Aging-resistant self-adhesive asphalt mastic, preparation method and application thereof
By combining modified amino-modified cellulose nanocrystal powder with carbon black hybrids, silane coupling agents, and polyborosiloxanes, an aging-resistant self-adhesive asphalt compound was prepared. This solved the problems of debonding and cracking of self-adhesive polymer-modified asphalt waterproof membranes under the influence of heat aging and rainwater, achieving excellent anti-aging performance and long service life.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- HENGHE MATERIALS & SCI TECH CO LTD
- Filing Date
- 2024-12-03
- Publication Date
- 2026-06-12
AI Technical Summary
Self-adhesive polymer-modified bitumen waterproof membranes are prone to aging during service due to heat and rain, leading to debonding and cracking, and thus failing to meet the requirements of GB 55030-2022 "General Specification for Waterproofing of Buildings and Municipal Projects" for heat aging, water resistance and joint peeling performance.
A specific process was used to prepare aging-resistant self-adhesive asphalt rubber by using modified amino-modified cellulose nanocrystal powder, carbon black hybrid, silane coupling agent, and polyborosiloxane, forming a multidimensional hybrid network and reversible physical cross-linking structure, which enhances the mechanical properties and interfacial bonding of the rubber.
It improves the tensile strength, tear strength and heat resistance of self-adhesive asphalt compound, significantly enhances the anti-aging properties of waterproof membrane, and extends its service life.
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Abstract
Description
Technical Field
[0001] This invention belongs to the field of waterproof materials technology, and specifically relates to an aging-resistant self-adhesive asphalt compound, its preparation method, and its application. Background Technology
[0002] Self-adhesive polymer-modified bitumen waterproof membranes (hereinafter referred to as self-adhesive waterproof membranes) have excellent advantages such as low-temperature crack resistance, puncture self-healing, and convenient installation, and are increasingly widely used in building waterproofing projects. However, self-adhesive waterproof membranes will age under the influence of heat and rainwater during service, leading to delamination and cracking, thus causing building leaks. In response to the serious problem of building leaks, GB 55030-2022 "General Specification for Waterproofing of Buildings and Municipal Engineering" was promulgated, which puts forward higher requirements for the thermal aging, water resistance, and joint peel performance of waterproof materials. Therefore, it is essential to improve the overall performance of self-adhesive waterproof membranes. Summary of the Invention
[0003] The technical problem to be solved by the present invention is to provide an aging-resistant self-adhesive asphalt compound, its preparation method and application. The asphalt compound can be used in self-adhesive waterproof membranes, has excellent resistance to various aging properties, long service life and good application prospects.
[0004] This invention provides an aging-resistant self-adhesive asphalt compound, comprising the following components by weight:
[0005]
[0006] Preferably, the modified amino-modified cellulose nanocrystal powder is obtained by ball milling and spray drying of carbon black and amino-modified cellulose nanocrystals (CCP).
[0007] Preferably, the mass ratio of carbon black to amino-modified cellulose nanocrystals is 85-95:5-15.
[0008] Preferably, the carbon black is furnace black or channel black; the particle size of the aminated cellulose nanocrystals is 60-80 nm.
[0009] Preferably, the petroleum asphalt is one or more of 70#-300#.
[0010] Preferably, the styrene-butadiene rubber is solution-polymerized styrene-butadiene rubber (SSBR).
[0011] Preferably, the inorganic filler is one or more of the following: light calcium carbonate, heavy calcium carbonate, clay, talc powder, mica powder, montmorillonite, fly ash, and cement powder.
[0012] Preferably, the coupling agent is a silane coupling agent, including at least one selected from propenyltriethoxysilane, γ-aminopropyltriethoxysilane, and vinyltriethoxysilane.
[0013] Preferably, the base oil is one or more of aromatic mineral oils and naphthenic mineral oils.
[0014] This invention also provides a method for preparing an aging-resistant self-adhesive asphalt compound, comprising the following steps:
[0015] (1) Heat the petroleum asphalt to 140-150℃ according to the weight parts, add the base oil and stir to obtain mixture A;
[0016] (2) Then heat the mixture to 210-230℃, add styrene-butadiene rubber and styrene-butadiene-styrene block copolymer to mixture A, and stir for 30-40 minutes. After stirring evenly, slowly cool the mixture to 170-175℃ to obtain mixture B.
[0017] (3) Add polyborosiloxane and coupling agent to mixture B, maintain the temperature at 170-175℃, stir for 60-80 min to obtain mixture C;
[0018] (4) Add the modified amino-modified cellulose nanocrystal powder to mixture C, heat to 180-190℃, stir for 70-90 min to obtain mixture D;
[0019] (5) Add inorganic filler to mixture D, cool to 160-170℃ for thermal crosslinking reaction, stir at 30-50 rpm for 1-2 hours, and discharge at 155-165℃ to obtain the self-adhesive asphalt compound.
[0020] The present invention also provides an aging-resistant self-adhesive asphalt compound for use in the preparation of asphalt waterproof membranes.
[0021] Further, the self-adhesive asphalt adhesive is poured onto the base material, then covered with a PET film and allowed to cool naturally at room temperature to obtain the asphalt waterproof membrane.
[0022] Beneficial effects
[0023] (1) The self-adhesive asphalt compound of the present invention incorporates carbon black / amino cellulose nanocrystal powder. Cellulose nanocrystals have excellent properties such as high strength, high elastic modulus, large aspect ratio, and large specific surface area. Their one-dimensional structure provides the possibility for them to form a hybrid with carbon black. The carbon black / CCP hybrid helps to build a multidimensional hybrid network in styrene-butadiene rubber, which improves the tensile strength and tear strength of the compound and enhances its mechanical properties.
[0024] (2) In this invention, a silane coupling agent is added to the self-adhesive asphalt rubber compound. Since it contains compounds with multiple functional groups, the hydrolyzable group at one end of the silane coupling agent undergoes a condensation reaction with the hydroxyl groups on the surface of CCP, making the surface of CCP change from hydrophilic to hydrophobic. This effectively reduces the agglomeration of carbon black / CCP filler with petroleum asphalt and styrene-butadiene rubber matrix, giving it better dispersibility. The organic group at the other end of the coupling agent is connected to the carboxyl group of petroleum asphalt, forming a molecular bridge between carbon black / CCP and the asphalt matrix, which enhances the interfacial bonding force between the filler and the organic matrix.
[0025] (3) Compared with ordinary organopolysiloxanes, the polyborosiloxane of the present invention has superior high temperature resistance, oxidation resistance and high stability. The boron atoms in the Si-O-B part of the chain can form reversible B-O electron bridge pairs with the oxygen atoms in the adjacent polyborosiloxane chain, thereby forming a reversible physical cross-linking network structure. At the same time, it can better combine the asphalt matrix, styrene-butadiene rubber and inorganic fillers, thereby increasing the aging resistance and enhancing the strength and heat resistance of the rubber compound. Detailed Implementation
[0026] The present invention will be further illustrated below with reference to specific embodiments. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the invention. Furthermore, it should be understood that after reading the teachings of this invention, those skilled in the art can make various alterations or modifications to the invention, and these equivalent forms also fall within the scope defined by the appended claims.
[0027] Example 1
[0028] The aging-resistant self-adhesive asphalt compound provided in this embodiment comprises the following components by weight:
[0029] 45 parts petroleum asphalt, 25 parts styrene-butadiene rubber, 6 parts modified amino-modified cellulose nanocrystal powder, 13 parts SBS, 4 parts polyborosiloxane, 25 parts inorganic filler, 0.5 parts coupling agent, and 7 parts base oil.
[0030] The modified aminated cellulose nanocrystal powder was prepared by the following method: Carbon black and an aqueous dispersion of aminated cellulose nanocrystals (CCP) were mixed, and the mixture was then poured into a ball mill jar and ball-milled at 200 r / min for 2 h to obtain a carbon black / CCP hybrid slurry. The carbon black / CCP hybrid slurry was diluted and spray-dried at 180°C using a spray dryer to obtain the carbon black / CCP hybrid powder, i.e., the modified aminated cellulose nanocrystal powder.
[0031] The carbon black is furnace-processed carbon black.
[0032] The carbon black / CCP mass ratio is 95 / 5.
[0033] The CCP particle size is 60 nm.
[0034] The petroleum asphalt is 70#.
[0035] The base oil is an aromatic mineral oil.
[0036] The styrene-butadiene rubber is solution-polymerized styrene-butadiene rubber (SSBR).
[0037] The coupling agent is propylenetriethoxysilane.
[0038] The inorganic filler is light calcium carbonate.
[0039] The preparation method includes the following steps:
[0040] (1) Heat petroleum asphalt to 140°C, add base oil and stir for 30 minutes to obtain mixture A;
[0041] (2) Heat to 220℃, add styrene-butadiene rubber and SBS elastomer to mixture A prepared in step 1, and stir at this temperature for 30 minutes. After stirring evenly, slowly cool to 170℃ to obtain mixture B;
[0042] (3) Add polyborosiloxane and coupling agent to the mixture B prepared in step 2, keep the temperature at 170℃ and stir for 70 min to obtain mixture C;
[0043] (4) Add the modified amino-modified cellulose nanocrystal powder to the mixture C prepared in step 3, heat it to 180°C, stir for 80 min, and obtain mixture D;
[0044] (5) Add polyborosiloxane and inorganic filler to the mixture D prepared in step 4, and cool it to 160°C for thermal crosslinking reaction. Stir at 40 rpm for 2 hours and discharge at 155°C to obtain the self-adhesive asphalt compound.
[0045] (6) Quickly pour the above self-adhesive asphalt material onto the composite aluminum mold, control the thickness of the molded sample to be 1.5 mm, then cover it with PET film and allow it to cool naturally at room temperature to obtain asphalt waterproof membrane.
[0046] Example 2
[0047] The aging-resistant self-adhesive asphalt compound provided in this embodiment comprises the following components by weight:
[0048] The composition includes 45 parts petroleum asphalt, 23 parts styrene-butadiene rubber, 7 parts modified amino-modified cellulose nanocrystal powder, 15 parts SBS, 4 parts polyborosiloxane, 22 parts inorganic filler, 0.5 parts coupling agent, and 7 parts base oil.
[0049] The modified aminated cellulose nanocrystal powder was prepared by the following method: Carbon black and an aqueous dispersion of aminated cellulose nanocrystals (CCP) were mixed, and the mixture was then poured into a ball mill jar and ball-milled at 200 r / min for 2 h to obtain a carbon black / CCP hybrid slurry. The carbon black / CCP hybrid slurry was diluted and spray-dried at 180°C using a spray dryer to obtain the carbon black / CCP hybrid powder, i.e., the modified aminated cellulose nanocrystal powder.
[0050] The carbon black is furnace-processed carbon black.
[0051] The carbon black / CCP mass ratio is 90 / 10.
[0052] The CCP particle size is 60 nm.
[0053] The petroleum asphalt is 70#.
[0054] The base oil is an aromatic mineral oil.
[0055] The styrene-butadiene rubber is solution-polymerized styrene-butadiene rubber (SSBR).
[0056] The coupling agent is propylenetriethoxysilane.
[0057] The inorganic filler is light calcium carbonate.
[0058] The preparation method includes the following steps:
[0059] (1) Heat petroleum asphalt to 140°C, add base oil and stir for 30 minutes to obtain mixture A;
[0060] (2) Heat to 220℃, add styrene-butadiene rubber and SBS elastomer to mixture A prepared in step 1, and stir at this temperature for 30 minutes. After stirring evenly, slowly cool to 170℃ to obtain mixture B;
[0061] (3) Add polyborosiloxane and coupling agent to the mixture B prepared in step 2, keep the temperature at 170℃ and stir for 70 min to obtain mixture C;
[0062] (4) Add the modified amino-modified cellulose nanocrystal powder to the mixture C prepared in step 3, heat it to 180°C, stir for 80 min, and obtain mixture D;
[0063] (5) Add polyborosiloxane and inorganic filler to the mixture D prepared in step 4, and cool it to 160°C for thermal crosslinking reaction. Stir at 40 rpm for 2 hours and discharge at 155°C to obtain the self-adhesive asphalt compound.
[0064] (6) Quickly pour the above self-adhesive asphalt material onto the composite aluminum mold, control the thickness of the molded sample to be 1.5 mm, then cover it with PET film and allow it to cool naturally at room temperature to obtain asphalt waterproof membrane.
[0065] Example 3
[0066] The aging-resistant self-adhesive asphalt compound provided in this embodiment comprises the following components by weight:
[0067] The composition includes 45 parts petroleum asphalt, 19 parts styrene-butadiene rubber, 6 parts modified amino-modified cellulose nanocrystal powder, 14 parts SBS, 4 parts polyborosiloxane, 24 parts inorganic filler, 0.5 parts coupling agent, and 7 parts base oil.
[0068] The modified aminated cellulose nanocrystal powder was prepared by the following method: Carbon black and an aqueous dispersion of aminated cellulose nanocrystals (CCP) were mixed at a certain mass ratio, and then the mixture was poured into a ball mill jar and ball-milled at 200 r / min for 2 h to obtain a carbon black / CCP hybrid slurry. The carbon black / CCP hybrid slurry was diluted and spray-dried at 180℃ using a spray dryer to obtain the carbon black / CCP hybrid powder, i.e., the modified aminated cellulose nanocrystal powder.
[0069] The carbon black is furnace-processed carbon black.
[0070] The carbon black / CCP mass ratio is 85 / 15.
[0071] The CCP particle size is 60 nm.
[0072] The petroleum asphalt is 70#.
[0073] The base oil is an aromatic mineral oil.
[0074] The styrene-butadiene rubber is solution-polymerized styrene-butadiene rubber (SSBR).
[0075] The coupling agent is propylenetriethoxysilane.
[0076] The inorganic filler is light calcium carbonate.
[0077] The preparation method includes the following steps:
[0078] (1) Heat petroleum asphalt to 140°C, add base oil and stir for 30 minutes to obtain mixture A;
[0079] (2) Heat to 220℃, add styrene-butadiene rubber and SBS elastomer to mixture A prepared in step 1, and stir at this temperature for 30 minutes. After stirring evenly, slowly cool to 170℃ to obtain mixture B;
[0080] (3) Add polyborosiloxane and coupling agent to the mixture B prepared in step 2, keep the temperature at 170℃ and stir for 70 min to obtain mixture C;
[0081] (4) Add the modified amino-modified cellulose nanocrystal powder to the mixture C prepared in step 3, heat it to 180°C, stir for 80 min, and obtain mixture D;
[0082] (5) Add polyborosiloxane and inorganic filler to the mixture D prepared in step 4, and cool it to 160°C for thermal crosslinking reaction. Stir at 40 rpm for 2 hours and discharge at 155°C to obtain the self-adhesive asphalt compound.
[0083] (6) Quickly pour the above self-adhesive asphalt material onto the composite aluminum mold, control the thickness of the molded sample to be 1.5 mm, then cover it with PET film and allow it to cool naturally at room temperature to obtain asphalt waterproof membrane.
[0084] Example 4
[0085] The aging-resistant self-adhesive asphalt compound provided in this embodiment comprises the following components by weight:
[0086] The composition includes 45 parts petroleum asphalt, 25 parts styrene-butadiene rubber, 7 parts modified amino-modified cellulose nanocrystal powder, 13 parts SBS, 5 parts polyborosiloxane, 23 parts inorganic filler, 0.5 parts coupling agent, and 7 parts base oil.
[0087] The modified aminated cellulose nanocrystal powder was prepared by the following method: Carbon black and an aqueous dispersion of aminated cellulose nanocrystals (CCP) were mixed, and the mixture was then poured into a ball mill jar and ball-milled at 200 r / min for 2 h to obtain a carbon black / CCP hybrid slurry. The carbon black / CCP hybrid slurry was diluted and spray-dried at 180°C using a spray dryer to obtain the carbon black / CCP hybrid powder, i.e., the modified aminated cellulose nanocrystal powder.
[0088] The carbon black is furnace-processed carbon black.
[0089] The carbon black / CCP mass ratio is 95 / 5.
[0090] The CCP particle size is 60 nm.
[0091] The petroleum asphalt is 70#.
[0092] The base oil is an aromatic mineral oil.
[0093] The styrene-butadiene rubber is solution-polymerized styrene-butadiene rubber (SSBR).
[0094] The coupling agent is a silane coupling agent, including propylenetriethoxysilane.
[0095] The inorganic filler is light calcium carbonate.
[0096] The preparation method includes the following steps:
[0097] (1) Heat petroleum asphalt to 140°C, add base oil and stir for 30 minutes to obtain mixture A;
[0098] (2) Heat to 220℃, add styrene-butadiene rubber and SBS elastomer to mixture A prepared in step 1, and stir at this temperature for 30 minutes. After stirring evenly, slowly cool to 170℃ to obtain mixture B;
[0099] (3) Add polyborosiloxane and coupling agent to the mixture B prepared in step 2, keep the temperature at 170℃ and stir for 70 min to obtain mixture C;
[0100] (4) Add the modified amino-modified cellulose nanocrystal powder to the mixture C prepared in step 3, heat it to 180°C, stir for 80 min, and obtain mixture D;
[0101] (5) Add polyborosiloxane and inorganic filler to the mixture D prepared in step 4, and cool it to 160°C for thermal crosslinking reaction. Stir at 40 rpm for 2 hours and discharge at 155°C to obtain the self-adhesive asphalt compound.
[0102] (6) Quickly pour the above self-adhesive asphalt material onto the composite aluminum mold, control the thickness of the molded sample to be 1.5 mm, then cover it with PET film and allow it to cool naturally at room temperature to obtain asphalt waterproof membrane.
[0103] Example 5
[0104] The aging-resistant self-adhesive asphalt compound provided in this embodiment comprises the following components by weight:
[0105] The composition includes 45 parts petroleum asphalt, 25 parts styrene-butadiene rubber, 7 parts modified amino-modified cellulose nanocrystal powder, 15 parts SBS, 6 parts polyborosiloxane, 20 parts inorganic filler, 0.5 parts coupling agent, and 7 parts base oil.
[0106] The modified aminated cellulose nanocrystal powder was prepared by the following method: Carbon black and an aqueous dispersion of aminated cellulose nanocrystals (CCP) were mixed, and the mixture was then poured into a ball mill jar and ball-milled at 200 r / min for 2 h to obtain a carbon black / CCP hybrid slurry. The carbon black / CCP hybrid slurry was diluted and spray-dried at 180°C using a spray dryer to obtain the carbon black / CCP hybrid powder, i.e., the modified aminated cellulose nanocrystal powder.
[0107] The carbon black is furnace-processed carbon black.
[0108] The carbon black / CCP mass ratio is 90 / 10.
[0109] The CCP particle size is 60 nm.
[0110] The petroleum asphalt is 70#.
[0111] The base oil is an aromatic mineral oil.
[0112] The styrene-butadiene rubber is solution-polymerized styrene-butadiene rubber (SSBR).
[0113] The coupling agent is propylenetriethoxysilane.
[0114] The inorganic filler is light calcium carbonate.
[0115] The preparation method includes the following steps:
[0116] (1) Heat petroleum asphalt to 140°C, add base oil and stir for 30 minutes to obtain mixture A;
[0117] (2) Heat to 220℃, add styrene-butadiene rubber and SBS elastomer to mixture A prepared in step 1, and stir at this temperature for 30 minutes. After stirring evenly, slowly cool to 170℃ to obtain mixture B;
[0118] (3) Add polyborosiloxane and coupling agent to the mixture B prepared in step 2, keep the temperature at 170℃ and stir for 70 min to obtain mixture C;
[0119] (4) Add the modified amino-modified cellulose nanocrystal powder to the mixture C prepared in step 3, heat it to 180°C, stir for 80 min, and obtain mixture D;
[0120] (5) Add polyborosiloxane and inorganic filler to the mixture D prepared in step 4, and cool it to 160°C for thermal crosslinking reaction. Stir at 40 rpm for 2 hours and discharge at 155°C to obtain the self-adhesive asphalt compound.
[0121] (6) Quickly pour the above self-adhesive asphalt material onto the composite aluminum mold, control the thickness of the molded sample to be 1.5 mm, then cover it with PET film and allow it to cool naturally at room temperature to obtain asphalt waterproof membrane.
[0122] Example 6
[0123] The aging-resistant self-adhesive asphalt compound provided in this embodiment comprises the following components by weight:
[0124] 45 parts petroleum asphalt, 25 parts styrene-butadiene rubber, 6 parts modified amino-modified cellulose nanocrystal powder, 13 parts SBS, 6 parts polyborosiloxane, 25 parts inorganic filler, 0.5 parts coupling agent, and 7 parts base oil.
[0125] The modified aminated cellulose nanocrystal powder was prepared by the following method: Carbon black and an aqueous dispersion of aminated cellulose nanocrystals (CCP) were mixed, and the mixture was then poured into a ball mill jar and ball-milled at 200 r / min for 2 h to obtain a carbon black / CCP hybrid slurry. The carbon black / CCP hybrid slurry was diluted and spray-dried at 180°C using a spray dryer to obtain the carbon black / CCP hybrid powder, i.e., the modified aminated cellulose nanocrystal powder.
[0126] The carbon black is furnace-processed carbon black.
[0127] The carbon black / CCP mass ratio is 85 / 15.
[0128] The CCP particle size is 60 nm.
[0129] The petroleum asphalt is 70#.
[0130] The base oil is an aromatic mineral oil.
[0131] The styrene-butadiene rubber is solution-polymerized styrene-butadiene rubber (SSBR).
[0132] The coupling agent is propylenetriethoxysilane.
[0133] The inorganic filler is light calcium carbonate.
[0134] The preparation method includes the following steps:
[0135] (1) Heat petroleum asphalt to 140°C, add base oil and stir for 30 minutes to obtain mixture A;
[0136] (2) Heat to 220℃, add styrene-butadiene rubber and SBS elastomer to mixture A prepared in step 1, and stir at this temperature for 30 minutes. After stirring evenly, slowly cool to 170℃ to obtain mixture B;
[0137] (3) Add polyborosiloxane and coupling agent to the mixture B prepared in step 2, keep the temperature at 170℃ and stir for 70 min to obtain mixture C;
[0138] (4) Add the modified amino-modified cellulose nanocrystal powder to the mixture C prepared in step 3, heat it to 180°C, stir for 80 min, and obtain mixture D;
[0139] (5) Add polyborosiloxane and inorganic filler to the mixture D prepared in step 4, and cool it to 160°C for thermal crosslinking reaction. Stir at 40 rpm for 2 hours and discharge at 155°C to obtain the self-adhesive asphalt compound.
[0140] (6) Quickly pour the above self-adhesive asphalt material onto the composite aluminum mold, control the thickness of the molded sample to be 1.5 mm, then cover it with PET film and allow it to cool naturally at room temperature to obtain asphalt waterproof membrane.
[0141] Comparative Example 1
[0142] The aging-resistant self-adhesive asphalt compound provided in this comparative example comprises the following components in parts by weight:
[0143] 45 parts petroleum asphalt, 25 parts styrene-butadiene rubber, 13 parts SBS, 6 parts polyborosiloxane, 30 parts inorganic filler, 0.5 parts coupling agent, and 7 parts base oil.
[0144] The carbon black is furnace-processed carbon black.
[0145] The CCP particle size is 60 nm.
[0146] The petroleum asphalt is 70#.
[0147] The base oil is an aromatic mineral oil.
[0148] The styrene-butadiene rubber is solution-polymerized styrene-butadiene rubber (SSBR).
[0149] The coupling agent is a silane coupling agent, including propylenetriethoxysilane.
[0150] The inorganic filler is light calcium carbonate.
[0151] The preparation method includes the following steps:
[0152] (1) Heat petroleum asphalt to 140°C, add base oil and stir for 30 minutes to obtain mixture A;
[0153] (2) Heat to 220℃, add styrene-butadiene rubber and SBS elastomer to mixture A prepared in step 1, and stir at this temperature for 30 minutes. After stirring evenly, slowly cool to 170℃ to obtain mixture B;
[0154] (3) Add polyborosiloxane and coupling agent to the mixture B prepared in step 2, keep the temperature at 170℃ and stir for 70 min to obtain mixture C;
[0155] (4) Add the modified amino-modified cellulose nanocrystal powder to the mixture C prepared in step 3, heat it to 180°C, stir for 80 min, and obtain mixture D;
[0156] (5) Add polyborosiloxane and inorganic filler to the mixture D prepared in step 4, and cool it to 160°C for thermal crosslinking reaction. Stir at 40 rpm for 2 hours and discharge at 155°C to obtain the self-adhesive asphalt compound.
[0157] (6) Quickly pour the above self-adhesive asphalt material onto the composite aluminum mold, control the thickness of the molded sample to be 1.5 mm, then cover it with PET film and allow it to cool naturally at room temperature to obtain asphalt waterproof membrane.
[0158] Comparative Example 2
[0159] The aging-resistant self-adhesive asphalt compound provided in this embodiment comprises the following components by weight:
[0160] 45 parts petroleum asphalt, 25 parts styrene-butadiene rubber, 6 parts modified amino-modified cellulose nanocrystal powder, 11 parts SBS, 6 parts polydimethylsiloxane, 22 parts inorganic filler, 0.5 parts coupling agent, and 7 parts base oil.
[0161] The modified aminated cellulose nanocrystal powder was prepared by the following method: Carbon black and an aqueous dispersion of aminated cellulose nanocrystals (CCP) were mixed, and the mixture was then poured into a ball mill jar and ball-milled at 200 r / min for 2 h to obtain a carbon black / CCP hybrid slurry. The carbon black / CCP hybrid slurry was diluted and spray-dried at 180°C using a spray dryer to obtain the carbon black / CCP hybrid powder, i.e., the modified aminated cellulose nanocrystal powder.
[0162] The carbon black is furnace-processed carbon black.
[0163] The carbon black / CCP mass ratio is 95 / 5.
[0164] The CCP particle size is 60 nm.
[0165] The petroleum asphalt is 70#.
[0166] The base oil is an aromatic mineral oil.
[0167] The styrene-butadiene rubber is solution-polymerized styrene-butadiene rubber (SSBR).
[0168] The coupling agent is propylenetriethoxysilane.
[0169] The inorganic filler is light calcium carbonate.
[0170] The preparation method includes the following steps:
[0171] (1) Heat petroleum asphalt to 140°C, add base oil and stir for 30 minutes to obtain mixture A;
[0172] (2) Heat to 220℃, add styrene-butadiene rubber and SBS elastomer to mixture A prepared in step 1, and stir at this temperature for 30 minutes. After stirring evenly, slowly cool to 170℃ to obtain mixture B;
[0173] (3) Add polyborosiloxane and coupling agent to the mixture B prepared in step 2, keep the temperature at 170℃ and stir for 70 min to obtain mixture C;
[0174] (4) Add the modified amino-modified cellulose nanocrystal powder to the mixture C prepared in step 3, heat it to 180°C, stir for 80 min, and obtain mixture D;
[0175] (5) Add polyborosiloxane and inorganic filler to the mixture D prepared in step 4, and cool it to 160°C for thermal crosslinking reaction. Stir at 40 rpm for 2 hours and discharge at 155°C to obtain the self-adhesive asphalt compound.
[0176] (6) Quickly pour the above self-adhesive asphalt material onto the composite aluminum mold, control the thickness of the molded sample to be 1.5 mm, then cover it with PET film and allow it to cool naturally at room temperature to obtain asphalt waterproof membrane.
[0177] Performance testing
[0178] The prepared asphalt waterproof membrane underwent an aging test. The aging time and temperature were 10 days and 70℃, respectively, and the test conditions were hot aging in a forced-air oven. After the aging test, the tensile properties, nail tear strength, tack, peel strength, and appearance of the asphalt waterproof membrane before and after aging were compared according to the relevant provisions of GB / T18244 2000 "Test Methods for Aging of Building Waterproofing Materials". Specific data are shown in Tables 1 and 2.
[0179] Table 1
[0180]
[0181] Table 2
[0182]
[0183]
[0184] A comparison of the data in Tables 1 and 2 shows that in Comparative Example 1, no modified amino-modified cellulose nanocrystal powder was used, resulting in a decrease in all properties after heat aging. In Comparative Example 2, polydimethylsilane was used instead of polyborosiloxane, leading to a significant decrease in nail tear strength and peel strength after heat aging, and the appearance of cracks. Compared to Comparative Examples 1-2, Examples 1-6 showed little decrease in the main properties of the asphalt waterproof membrane, such as tensile properties, nail tear strength, tackiness, and peel strength, after heat aging, and no cracks appeared on the surface after aging. Therefore, the self-adhesive asphalt compound of the present invention exhibits excellent resistance to heat aging and oxidation aging when used to make asphalt waterproof membranes.
Claims
1. An aging-resistant self-adhesive asphalt compound, characterized in that: By weight, it includes the following components:
2. The aging-resistant self-adhesive asphalt compound according to claim 1, characterized in that: The modified amino-modified cellulose nanocrystal powder is obtained by ball milling and spray drying carbon black and amino-modified cellulose nanocrystals.
3. The aging-resistant self-adhesive asphalt compound according to claim 2, characterized in that: The mass ratio of carbon black to amino-modified cellulose nanocrystals is 85-95:5-15.
4. The aging-resistant self-adhesive asphalt compound according to claim 1, characterized in that: The inorganic filler is one or more of the following: light calcium carbonate, heavy calcium carbonate, clay, talc powder, mica powder, montmorillonite, fly ash, and cement powder.
5. The aging-resistant self-adhesive asphalt compound according to claim 1, characterized in that: The coupling agent is a silane coupling agent.
6. The aging-resistant self-adhesive asphalt compound according to claim 1, characterized in that: The base oil is one or more of aromatic mineral oils and naphthenic mineral oils.
7. A method for preparing an aging-resistant self-adhesive asphalt compound as described in any one of claims 1-6, comprising the following steps: (1) Heat the petroleum asphalt to 140-150℃ according to the weight parts, add the base oil and stir to obtain mixture A; (2) Then heat the mixture to 210-230℃, add styrene-butadiene rubber and styrene-butadiene-styrene block copolymer to mixture A, and stir for 30-40 minutes. After stirring evenly, slowly cool the mixture to 170-175℃ to obtain mixture B. (3) Add polyborosiloxane and coupling agent to mixture B, maintain the temperature at 170-175℃, stir for 60-80 min to obtain mixture C; (4) Add the modified amino-modified cellulose nanocrystal powder to mixture C, heat to 180-190℃, stir for 70-90 min to obtain mixture D; (5) Add inorganic filler to mixture D, cool to 160-170℃ for thermal crosslinking reaction, stir at 30-50 rpm for 1-2 hours, and discharge at 155-165℃ to obtain the self-adhesive asphalt compound.
8. An aging-resistant self-adhesive bitumen compound as described in any one of claims 1-6 is used in the preparation of bitumen waterproof membranes.
9. The application according to claim 8, characterized in that: The self-adhesive asphalt compound is poured onto the base material, then covered with a PET film and allowed to cool naturally at room temperature to obtain the asphalt waterproof membrane.