CN114806471A - Light-curable rubber hot melt adhesive with extremely high thermal stability and preparation method thereof - Google Patents
Light-curable rubber hot melt adhesive with extremely high thermal stability and preparation method thereof Download PDFInfo
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- CN114806471A CN114806471A CN202110070156.7A CN202110070156A CN114806471A CN 114806471 A CN114806471 A CN 114806471A CN 202110070156 A CN202110070156 A CN 202110070156A CN 114806471 A CN114806471 A CN 114806471A
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 50
- 239000005060 rubber Substances 0.000 title claims abstract description 45
- 239000004831 Hot glue Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 229920005989 resin Polymers 0.000 claims abstract description 26
- 239000011347 resin Substances 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000003756 stirring Methods 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 12
- 239000005062 Polybutadiene Substances 0.000 claims description 11
- 239000003921 oil Substances 0.000 claims description 11
- 229920002857 polybutadiene Polymers 0.000 claims description 11
- 229920003002 synthetic resin Polymers 0.000 claims description 11
- 239000000057 synthetic resin Substances 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 230000000087 stabilizing effect Effects 0.000 claims description 9
- -1 4-dimethylaminobenzoic acid isooctyl ester Chemical class 0.000 claims description 8
- 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 7
- 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 7
- 239000003963 antioxidant agent Substances 0.000 claims description 7
- 230000003078 antioxidant effect Effects 0.000 claims description 7
- 239000003208 petroleum Substances 0.000 claims description 7
- 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 7
- 239000003999 initiator Substances 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 229920000642 polymer Polymers 0.000 claims description 6
- 150000003505 terpenes Chemical class 0.000 claims description 6
- 235000007586 terpenes Nutrition 0.000 claims description 6
- WPMYUUITDBHVQZ-UHFFFAOYSA-N 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoic acid Chemical compound CC(C)(C)C1=CC(CCC(O)=O)=CC(C(C)(C)C)=C1O WPMYUUITDBHVQZ-UHFFFAOYSA-N 0.000 claims description 5
- BXOUVIIITJXIKB-UHFFFAOYSA-N ethene;styrene Chemical group C=C.C=CC1=CC=CC=C1 BXOUVIIITJXIKB-UHFFFAOYSA-N 0.000 claims description 5
- 229920005996 polystyrene-poly(ethylene-butylene)-polystyrene Polymers 0.000 claims description 5
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 5
- 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 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 150000001721 carbon Chemical class 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 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 4
- 238000011049 filling Methods 0.000 claims description 3
- 229920003049 isoprene rubber Polymers 0.000 claims description 3
- 239000004014 plasticizer Substances 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 3
- FGHOOJSIEHYJFQ-UHFFFAOYSA-N (2,4-ditert-butylphenyl) dihydrogen phosphite Chemical compound CC(C)(C)C1=CC=C(OP(O)O)C(C(C)(C)C)=C1 FGHOOJSIEHYJFQ-UHFFFAOYSA-N 0.000 claims description 2
- SWCWTZPHRJUTRN-UHFFFAOYSA-N C=C.C(=C)C=CC1=CC=CC=C1 Chemical group C=C.C(=C)C=CC1=CC=CC=C1 SWCWTZPHRJUTRN-UHFFFAOYSA-N 0.000 claims description 2
- SSDSCDGVMJFTEQ-UHFFFAOYSA-N octadecyl 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)CCC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 SSDSCDGVMJFTEQ-UHFFFAOYSA-N 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 150000003440 styrenes Chemical class 0.000 claims 1
- 239000000853 adhesive Substances 0.000 abstract description 17
- 230000001070 adhesive effect Effects 0.000 abstract description 17
- 239000000806 elastomer Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 2
- 238000005286 illumination Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 22
- 230000000052 comparative effect Effects 0.000 description 19
- 239000000758 substrate Substances 0.000 description 18
- 239000003292 glue Substances 0.000 description 11
- 238000001723 curing Methods 0.000 description 7
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 4
- 230000032683 aging Effects 0.000 description 4
- 238000003848 UV Light-Curing Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000009863 impact test Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 230000003712 anti-aging effect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- RRHGJUQNOFWUDK-UHFFFAOYSA-N Isoprene Chemical class CC(=C)C=C RRHGJUQNOFWUDK-UHFFFAOYSA-N 0.000 description 1
- 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 description 1
- 230000009471 action Effects 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- FACXGONDLDSNOE-UHFFFAOYSA-N buta-1,3-diene;styrene Chemical class C=CC=C.C=CC1=CC=CC=C1.C=CC1=CC=CC=C1 FACXGONDLDSNOE-UHFFFAOYSA-N 0.000 description 1
- 238000010382 chemical cross-linking Methods 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000002431 foraging effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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- 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
- C09J153/00—Adhesives based on block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
- C09J153/02—Vinyl aromatic monomers and conjugated dienes
-
- 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
- C09J125/00—Adhesives based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Adhesives based on derivatives of such polymers
- C09J125/02—Homopolymers or copolymers of hydrocarbons
- C09J125/04—Homopolymers or copolymers of styrene
-
- 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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to a light-curable rubber hot melt adhesive with extremely high thermal stability and a preparation method thereof, which introduces light-curable reaction groups on the basis of the traditional SBC hot melt adhesive, so that the adhesive can react after UV illumination to obtain a certain cross-linked network elastomer, thereby greatly improving the high temperature resistance and high humidity resistance of the adhesive, being applicable to occasions with higher requirements such as structural bonding of electronic devices and the like, and improving the economic value of the adhesive; in addition, the use of the hydrogenated resin can lead the adhesive to be continuously used for a long time at a very high temperature, thereby improving the production efficiency and the benefit.
Description
Technical Field
The invention relates to the field of adhesives, in particular to a light-curable rubber hot melt adhesive with extremely high thermal stability and a preparation method thereof.
Background
The traditional SBC rubber type hot melt adhesive is formed by simply and physically mixing an SBC elastomer, petroleum resin, tackifying resin and a plasticizer, can obtain the hot melt adhesive with certain initial strength by formula adjustment, and is widely applied to the label, adhesive tape, packaging industries and the like. However, since no chemical crosslinking exists in the system, the product of the system is easy to age and has poor performance under severe weather conditions such as high temperature and high humidity after being used. In addition, under the high temperature condition, if more non-hydrogenated resin is used, the glue is easy to crosslink and solidify, the use of the glue is influenced, and the production efficiency is reduced and the cost is improved due to the shutdown action accompanying the replacement of the glue.
Disclosure of Invention
The invention aims to provide a light-curable rubber hot melt adhesive with extremely high thermal stability and a preparation method thereof.
In order to achieve the above purpose, the solution of the invention is:
a light-curable rubber hot melt adhesive with extremely high thermal stability is characterized by comprising the following raw materials in parts by weight:
further, the hydrogenated SBC rubber polymer is one or more of styrene-ethylene/butylene-styrene, styrene-ethylene/propylene-styrene, styrene-ethylene/butylene/styrene-styrene, maleic anhydride-reacted styrene-ethylene/butylene-styrene, and terminal vinyl styrene-ethylene/propylene-styrene.
Further, the hydrogenated vinyl-terminated polybutadiene or hydrogenated isoprene rubber is a liquid rubber with at least one terminal group having a vinyl functional group.
Further, the hydrogenated synthetic resin is one or a mixture of hydrogenated carbon five petroleum resin, carbon nine petroleum resin, carbon five/carbon nine petroleum resin and styrene resin.
Furthermore, the tackifying resin is rosin, rosin derivatives, terpene resin or one or a mixture of terpene resin derivatives.
Further, the photo-free radical initiator is one or a mixture of 2,4,6 (trimethyl benzoyl) diphenyl phosphine oxide, 4-dimethylaminobenzoic acid isooctyl ester and 2, 4-diethylthioxanthone.
Further, the plasticizer is one of naphthenic oils.
Further, the antioxidant is one or more of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, tri [2, 4-di-tert-butylphenyl ] phosphite and beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl ester.
A preparation method of a light-curable rubber hot-melt adhesive with extremely high thermal stability is characterized by comprising the following steps:
step one, adding 20-40 parts of hydrogenated SBC rubber polymer, 0-35 parts of naphthenic oil and 0.2-1 part of antioxidant into a reactor, heating to 140-170 ℃, stirring until all materials are molten, and stabilizing the reaction for 15 min;
under the stirring condition, adding 5-10 parts of hydrogenated terminal vinyl polybutadiene or hydrogenated terminal isoprene rubber, 0-20 parts of tackifying resin, 35-45 parts of hydrogenated synthetic resin and 0.2-1 part of photo-free radical initiator, stirring for 30min, defoaming, filling into an opaque rubber tube, and sealing and storing;
the parts of the components are all parts by weight
The invention introduces the photo-curable reactive group on the basis of the traditional SBC hot melt adhesive, so that the adhesive can react after UV illumination to obtain a certain cross-linked network elastomer, thereby greatly improving the high temperature resistance and high humidity resistance of the elastomer, being used for occasions with higher requirements such as structural bonding of electronic devices and the like, and improving the economic value of the elastomer; in addition, the use of the hydrogenated resin can lead the adhesive to be continuously used for a long time at a very high temperature, thereby improving the production efficiency and the benefit.
Detailed Description
The following detailed description of the embodiments of the present invention is intended to be illustrative, and not to be construed as limiting the invention.
Example 1
Adding 20 parts of styrene-ethylene-styrene, 15 parts of naphthenic oil and 0.2 part of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) n-octadecyl propionate into a reactor, heating to 140 ℃ and 170 ℃, stirring until all materials are molten, and stabilizing the reaction for 15 min; then, 10 parts of hydrogenated vinyl-terminated polybutadiene liquid rubber, 10 parts of rosin, 45 parts of hydrogenated synthetic resin and 0.2 part of 2, 4-diethylthioxanthone were added under stirring, stirred for 30min, defoamed, filled in an opaque hose, and sealed and stored.
Example 2
Adding 30 parts of styrene-ethylene-styrene, 20 parts of naphthenic oil and 0.5 part of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester into a reactor, heating to 140 ℃ and 170 ℃, stirring until all materials are molten, and stabilizing the reaction for 15 min; then, 5 parts of hydrogenated vinyl-terminated polybutadiene liquid rubber, 10 parts of terpene resin, 35 parts of hydrogenated synthetic resin and 0.5 part of 2, 4-diethylthioxanthone were added under stirring, stirred for 30min, defoamed, filled into an opaque hose, and sealed and stored.
Example 3
Adding 30 parts of maleic anhydride-modified styrene-ethylene/butylene-styrene, 35 parts of naphthenic oil and 1 part of tris [2, 4-di-tert-butylphenyl ] phosphite into a reactor, then heating to 140 ℃ and 170 ℃, stirring until all materials are molten, and stabilizing the reaction for 15 min; then, 5 parts of hydrogenated vinyl-terminated polybutadiene liquid rubber, 35 parts of hydrogenated synthetic resin and 0.2 part of 2,4,6 (trimethylbenzoyl) diphenylphosphine oxide were added under stirring, stirred for 30min, and finally defoamed, filled into an opaque hose, and sealed and stored.
Example 4
Adding 40 parts of styrene-ethylene-styrene and 1 part of antioxidant into a reactor, then heating to 140-170 ℃, stirring until all materials are molten, and stabilizing the reaction for 15 min; then, 10 parts of hydrogenated vinyl-terminated polybutadiene liquid rubber, 45 parts of hydrogenated synthetic resin, 20 parts of rosin and 0.22, 4-diethylthioxanthone were added under stirring, stirred for 30min, defoamed, filled into an opaque hose, and sealed and stored.
Example 5
Adding 40 parts of hydrogenated styrene-butadiene-styrene with vinyl end groups, 15 parts of naphthenic oil and 1 part of antioxidant into a reactor, then heating to 140 ℃ and 170 ℃, stirring until all materials are molten, and stabilizing the reaction for 15 min; then, 5 parts of hydrogenated vinyl-terminated polybutadiene liquid rubber, 35 parts of hydrogenated synthetic resin, 5 parts of terpene resin and 1 part of 2,4,6 (trimethylbenzoyl) diphenylphosphine oxide are added under stirring, stirred for 30min, defoamed, filled into an opaque rubber tube, and sealed and stored.
Comparative example 1
Adding 20 parts of styrene-ethylene-styrene, 15 parts of naphthenic oil and 0.2 part of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester into a reactor, heating to 140-170 ℃, stirring until all materials are molten, and stabilizing the reaction for 15 min; then, under the stirring condition, adding 20 parts of rosin and 45 parts of styrene resin, stirring for 30min, finally defoaming, filling into an opaque rubber tube, sealing and storing; is a traditional SBC rubber hot melt adhesive.
Comparative example 2
Adding 20 parts of non-hydrogenated SBC rubber polymer 15 parts of naphthenic oil and 0.2 part of antioxidant into a reactor, then heating to 140-; then, 10 parts of non-hydrogenated vinyl-terminated polybutadiene liquid rubber, 10 parts of tackifying resin, 45 parts of non-hydrogenated synthetic resin and 0.2 part of photo-radical initiator are added under stirring, stirred for 30min, defoamed, filled into an opaque rubber tube, sealed and stored.
Comparative example 3
Adding 20 parts of partially hydrogenated SBC rubber polymer, 15 parts of naphthenic oil and 0.2 part of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester into a reactor, heating to 140 ℃ and 170 ℃, stirring until all materials are molten, and stabilizing the reaction for 15 min; then, 10 parts of partially hydrogenated vinyl-terminated polybutadiene liquid rubber, 10 parts of tackifying resin, 45 parts of partially hydrogenated synthetic resin and 0.2 part of photo-radical initiator are added under stirring, stirred for 30min, defoamed, filled into an opaque rubber tube, sealed and stored.
The parts mentioned in the above comparative examples and examples are parts by weight.
The samples obtained in comparative examples 1-3 and examples 1-5 were subjected to the following performance tests, the specific test methods were as follows:
1. the viscosity test adopts a Brookfield rotational viscometer, the tested sample is preheated for 10min at 170 ℃, the completely preheated sample is poured into a sample cup, the sample cup is fixed in a heater, the position is adjusted to ensure that a rotor on the viscometer is positioned at the center of the tested sample in the sample cup, the temperature of the heater is adjusted, the rotor and the tested sample are kept constant in the sample cup for 10min, the temperature of the sample is ensured to be stable at 170 ℃, and the temperature of the sample is within +/-1 ℃ of the specified temperature; the temperature is kept constant at 170 ℃, the rotor is opened, and after rotating for 20min, the viscosity data at this time is read, wherein the viscosity unit is 'cps'.
2. Attenuation test method of glue amount by continuous heating at 170 ℃ for 48 hours:
heating the glue to 170 ℃, testing the glue yield for 20s at a certain air pressure as m1, baking the sealed glue in an oven at 170 ℃ for 48 hours, testing the glue yield for 20s at the same air pressure or 170 ℃ as m2, and calculating the glue yield attenuation (m2-m1)/m1 × 100%
3. And (3) testing the thrust strength:
1) testing of initial thrust strength of UV curing: dispensing a tested sample adhesive on the surface of a substrate by a table type dispenser, then placing the substrate into an ultraviolet irradiation instrument for curing, bonding two substrates together by using a substrate mold, controlling the thickness of the adhesive to be 0.15mm and the weight of the adhesive to be 0.05 +/-0.003 g, maintaining the pressure by using a force of 2kg, placing the substrate in an environment with the temperature of 23 +/-2 ℃ and the relative humidity of 50 +/-5 ℃ for 5min for initial time, testing by using a three-pin universal testing machine until the initial time is up, loading a sample by using a clamp of the testing machine at the moving speed of 10mm/min, and recording the maximum load and bonding area of the sample damaged by thrust;
2) testing the final thrust strength Mpa: the method comprises the following steps of dispensing a tested sample adhesive on the surface of a substrate by a table type dispenser, then placing the substrate into an ultraviolet irradiation instrument for curing, bonding two substrates together by using a substrate mold, controlling the thickness of the adhesive to be 0.15mm and the weight of the adhesive to be 0.05 +/-0.003 g, maintaining the pressure by using a 2kg force, placing the substrate in an environment with the temperature of 23 +/-2 ℃ and the relative humidity of 50 +/-5 ℃ for 48 hours for final curing, testing by using a three-throw universal testing machine when the time is up, loading a sample by a clamp of the testing machine at the moving speed of 10mm/min, and recording the maximum load and the bonding area of the thrust damage of the sample.
The UV curing is carried out by adopting a professional ultraviolet irradiation instrument and setting the irradiation intensity of ultraviolet light to be 1000mw/cm 2 UV。。
4. Dupont ball impact test:
dispensing a tested sample adhesive on the surface of a substrate by a table type dispenser, then placing the substrate into an ultraviolet irradiation instrument for curing, bonding two substrates together by using a substrate mold, controlling the thickness of the adhesive to be 0.15mm and the weight of the adhesive to be 0.05 +/-0.003 g, maintaining the pressure by using 2kg of force, placing the substrate in an environment with the temperature of 23 +/-2 ℃ and the relative humidity of 50 +/-5 ℃ for 48h for final curing, placing the cured substrate into a DuPont ball impact tester, and recording impact data of the tested sample when the substrate is peeled off under the conditions of 200g and 70 mm.
5. High temperature and high humidity aging test:
and (3) curing the tested sample for 48h (the curing process is the same as that of the DuPont falling ball impact test), aging the sample in an Aisbeck constant-temperature and constant-humidity box, aging the sample in the Aisbeck constant-temperature and constant-humidity box for 72h, taking out the tested sample, and testing the aged strength of the sample by adopting a normal-temperature pushing method. The test selects two environmental conditions for aging, wherein one environmental condition is that the temperature is 85 ℃ and the humidity is 85 percent; another environmental condition is a temperature of 60 ℃ and a humidity of 90%.
In the above tests, adhesion tests were performed mainly on three more common substrate combinations of ABS/ABS, PS/SS ink glass/PBT;
the test data are collated to obtain the following tables I to III:
table A comparison of the viscosity, damping, and thrust Strength tests of comparative examples 1-3 and examples 1-5
As can be seen from the test data in Table I, the test data of examples 1-5 have the following characteristics compared with comparative examples 1-3:
1. the viscosity is improved to some extent, but within a reasonable range, the use of the product is not influenced;
2. under the condition that the temperature is 170 ℃ for 48 hours, the glue yield of the examples 1-5 is reduced less under the same air pressure, and the glue yield of the comparative examples 1-3 is reduced obviously, which shows that the thermal stability of the examples 1-5 is obviously superior to that of the comparative examples 1-3;
3. after UV curing, the initial thrust strength of the examples 1-5 is higher than that of the comparative example 1, and the final strength of the 48-hour film is obviously improved compared with that of the comparative example 1, which shows that the bonding effect of the SBR rubber hot melt adhesive is obviously improved compared with that of the traditional SBR rubber hot melt adhesive; the initial thrust strength of the examples 1-5 is similar to or improved to a certain extent compared with the comparative examples 2-3, and the final strength of the 48-hour is similar to or obviously improved compared with the comparative examples 2-3, which shows that the bonding effect of the adhesive is not lost or even improved to some extent.
Table two: DuPont ball impact test comparison of comparative examples 1-3 and examples 1-5
From the detection data in table two, it can be seen that the dupont falling ball impact of examples 1-5 is improved more than that of comparative example 1, which indicates that the anti-peeling effect of the present patent is improved higher than that of the traditional SBR rubber type hot melt adhesive; the DuPont falling ball impact achieved in examples 1-5 is similar to that achieved in comparative examples 2-3, thereby demonstrating that the products obtained in this patent exhibit improved thermal stability without loss of peel resistance.
Table three: comparison of high temperature and high humidity aging test between comparative examples 1 to 3 and examples 1 to 5
As noted in the comparison of the data in table three, the adhesion strength values of examples 1 to 5 were much improved compared with comparative example 1 in the high-temperature and high-humidity environment, which indicates that the anti-aging effect of the SBR rubber hot melt adhesive is improved more than that of the conventional SBR rubber hot melt adhesive under the high-temperature and high-humidity conditions; similar to or slightly improved from comparative examples 2 to 3, it is demonstrated that the product obtained by the present invention has no loss of the anti-aging effect under high temperature and high humidity conditions while improving the thermal stability.
The above description is only an embodiment of the present invention, and is not intended to limit the design of the present invention, and all equivalent changes made according to the design key of the present invention fall within the protection scope of the present invention.
In the description of the specification, reference to the description of "one embodiment," "some embodiments," "an example," "a specific example," or "some examples" or the like means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (9)
1. A light-curable rubber hot melt adhesive with extremely high thermal stability is characterized by comprising the following raw materials in parts by weight:
2. a photocurable rubber hot melt adhesive with extremely high thermal stability as claimed in claim 1, wherein: the hydrogenated SBC rubber polymer is one or more of styrene-ethylene/butylene-styrene, styrene-ethylene/propylene-styrene, styrene-ethylene/butylene/styrene-styrene, maleic anhydride-reacted styrene-ethylene/butylene-styrene and terminal vinyl styrene-ethylene/propylene-styrene.
3. A photocurable rubber hot melt adhesive with extremely high thermal stability as claimed in claim 1, wherein: the hydrogenated vinyl-terminated polybutadiene or hydrogenated isoprene-terminated rubber is a liquid rubber with at least one terminal group carrying vinyl functional groups.
4. A photocurable rubber hot melt adhesive with extremely high thermal stability as claimed in claim 1, wherein: the hydrogenated synthetic resin is one or a mixture of hydrogenated carbon five petroleum resin, hydrogenated carbon nine petroleum resin, hydrogenated carbon five/carbon nine petroleum resin and hydrogenated styrene resin.
5. A photocurable rubber hot melt adhesive with extremely high thermal stability as claimed in claim 1, wherein: the tackifying resin is rosin, rosin derivatives, terpene resin or one or a mixture of terpene resin derivatives.
6. A photocurable rubber hot melt adhesive with extremely high thermal stability as claimed in claim 1, wherein: the photo-free radical initiator is one or a mixture of 2,4,6 (trimethyl benzoyl) diphenyl phosphine oxide, 4-dimethylaminobenzoic acid isooctyl ester and 2, 4-diethyl thioxanthone.
7. A photocurable rubber hot melt adhesive with extremely high thermal stability as claimed in claim 1, wherein: the plasticizer is one of naphthenic oils.
8. A photocurable rubber hot melt adhesive with extremely high thermal stability as claimed in claim 1, wherein: the antioxidant is one or more of tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester, tri [2, 4-di-tert-butylphenyl ] phosphite and beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl ester.
9. A preparation method of a light-curable rubber hot-melt adhesive with extremely high thermal stability is characterized by comprising the following steps:
step one, adding 20-40 parts of hydrogenated SBC rubber polymer, 0-35 parts of naphthenic oil and 0.2-1 part of antioxidant into a reactor, heating to 140-170 ℃, stirring until all materials are molten, and stabilizing the reaction for 15 min;
under the stirring condition, adding 5-10 parts of hydrogenated terminal vinyl polybutadiene or hydrogenated terminal isoprene rubber, 0-20 parts of tackifying resin, 35-45 parts of hydrogenated synthetic resin and 0.2-1 part of photo-free radical initiator, stirring for 30min, defoaming, filling into an opaque rubber tube, and sealing and storing;
the parts of the components are parts by weight.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115651573A (en) * | 2022-10-27 | 2023-01-31 | 广州市豪特粘接材料有限公司 | Hot melt adhesive, preparation method thereof and removable film label prepared from hot melt adhesive |
| CN117417726A (en) * | 2023-12-15 | 2024-01-19 | 广州鹿山新材料股份有限公司 | UV (ultraviolet) curing rubber pressure-sensitive adhesive as well as preparation method and application thereof |
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| KR20130063938A (en) * | 2011-12-07 | 2013-06-17 | 제일모직주식회사 | Photo-curable adhesive composition and display device comprising the same |
| CN103958628A (en) * | 2011-11-14 | 2014-07-30 | 汉高美国知识产权有限责任公司 | Adhesive compositions |
| CN107699172A (en) * | 2017-09-22 | 2018-02-16 | 广东能辉新材料科技有限公司 | Photocuring hot-fusible pressure-sensitive adhesive |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115651573A (en) * | 2022-10-27 | 2023-01-31 | 广州市豪特粘接材料有限公司 | Hot melt adhesive, preparation method thereof and removable film label prepared from hot melt adhesive |
| CN115651573B (en) * | 2022-10-27 | 2023-11-28 | 广州市豪特粘接材料有限公司 | Hot melt adhesive, preparation method thereof and removable film label prepared from hot melt adhesive |
| CN117417726A (en) * | 2023-12-15 | 2024-01-19 | 广州鹿山新材料股份有限公司 | UV (ultraviolet) curing rubber pressure-sensitive adhesive as well as preparation method and application thereof |
| CN117417726B (en) * | 2023-12-15 | 2024-03-15 | 广州鹿山新材料股份有限公司 | UV (ultraviolet) curing rubber pressure-sensitive adhesive as well as preparation method and application thereof |
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