CN105542687A - Preparation technology of acrylate adhesive and acrylate adhesive product - Google Patents
Preparation technology of acrylate adhesive and acrylate adhesive product Download PDFInfo
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- CN105542687A CN105542687A CN201610109842.XA CN201610109842A CN105542687A CN 105542687 A CN105542687 A CN 105542687A CN 201610109842 A CN201610109842 A CN 201610109842A CN 105542687 A CN105542687 A CN 105542687A
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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
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
- C09J9/02—Electrically-conducting adhesives
-
- 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
- C08F220/1804—C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (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
A preparation technology of an acrylate adhesive comprises the following steps: a, raw materials are taken in a weight ratio; b, part of butyl acrylate, iso-octyl acrylate and ethyl acetate are taken and added to a reactor and stirred; c, part of acrylic acid and 2-hydroxyethyl acrylate are taken and added to the reactor in the step b and stirred; d, part of butyl acrylate, ethyl acetate, acrylic acid and 2-hydroxyethyl acrylate are taken and added to the reactor in the step c and stirred; e, an initiator is taken, divided into 6 parts and dissolved in ethyl acetate respectively, six solutions are added to the reactor in the step d sequentially, and after addition, the mixture is stirred; f, resin is taken and dissolved in ethyl acetate, the mixture after dissolution is added to the reactor in the step e and stirred, and the acrylate adhesive is obtained. According to the preparation technology, a non-toluene solvent is used, environment-friendliness is realized, the technology is optimized, the polymer dispersion is improved, and a down-stream product meets the environmental protection requirements for low VOC (volatile organic compounds) quantity and low total carbon on the premise that the performance is guaranteed.
Description
Technical field
The invention belongs to adhesive area, be specifically related to a kind of acrylic ester adhesive preparation technology, and the acrylic ester adhesive prepared.
Background technology
At present, in the process preparing acrylic ester adhesive, the mixed solvent of usual use toluene solvant or toluene and ethyl acetate, from the angle of technology controlling and process and product performance, toluene, ethyl acetate can promote high molecular dispersiveness, thus performance is more superior, but from the angle of environmental protection, more and more stricter to the requirement of environment at present, toluene is as high boiling point toxic chemical solvent, conflicted gradually, require in high-end acrylic acid adhesive, not re-use toluene as dilution medium, but when using non-toluene kind solvent, traditional preparation technology is difficult to obtain good product performance, need to make improvement to technique.
Summary of the invention
For deficiency of the prior art, an object of the present invention is to provide a kind of acrylic ester adhesive preparation technology be applicable to without toluene solvant, and two of object of the present invention is to provide this technique and prepares acrylic ester adhesive.
An object of the present invention is achieved through the following technical solutions:
A kind of acrylic ester adhesive preparation technology, is characterized in that, comprise the following steps:
A. following raw material is got by weight:
B. get 400 ~ 500 parts of butyl acrylates, 60 ~ 80 parts of Isooctyl acrylate monomers, 500 ~ 600 parts of ethyl acetate join in reactor, stir 1 ~ 2 hour at 60 DEG C ~ 75 DEG C;
C. get 40 ~ 50 parts of vinylformic acid, 4 ~ 5 parts of vinylformic acid-2-hydroxyl ethyl esters join in the reactor in step b, stir 0.5 ~ 1 hour at 60 DEG C ~ 75 DEG C;
D. get 200 ~ 300 parts of butyl acrylates, 100 ~ 120 parts of ethyl acetate, 15 ~ 20 parts of vinylformic acid, 1 ~ 2 part of vinylformic acid-2-hydroxyl ethyl ester join in the reactor in step c, stir 1 ~ 2 hour at 60 DEG C ~ 75 DEG C;
E. get respectively initiator 1.1 ~ 1.9 parts, 0.6 ~ 0.8 part, 0.6 ~ 0.8 part, 0.3 ~ 0.4 part, 0.4 ~ 0.5 part, 4 ~ 5.6 parts, get respectively ethyl acetate 10 parts, 5 parts, 5 parts, 5 parts, 5 parts, 14 parts, got initiator is dissolved in successively in got ethyl acetate, and obtain six parts of solution are joined in the reactor in steps d successively, feeding interval is 20 ~ 40 minutes, after reinforced end, stir 0.5 ~ 2 hour at 70 DEG C ~ 80 DEG C;
F. get 200 ~ 230 parts of resins to be dissolved in 500 ~ 600 parts of ethyl acetate, join in the reactor in step e after dissolving, stir 0.5 ~ 1 hour at 80 DEG C ~ 85 DEG C, obtain acrylic ester adhesive.
In the present invention, do not use toluene as solvent, what avoid environment is unfriendly, simultaneously in order to make the acrylic ester adhesive obtained have good dispersiveness, raw material, initiator gradation is added, the excellent property of obtained product in the present invention.
Further, described initiator is AIBN, and described resin is Gum Rosin.
Two of object of the present invention there is provided a kind of acrylic ester adhesive, and this acrylic ester adhesive is prepared by above preparation technology.
Compared with prior art, the present invention has following beneficial effect: in the preparation technology of acrylic ester adhesive of the present invention, use non-toluene solvant, environmentally friendly, optimize technique, raw material and initiator are added in gradation, improve polymer dispersiveness simultaneously, under the condition of guaranteed performance, derived product is reached, and low VOC measures, the environmental requirement of low total carbon.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment one
A kind of acrylic ester adhesive preparation technology, comprises the following steps:
A. following raw material is got by weight: butyl acrylate 600 parts; Isooctyl acrylate monomer 60 parts; 55 parts, vinylformic acid; Ethyl acetate 1144 parts; Vinylformic acid-2-hydroxyl ethyl ester 5 parts; AIBN7 part; Gum Rosin 200 parts;
B. get 400 parts of butyl acrylates, 60 parts of Isooctyl acrylate monomers, 500 parts of ethyl acetate join in reactor, stir 1 hour at 60 ~ 65 DEG C;
C. get 40 parts of vinylformic acid, 4 parts of vinylformic acid-2-hydroxyl ethyl esters join in the reactor in step b, stir 0.5 hour at 60 ~ 65 DEG C;
D. get 200 parts of butyl acrylates, 100 parts of ethyl acetate, 15 parts of vinylformic acid, 1 part of vinylformic acid-2-hydroxyl ethyl ester join in the reactor in step c, stir 1 hour at 60 ~ 65 DEG C;
E. get respectively AIBN1.1 part, 0.6 part, 0.6 part, 03 part, 0.4 part, 4 parts, get respectively ethyl acetate 10 parts, 5 parts, 5 parts, 5 parts, 5 parts, 14 parts, got AIBN is dissolved in successively in got ethyl acetate, and obtain six parts of solution are joined in the reactor in steps d successively, feeding interval is 20 minutes, after reinforced end, stir 1 hour at 70 ~ 80 DEG C;
F. get 200 parts of Gum Rosins to be dissolved in 500 parts of ethyl acetate, join in the reactor in step e after dissolving, stir 1 hour at 80 DEG C, obtain acrylic ester adhesive.
Embodiment two
A kind of acrylic ester adhesive preparation technology, comprises the following steps:
A. following raw material is got by weight: butyl acrylate 800 parts; Isooctyl acrylate monomer 80 parts; 70 parts, vinylformic acid; Ethyl acetate 1364 parts; Vinylformic acid-2-hydroxyl ethyl ester 7 parts; AIBN10 part; Gum Rosin 230 parts; Conducting powder 1.3 parts;
B. get 500 parts of butyl acrylates, 80 parts of Isooctyl acrylate monomers, 600 parts of ethyl acetate join in reactor, stir 1 hour at 65 ~ 75 DEG C;
C. get 50 parts of vinylformic acid, 5 parts of vinylformic acid-2-hydroxyl ethyl esters join in the reactor in step b, stir 0.5 hour at 65 ~ 75 DEG C;
D. get 300 parts of butyl acrylates, 120 parts of ethyl acetate, 20 parts of vinylformic acid, 2 parts of vinylformic acid-2-hydroxyl ethyl esters join in the reactor in step c, stir 1 hour at 65 ~ 75 DEG C;
E. get respectively AIBN1.9 part, 0.8 part, 0.8 part, 0.4 part, 0.5 part, 5.6 parts, get respectively ethyl acetate 10 parts, 5 parts, 5 parts, 5 parts, 5 parts, 14 parts, got AIBN is dissolved in successively in got ethyl acetate, and obtain six parts of solution are joined in the reactor in steps d successively, feeding interval is 40 minutes, after reinforced end, stir 1 hour at 75 ~ 78 DEG C;
F. get 230 parts of Gum Rosins to be dissolved in 530 parts of ethyl acetate, join after dissolving in the reactor in step e, and add 1.3 parts of conducting powder, stir 1 hour at 80 ~ 81 DEG C, obtain acrylic ester adhesive.
Conducting powder in the present embodiment can be iron powder or Graphite Powder 99, has the function of conduction and anti-electrostatic.
Embodiment three
A kind of acrylic ester adhesive preparation technology, comprises the following steps:
A. following raw material is got by weight: butyl acrylate 750 parts; Isooctyl acrylate monomer 70 parts; 65 parts, vinylformic acid; Ethyl acetate 1294 parts; Vinylformic acid-2-hydroxyl ethyl ester 6 parts; AIBN9 part; Gum Rosin 200 parts;
B. get 450 parts of butyl acrylates, 70 parts of Isooctyl acrylate monomers, 550 parts of ethyl acetate join in reactor, stir 1 hour at 65 ~ 75 DEG C;
C. get 45 parts of vinylformic acid, 4.5 parts of vinylformic acid-2-hydroxyl ethyl esters join in the reactor in step b, stir 0.5 hour at 65 ~ 75 DEG C;
D. get 300 parts of butyl acrylates, 150 parts of ethyl acetate, 20 parts of vinylformic acid, 1.5 parts of vinylformic acid-2-hydroxyl ethyl esters join in the reactor in step c, stir 1 hour at 65 ~ 75 DEG C;
E. get respectively AIBN1.8 part, 0.7 part, 0.8 part, 0.6 part, 0.6 part, 4.5 parts, get respectively ethyl acetate 10 parts, 5 parts, 5 parts, 5 parts, 5 parts, 14 parts, got AIBN is dissolved in successively in got ethyl acetate, and obtain six parts of solution are joined in the reactor in steps d successively, feeding interval is 30 minutes, after reinforced end, stir 1 hour at 75 ~ 78 DEG C;
F. get 220 parts of Gum Rosins to be dissolved in 550 parts of ethyl acetate, join in the reactor in step e after dissolving, stir 1 hour at 80 ~ 82 DEG C, obtain acrylic ester adhesive.
Carry out performance test to the product in the above embodiment of the present invention, and contrast with using the like product of toluene solvant, the results are shown in following table, each VOC content in table is the detected result of derived product (as adhesive tape).
| Currently available products | Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Viscosity (Pas) | 44-46 | 45-48 | 44-49 | 46-49 |
| Solid content (%) | 50-90 | 40-80 | 40-70 | 50-70 |
| Clinging power (N) | 1000-1400 | 1000-1400 | 1000-1400 | 1000-1400 |
| Initial bonding strength (N) | 0-0.7 | 0-0.7 | 0-0.65 | 0-0.7 |
| Confining force (N) | 8-16 | 8-15 | 8-16 | 8-15 |
| VOC (toluene) | ＞100ppm | Nothing | Nothing | Nothing |
| VOC (ethyl acetate) | ＞100ppm | ＜50ppm | ＜50ppm | ＜50ppm |
| VOC (total carbon) | ＞100ppm | ＜100ppm | ＜100ppm | ＜100ppm |
Data as can be seen from above form, in embodiment 1 ~ 3, use product prepared by non-toluene solvant in the present invention, compared with using the product of toluene solvant in prior art, basic indifference in performance, and derived product has eco-friendly performance, without the volatilization of toluene.Meanwhile, due to the method adopting gradation reinforced in preparation method of the present invention, effectively prevent the generation of implode, and the dispersity of product is high, thus makes the VOC of derived product measure (ethyl acetate and total carbon) obviously to reduce.
In addition, in embodiments of the invention 2, be added with conducting powder (can be iron powder or Graphite Powder 99) in the product, under the prerequisite not affecting product performance, the accumulation of static electricity in derived product can be prevented, there are good market outlook.
Protection scope of the present invention includes but not limited to above embodiment, and protection scope of the present invention is as the criterion with claims, and any replacement that those skilled in the art will find apparent that, distortion, improvement made this technology all falls into protection scope of the present invention.
Claims (3)
1. an acrylic ester adhesive preparation technology, is characterized in that, comprises the following steps:
A. following raw material is got by weight:
B. get 400 ~ 500 parts of butyl acrylates, 60 ~ 80 parts of Isooctyl acrylate monomers, 500 ~ 600 parts of ethyl acetate join in reactor, stir 1 ~ 2 hour at 60 DEG C ~ 75 DEG C;
C. get 40 ~ 50 parts of vinylformic acid, 4 ~ 5 parts of vinylformic acid-2-hydroxyl ethyl esters join in the reactor in step b, stir 0.5 ~ 1 hour at 60 DEG C ~ 75 DEG C;
D. get 200 ~ 300 parts of butyl acrylates, 100 ~ 120 parts of ethyl acetate, 15 ~ 20 parts of vinylformic acid, 1 ~ 2 part of vinylformic acid-2-hydroxyl ethyl ester join in the reactor in step c, stir 1 ~ 2 hour at 60 DEG C ~ 75 DEG C;
E. get respectively initiator 1.1 ~ 1.9 parts, 0.6 ~ 0.8 part, 0.6 ~ 0.8 part, 0.3 ~ 0.4 part, 0.4 ~ 0.5 part, 4 ~ 5.6 parts, get respectively ethyl acetate 10 parts, 5 parts, 5 parts, 5 parts, 5 parts, 14 parts, got initiator is dissolved in successively in got ethyl acetate, and obtain six parts of solution are joined in the reactor in steps d successively, feeding interval is 20 ~ 40 minutes, after reinforced end, stir 0.5 ~ 2 hour at 70 DEG C ~ 80 DEG C;
F. get 200 ~ 230 parts of resins to be dissolved in 500 ~ 600 parts of ethyl acetate, join in the reactor in step e after dissolving, stir 0.5 ~ 1 hour at 80 DEG C ~ 85 DEG C, obtain acrylic ester adhesive.
2. a kind of acrylic ester adhesive preparation technology according to claim 1, is characterized in that, described initiator is AIBN, and described resin is Gum Rosin.
3. an acrylic ester adhesive, is characterized in that, this acrylic ester adhesive is prepared by the preparation technology described in any one of claim 1 ~ 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610109842.XA CN105542687B (en) | 2016-02-29 | 2016-02-29 | A kind of acrylate adhesive preparation technology and products thereof |
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|---|---|---|---|
| CN201610109842.XA CN105542687B (en) | 2016-02-29 | 2016-02-29 | A kind of acrylate adhesive preparation technology and products thereof |
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| CN105542687A true CN105542687A (en) | 2016-05-04 |
| CN105542687B CN105542687B (en) | 2017-11-17 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106398603A (en) * | 2016-09-28 | 2017-02-15 | 安佐化学有限公司 | High-adhesiveness acrylate adhesive and process for preparing same |
| CN106398602A (en) * | 2016-09-28 | 2017-02-15 | 安佐化学有限公司 | Anti-static high-viscosity acrylate adhesive and preparation process thereof |
| CN106520031A (en) * | 2016-09-28 | 2017-03-22 | 安佐化学有限公司 | Environment-friendly acrylate adhesive and preparation process thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101649165A (en) * | 2009-08-31 | 2010-02-17 | 广东达美胶粘制品有限公司 | Ultraviolet curing pressure sensitive adhersive for polyethylene protective film and preparation method thereof |
| CN101818033A (en) * | 2010-01-22 | 2010-09-01 | 北京高盟新材料股份有限公司 | Alcohol-soluble composite film adhesive and preparation method thereof |
| CN105315926A (en) * | 2015-03-27 | 2016-02-10 | 西安航天三沃化学有限公司 | High-stripping-resistance acrylate pressure-sensitive adhesive and preparation method thereof |
-
2016
- 2016-02-29 CN CN201610109842.XA patent/CN105542687B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101649165A (en) * | 2009-08-31 | 2010-02-17 | 广东达美胶粘制品有限公司 | Ultraviolet curing pressure sensitive adhersive for polyethylene protective film and preparation method thereof |
| CN101818033A (en) * | 2010-01-22 | 2010-09-01 | 北京高盟新材料股份有限公司 | Alcohol-soluble composite film adhesive and preparation method thereof |
| CN105315926A (en) * | 2015-03-27 | 2016-02-10 | 西安航天三沃化学有限公司 | High-stripping-resistance acrylate pressure-sensitive adhesive and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106398603A (en) * | 2016-09-28 | 2017-02-15 | 安佐化学有限公司 | High-adhesiveness acrylate adhesive and process for preparing same |
| CN106398602A (en) * | 2016-09-28 | 2017-02-15 | 安佐化学有限公司 | Anti-static high-viscosity acrylate adhesive and preparation process thereof |
| CN106520031A (en) * | 2016-09-28 | 2017-03-22 | 安佐化学有限公司 | Environment-friendly acrylate adhesive and preparation process thereof |
| CN106398602B (en) * | 2016-09-28 | 2018-07-24 | 安佐化学有限公司 | A kind of antistatic high-adhesive acrylate adhesive and its preparation process |
| CN106398603B (en) * | 2016-09-28 | 2018-07-24 | 安佐化学有限公司 | A kind of high-adhesive acrylate adhesive and its preparation process |
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| CN105542687B (en) | 2017-11-17 |
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Denomination of invention: A preparation process of acrylate adhesive and its product Effective date of registration: 20211026 Granted publication date: 20171117 Pledgee: Dushangang sub branch of Zhejiang Pinghu Rural Commercial Bank Co., Ltd Pledgor: YASUSA CHEMICAL Co.,Ltd. Registration number: Y2021330001966 |
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