CN114437650B - High-heat-resistant creep waterproof butyl pressure-sensitive adhesive and preparation method thereof - Google Patents
High-heat-resistant creep waterproof butyl pressure-sensitive adhesive and preparation method thereof Download PDFInfo
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- CN114437650B CN114437650B CN202111633915.2A CN202111633915A CN114437650B CN 114437650 B CN114437650 B CN 114437650B CN 202111633915 A CN202111633915 A CN 202111633915A CN 114437650 B CN114437650 B CN 114437650B
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- 239000004820 Pressure-sensitive adhesive Substances 0.000 title claims abstract description 68
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 229920005549 butyl rubber Polymers 0.000 claims abstract description 61
- 229920005989 resin Polymers 0.000 claims abstract description 44
- 239000011347 resin Substances 0.000 claims abstract description 44
- 239000003208 petroleum Substances 0.000 claims abstract description 42
- 239000000945 filler Substances 0.000 claims abstract description 22
- 239000007822 coupling agent Substances 0.000 claims abstract description 21
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 19
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 19
- 229920002367 Polyisobutene Polymers 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 16
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 7
- 229920001935 styrene-ethylene-butadiene-styrene Polymers 0.000 claims abstract 7
- 238000003756 stirring Methods 0.000 claims description 17
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 239000000203 mixture Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 13
- 238000002156 mixing Methods 0.000 claims description 11
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 8
- 239000003999 initiator Substances 0.000 claims description 8
- -1 2,2,6,6-tetramethylpiperidinyl Chemical group 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 239000007800 oxidant agent Substances 0.000 claims description 5
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 4
- OLFNXLXEGXRUOI-UHFFFAOYSA-N 2-(benzotriazol-2-yl)-4,6-bis(2-phenylpropan-2-yl)phenol Chemical compound C=1C(N2N=C3C=CC=CC3=N2)=C(O)C(C(C)(C)C=2C=CC=CC=2)=CC=1C(C)(C)C1=CC=CC=C1 OLFNXLXEGXRUOI-UHFFFAOYSA-N 0.000 claims description 4
- 238000007605 air drying Methods 0.000 claims description 4
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000004806 packaging method and process Methods 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- ZSSVCEUEVMALRD-UHFFFAOYSA-N 2-[4,6-bis(2,4-dimethylphenyl)-1,3,5-triazin-2-yl]-5-(octyloxy)phenol Chemical compound OC1=CC(OCCCCCCCC)=CC=C1C1=NC(C=2C(=CC(C)=CC=2)C)=NC(C=2C(=CC(C)=CC=2)C)=N1 ZSSVCEUEVMALRD-UHFFFAOYSA-N 0.000 claims description 3
- 239000005995 Aluminium silicate Substances 0.000 claims description 3
- HECLRDQVFMWTQS-UHFFFAOYSA-N Dicyclopentadiene Chemical class C1C2C3CC=CC3C1C=C2 HECLRDQVFMWTQS-UHFFFAOYSA-N 0.000 claims description 3
- 235000012211 aluminium silicate Nutrition 0.000 claims description 3
- 239000012964 benzotriazole Substances 0.000 claims description 3
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 3
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000010445 mica Substances 0.000 claims description 3
- 229910052618 mica group Inorganic materials 0.000 claims description 3
- KDYFGRWQOYBRFD-UHFFFAOYSA-L succinate(2-) Chemical compound [O-]C(=O)CCC([O-])=O KDYFGRWQOYBRFD-UHFFFAOYSA-L 0.000 claims description 3
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 3
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 claims description 3
- 229940116351 sebacate Drugs 0.000 claims description 2
- CXMXRPHRNRROMY-UHFFFAOYSA-L sebacate(2-) Chemical compound [O-]C(=O)CCCCCCCCC([O-])=O CXMXRPHRNRROMY-UHFFFAOYSA-L 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 27
- 239000004576 sand Substances 0.000 abstract description 12
- 230000001070 adhesive effect Effects 0.000 abstract description 10
- 239000000853 adhesive Substances 0.000 abstract description 8
- 238000012360 testing method Methods 0.000 description 40
- 239000005038 ethylene vinyl acetate Substances 0.000 description 32
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 32
- 230000000052 comparative effect Effects 0.000 description 22
- 238000006243 chemical reaction Methods 0.000 description 11
- 150000003254 radicals Chemical class 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 238000010276 construction Methods 0.000 description 7
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 6
- 230000032683 aging Effects 0.000 description 6
- 239000011083 cement mortar Substances 0.000 description 6
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical group CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 4
- 239000004568 cement Substances 0.000 description 4
- 239000003292 glue Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- XYLMUPLGERFSHI-UHFFFAOYSA-N alpha-Methylstyrene Chemical compound CC(=C)C1=CC=CC=C1 XYLMUPLGERFSHI-UHFFFAOYSA-N 0.000 description 3
- 239000000155 melt Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical compound CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 2
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical compound CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 229920001971 elastomer Polymers 0.000 description 2
- 229920001903 high density polyethylene Polymers 0.000 description 2
- 239000004700 high-density polyethylene Substances 0.000 description 2
- 239000012943 hotmelt Substances 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000011120 plywood Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000004224 protection Effects 0.000 description 2
- HFZUCAXQSOLOAD-UHFFFAOYSA-N C(CCCCCCCCC(=O)O)(=O)O.CC1(N(C(CCC1)(C)C)O)C Chemical compound C(CCCCCCCCC(=O)O)(=O)O.CC1(N(C(CCC1)(C)C)O)C HFZUCAXQSOLOAD-UHFFFAOYSA-N 0.000 description 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 239000011398 Portland cement Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000006750 UV protection Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000010073 coating (rubber) Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 125000004185 ester group Chemical group 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-M hydroperoxide group Chemical group [O-]O MHAJPDPJQMAIIY-UHFFFAOYSA-M 0.000 description 1
- 150000002432 hydroperoxides Chemical class 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000007719 peel strength test Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 230000005501 phase interface Effects 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 230000036316 preload Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Chemical group 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000009864 tensile test Methods 0.000 description 1
- 238000003878 thermal aging Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
- C09J123/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
- C09J123/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
- C09J123/22—Copolymers of isobutene; Butyl rubber ; Homo- or copolymers of other iso-olefines
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J157/00—Adhesives based on unspecified polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09J157/02—Copolymers of mineral oil hydrocarbons
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/302—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being pressure-sensitive, i.e. tacky at temperatures inferior to 30°C
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a high-heat-resistant creep waterproof butyl pressure-sensitive adhesive and a preparation method thereof, wherein the high-heat-resistant creep waterproof butyl pressure-sensitive adhesive is prepared from the following components in parts by weight: 10-70 parts of butyl rubber, 20-40 parts of polyisobutylene, 1-5 parts of antioxidant, 20-50 parts of petroleum resin, 5-10 parts of SEBS, 5-10 parts of MAH-g-EVA, 10-40 parts of filler, 1-5 parts of anti-ultraviolet agent and 1-5 parts of coupling agent. The invention has the innovation points that the butyl rubber, the SEBS and the MAH-g-EVA are selected and matched with other auxiliary agents, the heat-resistant creep of the butyl rubber can be greatly improved under the condition that the bonding performance of the butyl pressure-sensitive adhesive is kept, and the sand surface of the waterproof coiled material is ensured not to overflow the adhesive at high temperature and not to stick the coil after being stored for a long time.
Description
Technical Field
The invention relates to a pressure-sensitive adhesive technology, in particular to a high-heat-resistant creep waterproof butyl pressure-sensitive adhesive and a preparation method thereof.
Background
Butyl rubber pressure-sensitive adhesive is more and more used on macromolecule waterproof coiled materials due to excellent waterproof effect, however, the existing butyl rubber waterproof adhesive has serious cold flow, when macromolecule pre-paved waterproof coiled materials coated by the butyl rubber waterproof adhesive are placed for a long time, the butyl rubber pressure-sensitive adhesive can be adhered to the back of the coiled materials, and the coiled materials can not be unfolded during construction. At high temperature, the flow of butyl rubber pressure-sensitive adhesive molecules is accelerated, the adhesive overflows from the sand surface, and the foot is stuck during the construction of workers, so that the subsequent construction cannot be carried out. In the prior art, a report of a waterproof coiled material butyl rubber is provided, for example, the disclosure No. CN107603537A, the invention is named as a hot-melt pressure-sensitive adhesive and a preparation method thereof, SEBS and alpha-methyl styrene are introduced to improve the heat-resistant creep property of the butyl rubber, and the problems of no flowing, no dripping and no displacement of the butyl rubber after being aged for 2h by hot air at 70 ℃, but the solubility parameter (delta = 8.7) of the alpha-methyl styrene resin is too close to the styrene phase (delta = 9.1) of an SEBS rigid chain segment, the alpha-methyl styrene resin can be compatible with the styrene phase (delta = 9.1), the SEBS rigid styrene phase segment is damaged, the heat resistance of a system is reduced, the cold flow property of the butyl pressure-sensitive adhesive cannot be reduced, and the coiled material is sticky and has sand surface overflow. The invention discloses a preparation method of EVA or AEM modified butyl rubber pressure-sensitive adhesive with publication number CN110862792A, which utilizes ester group of EVA or AEM to improve the bonding strength of color steel plates, cement plates and the like, but EVA and butyl rubber have different polarities and are incompatible, cannot be fused into a butyl rubber molecular system, and cannot improve the heat-resistant creep property of butyl rubber.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a waterproof butyl pressure-sensitive adhesive with high thermal creep resistance.
The second purpose of the invention is to provide a preparation method of the high heat-resistant creep waterproof butyl pressure-sensitive adhesive.
One of the purposes of the invention is realized by adopting the following technical scheme: the high-heat-resistance creep-resistant waterproof butyl pressure-sensitive adhesive is prepared from the following components in parts by weight: 10-70 parts of butyl rubber, 20-40 parts of polyisobutylene, 1-5 parts of antioxidant, 20-50 parts of petroleum resin, 5-10 parts of SEBS, 5-10 parts of MAH-g-EVA, 10-40 parts of filler, 1-5 parts of anti-ultraviolet agent and 1-5 parts of coupling agent.
Further, the high heat-resistant creep-resistant waterproof butyl pressure-sensitive adhesive is prepared from the following components in parts by weight: 15-30 parts of butyl rubber, 22-30 parts of polyisobutylene, 1-3 parts of antioxidant, 20-30 parts of petroleum resin, 5-8 parts of SEBS, 5-8 parts of MAH-g-EVA, 15-30 parts of filler, 1-2 parts of anti-ultraviolet agent and 1-2 parts of coupling agent.
Further, the mass ratio of the butyl rubber, the SEBS and the MAH-g-EVA is (2-6): 1:1.
Further, the MAH-g-EVA is prepared by the following method:
adding a certain amount of MAH and initiator DCP into acetone as a solvent, uniformly stirring and dissolving, mixing and stirring with EVA in a high-speed stirrer for 5-10min, discharging, mixing, melting and grafting at 150-180 ℃ by a double-screw extruder, granulating, air drying, and packaging for later use;
the mass ratio of the MAH to the EVA is (1-3): 100, respectively; the mass ratio of the initiator DCP to the EVA is (0.2-2): 100, respectively; the mass ratio of the acetone to the MAH is (1-5): 1.
further, the antioxidant is a mixture of two selected from an oxidant 1010 and an oxidant 168.
Further, the petroleum resin is selected from one or a mixture of more than two of C5 petroleum resin, C9 petroleum resin, C5/C9 copolymerized petroleum resin, hydrogenated DCPD petroleum resin, hydrogenated C5 petroleum resin or hydrogenated C9 petroleum resin.
Further, the filler is selected from one or a mixture of more than two of calcium carbonate, kaolin, mica powder and transparent powder.
Further, the anti-uv agent is selected from one or a mixture of two or more of 2- (2H-benzotriazol-2-yl) -4,6-bis (1-methyl-1-phenylethyl) phenol, 2- [4,6-bis (2,4-dimethylphenyl) -1,3,5-triazin-2-yl ] -5- (octyloxy) phenol, 2- (2, -hydroxy-5, -methyl) -benzotriazole, [1- (2, -hydroxy) -2,2,6,6-tetramethyl-4-hydroxypiperidine succinate ], bis 2,2,6,6-tetramethylpiperidinol sebacate, poly- { [6- [ (1,1,3,3, -tetramethylbutyl) -amino ]1,3,5, -triazine-2,4-diyl ] [ (2,2,6,6-tetramethylpiperidinyl) -imino ] -1,6-hexanediyl- [ (2,2,6,6-tetramethylpiperidinyl) -imino ] }.
The coupling agent is one or more of methyl triethoxysilane, vinyl triethoxysilane, gamma-aminopropyl triethoxysilane, gamma- (2,3-glycidoxy) propyl trimethoxysilane and gamma- (methacryloyloxy) propyl trimethoxysilane.
The second purpose of the invention is realized by adopting the following technical scheme: a preparation method of a high heat-resistant creep waterproof butyl pressure-sensitive adhesive specifically comprises the following steps:
(1) Adding polyisobutylene and an antioxidant in a formula ratio into a kneader, and heating to 160 +/-5 ℃;
(2) Then adding the butyl rubber, SEBS, MAH-g-EVA, the coupling agent and the filler according to the formula ratio, stirring for 50min in vacuum, and keeping the temperature at 160 +/-5 ℃;
(3) Finally, adding the petroleum resin and the anti-ultraviolet auxiliary agent in the formula amount, uniformly stirring in vacuum for 20min, keeping the temperature at 145 +/-5 ℃, discharging, and cooling to room temperature to obtain the high-heat-resistance creep waterproof butyl pressure-sensitive adhesive;
the high heat-resistant creep waterproof butyl pressure-sensitive adhesive comprises the following components in parts by weight: 10-70 parts of butyl rubber, 20-40 parts of polyisobutylene, 1-5 parts of antioxidant, 20-50 parts of petroleum resin, 5-10 parts of SEBS, 5-10 parts of MAH-g-EVA, 10-40 parts of filler, 1-5 parts of anti-ultraviolet agent and 1-5 parts of coupling agent.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, through the selection of the butyl rubber, the SEBS and the MAH-g-EVA, and the combination of other auxiliary agents, the heat-resistant creep of the butyl rubber can be greatly improved under the condition that the bonding performance of the butyl pressure-sensitive adhesive is maintained in the whole system, and the sand surface of the waterproof coiled material is ensured not to overflow glue at high temperature and not to be stuck to a roll after being stored for a long time.
Detailed Description
The present invention is further described below with reference to specific embodiments, and it should be noted that, without conflict, various embodiments or technical features described below may be arbitrarily combined to form a new embodiment.
In the present invention, all parts and percentages are by weight, unless otherwise specified, and the equipment and materials used are commercially available or commonly used in the art. The methods in the following examples are conventional in the art unless otherwise specified.
The invention also provides a high heat-resistant creep waterproof butyl pressure-sensitive adhesive which is prepared from the following components in parts by weight: 10-70 parts of butyl rubber, 20-40 parts of polyisobutylene, 1-5 parts of antioxidant, 20-50 parts of petroleum resin, 5-10 parts of SEBS, 5-10 parts of MAH-g-EVA, 10-40 parts of filler, 1-5 parts of anti-ultraviolet agent and 1-5 parts of coupling agent.
As a further embodiment, the high thermal creep resistant waterproof butyl pressure-sensitive adhesive is prepared from the following components in parts by weight: 15-30 parts of butyl rubber, 22-30 parts of polyisobutylene, 1-3 parts of antioxidant, 20-30 parts of petroleum resin, 5-8 parts of SEBS, 5-8 parts of MAH-g-EVA, 15-30 parts of filler, 1-2 parts of anti-ultraviolet agent and 1-2 parts of coupling agent.
The invention belongs to the field of pressure-sensitive adhesives for waterproof coiled materials, and butyl rubber is a copolymer synthesized by isobutene and a small amount of isoprene, has few unsaturated bonds, excellent weather resistance, extremely low air permeability and good waterproof effect; however, the pure butyl rubber pressure-sensitive adhesive has serious cold flow, the coiled material is stored for a long time, or when the coiled material is at high temperature, the sand surface of the coiled material can sink into the pressure-sensitive adhesive layer to cause coil sticking, and the foot sticking cannot be performed during the construction of workers; the invention improves the heat-resistant creep property of butyl rubber by adding SEBS (styrene-ethylene butylene block copolymer) and MAH-g-EVA (maleic anhydride modified ethylene-vinyl acetate copolymer). SEBS and MAH-g-EVA are both high polymer molecules, and the important characteristic of SEBS is that two phases are separated, the middle section is a continuous ethylene-butylene rubber phase chain segment, and the end group is a dispersed polystyrene plastic phase chain segment. The invention selects MAH-g-EVA, the modified EVA has a three-dimensional network result, when the butyl rubber is added with SEBS and MAH-g-EVA high polymer at the same time, the network of the SEBS and the MAH-g-EVA are mutually cross-linked and entangled, the butyl rubber pressure-sensitive adhesive permeates into the network to form a system with soft dispersed phase and hard continuous phase, and the MAH-g-EVA improves the polarity of the EVA, promotes the compatibility of the SEBS, the butyl rubber and the MAH-g-EVA, and promotes the intermolecular growth chain entanglement of the three systems, improves the heat-resistant creep of the butyl pressure-sensitive adhesive, and the system can greatly improve the heat-resistant creep of the butyl rubber under the condition of keeping the basic performance of the butyl pressure-sensitive adhesive, so that the sand surface of the waterproof roll is free of glue overflow at high temperature for a long time, and the roll is not sticky after being stored for a long time.
The polyisobutylene is added to play a plasticizing role, so that the mixing processing of three systems of butyl rubber, SEBS and MAH-g-EVA is facilitated; and compared with the traditional rubber oil plasticizer, the polyisobutylene has a longer molecular chain, has the same polarity with the butyl rubber, has good compatibility, is entangled among molecules during processing and mixing, and is not easy to extract at high temperature.
The petroleum resin mainly has a tackifying effect and improves the adhesiveness of the butyl rubber.
The thermal oxidation process of organic compounds is a series of free radical chain reactions, and under the action of heat, light or oxygen, chemical bonds of organic molecules are broken to generate active free radicals and hydroperoxides. The hydroperoxide undergoes decomposition reactions, which also generate hydroxyl radicals and hydroxyl radicals. These radicals can initiate a series of radical chain reactions leading to fundamental changes in the structure and properties of organic compounds. The antioxidant of the present invention has the function of eliminating the free radicals just generated or promoting the decomposition of hydroperoxide to prevent the chain reaction.
The addition of the filler of the invention has the effects of reducing the cost and improving the elastic modulus of the butyl rubber so as to improve the heat-resistant creep property of the butyl rubber.
The ultraviolet resistant agent of the invention is added to absorb ultraviolet rays, so that the ultraviolet resistant agent becomes harmless energy to be released or consumed, thereby not preventing the degradation and damage effect on the butyl rubber.
The invention introduces the coupling agent, improves the compatibility of the filler and an organic system, enables the filler to be uniformly embedded into the SEBS and MAH-g-EVADE entangled network, improves the rigidity of the system under the condition of ensuring viscoelasticity, improves the heat-resistant slippage performance of the SEBS and MAH-g-EVA molecular networks, and further improves the heat-resistant creep deformation of the butyl rubber.
In a further embodiment, the mass ratio of the butyl rubber, the SEBS and the MAH-g-EVA is (2-6): 1:1. The mass ratio of butyl rubber, SEBS and MAH-g-EVA is 4: 5363 the relationship of 1:1 is to optimize the compatibility of the SEBS, the butyl rubber and the MAH-g-EVA, improve the heat-resistant creep of the butyl pressure-sensitive adhesive due to the entanglement of the growth chain among the molecules of the three systems, and not only improve the adhesive property of the butyl pressure-sensitive adhesive, but also greatly improve the heat-resistant creep of the butyl adhesive.
As a further embodiment, the MAH-g-EVA is prepared by the following method:
adding a certain amount of MAH and initiator DCP into acetone as a solvent, uniformly stirring and dissolving, mixing and stirring with EVA in a high-speed stirrer for 5-10min, discharging, mixing, melting and grafting at 150-180 ℃ by a double-screw extruder, granulating, air drying, and packaging for later use;
the mass ratio of the MAH to the EVA is (1-3): 100, respectively; the mass ratio of the initiator DCP to the EVA is (0.2-2): 100, respectively; the mass ratio of the acetone to the MAH is (1-5): 1.
the VA content of the MAH-g-EVA is determined by the VA content of the EVA, the VA content is less than 25 percent, the polarity is low, the compatibility with the MAH is poor, the grafting rate is low, and the heat resistance of the butyl rubber cannot be improved. The content of VA is more than 30 percent, the content of EVA vinyl acetate chain segments is more, more macromolecular free radicals are generated in the same time, but because the strongly polar MAH monomer forms a separated phase in the melting grafting process and reacts at a two-phase interface, the macromolecular free radicals are easy to react with each other under more conditions to be consumed, so that the EVA body is copolymerized, the grafting rate with the MAH is low, the test shows that the effect of combining the cost and the availability of materials is optimal, and the VA content is 28 percent.
As a further embodiment, the antioxidant is selected from a mixture of two of the oxidants 1010, 168.
As a further embodiment, the petroleum resin is selected from one or a mixture of two or more of C5 petroleum resin, C9 petroleum resin, C5/C9 copolymerized petroleum resin, hydrogenated DCPD petroleum resin, hydrogenated C5 petroleum resin, or hydrogenated C9 petroleum resin.
As a further embodiment, the filler is selected from one or a mixture of two or more of calcium carbonate, kaolin, mica powder and transparent powder.
As a further embodiment, the anti-UV agent is selected from one or more of 2- (2H-benzotriazol-2-yl) -4,6-bis (1-methyl-1-phenylethyl) phenol, 2- [4,6-bis (2,4-dimethylphenyl) -1,3,5-triazin-2-yl ] -5- (octyloxy) phenol, 2- (2, -hydroxy-5, -methyl) -benzotriazole, [1- (2, -hydroxy) -2,2,6,6-tetramethyl-4-hydroxypiperidine succinate ], bis 2,2,6,6, -tetramethylpiperidinol sebacate, poly- { [6- [ (1,1,3,3, -tetramethylbutyl) -amino ]1,3,5, -triazine-2,4-diyl ] [ (3264 zxft) -tetramethylpiperidinyl) -imino ] -1,6-hexanediyl- [ (3434 zxft) -3434-tetramethylpiperidinyl) -imino ] }.
In a further embodiment, the coupling agent is selected from the group consisting of methyltriethoxysilane, vinyltriethoxysilane, gamma-aminopropyltriethoxysilane, gamma- (2,3-glycidoxy) propyltrimethoxysilane, gamma- (methacryloyloxy) propyltrimethoxysilane, and mixtures of two or more thereof.
The invention also provides a preparation method of the high-heat-resistant creep waterproof butyl pressure-sensitive adhesive, which comprises the following steps:
(1) Adding polyisobutylene and an antioxidant in a formula ratio into a kneader, and heating to 160 +/-5 ℃;
(2) Then adding the butyl rubber, SEBS, MAH-g-EVA, the coupling agent and the filler according to the formula ratio, stirring for 50min in vacuum, and keeping the temperature at 160 +/-5 ℃;
(3) Finally, adding the petroleum resin and the anti-ultraviolet auxiliary agent in the formula amount, uniformly stirring in vacuum for 20min, keeping the temperature at 145 +/-5 ℃, discharging, and cooling to room temperature to obtain the high-heat-resistance creep waterproof butyl pressure-sensitive adhesive;
the high heat-resistant creep waterproof butyl pressure-sensitive adhesive comprises the following components in parts by weight: 10-70 parts of butyl rubber, 20-40 parts of polyisobutylene, 1-5 parts of antioxidant, 20-50 parts of petroleum resin, 5-10 parts of SEBS, 5-10 parts of MAH-g-EVA, 10-40 parts of filler, 1-5 parts of anti-ultraviolet agent and 1-5 parts of coupling agent.
The following are specific examples of the present invention, and raw materials, equipments and the like used in the following examples can be obtained by purchasing them unless otherwise specified.
Examples 1 to 4 and comparative examples 1 to 6
The raw materials are weighed according to the mixture ratio in the following table 1, the pressure-sensitive adhesive is prepared according to the preparation method after the table 1, and the pressure-sensitive adhesives of different embodiments are correspondingly obtained, and the details are shown in the table 1:
TABLE 1 raw material proportioning tables for examples 1-4 and comparative examples 1-6
Wherein, mooney viscosity ML100 ℃ of the butyl rubber in the table 1 is 1+4, and the polyisobutene adopts the polyisobutene which is the Shandong Hongyi petrochemical industry Co.Ltd. number 6095; the antioxidant adopts 1010 of Basff; the petroleum resin is hydrogenated petroleum resin; MAH-g-EVA was prepared by the following method, the VA content of MAH-g-EVA of examples 1-4 and comparative examples 1-4 was 28%, the VA content of MAH-g-EVA of comparative example 5 was 14%, and the VA content of MAH-g-EVA of comparative example 6 was 33%; the filler adopts calcium carbonate; 2- (2H-benzotriazole-2-yl) -4,6-di (1-methyl-1-phenylethyl) phenol is adopted as the uvioresistant agent; the coupling agent adopts gamma-aminopropyl triethoxysilane.
Examples 1-4 and comparative examples 1-6, comprising the steps of:
(1) Adding polyisobutylene and an antioxidant in a formula ratio into a kneader, and heating to 160 +/-5 ℃;
(2) Then adding the butyl rubber, SEBS, MAH-g-EVA, the coupling agent and the filler according to the formula ratio, stirring for 50min in vacuum, and keeping the temperature at 160 +/-5 ℃;
(3) And finally, adding the petroleum resin and the anti-ultraviolet auxiliary agent in the formula amount, uniformly stirring in vacuum for 20min, keeping the temperature at 145 +/-5 ℃, discharging, and cooling to room temperature to obtain the butyl pressure-sensitive adhesive.
The MAH-g-EVA is prepared by the following method: adding a certain amount of MAH and initiator DCP into acetone as a solvent, uniformly stirring and dissolving, mixing and stirring with EVA in a high-speed stirrer for 5-10min, discharging, mixing, melting and grafting at 150-180 ℃ by a double-screw extruder, granulating, air drying, and packaging for later use; the mass ratio of the MAH to the EVA of the examples 1-4 and the comparative examples 1-6 is 2:100, respectively; the mass ratio of the initiator DCP to the EVA is 1.5:100, respectively; the mass ratio of the acetone to the MAH is 3:1.
taking example 4 as an example, comparative example 1 is different from example 4 in that a petroleum resin is substituted for butyl rubber, and the remaining components are used in the same amount.
Taking example 4 as an example, comparative example 2 is different from example 4 in that a petroleum resin is substituted for SEBS, and the rest components are used in the same amount.
Taking example 4 as an example, comparative example 3 is different from example 4 in that a petroleum resin is substituted for MAH-g-EVA, and the remaining components are in the same amount.
Taking example 4 as an example, comparative example 4 is different from example 4 in that a petroleum resin is substituted for the coupling agent, and the remaining components are used in the same amount.
Taking example 4 as an example, comparative example 5 is different from example 4 in that the VA of the EVA selected is 14, and the other components and the using amount are the same.
Taking example 4 as an example, comparative example 6 is different from example 4 in that EVA selected has VA of 33, and the rest components and the use amount are the same.
Comparative example 7 is a product of the prior art, self-made according to the instruction manual example 3 of publication No. CN107603537a entitled "hot melt type pressure sensitive adhesive and method for preparing the same".
Comparative example 8 is a prior art product, homemade according to the instruction of publication No. CN110862792a entitled "method for preparing EVA or AEM modified butyl rubber pressure sensitive adhesive" example 1.
Effect evaluation and Performance detection
The butyl pressure sensitive adhesives of examples 1-4 and comparative examples 1-8 were tested for their properties, and the test items and results are shown in tables 2-3.
Preparing a coiled material: the butyl rubber pressure sensitive adhesive obtained according to the embodiment and the comparative example is uniformly coated on an HDPE coil with the thickness of 1.0mm, the coating thickness is 300 +/-10 mu m, then cement sand is spread on the surface of the adhesive, a 2kg roller is used for pressing back and forth twice, the sand is compacted, floating sand is removed by a brush, and the waterproof coil is prepared.
1. Heat resistance test
The method comprises the following steps of removing antisticking materials from coiled materials, cutting the coiled materials into test pieces with the longitudinal length of 100mm and the transverse length of 50mm, wherein the number of the test pieces is 3, adhering the test pieces on a plywood which is at least 10mm larger than the edge of the test piece, enabling butyl rubber to face outwards, vertically suspending the plywood in an oven which is adjusted to be (120 +/-2) DEG C, aging for 2h, measuring the slippage between a rubber coating layer at any end of the test piece and HDPE by using a ruler with the precision of 0.5mm, and taking the value of the test piece with the maximum slippage as the slippage test result, wherein the smaller the numerical value is, the better the heat-resistant creep is represented.
2. Low temperature flexibility test
The waterproof coiled material is cut into test pieces with the length of 150mm and the width of 25mm, the number of the test pieces is 10, the upper surfaces of the 5 test pieces, the lower surfaces of the 5 test pieces are respectively tested, the diameter of a bending shaft is 30mm, the temperature of the environment is minus 35 ℃, the test is carried out for 2h, the low-temperature flexibility is tested, the butyl pressure-sensitive adhesive layer has no crack, and the low-temperature flexibility is indicated to pass.
3. Glue overflow test
The coiled material is cut into a test piece with the thickness of 150mm multiplied by 50mm, the sand surface is upward, the test piece is horizontally placed into an oven which is adjusted to the temperature of (70 +/-2), the aging time when the glue overflow phenomenon occurs is recorded, the aging time is recorded in days (d), and the longer the time is, the better the heat-resistant creep deformation is.
4. Non-treated Cement mortar Peel Strength test
The size of the bonding surface of the test piece is 70mm multiplied by 50mm, cement mortar is stirred by an automatic cement stirring machine according to a standard proportion, a mold with the size of 130mm multiplied by 50mm is placed on the polymer coiled material, the bonding surface is upward, the stirred cement mortar is poured into the mold, the mixture is compacted for 20s and the thickness is 30-50mm, 5 test pieces are manufactured at one time, the test pieces are placed at the temperature of (20 +/-2) DEG C for 24h and are demoulded, and the test pieces are maintained for 7d under the standard maintenance condition. Wherein, the mixing proportion of cement mortar is as follows: strength grade 42.5 portland cement to ISO standard sand to water = 1: 2: 0.4.
The test piece is placed in a (23 +/-2) DEG C chamber for 4h, a mortar board is arranged on a clamp at one end of a testing machine, one end of the coiled material which is not bonded is turned over by 180 degrees and is clamped in a clamp at the other end of the testing machine, so that the longitudinal axis of the test piece is superposed with the axes of the tensile testing machine and the clamp, the distance between the clamps is at least 100mm, and the pre-load is not born. The test was carried out at (23. + -.2) ℃ and the tensile rate was (100. + -.10) mm/min, the average force divided by the specimen width was taken as the peel strength in N/mm, and the test results were taken as the arithmetic average of the results of 5 specimens, with larger values being better. The pressure-sensitive adhesive is mainly used for bonding the waterproof board and the building main body, and the higher the peeling strength is, the better the bonding strength is, and the better the waterproof effect is.
5. Test of peel strength of cement mortar after thermal aging treatment
And (3) removing the isolation material on the surface of the test piece, horizontally placing the test piece in a (70 +/-2) DEG C oven for (168 +/-2) h, taking out the test piece, placing the test piece in a (23 +/-2) DEG C chamber for 24h, and testing the peel strength of the test piece in a non-treatment mode, wherein the larger the numerical value is, the better the heat-resistant aging performance of the butyl pressure-sensitive adhesive is.
6. Test of peeling strength of cement mortar after ultraviolet aging
Removing the surface isolation material of the test piece, placing the test piece with the adhesive surface facing upwards into a xenon arc lamp aging instrument meeting the requirements of GB/T16422.2, wherein the radiation intensity is (60 +/-2) W/m2 (300 nm-400 nm), and the black mark temperature is (65 +/-3) DEG C. Spraying for 18min every 2h while irradiating, and accumulating the irradiation time for 72h +/-5 min. Taking out, placing in a room at (23 +/-2) DEG C for 24h, and testing the peel strength of the butyl pressure-sensitive adhesive in a non-treatment mode, wherein the larger the value is, the better the ultraviolet resistance of the butyl pressure-sensitive adhesive is.
Table 2 shows the data of the pressure-sensitive adhesive performance test of each example
TABLE 3 comparison data of properties of butyl rubber pressure-sensitive adhesive of the present invention and conventional pressure-sensitive adhesive of the same type of comparative example
As shown in the table above, the butyl pressure-sensitive adhesive provided by the invention is prepared by selecting the butyl rubber, the SEBS and the MAH-g-EVA, and then matching with other auxiliary agents, so that the heat-resistant creep of the butyl rubber can be greatly improved under the condition that the bonding performance of the butyl pressure-sensitive adhesive is maintained, the sand surface of the waterproof coiled material is ensured not to overflow at high temperature, the coiled material is not adhered during long-term storage, feet are not adhered during high-temperature construction, the construction efficiency is improved, and the construction cost is saved. Among them, the butyl pressure sensitive adhesive of example 4 is the most excellent in adhesive property and thermal creep resistance.
From example 4 and comparative examples 1-3, it is known that butyl rubber, SEBS and MAH-g-EVA have one of the three systems, and one of the three systems is absent, so that the butyl rubber pressure sensitive adhesive cannot be modified, and the adhesive strength of the cement base material and the heat creep resistance of the butyl pressure sensitive adhesive are greatly influenced.
Compared with the comparative example 4, the addition of the coupling agent can improve the compatibility of the inorganic filler and the organic system, so that the filler is uniformly dispersed in the organic mixture, and the rigidity of the system is improved under the condition of ensuring the viscoelasticity, thereby improving the thermal creep resistance of the system.
As can be seen from example 4, comparative example 5 and comparative example 6, the MAH-g-EVA having a VA content of 28 is the best in overall performance. The melt grafting reaction belongs to heterogeneous reaction, the dispersion degree between phases is determined by the difference of viscosity and polarity of each component in a molten state in a reaction system, the polarity of MAH is strong, the molten MAH in the molten state is not uniformly dispersed in a polymer matrix but tends to form a separated phase in the melt grafting process, the grafting reaction occurs on a phase interface of the two phases, the polarity of EVA with 14% of VA content is lower than that of EVA with higher VA content, the compatibility with MAH is poorer, and thus the grafting rate is lower; in addition, the grafting reaction mainly occurs in the vinyl acetate chain segment part in the EVA main chain, and the reaction is not easy to occur even if the VA content is too low. EVA with 28% and 33% VA has higher polarity and better compatibility with MAH, so the grafting rate is higher than that of EVA with 14% VA. The EVA vinyl acetate chain segment with 33% of VA content has more content, and the macromolecular free radicals generated by the reaction in the same time are more, but because the strongly polar MAH monomer forms a separated phase in the melt grafting process and the reaction occurs at a two-phase interface, the macromolecular free radicals are easy to react with each other to be consumed in more cases, so that the grafting ratio of the EVA vinyl acetate chain segment with 33% of VA content is slightly lower than that of the EVA with 28% of VA content. Therefore, the EVA with 14% of VA cannot form a tight molecular network entanglement with the SEBS due to the excessively low grafting ratio, and further cannot improve the heat creep resistance and other bonding properties of the butyl pressure-sensitive adhesive. The EVA with the higher VA content of 33 percent is subjected to side reaction more easily, so that the EVA body is copolymerized, a macromolecular product which is difficult to be compatible with SEBS and butyl rubber is generated, the integral viscoelasticity of the butyl pressure-sensitive adhesive is reduced, and the bonding strength of the pressure-sensitive adhesive is reduced.
The above embodiments are only preferred embodiments of the present invention, and the protection scope of the present invention is not limited thereby, and any insubstantial changes and substitutions made by those skilled in the art based on the present invention are within the protection scope of the present invention.
Claims (9)
1. The high-heat-creep-resistance waterproof butyl pressure-sensitive adhesive is characterized by being prepared from the following components in parts by weight: 10-70 parts of butyl rubber, 20-40 parts of polyisobutylene, 1-5 parts of antioxidant, 20-50 parts of petroleum resin, 5-10 parts of SEBS, 5-10 parts of MAH-g-EVA, 10-40 parts of filler, 1-5 parts of anti-ultraviolet agent and 1-5 parts of coupling agent.
The mass ratio of the butyl rubber, the SEBS and the MAH-g-EVA is (2-6): 1:1; the VA content of the MAH-g-EVA is 28%.
2. The high thermal creep resistant waterproof butyl pressure sensitive adhesive as claimed in claim 1, which is prepared from the following components in parts by weight: 15-30 parts of butyl rubber, 22-30 parts of polyisobutylene, 1-3 parts of antioxidant, 20-30 parts of petroleum resin, 5-8 parts of SEBS, 5-8 parts of MAH-g-EVA, 15-30 parts of filler, 1-2 parts of anti-ultraviolet agent and 1-2 parts of coupling agent.
3. The high thermal creep resistant waterproof butyl pressure sensitive adhesive of claim 1, wherein the MAH-g-EVA is prepared by the following method:
adding a certain amount of MAH and initiator DCP into acetone as a solvent, uniformly stirring and dissolving, mixing and stirring with EVA in a high-speed stirrer for 5-10min, discharging, mixing, melting and grafting at 150-180 ℃ by a double-screw extruder, granulating, air drying, and packaging for later use;
the mass ratio of the MAH to the EVA is (1-3): 100, respectively; the mass ratio of the initiator DCP to the EVA is (0.2-2): 100, respectively; the mass ratio of the acetone to the MAH is (1-5): 1.
4. the high thermal creep resistant water-resistant butyl pressure sensitive adhesive of claim 1 wherein the antioxidant is a mixture of two selected from the group consisting of oxidizing agent 1010 and oxidizing agent 168.
5. The high thermal creep resistant water-proof butyl pressure sensitive adhesive according to claim 1, wherein the petroleum resin is selected from one or a mixture of two or more of C5 petroleum resin, C9 petroleum resin, C5/C9 copolymerized petroleum resin, hydrogenated DCPD petroleum resin, hydrogenated C5 petroleum resin or hydrogenated C9 petroleum resin.
6. The high thermal creep resistant waterproof butyl pressure sensitive adhesive according to claim 1, wherein the filler is selected from one or a mixture of more than two of calcium carbonate, kaolin, mica powder and transparent powder.
7. The high thermal creep resistant waterproof butyl pressure sensitive adhesive of claim 1, wherein the anti-uv agent is selected from one or more of 2- (2H-benzotriazol-2-yl) -4,6-bis (1-methyl-1-phenylethyl) phenol, 2- [4,6-bis (2,4-dimethylphenyl) -1,3,5-triazin-2-yl ] -5- (octyloxy) phenol, 2- (2, -hydroxy-5, -methyl) -benzotriazole, [1- (2, -hydroxy) -2,2,6,6-tetramethyl-4-hydroxypiperidine succinate ], bis 2,2,6,6, -tetramethylpiperidinol sebacate, poly- { [6- [ (1,1,3,3, -tetramethylbutyl) -amino ]1,3,5, -triazine-2,4-diyl ] [ (2,2,6,6-tetramethylpiperidinyl) -3282 zxft- [ (3434) -tetramethylpiperidinyl).
8. The high thermal creep resistant waterproof butyl pressure sensitive adhesive according to claim 1, wherein the coupling agent is selected from one or a mixture of two or more of methyltriethoxysilane, vinyltriethoxysilane, gamma-aminopropyltriethoxysilane, gamma- (2,3-glycidoxy) propyltrimethoxysilane, and gamma- (methacryloyloxy) propyltrimethoxysilane.
9. The preparation method of the high thermal creep resistant waterproof butyl pressure-sensitive adhesive according to any one of claims 1 to 8, which comprises the following steps:
(1) Adding polyisobutylene and an antioxidant in a formula ratio into a kneader, and heating to 160 +/-5 ℃;
(2) Then adding the butyl rubber, SEBS, MAH-g-EVA, the coupling agent and the filler according to the formula ratio, stirring for 50min in vacuum, and keeping the temperature at 160 +/-5 ℃;
(3) Finally, adding the petroleum resin and the anti-ultraviolet auxiliary agent in the formula amount, uniformly stirring in vacuum for 20min, keeping the temperature at 145 +/-5 ℃, discharging, and cooling to room temperature to obtain the high-heat-resistance creep waterproof butyl pressure-sensitive adhesive;
the high heat-resistant creep waterproof butyl pressure-sensitive adhesive comprises the following components in parts by weight: 10-70 parts of butyl rubber, 20-40 parts of polyisobutylene, 1-5 parts of antioxidant, 20-50 parts of petroleum resin, 5-10 parts of SEBS, 5-10 parts of MAH-g-EVA, 10-40 parts of filler, 1-5 parts of anti-ultraviolet agent and 1-5 parts of coupling agent.
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| JP2011195797A (en) * | 2010-03-17 | 2011-10-06 | Okong Co Ltd | Hot melt adhesive composition |
| CN110028915A (en) * | 2019-04-26 | 2019-07-19 | 江苏达胜热缩防护用品有限公司 | A kind of Pipeline joint anticorrosion low form 3PE dry film hot melt adhesive and preparation method thereof |
| CN110229633A (en) * | 2019-06-28 | 2019-09-13 | 广东能辉新材料科技有限公司 | High temperature resistant type waterproof roll |
| CN110358476A (en) * | 2019-05-30 | 2019-10-22 | 廊坊市中油嘉昱防腐技术有限公司 | A kind of high temperature resistant butyl pressure sensitive adhesive and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2011195797A (en) * | 2010-03-17 | 2011-10-06 | Okong Co Ltd | Hot melt adhesive composition |
| CN110028915A (en) * | 2019-04-26 | 2019-07-19 | 江苏达胜热缩防护用品有限公司 | A kind of Pipeline joint anticorrosion low form 3PE dry film hot melt adhesive and preparation method thereof |
| CN110358476A (en) * | 2019-05-30 | 2019-10-22 | 廊坊市中油嘉昱防腐技术有限公司 | A kind of high temperature resistant butyl pressure sensitive adhesive and preparation method thereof |
| CN110229633A (en) * | 2019-06-28 | 2019-09-13 | 广东能辉新材料科技有限公司 | High temperature resistant type waterproof roll |
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