CN117264583A - Preparation method of high-viscosity hot-melt pressure-sensitive adhesive - Google Patents
Preparation method of high-viscosity hot-melt pressure-sensitive adhesive Download PDFInfo
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- CN117264583A CN117264583A CN202311199013.1A CN202311199013A CN117264583A CN 117264583 A CN117264583 A CN 117264583A CN 202311199013 A CN202311199013 A CN 202311199013A CN 117264583 A CN117264583 A CN 117264583A
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- China
- Prior art keywords
- resin
- agent
- sensitive adhesive
- melt pressure
- hot
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 239000004820 Pressure-sensitive adhesive Substances 0.000 title claims abstract description 85
- 239000012943 hotmelt Substances 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 229920005989 resin Polymers 0.000 claims abstract description 105
- 239000011347 resin Substances 0.000 claims abstract description 105
- 239000007788 liquid Substances 0.000 claims abstract description 84
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 76
- 239000003921 oil Substances 0.000 claims abstract description 64
- 239000000203 mixture Substances 0.000 claims abstract description 37
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 35
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 32
- 239000002562 thickening agent Substances 0.000 claims abstract description 31
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 29
- 238000002156 mixing Methods 0.000 claims abstract description 26
- 239000004636 vulcanized rubber Substances 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000011049 filling Methods 0.000 claims abstract description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000007822 coupling agent Substances 0.000 claims abstract description 20
- 239000004014 plasticizer Substances 0.000 claims abstract description 20
- 229940124543 ultraviolet light absorber Drugs 0.000 claims abstract description 17
- 239000006097 ultraviolet radiation absorber Substances 0.000 claims abstract description 17
- 239000000945 filler Substances 0.000 claims abstract description 14
- 238000004062 sedimentation Methods 0.000 claims abstract description 7
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 51
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims description 51
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 51
- -1 acrylic ester Chemical class 0.000 claims description 38
- 239000003208 petroleum Substances 0.000 claims description 24
- 230000003712 anti-aging effect Effects 0.000 claims description 22
- 239000002798 polar solvent Substances 0.000 claims description 21
- 150000003505 terpenes Chemical class 0.000 claims description 18
- 235000007586 terpenes Nutrition 0.000 claims description 18
- JHPBZFOKBAGZBL-UHFFFAOYSA-N (3-hydroxy-2,2,4-trimethylpentyl) 2-methylprop-2-enoate Chemical compound CC(C)C(O)C(C)(C)COC(=O)C(C)=C JHPBZFOKBAGZBL-UHFFFAOYSA-N 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- 150000001412 amines Chemical class 0.000 claims description 14
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 12
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims description 12
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical compound FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 claims description 12
- 239000003822 epoxy resin Substances 0.000 claims description 12
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims description 12
- 229920001083 polybutene Polymers 0.000 claims description 12
- 229920000647 polyepoxide Polymers 0.000 claims description 12
- 150000002148 esters Chemical class 0.000 claims description 11
- 229920001971 elastomer Polymers 0.000 claims description 10
- 239000005060 rubber Substances 0.000 claims description 10
- BTJPUDCSZVCXFQ-UHFFFAOYSA-N 2,4-diethylthioxanthen-9-one Chemical compound C1=CC=C2C(=O)C3=CC(CC)=CC(CC)=C3SC2=C1 BTJPUDCSZVCXFQ-UHFFFAOYSA-N 0.000 claims description 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 9
- 229920002367 Polyisobutene Polymers 0.000 claims description 9
- 229920006026 co-polymeric resin Polymers 0.000 claims description 9
- 238000007334 copolymerization reaction Methods 0.000 claims description 9
- 239000000839 emulsion Substances 0.000 claims description 9
- 125000005456 glyceride group Chemical group 0.000 claims description 9
- 229940057995 liquid paraffin Drugs 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 229920006122 polyamide resin Polymers 0.000 claims description 9
- 150000003254 radicals Chemical class 0.000 claims description 9
- 229920006337 unsaturated polyester resin Polymers 0.000 claims description 9
- IOJUPLGTWVMSFF-UHFFFAOYSA-N benzothiazole Chemical compound C1=CC=C2SC=NC2=C1 IOJUPLGTWVMSFF-UHFFFAOYSA-N 0.000 claims description 8
- MZRQZJOUYWKDNH-UHFFFAOYSA-N diphenylphosphoryl-(2,3,4-trimethylphenyl)methanone Chemical compound CC1=C(C)C(C)=CC=C1C(=O)P(=O)(C=1C=CC=CC=1)C1=CC=CC=C1 MZRQZJOUYWKDNH-UHFFFAOYSA-N 0.000 claims description 8
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 8
- DPZSNGJNFHWQDC-ARJAWSKDSA-N (z)-2,3-diaminobut-2-enedinitrile Chemical compound N#CC(/N)=C(/N)C#N DPZSNGJNFHWQDC-ARJAWSKDSA-N 0.000 claims description 6
- 229910015900 BF3 Inorganic materials 0.000 claims description 6
- 239000004593 Epoxy Substances 0.000 claims description 6
- 235000021355 Stearic acid Nutrition 0.000 claims description 6
- MBHRHUJRKGNOKX-UHFFFAOYSA-N [(4,6-diamino-1,3,5-triazin-2-yl)amino]methanol Chemical compound NC1=NC(N)=NC(NCO)=N1 MBHRHUJRKGNOKX-UHFFFAOYSA-N 0.000 claims description 6
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 6
- 150000001721 carbon Chemical class 0.000 claims description 6
- 229920006037 cross link polymer Polymers 0.000 claims description 6
- MCPKSFINULVDNX-UHFFFAOYSA-N drometrizole Chemical compound CC1=CC=C(O)C(N2N=C3C=CC=CC3=N2)=C1 MCPKSFINULVDNX-UHFFFAOYSA-N 0.000 claims description 6
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims description 6
- 239000004312 hexamethylene tetramine Substances 0.000 claims description 6
- 150000002460 imidazoles Chemical class 0.000 claims description 6
- 239000000395 magnesium oxide Substances 0.000 claims description 6
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 6
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 6
- DEQZTKGFXNUBJL-UHFFFAOYSA-N n-(1,3-benzothiazol-2-ylsulfanyl)cyclohexanamine Chemical compound C1CCCCC1NSC1=NC2=CC=CC=C2S1 DEQZTKGFXNUBJL-UHFFFAOYSA-N 0.000 claims description 6
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 6
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 6
- 150000007524 organic acids Chemical class 0.000 claims description 6
- 229920001568 phenolic resin Polymers 0.000 claims description 6
- 239000005011 phenolic resin Substances 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 6
- 229940116351 sebacate Drugs 0.000 claims description 6
- CXMXRPHRNRROMY-UHFFFAOYSA-L sebacate(2-) Chemical compound [O-]C(=O)CCCCCCCCC([O-])=O CXMXRPHRNRROMY-UHFFFAOYSA-L 0.000 claims description 6
- 239000008117 stearic acid Substances 0.000 claims description 6
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 6
- 229920002554 vinyl polymer Polymers 0.000 claims description 6
- 239000011787 zinc oxide Substances 0.000 claims description 6
- 239000012467 final product Substances 0.000 claims description 5
- GLDOVTGHNKAZLK-UHFFFAOYSA-N octadecan-1-ol Chemical compound CCCCCCCCCCCCCCCCCCO GLDOVTGHNKAZLK-UHFFFAOYSA-N 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 3
- CMLFRMDBDNHMRA-UHFFFAOYSA-N 2h-1,2-benzoxazine Chemical compound C1=CC=C2C=CNOC2=C1 CMLFRMDBDNHMRA-UHFFFAOYSA-N 0.000 claims description 3
- JKIJEFPNVSHHEI-UHFFFAOYSA-N Phenol, 2,4-bis(1,1-dimethylethyl)-, phosphite (3:1) Chemical compound CC(C)(C)C1=CC(C(C)(C)C)=CC=C1OP(OC=1C(=CC(=CC=1)C(C)(C)C)C(C)(C)C)OC1=CC=C(C(C)(C)C)C=C1C(C)(C)C JKIJEFPNVSHHEI-UHFFFAOYSA-N 0.000 claims description 3
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 claims description 3
- 238000005266 casting Methods 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 2
- 229940079865 intestinal antiinfectives imidazole derivative Drugs 0.000 claims description 2
- 239000011259 mixed solution Substances 0.000 claims description 2
- 238000003860 storage Methods 0.000 abstract description 8
- 230000003647 oxidation Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 238000005303 weighing Methods 0.000 abstract description 5
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000005336 cracking Methods 0.000 abstract description 4
- 230000002265 prevention Effects 0.000 abstract 1
- 230000032683 aging Effects 0.000 description 15
- 238000010438 heat treatment Methods 0.000 description 4
- 229920000459 Nitrile rubber Polymers 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 231100000053 low toxicity Toxicity 0.000 description 3
- 239000002480 mineral oil Substances 0.000 description 3
- 235000010446 mineral oil Nutrition 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 150000002978 peroxides Chemical class 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 239000002861 polymer material Substances 0.000 description 3
- 230000002035 prolonged effect Effects 0.000 description 3
- 230000001681 protective effect Effects 0.000 description 3
- 230000009467 reduction Effects 0.000 description 3
- 230000002195 synergetic effect Effects 0.000 description 3
- 238000003809 water extraction Methods 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 1
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000123 paper Substances 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- 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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- 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
- 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
- C09J161/00—Adhesives based on condensation polymers of aldehydes or ketones; Adhesives based on derivatives of such polymers
- C09J161/04—Condensation polymers of aldehydes or ketones with phenols only
- C09J161/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
-
- 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
- C09J161/00—Adhesives based on condensation polymers of aldehydes or ketones; Adhesives based on derivatives of such polymers
- C09J161/04—Condensation polymers of aldehydes or ketones with phenols only
- C09J161/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
- C09J161/12—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols with polyhydric phenols
-
- 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
- C09J161/00—Adhesives based on condensation polymers of aldehydes or ketones; Adhesives based on derivatives of such polymers
- C09J161/34—Condensation polymers of aldehydes or ketones with monomers covered by at least two of the groups C09J161/04, C09J161/18 and C09J161/20
-
- 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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
- C09J163/04—Epoxynovolacs
-
- 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
- C09J171/00—Adhesives based on polyethers obtained by reactions forming an ether link in the main chain; Adhesives based on derivatives of such polymers
- C09J171/08—Polyethers derived from hydroxy compounds or from their metallic derivatives
- C09J171/10—Polyethers derived from hydroxy compounds or from their metallic derivatives from phenols
-
- 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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/222—Magnesia, i.e. magnesium oxide
-
- 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
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a preparation method of a high-viscosity hot-melt pressure-sensitive adhesive, which relates to the technical field of hot-melt pressure-sensitive adhesive preparation and comprises the steps of preparing a base material, mixing, preparing a modified liquid, adding a filler, curing and forming, and weighing the base material in the following proportion: 2.5% of plasticizer, 2.5% of thickener, 2.5% of tackifier, 2.5% of resin, 2% of photoinitiator, 2% of ultraviolet light absorber, 1.5% of antioxidant, 2.5% of curing agent, 0.5% of coupling agent, 1% of cross-linking agent, 1.5% of filling oil, 1.5% of vulcanized rubber composition, 1.5% of vulcanizing agent and 1.5% of accelerator, and adding water 2% and 1.5% of alcohol. The preparation method of the high-viscosity hot-melt pressure-sensitive adhesive has the advantages of strong pillbox increasing capability, good sedimentation resistance and mildew resistance, high practicality of the hot-melt pressure-sensitive adhesive, high oxidation resistance strength of the hot-melt pressure-sensitive adhesive, cracking prevention of the cured hot-melt pressure-sensitive adhesive, and long storage time.
Description
Technical Field
The invention relates to the technical field of hot-melt pressure-sensitive adhesive preparation, in particular to a preparation method of a high-viscosity hot-melt pressure-sensitive adhesive.
Background
The hot melt pressure-sensitive adhesive is a novel adhesive tape which is mainly prepared by mixing synthetic rubber, resin, rubber oil and the like, heating the mixture into a molten state, and then coating the molten state on base materials such as cotton paper, cloth or plastic film, and the like, and is a third-generation pressure-sensitive adhesive product after solvent-type pressure-sensitive adhesive and emulsion-type pressure-sensitive adhesive.
The low cost of the hot-melt pressure-sensitive adhesive is the greatest advantage, but the defect is that the viscosity is easily affected by temperature, so that the viscosity of the formed hot-melt pressure-sensitive adhesive is weaker, the density of the hot-melt pressure-sensitive adhesive is smaller, and the high viscosity of the hot-melt pressure-sensitive adhesive can be affected; the hot-melt pressure-sensitive adhesive is easy to age after heat aging and ultraviolet light irradiation, so that the oxidation resistance of the hot-melt pressure-sensitive adhesive is weaker; the hot-melt pressure-sensitive adhesive needs to be cured when being molded, but the existing hot-melt pressure-sensitive adhesive has low curing speed, the surface of the cured hot-melt pressure-sensitive adhesive is easy to crack, and the storage stability is weak.
Disclosure of Invention
The invention mainly aims to provide a preparation method of a high-viscosity hot-melt pressure-sensitive adhesive, so as to solve the problems in the background.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: the preparation method of the high-viscosity hot-melt pressure-sensitive adhesive comprises the steps of preparing a base material, mixing and stirring, preparing a modified liquid, adding a filler, curing and forming, and weighing the base material according to the following proportion: 2.5% of plasticizer, 2.5% of thickener, 2.5% of tackifier, 2.5% of resin, 2% of photoinitiator, 2% of ultraviolet light absorber, 1.5% of antioxidant, 2.5% of curing agent, 0.5% of coupling agent, 1% of cross-linking agent, 1.5% of filling oil, 1.5% of vulcanized rubber composition, 1.5% of vulcanizing agent and 1.5% of accelerator, and adding water 2% and 1.5% of alcohol and other polar solvents;
the base material is prepared by weighting 2.5% of plasticizer, 2.5% of thickening agent, 2.5% of tackifier, 2.5% of resin, 2% of photoinitiator, 2% of ultraviolet light absorber, 1.5% of antioxidant, 2.5% of curing agent, 0.5% of coupling agent, 1% of cross-linking agent, 1.5% of filling oil, 1.5% of vulcanized rubber composition, 1.5% of vulcanizing agent and 1.5% of accelerator, 2% of water, 1.5% of alcohol and other polar solvents according to weight proportion;
the mixing treatment is to mix the prepared base materials through a stirrer, a temperature controller, a pulverizer and other equipment to obtain a mixed solution;
the prepared modified liquid is used for adding a tackifier and a thickener into the mixed liquid, and adding filling oil to prepare the modified liquid;
the filler is used for adding an antioxidant into the modified liquid, dissolving the antioxidant and polar solvents such as water, alcohol and the like in esters, and then stirring the mixture to obtain hot-melt pressure-sensitive adhesive mixed liquid;
the solidifying and forming process is to add cross-linking agent and promoter into the mixed liquid to disperse uniformly, then add vulcanized rubber composition and vulcanizing agent, solidify and cool the mixed liquid to obtain the final product.
The plasticizer is at least one of unsaturated polyester resin, polyamide resin, naphthenic base rubber softening oil, liquid polyisobutene, naphthenic oil, liquid paraffin and white oil;
the weight proportion of the unsaturated polyester resin, the polyamide resin, the naphthenic rubber softening oil, the liquid polyisobutene, the naphthenic oil, the liquid paraffin and the white oil is 0.3% -0.5% of the unsaturated polyester resin, 0.3% -0.5% of the polyamide resin, 0.3% -0.5% of the naphthenic rubber softening oil, 0.3% -0.5% of the liquid polyisobutene, 0.3% -0.5% of the naphthenic oil, 0.3% -0.5% of the liquid paraffin and 0.3% -0.5% of the white oil;
the thickener is a cross-linked polymer emulsion thickener formed by copolymerization of acrylic ester and methacrylic ester;
the weight proportion of the cross-linked polymer emulsion thickener formed by copolymerization of acrylic ester and methacrylic ester is 0.2-0.4% of acrylic ester and 0.2-0.4% of methacrylic ester.
The tackifier is at least one of terpene tackifying resin, petroleum resin, copolymer resin, rosin modified tackifying resin, hydrogenated rosin, polymerized rosin, rosin glyceride, resin, ancient road resin and modified rosin;
the weight proportion of the terpene tackifying resin, the petroleum resin, the copolymer resin, the rosin modified tackifying resin, the hydrogenated rosin, the polymerized rosin, the rosin glyceride, the resin, the ancient road resin and the modified rosin is 0.3-0.6% of the terpene tackifying resin, 0.3-0.6% of the petroleum resin, 0.3-0.6% of the copolymer resin, 0.3-0.6% of the rosin modified tackifying resin, 0.3-0.6% of the hydrogenated rosin, 0.3-0.6% of the polymerized rosin, 0.3-0.6% of the rosin glyceride, 0.3-0.6% of the resin, 0.3-0.6% of the ancient road resin and 0.3-0.6% of the modified rosin;
the resin is at least one of E-44 bisphenol A epoxy resin, E-51 bisphenol A epoxy resin, E-20 bisphenol A epoxy resin, E-12 bisphenol A epoxy resin, F-51 linear phenolic epoxy resin, F-44 linear phenolic epoxy resin, PYSM resin, FB resin, bisphenol A linear phenolic resin, active alkyl phenolic resin, benzoxazine resin, hydrogenated carbon five petroleum resin and fully hydrogenated carbon nine petroleum resin;
the weight proportion of the resin is 0.5% -1%;
the photoinitiator is at least one of 2,4,6 (trimethyl benzoyl) diphenyl phosphine oxide, 4-dimethyl amino benzoic acid isooctyl ester and 2, 4-diethyl thioxanthone;
the weight proportion of the 2,4,6 (trimethyl benzoyl) diphenyl phosphine oxide, the 4-dimethyl amino benzoic acid isooctyl ester and the 2, 4-diethyl thioxanthone is 0.2% -1% of 2,4,6 (trimethyl benzoyl) diphenyl phosphine oxide, 0.2% -1% of 4-dimethyl amino benzoic acid isooctyl ester and 0.2% -1% of 2, 4-diethyl thioxanthone;
the ultraviolet light absorber is at least one of 2- (2 '-hydroxy-5' -methylphenyl) benzotriazole and bis (2, 6-tetramethyl-4-piperidinyl) sebacate;
the weight proportion of the 2- (2 '-hydroxy-5' -methylphenyl) benzotriazole and bis (2, 6-tetramethyl-4-piperidinyl) sebacate is 0.5% -2%.
The antioxidant is at least one of pentaerythritol tetra- [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], tris [2, 4-di-tert-butylphenyl ] phosphite, a free radical terminator, a hydroperoxide decomposer and n-octadecanol beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate;
the weight proportion of the antioxidant is 0.5% -1%;
the curing agent is an epoxy resin curing agent;
the weight proportion of the epoxy resin curing agent is 2%.
At least one of coupling agent amine, epoxy, vinyl and acrylic ester;
the weight proportion of the coupling agent amine, epoxy, vinyl and acrylic ester is 0.3-1%;
the cross-linking agent is at least one single substance or mixture of dinitrile amine and derivatives thereof, hexamethylenetetramine, methylolmelamine, hexamethylenemelamine, diaminomaleonitrile and derivatives thereof, boron trifluoride gum complex, imidazole derivatives and organic acid hydrazide;
the weight proportion of the dinitrile amine and the derivative thereof, the hexamethylenetetramine, the methylolmelamine, the hexamethylenemelamine, the diaminomaleonitrile and the derivative thereof, the boron trifluoride glue complex, the imidazole derivative and the organic acid hydrazide is 0.4-1 percent.
The filling oil is polybutene oil; the weight proportion of the polybutene oil is 2%;
the vulcanized rubber composition is a mixture of a vulcanizing agent, an accelerator and an anti-aging agent, and the anti-aging agent is an anti-aging agent D or an anti-aging agent MBZ;
the mixture of the vulcanizing agent, the accelerator and the anti-aging agent is that the anti-aging agent D or the anti-aging agent MBZ has the weight proportion of 0.5 to 1.2 percent.
The vulcanizing agent is any one of zinc oxide, magnesium oxide and stearic acid;
the weight proportion of the zinc oxide, the magnesium oxide and the stearic acid is 0.3% -1%;
the accelerator is one of N-cyclohexyl-2-benzothiazole sulfenamide or N, N-diethyl dithioamino benzothiazole;
the weight proportion of the N-cyclohexyl-2-benzothiazole sulfenamide or the N, N-diethyl dithioamino benzothiazole is 0.2% -0.8%.
A preparation method of a high-viscosity hot-melt pressure-sensitive adhesive comprises the following steps:
step one: preparing base materials, namely preparing raw materials such as a plasticizer, a thickener, a tackifier, resin, a photoinitiator, an ultraviolet light absorber, an antioxidant, a curing agent, a coupling agent, an accelerator, a crosslinking agent and filling oil after weight balancing according to weight balancing proportion;
step two: mixing, namely crushing and stirring the prepared base materials through equipment such as a stirrer, a temperature controller, a crusher and the like to realize the mixing of the base materials to obtain mixed liquid;
step three: preparing a modified liquid, adding rosin modified tackifying resin, terpene tackifying resin, petroleum resin, acrylic ester and methacrylic ester into the mixed liquid, and adding polybutene oil to prepare the modified liquid;
step four: adding filler, adding one of a free radical terminator and a hydroperoxide decomposer into the modified liquid, dissolving the modified liquid and polar solvents such as water, alcohol and the like in esters, and stirring to obtain hot-melt pressure-sensitive adhesive mixed liquid;
step five: and (3) curing and forming to obtain a finished product, adding a cross-linking agent and an accelerator for uniform dispersion, casting to form a film, adding a vulcanized rubber composition and a vulcanizing agent, and curing and cooling the mixed liquid after mixing to obtain the high-viscosity anti-sedimentation hot-melt pressure-sensitive adhesive.
The invention has the following beneficial effects:
1. according to the invention, the rosin modified tackifying resin, the terpene tackifying resin and the petroleum resin are added, and the crosslinking type high polymer emulsion thickener formed by copolymerization of acrylic ester and methacrylic ester is mixed to obtain the high-viscosity modified liquid, so that the prepared hot-melt pressure-sensitive adhesive has good leveling property and fluidity, strong pilling resistance and good sedimentation and mildew resistance, and molecules such as the petroleum resin and the terpene tackifying resin have good ageing resistance, so that the formed hot-melt pressure-sensitive adhesive has high viscosity, the density of the hot-melt pressure-sensitive adhesive is increased, the ageing resistance is stronger, the mineral oil is replaced by the polybutene oil by the added filling oil, the cohesive force and the heat resistance of the hot-melt pressure-sensitive adhesive are greatly improved, the formula cost of the adhesive is reduced, and the practicability of the hot-melt pressure-sensitive adhesive is improved.
2. According to the invention, one of the free radical terminator and the hydroperoxide decomposer is added and is slightly dissolved in the ester with polar solvents such as water, alcohol and the like, so that the prepared hot-melt pressure-sensitive adhesive has protective effect on aging caused by oxygen, heat and moon light, thereby realizing environmental protection and pollution reduction, and the peroxide which is generated by heating the decomposable polymer material with low toxicity and good thermal stability has strong water extraction resistance and can be recycled after being soaked in hot water, the quality is not influenced, and the hot-melt pressure-sensitive adhesive has excellent synergistic effect after being subjected to heat aging and ultraviolet light irradiation, and the oxidation resistance strength of the hot-melt pressure-sensitive adhesive is improved.
3. According to the invention, the crosslinking agent and the accelerator are combined, the accelerator is in an amount larger than that of the crosslinking agent, and the vulcanized rubber composition and the vulcanizing agent are added for reaction and fusion during mixing, so that the curing speed of the prepared hot-melt pressure-sensitive adhesive is obviously improved, the hot-melt pressure-sensitive adhesive is easy to be pasted and convenient to operate, the antioxidant is added into ingredients, the adding amount is 0.3-1% of the total amount, the cured hot-melt pressure-sensitive adhesive is prevented from cracking, the storage time is prolonged, and the added liquid nitrile rubber and polyester plasticizer can increase the storage stability of the cured hot-melt pressure-sensitive adhesive.
Drawings
FIG. 1 is a system overall architecture diagram of a method for preparing a high-viscosity hot-melt pressure-sensitive adhesive of the present invention;
FIG. 2 is a schematic diagram of a blending process for preparing a high viscosity hot melt pressure sensitive adhesive according to the present invention;
FIG. 3 is a schematic diagram of the structure of a modified liquid obtained by the method for preparing a high-viscosity hot-melt pressure-sensitive adhesive according to the present invention;
FIG. 4 is a schematic illustration of a preparation process of a method for preparing a high-viscosity hot-melt pressure-sensitive adhesive according to the present invention.
Detailed Description
The invention is further described in connection with the following detailed description, in order to make the technical means, the creation characteristics, the achievement of the purpose and the effect of the invention easy to understand.
Example 1
Please refer to fig. 1-2: the preparation method of the high-viscosity hot-melt pressure-sensitive adhesive comprises the steps of preparing a base material, mixing and stirring, preparing a modified liquid, adding a filler, curing and forming, and weighing the base material according to the following proportion: 2.5% of plasticizer, 2.5% of thickener, 2.5% of tackifier, 2.5% of resin, 2% of photoinitiator, 2% of ultraviolet light absorber, 1.5% of antioxidant, 2.5% of curing agent, 0.5% of coupling agent, 1% of cross-linking agent, 1.5% of filling oil, 1.5% of vulcanized rubber composition, 1.5% of vulcanizing agent and 1.5% of accelerator, and adding water 2% and 1.5% of alcohol and other polar solvents;
the base material is prepared by weighting 2.5 percent of plasticizer, 2.5 percent of thickening agent, 2.5 percent of tackifier, 2.5 percent of resin, 2 percent of photoinitiator, 2 percent of ultraviolet light absorber, 1.5 percent of antioxidant, 2.5 percent of curing agent, 0.5 percent of coupling agent, 1 percent of cross-linking agent, 1.5 percent of filling oil, 1.5 percent of vulcanized rubber composition, 1.5 percent of vulcanizing agent and 1.5 percent of accelerator, and the like with 2 percent of water, 1.5 percent of alcohol and other polar solvents according to weight proportion;
mixing the prepared base materials by using equipment such as a stirrer, a temperature controller, a pulverizer and the like to obtain mixed liquid;
the obtained modified liquid is used for adding a tackifier and a thickener into the mixed liquid, and adding filling oil to obtain the modified liquid;
adding filler for adding antioxidant into the modified liquid, dissolving the antioxidant and polar solvents such as water, alcohol and the like in esters, and stirring to obtain hot-melt pressure-sensitive adhesive mixed liquid;
the solidifying and forming process is to add cross-linking agent and promoter into the mixed liquid to disperse uniformly, then add vulcanized rubber composition and vulcanizing agent, solidify and cool the mixed liquid to obtain the final product.
The plasticizer is at least one of unsaturated polyester resin, polyamide resin, naphthenic rubber softening oil, liquid polyisobutylene, naphthenic oil, liquid paraffin and white oil;
the weight proportion of the unsaturated polyester resin, the polyamide resin, the naphthenic rubber softening oil, the liquid polyisobutene, the naphthenic oil, the liquid paraffin and the white oil is 0.3% -0.5% of the unsaturated polyester resin, 0.3% -0.5% of the polyamide resin, 0.3% -0.5% of the naphthenic rubber softening oil, 0.3% -0.5% of the liquid polyisobutene, 0.3% -0.5% of the naphthenic oil, 0.3% -0.5% of the liquid paraffin and 0.3% -0.5% of the white oil;
the thickener is a cross-linking type high polymer emulsion thickener formed by copolymerization of acrylic ester and methacrylic ester;
the weight proportion of the cross-linked polymer emulsion thickener formed by copolymerization of acrylic ester and methacrylic ester is 0.2-0.4% of acrylic ester and 0.2-0.4% of methacrylic ester.
The tackifier is at least one of terpene tackifying resin, petroleum resin, copolymer resin, rosin modified tackifying resin, hydrogenated rosin, polymerized rosin, rosin glyceride, resin, ancient road resin and modified rosin;
the weight proportion of terpene tackifying resin, petroleum resin, copolymer resin, rosin modified tackifying resin, hydrogenated rosin, polymerized rosin, rosin glyceride, resin, ancient road resin and modified rosin is that the terpene tackifying resin is 0.3-0.6%, the petroleum resin is 0.3-0.6%, the copolymer resin is 0.3-0.6%, the rosin modified tackifying resin is 0.3-0.6%, the hydrogenated rosin is 0.3-0.6%, the polymerized rosin is 0.3-0.6%, the rosin glyceride is 0.3-0.6%, the resin is 0.3-0.6%, the ancient road resin is 0.3-0.6% and the modified rosin is 0.3-0.6%;
the resin is at least one of E-44 bisphenol A epoxy resin, E-51 bisphenol A epoxy resin, E-20 bisphenol A epoxy resin, E-12 bisphenol A epoxy resin, F-51 linear phenolic epoxy resin, F-44 linear phenolic epoxy resin, PYSM resin, FB resin, bisphenol A linear phenolic resin, active alkyl phenolic resin, benzoxazine resin, hydrogenated carbon penta petroleum resin and fully hydrogenated carbon nine petroleum resin;
the weight proportion of the resin is 0.5% -1%.
The high-viscosity modified liquid is prepared by adding rosin modified tackifying resin, terpene tackifying resin and petroleum resin and mixing a cross-linked polymer emulsion thickener formed by copolymerization of acrylic ester and methacrylic ester, so that the prepared hot-melt pressure-sensitive adhesive has good leveling property and fluidity, strong pilling resistance and good sedimentation resistance, and molecules such as petroleum resin and terpene tackifying resin have good ageing resistance, so that the formed hot-melt pressure-sensitive adhesive has high viscosity, the density of the hot-melt pressure-sensitive adhesive is increased, the ageing resistance is stronger, the mineral oil is replaced by polybutene oil by the added filling oil, the cohesion and the heat resistance of the hot-melt pressure-sensitive adhesive are greatly improved, the formula cost of the adhesive is reduced, and the practicability of hot melting is improved.
Example two
Please refer to fig. 3: the preparation method of the high-viscosity hot-melt pressure-sensitive adhesive comprises the steps of preparing a base material, mixing and stirring, preparing a modified liquid, adding a filler, curing and forming, and weighing the base material according to the following proportion: 2.5% of plasticizer, 2.5% of thickener, 2.5% of tackifier, 2.5% of resin, 2% of photoinitiator, 2% of ultraviolet light absorber, 1.5% of antioxidant, 2.5% of curing agent, 0.5% of coupling agent, 1% of cross-linking agent, 1.5% of filling oil, 1.5% of vulcanized rubber composition, 1.5% of vulcanizing agent and 1.5% of accelerator, and adding water 2% and 1.5% of alcohol and other polar solvents;
the base material is prepared by weighting 2.5 percent of plasticizer, 2.5 percent of thickening agent, 2.5 percent of tackifier, 2.5 percent of resin, 2 percent of photoinitiator, 2 percent of ultraviolet light absorber, 1.5 percent of antioxidant, 2.5 percent of curing agent, 0.5 percent of coupling agent, 1 percent of cross-linking agent, 1.5 percent of filling oil, 1.5 percent of vulcanized rubber composition, 1.5 percent of vulcanizing agent and 1.5 percent of accelerator, and the like with 2 percent of water, 1.5 percent of alcohol and other polar solvents according to weight proportion;
mixing the prepared base materials by using equipment such as a stirrer, a temperature controller, a pulverizer and the like to obtain mixed liquid;
the obtained modified liquid is used for adding a tackifier and a thickener into the mixed liquid, and adding filling oil to obtain the modified liquid;
adding filler for adding antioxidant into the modified liquid, dissolving the antioxidant and polar solvents such as water, alcohol and the like in esters, and stirring to obtain hot-melt pressure-sensitive adhesive mixed liquid;
the solidifying and forming process is to add cross-linking agent and promoter into the mixed liquid to disperse uniformly, then add vulcanized rubber composition and vulcanizing agent, solidify and cool the mixed liquid to obtain the final product.
The photoinitiator is at least one of 2,4,6 (trimethyl benzoyl) diphenyl phosphine oxide, 4-dimethyl amino benzoic acid isooctyl ester and 2, 4-diethyl thioxanthone;
the weight proportion of 2,4,6 (trimethyl benzoyl) diphenyl phosphine oxide, 4-dimethyl amino benzoic acid isooctyl ester and 2, 4-diethyl thioxanthone is 0.2% -1%, 4-dimethyl amino benzoic acid isooctyl ester 0.2% -1% and 2, 4-diethyl thioxanthone 0.2% -1%;
the ultraviolet light absorber is at least one of 2- (2 '-hydroxy-5' -methylphenyl) benzotriazole and bis (2, 6-tetramethyl-4-piperidinyl) sebacate;
the weight proportion of 2- (2 '-hydroxy-5' -methylphenyl) benzotriazole and bis (2, 6-tetramethyl-4-piperidinyl) sebacate is 0.5% -2%.
The antioxidant is at least one of pentaerythritol tetra- [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], tris- [2, 4-di-tert-butylphenyl ] phosphite, a free radical terminator, a hydroperoxide decomposer and n-stearyl beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate;
the weight proportion of the antioxidant is 0.5% -1%;
the curing agent is an epoxy resin curing agent;
the weight proportion of the epoxy resin curing agent is 2%.
By adding one of the free radical terminator and the hydroperoxide decomposer, the hot-melt pressure-sensitive adhesive is slightly dissolved in esters with polar solvents such as water, alcohol and the like, so that the prepared hot-melt pressure-sensitive adhesive has protective effect on aging caused by oxygen, heat and moonlight, thereby realizing environmental protection and pollution reduction, and the peroxide which is generated by heating a decomposable polymer material with low toxicity and good thermal stability has strong water extraction resistance, can be recycled after being soaked in hot water, has no influence on quality, has excellent synergistic effect when being compounded with phenolic or amine antioxidants, ensures that the hot-melt pressure-sensitive adhesive is prevented from aging after heat aging and ultraviolet light irradiation, and improves the oxidation resistance strength of the hot-melt pressure-sensitive adhesive.
Example III
Please refer to fig. 4: the preparation method of the high-viscosity hot-melt pressure-sensitive adhesive comprises the steps of preparing a base material, mixing and stirring, preparing a modified liquid, adding a filler, curing and forming, and weighing the base material according to the following proportion: 2.5% of plasticizer, 2.5% of thickener, 2.5% of tackifier, 2.5% of resin, 2% of photoinitiator, 2% of ultraviolet light absorber, 1.5% of antioxidant, 2.5% of curing agent, 0.5% of coupling agent, 1% of cross-linking agent, 1.5% of filling oil, 1.5% of vulcanized rubber composition, 1.5% of vulcanizing agent and 1.5% of accelerator, and adding water 2% and 1.5% of alcohol and other polar solvents;
the base material is prepared by weighting 2.5 percent of plasticizer, 2.5 percent of thickening agent, 2.5 percent of tackifier, 2.5 percent of resin, 2 percent of photoinitiator, 2 percent of ultraviolet light absorber, 1.5 percent of antioxidant, 2.5 percent of curing agent, 0.5 percent of coupling agent, 1 percent of cross-linking agent, 1.5 percent of filling oil, 1.5 percent of vulcanized rubber composition, 1.5 percent of vulcanizing agent and 1.5 percent of accelerator, and the like with 2 percent of water, 1.5 percent of alcohol and other polar solvents according to weight proportion;
mixing the prepared base materials by using equipment such as a stirrer, a temperature controller, a pulverizer and the like to obtain mixed liquid;
the obtained modified liquid is used for adding a tackifier and a thickener into the mixed liquid, and adding filling oil to obtain the modified liquid;
adding filler for adding antioxidant into the modified liquid, dissolving the antioxidant and polar solvents such as water, alcohol and the like in esters, and stirring to obtain hot-melt pressure-sensitive adhesive mixed liquid;
the solidifying and forming process is to add cross-linking agent and promoter into the mixed liquid to disperse uniformly, then add vulcanized rubber composition and vulcanizing agent, solidify and cool the mixed liquid to obtain the final product.
At least one of coupling agents amine, epoxy, vinyl and acrylic ester;
the weight proportion of the coupling agent amine, epoxy, vinyl and acrylic ester is 0.3-1%;
the cross-linking agent is at least one single substance or mixture of dinitrile amine and its derivative, hexamethylenetetramine, methylolmelamine, hexamethylenemelamine, diaminomaleonitrile and its derivative, boron trifluoride gel complex, imidazole derivative and organic acid hydrazide;
the weight proportion of dinitrile amine and its derivative, hexamethylenetetramine, hydroxymethyl melamine, hexamethylenemelamine, diaminomaleonitrile and its derivative, boron trifluoride complex, imidazole derivative and organic acid hydrazide is 0.4% -1%.
The filling oil is polybutene oil; the weight proportion of polybutene oil is 2%;
the vulcanized rubber composition is a mixture of a vulcanizing agent, an accelerator and an anti-aging agent, and the anti-aging agent is an anti-aging agent D or an anti-aging agent MBZ;
the mixture of vulcanizing agent, accelerator and anti-aging agent, the anti-aging agent is anti-aging agent D or anti-aging agent MBZ, and the weight proportion is 0.5% -1.2%.
The vulcanizing agent is any one of zinc oxide, magnesium oxide and stearic acid;
the weight proportion of zinc oxide, magnesium oxide and stearic acid is 0.3% -1%;
the accelerator is one of N-cyclohexyl-2-benzothiazole sulfenamide or N, N-diethyl dithio amino benzothiazole;
the weight proportion of the N-cyclohexyl-2-benzothiazole sulfenamide or the N, N-diethyl dithio amino benzothiazole is 0.2% -0.8%.
The vulcanized rubber composition and the vulcanizing agent are added for reaction and fusion during mixing, so that the curing speed of the prepared hot-melt pressure-sensitive adhesive is obviously improved, the hot-melt pressure-sensitive adhesive is easy to be pasted and convenient to operate, the antioxidant 1010 and 225 of the compound formula are added in the ingredients, the addition amount is 0.3-1% of the total amount, the cured hot-melt pressure-sensitive adhesive is prevented from cracking, the storage time is prolonged, and the storage stability of the liquid nitrile rubber and the polyester plasticizer can be improved.
According to the preparation method of the high-viscosity hot-melt pressure-sensitive adhesive, in the process of preparing the hot-melt pressure-sensitive adhesive, the rosin modified tackifying resin, the terpene tackifying resin and the petroleum resin are added, and the crosslinking type high-molecular emulsion thickener formed by copolymerization of acrylic ester and methacrylic ester is mixed to obtain the high-viscosity modified liquid, so that the prepared hot-melt pressure-sensitive adhesive has good leveling property and fluidity, the pilling increasing capability is high, the sedimentation resistance and the mildew resistance are good, and molecules such as the petroleum resin and the terpene tackifying resin have good ageing resistance, so that the formed hot-melt pressure-sensitive adhesive has high viscosity, the density of the hot-melt pressure-sensitive adhesive is increased, the ageing resistance is stronger, the mineral oil is replaced by the polybutene oil, the cohesive force and the heat resistance of the hot-melt pressure-sensitive adhesive are greatly improved, the formula cost of the adhesive is reduced, and the practicability of the hot-melt pressure-sensitive adhesive is improved; by adding one of the free radical terminator and the hydroperoxide decomposer, the hot-melt pressure-sensitive adhesive is slightly dissolved in esters with polar solvents such as water, alcohol and the like, so that the prepared hot-melt pressure-sensitive adhesive has protective effect on aging caused by oxygen, heat and moonlight, thereby realizing environmental protection and pollution reduction, and the peroxide which is generated by heating a decomposable polymer material with low toxicity and good thermal stability has strong water extraction resistance, can be recycled after being soaked in hot water, has no influence on quality, has excellent synergistic effect when being compounded with phenolic or amine antioxidants, ensures that the hot-melt pressure-sensitive adhesive is prevented from aging after heat aging and ultraviolet light irradiation, and improves the oxidation resistance strength of the hot-melt pressure-sensitive adhesive; the crosslinking agent and the accelerator are combined, the amount of the accelerator is larger than that of the crosslinking agent, the vulcanized rubber composition and the vulcanizing agent are added to react and fuse during mixing, so that the curing speed of the prepared hot-melt pressure-sensitive adhesive is obviously improved, the hot-melt pressure-sensitive adhesive is easy to be pasted and convenient to operate, the antioxidant is added into ingredients, the total amount of the antioxidant is 0.3-1%, the cured hot-melt pressure-sensitive adhesive is prevented from cracking, the storage time is prolonged, and the storage stability of the liquid nitrile rubber and the polyester plasticizer can be improved. The whole hot-melt pressure-sensitive adhesive has the advantages of simple preparation process, strong practicability, high viscosity and good use effect.
A preparation method of a high-viscosity hot-melt pressure-sensitive adhesive comprises the following steps:
step one: preparing base materials, namely preparing raw materials such as a plasticizer, a thickener, a tackifier, resin, a photoinitiator, an ultraviolet light absorber, an antioxidant, a curing agent, a coupling agent, an accelerator, a crosslinking agent and filling oil after weight balancing according to weight balancing proportion;
step two: mixing, namely crushing and stirring the prepared base materials through equipment such as a stirrer, a temperature controller, a crusher and the like to realize the mixing of the base materials to obtain mixed liquid;
step three: preparing a modified liquid, adding rosin modified tackifying resin, terpene tackifying resin, petroleum resin, acrylic ester and methacrylic ester into the mixed liquid, and adding polybutene oil to prepare the modified liquid;
step four: adding filler, adding one of a free radical terminator and a hydroperoxide decomposer into the modified liquid, dissolving the modified liquid and polar solvents such as water, alcohol and the like in esters, and stirring to obtain hot-melt pressure-sensitive adhesive mixed liquid;
step five: and (3) curing and forming to obtain a finished product, adding a cross-linking agent and an accelerator for uniform dispersion, casting to form a film, adding a vulcanized rubber composition and a vulcanizing agent, and curing and cooling the mixed liquid after mixing to obtain the high-viscosity anti-sedimentation hot-melt pressure-sensitive adhesive.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. The preparation system of the high-viscosity hot-melt pressure-sensitive adhesive is characterized by comprising the steps of preparing a base material, mixing, preparing a modified liquid, adding a filler, curing and forming, and the following weight proportion base materials: 2.5% of plasticizer, 2.5% of thickener, 2.5% of tackifier, 2.5% of resin, 2% of photoinitiator, 2% of ultraviolet light absorber, 1.5% of antioxidant, 2.5% of curing agent, 0.5% of coupling agent, 1% of cross-linking agent, 1.5% of filling oil, 1.5% of vulcanized rubber composition, 1.5% of vulcanizing agent and 1.5% of accelerator, and adding water 2% and 1.5% of alcohol and other polar solvents;
the base material is prepared by weighting 2.5% of plasticizer, 2.5% of thickening agent, 2.5% of tackifier, 2.5% of resin, 2% of photoinitiator, 2% of ultraviolet light absorber, 1.5% of antioxidant, 2.5% of curing agent, 0.5% of coupling agent, 1% of cross-linking agent, 1.5% of filling oil, 1.5% of vulcanized rubber composition, 1.5% of vulcanizing agent and 1.5% of accelerator, 2% of water, 1.5% of alcohol and other polar solvents according to weight proportion;
the mixing treatment is to mix the prepared base materials through a stirrer, a temperature controller, a pulverizer and other equipment to obtain a mixed solution;
the prepared modified liquid is used for adding a tackifier and a thickener into the mixed liquid, and adding filling oil to prepare the modified liquid;
the filler is used for adding an antioxidant into the modified liquid, dissolving the antioxidant and polar solvents such as water, alcohol and the like in esters, and then stirring the mixture to obtain hot-melt pressure-sensitive adhesive mixed liquid;
the solidifying and forming process is to add cross-linking agent and promoter into the mixed liquid to disperse uniformly, then add vulcanized rubber composition and vulcanizing agent, solidify and cool the mixed liquid to obtain the final product.
2. The system according to claim 1, wherein: the plasticizer is at least one of unsaturated polyester resin, polyamide resin, naphthenic base rubber softening oil, liquid polyisobutene, naphthenic oil, liquid paraffin and white oil;
the weight proportion of the unsaturated polyester resin, the polyamide resin, the naphthenic rubber softening oil, the liquid polyisobutene, the naphthenic oil, the liquid paraffin and the white oil is 0.3% -0.5% of the unsaturated polyester resin, 0.3% -0.5% of the polyamide resin, 0.3% -0.5% of the naphthenic rubber softening oil, 0.3% -0.5% of the liquid polyisobutene, 0.3% -0.5% of the naphthenic oil, 0.3% -0.5% of the liquid paraffin and 0.3% -0.5% of the white oil;
the thickener is a cross-linked polymer emulsion thickener formed by copolymerization of acrylic ester and methacrylic ester;
the weight proportion of the cross-linked polymer emulsion thickener formed by copolymerization of acrylic ester and methacrylic ester is 0.2-0.4% of acrylic ester and 0.2-0.4% of methacrylic ester.
3. The system according to claim 1, wherein: the tackifier is at least one of terpene tackifying resin, petroleum resin, copolymer resin, rosin modified tackifying resin, hydrogenated rosin, polymerized rosin, rosin glyceride, resin, ancient road resin and modified rosin;
the weight proportion of the terpene tackifying resin, the petroleum resin, the copolymer resin, the rosin modified tackifying resin, the hydrogenated rosin, the polymerized rosin, the rosin glyceride, the resin, the ancient road resin and the modified rosin is 0.3-0.6% of the terpene tackifying resin, 0.3-0.6% of the petroleum resin, 0.3-0.6% of the copolymer resin, 0.3-0.6% of the rosin modified tackifying resin, 0.3-0.6% of the hydrogenated rosin, 0.3-0.6% of the polymerized rosin, 0.3-0.6% of the rosin glyceride, 0.3-0.6% of the resin, 0.3-0.6% of the ancient road resin and 0.3-0.6% of the modified rosin;
the resin is at least one of E-44 bisphenol A epoxy resin, E-51 bisphenol A epoxy resin, E-20 bisphenol A epoxy resin, E-12 bisphenol A epoxy resin, F-51 linear phenolic epoxy resin, F-44 linear phenolic epoxy resin, PYSM resin, FB resin, bisphenol A linear phenolic resin, active alkyl phenolic resin, benzoxazine resin, hydrogenated carbon five petroleum resin and fully hydrogenated carbon nine petroleum resin;
the weight proportion of the resin is 0.5% -1%;
the photoinitiator is at least one of 2,4,6 (trimethyl benzoyl) diphenyl phosphine oxide, 4-dimethyl amino benzoic acid isooctyl ester and 2, 4-diethyl thioxanthone;
the weight proportion of the 2,4,6 (trimethyl benzoyl) diphenyl phosphine oxide, the 4-dimethyl amino benzoic acid isooctyl ester and the 2, 4-diethyl thioxanthone is 0.2% -1% of 2,4,6 (trimethyl benzoyl) diphenyl phosphine oxide, 0.2% -1% of 4-dimethyl amino benzoic acid isooctyl ester and 0.2% -1% of 2, 4-diethyl thioxanthone;
the ultraviolet light absorber is at least one of 2- (2 '-hydroxy-5' -methylphenyl) benzotriazole and bis (2, 6-tetramethyl-4-piperidinyl) sebacate;
the weight proportion of the 2- (2 '-hydroxy-5' -methylphenyl) benzotriazole and bis (2, 6-tetramethyl-4-piperidinyl) sebacate is 0.5% -2%.
4. A system according to claim 3, characterized in that: the antioxidant is at least one of pentaerythritol tetra- [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], tris [2, 4-di-tert-butylphenyl ] phosphite, a free radical terminator, a hydroperoxide decomposer and n-octadecanol beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate;
the weight proportion of the antioxidant is 0.5% -1%;
the curing agent is an epoxy resin curing agent;
the weight proportion of the epoxy resin curing agent is 2%.
5. The system according to claim 1, wherein: at least one of coupling agent amine, epoxy, vinyl and acrylic ester;
the weight proportion of the coupling agent amine, epoxy, vinyl and acrylic ester is 0.3-1%;
the cross-linking agent is at least one single substance or mixture of dinitrile amine and derivatives thereof, hexamethylenetetramine, methylolmelamine, hexamethylenemelamine, diaminomaleonitrile and derivatives thereof, boron trifluoride gum complex, imidazole derivatives and organic acid hydrazide;
the weight proportion of the dinitrile amine and the derivative thereof, the hexamethylenetetramine, the methylolmelamine, the hexamethylenemelamine, the diaminomaleonitrile and the derivative thereof, the boron trifluoride glue complex, the imidazole derivative and the organic acid hydrazide is 0.4-1 percent.
6. The system according to claim 5, wherein: the filling oil is polybutene oil; the weight proportion of the polybutene oil is 2%;
the vulcanized rubber composition is a mixture of a vulcanizing agent, an accelerator and an anti-aging agent, and the anti-aging agent is an anti-aging agent D or an anti-aging agent MBZ;
the mixture of the vulcanizing agent, the accelerator and the anti-aging agent is that the anti-aging agent D or the anti-aging agent MBZ has the weight proportion of 0.5 to 1.2 percent.
7. The system according to claim 1, wherein: the vulcanizing agent is any one of zinc oxide, magnesium oxide and stearic acid;
the weight proportion of the zinc oxide, the magnesium oxide and the stearic acid is 0.3% -1%;
the accelerator is one of N-cyclohexyl-2-benzothiazole sulfenamide or N, N-diethyl dithioamino benzothiazole;
the weight proportion of the N-cyclohexyl-2-benzothiazole sulfenamide or the N, N-diethyl dithioamino benzothiazole is 0.2% -0.8%.
8. A preparation method of a high-viscosity hot-melt pressure-sensitive adhesive comprises the following steps:
step one: preparing base materials, namely preparing raw materials such as a plasticizer, a thickener, a tackifier, resin, a photoinitiator, an ultraviolet light absorber, an antioxidant, a curing agent, a coupling agent, an accelerator, a crosslinking agent and filling oil after weight balancing according to weight balancing proportion;
step two: mixing, namely crushing and stirring the prepared base materials through equipment such as a stirrer, a temperature controller, a crusher and the like to realize the mixing of the base materials to obtain mixed liquid;
step three: preparing a modified liquid, adding rosin modified tackifying resin, terpene tackifying resin, petroleum resin, acrylic ester and methacrylic ester into the mixed liquid, and adding polybutene oil to prepare the modified liquid;
step four: adding filler, adding one of a free radical terminator and a hydroperoxide decomposer into the modified liquid, dissolving the modified liquid and polar solvents such as water, alcohol and the like in esters, and stirring to obtain hot-melt pressure-sensitive adhesive mixed liquid;
step five: and (3) curing and forming to obtain a finished product, adding a cross-linking agent and an accelerator for uniform dispersion, casting to form a film, adding a vulcanized rubber composition and a vulcanizing agent, and curing and cooling the mixed liquid after mixing to obtain the high-viscosity anti-sedimentation hot-melt pressure-sensitive adhesive.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117965144A (en) * | 2024-04-02 | 2024-05-03 | 中国石油大学(华东) | Resin mortar plugging system suitable for fracture-cavity stratum, and preparation and application thereof |
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