Modified asphalt coating material and preparation method thereof, and exposed flame-retardant waterproofing membrane
By using rock asphalt, chlorinated butyl rubber, desulfurization glue powder and flame retardant in the asphalt waterproof roll, a modified asphalt cover material is formed, which solves the problems of poor flame retardancy and aging of waterproof layer in the traditional asphalt waterproof roll material, and achieves a waterproof roll with high old resistance, adhesion and flame retardancy.
Patent Information
- Application Number
- CN202311874304.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-12-29
- Publication Date
- 2025-03-04
- Estimated Expiration
- 2043-12-29
AI Technical Summary
Traditional asphalt waterproof coils use a large amount of combustible polymers and flammable oil, which cannot achieve flame retardant effect. The surface materials of mineral particles are prone to fall off during use and construction, resulting in aging of the waterproof layer, poor low temperature flexibility and adhesion, and prone to water seepage.
A modified asphalt coating material is provided, through the coordinated cooperation of rock asphalt, chlorinated butyl rubber, desulfurization glue powder, and flame retardant, forming a coating with a combination of multi-component action, improving its old resistance, adhesive properties and flame retardant properties, so that the flame retardant reaches the requirements of B2.
The stable and old-age resistance and bonding properties of modified asphalt coating materials are achieved while improving flame retardant properties, so that the waterproof coil has a higher service life and better anti-viscosity and weather resistance.
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Figure BDA0004650812120000151
Abstract
Description
Technical Field
[0001] The present application belongs to the technical field of waterproof coiled materials, and specifically relates to a modified asphalt coating material and a preparation method thereof, and an exposed flame-retardant waterproof coiled material. Background Art
[0002] Traditional asphalt waterproofing membranes are mainly made of high-quality road asphalt as the main material, waste engine oil, line oil, rubber oil, etc. as softening oil, and high molecular polymers are modified. A large amount of flammable polymers and flammable oils are used, and the flame retardant effect cannot be achieved. In addition, when mineral granules are used as surface materials for exposed waterproofing membranes, the mineral sand is easy to fall off and be washed away by rain during use and construction, which is easy to block the drainage outlet. Its UV resistance fails, resulting in aging of the waterproof layer, making the low-temperature flexibility of the waterproof membrane worse, the adhesion worse, and it is easy to seep water. Summary of the invention
[0003] The embodiments of the present application provide a modified asphalt coating material and a preparation method thereof, and an exposed flame-retardant waterproof membrane, so as to stabilize the aging resistance and bonding performance while improving the flame retardant performance.
[0004] In the first aspect, an embodiment of the present application provides a modified asphalt coating, comprising the following raw material components in parts by weight: asphalt, 28-66 parts; rock asphalt, 3-10 parts; tackifier, 10-15 parts; SBS, 3-6 parts; chlorobutyl rubber, 2-5 parts; desulfurized rubber powder, 5-10 parts; silane coupling agent modified heavy calcium powder, 12-20 parts; and flame retardant, 5-15 parts.
[0005] According to an embodiment of the first aspect of the present application, the raw material components satisfy at least one of the following conditions:
[0006] (1) Based on the mass of the silane coupling agent modified heavy calcium powder, the mass fraction of the silane coupling agent is 1.5% to 5%;
[0007] (2) The degree of chlorination of chlorinated butyl rubber is 1.8% to 4.5%;
[0008] (3) SBS is a star-shaped SBS, wherein the mass ratio of styrene to butadiene is (2.8-3.5):(7.2-6.5), the melt index is ≤1, and the weight average molecular weight is 18-30W;
[0009] (4) The softening point of rock asphalt is 145-160°C, the needle penetration is less than 1, and the solubility is >96%.
[0010] According to an embodiment of the first aspect of the present application, the silane coupling agent modified heavy calcium powder comprises the following steps to prepare the obtained product, the steps comprising:
[0011] The heavy calcium powder is mixed with a solvent to obtain a suspension; stearic acid is added to the suspension, stirred and mixed, and then a silane coupling agent is added, stirred and mixed to obtain a mixed system; the mixed system is dried and ground to obtain a silane coupling agent-modified heavy calcium powder.
[0012] According to an embodiment of the first aspect of the present application, the raw material components satisfy at least one of the following conditions:
[0013] (1) The particle size of the rubber powder is 10-40 mm;
[0014] (2) The particle size of the silane coupling agent modified heavy calcium powder is 0.075 mm to 0.084 mm;
[0015] (3) The particle size of the flame retardant is 0.013 mm to 0.026 mm.
[0016] According to an embodiment of the first aspect of the present application, the tackifier includes one or more of rubber oil R9, environmentally friendly aromatic oil, butyl oleate, and trioctyl citrate.
[0017] According to an embodiment of the first aspect of the present application, the flame retardant includes one or more of magnesium hydroxide, aluminum hydroxide, decabromodiphenylethane, antimony trioxide, taurine, polyphosphates, and chlorinated polyethylene.
[0018] In a second aspect, the present application provides a method for preparing a modified asphalt coating, comprising the following steps:
[0019] Providing raw materials according to the raw material components and weight portions contained in the above-mentioned coating material;
[0020] Adding asphalt into a reaction container, and adding a tackifier into the reaction container during stirring to obtain a first mixture;
[0021] The SBS, the chlorinated butyl rubber, the rock asphalt and the first mixture are mixed and stirred to obtain a second mixture;
[0022] After the desulfurized rubber powder is mixed with the second mixture, fillers and flame retardants are added and mixed and stirred to obtain a modified asphalt coating material.
[0023] According to an embodiment of the first aspect of the present application, the silane coupling agent modified heavy calcium powder is prepared by the following method: mixing the heavy calcium powder with a solvent to obtain a suspension; adding stearic acid to the suspension and stirring and mixing, and then adding a silane coupling agent and stirring and mixing to obtain a mixed system; and drying and grinding the mixed system to obtain the silane coupling agent modified heavy calcium powder.
[0024] According to an embodiment of the first aspect of the present application, the step of obtaining the second mixture includes: mixing and stirring SBS, chlorinated butyl rubber, rock asphalt and the first mixture at a temperature of 130°C-180°C, and the mixing and stirring includes stirring at a low speed of 50-130 r / min for 5-15 minutes, and then stirring at a high speed of 400-800 r / min for 2.5h-3h.
[0025] In the third aspect, an embodiment of the present application provides an exposed flame-retardant waterproof membrane, comprising a main substrate layer, a coating layer covering both sides of the main substrate layer, a mineral particle layer covering at least one side of the coating layer, and an isolation protective layer covering the mineral particle layer; wherein the coating layer is formed by the modified asphalt coating material described above in the claim or by the modified asphalt coating material prepared by the above-mentioned preparation method.
[0026] According to an embodiment of the third aspect of the present application, the thickness of the isolation protection layer is 0.3-0.5 mm; and / or,
[0027] The isolation protection layer is formed by a polymer emulsion, and the polymer emulsion includes one or more of silane-modified acrylic emulsion, pure acrylic emulsion, and fluorocarbon emulsion.
[0028] Compared with the prior art, this application has at least the following beneficial effects:
[0029] The modified asphalt coating provided by the present application is a synergistic combination of rock asphalt, chlorinated butyl rubber, desulfurized rubber powder, and flame retardant. Under the joint action of multiple components, the aging resistance and bonding performance of the coating can be stabilized while improving the flame retardant performance, so that the flame retardancy reaches the B2 level requirement. Among them, rock asphalt provides high strength and aging resistance, modified butyl rubber can improve the inorganic material peeling strength and flame retardancy of asphalt coil, and desulfurized rubber powder has better active reaction, enhances the bonding performance of asphalt, and improves the weather resistance of asphalt. In addition, the Si-O alkyl in the heavy calcium powder modified by the silane coupling agent connects the asphalt and the inorganic mineral particles to form a chemical bond, increasing the adhesion between them, and at the same time improving the flame retardancy and adhesion of the waterproof coiled material prepared by the modified asphalt coating to the inorganic mineral particles. It has good energy-saving and environmental protection properties and is friendly to production workers and the social environment. DETAILED DESCRIPTION
[0030] In order to make the invention purpose, technical scheme and beneficial technical effect of the present application clearer, the present application is further described in detail below in conjunction with the embodiments. It should be understood that the embodiments described in this specification are only for explaining the present application, not for limiting the present application.
[0031] For simplicity, only some numerical ranges are explicitly disclosed herein. However, any lower limit can be combined with any upper limit to form an unambiguous range; and any lower limit can be combined with other lower limits to form an unambiguous range, and any upper limit can be combined with any other upper limit to form an unambiguous range. In addition, although not explicitly stated, each point or single value between the range endpoints is included in the range. Thus, each point or single value can be combined with any other point or single value as its own lower limit or upper limit or with other lower limits or upper limits to form an unambiguous range.
[0032] In the description herein, when a composition is described as containing, comprising or including specific components, or when a process is described as containing, comprising or including specific process steps, it is expected that the composition of the present application also consists essentially of or consists of the components, and the process of the present application also consists essentially of or consists of the process steps.
[0033] The use of the terms "including," "comprising," "containing," and "having" should generally be interpreted as open ended and non-limiting unless expressly stated otherwise.
[0034] In the description of this article, it should be noted that, unless otherwise specified, “above” and “below” are inclusive of the number itself, and the “multiple” in “one or more” means more than two.
[0035] The above-mentioned summary of the invention of the present application is not intended to describe each disclosed embodiment or each implementation in the present application. The following description more specifically illustrates exemplary embodiments. In many places throughout the application, guidance is provided by a series of examples, which can be used in various combinations. In each example, enumeration is only used as a representative group and should not be interpreted as exhaustive.
[0036] The inventors of this application noticed that the existing modified asphalt waterproof membrane uses a large amount of flammable polymers and flammable oils, which cannot achieve a flame retardant effect. In addition, when mineral particles are used as surface materials for exposed waterproof membranes, the mineral sand is easy to fall off and be washed away by rain during use and construction, which is easy to block the drain outlet. Its UV resistance fails, resulting in aging of the waterproof layer, making the low-temperature flexibility of the waterproof membrane worse, the adhesion worse, and prone to water seepage.
[0037] To this end, the inventors of the present application have conducted extensive research and provided a modified asphalt coating material and a preparation method thereof, and an exposed flame-retardant waterproof membrane, aiming to stabilize the aging resistance and bonding properties while improving the flame retardant properties.
[0038] Modified asphalt coating
[0039] In the first aspect, an embodiment of the present application provides a modified asphalt coating, comprising the following raw material components in parts by weight: asphalt, 28-66 parts; rock asphalt, 3-10 parts; tackifier, 10-15 parts; SBS, 3-6 parts; chlorobutyl rubber, 2-5 parts; desulfurized rubber powder, 5-10 parts; silane coupling agent modified heavy calcium powder, 12-20 parts; and flame retardant, 5-15 parts.
[0040] The modified asphalt coating provided in the embodiment of the present application is a synergistic combination of rock asphalt, SBS, chlorinated butyl rubber, desulfurized rubber powder, and flame retardant. The combined action of multiple components can achieve the goal of stabilizing the aging resistance and bonding properties of the coating while improving the flame retardancy, so that the flame retardancy reaches the B2 level requirement.
[0041] The asphalt in the embodiment of the present application is commonly used asphalt for roads, for example, the asphalt includes one of No. 70 (70#) asphalt and No. 90 (90#) asphalt or a mixture of the two. The asphalt has a softening point of 45-50°C at 26°C and a needle penetration of 65-100, and has excellent water resistance, aging resistance, chemical corrosion resistance and good bonding performance. Exemplarily, the weight proportions of asphalt are 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 53, 54, 55, 56, 57, 58, 59, 60, 61, 62, 63, 64, 65, 66, or a range consisting of any two of the above values. Flame retardants can improve flame retardant properties. Based on the weight proportion of asphalt being 28-66 parts, the weight proportion of flame retardants is 5-15 parts. Exemplarily, the weight proportion of flame retardants is 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts or a range consisting of any two of the above values.
[0042] The inventors of the present application have noticed in experiments that adding flame retardants to asphalt coatings can significantly improve the flame retardancy of waterproof membranes, but it has a significant impact on the bonding performance, weather resistance, and aging resistance. Therefore, the inventors of the present application have conducted a large number of experimental studies and added rock asphalt, chlorinated butyl rubber, desulfurized rubber powder and other components to the asphalt coating system to form a modified asphalt coating to improve its performance.
[0043] Rock asphalt provides high strength and anti-aging properties, and modified butyl rubber can improve the inorganic material peel strength and flame retardancy of asphalt coils. On the basis of 28-66 parts by weight of asphalt and 5-15 parts by weight of flame retardant, the weight of rock asphalt is 3-10 parts; illustratively, the weight of rock asphalt is 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts or a range consisting of any two of the above values.
[0044] Chlorobutyl rubber can improve the peel strength and flame retardancy between the asphalt coating and the inorganic material in the waterproofing membrane. Based on the weight percentage of asphalt and rock asphalt, the weight percentage of chlorobutyl rubber is 2-5 parts; illustratively, the weight percentage of chlorobutyl rubber is 2 parts, 3 parts, 4 parts, 5 parts or a range consisting of any two of the above values.
[0045] The desulfurized rubber powder has better active reaction, enhances the bonding performance of asphalt, and improves the weather resistance of the asphalt coating system. Based on the weight percentage of asphalt, rock asphalt and chlorobutyl rubber, the weight percentage of the desulfurized rubber powder is 5-10 parts; illustratively, the weight percentage of the desulfurized rubber powder is 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts or a range consisting of any two of the above values.
[0046] The inventors of the present application noticed in experiments that the synergistic combination of rock asphalt, chlorinated butyl rubber, desulfurized rubber powder and flame retardant, which cannot be balanced by a single component, can achieve the flame retardancy B2 level requirement without reducing the other properties of the waterproof membrane, thus meeting various construction requirements.
[0047] In addition, the embodiment of the present application introduces silane coupling agent modified heavy calcium powder into the modified asphalt coating. On the one hand, the modified asphalt coating can improve the strength of the coating. On the other hand, the Si-O alkyl in the silane coupling agent modified heavy calcium powder connects the asphalt and the inorganic mineral particles to form a chemical bond, increasing the adhesion between them, while improving the flame retardancy and adhesion of the waterproof roll formed by the modified asphalt coating to the inorganic mineral particles, with good energy conservation and environmental protection, and is friendly to production workers and the social environment. The weight proportion of the silane coupling agent modified heavy calcium powder is 12-20 parts; illustratively, the weight proportion of the silane coupling agent modified heavy calcium powder is 12 parts, 13 parts, 14 parts, 15 parts, 16 parts, 17 parts, 18 parts, 19 parts, 20 parts or a range consisting of any two of the above values.
[0048] SBS can significantly improve the initial adhesion of asphalt rolls and the bonding with mineral particles, effectively reducing the shedding of mineral particles. The weight percentage of SBS is 3-6 parts; for example, the weight percentage of SBS is 3 parts, 4 parts, 5 parts, 6 parts or a range consisting of any two of the above values.
[0049] In some embodiments, based on the mass of the silane coupling agent-modified heavy calcium powder, the mass fraction of the silane coupling agent is 1.5% to 5%. For example, the mass fraction of the silane coupling agent is 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, or a range consisting of any two of the above values.
[0050] In the embodiments of the present application, by adjusting the ratio of silane coupling agent to heavy calcium powder in the silane coupling agent modified heavy calcium powder within the above range, the silane coupling agent can be connected to the heavy calcium powder on one side, and can fully form chemical bonds with inorganic mineral particles on the other side, thereby increasing the adhesion between them, thereby improving the weather resistance and aging resistance of the waterproof membrane prepared by the modified asphalt coating.
[0051] In some embodiments, the chlorination degree of the chlorinated butyl rubber is 1.8% to 4.5%. For example, the mass fraction of the silane coupling agent is 1.8%, 2%, 2.2%, 2.5%, 2.8%, 3%, 3.2%, 3.5%, 3.8%, 4%, 4.2%, 4.5% or a range consisting of any two of the above values.
[0052] In the embodiments of the present application, by adjusting the chlorination degree of the chlorinated butyl rubber within the above range, the modified asphalt coating can have excellent adhesion, improve the flame retardancy of the modified asphalt coating, and increase its resistance to heat and oxygen aging.
[0053] In some embodiments, the SBS is a star-shaped SBS, wherein the mass ratio of styrene to butadiene is (2.8-3.5):(7.2-6.5), the melt index is ≤1, and the weight average molecular weight is 18-30W.
[0054] Illustratively, the star-shaped SBS has a total weight of 10 parts by weight, and the mass ratio of styrene to butadiene is 2.8:7.2, 3.0:7.0, 3.1:6.9, 3.2:6.8, 3.3:6.7, 3.4:6.6, 3.5:6.5 or a range consisting of any two of the above ratios.
[0055] Illustratively, the weight average molecular weight of the star-shaped SBS is 18W, 19W, 20W, 21W, 22W, 23W, 24W, 25W, 26W, 27W, 28W, 29W, 30W, or a range consisting of any two of the above values, for example, 18W represents 180,000.
[0056] In the embodiments of the present application, a suitable type of SBS is selected so that the SBS cooperates with other components of the modified asphalt coating material to achieve good initial adhesion.
[0057] In some embodiments, the rock asphalt has a softening point of 145-160° C., a needle penetration of less than 1, and a solubility of >96%.
[0058] Exemplarily, the softening point of rock asphalt is 145°C, 146°C, 147°C, 148°C, 149°C, 150°C, 151°C, 152°C, 153°C, 154°C, 155°C, 156°C, 157°C, 158°C, 159°C, 160°C or a range consisting of any two of the above values.
[0059] In the embodiments of the present application, rock asphalt with a suitable softening point is selected, which can be softened and mixed with other components of the modified asphalt coating at a suitable temperature.
[0060] In some embodiments, the silane coupling agent modified heavy calcium powder comprises the following steps to prepare the obtained product, the steps comprising:
[0061] The heavy calcium powder is mixed with a solvent to obtain a suspension; stearic acid is added to the suspension, stirred and mixed, and then a silane coupling agent is added, stirred and mixed to obtain a mixed system; the mixed system is dried and ground to obtain a silane coupling agent-modified heavy calcium powder.
[0062] The present application pre-treats the heavy calcium powder with stearic acid and then performs surface modification with a silane coupling agent, thereby improving the compatibility and dispersibility of the modified heavy calcium powder with asphalt, SBS, chlorobutyl rubber, and flame retardant, and forming a more stable combination between organic and inorganic substances through chemical bond connection; thereby improving the overall flame retardancy and initial adhesion of the modified asphalt coating.
[0063] In some embodiments, the particle size of the rubber powder is 10-40 mm. The desulfurized rubber powder can be recycled rubber powder obtained by desulfurizing waste rubber, wherein the waste rubber is ground and crushed at low temperature into rubber particles with a certain particle size, and then desulfurized with a high-temperature solvent to obtain recycled rubber powder. Desulfurized rubber powder reduces production waste gas emissions and is environmentally friendly.
[0064] In some embodiments, the particle size of the silane coupling agent modified heavy calcium powder is 0.075 mm to 0.084 mm.
[0065] In some embodiments, the particle size of the flame retardant is 0.013 mm to 0.026 mm.
[0066] The present application improves the performance of the modified asphalt coating by adjusting the particle size of each component within the above range. If the particle size is too small, it is easy to agglomerate. By adjusting the particle size of each component within the above range, it is beneficial to improve the stability and bonding performance of the modified asphalt coating.
[0067] In some embodiments, the tackifier includes one or more of base oil, rubber oil R9, environmentally friendly aromatic oil, butyl oleate, and trioctyl citrate, and the tackifier is used to adjust the viscosity of the modified asphalt coating system.
[0068] The base oil in the embodiments of the present application refers to the liquid component constituting the finished lubricating oil and grease.
[0069] In some embodiments, the flame retardant includes one or more of magnesium hydroxide, aluminum hydroxide, decabromodiphenylethane, antimony trioxide, taurine, polyphosphates, and chlorinated polyethylene.
[0070] Preparation method of modified asphalt coating material
[0071] In a second aspect, the present application provides a method for preparing a modified asphalt coating, comprising the following steps:
[0072] Providing raw materials according to the raw material components and weight portions contained in the above-mentioned coating material;
[0073] Adding asphalt into a reaction container, and adding a tackifier into the reaction container during stirring to obtain a first mixture;
[0074] The SBS, the chlorinated butyl rubber, the rock asphalt and the first mixture are mixed and stirred to obtain a second mixture;
[0075] After the desulfurized rubber powder is mixed with the second mixture, fillers and flame retardants are added and mixed and stirred to obtain a modified asphalt coating material.
[0076] The preparation method of the modified asphalt coating provided in the present application is simple and easy, has low requirements on equipment, is well compatible with existing processes, and has great potential for large-scale application.
[0077] In some embodiments, the silane coupling agent modified heavy calcium powder is prepared by: mixing the heavy calcium powder with a solvent to obtain a suspension; adding stearic acid to the suspension and stirring and mixing, and then adding a silane coupling agent and stirring and mixing to obtain a mixed system; and dry grinding the mixed system to obtain the silane coupling agent modified heavy calcium powder.
[0078] Adding asphalt into a reaction container and then adding a tackifier into the reaction container during stirring can make the asphalt and the tackifier mixed more evenly.
[0079] In the embodiment of the present application, the viscosity enhancer can be added to the reaction container containing asphalt in multiple times to improve the uniformity of the mixing process.
[0080] In some embodiments, the step of obtaining the second mixture includes: mixing SBS, chlorobutyl rubber, rock asphalt and the first mixture at a temperature of 130°C-180°C, and the mixing includes stirring at a low speed of 50-130 r / min for 5-15 min, and then stirring at a high speed of 400-800 r / min for 2.5h-3h. The main purpose of performing low-speed mixing and then high-speed mixing in the embodiment of the present application is to make SBS, chlorobutyl rubber, and rock asphalt more evenly dispersed and dissolved in the asphalt, thereby better modifying the base asphalt.
[0081] Flame retardant waterproof membrane
[0082] In the third aspect, an embodiment of the present application provides an exposed flame-retardant waterproof membrane, comprising a main substrate layer, a coating layer covering both sides of the main substrate layer, a mineral particle layer covering at least one side of the coating layer, and an isolation protective layer covering the mineral particle layer; wherein the coating layer is formed by the above-mentioned modified asphalt coating material or by the modified asphalt coating material prepared by the above-mentioned preparation method.
[0083] The exposed flame-retardant waterproof membrane provided by the present application adopts the above-mentioned modified asphalt coating material, and by spraying an isolation protective layer on the mineral particle layer, a protective film with a certain thickness is formed on the surface of the mineral particle layer, and van der Waals bonds are formed with the surface of the mineral particles to form an overall skin-like water erosion resistance, and has excellent salt spray resistance, alkali resistance, corrosion resistance, strong adhesion, good water resistance, excellent anti-rebound and excellent weather resistance, etc., which significantly improves the aging resistance, storage stability and UV aging resistance of the waterproof membrane, has a longer service life, and is suitable for exposed scenes.
[0084] In some embodiments, the thickness of the isolation protection layer is 0.3-0.5 mm.
[0085] In some embodiments, the isolation protection layer is formed of a polymer emulsion, and the polymer emulsion includes one or more of a silane-modified acrylic emulsion, a pure acrylic emulsion, and a fluorocarbon emulsion.
[0086] Example
[0087] The following examples more specifically describe the disclosure of the present application, which are intended for illustrative purposes only, as it will be apparent to those skilled in the art that various modifications and variations are possible within the scope of the disclosure of the present application. Unless otherwise stated, all parts, percentages, and ratios reported in the following examples are by weight, and all reagents used in the examples are commercially available or synthesized according to conventional methods and can be used directly without further processing, and the instruments used in the examples are commercially available.
[0088] The sources of raw materials used in the following examples are as follows:
[0089] 70# Asphalt, Lunt Petrochemical Co., Ltd.,
[0090] 90# Asphalt, Gaofu Petrochemical Co., Ltd.,
[0091] Rock Asphalt, Anhui Zhongyin Natural Rock Asphalt Technology Co., Ltd.,
[0092] SBS, Baling Petrochemical Company,
[0093] Chlorobutyl rubber, Jinan Hongcheng Chemical Co., Ltd.,
[0094] Desulfurized rubber powder, Hairui Environmental Protection New Materials Technology Co., Ltd.,
[0095] Silane coupling agent, 3-methacryloxypropyltrimethoxysilane, was purchased from Aladdin Biochemical Technology Co., Ltd.
[0096] Other raw materials not otherwise specified are common commercially available products.
[0097] Silane coupling agent modified heavy calcium powder is prepared by the following method:
[0098] Mix 100 g of heavy calcium powder with 300 ml of solvent (the volume ratio of water to alcohol is 2:0.5) to obtain a suspension;
[0099] 5.8 g of stearic acid was added to the suspension and stirred and mixed, and then 3 g of a silane coupling agent was added and stirred and mixed to obtain a mixed system;
[0100] The mixed system is dried and ground to obtain silane coupling agent modified heavy calcium powder with a particle size of 0.084 mm.
[0101] Example 1
[0102] A modified asphalt coating material comprises the following raw material components in percentage by weight:
[0103] Asphalt, 44 parts, asphalt is 70 / 90# asphalt, mass ratio is 1:2.6;
[0104] Rock asphalt, 5 parts, softening point is 152°C, needle penetration is less than 1, solubility> 96%;
[0105] 11 parts of tackifier, which is formed by mixing base oil and rubber oil R9 in a ratio of 1:0.65;
[0106] SBS, 6 parts, SBS is star-shaped SBS, wherein the mass ratio of styrene to butadiene is 2.8:7.2, the melt index is ≤1, and the weight average molecular weight is 26W;
[0107] Chlorobutyl rubber, 2 parts, chlorination degree 3%;
[0108] Desulfurized rubber powder, 10 parts;
[0109] Filler: silane coupling agent modified nano calcium carbonate powder, 17 parts, silane coupling agent content is 2%;
[0110] Flame retardant, 5 parts, the flame retardant is a mixture of magnesium hydroxide and polyphosphate, the mass ratio of magnesium hydroxide: polyphosphate is 2:0.5;
[0111] Protective layer emulsion 0.5-1.5mm
[0112] Preparation method of modified asphalt coating:
[0113] Step 1: Asphalt and a tackifier accounting for half of the total weight of the tackifier are weighed according to the weight fractions and added into the reactor, and the temperature is raised and stirred at a low speed for 15-20 minutes;
[0114] Step 2: Add the remaining viscosity enhancer into the stirred reactor and stir for 10-15 minutes;
[0115] Step 3: The temperature rises to 130-180°C, and chlorobutyl rubber SBS and rock asphalt are slowly added to step 1 and stirred. Stir at a low speed for 5-15 minutes, keep warm at 180°C, and stir at a high speed for 2.5-3 hours;
[0116] Step 4: Add the desulfurized rubber powder into step 2 and stir at high speed for 1-2 hours;
[0117] Step 5: Add filler and flame retardant into step 4 and stir evenly, then cool to 160-170°C to obtain modified asphalt coating.
[0118] Exposible flame-retardant waterproof membrane and preparation method:
[0119] The modified asphalt coating material is evenly coated on both sides of the dried, oil-impregnated and squeezed main substrate layer in two layers, and a structure of a lower surface protective layer, a lower surface coating layer, a pre-impregnated main substrate layer, and an upper surface coating layer is formed from bottom to top;
[0120] On one side of the main substrate layer, mineral particles are evenly coated on the upper surface coating layer to form a mineral particle layer, a 10 cm overlap is left on the upper surface coating layer, an isolation layer is covered on the overlap and the lower surface coating layer, and then after cooling, a polymer emulsion of 0.3-0.5 mm is sprayed on the upper surface mineral granular layer to form an isolation protective layer, and the emulsion is dried by heat drying to set the shape to obtain an exposed flame-retardant waterproof membrane.
[0121] The polymer emulsion is a silane-modified acrylic emulsion, and the inorganic mineral particles are dust-free shale particles and sintered mineral particles / clay particles.
[0122] Example 2
[0123] This embodiment provides a method for preparing and molding an exposed flame-retardant SBS modified asphalt waterproofing coiled material coating, comprising the following raw material components in percentage by weight:
[0124] Asphalt, 44 parts, the asphalt is 90# petroleum asphalt;
[0125] Rock asphalt, 5 parts, softening point is 152°C, needle penetration is less than 1, solubility> 96%;
[0126] Thickener, 11 parts, the thickener is a mixed reagent of trioctyl citrate and environmentally friendly organic aromatic oil, the ratio is 1:1.5.
[0127] SBS, 6 parts, SBS is star-shaped SBS, wherein the mass ratio of styrene to butadiene is 2.8:7.2, melt index ≤ 1, and weight average molecular weight 25W;
[0128] Chlorobutyl rubber, 2 parts, chlorination degree 3%;
[0129] Regenerated desulfurized rubber powder 10
[0130] Filler, silane coupling agent modified nano calcium carbonate powder, 12 parts, silane coupling agent content is 4%;
[0131] 10 parts of flame retardant, which is a mixture of antimony trioxide and polyphosphate, with the ratio of antimony trioxide to polyphosphate being 1.5:0.5;
[0132] Protective layer emulsion 0.5-1.5mm
[0133] Preparation method of modified asphalt coating:
[0134] Step 1: Asphalt and two-thirds of the total weight of the tackifier are weighed according to weight fractions and added into the reactor, and the temperature is raised and stirred at a low speed for 15-20 minutes;
[0135] Step 2: Add the remaining viscosity enhancer into the stirred reactor and stir for 10-15 minutes;
[0136] Step 3: The temperature rises to 130-180°C, and chlorobutyl rubber, SBS, and rock asphalt are slowly added to step 1 and stirred. Stir at a low speed for 5-15 minutes, keep warm at 180°C, and stir at a high speed for 2.5-3 hours;
[0137] Step 4: Add the desulfurized rubber powder into step 2 and stir at high speed for 1-2 hours;
[0138] Step 5: Add the filler and flame retardant into step 4 and stir evenly, then cool to 160-170°C to obtain the wet-laid modified asphalt waterproofing membrane coating material.
[0139] Exposible flame-retardant waterproof membrane and preparation method:
[0140] The modified asphalt coating material is evenly coated on both sides of the dried, oil-impregnated and squeezed main substrate layer in two layers, and a structure of a lower surface protective layer, a lower surface coating layer, a pre-impregnated main substrate layer, and an upper surface coating layer is formed from bottom to top;
[0141] On one side of the main substrate layer, mineral particles are uniformly coated on the upper surface coating layer to form a mineral particle layer, a 10 cm overlap is left on the upper surface coating layer, an isolation layer is covered on the overlap and the lower surface coating layer, and then after cooling, a polymer emulsion of 0.3-0.5 mm is sprayed on the upper surface mineral granular layer to form an isolation protection layer, and the exposed flame-retardant SBS modified asphalt waterproof membrane is obtained after the emulsion is dried and shaped by heat drying.
[0142] The polymer emulsion is a silane-modified acrylic emulsion, and the mineral particles are dust-free sintered mineral particles.
[0143] Example 3
[0144] This embodiment provides a method for preparing and molding an exposed flame-retardant SBS modified asphalt waterproofing coiled material coating, comprising the following raw material components in percentage by weight:
[0145] Asphalt, 38 parts, asphalt is 70# asphalt;
[0146] Rock asphalt, 4 parts,
[0147] Thickener, 10 parts, the thickener is a mixed reagent of cyclohexane oil and rubber oil R9, the ratio is 1:0.75.
[0148] SBS, 6 parts, SBS is star-shaped SBS, styrene:butadiene mass ratio is 3.2:6.8, melt index ≤1, weight average molecular weight 28W;
[0149] Chlorobutyl rubber, 3 parts, chlorination degree 2%;
[0150] Desulfurized rubber powder, 6 parts,
[0151] Filler: 25 parts of nano calcium carbonate powder modified by silane coupling agent, with a silane coupling agent content of 3%;
[0152] Flame retardant, 8 parts, the flame retardant is a mixture of magnesium hydroxide and polyphosphate, the mass ratio of magnesium hydroxide: polyphosphate is 2:0.5;
[0153] Preparation method of modified asphalt coating:
[0154] Step 1: Asphalt and a tackifier accounting for one third of the total weight of the tackifier are weighed according to weight fractions and added into a reactor, and the mixture is heated and stirred at a low speed for 15-20 minutes;
[0155] Step 2: Add the viscosity enhancer into the stirred reactor and stir for 10-15 minutes;
[0156] Step 3: The temperature rises to 130-180°C, and chlorobutyl rubber SBS and rock asphalt are slowly added to step 1 and stirred. Stir at a low speed for 5-15 minutes, keep warm at 180°C, and stir at a high speed for 2.5-3 hours;
[0157] Step 4: Add the desulfurized rubber powder into step 2 and stir at high speed for 1-2 hours;
[0158] Step 5: Add the filler and flame retardant into step 4 and stir evenly, then cool to 160-170°C to obtain the wet-laid modified asphalt waterproofing membrane coating material.
[0159] Exposible flame-retardant waterproof membrane and preparation method:
[0160] The modified asphalt coating material is evenly coated on both sides of the dried, oil-impregnated and squeezed main substrate layer in two layers, and a structure of a lower surface protective layer, a lower surface coating layer, a pre-impregnated main substrate layer, and an upper surface coating layer is formed from bottom to top;
[0161] Furthermore, on one side of the main substrate layer, mineral particles are uniformly coated on the upper surface coating layer to form a mineral particle layer, a 10 cm overlap is left on the upper surface coating layer, an isolation layer is covered on the overlap and the lower surface coating layer, and then after cooling, a polymer emulsion of 0.3-0.5 mm is sprayed on the upper surface mineral granular layer to form an isolation protective layer, and the emulsion is dried by heat drying to set the shape to obtain the exposed flame-retardant SBS modified asphalt waterproof membrane.
[0162] The polymer emulsion is pure acrylic emulsion, and the mineral particles are dust-free shale particles.
[0163] Comparative Example 1
[0164] The components and weight proportions are similar to those of Example 1, the main difference being that an equal amount of rock asphalt is replaced with 90# asphalt.
[0165] Comparative Example 2
[0166] The components and weight proportions are similar to those of Example 2, the main difference being that an equal amount of the flame retardant is replaced by stone powder.
[0167] Comparative Example 3
[0168] The components and weight proportions are similar to those of Example 3, the main differences being that an equal amount of chlorinated butyl rubber is replaced by ordinary butyl rubber, and the upper surface of the waterproof membrane is not covered with a polymer emulsion.
[0169] Comparative Example 4
[0170] The components and weight proportions are similar to those of Example 1, and the main difference from Example 1 is that the flame retardant is replaced by stone powder in equal amounts.
[0171] Comparative Example 5
[0172] The components and weight proportions are similar to those of Example 1, the main difference being that the modified butyl rubber is replaced by butyl rubber in equal amounts.
[0173] Comparative Example 6
[0174] The components and weight proportions are similar to those of Example 1, the main difference being that an equal amount of rock asphalt is replaced by asphalt, and an equal amount of chlorinated butyl rubber is replaced by butyl rubber.
[0175] Comparative Example 7
[0176] The components and weight parts are similar to those of Example 1, the main difference being that 17 parts of silane coupling agent-modified nano calcium carbonate powder are replaced with 0.34 parts of silane coupling agent and 16.66 parts of nano calcium carbonate powder.
[0177] Test Results
[0178] The samples prepared in the examples and comparative examples were tested according to GB 328-2007 and GB 8624-2012.
[0179] The following table shows the performance test results of the modified asphalt coating material samples prepared in Examples 1 to 3 and Comparative Examples 1 to 7:
[0180]
[0181] From Examples 1 to 3, it can be seen that the modified asphalt coating and the exposed flame-retardant waterproof roll rock asphalt, SBS, chlorinated butyl rubber, desulfurized rubber powder, and flame retardant provided in the present application can achieve the synergistic combination of stabilizing the aging resistance and bonding properties of the coating while improving the flame retardancy, so that the flame retardancy reaches the B2 level requirement.
[0182] Compared with Example 1, in Comparative Example 1, the rock asphalt is replaced by 90# asphalt in equal amounts, and it can be seen that the aging resistance is reduced; similar to the components and weight proportions of Example 2, in Comparative Example 2, the flame retardant is replaced by stone powder in equal amounts, and it can be seen that the flame retardant performance is reduced and cannot meet the B2 grade requirement; compared with Example 3, in Comparative Example 3, the chlorinated butyl rubber is replaced by ordinary butyl rubber in equal amounts, and the upper surface of the waterproof membrane is not covered with emulsion, the peeling strength between the membrane and the cement mortar is significantly reduced, and the flame retardant performance is reduced. The reason is that the chlorinated butyl rubber has certain flame retardancy and adhesion to cement mortar due to its chlorination, while the ordinary butyl rubber is flammable; compared with Example 1, in Comparative Example 4, the flame retardant is removed and replaced by stone powder in equal amounts. It can be seen that the peeling strength with cement is improved and the low-temperature flexibility is better, and the flame retardancy is significantly reduced to unqualified, because rock asphalt, SBS , chlorinated butyl rubber, and desulfurized rubber powder cannot provide effective flame retardant effect in modified asphalt coatings; compared with Example 1, Comparative Example 5 replaces an equal amount of chlorinated butyl rubber with butyl rubber. It can be seen that the flame retardant performance decreases, the peel strength decreases by 20%, and the cement peeling is unqualified. The reason is that the addition of flame retardants will affect the low temperature and cement peeling strength of the modified asphalt coating, resulting in unqualified performance. Other components need to be added to cooperate with it to achieve modified asphalt coils with good flame retardancy and physical properties; compared with Example 1, Comparative Example 6 replaces an equal amount of rock asphalt with asphalt, and an equal amount of chlorinated butyl rubber with butyl rubber. It can be seen that the adhesion of mineral particles decreases to an unqualified level, the peeling strength with cement is also reduced to an unqualified level, and the flame retardancy decreases to B2E level. The reason is to offset the negative impact of the flame retardant, and these two play a role in affecting the relevant performance in this system. Compared with Example 1, Comparative Example 7 replaces the silane coupling agent modified nano calcium carbonate powder with an equal amount of a mixture of a silane coupling agent and nano calcium carbonate powder. It can be seen that the adhesion of the mineral particles is reduced to an unqualified level, the low-temperature flexibility after aging is unqualified and the peel strength is reduced. This may be due to the unstable chemical bond between the organic and inorganic substances, resulting in a decrease in performance.
[0183] The above is only a specific implementation of the present application, but the protection scope of the present application is not limited thereto. Any technician familiar with the technical field can easily think of various equivalent modifications or replacements within the technical scope disclosed in the present application, and these modifications or replacements should be included in the protection scope of the present application. Therefore, the protection scope of the present application shall be based on the protection scope of the claims.
Claims
1. A modified asphalt coating material, characterized in that: The raw material components include the following parts by weight: Asphalt, 28-66 parts; Rock asphalt, 3-10 parts; Tackifier, 10-15 parts; SBS, 3-6 parts; the SBS is a star-shaped SBS, wherein the mass ratio of styrene to butadiene is (2.8-3.5): (7.2-6.5), the melt index is ≤1, and the weight average molecular weight is 18-30W; Chlorobutyl rubber, 2-5 parts, wherein the chlorination degree of the chlorinated butyl rubber is 1.8% to 4.5%; Desulfurized rubber powder, 5-10 parts; 12-20 parts of silane coupling agent modified heavy calcium powder, wherein the silane coupling agent modified heavy calcium powder is silane coupling agent modified heavy calcium powder using 3-methacryloxypropyltrimethoxysilane as a silane coupling agent, and based on the mass of the silane coupling agent modified heavy calcium powder, the mass fraction of the silane coupling agent is 1.5% to 5%; Flame retardant, 5-15 parts, the flame retardant includes one or more of magnesium hydroxide, aluminum hydroxide, decabromodiphenylethane, antimony trioxide, taurine, polyphosphates, and chlorinated polyethylene.
2. The modified asphalt coating material according to claim 1, characterized in that: The rock asphalt has a softening point of 145-160°C, a needle penetration of less than 1, and a solubility of >96%.
3. The modified asphalt coating material according to claim 1, characterized in that: The silane coupling agent modified heavy calcium powder comprises a product prepared by the following steps, wherein the steps include: Mixing heavy calcium powder with a solvent to obtain a suspension; After adding stearic acid to the suspension and stirring and mixing, adding a silane coupling agent and stirring and mixing to obtain a mixed system; The mixed system is dried and ground to obtain silane coupling agent modified heavy calcium powder.
4. The modified asphalt coating material according to claim 1 or 3, characterized in that: The raw material components meet at least one of the following conditions: (1) The particle size of the rubber powder is 10-40 mm; (2) The particle size of the silane coupling agent modified heavy calcium powder is 0.075 mm ~ 0.084 mm; (3) The particle size of the flame retardant is 0.013 mm to 0.026 mm.
5. The modified asphalt coating material according to claim 1, characterized in that: The tackifier includes one or more of base oil, rubber oil R9, environmentally friendly aromatic oil, butyl oleate, and trioctyl citrate.
6. A method for preparing a modified asphalt coating, characterized in that: The following steps are involved: Providing raw materials according to the raw material components and weight proportions contained in the coating material according to any one of claims 1 to 5; Adding asphalt into a reaction container, and adding a viscosity enhancer into the reaction container during stirring to obtain a first mixture; The SBS, the chlorinated butyl rubber, the rock asphalt and the first mixture are mixed and stirred to obtain a second mixture; After the desulfurized rubber powder is mixed with the second mixture, the silane coupling agent-modified heavy calcium powder and the flame retardant are added, mixed and stirred to obtain a modified asphalt coating material.
7. The method for preparing the modified asphalt coating according to claim 6, characterized in that: The silane coupling agent modified heavy calcium powder is prepared by the following method: Mixing heavy calcium powder with a solvent to obtain a suspension; After adding stearic acid to the suspension and stirring and mixing, adding a silane coupling agent and stirring and mixing to obtain a mixed system; The mixed system is dried and ground to obtain silane coupling agent modified heavy calcium powder.
8. The method for preparing the modified asphalt coating according to claim 6, characterized in that: The step of obtaining the second mixture includes: mixing SBS, chlorinated butyl rubber, rock asphalt and the first mixture at a temperature of 130°C-180°C, wherein the mixing and stirring includes stirring at a low speed of 50-130 r / min for 5-15 minutes and then stirring at a high speed of 400-800 r / min for 2.5h-3h.
9. An exposed flame-retardant waterproof membrane, characterized in that: It comprises a main substrate layer, a coating layer covering both sides of the main substrate layer, a mineral particle layer covering at least one side of the coating layer, and an isolation protection layer covering the mineral particle layer; Wherein, the coating layer is formed by the modified asphalt coating material described in any one of claims 1 to 5 or by the modified asphalt coating material prepared by the preparation method described in any one of claims 6 to 8.
10. The flame-retardant waterproof membrane capable of being exposed according to claim 9, characterized in that: The thickness of the isolation protection layer is 0.3-0.5 mm; and / or, The isolation protection layer is formed by a polymer emulsion, and the polymer emulsion includes one or more of silane-modified acrylic emulsion, pure acrylic emulsion, and fluorocarbon emulsion.
Citation Information
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