] Step 3: 10 kg of polybutylene glycol with a molecular weight of 2000 was added to a flask and heated to completely melt. Then the flask was vacuum dried at 120°C for 30 min. After that, 4.5 kg of isophorone diisocyanate, 3.5 kg of toluene diisocyanate and 30 g of dibutyltin dilaurate were added to the flask, and reacted at 90°C for 2 h under nitrogen protection. The temperature of the reaction system was reduced to 75°C, 800 mL of ethylene glycol was added to the reaction system and stirred rapidly for 20 min. Then 320 g of calcium carbonate powder was added and stirred for 30 min to obtain a reaction type polyurethane elastomer.

[0050] Step 4: 6 kg of polyphenyl ether and 60 L of chlorobenzene were added to a flask, and stirred until the polyphenyl ether was completely dissolved. Then 0.25 kg of azobisisobutyronitrile and 9.8 kg of N-bromosuccinimide were added to the flask, and refluxed for 4 h under nitrogen protection. After the reaction was completed, the product was precipitated with anhydrous ethanol, and then dried, crushed, dissolved in chloroform and filtered. The insoluble impurities were removed, and then precipitated with anhydrous ethanol again, and dried to obtain brominated polyphenyl ether. 3 kg of brominated polyphenyl ether was dissolved in 10 L of N-methyl pyrrolidone, and then 6 L of trimethylamine was added and reacted at 60°C for 12 h to obtain a quaternary ammonium polyphenyl ether.

[0051] Step 5: 4.5 kg of styrene-isoprene-styrene block copolymer, 0.5 kg of quaternary ammonium polyphenyl ether, 4 kg of reaction type polyurethane elastomer, 0.5 kg of copolyether elastomer, 1.8 kg of hydrogenated petroleum resin, 0.1 kg of photoinitiator 1173 and 0.1 kg of antioxidant 1330 were added to a mixing machine for melt blending to obtain a hot melt adhesive melt.

[0052] Example 4

[0053] A high-adhesion self-adhesive waterproof coiled material for walls was prepared, including the following steps:

[0054] Step one: HDPE film is unwound, and then the hot melt adhesive melt prepared in Example 1 is coated on the surface of the HDPE film, the reaction sand is paved on the surface of the hot melt adhesive melt, and after rolling and bonding, it is cured with ultraviolet light to prepare a sand belt with sand layer and hot melt adhesive layer, which is wound for standby use;

[0055] Step two: the sand belt is unwound, and the self-adhesive is coated on one side of the sand layer of the HDPE film raw material, the processing of the self-adhesive layer is completed, and then the release paper is covered on the side of the self-adhesive layer away from the HDPE film to obtain the high-adhesion self-adhesive waterproof roll for wall surface.

[0056] Among them, the thickness of the sand layer is 0.5mm; the thickness of the hot melt adhesive layer is 0.5mm; the thickness of the HDPE film is 0.5mm; and the thickness of the self-adhesive layer is 0.1mm.

[0057] Example 5

[0058] Preparation of high-adhesion self-adhesive waterproof roll for wall surface includes the following steps:

[0059] Step one: HDPE film is unwound, and then the hot melt adhesive melt prepared in Example 2 is coated on the surface of the HDPE film, the reaction sand is paved on the surface of the hot melt adhesive melt, and after rolling and bonding, it is cured with ultraviolet light to prepare a sand belt with sand layer and hot melt adhesive layer, which is wound for standby use;

[0060] Step two: the sand belt is unwound, and the self-adhesive is coated on one side of the sand layer of the HDPE film raw material, the processing of the self-adhesive layer is completed, and then the release paper is covered on the side of the self-adhesive layer away from the HDPE film to obtain the high-adhesion self-adhesive waterproof roll for wall surface.

[0061] Among them, the thickness of the sand layer is 1mm; the thickness of the hot melt adhesive layer is 1mm; the thickness of the HDPE film is 0.8mm; and the thickness of the self-adhesive layer is 1mm.

[0062] Example 6

[0063] Preparation of high-adhesion self-adhesive waterproof roll for wall surface includes the following steps:

[0064] Step one: HDPE film is unwound, and then the hot melt adhesive melt prepared in Example 3 is coated on the surface of the HDPE film, the reaction sand is paved on the surface of the hot melt adhesive melt, and after rolling and bonding, it is cured with ultraviolet light to prepare a sand belt with sand layer and hot melt adhesive layer, which is wound for standby use;

[0065] Step two: the sand belt is unwound, and the self-adhesive is coated on one side of the sand layer of the HDPE film raw material, the processing of the self-adhesive layer is completed, and then the release paper is covered on the side of the self-adhesive layer away from the HDPE film to obtain the high-adhesion self-adhesive waterproof roll for wall surface.

[0066] The thickness of the sand layer is 2 mm; the thickness of the hot melt adhesive layer is 2 mm; the thickness of the HDPE film is 1 mm; and the thickness of the self-adhesive layer is 1.5 mm.

[0067] Comparative Example 1: On the basis of Example 3, no reactive polyurethane elastomer is added, and the remaining steps remain unchanged to prepare a hot melt adhesive melt, and then a high-adhesion self-adhesive waterproof roll for walls is prepared according to the method of Example 6.

[0068] Comparative Example 2: On the basis of Example 3, no copolyether elastomer is added, and the remaining steps remain unchanged to prepare a hot melt adhesive melt, and then a high-adhesion self-adhesive waterproof roll for walls is prepared according to the method of Example 6.

[0069] Comparative Example 3: On the basis of Example 3, no quaternized polyphenyl ether is added, and the remaining steps remain unchanged to prepare a hot melt adhesive melt, and then a high-adhesion self-adhesive waterproof roll for walls is prepared according to the method of Example 6.

[0070] The above-mentioned reaction sand is purchased from Zhenjiang Hualong Color Sand Factory. The self-adhesive includes components by mass fraction: 70# asphalt petroleum 45 parts, styrene-isoprene-styrene block copolymer 8 parts, hydrogenated petroleum resin 5 parts, polyisobutylene 4 parts, naphthenic oil 10 parts, and calcium carbonate powder 10 parts.

[0071] The hot melt adhesive melt of each group of waterproof rolls in Example 4-Example 6 and Comparative Example 1-Comparative Example 3 is tested for performance. The peel strength test is performed according to GB / T 2791-1995 “Adhesive T Peel Strength Test Method”; the viscosity test is performed according to HG / T 3660-1999 “Determination of the Melt Viscosity of Hot Melt Adhesive”; the hot melt adhesive melt is filled in a 10 mm x 10 mm x 10 mm mold, and the complete curing time is recorded; then the low-temperature bending test is performed on each group of waterproof rolls in Example 4-Example 6 and Comparative Example 1-Comparative Example 3, two 100 mm x 50 mm samples are taken from each group, the sand layer is outward, the 50 mm edge is overlapped, the distance between the upper and lower plates of the bending instrument is adjusted to three times the thickness of the measured roll, then the upper and lower plates of the bending instrument are opened, two samples in the same direction are placed on the lower plate of the bending instrument, the overlapped edge is towards the pivot and aligned with the scale line, then the whole is placed in a low-temperature box, and kept at -25℃ and -40℃ for 1 h, then the upper plate is lowered to the adjusted position within 1 s, and kept for 1 s, then the sample is taken out, and after recovering to room temperature, the sample is observed for cracks at the bending position, and if there is no crack, it is qualified, otherwise it is unqualified. The results are shown in Table 1:

[0072] Table 1

[0073]

[0074]

[0075] As can be seen from Table 1, the hot melt adhesive melt used in Examples 4-5 has a higher viscosity, and the time required for complete curing is longer in Comparative Example 3 where the quaternary ammonium polyphenyl ether is not added, and the low-temperature bending performance of the waterproofing membrane in Examples 4-6 is better.

[0076] It is to be understood that the terminology used herein such as the terms "comprise", "comprising", or any other variant thereof is open, and that the terms are intended to encompass both the presence of stated elements as well as the presence of additional elements not specifically listed. It is also to be understood that the terminology "or" as used herein is used to link a list of elements, for example, A or B, and is not, however, intended to exclude more than one of the elements, for example, A and B.

[0077] While the embodiments of the application have been shown and described, it is to be understood that the application is not limited to these embodiments and that modifications, changes, substitutions and variations can be made without departing from the spirit and scope of the application, which is defined solely by the appended claims and their equivalents.

Claims

1. A process for the production of a high tack self-adhering waterproofing membrane for walls, characterized in that, Comprising the following steps: The hot melt adhesive melt is coated on the surface of the HDPE film, and then the reaction sand is paved on the surface of the hot melt adhesive melt, and after rolling and bonding, it is cured by ultraviolet light to prepare a sand belt with sand layer and hot melt adhesive layer; the self-adhesive layer is processed by coating self-adhesive on one side of the HDPE film raw material sand layer, and then the isolation paper is covered on the side of the self-adhesive layer away from the HDPE film to obtain the high-adhesion self-adhesive waterproof coiled material for wall surface; The hot melt adhesive melt is prepared by the following steps: Step one: polybutylene glycol is added to a flask and heated and melted and dried, isophorone diisocyanate, toluene diisocyanate and dibutyltin dilaurate are added to the flask, and the reaction is carried out under the conditions of nitrogen protection and 80-90℃ for 1.5-2h, the temperature is lowered to 75℃, ethylene glycol is added and stirred for 15-20min, then calcium carbonate powder is added and stirred for 15-30min to obtain a reaction type polyurethane elastomer; Step two: styrene-isoprene-styrene block copolymer, quaternary ammonium polyphenyl ether, reaction type polyurethane elastomer, copolyether elastomer, hydrogenated petroleum resin, photoinitiator and antioxidant are added to a mixing machine for melt blending to obtain a hot melt adhesive melt; The quaternary ammonium polyphenyl ether is prepared by the following steps: Polyphenyl ether and chlorobenzene are added to a flask and stirred to dissolve, azobisisobutyronitrile and N-bromosuccinimide are added to the flask, and the reaction is carried out under reflux for 4h under nitrogen protection, the product is dried after precipitation, and the product is crushed and purified to obtain brominated polyphenyl ether; the brominated polyphenyl ether is dissolved in N-methyl pyrrolidone, and then trimethylamine is added and the reaction is carried out at 60℃ for 12h to obtain quaternary ammonium polyphenyl ether; The copolyether elastomer is prepared by the following steps: Tetrahydrofuran, epichlorohydrin and glycidyl methyl ether are added to a flask and stirred for 2-5min, an initiator is added to the flask and the reaction is carried out at 25℃ for 7-9h, then potassium hydroxide solution and acetone are added to the flask and the temperature is raised to 50℃ for 30min, and the liquid is separated and extracted to obtain the copolyether elastomer.

2. The production process of a high-adhesion self-adhered waterproofing membrane for walls according to claim 1, characterized in that, The thickness of the sand layer is 0.5-2mm; the thickness of the hot melt adhesive layer is 0.5-2mm; the thickness of the self-adhesive layer is 0.1-1.5mm.

3. The production process of a high-adhesion self-adhered waterproofing membrane for walls according to claim 1, characterized in that, The amount ratio of the polybutylene glycol, isophorone diisocyanate, toluene diisocyanate, dibutyltin dilaurate, ethylene glycol and calcium carbonate powder in step one is 100g:40-45g:30-35g:0.1-0.3g:6-8mL:1.5-3.2g.

4. The production process of a high-adhesion self-adhered waterproofing membrane for walls according to claim 1, characterized in that, The amount ratio of the polyphenyl ether, chlorobenzene, azobisisobutyronitrile and N-bromosuccinimide is 6g:60mL:0.25g:9.8g.

5. The production process of a high-tack self-adhered waterproofing membrane for walls according to claim 1, characterized in that, The amount ratio of the brominated polyphenyl ether, N-methyl pyrrolidone and trimethylamine is 3g:10mL:6mL.

6. The production process of a high-tack self-adhered waterproofing membrane for walls according to claim 1, characterized in that, The amount ratio of the styrene-isoprene-styrene block copolymer, quaternary ammonium polyphenyl ether, reaction type polyurethane elastomer, copolyether elastomer, hydrogenated petroleum resin, photoinitiator and antioxidant is 4-4.5kg:0.25-0.5kg:2-4kg:0.2-0.5kg:1-1.8kg:0.03-0.1kg:0.05-0.1kg.

7. The production process of a high-tack self-adhered waterproofing membrane for walls according to claim 1, characterized in that, The initiator is prepared by the following steps: At 20-30℃, toluene and diphenyl sulfoxide are added to a flask and stirred to dissolve, boron trifluoride ether solution is added to the flask and stirring is continued for 30-40 min, and after extraction with n-hexane, the initiator is obtained.

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