Modified illite and preparation method thereof, composition for non-asphalt-based bonding material layer, non-asphalt-based bonding material layer and preparation method thereof, and non-asphalt-based pre-laid waterproof coiled material

Through modified illite treatment and composition design, a non-asphalt-based adhesive layer was prepared, which solved the weather resistance and environmental protection problems of non-asphalt-based waterproof membranes, improved the bonding strength and antibacterial properties, reduced the release of volatiles, and achieved an efficient and environmentally friendly waterproof effect.

CN120665532AActive Publication Date: 2025-09-19KESHUN WATERPROOF TECH CO LTD
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Patent Information

Application Number
CN202510625504.0
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-05-15
Publication Date
2025-09-19
Estimated Expiration
2045-05-15

AI Technical Summary

Technical Problem

Existing non-asphalt-based waterproof membranes have deficiencies in weather resistance, aging resistance and environmental friendliness, and the materials release volatile components during use, affecting the environment and service life.

Method used

Modified illite is used as a modified filler. By treating it with diamine reagents and long-chain alkyl quaternary ammonium salts, the interlayer gap is expanded and combined with quaternary ammonium salts to prepare a non-asphalt-based adhesive. The non-asphalt-based adhesive layer is formed by combining with matrix oil, tackifying resin and polymer modifier to constitute a non-asphalt-based pre-laid waterproof membrane.

Benefits of technology

It improves the bonding strength, anti-aging performance and antibacterial effect of non-asphalt-based pre-laid waterproof membranes, while reducing the content of volatile organic compounds, achieving environmental protection and durability.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention relates to the technical field of waterproof coiled materials, and discloses modified illite and a preparation method thereof, a composition for a non-asphalt-based bonding material layer, the non-asphalt-based bonding material layer and a preparation method thereof, and a non-asphalt-based pre-laid waterproof coiled material. The method for preparing the modified illite comprises the following steps: (1) carrying out first contact on a raw material illite and a diamine reagent to obtain an intermediate I; the concentration of the diamine reagent is 0.4 mol / L to 0.6 mol / L; and (2) carrying out second contact on the intermediate I and a modified solution to obtain the modified illite, the modified solution contains long-chain alkyl quaternary ammonium salt with the concentration of 0.1 mol / L to 0.5 mol / L. The non-asphalt-based pre-paved waterproof coiled material prepared by the preparation method disclosed by the invention has the advantages of being excellent in adhesive property and aging resistance, and also has the advantage of being green and environment-friendly.
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Description

Technical Field

[0001] The present invention relates to the technical field of waterproofing membranes, and in particular to a modified illite and a preparation method thereof, a composition for a non-asphalt-based adhesive layer, a non-asphalt-based adhesive layer and a preparation method thereof, and a non-asphalt-based pre-laid waterproofing membrane. Background Art

[0002] Waterproof membrane is mainly used for building walls, roofs, tunnels, roads, etc. It is a flexible building material product that can be rolled into a roll to prevent external rainwater and groundwater leakage. It serves as a leak-proof connection between the project foundation and the building. It is the first barrier to waterproofing the entire project and plays a vital role in the entire project.

[0003] Waterproof membranes mainly include asphalt-based waterproof membranes and non-asphalt-based waterproof membranes. Due to the major defects of asphalt-based waterproof membranes in terms of environmental protection, construction safety, and water resistance, more and more research is focused on non-asphalt-based waterproof membranes under the demand for green buildings and long-term waterproofing.

[0004] Non-asphalt-based waterproof membranes are generally based on synthetic rubber, synthetic resin or a blend of the two, with appropriate amounts of chemical additives and fillers added, and are rollable sheet-like waterproof materials made through processes such as mixing, extrusion or calendering.

[0005] CN205112564U discloses a non-asphalt-based strong cross-membrane self-adhesive waterproof membrane. The membrane comprises, from top to bottom, an upper protective layer, an anti-ultraviolet layer, a first waterproof membrane layer, a non-asphalt base layer, a polyester lining layer, a non-asphalt base layer, a second waterproof membrane layer, and a barrier membrane. The membrane exhibits excellent high and low temperature resistance, tear strength, nail rod tear strength, and elongation. However, this solution enhances material strength through the coordinated action of a multi-layer structure, and the polyester lining layer contains starch glue, which is prone to mold and failure, significantly shortening the service life of the membrane.

[0006] CN105086895A discloses a hot melt adhesive for non-asphalt-based pre-paved polymer waterproofing membrane and a preparation method thereof. The hot melt adhesive comprises: 10-30 parts of cyclohexane oil, 0.1-3 parts of an antioxidant, 0.1-1 part of a silane coupling agent, 0.1-1 part of nano-sized titanium dioxide, 0.1-1 part of nano-sized zinc oxide, 20-32 parts of styrene-isoprene-styrene copolymer, 1-5 parts of styrene-hydrogenated isoprene-diblock copolymer, 15-30 parts of C5 / C9 copolymerized petroleum resin, and 20-35 parts of C5 hydrogenated petroleum resin; the weight ratio of the C5 fraction to the C9 fraction in the C5 / C9 copolymerized petroleum resin is (70-90):(7-11), and the softening point of the C5 / C9 copolymerized petroleum resin is 95-110°C. The non-asphalt-based pre-laid polymer waterproof membrane prepared using this hot-melt adhesive has good weather resistance and bonding strength. However, the anti-aging and waterproof properties of this material are difficult to evaluate, and the raw materials used will release more volatile components during production and long-term use, which is not in line with environmental protection concepts. Secondly, this waterproof membrane has some restrictions on the use environment, and its service life is extremely limited in cold and humid environments.

[0007] Therefore, it is of great significance to develop a new type of non-asphalt-based pre-paved waterproof membrane. Summary of the Invention

[0008] The purpose of the present invention is to provide an environmentally friendly non-asphalt-based pre-laid waterproof membrane with high bonding strength, excellent anti-aging and waterproof properties, and excellent antibacterial properties.

[0009] In order to achieve the above object, the first aspect of the present invention provides a method for preparing modified illite, the method comprising:

[0010] (1) contacting the raw material illite with a diamine reagent to obtain an intermediate I; the concentration of the diamine reagent is 0.4-0.6 mol / L;

[0011] (2) contacting the intermediate I with a modification solution for a second time to obtain the modified illite; the modification solution contains a long-chain alkyl quaternary ammonium salt with a concentration of 0.1-0.5 mol / L.

[0012] The second aspect of the present invention provides modified illite prepared by the method described in the first aspect.

[0013] The third aspect of the present invention provides a composition for non-asphalt-based adhesives, the composition comprising a main agent and auxiliary agents, the main agent being a matrix oil, a tackifying resin, a polymer modifier, and a modified filler;

[0014] Relative to 100 parts by weight of the modified filler, the content of the base oil is 100-250 parts by weight, the content of the tackifying resin is 50-100 parts by weight, and the content of the polymer modifier is 30-80 parts by weight;

[0015] The polymer modifier is selected from at least one of styrene-butadiene-styrene triblock copolymer, styrene-butadiene rubber, hydrogenated styrene-butadiene block copolymer and styrene-isoprene-styrene triblock copolymer;

[0016] The modified filler is the modified illite described in the second aspect.

[0017] The fourth aspect of the present invention provides a method for preparing a non-asphalt-based adhesive, which is carried out using the components in the composition described in the third aspect. The method comprises: stirring and mixing the components in the composition to obtain the non-asphalt-based adhesive.

[0018] The fifth aspect of the present invention provides a non-asphalt-based adhesive prepared by the method described in the fourth aspect.

[0019] The sixth aspect of the present invention provides a non-asphalt-based pre-laid waterproofing membrane, which includes reactive sand, a non-asphalt-based adhesive layer, a strong cross membrane and an isolation membrane. The non-asphalt-based adhesive layer is formed by the non-asphalt-based adhesive described in the fifth aspect.

[0020] This invention utilizes illite's potassium-rich, aluminum-rich properties, and its ability to freely release negative ions and far-infrared radiation. Treating the illite with a diamine reagent increases the interlayer gaps. The illite is then exposed to a long-chain alkyl quaternary ammonium salt reagent, allowing the long-chain alkyl group to further penetrate the material, expanding the interlayer gaps. Simultaneously, some of the quaternary ammonium salt binds to the illite surface, resulting in the modified illite described herein. This modified illite can be used in non-asphalt-based adhesives to significantly enhance the overall adsorption and antibacterial properties of the material.

[0021] Through the above technical solution, the present invention also has at least the following beneficial technical effects:

[0022] (1) When the modified illite prepared by the method for modifying illite provided by the present invention is used as a modified filler to prepare a non-asphalt-based adhesive, the obtained non-asphalt-based adhesive has excellent antibacterial properties. At the same time, the non-asphalt-based adhesive has a low content of organic volatiles, reflecting safer, more environmentally friendly and reliable characteristics.

[0023] (2) The non-asphalt-based pre-laid waterproofing membrane provided by the present invention has good bonding properties and aging resistance. DETAILED DESCRIPTION

[0024] The endpoints of the ranges and any values ​​disclosed herein are not limited to the precise ranges or values, and these ranges or values ​​should be understood to include values ​​close to these ranges or values. For numerical ranges, the endpoints of each range, the endpoints of each range and individual point values, and the individual point values ​​can be combined with each other to obtain one or more new numerical ranges, which should be considered to be specifically disclosed herein.

[0025] As mentioned above, the first aspect of the present invention provides a method for preparing modified illite, the method comprising:

[0026] (1) contacting the raw material illite with a diamine reagent to obtain an intermediate I; the concentration of the diamine reagent is 0.4-0.6 mol / L;

[0027] (2) contacting the intermediate I with a modification solution for a second time to obtain the modified illite; the modification solution contains a long-chain alkyl quaternary ammonium salt with a concentration of 0.1-0.5 mol / L.

[0028] Preferably, the water content of the raw material illite is not higher than 2 wt %, and the average diameter of the raw material illite is 20-150 μm.

[0029] More preferably, the diamine reagent is selected from at least one of ethylenediamine, 1,2-propylenediamine and 1,3-propylenediamine.

[0030] More preferably, the long-chain alkyl quaternary ammonium salt is at least one selected from cetyltrimethylammonium bromide, cetyltrimethylammonium chloride and dodecyltrimethylammonium bromide.

[0031] According to a specific embodiment, before obtaining the raw illite, the following steps are further included: crushing and grinding the prepared illite raw material to an average particle diameter of 20-150 μm, and drying in an oven at 140-160° C. to remove free water and some bound water from the material, resulting in a moisture content of no more than 2 wt %. In the present invention, the moisture content of the raw illite is determined by a drying method.

[0032] Preferably, the conditions for the first contact and the second contact are independently selected from: temperature of 70-90° C., time of 4-8 h, and rotation speed of 60-300 rpm.

[0033] According to a specific embodiment, in step (1), before obtaining the intermediate I, the process further includes washing and drying the material after the first contact.

[0034] According to a specific embodiment, in step (2), after the second contact is completed, the obtained product is further subjected to separation, washing and drying treatment to obtain the modified illite.

[0035] According to a preferred embodiment, in step (2), the modified illite may be further ground and pulverized to make the particle size distribution of the modified illite more uniform, and the average particle size of the modified illite is 13-74 μm.

[0036] The present invention has no special requirements on the volume of the ethylenediamine solution and the modified solution, as long as the raw material illite and the intermediate I can be completely immersed.

[0037] As mentioned above, the second aspect of the present invention provides modified illite prepared by the method described in the first aspect.

[0038] As mentioned above, the third aspect of the present invention provides a composition for non-asphalt-based adhesives, the composition consisting of a main agent and auxiliary agents, the main agent being a matrix oil, a tackifying resin, a polymer modifier, and a modified filler;

[0039] Relative to 100 parts by weight of the modified filler, the content of the base oil is 100-250 parts by weight, the content of the tackifying resin is 50-100 parts by weight, and the content of the polymer modifier is 30-80 parts by weight;

[0040] The polymer modifier is selected from at least one of styrene-butadiene-styrene triblock copolymer, styrene-butadiene rubber, hydrogenated styrene-butadiene block copolymer and styrene-isoprene-styrene triblock copolymer;

[0041] The modified filler is the modified illite described in the second aspect.

[0042] Preferably, the polymer modifier is a combination of styrene-butadiene-styrene triblock copolymer (SBS), styrene-butadiene rubber (SBR), and styrene-isoprene-styrene triblock copolymer (SIS) in a weight ratio of 1.5-2:1.2-1.5:1. The inventors of the present invention have discovered that in this preferred embodiment, the non-asphalt-based pre-paved waterproofing membrane produced by the present invention exhibits superior aging resistance and adhesion properties.

[0043] More preferably, the base oil is selected from at least one of aromatic paraffinic oil, naphthenic oil and reduced line oil.

[0044] Further preferably, the tackifying resin is selected from at least one of C5 petroleum resin, C9 petroleum resin, coumarone resin, rosin resin and terpene resin.

[0045] According to a preferred embodiment, the auxiliary agent includes a coupling agent, a wax substance and a pigment; relative to 100 parts by weight of the modified filler, the content of the coupling agent is 0.5-1.5 parts by weight, the content of the wax substance is 3-15 parts by weight, and the content of the pigment is 5-15 parts by weight.

[0046] According to a more preferred embodiment, in the auxiliary agent, the coupling agent is selected from γ-(2,3-epoxypropoxy)propyltrimethoxysilane and / or γ-methacryloxypropyltrimethoxysilane.

[0047] According to a particularly preferred embodiment, the wax material is selected from at least one of PE wax, PP wax and amide wax.

[0048] More preferably, the pigment is iron oxide red and / or emerald green, and has an average diameter of 2-35 μm.

[0049] As mentioned above, the fourth aspect of the present invention provides a method for preparing a non-asphalt-based adhesive, which is carried out using the components in the composition described in the third aspect. The method includes: stirring and mixing the components in the composition to obtain the non-asphalt-based adhesive.

[0050] Preferably, the stirring and mixing conditions include: temperature of 160-180° C. and time of 5-8 h.

[0051] According to a preferred embodiment, the method for preparing the non-asphalt-based adhesive comprises the following steps:

[0052] 1) Add the base oil and tackifying resin into a reactor preheated to 160-170° C., heat and stir for 20 minutes to obtain intermediate material I;

[0053] 2) mixing the polymer modifier, coupling agent, wax substance and the intermediate material I, and stirring at 175-185° C. for 3 hours to obtain the intermediate material II;

[0054] 3) The modified filler and pigment are mixed with the intermediate material II, maintained at a temperature of 175-185° C., stirred for 1 hour, and then a coupling agent is added, and the mixture is reacted at 165-175° C. for 1 hour to obtain the non-asphalt-based adhesive.

[0055] As mentioned above, the fifth aspect of the present invention provides a non-asphalt-based adhesive prepared by the method described in the fourth aspect.

[0056] As mentioned above, the sixth aspect of the present invention provides a non-asphalt-based pre-laid waterproofing membrane, which includes reactive sand, a non-asphalt-based adhesive layer, a strong cross membrane, a non-asphalt-based adhesive layer, and an isolation membrane. The non-asphalt-based adhesive layer is formed by the non-asphalt-based adhesive described in the fifth aspect.

[0057] Preferably, the average diameter of the reaction sand is 400-800 μm.

[0058] Further preferably, the strong cross film is a four-layer laminated strong cross film with an average thickness of 190-320 μm.

[0059] Particularly preferably, the isolation film is selected from silicon-coated PE release film and / or PET release film.

[0060] In the present invention, the non-asphalt-based pre-laid waterproof membrane comprises, from top to bottom, reactive sand, a non-asphalt-based adhesive layer, a strong cross membrane, a non-asphalt-based adhesive layer and an isolation membrane.

[0061] The present invention will be described in detail below by way of examples. In the following examples, unless otherwise specified, all instruments and raw materials used are commercially available.

[0062] Some of the raw materials and their sources used in the following examples are as follows:

[0063] Raw material illite:

[0064] Raw material illite-I: average diameter 50 μm;

[0065] Raw material illite-II: average diameter 400 μm;

[0066] Strong cross film: Four-layer laminated strong cross film, average thickness 280μm, purchased from Yushi Plastic Industry Company;

[0067] Reaction sand: average diameter 500 μm, purchased from Beijing Hualin Ruisi Company;

[0068] Isolation film: PET release film;

[0069] C5 petroleum resin: molecular weight 1400, purchased from Guangzhou Tiankai Chemical Company;

[0070] Rosin resin: purchased from Puyang Zhongke Xinyuan Petrochemical Company;

[0071] Styrene-butadiene-styrene triblock copolymer (SBS): brand 411#, purchased from LG Company;

[0072] Styrene-butadiene rubber (SBR): brand 095, purchased from Shandong Gaoshi Company;

[0073] Styrene-isoprene-styrene triblock copolymer (SIS): brand 1105, purchased from Yueyang Petrochemical Company;

[0074] γ-(2,3-Epoxypropyloxy)propyltrimethoxysilane: purchased from MacLean Reagent Company;

[0075] γ-Methacryloxypropyltrimethoxysilane: purchased from MacLean Reagent Company;

[0076] PE wax: brand 4010, purchased from Comino New Materials Company;

[0077] PP wax: brand 406, purchased from Qingdao Sino Chemical Company;

[0078] Amide wax: brand 206, purchased from Tianshi Wax Powder Company;

[0079] Aromatic oil: brand R9, purchased from Guangzhou Dagang Company;

[0080] Naphthenic oil: brand 4006, purchased from Guangzhou Dagang Company;

[0081] Iron oxide red: average diameter 20 μm, purchased from Guangzhou Chutian Pigment Company;

[0082] Iron oxide green: average diameter 30 μm, purchased from Guangzhou Chutian Pigment Company;

[0083] Heavy calcium: average diameter 75 μm, purchased from Qixia Rongguan Company.

[0084] Preparation Example 1

[0085] This preparation example is used to illustrate the preparation of the modified illite provided by the present invention, and includes the following steps:

[0086] (1) Illite-I, a raw material having a water content of 0.05 wt% after drying, was immersed in a 0.5 mol / L ethylenediamine solution for first contact. The conditions for the first contact included: temperature of 80° C., time of 7 h, and rotation speed of 300 rpm.

[0087] (2) The material after the first contact is centrifuged to separate the solid product, which is then washed with deionized water until the ethylenediamine is completely removed (infrared detection is performed to determine whether the washing liquid still contains ethylenediamine), and then dried at 80° C. for 12 h to obtain intermediate I.

[0088] (3) The intermediate I was immersed in a 0.4 mol / L hexadecyltrimethylammonium bromide aqueous solution for a second contact. The conditions for the second contact included: a temperature of 70° C., a time of 5 h, and a rotation speed of 250 rpm.

[0089] (4) The material after the second contact is centrifuged to separate the solid product, which is then washed with deionized water until no bromide ions are detected (detected by silver nitrate solution), and then the washed product is dried at 80° C. for 12 h to obtain the modified illite A1.

[0090] Preparation Example 2

[0091] (1) Illite-I, a raw material having a water content of 0.1 wt% after drying, was immersed in a 1,3-propylenediamine solution with a concentration of 0.4 mol / L for first contact. The conditions for the first contact included: a temperature of 70° C., a time of 9 h, and a rotation speed of 200 rpm.

[0092] (2) The material after the first contact is centrifuged to separate the solid product, which is then washed with deionized water until 1,3-propylenediamine is completely removed (infrared detection is performed to determine whether the washing liquid still contains 1,3-propylenediamine), and then dried at 80° C. for 12 h to obtain intermediate I.

[0093] (3) The intermediate I was immersed in a 0.1 mol / L aqueous solution of dodecyltrimethylammonium bromide for a second contact. The conditions of the second contact included: a temperature of 80° C., a time of 4 h, and a rotation speed of 200 rpm.

[0094] (4) The material after the second contact is centrifuged to separate the solid product, which is then washed with deionized water until no bromide ions are detected (detected by silver nitrate solution), and then the washed product is dried at 80° C. for 12 h to obtain the modified illite A2.

[0095] Preparation Example 3

[0096] (1) The raw material illite-II having a water content of 0.05 wt% after drying is immersed in a 0.5 mol / L ethylenediamine solution for first contact. The conditions of the first contact include: temperature of 80° C., time of 7 h, and rotation speed of 300 rpm.

[0097] (2) The material after the first contact is centrifuged to separate the solid product, which is then washed with deionized water until the ethylenediamine is completely removed (infrared detection is performed to determine whether the washing liquid still contains ethylenediamine), and then dried at 80° C. for 12 h to obtain intermediate I.

[0098] (3) The intermediate I was immersed in a 0.4 mol / L hexadecyltrimethylammonium bromide aqueous solution for a second contact. The conditions for the second contact included: a temperature of 70° C., a time of 5 h, and a rotation speed of 300 rpm.

[0099] (4) The material after the second contact is centrifuged to separate the solid product, which is then washed with deionized water until no bromide ions are detected (detected by silver nitrate solution), and then the washed product is dried at 80° C. for 12 h to obtain the modified illite A3.

[0100] Comparative Preparation Example 1

[0101] (1) Illite-I, a raw material having a water content of 0.05 wt% after drying, was immersed in a 0.5 mol / L ethylenediamine solution for first contact. The conditions for the first contact included: temperature of 80° C., time of 7 h, and rotation speed of 300 rpm.

[0102] (2) The material after the first contact is centrifuged to separate the solid product, which is then washed with deionized water until the ethylenediamine is completely removed (infrared detection is performed to determine whether the washing liquid still contains ethylenediamine), and then dried at 80° C. for 12 h to obtain intermediate I.

[0103] (3) The intermediate I was immersed in a 0.4 mol / L sodium dodecyl sulfate aqueous solution for a second contact. The conditions of the second contact included: a temperature of 70° C., a time of 5 h, and a rotation speed of 250 rpm.

[0104] (4) The material after the second contact is centrifuged to separate the solid product, which is then washed with deionized water until no bromide ions are detected (detected by silver nitrate solution), and then the washed product is dried at 80° C. for 12 hours to obtain the modified illite D-A1.

[0105] Comparative Preparation Example 2

[0106] (1) Illite-I, a raw material having a water content of 0.05 wt% after drying, was immersed in a 0.5 mol / L ethylenediamine solution for first contact. The conditions for the first contact included: temperature of 80° C., time of 7 h, and rotation speed of 300 rpm.

[0107] (2) The material after the first contact is centrifuged to separate the solid product, which is then washed with deionized water until the ethylenediamine is completely removed (infrared detection is performed to determine whether the washing liquid still contains ethylenediamine), and then dried at 80° C. for 12 h to obtain the modified illite D-A2.

[0108] Comparative Preparation Example 3

[0109] (1) Illite-I raw material with a water content of 0.05 wt% after drying was immersed in a 0.4 mol / L hexadecyltrimethylammonium bromide aqueous solution, wherein the immersion conditions included: temperature of 70° C., time of 5 h, and rotation speed of 300 rpm.

[0110] (2) The soaked material is centrifuged to separate the solid product, which is then washed with deionized water until no bromide ions are detected (detected by silver nitrate solution), and the washed product is then dried at 80° C. for 12 h to obtain the modified illite D-A3.

[0111] The embodiments of the present invention are used to prepare non-asphalt-based adhesives. The amounts of raw materials used in the following examples are all in parts by weight unless otherwise specified, and each part by weight represents 10 g.

[0112] Example 1

[0113] S1: Add the base oil and tackifying resin into a reactor preheated to 160°C, heat and stir for 20 minutes to obtain intermediate material I;

[0114] S2: stirring and mixing the polymer modifier, coupling agent, wax substance and the intermediate I at 180° C. for 3 hours to obtain intermediate material II;

[0115] S3: stirring and mixing the modified filler, pigment and the intermediate material II at 180° C. for 1 hour, then adding a coupling agent, stirring and reacting at 170° C. for 1 hour to obtain the non-asphalt-based adhesive;

[0116] The specific material types, dosages and process parameters of this example are shown in Table 1.

[0117] Unless otherwise specified, Examples 2 and 3 were carried out with reference to the method of Example 1, except that the types of substances, amounts and process parameters used in the examples were different. For details, see Table 1.

[0118] Table 1

[0119]

[0120] Example 4

[0121] This example is carried out by referring to the method of Example 1, except that this example uses equal parts by weight of styrene-butadiene-styrene triblock copolymer (SBS) to replace the polymer modifier in Example 1 to obtain a non-asphalt-based adhesive B4.

[0122] Example 5

[0123] This example was carried out by referring to the method of Example 1, except that this example used modified illite A3 in equal parts by weight to replace the modified illite A1 in Example 1, to obtain a non-asphalt-based adhesive B5.

[0124] Comparative Example 1

[0125] This comparative example was carried out with reference to the method of Example 1, except that this comparative example used an equal weight portion of modified illite D-A1 to replace the modified illite A1 in Example 1 to obtain a non-asphalt-based adhesive D-B1.

[0126] Comparative Example 2

[0127] This comparative example was carried out with reference to the method of Example 1, except that this comparative example used modified illite D-A2 in equal parts by weight to replace the modified illite A1 in Example 1 to obtain a non-asphalt-based adhesive D-B2.

[0128] Comparative Example 3

[0129] This comparative example was carried out with reference to the method of Example 1, except that this comparative example used modified illite D-A3 in equal parts by weight to replace the modified illite A1 in Example 1 to obtain a non-asphalt-based adhesive D-B3.

[0130] Comparative Example 4

[0131] This comparative example was carried out with reference to the method of Example 1, except that the modified illite A1 in Example 1 was replaced with an equal weight portion of heavy calcium carbonate to obtain a non-asphalt-based adhesive D-B4.

[0132] Comparative Example 5

[0133] This comparative example was carried out by referring to the method of Example 1, except that the raw material illite-I was used in equal parts by weight to replace the modified illite A1 in Example 1 to obtain a non-asphalt-based adhesive D-B5.

[0134] Test Example 1

[0135] This test example is used to determine the volatile matter (VOC) content and antibacterial properties of the non-asphalt-based adhesive obtained above.

[0136] Specifically, the volatile matter (VOC) content of the non-asphalt-based adhesive obtained above was tested with reference to DB 11-1983-2022. Staphylococcus aureus was selected as the test bacteria with reference to GB / T 21866-2008 standard to test the antibacterial rate of the non-asphalt-based adhesive. The test results are shown in Table 2.

[0137] Table 2

[0138] Self-adhesive layer VOC / ≤10g / kg Antibacterial rate of self-adhesive layer / % Example 1 8.6 97.2 Example 2 6.3 96.8 Example 3 4.6 96.6 Example 4 8.3 97.0 Example 5 10.7 86.2 Comparative Example 1 12.1 76.4 Comparative Example 2 16.7 70.1 Comparative Example 3 15.4 82.3 Comparative Example 4 29.2 60.2 Comparative Example 5 20.5 67.6

[0139] Test Example 2

[0140] This test example is used to determine the physical and chemical properties of non-asphalt-based pre-laid waterproof membranes containing the above-mentioned non-asphalt-based adhesives.

[0141] The above-mentioned non-asphalt-based adhesives were respectively formed on both sides of the strong cross membrane, and the discharge thickness was controlled to be about 1.5 mm. The upper and lower surfaces were then covered with reactive sand and isolation membranes, and pressed firmly to obtain the non-asphalt-based pre-laid waterproof membranes, which were named C1, C2, C3, C4, C5, D-C1, D-C2, D-C3, D-C4 and D-C5 in sequence.

[0142] The low-temperature flexibility limit temperature, the low-temperature limit temperature after 14 days of heat aging, and the peeling strength with post-cast concrete of the non-asphalt-based pre-paved waterproof membrane obtained above were tested with reference to the T / CECS10197-2022 polymer membrane-based pre-paved waterproof membrane standard. The test results are shown in Table 3.

[0143] Table 3

[0144]

[0145] It can be seen from the results in Table 2 and Table 3 that the non-asphalt-based adhesive provided by the present invention has a low volatile matter VOC content and excellent antibacterial performance. The non-asphalt-based pre-laid waterproof membrane provided by the present invention not only has excellent bonding performance and aging resistance, but also has the advantage of being green and environmentally friendly.

[0146] The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the technical concept of the present invention, various simple variations of the technical solution of the present invention may be made, including combining the various technical features in any other appropriate manner. These simple variations and combinations should also be regarded as disclosed in the present invention and fall within the scope of protection of the present invention.

Claims

1. A method for preparing modified illite, characterized in that: The method includes: (1) contacting the raw material illite with a diamine reagent to obtain an intermediate I; the concentration of the diamine reagent is 0.4-0.6 mol / L; (2) contacting the intermediate I with a modification solution for a second time to obtain the modified illite; the modification solution contains a long-chain alkyl quaternary ammonium salt with a concentration of 0.1-0.5 mol / L.

2. The method according to claim 1, wherein The water content of the raw material illite is not higher than 2 wt %, and the average diameter of the raw material illite is 20-150 μm; and / or, the diamine reagent is selected from at least one of ethylenediamine, 1,2-propylenediamine and 1,3-propylenediamine; And / or, the long-chain alkyl quaternary ammonium salt is at least one selected from cetyltrimethylammonium bromide, cetyltrimethylammonium chloride and dodecyltrimethylammonium bromide; And / or, the conditions of the first contact and the second contact are independently selected from: temperature of 70-90° C., time of 4-8 h, and rotation speed of 60-300 rpm.

3. Modified illite prepared by the method according to claim 1 or 2.

4. A composition for non-asphalt-based adhesives, characterized in that: The composition is composed of a main agent and auxiliary agents, wherein the main agent is a matrix oil, a tackifying resin, a polymer modifier and a modified filler; Relative to 100 parts by weight of the modified filler, the content of the base oil is 100-250 parts by weight, the content of the tackifying resin is 50-100 parts by weight, and the content of the polymer modifier is 30-80 parts by weight; The polymer modifier is selected from at least one of styrene-butadiene-styrene triblock copolymer, styrene-butadiene rubber, hydrogenated styrene-butadiene block copolymer and styrene-isoprene-styrene triblock copolymer; The modified filler is the modified illite described in claim 3.

5. The composition according to claim 4, wherein The polymer modifier is a combination of styrene-butadiene-styrene triblock copolymer, styrene-butadiene rubber and styrene-isoprene-styrene triblock copolymer in a weight ratio of 1.5-2:1.2-1.5:1; And / or, the base oil is selected from at least one of aromatic paraffin oil, naphthenic oil and reduced line oil; And / or, the tackifying resin is selected from at least one of C5 petroleum resin, C9 petroleum resin, coumarone resin, rosin resin and terpene resin.

6. The composition according to claim 4, wherein The auxiliary agents include coupling agents, wax substances and pigments; Relative to 100 parts by weight of the modified filler, the content of the coupling agent is 0.5-1.5 parts by weight, the content of the wax material is 3-15 parts by weight, and the content of the pigment is 5-15 parts by weight.

7. The composition according to claim 6, wherein In the auxiliary agent, the coupling agent is selected from γ-(2,3-epoxypropoxy)propyltrimethoxysilane and / or γ-methacryloxypropyltrimethoxysilane; And / or, the wax material is selected from at least one of PE wax, PP wax and amide wax; And / or, the pigment is iron oxide red and / or oxidized emerald green, and has an average diameter of 2-35 μm.

8. A method for preparing a non-asphalt-based adhesive, characterized in that: The method is carried out using the components of the composition according to any one of claims 4 to 7, and comprises: stirring and mixing the components of the composition to obtain the non-asphalt-based adhesive; And / or, the stirring and mixing conditions include: temperature of 160-180° C. and time of 5-8 hours.

9. The non-asphalt-based adhesive prepared according to the method of claim 8.

10. A non-asphalt-based pre-laid waterproofing membrane, characterized in that: The non-asphalt-based pre-laid waterproofing membrane comprises reactive sand, a non-asphalt-based adhesive layer, a strong cross membrane and an isolation membrane, wherein the non-asphalt-based adhesive layer is formed by the non-asphalt-based adhesive according to claim 9; and / or, the average diameter of the reaction sand is 400-800 μm; And / or, the strong cross membrane is a four-layer laminated strong cross membrane with an average thickness of 190-320 μm; And / or, the isolation film is selected from silicon-coated PE release film and / or PET release film.

Citation Information

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