CN114214007A - High-temperature color-change pressure-sensitive adhesive and preparation method thereof - Google Patents
High-temperature color-change pressure-sensitive adhesive and preparation method thereof Download PDFInfo
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- CN114214007A CN114214007A CN202111641676.5A CN202111641676A CN114214007A CN 114214007 A CN114214007 A CN 114214007A CN 202111641676 A CN202111641676 A CN 202111641676A CN 114214007 A CN114214007 A CN 114214007A
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- sensitive adhesive
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- acrylate
- pressure
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- 239000004820 Pressure-sensitive adhesive Substances 0.000 title claims abstract description 93
- 238000002360 preparation method Methods 0.000 title claims description 21
- 239000003094 microcapsule Substances 0.000 claims abstract description 35
- 229920001577 copolymer Polymers 0.000 claims abstract description 32
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 31
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 31
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims abstract description 31
- DXPPIEDUBFUSEZ-UHFFFAOYSA-N 6-methylheptyl prop-2-enoate Chemical compound CC(C)CCCCCOC(=O)C=C DXPPIEDUBFUSEZ-UHFFFAOYSA-N 0.000 claims abstract description 31
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims abstract description 31
- GMSCBRSQMRDRCD-UHFFFAOYSA-N dodecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCOC(=O)C(C)=C GMSCBRSQMRDRCD-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000003999 initiator Substances 0.000 claims abstract description 21
- 239000002904 solvent Substances 0.000 claims abstract description 21
- 239000002994 raw material Substances 0.000 claims abstract description 15
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical group CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 42
- 238000010438 heat treatment Methods 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 30
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 28
- MPIAGWXWVAHQBB-UHFFFAOYSA-N [3-prop-2-enoyloxy-2-[[3-prop-2-enoyloxy-2,2-bis(prop-2-enoyloxymethyl)propoxy]methyl]-2-(prop-2-enoyloxymethyl)propyl] prop-2-enoate Chemical compound C=CC(=O)OCC(COC(=O)C=C)(COC(=O)C=C)COCC(COC(=O)C=C)(COC(=O)C=C)COC(=O)C=C MPIAGWXWVAHQBB-UHFFFAOYSA-N 0.000 claims description 28
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 16
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 14
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical group C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 14
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 14
- 239000011248 coating agent Substances 0.000 claims description 14
- 238000000576 coating method Methods 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 14
- 229910052757 nitrogen Inorganic materials 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 14
- 238000005303 weighing Methods 0.000 claims description 14
- 239000000203 mixture Substances 0.000 claims description 11
- MDYPDLBFDATSCF-UHFFFAOYSA-N nonyl prop-2-enoate Chemical compound CCCCCCCCCOC(=O)C=C MDYPDLBFDATSCF-UHFFFAOYSA-N 0.000 claims description 8
- NOWKCMXCCJGMRR-UHFFFAOYSA-N Aziridine Chemical compound C1CN1 NOWKCMXCCJGMRR-UHFFFAOYSA-N 0.000 claims description 4
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 4
- 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 4
- 239000006185 dispersion Substances 0.000 claims description 4
- 239000000839 emulsion Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- LIZLYZVAYZQVPG-UHFFFAOYSA-N (3-bromo-2-fluorophenyl)methanol Chemical compound OCC1=CC=CC(Br)=C1F LIZLYZVAYZQVPG-UHFFFAOYSA-N 0.000 claims description 2
- ZDQNWDNMNKSMHI-UHFFFAOYSA-N 1-[2-(2-prop-2-enoyloxypropoxy)propoxy]propan-2-yl prop-2-enoate Chemical compound C=CC(=O)OC(C)COC(C)COCC(C)OC(=O)C=C ZDQNWDNMNKSMHI-UHFFFAOYSA-N 0.000 claims description 2
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 2
- 239000011790 ferrous sulphate Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 238000009775 high-speed stirring Methods 0.000 claims description 2
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- HLZKNKRTKFSKGZ-UHFFFAOYSA-N tetradecan-1-ol Chemical compound CCCCCCCCCCCCCCO HLZKNKRTKFSKGZ-UHFFFAOYSA-N 0.000 claims description 2
- 229940070527 tourmaline Drugs 0.000 claims description 2
- 229910052613 tourmaline Inorganic materials 0.000 claims description 2
- 239000011032 tourmaline Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000005336 cracking Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 10
- BCZKGLVONDGCTF-UHFFFAOYSA-N C(C=C)(=O)OCCCC.C(C=C)(=O)OCCCCCCCCC Chemical compound C(C=C)(=O)OCCCC.C(C=C)(=O)OCCCCCCCCC BCZKGLVONDGCTF-UHFFFAOYSA-N 0.000 description 9
- 230000001070 adhesive effect Effects 0.000 description 9
- 239000000853 adhesive Substances 0.000 description 8
- 239000002390 adhesive tape Substances 0.000 description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 5
- 229910052744 lithium Inorganic materials 0.000 description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 229910001416 lithium ion Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000306 component Substances 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000003466 welding Methods 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
- C09J133/00—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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/08—Homopolymers or copolymers of acrylic acid esters
-
- 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
- C09J133/00—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 only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Adhesives based on derivatives of such polymers
- C09J133/04—Homopolymers or copolymers of esters
- C09J133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
- C09J133/062—Copolymers with monomers not covered by C09J133/06
- C09J133/066—Copolymers with monomers not covered by C09J133/06 containing -OH groups
-
- 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
Abstract
The invention provides a high-temperature color-changing pressure-sensitive adhesive which comprises the following raw materials: 12-23 parts of butyl acrylate-nonyl acrylate copolymer, 5-8 parts of hydroxyethyl acrylate, 8-20 parts of isooctyl acrylate, 6-18 parts of lauryl methacrylate, 3-10 parts of acrylamide, 5-12 parts of acrylic acid, 2-6 parts of initiator, 1-5 parts of thermochromic microcapsule and 42-50 parts of solvent. The high-temperature color-changing pressure-sensitive adhesive has high-temperature resistance, does not cause cracking at high temperature, changes in color along with temperature change, and is convenient to operate.
Description
Technical Field
The invention belongs to the technical field of adhesives, and particularly relates to a high-temperature color-change pressure-sensitive adhesive and a preparation method thereof.
Background
With the gradual progress of new energy automobiles in social life, the yield of new energy automobiles is increased day by day, and the market provides new requirements and challenges for improving the processing efficiency of new energy automobile parts, so how to improve the production efficiency of a battery, which is one of the main core components of the new energy automobiles, also becomes an important influence factor for improving the competitiveness and economic benefit of new energy automobile enterprises. In the assembly and production process of the lithium ion battery, a special adhesive tape is generally used for fixing, insulating and protecting the tab position of the lithium ion battery. The special adhesive tape for the lithium battery generally adopts a high-molecular PI film as a base material, and special glue is coated on the base material, wherein the thickness of the special adhesive tape is 20-100 mm. The adhesive tape special for the lithium battery generally has the advantages of good viscosity, no residual adhesive left after the adhesive tape is uncovered, high temperature resistance, electrolyte resistance, high electrical insulation and the like.
The acrylate adhesive has the characteristics of simple operation, quick curing at room temperature, adjustable curing rate, oil surface bonding, no need of strict metering for two-component proportioning, strong bonding property, wide applicability and the like; therefore, in recent years, the acrylate adhesive is widely applied to structural bonding in the industries of rail transit, electronics, electrical appliances, automobiles, aviation, ships and the like.
However, the existing acrylate adhesive has poor high-temperature resistance, the stripping force is improved to more than 3N/mm under the condition that the non-stick knife cannot be realized, a welding spot part is stuck, and the sticking is realized after baking for 24H at 85 ℃ without glue failure.
Therefore, the need of the existing lithium battery processing process can be better met only by developing an adhesive tape which is resistant to high temperature, shows color change at high temperature and is easy to tear off quickly.
Disclosure of Invention
The invention aims to provide a high-temperature color-change pressure-sensitive adhesive with high peel strength and a preparation method thereof, aiming at solving the problems that the pressure-sensitive adhesive in the prior art has poor high-temperature resistance and is difficult to peel at high temperature in the processing process of a lithium battery electrode.
In order to achieve the purposes, the specific scheme is as follows:
a high-temperature color-changing pressure-sensitive adhesive comprises the following raw materials: 12-23 parts of butyl acrylate-nonyl acrylate copolymer, 5-8 parts of hydroxyethyl acrylate, 8-20 parts of isooctyl acrylate, 6-18 parts of lauryl methacrylate, 3-10 parts of acrylamide, 5-12 parts of acrylic acid, 2-6 parts of initiator, 1-5 parts of thermochromic microcapsule and 42-50 parts of solvent.
According to the technical scheme of the invention, the butyl acrylate-nonyl acrylate copolymer is preferably prepared by the following steps: 40-50 parts of butyl acrylate and 5-15 parts of nonyl acrylate, adding 3-6 parts of aziridine, and reacting at 75-80 ℃ for 20-80min to obtain the butyl acrylate-nonyl acrylate copolymer.
Preferably, the initiator is benzoyl peroxide.
Preferably, the solvent is ethyl acetate.
The preparation method of the thermochromic microcapsule comprises the following steps: 1-3 parts of crystal violet lactone, 2-6 parts of bisphenol A, 25-32 parts of n-tetradecanol, 2-4 parts of butyl methacrylate, 0.1-0.5 part of tripropylene glycol diacrylate and 0.5-2 parts of 3- (methacryloyloxy) propyl trimethoxy silane treated nano tourmaline are mixed, heated and melted, 2-4 parts of OP-10 and 0.1-2 parts of sodium dodecyl benzene sulfonate are added, and the mixture is stirred and uniformly dispersed at constant temperature to obtain a dispersion liquid; adding 80 parts by weight of water into the dispersion liquid under high-speed stirring, and uniformly stirring to obtain emulsion; adding 1-3 parts by weight of potassium persulfate into the emulsion, heating to 25-32 ℃, slowly adding 0.5-3 parts by weight of ferrous sulfate, reacting for 3 hours, filtering, cleaning, and drying to obtain the thermochromic microcapsule.
According to the technical scheme of the invention, the preparation method of the high-temperature color-changeable pressure-sensitive adhesive is as follows: 1) weighing butyl acrylate-nonyl acrylate copolymer, butyl acrylate, hydroxyethyl acrylate, isooctyl acrylate, lauryl methacrylate, acrylamide, acrylic acid, an initiator, a thermochromic microcapsule and a solvent; 2) adding butyl acrylate, hydroxyethyl acrylate, isooctyl acrylate, lauryl methacrylate, acrylamide and acrylic acid into a reaction kettle, uniformly stirring, adding a solvent and an initiator, introducing high-purity nitrogen at room temperature, heating to 80-85 ℃, 3) then adding a butyl acrylate-nonyl acrylate copolymer and a thermochromic microcapsule, heating to 88-95 ℃, keeping the temperature for 1-3h, 4) cooling to room temperature to obtain a high-temperature thermochromic pressure-sensitive adhesive solution, and controlling the viscosity of the high-temperature thermochromic pressure-sensitive adhesive solution at 3000mpas of 2000 and the solid content at 38-42%; 5) and adding the prepared high-temperature color-changing pressure-sensitive adhesive solution into 1-3% dipentaerythritol hexaacrylate (DPHA), uniformly stirring, defoaming, coating on a bottom release film, drying by an oven at 120 ℃ for 5min and at 150 ℃ for 15min, and covering the top release film to obtain the high-temperature color-changing pressure-sensitive adhesive.
Compared with the prior art, the invention has the following technical effects:
the high-temperature color-changing pressure-sensitive adhesive has high-temperature resistance, does not cause cracking at high temperature, changes in color along with temperature change, and is convenient to operate.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A first part:
preparing a butyl acrylate-nonyl acrylate copolymer, 42 parts by weight of butyl acrylate and 10 parts by weight of nonyl acrylate, adding 5 parts by weight of aziridine, and reacting at the temperature of 75-80 ℃ for 20-80min to obtain a butyl acrylate-nonyl acrylate copolymer A.
Example 1
A high-temperature color-change pressure-sensitive adhesive is prepared by weighing the following raw materials:
butyl acrylate-nonyl acrylate copolymer A120 g;
80g of hydroxyethyl acrylate;
180g of isooctyl acrylate;
60g of lauryl methacrylate;
30g of acrylamide;
120g of acrylic acid;
60g of benzoyl peroxide;
50g of thermochromic microcapsules;
and 420g of ethyl acetate.
The preparation process comprises the following steps: 1) adding butyl acrylate, hydroxyethyl acrylate, isooctyl acrylate, lauryl methacrylate, acrylamide and acrylic acid into a reaction kettle, uniformly stirring, adding a solvent and an initiator, introducing high-purity nitrogen at room temperature, heating to 80-85 ℃, 2) then adding a butyl acrylate-nonyl acrylate copolymer A and a thermochromic microcapsule, heating to 88-95 ℃, keeping the temperature for 1-3h, 3) cooling to room temperature to obtain a high-temperature photochromic pressure-sensitive adhesive solution, and controlling the viscosity of the high-temperature photochromic pressure-sensitive adhesive solution at 3000mpas of 2000 and the solid content at 38-42%; 4) and adding the prepared high-temperature color-changing pressure-sensitive adhesive solution into 1-3% dipentaerythritol hexaacrylate (DPHA), uniformly stirring, defoaming, coating on a bottom release film, drying by an oven at 120 ℃ for 5min and at 150 ℃ for 15min, and covering the top release film to obtain the high-temperature color-changing pressure-sensitive adhesive of the embodiment 1.
Example 2
A high-temperature color-change pressure-sensitive adhesive is prepared by weighing the following raw materials:
butyl acrylate-nonyl acrylate copolymer A160 g;
50g of hydroxyethyl acrylate;
150g of isooctyl acrylate;
100g of lauryl methacrylate;
60g of acrylamide;
80g of acrylic acid;
40g of benzoyl peroxide;
30g of thermochromic microcapsules;
460g of ethyl acetate.
The preparation process comprises the following steps: 1) adding butyl acrylate, hydroxyethyl acrylate, isooctyl acrylate, lauryl methacrylate, acrylamide and acrylic acid into a reaction kettle, uniformly stirring, adding a solvent and an initiator, introducing high-purity nitrogen at room temperature, heating to 80-85 ℃, 2) then adding a butyl acrylate-nonyl acrylate copolymer A and a thermochromic microcapsule, heating to 88-95 ℃, keeping the temperature for 1-3h, 3) cooling to room temperature to obtain a high-temperature photochromic pressure-sensitive adhesive solution, and controlling the viscosity of the high-temperature photochromic pressure-sensitive adhesive solution at 3000mpas of 2000 and the solid content at 38-42%; 4) and adding the prepared high-temperature color-changing pressure-sensitive adhesive solution into 1-3% dipentaerythritol hexaacrylate (DPHA), uniformly stirring, defoaming, coating on a bottom release film, drying by an oven at 120 ℃ for 5min and at 150 ℃ for 15min, and covering the top release film to obtain the high-temperature color-changing pressure-sensitive adhesive of the embodiment 2.
Example 3
A high-temperature color-change pressure-sensitive adhesive is prepared by weighing the following raw materials:
butyl acrylate-nonyl acrylate copolymer A200 g;
70g of hydroxyethyl acrylate;
120g of isooctyl acrylate;
140g of lauryl methacrylate;
80g of acrylamide;
100g of acrylic acid;
50g of benzoyl peroxide;
10g of thermochromic microcapsules;
500g of ethyl acetate.
The preparation process comprises the following steps: 1) adding butyl acrylate, hydroxyethyl acrylate, isooctyl acrylate, lauryl methacrylate, acrylamide and acrylic acid into a reaction kettle, uniformly stirring, adding a solvent and an initiator, introducing high-purity nitrogen at room temperature, heating to 80-85 ℃, 2) then adding a butyl acrylate-nonyl acrylate copolymer A and a thermochromic microcapsule, heating to 88-95 ℃, keeping the temperature for 1-3h, 3) cooling to room temperature to obtain a high-temperature photochromic pressure-sensitive adhesive solution, and controlling the viscosity of the high-temperature photochromic pressure-sensitive adhesive solution at 3000mpas of 2000 and the solid content at 38-42%; 4) and adding the prepared high-temperature color-changing pressure-sensitive adhesive solution into 1-3% dipentaerythritol hexaacrylate (DPHA), uniformly stirring, defoaming, coating on a bottom release film, drying by an oven at 120 ℃ for 5min and at 150 ℃ for 15min, and covering the top release film to obtain the high-temperature color-changing pressure-sensitive adhesive of the embodiment 3.
Example 4
A high-temperature color-change pressure-sensitive adhesive is prepared by weighing the following raw materials:
butyl acrylate-nonyl acrylate copolymer A230 g;
60g of hydroxyethyl acrylate;
80g of isooctyl acrylate;
180g of lauryl methacrylate;
100g of acrylamide;
50g of acrylic acid;
30g of benzoyl peroxide;
20g of thermochromic microcapsules;
520g of ethyl acetate.
The preparation process comprises the following steps: 1) adding butyl acrylate, hydroxyethyl acrylate, isooctyl acrylate, lauryl methacrylate, acrylamide and acrylic acid into a reaction kettle, uniformly stirring, adding a solvent and an initiator, introducing high-purity nitrogen at room temperature, heating to 80-85 ℃, 2) then adding a butyl acrylate-nonyl acrylate copolymer A and a thermochromic microcapsule, heating to 88-95 ℃, keeping the temperature for 1-3h, 3) cooling to room temperature to obtain a high-temperature photochromic pressure-sensitive adhesive solution, and controlling the viscosity of the high-temperature photochromic pressure-sensitive adhesive solution at 3000mpas of 2000 and the solid content at 38-42%; 4) and adding the prepared high-temperature color-changing pressure-sensitive adhesive solution into 1-3% dipentaerythritol hexaacrylate (DPHA), uniformly stirring, defoaming, coating on a bottom release film, drying by an oven at 120 ℃ for 5min and at 150 ℃ for 15min, and covering the top release film to obtain the high-temperature color-changing pressure-sensitive adhesive of the embodiment 4.
The test tests were carried out on the high temperature color-change pressure-sensitive adhesive of 4 of the above examples 1 to 4, and the test results were as follows:
from the above test data of examples 1-4, it can be seen that the high temperature color change pressure sensitive adhesives of examples 1-4 have high resistance to high temperature, no significant change in peel force, no adhesive failure during high temperature baking, and high impact resistance at room temperature.
A second part:
preparing butyl acrylate-nonyl acrylate copolymer, 48 weight parts of butyl acrylate and 6 weight parts of nonyl acrylate, adding 3 weight parts of aziridine, and reacting at 75-80 ℃ for 20-80min to obtain butyl acrylate-nonyl acrylate copolymer B.
Example 5
A high-temperature color-change pressure-sensitive adhesive is prepared by weighing the following raw materials:
butyl acrylate-nonyl acrylate copolymer B120 g;
80g of hydroxyethyl acrylate;
180g of isooctyl acrylate;
60g of lauryl methacrylate;
30g of acrylamide;
120g of acrylic acid;
60g of benzoyl peroxide;
50g of thermochromic microcapsules;
and 420g of ethyl acetate.
The preparation process comprises the following steps: 1) adding butyl acrylate, hydroxyethyl acrylate, isooctyl acrylate, lauryl methacrylate, acrylamide and acrylic acid into a reaction kettle, uniformly stirring, adding a solvent and an initiator, introducing high-purity nitrogen at room temperature, heating to 80-85 ℃, 2) then adding a butyl acrylate-nonyl acrylate copolymer B and a thermochromic microcapsule, heating to 88-95 ℃, keeping the temperature for 1-3h, 3) cooling to room temperature to obtain a high-temperature photochromic pressure-sensitive adhesive solution, and controlling the viscosity of the high-temperature photochromic pressure-sensitive adhesive solution at 3000mpas of 2000 and the solid content at 38-42%; 4) and adding the prepared high-temperature color-changing pressure-sensitive adhesive solution into 1-3% dipentaerythritol hexaacrylate (DPHA), uniformly stirring, defoaming, coating on a bottom release film, drying by an oven at 120 ℃ for 5min and at 150 ℃ for 15min, and covering the top release film to obtain the high-temperature color-changing pressure-sensitive adhesive of the embodiment 5.
Example 6
A high-temperature color-change pressure-sensitive adhesive is prepared by weighing the following raw materials:
butyl acrylate-nonyl acrylate copolymer B160 g;
50g of hydroxyethyl acrylate;
150g of isooctyl acrylate;
100g of lauryl methacrylate;
60g of acrylamide;
80g of acrylic acid;
40g of benzoyl peroxide;
30g of thermochromic microcapsules;
460g of ethyl acetate.
The preparation process comprises the following steps: 1) adding butyl acrylate, hydroxyethyl acrylate, isooctyl acrylate, lauryl methacrylate, acrylamide and acrylic acid into a reaction kettle, uniformly stirring, adding a solvent and an initiator, introducing high-purity nitrogen at room temperature, heating to 80-85 ℃, 2) then adding a butyl acrylate-nonyl acrylate copolymer B and a thermochromic microcapsule, heating to 88-95 ℃, keeping the temperature for 1-3h, 3) cooling to room temperature to obtain a high-temperature photochromic pressure-sensitive adhesive solution, and controlling the viscosity of the high-temperature photochromic pressure-sensitive adhesive solution at 3000mpas of 2000 and the solid content at 38-42%; 4) and adding the prepared high-temperature color-changing pressure-sensitive adhesive solution into 1-3% dipentaerythritol hexaacrylate (DPHA), uniformly stirring, defoaming, coating on a bottom release film, drying by an oven at 120 ℃ for 5min and at 150 ℃ for 15min, and covering the top release film to obtain the high-temperature color-changing pressure-sensitive adhesive of the embodiment 6.
Example 7
A high-temperature color-change pressure-sensitive adhesive is prepared by weighing the following raw materials:
butyl acrylate-nonyl acrylate copolymer B200 g;
70g of hydroxyethyl acrylate;
120g of isooctyl acrylate;
140g of lauryl methacrylate;
80g of acrylamide;
100g of acrylic acid;
50g of benzoyl peroxide;
10g of thermochromic microcapsules;
500g of ethyl acetate.
The preparation process comprises the following steps: 1) adding butyl acrylate, hydroxyethyl acrylate, isooctyl acrylate, lauryl methacrylate, acrylamide and acrylic acid into a reaction kettle, uniformly stirring, adding a solvent and an initiator, introducing high-purity nitrogen at room temperature, heating to 80-85 ℃, 2) then adding a butyl acrylate-nonyl acrylate copolymer B and a thermochromic microcapsule, heating to 88-95 ℃, keeping the temperature for 1-3h, 3) cooling to room temperature to obtain a high-temperature photochromic pressure-sensitive adhesive solution, and controlling the viscosity of the high-temperature photochromic pressure-sensitive adhesive solution at 3000mpas of 2000 and the solid content at 38-42%; 4) and adding the prepared high-temperature color-changing pressure-sensitive adhesive solution into 1-3% dipentaerythritol hexaacrylate (DPHA), uniformly stirring, defoaming, coating on a bottom release film, drying by an oven at 120 ℃ for 5min and at 150 ℃ for 15min, and covering the top release film to obtain the high-temperature color-changing pressure-sensitive adhesive of the embodiment 7.
Example 8
A high-temperature color-change pressure-sensitive adhesive is prepared by weighing the following raw materials:
butyl acrylate-nonyl acrylate copolymer B230 g;
60g of hydroxyethyl acrylate;
80g of isooctyl acrylate;
180g of lauryl methacrylate;
100g of acrylamide;
50g of acrylic acid;
30g of benzoyl peroxide;
20g of thermochromic microcapsules;
520g of ethyl acetate.
The preparation process comprises the following steps: 1) adding butyl acrylate, hydroxyethyl acrylate, isooctyl acrylate, lauryl methacrylate, acrylamide and acrylic acid into a reaction kettle, uniformly stirring, adding a solvent and an initiator, introducing high-purity nitrogen at room temperature, heating to 80-85 ℃, 2) then adding a butyl acrylate-nonyl acrylate copolymer B and a thermochromic microcapsule, heating to 88-95 ℃, keeping the temperature for 1-3h, 3) cooling to room temperature to obtain a high-temperature photochromic pressure-sensitive adhesive solution, and controlling the viscosity of the high-temperature photochromic pressure-sensitive adhesive solution at 3000mpas of 2000 and the solid content at 38-42%; 4) and adding the prepared high-temperature color-changing pressure-sensitive adhesive solution into 1-3% dipentaerythritol hexaacrylate (DPHA), uniformly stirring, defoaming, coating on a bottom release film, drying by an oven at 120 ℃ for 5min and at 150 ℃ for 15min, and covering the top release film to obtain the high-temperature color-changing pressure-sensitive adhesive of the embodiment 8.
The test tests were carried out on the high temperature color-change pressure-sensitive adhesives of 4 of the above examples 5 to 8, and the test results were as follows:
from the above test data of examples 5-8, it can be seen that the high temperature color change pressure sensitive adhesives of examples 5-8 are closer to those of examples 1-4, and have high temperature resistance, no obvious change in peel force, no adhesive failure during high temperature baking, and high impact resistance at normal temperature.
And a third part:
comparative example 1
A high-temperature color-change pressure-sensitive adhesive is prepared by weighing the following raw materials:
butyl acrylate-nonyl acrylate mixture 120 g; (butyl acrylate 96g + nonyl acrylate 24g)
80g of hydroxyethyl acrylate;
180g of isooctyl acrylate;
60g of lauryl methacrylate;
30g of acrylamide;
120g of acrylic acid;
60g of benzoyl peroxide;
50g of thermochromic microcapsules;
and 420g of ethyl acetate.
The preparation process comprises the following steps: 1) adding butyl acrylate, hydroxyethyl acrylate, isooctyl acrylate, lauryl methacrylate, acrylamide and acrylic acid into a reaction kettle, uniformly stirring, adding a solvent and an initiator, introducing high-purity nitrogen at room temperature, heating to 80-85 ℃, 2) then adding a butyl acrylate-nonyl acrylate mixture and a thermochromic microcapsule, heating to 88-95 ℃, keeping the temperature for 1-3h, 3) cooling to room temperature to obtain a high-temperature thermochromic pressure-sensitive adhesive solution, and controlling the viscosity of the high-temperature thermochromic pressure-sensitive adhesive solution at 3000mpas of 2000 and the solid content at 38-42%; 4) and adding the prepared high-temperature color-changing pressure-sensitive adhesive solution into 1-3% dipentaerythritol hexaacrylate (DPHA), uniformly stirring, defoaming, coating on a bottom release film, drying by an oven at 120 ℃ for 5min and at 150 ℃ for 15min, and covering the top release film to obtain the pressure-sensitive adhesive of the comparative example 1.
Comparative example 2
A high-temperature color-change pressure-sensitive adhesive is prepared by weighing the following raw materials:
160g of a butyl acrylate-nonyl acrylate mixture; (butyl acrylate 120g + nonyl acrylate 40g)
50g of hydroxyethyl acrylate;
150g of isooctyl acrylate;
100g of lauryl methacrylate;
60g of acrylamide;
80g of acrylic acid;
40g of benzoyl peroxide;
30g of thermochromic microcapsules;
460g of ethyl acetate.
The preparation process comprises the following steps: 1) adding butyl acrylate, hydroxyethyl acrylate, isooctyl acrylate, lauryl methacrylate, acrylamide and acrylic acid into a reaction kettle, uniformly stirring, adding a solvent and an initiator, introducing high-purity nitrogen at room temperature, heating to 80-85 ℃, 2) then adding a butyl acrylate-nonyl acrylate mixture and a thermochromic microcapsule, heating to 88-95 ℃, keeping the temperature for 1-3h, 3) cooling to room temperature to obtain a high-temperature thermochromic pressure-sensitive adhesive solution, and controlling the viscosity of the high-temperature thermochromic pressure-sensitive adhesive solution at 3000mpas of 2000 and the solid content at 38-42%; 4) and adding the prepared high-temperature color-changing pressure-sensitive adhesive solution into 1-3% dipentaerythritol hexaacrylate (DPHA), uniformly stirring, defoaming, coating on a bottom release film, drying by an oven at 120 ℃ for 5min and at 150 ℃ for 15min, and covering the top release film to obtain the pressure-sensitive adhesive of the comparative example 2.
Comparative example 3
A high-temperature color-change pressure-sensitive adhesive is prepared by weighing the following raw materials:
butyl acrylate-nonyl acrylate mixture 200 g; (butyl acrylate 150g + nonyl acrylate 50g)
70g of hydroxyethyl acrylate;
120g of isooctyl acrylate;
140g of lauryl methacrylate;
80g of acrylamide;
100g of acrylic acid;
50g of benzoyl peroxide;
10g of thermochromic microcapsules;
500g of ethyl acetate.
The preparation process comprises the following steps: 1) adding butyl acrylate, hydroxyethyl acrylate, isooctyl acrylate, lauryl methacrylate, acrylamide and acrylic acid into a reaction kettle, uniformly stirring, adding a solvent and an initiator, introducing high-purity nitrogen at room temperature, heating to 80-85 ℃, 2) then adding a butyl acrylate-nonyl acrylate mixture and a thermochromic microcapsule, heating to 88-95 ℃, keeping the temperature for 1-3h, 3) cooling to room temperature to obtain a high-temperature thermochromic pressure-sensitive adhesive solution, and controlling the viscosity of the high-temperature thermochromic pressure-sensitive adhesive solution at 3000mpas of 2000 and the solid content at 38-42%; 4) and adding the prepared high-temperature color-changing pressure-sensitive adhesive solution into 1-3% dipentaerythritol hexaacrylate (DPHA), uniformly stirring, defoaming, coating on a bottom release film, drying by an oven at 120 ℃ for 5min and at 150 ℃ for 15min, and covering the top release film to obtain the pressure-sensitive adhesive of the comparative example 3.
Comparative example 4
A high-temperature color-change pressure-sensitive adhesive is prepared by weighing the following raw materials:
butyl acrylate-nonyl acrylate mixture 230 g; (butyl acrylate 190g + nonyl acrylate 40g)
60g of hydroxyethyl acrylate;
80g of isooctyl acrylate;
180g of lauryl methacrylate;
100g of acrylamide;
50g of acrylic acid;
30g of benzoyl peroxide;
20g of thermochromic microcapsules;
520g of ethyl acetate.
The preparation process comprises the following steps: 1) adding butyl acrylate, hydroxyethyl acrylate, isooctyl acrylate, lauryl methacrylate, acrylamide and acrylic acid into a reaction kettle, uniformly stirring, adding a solvent and an initiator, introducing high-purity nitrogen at room temperature, heating to 80-85 ℃, 2) then adding a butyl acrylate-nonyl acrylate mixture and a thermochromic microcapsule, heating to 88-95 ℃, keeping the temperature for 1-3h, 3) cooling to room temperature to obtain a high-temperature thermochromic pressure-sensitive adhesive solution, and controlling the viscosity of the high-temperature thermochromic pressure-sensitive adhesive solution at 3000mpas of 2000 and the solid content at 38-42%; 4) and adding the prepared high-temperature color-changing pressure-sensitive adhesive solution into 1-3% dipentaerythritol hexaacrylate (DPHA), uniformly stirring, defoaming, coating on a bottom release film, drying by an oven at 120 ℃ for 5min and at 150 ℃ for 15min, and covering the top release film to obtain the pressure-sensitive adhesive of the comparative example 4.
The pressure-sensitive adhesives of comparative examples 1 to 4 described above were subjected to test tests, and the test results were as follows:
from the above data, it can be seen that the peel force is greater after normal temperature or high temperature treatment, and there is adhesive residue, and the overall pressure sensitive adhesive effect is inferior to examples 1-8. The difference between the butyl acrylate-nonyl acrylate copolymer and the butyl acrylate-nonyl acrylate mixture has a greater effect on the performance of the pressure-sensitive adhesive.
The pressure-sensitive adhesives of the embodiments 1-8 and the comparative examples 1-4 have high-temperature color change performance, and can effectively observe the existing temperature, adjust the temperature in time and improve the processing and detection efficiency of the battery in the processing process of the automatic production line of the lithium battery electrode.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (6)
1. A high-temperature color-changing pressure-sensitive adhesive comprises the following raw materials: 12-23 parts of butyl acrylate-nonyl acrylate copolymer, 5-8 parts of hydroxyethyl acrylate, 8-20 parts of isooctyl acrylate, 6-18 parts of lauryl methacrylate, 3-10 parts of acrylamide, 5-12 parts of acrylic acid, 2-6 parts of initiator, 1-5 parts of thermochromic microcapsule and 42-50 parts of solvent.
2. The thermochromic pressure sensitive adhesive of claim 1, wherein: the preparation method of the butyl acrylate-nonyl acrylate copolymer comprises the following steps: 40-50 parts of butyl acrylate and 5-15 parts of nonyl acrylate, adding 3-6 parts of aziridine, and reacting at 75-80 ℃ for 20-80min to obtain the butyl acrylate-nonyl acrylate copolymer.
3. The thermochromic pressure sensitive adhesive of claim 1, wherein: the initiator is benzoyl peroxide.
4. The thermochromic pressure sensitive adhesive of claim 1, wherein: the solvent is ethyl acetate.
5. The thermochromic pressure sensitive adhesive of claim 1, wherein: the preparation method of the thermochromic microcapsule comprises the following steps: 1-3 parts of crystal violet lactone, 2-6 parts of bisphenol A, 25-32 parts of n-tetradecanol, 2-4 parts of butyl methacrylate, 0.1-0.5 part of tripropylene glycol diacrylate and 0.5-2 parts of 3- (methacryloyloxy) propyl trimethoxy silane treated nano tourmaline are mixed, heated and melted, 2-4 parts of OP-10 and 0.1-2 parts of sodium dodecyl benzene sulfonate are added, and the mixture is stirred and uniformly dispersed at constant temperature to obtain a dispersion liquid; adding 80 parts by weight of water into the dispersion liquid under high-speed stirring, and uniformly stirring to obtain emulsion; adding 1-3 parts by weight of potassium persulfate into the emulsion, heating to 25-32 ℃, slowly adding 0.5-3 parts by weight of ferrous sulfate, reacting for 3 hours, filtering, cleaning, and drying to obtain the thermochromic microcapsule.
6. The thermochromic pressure sensitive adhesive of claim 1, wherein: the preparation method of the high-temperature color-changeable pressure-sensitive adhesive comprises the following steps: 1) weighing butyl acrylate-nonyl acrylate copolymer, butyl acrylate, hydroxyethyl acrylate, isooctyl acrylate, lauryl methacrylate, acrylamide, acrylic acid, an initiator, a thermochromic microcapsule and a solvent; 2) adding butyl acrylate, hydroxyethyl acrylate, isooctyl acrylate, lauryl methacrylate, acrylamide and acrylic acid into a reaction kettle, uniformly stirring, adding a solvent and an initiator, introducing high-purity nitrogen at room temperature, heating to 80-85 ℃, 3) then adding a butyl acrylate-nonyl acrylate copolymer and a thermochromic microcapsule, heating to 88-95 ℃, keeping the temperature for 1-3h, 4) cooling to room temperature to obtain a high-temperature thermochromic pressure-sensitive adhesive solution, and controlling the viscosity of the high-temperature thermochromic pressure-sensitive adhesive solution at 3000mpas of 2000 and the solid content at 38-42%; 5) and adding the prepared high-temperature color-changing pressure-sensitive adhesive solution into 1-3% dipentaerythritol hexaacrylate (DPHA), uniformly stirring, defoaming, coating on a bottom release film, drying by an oven at 120 ℃ for 5min and at 150 ℃ for 15min, and covering the top release film to obtain the high-temperature color-changing pressure-sensitive adhesive.
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| CN110669459A (en) * | 2019-10-31 | 2020-01-10 | 东莞市骏青电子科技有限公司 | High-pressure color-changing pressure-sensitive adhesive, preparation method thereof, adhesive tape and application of high-pressure color-changing pressure-sensitive adhesive |
| CN111604014A (en) * | 2020-05-29 | 2020-09-01 | 福建拓烯新材料科技有限公司 | Preparation method of color-changing microcapsule capable of being applied to textile and color-changing microcapsule |
| CN113717315A (en) * | 2021-09-15 | 2021-11-30 | 江苏晶华新材料科技有限公司 | High-temperature-resistant acrylate pressure-sensitive adhesive and preparation method thereof |
| CN113817416A (en) * | 2021-08-25 | 2021-12-21 | 南京汇鑫光电材料有限公司 | High-reworkability acrylate pressure-sensitive adhesive tape and preparation method thereof |
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- 2021-12-29 CN CN202111641676.5A patent/CN114214007A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108219694A (en) * | 2017-12-21 | 2018-06-29 | 四川东材科技集团股份有限公司 | A kind of lithium battery environment friendly heat resistant terminal adhesive tape and preparation method thereof |
| CN110669459A (en) * | 2019-10-31 | 2020-01-10 | 东莞市骏青电子科技有限公司 | High-pressure color-changing pressure-sensitive adhesive, preparation method thereof, adhesive tape and application of high-pressure color-changing pressure-sensitive adhesive |
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