A high-viscosity anti-shedding waterproof coiled material and its preparation method

Abstract

The present invention relates to the technical field of waterproofing membranes, and proposes a high-viscosity, anti-shedding waterproofing membrane and a preparation method thereof. The high-viscosity, anti-shedding waterproofing membrane comprises, from top to bottom, an anti-sticking protective layer, a base layer, an adhesive layer, and a separator. The adhesive layer comprises the following components in parts by weight: 60-75 parts of polysulfide rubber, 10-15 parts of tackifying resin, 5-10 parts of tackifier, 20-30 parts of filler, 1-3 parts of vulcanizing agent, and 0.5-1.5 parts of antioxidant. The polysulfide rubber comprises a first polysulfide rubber and a second polysulfide rubber, the first polysulfide rubber and the second polysulfide rubber having different thiol group contents, and the mass ratio of the first polysulfide rubber to the second polysulfide rubber is 1:3-3:1. The above technical solution solves the problems of low long-term bonding strength, easy shedding, and low elongation retention of waterproofing membranes in related technologies.

Description

Technical Field

[0001] The present invention relates to the technical field of waterproof coiled materials, and in particular to a high-viscosity and anti-shedding waterproof coiled material and a preparation method thereof. Background Art

[0002] With the continuous development of modern construction projects, the performance requirements for waterproof membranes are increasing. Among many building materials, waterproof membranes play a vital role. They can effectively prevent moisture penetration and protect the structural safety and service life of buildings. However, traditional waterproof membranes often have some problems in practical applications. On the one hand, the bonding strength is insufficient and they are prone to falling off during use. Especially in complex construction environments and long-term use, affected by factors such as temperature changes and deformation of the base layer, the bonding force between the waterproof membrane and the base layer gradually weakens, resulting in a significant reduction in the waterproof effect. On the other hand, the elongation retention rate of traditional waterproof membranes is limited, making it difficult to adapt to the deformation of buildings caused by thermal expansion and contraction, and they are prone to cracking and other problems, thereby destroying the integrity of the waterproof system. Therefore, it is urgent to develop a long-lasting, high-adhesion, anti-falling, and high elongation retention waterproof membrane. Summary of the Invention

[0003] The present invention provides a high-viscosity and anti-shedding waterproof coiled material and a preparation method thereof, which solves the problems of low long-term bonding strength, easy shedding, and low elongation retention of waterproof coiled materials in the related art.

[0004] The technical solution of the present invention is as follows: The present invention provides a high-viscosity anti-shedding waterproof membrane, which comprises, from top to bottom, an anti-sticking protective layer, a base layer, an adhesive layer, and a separator. The adhesive layer comprises the following components in parts by weight: 60-75 parts of polysulfide rubber, 10-15 parts of tackifying resin, 5-10 parts of tackifier, 20-30 parts of filler, 1-3 parts of vulcanizing agent, and 0.5-1.5 parts of antioxidant;

[0005] The polysulfide rubber includes a first polysulfide rubber and a second polysulfide rubber. The first polysulfide rubber and the second polysulfide rubber have different thiol group contents. The mass ratio of the first polysulfide rubber to the second polysulfide rubber is 1:3 to 3:1.

[0006] As a further technical solution, the thiol group content of the first polysulfide rubber is 1.1wt%~1.65wt%, the thiol group content of the second polysulfide rubber is 2.44wt%~2.87wt%, and the mass ratio of the first polysulfide rubber to the second polysulfide rubber is 1:1~2.

[0007] As a further technical solution, the raw materials also include butylpyrrolidone rubber, and the mass ratio of the butylpyrrolidone rubber to the polysulfide rubber is 2~3:6.

[0008] In the present invention, butylpyridine rubber is added and mixed with polysulfide rubber. The addition of butylpyridine rubber can form a synergistic effect with the polysulfide rubber, enhance the cohesive force of the adhesive layer and the adhesion to the substrate, and ensure that the bonding between the waterproof membrane and the base layer is long-term and effective. In addition, the butylpyridine rubber has good high-temperature resistance and flexibility, can avoid the waterproof membrane from cracking and leakage caused by temperature increase, and enhance the thermal aging elongation retention rate of the waterproof membrane.

[0009] As a further technical solution, the tackifying resin includes one or more of coumarone resin, petroleum resin, and rosin resin.

[0010] As a further technical solution, the tackifier includes one or both of naphthenic oil and paraffin oil.

[0011] As a further technical solution, the filler includes one or more of carbon black, calcium carbonate, and kaolin.

[0012] As a further technical solution, the vulcanizing agent includes one or more of dicumyl peroxide, benzoyl peroxide, and diisopropyl peroxydicarbonate.

[0013] As a further technical solution, the antioxidant includes one or more of antioxidant RD, antioxidant MB, and antioxidant AW.

[0014] As a further technical solution, the preparation method of the adhesive for the adhesive layer includes the following steps: weighing the raw materials, heating them, mixing and kneading them, and cooling them to obtain the adhesive for the adhesive layer.

[0015] The present invention also proposes a method for preparing a high-viscosity anti-shedding waterproof roll material, comprising the following steps: applying an adhesive on one side of a tire base layer to form an adhesive layer, arranging the anti-sticking protective layer, tire base layer, adhesive layer, and isolation film in sequence, and rolling them up after cooling and shaping them with a roller to obtain a high-viscosity anti-shedding waterproof roll material.

[0016] The working principle and beneficial effects of the present invention are:

[0017] In the present invention, polysulfide rubbers with different thiol group contents are added as raw materials to exert the synergistic effect of the two, thereby improving the compatibility and reactivity of the polysulfide rubber with other materials in the waterproof membrane, and improving the bonding force between the adhesive layer and the base layer of the waterproof membrane and other materials, so that the waterproof membrane can be more firmly adhered to the surface of the building, effectively preventing the membrane from shifting and falling off, and enhancing the long-term bonding strength of the waterproof membrane. DETAILED DESCRIPTION

[0018] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.

[0019] In the following examples and comparative examples:

[0020] First polysulfide rubber: thiol content is 1.1wt%~1.65wt%, model is JLY-115, average molecular weight is 5000, manufacturer is Huludao Keda Petrochemical Co., Ltd.

[0021] Second polysulfide rubber: thiol content 2.44wt%~2.87wt%, model JLY-1225, average molecular weight 2500, manufacturer Huludao Keda Petrochemical Co., Ltd.

[0022] Anti-stick protective layer: aluminum foil protective layer, thickness of 0.1mm;

[0023] Tire base: glass fiber base, thickness is 1mm;

[0024] Isolation film: polyethylene isolation film, thickness 0.1mm;

[0025] Adhesive layer: thickness 0.3mm;

[0026] Coumarone resin: model C120;

[0027] Petroleum resin: Model C9;

[0028] Rosin resin: Model 424.

[0029] Example 1

[0030] Preparation of adhesive for adhesive layer: 60 parts of polysulfide rubber, 10 parts of coumarone resin, 5 parts of naphthenic oil, 20 parts of carbon black, 1 part of dicumyl peroxide, and 0.5 parts of antioxidant RD were weighed and placed in a kneader, heated to 160°C and kneaded for 2 hours. After cooling, the adhesive for adhesive layer was obtained, wherein the 60 parts of polysulfide rubber included 40 parts of the first polysulfide rubber and 20 parts of the second polysulfide rubber;

[0031] A preparation method of a high-viscosity anti-shedding waterproof coiled material comprises the following steps: arranging an anti-sticking protective layer, a base layer, an adhesive layer, and an isolation film in sequence, cooling and shaping the coiled material with a roller, and then rolling the coiled material to obtain the high-viscosity anti-shedding waterproof coiled material.

[0032] Example 2

[0033] Preparation of adhesive for adhesive layer: 66 parts of polysulfide rubber, 12 parts of petroleum resin, 8 parts of naphthenic oil, 25 parts of calcium carbonate, 2 parts of benzoyl peroxide, and 1 part of antioxidant MB were weighed and placed in a kneader, heated to 170°C and kneaded for 1.5 hours, and then cooled to obtain the adhesive for adhesive layer, wherein the 66 parts of polysulfide rubber include 44 parts of the first polysulfide rubber and 22 parts of the second polysulfide rubber;

[0034] A preparation method of a high-viscosity anti-shedding waterproof coiled material comprises the following steps: arranging an anti-sticking protective layer, a base layer, an adhesive layer, and an isolation film in sequence, cooling and shaping the coiled material with a roller, and then rolling the coiled material to obtain the high-viscosity anti-shedding waterproof coiled material.

[0035] Example 3

[0036] Preparation of adhesive for adhesive layer: 75 parts of polysulfide rubber, 15 parts of rosin resin, 10 parts of paraffin oil, 30 parts of kaolin, 3 parts of diisopropyl peroxydicarbonate, and 1.5 parts of antioxidant AW are weighed and placed in a kneader, heated to 180°C and kneaded for 1 hour, and then cooled to obtain the adhesive for adhesive layer, wherein the 75 parts of polysulfide rubber include 50 parts of the first polysulfide rubber and 25 parts of the second polysulfide rubber;

[0037] A preparation method of a high-viscosity anti-shedding waterproof coiled material comprises the following steps: arranging an anti-sticking protective layer, a base layer, an adhesive layer, and an isolation film in sequence, cooling and shaping the coiled material with a roller, and then rolling the coiled material to obtain the high-viscosity anti-shedding waterproof coiled material.

[0038] Example 4

[0039] Compared with Example 1, Example 4 is different in that the 60 parts of polysulfide rubber include 30 parts of the first polysulfide rubber and 30 parts of the second polysulfide rubber.

[0040] Example 5

[0041] Compared with Example 1, Example 5 is different in that the 60 parts of polysulfide rubber include 20 parts of the first polysulfide rubber and 40 parts of the second polysulfide rubber.

[0042] Example 6

[0043] Compared with Example 1, Example 6 is different in that the 60 parts of polysulfide rubber include 10 parts of the first polysulfide rubber and 50 parts of the second polysulfide rubber.

[0044] Example 7

[0045] Compared with Example 5, the difference of Example 7 is that the preparation of the adhesive for the adhesive layer includes the following steps: weighing 60 parts of polysulfide rubber, 10 parts of coumarone resin, 5 parts of cyclohexane oil, 20 parts of carbon black, 1 part of diisopropylbenzene peroxide, 0.5 parts of antioxidant RD, and 10 parts of butylpyrrolidone rubber, placing them in a kneader, heating to 160°C and kneading for 2 hours, and then cooling to obtain the adhesive for the adhesive layer, wherein the 60 parts of polysulfide rubber include 40 parts of the first polysulfide rubber and 20 parts of the second polysulfide rubber.

[0046] Example 8

[0047] Compared with Example 7, the difference in Example 8 is that the amount of butylpyridine rubber added is 20 parts.

[0048] Example 9

[0049] Compared with Example 7, the difference in Example 9 is that the amount of butylpyridine rubber added is 30 parts.

[0050] Example 10

[0051] Compared with Example 7, the difference in Example 10 is that the amount of butylpyrrolidone rubber added is 40 parts.

[0052] Comparative Example 1

[0053] Compared with Example 1, Comparative Example 1 is different in that the 60 parts of polysulfide rubber include only the first polysulfide rubber.

[0054] Comparative Example 2

[0055] Compared with Example 1, Comparative Example 2 is different in that the 60 parts of polysulfide rubber only include the second polysulfide rubber.

[0056] The high-viscosity, anti-shedding waterproof membranes prepared in Examples 1 to 10 and Comparative Examples 1 to 2 were tested according to the following method:

[0057] 1. Adhesion: According to the adhesion test method specified in GB / T 35467-2017 "Wet-laid waterproof membrane", the adhesion of the sample is tested. The thickness of the sample is 1.6mm.

[0058] 2. Heat aging elongation retention rate: According to the test method for elongation at break specified in GB / T 328.9-2007 "Test methods for building waterproof membranes Part 9: Tensile properties of polymer waterproof membranes", the elongation of the sample at break was tested. The sample was placed horizontally in an oven at (80±2)°C for (168±2) h. After being taken out and placed at (23±2)°C for 24 h, the elongation at break after heat aging was tested. The heat aging elongation retention rate of the sample was calculated. The thickness of the sample was 1.6 mm. Heat aging elongation retention rate = (elongation after heat aging / elongation before heat aging) × 100%.

[0059] The test results are shown in the following table:

[0060] Table 1 Test results of the adhesiveness of the high-viscosity anti-shedding waterproof membranes prepared in Examples 1 to 10 and Comparative Examples 1 to 2

[0061]

[0062] Compared with Example 1, Comparative Example 1 added only the first polysulfide rubber, while Comparative Example 2 added only the second polysulfide rubber. The results showed that Example 1 had greater sustained adhesion than Comparative Examples 1 and 2, indicating that the first and second polysulfide rubbers synergistically enhance the long-term bond strength of the waterproof membrane. Compared with Example 1, Examples 4 to 6 added different mass ratios of the first and second polysulfide rubbers. The results showed that Examples 4 and 5 had greater sustained adhesion than Examples 1 and 6, indicating that a mass ratio of 1:1 to 2 between the first and second polysulfide rubbers yields superior long-term bond strength to the waterproof membrane.

[0063] Compared with Example 5, Examples 7 to 10 added butylpyridine rubber. As a result, the sustained adhesion of Examples 7 to 10 was greater than that of Example 5, indicating that the addition of butylpyridine rubber can enhance the long-term bond strength of the waterproof membrane. In Examples 7 to 10, different masses of butylpyridine rubber were added. As a result, the sustained adhesion of Examples 8 and 9 was greater than that of Examples 7 and 10, indicating that when the mass ratio of butylpyridine rubber to polysulfide rubber is 2 to 3:6, the long-term bond strength of the resulting waterproof membrane is better.

[0064] Table 2 Test results of thermal aging elongation retention of high-viscosity anti-shedding waterproof membranes prepared in Examples 5 and 7 to 10

[0065]

[0066] Compared with Example 5, Examples 7 to 10 added butylpyridine rubber. As a result, the longitudinal and transverse heat aging elongation retention rates of Examples 7 to 10 were greater than those of Example 5, indicating that the addition of butylpyridine rubber can enhance the heat aging elongation retention rate of the waterproof membrane. In Examples 7 to 10, different masses of butylpyridine rubber were added. As a result, the longitudinal and transverse heat aging elongation retention rates of Examples 8 and 9 were greater than those of Examples 7 and 10, indicating that when the mass ratio of butylpyridine rubber to polysulfide rubber is 2 to 3:6, the resulting waterproof membrane has a higher heat aging elongation retention rate.

[0067] The above are only preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A high-viscosity, anti-shedding waterproof membrane, characterized in that: The tire comprises, from top to bottom, an anti-sticking protective layer, a tire base layer, an adhesive layer, and a separator. The adhesive layer comprises the following components in parts by weight: 60-75 parts of polysulfide rubber, 10-15 parts of a tackifying resin, 5-10 parts of a tackifier, 20-30 parts of a filler, 1-3 parts of a vulcanizing agent, and 0.5-1.5 parts of an antioxidant. The polysulfide rubber comprises a first polysulfide rubber and a second polysulfide rubber, and the first polysulfide rubber and the second polysulfide rubber have different thiol group contents. The thiol group content of the first polysulfide rubber is 1.1 wt% to 1.65 wt%, the thiol group content of the second polysulfide rubber is 2.44 wt% to 2.87 wt%, and the mass ratio of the first polysulfide rubber to the second polysulfide rubber is 1:1 to 2; The tackifier is one or both of naphthenic oil and paraffin oil.

2. The high-viscosity anti-shedding waterproof membrane according to claim 1, characterized in that: The raw materials also include butyl pyridine rubber, and the mass ratio of the butyl pyridine rubber to the polysulfide rubber is 2-3:

6.

3. The high-viscosity anti-shedding waterproof membrane according to claim 1, characterized in that: The tackifying resin includes one or more of coumarone resin, petroleum resin, and rosin resin.

4. The high-viscosity anti-shedding waterproof membrane according to claim 1, characterized in that: The filler includes one or more of carbon black, calcium carbonate and kaolin.

5. The high-viscosity anti-shedding waterproof membrane according to claim 1, characterized in that: The vulcanizing agent includes one or more of dicumyl peroxide, benzoyl peroxide, and diisopropyl peroxydicarbonate.

6. The high-viscosity anti-shedding waterproof membrane according to claim 1, characterized in that: The antioxidant includes one or more of antioxidant RD, antioxidant MB, and antioxidant AW.

7. The high-viscosity anti-shedding waterproof membrane according to claim 1, characterized in that: The preparation method of the adhesive for the adhesive layer comprises the following steps: weighing the raw materials, heating them, mixing and kneading them, and cooling them to obtain the adhesive for the adhesive layer.

8. The method for preparing a high-viscosity anti-shedding waterproof coiled material according to any one of claims 1 to 7, characterized in that: The method comprises the following steps: applying adhesive on one side of the tire base layer to form an adhesive layer, arranging the anti-sticking protective layer, the tire base layer, the adhesive layer and the isolation film in sequence, cooling and shaping them with a roller and then rolling them up to obtain a high-viscosity, anti-shedding and waterproof roll material.

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