CN110041860A - A kind of pressure-sensitive adhesive and preparation method thereof with high peeling force - Google Patents
A kind of pressure-sensitive adhesive and preparation method thereof with high peeling force Download PDFInfo
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- CN110041860A CN110041860A CN201910399891.5A CN201910399891A CN110041860A CN 110041860 A CN110041860 A CN 110041860A CN 201910399891 A CN201910399891 A CN 201910399891A CN 110041860 A CN110041860 A CN 110041860A
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- sensitive adhesive
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
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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
- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/10—Esters
- C08F220/12—Esters of monohydric alcohols or phenols
- C08F220/16—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
- C08F220/18—Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
- C08F220/1808—C8-(meth)acrylate, e.g. isooctyl (meth)acrylate or 2-ethylhexyl (meth)acrylate
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- 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 discloses a kind of pressure-sensitive adhesives with high peeling force, are made of the raw material for including following parts by weight: 45~55 parts of Isooctyl acrylate monomer, 4~9 parts of acrylamide, 40~50 parts of butyl acrylate, 7~12 parts of hydroxypropyl acrylate, 3~7 parts of methyl acrylate, the ethyl acetate and 70~90 parts of butanone, 1.3~2.2 parts of azodiisobutyronitrile, 0.6~1 part of lauryl mercaptan, 3~5 parts of toluene di-isocyanate(TDI) that mass ratio is 1:1.The tack of pressure-sensitive adhesive with high peeling force of the invention and sticky good, 180 ° of peeling force height are held, and 180 ° of peeling forces under the conditions of 90 DEG C still maintain higher, are firmly bonded, and plasticizer-resistant performance is good and temperature tolerance is good；Make solvent, small toxicity without using benzene, toluene etc. when the synthesis of pressure-sensitive adhesive, environmental protection has a wide range of application.
Description
Technical field
The present invention relates to field of adhesive technology, and in particular to a kind of pressure-sensitive adhesive and its preparation with high peeling force
Method.
Background technique
Pressure-sensitive adhesive, as the term suggests be exactly to pressure-sensitive adhesive, it be it is a kind of without in solvent, heat or
Other means only need to apply slight finger pressure, can be with the adhesive of adherend good bond.The characteristics of pressure-sensitive adhesive is to glue it
Be easy, take off be not difficult, not damaging of shelling, glue-line will not dry up in a longer period of time, thus pressure-sensitive adhesive is also referred to as adhesive sticker.
Just because of the These characteristics of pressure sensitive adhesive, pressure sensitive adhesive product has very extensive purposes.
Pressure-sensitive acrylate is the pressure sensitive adhesive being most widely used at present, it is acrylate monomer and other ethylene
The copolymer of class monomer.Pressure-sensitive acrylate mainly has solvent pressure-sensitive adhesive and emulsion-type pressure-sensitive.Wherein, solvent type pressure
Quick glue is widely used in many fields, and dosage accounts for 65% or more of entire pressure sensitive adhesive, especially recent two decades
It is very fast to carry out this kind of pressure sensitive adhesive development, and has gradually replaced the status of natural rubber pressure sensitive glue, is widely used in packaging, applies
The numerous areas such as cloth, transport, telecommunications, electric appliance, building materials, machinery, aerospace, light industry, medical treatment, family life.
But used pressure-sensitive adhesive there is problems at present:
1, the peeling force and adhesion strength of pressure-sensitive adhesive are not high enough, and adhesion firmness is inadequate；
2, the plasticizer-resistant performance of pressure-sensitive adhesive and temperature tolerance are poor；
3, make solvent using benzene, toluene etc. when the synthesis of pressure-sensitive adhesive, toxicity is big, not environmentally, limits it and uses model
It encloses.
Based on the above situation, the invention proposes a kind of pressure-sensitive adhesive and preparation method thereof with high peeling force, can
Effectively solve problem above.
Summary of the invention
The purpose of the present invention is to provide a kind of pressure-sensitive adhesive and preparation method thereof with high peeling force.Of the invention
The peeling force and adhesion strength of pressure-sensitive adhesive with high peeling force are high, are firmly bonded；And plasticizer-resistant performance is good and temperature tolerance
It is good；Make solvent, small toxicity without using benzene, toluene etc. when the synthesis of pressure-sensitive adhesive, environmental protection has a wide range of application.
In order to solve the above technical problems, present invention provide the technical scheme that
A kind of pressure-sensitive adhesive with high peeling force is made: Isooctyl acrylate monomer of the raw material for including following parts by weight
45~55 parts, 4~9 parts of acrylamide, 40~50 parts of butyl acrylate, 7~12 parts of hydroxypropyl acrylate, methyl acrylate 3~7
Part, the ethyl acetate and 70~90 parts of butanone, 1.3~2.2 parts of azodiisobutyronitrile, lauryl mercaptan 0.6~1 that mass ratio is 1:1
Part, 3~5 parts of toluene di-isocyanate(TDI).
The tack of pressure-sensitive adhesive with high peeling force of the invention and sticky good, 180 ° of peeling force height are held, and 90
180 ° of peeling forces under the conditions of DEG C still maintain higher, are firmly bonded, and plasticizer-resistant performance is good and temperature tolerance is good；Pressure-sensitive adhesive
Make solvent, small toxicity without using benzene, toluene etc. when the synthesis of agent, environmental protection has a wide range of application.
Preferably, first using Isooctyl acrylate monomer as soft monomer, acrylamide is functional hard monomer, and azodiisobutyronitrile is
The ethyl acetate and butanone that initiator, mass ratio are 1:1 are solvent, lauryl mercaptan is molecular weight regulator, carry out prepolymerization, obtain
To Azogroup-containing acrylamide prepolymer；Using butyl acrylate as soft monomer, hydroxypropyl acrylate is functional hard monomer, azodiisobutyronitrile
For initiator, mass ratio be 1:1 ethyl acetate and butanone is solvent, lauryl mercaptan is molecular weight regulator, carry out prepolymerization,
Obtain hydroxypropyl acrylate prepolymer；Then, above-mentioned Azogroup-containing acrylamide prepolymer and hydroxypropyl acrylate prepolymer are mixed, is added
Methyl acrylate and azodiisobutyronitrile, continue polymerization reaction, obtain pressure-sensitive sol solution (solvent pressure-sensitive adhesive)；Finally,
Hydrogenated rosin resin is added in above-mentioned pressure-sensitive sol solution, is stirred, it is made to be uniformly dispersed；It is cooled to room temperature to get arriving
The pressure-sensitive adhesive with high peeling force；In use, toluene di-isocyanate(TDI) is added to described with high peeling force
Pressure-sensitive adhesive can be used.
Preferably, the pressure-sensitive adhesive with high peeling force further includes the raw material of following parts by weight: hydrogenated rosin tree
25~35 parts of rouge.
Preferably, the toluene di-isocyanate(TDI) is Desmodur L67 and the Desmodur L75 of German Bayer AG
Compound mixture.
It is furthermore preferred that in the compounding mixture of the Desmodur L67 and Desmodur L75 Desmodur L67 and
The mass ratio of Desmodur L75 is 1:1.6~1.85.
The present invention also provides the preparation methods of the pressure-sensitive adhesive with high peeling force described in one kind, including following step
It is rapid:
S1: weigh respectively by weight 45~55 parts of Isooctyl acrylate monomer, 4~9 parts of acrylamide, butyl acrylate 40~
50 parts, 7~12 parts of hydroxypropyl acrylate, 3~7 parts of methyl acrylate, the ethyl acetate and butanone 70~90 that mass ratio is 1:1
Part, 1.3~2.2 parts of azodiisobutyronitrile, 0.6~1 part of lauryl mercaptan, 3~5 parts of toluene di-isocyanate(TDI), hydrogenated rosin resin
25~35 parts；
S2: using Isooctyl acrylate monomer as soft monomer, acrylamide is functional hard monomer, and azodiisobutyronitrile is to cause
The ethyl acetate and butanone that agent, mass ratio are 1:1 are solvent, lauryl mercaptan is molecular weight regulator, carry out polymerization reaction, will be complete
The Isooctyl acrylate monomer and acrylamide in portion, 2/5 azodiisobutyronitrile, half mass ratio be 1:1 ethyl acetate and fourth
Ketone, half lauryl mercaptan mixing after, carry out prepolymerization, obtain Azogroup-containing acrylamide prepolymer；
S3: using butyl acrylate as soft monomer, hydroxypropyl acrylate is functional hard monomer, and azodiisobutyronitrile is to cause
The ethyl acetate and butanone that agent, mass ratio are 1:1 are solvent, lauryl mercaptan is molecular weight regulator, carry out polymerization reaction, will be complete
The butyl acrylate and hydroxypropyl acrylate in portion, 2/5 azodiisobutyronitrile, half mass ratio be 1:1 ethyl acetate and
Butanone, half lauryl mercaptan mixing after, carry out prepolymerization, obtain hydroxypropyl acrylate prepolymer；
S4: above-mentioned Azogroup-containing acrylamide prepolymer and hydroxypropyl acrylate prepolymer are mixed, and methyl acrylate and residue is added
Azodiisobutyronitrile, continue polymerization reaction, obtain pressure-sensitive sol solution；
S5: hydrogenated rosin resin is added in above-mentioned pressure-sensitive sol solution, is stirred, it is made to be uniformly dispersed；It is cooled to
Room temperature is to get the pressure-sensitive adhesive described in high peeling force；
Wherein, point of the step S2 and S3 without sequencing；In use, toluene di-isocyanate(TDI) is added to described with height
It in the pressure-sensitive adhesive of peeling force, is uniformly mixed, that is, can be used.
Preferably, in step S2, when carrying out prepolymerization, temperature control at 81~83 DEG C, prepolymerization time is 20~
30min, pre-polymerization process are protected using N2.
Preferably, in step S3, when carrying out prepolymerization, temperature control at 77~79 DEG C, prepolymerization time is 20~
30min, pre-polymerization process are protected using N2.
Preferably, in step S4, when carrying out polymerization reaction, at 79~80 DEG C, prepolymerization time is 4~6h for temperature control,
Pre-polymerization process is protected using N2.
Preferably, in step S5, hydrogenated rosin resin is added in above-mentioned pressure-sensitive sol solution, is stirred, makes its point
It dissipates uniformly, and adds acetone, adjusting solid content is 40~50%；It is cooled to room temperature to get the pressure described in high peeling force
Sensitive adhesive.
Compared with prior art, the present invention have the following advantages that and the utility model has the advantages that
The tack of pressure-sensitive adhesive with high peeling force of the invention and sticky good, 180 ° of peeling force height are held, and 90
180 ° of peeling forces under the conditions of DEG C still maintain higher, are firmly bonded, and plasticizer-resistant performance is good and temperature tolerance is good；Pressure-sensitive adhesive
Make solvent, small toxicity without using benzene, toluene etc. when the synthesis of agent, environmental protection has a wide range of application.
For the present invention first using Isooctyl acrylate monomer as soft monomer, acrylamide is functional hard monomer, and azodiisobutyronitrile is
The ethyl acetate and butanone that initiator, mass ratio are 1:1 are solvent, lauryl mercaptan is molecular weight regulator, carry out prepolymerization, obtain
To Azogroup-containing acrylamide prepolymer；The short chain Azogroup-containing acrylamide prepolymer obtained in this way, it is neither too hard, nor too soft, it is evenly distributed.With butyl acrylate
For soft monomer, hydroxypropyl acrylate is functional hard monomer, the acetic acid second that azodiisobutyronitrile is initiator, mass ratio is 1:1
Ester and butanone are solvent, lauryl mercaptan is molecular weight regulator, carry out prepolymerization, obtain hydroxypropyl acrylate prepolymer；In this way
Obtained short chain hydroxypropyl acrylate prepolymer, it is neither too hard, nor too soft, it is evenly distributed.Then, by above-mentioned Azogroup-containing acrylamide prepolymer and third
The mixing of olefin(e) acid hydroxypropyl rouge prepolymer, is added methyl acrylate and azodiisobutyronitrile, continues polymerization reaction, obtain pressure sensitive adhesive
Solution；In the pressure sensitive adhesive long-chain polymer obtained in this way, short chain Azogroup-containing acrylamide prepolymer and short chain hydroxypropyl acrylate prepolymer
In block distributed, most of by methyl acrylate and its short chain link, molecular weight is higher, wider distribution, and is in certain gradient
Distribution, enough obtains biggish holding power and cohesive force, is firmly bonded after making its crosslinking curing, has high peeling force, and peeling force
It is balanced with mechanical properties such as holding powers, there is good comprehensive service performance.Finally, hydrogenated rosin resin is added to above-mentioned pressure
It in quick sol solution, is stirred, it is made to be uniformly dispersed；It is cooled to room temperature to get the pressure-sensitive adhesive described in high peeling force
Agent；In use, toluene di-isocyanate(TDI) is added to the pressure-sensitive adhesive with high peeling force, that is, can be used.Hydrogenation pine
The addition of botany bar gum is mainly used for adjusting peeling force, further increases peeling force.
It is pre- that the present invention using Isooctyl acrylate monomer as soft monomer, acrylamide is that short chain acrylamide is made in functional hard monomer
Polymers, butyl acrylate is soft monomer, hydroxypropyl acrylate is that short chain hydroxypropyl acrylate prepolymer is made in functional hard monomer,
With proper amount of methacrylate monomer, continue polymerization reaction, obtain pressure-sensitive sol solution, combines esters of acrylic acid gluing
The characteristic of agent and adhesive for polyurethane makes pressure-sensitive adhesive of the invention have good plasticizer-resistant performance good and high temperature resistant
Property.
Preparation method simple process of the invention, it is easy to operate, it ensure that the present invention has the pressure-sensitive adhesive of high peeling force
The comprehensive performance of agent.
Specific embodiment
It is right combined with specific embodiments below in order to make those skilled in the art more fully understand technical solution of the present invention
The preferred embodiments of the invention are described, but should not be understood as the limitation to this patent.
Test method described in following embodiments or test method are unless otherwise specified conventional method；The reagent
And material is obtained from routine business approach, or prepare in conventional manner unless otherwise specified.
Embodiment 1:
A kind of pressure-sensitive adhesive with high peeling force is made: Isooctyl acrylate monomer of the raw material for including following parts by weight
45~55 parts, 4~9 parts of acrylamide, 40~50 parts of butyl acrylate, 7~12 parts of hydroxypropyl acrylate, methyl acrylate 3~7
Part, the ethyl acetate and 70~90 parts of butanone, 1.3~2.2 parts of azodiisobutyronitrile, lauryl mercaptan 0.6~1 that mass ratio is 1:1
Part, 3~5 parts of toluene di-isocyanate(TDI).
Preferably, first using Isooctyl acrylate monomer as soft monomer, acrylamide is functional hard monomer, and azodiisobutyronitrile is
The ethyl acetate and butanone that initiator, mass ratio are 1:1 are solvent, lauryl mercaptan is molecular weight regulator, carry out prepolymerization, obtain
To Azogroup-containing acrylamide prepolymer；Using butyl acrylate as soft monomer, hydroxypropyl acrylate is functional hard monomer, azodiisobutyronitrile
For initiator, mass ratio be 1:1 ethyl acetate and butanone is solvent, lauryl mercaptan is molecular weight regulator, carry out prepolymerization,
Obtain hydroxypropyl acrylate prepolymer；Then, above-mentioned Azogroup-containing acrylamide prepolymer and hydroxypropyl acrylate prepolymer are mixed, is added
Methyl acrylate and azodiisobutyronitrile, continue polymerization reaction, obtain pressure-sensitive sol solution；Finally, by hydrogenated rosin resin
It is added in above-mentioned pressure-sensitive sol solution, is stirred, it is made to be uniformly dispersed；Being cooled to room temperature has high removing to get to described
The pressure-sensitive adhesive of power；In use, toluene di-isocyanate(TDI) is added to the pressure-sensitive adhesive with high peeling force
It uses.
Preferably, the pressure-sensitive adhesive with high peeling force further includes the raw material of following parts by weight: hydrogenated rosin tree
25~35 parts of rouge.
Preferably, the toluene di-isocyanate(TDI) is Desmodur L67 and the Desmodur L75 of German Bayer AG
Compound mixture.
It is furthermore preferred that in the compounding mixture of the Desmodur L67 and Desmodur L75 Desmodur L67 and
The mass ratio of Desmodur L75 is 1:1.6~1.85.
The present invention also provides the preparation methods of the pressure-sensitive adhesive with high peeling force described in one kind, including following step
It is rapid:
S1: weigh respectively by weight 45~55 parts of Isooctyl acrylate monomer, 4~9 parts of acrylamide, butyl acrylate 40~
50 parts, 7~12 parts of hydroxypropyl acrylate, 3~7 parts of methyl acrylate, the ethyl acetate and butanone 70~90 that mass ratio is 1:1
Part, 1.3~2.2 parts of azodiisobutyronitrile, 0.6~1 part of lauryl mercaptan, 3~5 parts of toluene di-isocyanate(TDI), hydrogenated rosin resin
25~35 parts；
S2: using Isooctyl acrylate monomer as soft monomer, acrylamide is functional hard monomer, and azodiisobutyronitrile is to cause
The ethyl acetate and butanone that agent, mass ratio are 1:1 are solvent, lauryl mercaptan is molecular weight regulator, carry out polymerization reaction, will be complete
The Isooctyl acrylate monomer and acrylamide in portion, 2/5 azodiisobutyronitrile, half mass ratio be 1:1 ethyl acetate and fourth
Ketone, half lauryl mercaptan mixing after, carry out prepolymerization, obtain Azogroup-containing acrylamide prepolymer；
S3: using butyl acrylate as soft monomer, hydroxypropyl acrylate is functional hard monomer, and azodiisobutyronitrile is to cause
The ethyl acetate and butanone that agent, mass ratio are 1:1 are solvent, lauryl mercaptan is molecular weight regulator, carry out polymerization reaction, will be complete
The butyl acrylate and hydroxypropyl acrylate in portion, 2/5 azodiisobutyronitrile, half mass ratio be 1:1 ethyl acetate and
Butanone, half lauryl mercaptan mixing after, carry out prepolymerization, obtain hydroxypropyl acrylate prepolymer；
S4: above-mentioned Azogroup-containing acrylamide prepolymer and hydroxypropyl acrylate prepolymer are mixed, and methyl acrylate and residue is added
Azodiisobutyronitrile, continue polymerization reaction, obtain pressure-sensitive sol solution；
S5: hydrogenated rosin resin is added in above-mentioned pressure-sensitive sol solution, is stirred, it is made to be uniformly dispersed；It is cooled to
Room temperature is to get the pressure-sensitive adhesive described in high peeling force；
Wherein, point of the step S2 and S3 without sequencing；In use, toluene di-isocyanate(TDI) is added to described with height
It in the pressure-sensitive adhesive of peeling force, is uniformly mixed, that is, can be used.
Preferably, in step S2, when carrying out prepolymerization, temperature control at 81~83 DEG C, prepolymerization time is 20~
30min, pre-polymerization process are protected using N2.
Preferably, in step S3, when carrying out prepolymerization, temperature control at 77~79 DEG C, prepolymerization time is 20~
30min, pre-polymerization process are protected using N2.
Preferably, in step S4, when carrying out polymerization reaction, at 79~80 DEG C, prepolymerization time is 4~6h for temperature control,
Pre-polymerization process is protected using N2.
Preferably, in step S5, hydrogenated rosin resin is added in above-mentioned pressure-sensitive sol solution, is stirred, makes its point
It dissipates uniformly, and adds acetone, adjusting solid content is 40~50%；It is cooled to room temperature to get the pressure described in high peeling force
Sensitive adhesive.
Embodiment 2:
A kind of pressure-sensitive adhesive with high peeling force is made: Isooctyl acrylate monomer of the raw material for including following parts by weight
45 parts, 4 parts of acrylamide, 40 parts of butyl acrylate, 7 parts of hydroxypropyl acrylate, 3 parts of methyl acrylate, the second that mass ratio is 1:1
Acetoacetic ester and 70 parts of butanone, 1.3 parts of azodiisobutyronitrile, 0.6 part of lauryl mercaptan, 3 parts of toluene di-isocyanate(TDI).
In the present embodiment, first using Isooctyl acrylate monomer as soft monomer, acrylamide is functional hard monomer, and azo two is different
The ethyl acetate and butanone that butyronitrile is initiator, mass ratio is 1:1 are solvent, lauryl mercaptan is molecular weight regulator, are carried out pre-
Polymerization, obtains Azogroup-containing acrylamide prepolymer；Using butyl acrylate as soft monomer, hydroxypropyl acrylate is functional hard monomer, azo
The ethyl acetate and butanone that bis-isobutyronitrile is initiator, mass ratio is 1:1 are solvent, lauryl mercaptan is molecular weight regulator, into
Row prepolymerization obtains hydroxypropyl acrylate prepolymer；Then, by above-mentioned Azogroup-containing acrylamide prepolymer and hydroxypropyl acrylate prepolymer
Mixing is added methyl acrylate and azodiisobutyronitrile, continues polymerization reaction, obtain pressure-sensitive sol solution；Finally, will hydrogenation
Rosin resin is added in above-mentioned pressure-sensitive sol solution, is stirred, it is made to be uniformly dispersed；It is cooled to room temperature to get the tool is arrived
There is the pressure-sensitive adhesive of high peeling force；In use, toluene di-isocyanate(TDI) is added to the pressure sensitive adhesive with high peeling force
Stick can be used.
In the present embodiment, the pressure-sensitive adhesive with high peeling force further includes the raw material of following parts by weight: hydrogenation
25 parts of rosin resin.
In the present embodiment, the toluene di-isocyanate(TDI) is the Desmodur L67 and Desmodur of German Bayer AG
The compounding mixture of L75.
In the present embodiment, Desmodur L67 in the compounding mixture of the Desmodur L67 and Desmodur L75
Mass ratio with Desmodur L75 is 1:1.6.
In the present embodiment, the preparation method of the pressure-sensitive adhesive with high peeling force, including the following steps:
S1: 45 parts of Isooctyl acrylate monomer, 4 parts of acrylamide, 40 parts of butyl acrylate, acrylic acid are weighed respectively by weight
7 parts of hydroxypropyl rouge, 3 parts of methyl acrylate, the ethyl acetate and 70 parts of butanone, 1.3 parts of azodiisobutyronitrile, ten that mass ratio is 1:1
Two 0.6 part of mercaptan, 3 parts of toluene di-isocyanate(TDI), 25 parts of hydrogenated rosin resin；
S2: using Isooctyl acrylate monomer as soft monomer, acrylamide is functional hard monomer, and azodiisobutyronitrile is to cause
The ethyl acetate and butanone that agent, mass ratio are 1:1 are solvent, lauryl mercaptan is molecular weight regulator, carry out polymerization reaction, will be complete
The Isooctyl acrylate monomer and acrylamide in portion, 2/5 azodiisobutyronitrile, half mass ratio be 1:1 ethyl acetate and fourth
Ketone, half lauryl mercaptan mixing after, carry out prepolymerization, obtain Azogroup-containing acrylamide prepolymer；
S3: using butyl acrylate as soft monomer, hydroxypropyl acrylate is functional hard monomer, and azodiisobutyronitrile is to cause
The ethyl acetate and butanone that agent, mass ratio are 1:1 are solvent, lauryl mercaptan is molecular weight regulator, carry out polymerization reaction, will be complete
The butyl acrylate and hydroxypropyl acrylate in portion, 2/5 azodiisobutyronitrile, half mass ratio be 1:1 ethyl acetate and
Butanone, half lauryl mercaptan mixing after, carry out prepolymerization, obtain hydroxypropyl acrylate prepolymer；
S4: above-mentioned Azogroup-containing acrylamide prepolymer and hydroxypropyl acrylate prepolymer are mixed, and methyl acrylate and residue is added
Azodiisobutyronitrile, continue polymerization reaction, obtain pressure-sensitive sol solution；
S5: hydrogenated rosin resin is added in above-mentioned pressure-sensitive sol solution, is stirred, it is made to be uniformly dispersed；It is cooled to
Room temperature is to get the pressure-sensitive adhesive described in high peeling force；
Wherein, point of the step S2 and S3 without sequencing；In use, toluene di-isocyanate(TDI) is added to described with height
It in the pressure-sensitive adhesive of peeling force, is uniformly mixed, that is, can be used.
In the present embodiment, in step S2, when carrying out prepolymerization, temperature is controlled at 81 DEG C, prepolymerization time 30min,
Pre-polymerization process is protected using N2.
In the present embodiment, in step S3, when carrying out prepolymerization, temperature is controlled at 77 DEG C, prepolymerization time 30min,
Pre-polymerization process is protected using N2.
In the present embodiment, in step S4, when carrying out polymerization reaction, temperature is controlled at 79 DEG C, prepolymerization time 6h, in advance
Polymerization process is protected using N2.
In the present embodiment, in step S5, hydrogenated rosin resin is added in above-mentioned pressure-sensitive sol solution, is stirred,
So that it is uniformly dispersed, and add acetone, adjusting solid content is 40%；It is cooled to room temperature to get having high peeling force described in
Pressure-sensitive adhesive.
Embodiment 3:
A kind of pressure-sensitive adhesive with high peeling force is made: Isooctyl acrylate monomer of the raw material for including following parts by weight
55 parts, 9 parts of acrylamide, 50 parts of butyl acrylate, 12 parts of hydroxypropyl acrylate, 7 parts of methyl acrylate, mass ratio be 1:1
Ethyl acetate and 90 parts of butanone, 2.2 parts of azodiisobutyronitrile, 1 part of lauryl mercaptan, 5 parts of toluene di-isocyanate(TDI).
In the present embodiment, first using Isooctyl acrylate monomer as soft monomer, acrylamide is functional hard monomer, and azo two is different
The ethyl acetate and butanone that butyronitrile is initiator, mass ratio is 1:1 are solvent, lauryl mercaptan is molecular weight regulator, are carried out pre-
Polymerization, obtains Azogroup-containing acrylamide prepolymer；Using butyl acrylate as soft monomer, hydroxypropyl acrylate is functional hard monomer, azo
The ethyl acetate and butanone that bis-isobutyronitrile is initiator, mass ratio is 1:1 are solvent, lauryl mercaptan is molecular weight regulator, into
Row prepolymerization obtains hydroxypropyl acrylate prepolymer；Then, by above-mentioned Azogroup-containing acrylamide prepolymer and hydroxypropyl acrylate prepolymer
Mixing is added methyl acrylate and azodiisobutyronitrile, continues polymerization reaction, obtain pressure-sensitive sol solution；Finally, will hydrogenation
Rosin resin is added in above-mentioned pressure-sensitive sol solution, is stirred, it is made to be uniformly dispersed；It is cooled to room temperature to get the tool is arrived
There is the pressure-sensitive adhesive of high peeling force；In use, toluene di-isocyanate(TDI) is added to the pressure sensitive adhesive with high peeling force
Stick can be used.
In the present embodiment, the pressure-sensitive adhesive with high peeling force further includes the raw material of following parts by weight: hydrogenation
35 parts of rosin resin.
In the present embodiment, the toluene di-isocyanate(TDI) is the Desmodur L67 and Desmodur of German Bayer AG
The compounding mixture of L75.
In the present embodiment, Desmodur L67 in the compounding mixture of the Desmodur L67 and Desmodur L75
Mass ratio with Desmodur L75 is 1:1.85.
In the present embodiment, the preparation method of the pressure-sensitive adhesive with high peeling force, including the following steps:
S1: 55 parts of Isooctyl acrylate monomer, 9 parts of acrylamide, 50 parts of butyl acrylate, acrylic acid are weighed respectively by weight
12 parts of hydroxypropyl rouge, 7 parts of methyl acrylate, the ethyl acetate and 90 parts of butanone, 2.2 parts of azodiisobutyronitrile, ten that mass ratio is 1:1
Two 1 part of mercaptan, 5 parts of toluene di-isocyanate(TDI), 35 parts of hydrogenated rosin resin；
S2: using Isooctyl acrylate monomer as soft monomer, acrylamide is functional hard monomer, and azodiisobutyronitrile is to cause
The ethyl acetate and butanone that agent, mass ratio are 1:1 are solvent, lauryl mercaptan is molecular weight regulator, carry out polymerization reaction, will be complete
The Isooctyl acrylate monomer and acrylamide in portion, 2/5 azodiisobutyronitrile, half mass ratio be 1:1 ethyl acetate and fourth
Ketone, half lauryl mercaptan mixing after, carry out prepolymerization, obtain Azogroup-containing acrylamide prepolymer；
S3: using butyl acrylate as soft monomer, hydroxypropyl acrylate is functional hard monomer, and azodiisobutyronitrile is to cause
The ethyl acetate and butanone that agent, mass ratio are 1:1 are solvent, lauryl mercaptan is molecular weight regulator, carry out polymerization reaction, will be complete
The butyl acrylate and hydroxypropyl acrylate in portion, 2/5 azodiisobutyronitrile, half mass ratio be 1:1 ethyl acetate and
Butanone, half lauryl mercaptan mixing after, carry out prepolymerization, obtain hydroxypropyl acrylate prepolymer；
S4: above-mentioned Azogroup-containing acrylamide prepolymer and hydroxypropyl acrylate prepolymer are mixed, and methyl acrylate and residue is added
Azodiisobutyronitrile, continue polymerization reaction, obtain pressure-sensitive sol solution；
S5: hydrogenated rosin resin is added in above-mentioned pressure-sensitive sol solution, is stirred, it is made to be uniformly dispersed；It is cooled to
Room temperature is to get the pressure-sensitive adhesive described in high peeling force；
Wherein, point of the step S2 and S3 without sequencing；In use, toluene di-isocyanate(TDI) is added to described with height
It in the pressure-sensitive adhesive of peeling force, is uniformly mixed, that is, can be used.
In the present embodiment, in step S2, when carrying out prepolymerization, temperature is controlled at 83 DEG C, prepolymerization time 20min,
Pre-polymerization process is protected using N2.
In the present embodiment, in step S3, when carrying out prepolymerization, temperature is controlled at 79 DEG C, prepolymerization time 20min,
Pre-polymerization process is protected using N2.
In the present embodiment, in step S4, when carrying out polymerization reaction, temperature is controlled at 80 DEG C, prepolymerization time 4h, in advance
Polymerization process is protected using N2.
In the present embodiment, in step S5, hydrogenated rosin resin is added in above-mentioned pressure-sensitive sol solution, is stirred,
So that it is uniformly dispersed, and add acetone, adjusting solid content is 50%；It is cooled to room temperature to get having high peeling force described in
Pressure-sensitive adhesive.
Embodiment 4:
A kind of pressure-sensitive adhesive with high peeling force is made: Isooctyl acrylate monomer of the raw material for including following parts by weight
50 parts, 6.8 parts of acrylamide, 45 parts of butyl acrylate, 9.3 parts of hydroxypropyl acrylate, 5.5 parts of methyl acrylate, mass ratio be
82 parts of ethyl acetate and butanone, 1.8 parts of azodiisobutyronitrile, 0.8 part of lauryl mercaptan, 4.4 parts of the toluene di-isocyanate(TDI) of 1:1.
In the present embodiment, first using Isooctyl acrylate monomer as soft monomer, acrylamide is functional hard monomer, and azo two is different
The ethyl acetate and butanone that butyronitrile is initiator, mass ratio is 1:1 are solvent, lauryl mercaptan is molecular weight regulator, are carried out pre-
Polymerization, obtains Azogroup-containing acrylamide prepolymer；Using butyl acrylate as soft monomer, hydroxypropyl acrylate is functional hard monomer, azo
The ethyl acetate and butanone that bis-isobutyronitrile is initiator, mass ratio is 1:1 are solvent, lauryl mercaptan is molecular weight regulator, into
Row prepolymerization obtains hydroxypropyl acrylate prepolymer；Then, by above-mentioned Azogroup-containing acrylamide prepolymer and hydroxypropyl acrylate prepolymer
Mixing is added methyl acrylate and azodiisobutyronitrile, continues polymerization reaction, obtain pressure-sensitive sol solution；Finally, will hydrogenation
Rosin resin is added in above-mentioned pressure-sensitive sol solution, is stirred, it is made to be uniformly dispersed；It is cooled to room temperature to get the tool is arrived
There is the pressure-sensitive adhesive of high peeling force；In use, toluene di-isocyanate(TDI) is added to the pressure sensitive adhesive with high peeling force
Stick can be used.
In the present embodiment, the pressure-sensitive adhesive with high peeling force further includes the raw material of following parts by weight: hydrogenation
31 parts of rosin resin.
In the present embodiment, the toluene di-isocyanate(TDI) is the Desmodur L67 and Desmodur of German Bayer AG
The compounding mixture of L75.
In the present embodiment, Desmodur L67 in the compounding mixture of the Desmodur L67 and Desmodur L75
Mass ratio with Desmodur L75 is 1:1.72.
In the present embodiment, the preparation method of the pressure-sensitive adhesive with high peeling force, including the following steps:
S1: 50 parts of Isooctyl acrylate monomer, 6.8 parts of acrylamide, 45 parts of butyl acrylate, propylene are weighed respectively by weight
9.3 parts of sour hydroxypropyl rouge, 5.5 parts of methyl acrylate, the ethyl acetate and 82 parts of butanone, azodiisobutyronitrile 1.8 that mass ratio is 1:1
Part, 0.8 part of lauryl mercaptan, 4.4 parts of toluene di-isocyanate(TDI), 31 parts of hydrogenated rosin resin；
S2: using Isooctyl acrylate monomer as soft monomer, acrylamide is functional hard monomer, and azodiisobutyronitrile is to cause
The ethyl acetate and butanone that agent, mass ratio are 1:1 are solvent, lauryl mercaptan is molecular weight regulator, carry out polymerization reaction, will be complete
The Isooctyl acrylate monomer and acrylamide in portion, 2/5 azodiisobutyronitrile, half mass ratio be 1:1 ethyl acetate and fourth
Ketone, half lauryl mercaptan mixing after, carry out prepolymerization, obtain Azogroup-containing acrylamide prepolymer；
S3: using butyl acrylate as soft monomer, hydroxypropyl acrylate is functional hard monomer, and azodiisobutyronitrile is to cause
The ethyl acetate and butanone that agent, mass ratio are 1:1 are solvent, lauryl mercaptan is molecular weight regulator, carry out polymerization reaction, will be complete
The butyl acrylate and hydroxypropyl acrylate in portion, 2/5 azodiisobutyronitrile, half mass ratio be 1:1 ethyl acetate and
Butanone, half lauryl mercaptan mixing after, carry out prepolymerization, obtain hydroxypropyl acrylate prepolymer；
S4: above-mentioned Azogroup-containing acrylamide prepolymer and hydroxypropyl acrylate prepolymer are mixed, and methyl acrylate and residue is added
Azodiisobutyronitrile, continue polymerization reaction, obtain pressure-sensitive sol solution；
S5: hydrogenated rosin resin is added in above-mentioned pressure-sensitive sol solution, is stirred, it is made to be uniformly dispersed；It is cooled to
Room temperature is to get the pressure-sensitive adhesive described in high peeling force；
Wherein, point of the step S2 and S3 without sequencing；In use, toluene di-isocyanate(TDI) is added to described with height
It in the pressure-sensitive adhesive of peeling force, is uniformly mixed, that is, can be used.
In the present embodiment, in step S2, when carrying out prepolymerization, temperature is controlled at 82 DEG C, prepolymerization time 25min,
Pre-polymerization process is protected using N2.
In the present embodiment, in step S3, when carrying out prepolymerization, temperature is controlled at 78 DEG C, prepolymerization time 25min,
Pre-polymerization process is protected using N2.
In the present embodiment, in step S4, when carrying out polymerization reaction, temperature is controlled at 79 DEG C, prepolymerization time 5h, in advance
Polymerization process is protected using N2.
In the present embodiment, in step S5, hydrogenated rosin resin is added in above-mentioned pressure-sensitive sol solution, is stirred,
So that it is uniformly dispersed, and add acetone, adjusting solid content is 46.5%；Being cooled to room temperature has high peeling force to get to described
Pressure-sensitive adhesive.
The pressure-sensitive adhesive and comparative example with high peeling force that the embodiment of the present invention 2 to embodiment 4 is obtained below
It is tested for the property, test result is as shown in table 1:
Wherein, comparative example is the Chinese patent application of Publication No. CN106634793A.
When test, the pressure-sensitive adhesive and comparative example with high peeling force that the embodiment of the present invention 2 to embodiment 4 obtains
Coating thickness be 50um, do backing with 50um aluminium foil and tested.180 ° of peel test forces are carried out under the conditions of 90 DEG C, it will
The sample made is placed in 90 DEG C of insulating box, is clipped with fixture, is directly tested at such a temperature after 20min.
Table 1
As can be seen from the above table, the pressure-sensitive adhesive with high peeling force of the invention has the advantage that
1, it the tack of the pressure-sensitive adhesive with high peeling force of the invention of the invention and holds viscosity and is significantly better than that
Comparative example, cohesive force is strong, is firmly bonded；
2,180 ° of peeling forces of the pressure-sensitive adhesive with high peeling force of the invention of the invention are farsighted much higher than comparison
Example, peel strength is big, excellent in mechanical performance；
3,180 ° of peeling forces under the conditions of 90 DEG C of pressure-sensitive adhesive with high peeling force of the invention of the invention are still
Keep higher, and significantly larger than comparative example, peel strength is big, excellent in mechanical performance, and heat resistance is good.
The above is only the preferred embodiment of the present invention, it is noted that above-mentioned preferred embodiment is not construed as pair
Limitation of the invention, protection scope of the present invention should be defined by the scope defined by the claims..For the art
For those of ordinary skill, without departing from the spirit and scope of the present invention, several improvements and modifications can also be made, these change
It also should be regarded as protection scope of the present invention into retouching.
Claims (10)
1. a kind of pressure-sensitive adhesive with high peeling force, which is characterized in that be made of the raw material for including following parts by weight: propylene
Different 45~55 parts of the monooctyl ester of acid, 4~9 parts of acrylamide, 40~50 parts of butyl acrylate, 7~12 parts of hydroxypropyl acrylate, acrylic acid
3~7 parts of methyl esters, the ethyl acetate and 70~90 parts of butanone, 1.3~2.2 parts of azodiisobutyronitrile, 12 sulphur that mass ratio is 1:1
0.6~1 part of alcohol, 3~5 parts of toluene di-isocyanate(TDI).
2. the pressure-sensitive adhesive according to claim 1 with high peeling force, which is characterized in that first with Isooctyl acrylate monomer
For soft monomer, acrylamide is functional hard monomer, azodiisobutyronitrile is initiator, mass ratio is 1:1 ethyl acetate and
Butanone is solvent, lauryl mercaptan is molecular weight regulator, carries out prepolymerization, obtains Azogroup-containing acrylamide prepolymer；With butyl acrylate
For soft monomer, hydroxypropyl acrylate is functional hard monomer, the acetic acid second that azodiisobutyronitrile is initiator, mass ratio is 1:1
Ester and butanone are solvent, lauryl mercaptan is molecular weight regulator, carry out prepolymerization, obtain hydroxypropyl acrylate prepolymer；Then,
Above-mentioned Azogroup-containing acrylamide prepolymer and hydroxypropyl acrylate prepolymer are mixed, methyl acrylate and azodiisobutyronitrile is added, after
It is continuous to carry out polymerization reaction, obtain pressure-sensitive sol solution；Finally, hydrogenated rosin resin is added in above-mentioned pressure-sensitive sol solution, stir
Mixing, makes it be uniformly dispersed；It is cooled to room temperature to get the pressure-sensitive adhesive described in high peeling force；In use, by toluene
Diisocyanate is added to the pressure-sensitive adhesive with high peeling force, that is, can be used.
3. the pressure-sensitive adhesive according to claim 1 with high peeling force, which is characterized in that described that there is high peeling force
Pressure-sensitive adhesive further include following parts by weight raw material: 25~35 parts of hydrogenated rosin resin.
4. the pressure-sensitive adhesive according to claim 1 with high peeling force, which is characterized in that the toluene diisocynate
Ester is the compounding mixture of Desmodur L67 and the Desmodur L75 of German Bayer AG.
5. the pressure-sensitive adhesive according to claim 4 with high peeling force, which is characterized in that the Desmodur L67
With Desmodur L75 compounding mixture in Desmodur L67 and Desmodur L75 mass ratio be 1:1.6~
1.85。
6. a kind of preparation method of such as pressure-sensitive adhesive described in any one of claim 1 to 5 with high peeling force, feature
It is, including the following steps:
S1: 45~55 parts of Isooctyl acrylate monomer, 4~9 parts of acrylamide, butyl acrylate 40~50 are weighed respectively by weight
70~90 parts of part, the ethyl acetate that 7~12 parts of hydroxypropyl acrylate, 3~7 parts of methyl acrylate, mass ratio are 1:1 and butanone,
1.3~2.2 parts of azodiisobutyronitrile, 0.6~1 part of lauryl mercaptan, 3~5 parts of toluene di-isocyanate(TDI), hydrogenated rosin resin 25~
35 parts；
S2: using Isooctyl acrylate monomer as soft monomer, acrylamide is functional hard monomer, and azodiisobutyronitrile is initiator, matter
The ethyl acetate and butanone is solvent, lauryl mercaptan is molecular weight regulator that amount ratio is 1:1, carry out polymerization reaction, by whole
Isooctyl acrylate monomer and acrylamide, 2/5 azodiisobutyronitrile, half mass ratio be the ethyl acetate and butanone, one of 1:1
After half lauryl mercaptan mixing, prepolymerization is carried out, Azogroup-containing acrylamide prepolymer is obtained；
S3: using butyl acrylate as soft monomer, hydroxypropyl acrylate is functional hard monomer, azodiisobutyronitrile be initiator,
The ethyl acetate and butanone that mass ratio is 1:1 are solvent, lauryl mercaptan is molecular weight regulator, carry out polymerization reaction, will be whole
Butyl acrylate and hydroxypropyl acrylate, 2/5 azodiisobutyronitrile, half mass ratio be 1:1 ethyl acetate and fourth
Ketone, half lauryl mercaptan mixing after, carry out prepolymerization, obtain hydroxypropyl acrylate prepolymer；
S4: above-mentioned Azogroup-containing acrylamide prepolymer and hydroxypropyl acrylate prepolymer are mixed, and methyl acrylate and remaining idol is added
Nitrogen bis-isobutyronitrile, continues polymerization reaction, obtains pressure-sensitive sol solution；
S5: hydrogenated rosin resin is added in above-mentioned pressure-sensitive sol solution, is stirred, it is made to be uniformly dispersed；It is cooled to room temperature,
Obtain the pressure-sensitive adhesive with high peeling force；
Wherein, point of the step S2 and S3 without sequencing；In use, toluene di-isocyanate(TDI) is added to described with high removing
It in the pressure-sensitive adhesive of power, is uniformly mixed, that is, can be used.
7. the preparation method of the pressure-sensitive adhesive according to claim 6 with high peeling force, which is characterized in that step S2
In, when carrying out prepolymerization, at 81~83 DEG C, prepolymerization time is 20~30min for temperature control, and pre-polymerization process is protected using N2
Shield.
8. the preparation method of the pressure-sensitive adhesive according to claim 6 with high peeling force, which is characterized in that step S3
In, when carrying out prepolymerization, at 77~79 DEG C, prepolymerization time is 20~30min for temperature control, and pre-polymerization process is protected using N2
Shield.
9. the preparation method of the pressure-sensitive adhesive according to claim 6 with high peeling force, which is characterized in that step S4
In, when carrying out polymerization reaction, at 79~80 DEG C, prepolymerization time is 4~6h for temperature control, and pre-polymerization process is protected using N2.
10. the preparation method of the pressure-sensitive adhesive according to claim 6 with high peeling force, which is characterized in that step
In S5, hydrogenated rosin resin is added in above-mentioned pressure-sensitive sol solution, is stirred, it is made to be uniformly dispersed, and add acetone, adjusted
Saving solid content is 40~50%；It is cooled to room temperature to get the pressure-sensitive adhesive described in high peeling force.
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| CN112409961A (en) * | 2020-11-16 | 2021-02-26 | 张家港保税区汇英聚福材料科技合伙企业(有限合伙) | High-peeling-force acrylate pressure-sensitive adhesive and preparation method thereof |
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