CN106967376A - A kind of solvent-type acrylic ester gum stick and preparation method thereof - Google Patents
A kind of solvent-type acrylic ester gum stick and preparation method thereof Download PDFInfo
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- CN106967376A CN106967376A CN201710182695.3A CN201710182695A CN106967376A CN 106967376 A CN106967376 A CN 106967376A CN 201710182695 A CN201710182695 A CN 201710182695A CN 106967376 A CN106967376 A CN 106967376A
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- Prior art keywords
- solvent
- added
- ethyl acetate
- initiator
- acrylic ester
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Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- 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
- 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
-
- 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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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The present invention relates to field of adhesive technology, a kind of solvent-type acrylic ester gum stick, including following component as mass fraction are specifically disclosed：Isooctyl acrylate monomer 20~40%, acrylic acid 1~3%, hydroxy-ethyl acrylate 1~4%, acrylonitrile 0.5~3%, solvent 50~70%, initiator 0.2~0.5%；The solvent uses ethyl acetate, toluene mixed system, and the initiator uses azodiisobutyronitrile.It is an advantage of the invention that the adhesive has relatively low peeling force, there is good adhesive force to base material, after HTHP on base material not cull.
Description
Technical field
The present invention relates to field of adhesive technology, a kind of solvent-type acrylic ester gum stick and its preparation side are particularly related to
Method.
Background technology
Surface protection film is primarily to prevent from being protected product surface during processing, transport, storage and its use
It is scratched, pollute and corrodes.Surface protection membrane adhesive tape category is numerous, has polyester (PET), polyvinyl chloride according to base material classification
(PVC), the type such as polyethylene (PE), polypropylene (PP) and paper substrate.Other nylon, makrolon, polyimides and other polyenes
The plastic foils such as hydrocarbon may be used to prepare surface protection tape.Surface protection tape is because peeling force is relatively low, easy to use, protection
Effect is widely used well, such as hardware industry, photovoltaic industry, plastic cement industry, printing industry, wires and cables industry, electronics
Industry.
The principal element of influence solvent-type acrylic ester Adhensive performance is the size of polymer molecular weight.Obtain preferably
Pressure-sensitive adhesive performance, it is necessary to improve the molecular weight of polymer.But increase molecular weight, the viscosity of polymer solution can rise.Especially
Its in the course of the polymerization process, viscosity rises that to cause to polymerize the heat answered not easy to lose, so as to cause implode.For surface protection
Adhesive may be subjected to high temperature, the influence of high pressure for a long time in use, by its from by protection surface peel when, quilt
Some culls often occur in protection surface.In order to solve this problem, typically need to reaction system add function monomer, and
Outside cross-linking agent is added into glue using preceding, the peeling force of adhesive is reduced, while there is preferable adhesive force to base material, through too high
After warm high pressure on base material not cull.
The content of the invention
It is an object of the invention to provide a kind of solvent-type acrylic ester gum stick and preparation method thereof, the adhesive have compared with
Low peeling force, has good adhesive force to base material, after HTHP on base material not cull.
To achieve these goals, present invention employs following technical scheme：A kind of solvent-type acrylic ester gum stick
And preparation method thereof, including following component as mass fraction：Isooctyl acrylate monomer 20~40%, acrylic acid 1~3%, third
Olefin(e) acid hydroxyl ethyl ester 1~4%, acrylonitrile 0.5~3%, solvent 50~70%, initiator 0.2~0.5%.
Wherein, the solvent uses ethyl acetate, toluene mixed system.
Wherein, the initiator uses azodiisobutyronitrile.
The method for preparing above-mentioned solvent-type acrylic ester gum stick, comprises the following steps：
1) according to component ratio described above, the ratio is the mass fraction percentage of gross mass, weighs acrylic acid
Different monooctyl ester, hydroxy-ethyl acrylate, acrylic acid, acrylonitrile, portion of ethyl acetate, thing mixed above is stirred and is added to reaction
In device, it is placed in 80 DEG C of water-baths；
2) micro initiator, the mixed liquor of ethyl acetate 1% are added for the first time, and 90 minutes are incubated after question response backflow, then
Micro initiator, the mixed liquor of ethyl acetate 1% are once added, time for adding is 30 minutes, is incubated 60 minutes, last time is mended
Plus the mixed liquor time for adding of remaining initiator, ethyl acetate 3% is 30 minutes, is incubated 2~3 hours；
3) after insulation terminates, toluene, remaining ethyl acetate is added, base rubber is obtained after cooling；
4) curing agent is added in most backward base rubber to be solidified, that is, obtain adhesive.
Further, step 4) described in base rubber and curing agent mass ratio be 100:1.
Further, step 4) in the curing agent added into base rubber be isocyanates, be the isocyanic acid of hexa-methylene two
Ester, the addition product of hexamethylene diisocyanate, XDI, '-diphenylmethane diisocyanate, toluene two
One or more in isocyanates.
The beneficial effects of the present invention are：Solvent-type acrylic ester gum stick proposed by the present invention and preparation method thereof, it is main
If preparing a kind of PET protection film acrylate adhesive, the diaphragm is mainly used in electronic product production process
Protection.
The adhesive has relatively low peeling force, less just viscous, there is certain venting quality, and repetition tears patch and do not fall glue, no
Cull, no ghost has good adhesive force to base material, after HTHP 72h, the still not cull on base material.
Embodiment
Below in conjunction with embodiments of the invention, the technical scheme in the embodiment of the present invention is clearly and completely retouched
State, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based on the present invention
In embodiment, the every other implementation that those of ordinary skill in the art are obtained under the premise of creative work is not made
Example, belongs to the scope of protection of the invention.
A kind of solvent-type acrylic ester gum stick, including following component as mass fraction：Isooctyl acrylate monomer 20~
40%th, acrylic acid 1~3%, hydroxy-ethyl acrylate 1~4%, acrylonitrile 0.5~3%, solvent 50~70%, initiator 0.2~
0.5%.
The solvent uses ethyl acetate, toluene mixed system.The initiator uses azodiisobutyronitrile.
Following four embodiment is enumerated to illustrate its preparation method：
Embodiment one：
First, it is that 29%, hydroxy-ethyl acrylate is that 1.5%, acrylic acid is that 1.5%, acrylonitrile is by Isooctyl acrylate monomer
1.5%th, ethyl acetate is that 46.8%, initiator is that 0.3%, toluene is 19.4% to weigh, and above proportioning is total mass fraction
Percentage；
Then Isooctyl acrylate monomer 29%, hydroxy-ethyl acrylate 1.5%, acrylic acid 1.5%, acrylonitrile 1.5%, acetic acid are taken
Ethyl ester 28%, five kinds of mixtures, which stir, by more than is added in reactor, is placed in 80 DEG C of water-baths, initiation is added for the first time
Agent 0.04%, the mixed liquor of ethyl acetate 1%, are incubated 90 minutes after question response backflow, initiator 0.06%, second are added again
The mixed liquor of acetoacetic ester 1%, time for adding is 30 minutes, is incubated 60 minutes, initiator 0.2%, acetic acid second are added for the last time
The mixed liquor time for adding of ester 3% is 30 minutes, is incubated 2 hours.After insulation terminates, ethyl acetate 13.8%, toluene are added
19.4%, obtain base rubber after cooling.Last to be solidified before use, adding curing agent into base rubber, wherein base rubber is with solidifying
The mass ratio of agent is 100:1.
Embodiment two：
First, it is that 33%, hydroxy-ethyl acrylate is that 2%, acrylic acid is that 1%, acrylonitrile is by Isooctyl acrylate monomer
0.5%th, ethyl acetate is that 46.8%, initiator is that 0.2%, toluene is 16.5% to weigh, and above proportioning is total mass fraction
Percentage；
Then Isooctyl acrylate monomer 33%, hydroxy-ethyl acrylate 2%, acrylic acid 1%, acrylonitrile 0.5%, ethyl acetate are taken
32.4%, five kinds of mixtures, which stir, by more than is added in reactor, is placed in 80 DEG C of water-baths, initiator is added for the first time
For the mixed liquor of 0.03%, ethyl acetate 1%, 90 minutes are incubated after question response backflow, initiator 0.07%, second are added again
The mixed liquor of acetoacetic ester 1%, time for adding is 30 minutes, is incubated 60 minutes, initiator 0.1%, acetic acid second are added for the last time
The mixed liquor time for adding of ester 3% is 30 minutes, is incubated 3 hours.After insulation terminates, ethyl acetate 9.4%, toluene are added
16.5%, obtain base rubber after cooling.Last to be solidified before use, adding curing agent into base rubber, wherein base rubber is with solidifying
The mass ratio of agent is 100:1.
Embodiment three：
First, it is that 36.8%, hydroxy-ethyl acrylate is that 1%, acrylic acid is that 1%, acrylonitrile is by Isooctyl acrylate monomer
2%th, ethyl acetate is that 43.5%, initiator is that 0.4%, toluene is 15.3% to weigh, and above proportioning is total mass fraction hundred
Divide ratio；
Then Isooctyl acrylate monomer 36.8%, hydroxy-ethyl acrylate 1%, acrylic acid 1%, acrylonitrile 2%, acetic acid second are weighed
Ester 34.2%, five kinds of mixtures, which stir, by more than is added in reactor, is placed in 80 DEG C of water-baths, initiation is added for the first time
Agent be 0.02%, the mixed liquor of ethyl acetate 1%, question response backflow after be incubated 90 minutes, add again initiator 0.08%,
The mixed liquor of ethyl acetate 1%, time for adding is 30 minutes, is incubated 60 minutes, initiator 0.3%, acetic acid are added for the last time
The mixed liquor time for adding of ethyl ester 3% is 30 minutes, is incubated 2 hours.After insulation terminates, ethyl acetate 4.3%, toluene are added
15.3%, obtain base rubber after cooling.Last to be solidified before use, adding curing agent into base rubber, wherein base rubber is with solidifying
The mass ratio of agent is 100:1.
Example IV：
First, it is that 25%, hydroxy-ethyl acrylate is that 2.5%, acrylic acid is that 3%, acrylonitrile is by Isooctyl acrylate monomer
3%th, ethyl acetate is that 50.5%, initiator is that 0.5%, toluene is 15.5% to weigh, and above proportioning is total mass fraction hundred
Divide ratio；
Then Isooctyl acrylate monomer 25%, hydroxy-ethyl acrylate 2.5%, acrylic acid 3%, acrylonitrile 3%, acetic acid second are weighed
Ester 34.7%, five kinds of mixtures, which stir, by more than is added in reactor, is placed in 80 DEG C of water-baths, initiation is added for the first time
Agent be 0.08%, the mixed liquor of ethyl acetate 1%, question response backflow after be incubated 90 minutes, add again initiator 0.12%,
The mixed liquor of ethyl acetate 1%, time for adding is 30 minutes, is incubated 60 minutes, initiator 0.3%, acetic acid are added for the last time
The mixed liquor time for adding of ethyl ester 3% is 30 minutes, is incubated 3 hours.After insulation terminates, ethyl acetate 10.8%, toluene are added
15.5%, obtain base rubber after cooling.Last to be solidified before use, adding curing agent into base rubber, wherein base rubber is with solidifying
The mass ratio of agent is 100:1.
Adhesive obtained above is coated with 10 μm on a pet film, after 65 DEG C solidify 24h, the PET film of this gluing pasted
72h is placed under 100 DEG C of baking ovens, 6-10MPa pressure on test black film, and by the composite membrane, throws off and black film is seen after glued membrane
On whether there is cull, as a result do not occur cull, show that the adhesive is resistant to high temperature and high pressure, with preferably not residual
Colloidality energy.
The performance of gained adhesive, specially following table are tested using pertinent instruments：
The acrylate adhesive of preparation is can be seen that from form, viscosity is in the range of 100~200cps, for PET film
There is preferable levelability and low spread for coating.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
God is with principle, and any modification, equivalent substitution and improvements made etc. should be included in the scope of the protection.
Claims (6)
1. a kind of solvent-type acrylic ester gum stick, it is characterised in that including following component as mass fraction：Acrylic acid is different
Monooctyl ester 20~40%, acrylic acid 1~3%, hydroxy-ethyl acrylate 1~4%, acrylonitrile 0.5~3%, solvent 50~70%, initiation
Agent 0.2~0.5%.
2. a kind of solvent-type acrylic ester gum stick according to claim 1, it is characterised in that：The solvent uses acetic acid
Ethyl ester, toluene mixed system.
3. a kind of solvent-type acrylic ester gum stick according to claim 1, it is characterised in that：The initiator uses even
Nitrogen bis-isobutyronitrile.
4. prepare the method for any one of the claims 1 to 3 solvent-type acrylic ester gum stick, it is characterised in that including with
Lower step：
1) according to component ratio described in claim 2, the ratio is the mass fraction percentage of gross mass, weighs acrylic acid
Different monooctyl ester, hydroxy-ethyl acrylate, acrylic acid, acrylonitrile, portion of ethyl acetate, thing mixed above is stirred and is added to reaction
In device, it is placed in 80 DEG C of water-baths；
2) micro initiator, the mixed liquor of ethyl acetate 1% are added for the first time, are incubated 90 minutes after question response backflow, again
Micro initiator, the mixed liquor of ethyl acetate 1% are added, time for adding is 30 minutes, is incubated 60 minutes, adds for the last time surplus
Remaining initiator, the mixed liquor time for adding of ethyl acetate 3% are 30 minutes, are incubated 2~3 hours；
3) after insulation terminates, toluene, remaining ethyl acetate is added, base rubber is obtained after cooling；
4) curing agent is added in most backward base rubber to be solidified, that is, obtain adhesive.
5. a kind of preparation method of solvent-type acrylic ester gum stick according to claim 4, it is characterised in that：Step 4)
Described in base rubber and curing agent mass ratio be 100:1.
6. a kind of preparation method of solvent-type acrylic ester gum stick according to claim 4, it is characterised in that：Step 4)
The middle curing agent added into base rubber is isocyanates, is hexamethylene diisocyanate, hexamethylene diisocyanate
One or more in addition product, XDI, '-diphenylmethane diisocyanate, toluene di-isocyanate(TDI).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710182695.3A CN106967376A (en) | 2017-03-24 | 2017-03-24 | A kind of solvent-type acrylic ester gum stick and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710182695.3A CN106967376A (en) | 2017-03-24 | 2017-03-24 | A kind of solvent-type acrylic ester gum stick and preparation method thereof |
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| CN106967376A true CN106967376A (en) | 2017-07-21 |
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| CN201710182695.3A Pending CN106967376A (en) | 2017-03-24 | 2017-03-24 | A kind of solvent-type acrylic ester gum stick and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108003817A (en) * | 2017-12-12 | 2018-05-08 | 宁波绿田胶粘制品有限公司 | High temperature surely glues acrylate pressure-sensitive adhesive and preparation method thereof |
| CN108753214A (en) * | 2018-06-22 | 2018-11-06 | 西安航天三沃化学有限公司 | A kind of antiultraviolet pressure sensitive adhesive and preparation method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102504732A (en) * | 2011-11-29 | 2012-06-20 | 广东达美新材料有限公司 | Solvent-based reticulated pressure-sensitive adhesive for polyethylene protective film and preparation method thereof |
| CN102559105A (en) * | 2011-12-31 | 2012-07-11 | 浙江星丰科技有限公司 | Preparation method for pressure-sensitive adhesive |
| CN104845564A (en) * | 2014-02-14 | 2015-08-19 | 江苏景宏新材料科技有限公司 | Preparation method of solvent-based polyacrylate pressure-sensitive adhesive for alkaline battery labelling |
-
2017
- 2017-03-24 CN CN201710182695.3A patent/CN106967376A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102504732A (en) * | 2011-11-29 | 2012-06-20 | 广东达美新材料有限公司 | Solvent-based reticulated pressure-sensitive adhesive for polyethylene protective film and preparation method thereof |
| CN102559105A (en) * | 2011-12-31 | 2012-07-11 | 浙江星丰科技有限公司 | Preparation method for pressure-sensitive adhesive |
| CN104845564A (en) * | 2014-02-14 | 2015-08-19 | 江苏景宏新材料科技有限公司 | Preparation method of solvent-based polyacrylate pressure-sensitive adhesive for alkaline battery labelling |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108003817A (en) * | 2017-12-12 | 2018-05-08 | 宁波绿田胶粘制品有限公司 | High temperature surely glues acrylate pressure-sensitive adhesive and preparation method thereof |
| CN108753214A (en) * | 2018-06-22 | 2018-11-06 | 西安航天三沃化学有限公司 | A kind of antiultraviolet pressure sensitive adhesive and preparation method |
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Application publication date: 20170721 |
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