CN104371607A - Acrylate emulsion pressure-sensitive adhesive with high solid content and low viscosity and preparation method thereof - Google Patents
Acrylate emulsion pressure-sensitive adhesive with high solid content and low viscosity and preparation method thereof Download PDFInfo
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Abstract
The invention provides an acrylate emulsion pressure-sensitive adhesive with a high solid content and low viscosity, and a preparation method thereof. The provided polyacrylate emulsion is prepared by synthesizing 2-ethylhexyl acrylate, butyl acrylate, vinyl acetate, methyl methacrylate, acrylic acid, 2-hydroxypropyl acrylate, vinyl acetate, carboxyl-containing functional monomers, and inter-crosslinked polyacrylate monomers through a pre-emulsifying semi-continuous polymerization technology. Compared to the prior, the provided adhesive has the characteristics of high solid content, which is not less than 65%, and low viscosity, which is less than 800 mPas at a temperature of 25 DEG C under a rotation speed of 60 rpm. The gel content of the adhesive is low, and the stability of the adhesive is good. The adhesive basically does not contain any nonyl phenol or contains very little nonyl phenol, is an environment-friendly acrylate emulsion pressure-sensitive adhesive, and can be used as a single-component pressure sensitive adhesive.
Description
Technical field
The invention belongs to pressure-sensitive adhesive, be specifically related to a kind of high-solid-content and low-viscosity acrylate emulsion and preparation method thereof.
Background technology
Emulsion pressure-sensitive is owing to taking water as medium, and rate of drying is slow, particularly large to some Amount of spread pressure sensitive adhesive goods, and dry problem is particularly outstanding, therefore, in emulsion pressure-sensitive application, needs to improve solid content and solves its dry problem.
The utilization ratio that high solid content emulsion pressure sensitive adhesive can improve production unit, the expense reducing transport, store, accelerate glue process in the rate of drying of latex, minimizing and just can reach the thickness required by product.But when the solid content of polymer emulsion is more than 50%, viscosity starts increase with solid content and sharply rise, viscosity increases makes the mixing of polymerization system, heat transfer becomes problem, and therefore, while synthesis of high solid content, viscosity can not be too high, and synthesis difficulty is larger.
Summary of the invention
The object of the present invention is to provide a kind of high-solid-content and low-viscosity acrylate emulsion.
The present invention also aims to the preparation method that above-mentioned high-solid-content and low-viscosity acrylate emulsion is provided.
High-solid-content and low-viscosity acrylate emulsion of the present invention is ethyl acrylate, butyl acrylate, vinyl acetate, methyl methacrylate, vinylformic acid, 2-hydroxypropyl acrylate, vinyl acetate, adopt the polyacrylate dispersion of pre-emulsification semi-continuous polymerzation technique synthesis containing carboxyl function monomer, interior crosslinked many acrylate monomers.
The present invention is polymerized by each component raw material and prepares, and its composition and ratio is counted as follows by weight:
Ethyl acrylate 30 ~ 42
Butyl acrylate 16.2 ~ 30
Butyl methacrylate 1 ~ 6
Methyl methacrylate 0 ~ 4
2-hydroxypropyl acrylate 0.2 ~ 3
Vinyl acetate 2 ~ 6
Containing carboxyl function monomer 0.5 ~ 2.4
Interior crosslinked many acrylate monomers 0.05 ~ 2
Anionic emulsifier A 0.1 ~ 0.25
Reactive emulsifier B 0 ~ 0.05
Ammonium persulphate 0.3 ~ 0.6
Sodium bicarbonate 0.2 ~ 0.6
Deionized water 28 ~ 35.
Of the present invention is vinylformic acid, methacrylic acid or their mixture containing carboxyl function monomer.
Interior crosslinked many acrylate monomers of the present invention are one or more in the many glycol esters of two (methyl) vinylformic acid, TriMethylolPropane(TMP) methacrylic ester.
Interior crosslinked many acrylate monomers of the present invention are one or more in Ethylene glycol dimethacrylate, diethyleneglycol dimethacrylate(DEGDMA), TEGDMA, dimethacrylate TEG ester.
Anionic emulsifier A of the present invention is that Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, sodium sulfo-succinate, preferred sodium sulfo-succinate synthetics, as emulsifying agent EF810, EF800 of Qing Te company not containing the tensio-active agent of nonyl phenol.
Reactive emulsifier B of the present invention itself participates in reaction, as allyloxy Nonyl pheno (10) ether ammonium sulfate containing double bond
(DNS-86), allyloxy Nonyl pheno (10) ether bis phosphoric acid (ANPEO-P).
The concrete steps of the preparation method of high-solid-content and low-viscosity acrylate emulsion stick of the present invention are as follows:
(1) by 53% ionized water, 7/8ths to whole emulsifying agent A, the ammonium persulphate of 4/7ths, the sodium bicarbonate of half and whole ethyl acrylates, butyl acrylate, 2-hydroxypropyl acrylate, vinyl acetate, methyl methacrylate and 1/3rd to add in emulsifying kettle emulsification 30 minutes containing carboxyl function monomer and 2-hydroxypropyl acrylate, obtained pre-emulsion 1;
(2) by the deionized water of the pre-emulsion 1,7% of 90%, 2/3rds containing carboxyl function monomer and 2/3rds 2-hydroxypropyl acrylate, all in crosslinked many acrylate monomers and emulsifying agent B to join in emulsifying kettle emulsification 15 minutes, obtained pre-emulsion 2;
(3) by the deionized water of 40%, remaining ammonium persulphate, sodium bicarbonate and emulsifying agent A add in container, and start stirring, add the pre-emulsion 1 of 10%, be warming up to when temperature rises to 65 DEG C
82 ± 1dEG C, still temperature rise is extremely
86 ± 1 DEG Creact 20 minutes again, then drip pre-emulsion 2, pre-emulsion 2 dropwised in about 2.5 hours, kept still temperature at 84 ± 1 DEG C in dropping process;
(4) dropwise, temperature of reaction is raised to 90 DEG C, insulation reaction 1 hour, is then cooled to 40 DEG C, filters discharging, obtain high-solid-content and low-viscosity acrylate emulsion stick with 60 mesh filter screens.
Compared with prior art, high-solid-content and low-viscosity acrylate emulsion of the present invention has the feature of high solids content (>=65%), low viscosity (< 800mPas, 25 DEG C, rotating speed 60rpm); Gel is few, good stability.
The acrylate emulsion prepared with the present invention does not substantially contain or on a small quantity containing nonyl phenol composition, belongs to environmentally-friendly acrylic ester emulsion pressure-sensitive; Good at the situation stability inferior not adding neutralizing agent, organic amine can be added or ammoniacal liquor is adjusted to pH value 7 ± 1 according to coating needs; The high-solid-content and low-viscosity acrylate emulsion stick obtained with the present invention can as point pressure sensitive adhesive use separately.
Embodiment
Embodiment 1
High-solid-content and low-viscosity acrylate emulsion stick of the present invention is polymerized by each component raw material and prepares in reaction flask, and its composition and ratio is counted as follows by weight:
Ethyl acrylate 30
Butyl acrylate 30
Butyl methacrylate 1.5
Methyl methacrylate 0.5
2-hydroxypropyl acrylate 0.35
Vinyl acetate 1.5
Vinylformic acid 0.2
TEGDMA 0.05
Anionic emulsifier EF810 0.2
Reactive emulsifier DNS-86 0
Ammonium persulphate 0.4
Bicarbonate of ammonia 0.3
Deionized water 35
The preparation method of high-solid-content and low-viscosity acrylate emulsion stick of the present invention, concrete steps are as follows:
(1) by 53% ionized water, 7/8ths emulsifying agent EF810, the ammonium persulphate of 4/7ths, the sodium bicarbonate of half and whole ethyl acrylates, butyl acrylate, 2-hydroxypropyl acrylate, vinyl acetate, methyl methacrylate and 1/3rd vinylformic acid and 2-hydroxypropyl acrylate to add in emulsifying kettle emulsification 30 minutes, obtained pre-emulsion 1;
(2) by the deionized water of 40%, remaining ammonium persulphate, sodium bicarbonate and emulsifying agent EF810 add with stirring, condensation, in the four-hole boiling flask of thermometer and charging opening, and start stirring, when temperature rises to 65 DEG C, add the pre-emulsion 1 of 10%, remaining pre-emulsion 1, whole TEGDMAs, remaining vinylformic acid, 2-hydroxypropyl acrylate and deionized water to join in emulsifying kettle emulsification 15 minutes, obtained pre-emulsion 2;
(3), after pre-emulsion 1 being dropped into reaction flask, be warming up to
82dEG C, still temperature rise is extremely
86dEG C react 20 minutes again, then drip pre-emulsion 2, pre-emulsion 2 dropwised in about 2.5 hours, kept still temperature at 84 ± 1 DEG C in dropping process;
(4) dropwise, temperature of reaction is raised to 90 DEG C, insulation reaction 1 hour, is then cooled to 40 DEG C, filters discharging, obtain high-solid-content and low-viscosity acrylate emulsion stick with 60 mesh filter screens.
The high-solid-content and low-viscosity acrylate emulsion stick solid content that the present invention obtains is 65%, gel fraction 0.055%, and emulsion viscosity is 450mPas(25 DEG C, rotating speed 60rpm).
Embodiment 2
High-solid-content and low-viscosity acrylate emulsion stick of the present invention is polymerized by each component raw material and prepares in reaction flask, and its composition and ratio is counted as follows by weight:
Ethyl acrylate 34
Butyl acrylate 25
Butyl methacrylate 3
Methyl methacrylate 0.5
2-hydroxypropyl acrylate 0.35
Vinyl acetate 1.25
Vinylformic acid 0.15
Ethylene glycol dimethacrylate 0.05
Anionic emulsifier EF800 0.15
Reactive emulsifier DNS-86 0.05
Ammonium persulphate 0.55
Sodium bicarbonate 0.25
Deionized water 35
The preparation method of high-solid-content and low-viscosity acrylate emulsion stick of the present invention, concrete steps are as follows:
(1) by 53% ionized water, 7/8ths emulsifying agent EF800, the ammonium persulphate of 4/7ths, the sodium bicarbonate of half and whole ethyl acrylates, butyl acrylate, 2-hydroxypropyl acrylate, vinyl acetate, methyl methacrylate and 1/3rd vinylformic acid and 2-hydroxypropyl acrylate to add in emulsifying kettle emulsification 30 minutes, obtained pre-emulsion 1;
(2) by the deionized water of 40%, remaining ammonium persulphate, sodium bicarbonate and emulsifying agent EF800 add with stirring, condensation, in the four-hole boiling flask of thermometer and charging opening, and start stirring, when temperature rises to 65 DEG C, add the pre-emulsion 1 of 10%, remaining pre-emulsion 1, whole TEGDMAs, DNS-86, remaining vinylformic acid, 2-hydroxypropyl acrylate and deionized water to join in emulsifying kettle emulsification 15 minutes, obtained pre-emulsion 2;
(3) after pre-emulsion 1 being dropped into reaction flask, be warming up to 82 DEG C, still temperature rise extremely
87 DEG Creact 20 minutes again, then drip pre-emulsion 2, pre-emulsion 2 dropwised in about 2.5 hours, kept still temperature at 84 ± 1 DEG C in dropping process;
(4) dropwise, temperature of reaction is raised to 90 DEG C, insulation reaction 1 hour, is then cooled to 40 DEG C, filters discharging, obtain high-solid-content and low-viscosity acrylate emulsion stick with 60 mesh filter screens.
The high-solid-content and low-viscosity acrylate emulsion stick solid content that the present invention obtains is 65%, and gel fraction 0.045%, emulsion viscosity is 660mP
as(25 DEG C, 60rpm).
Embodiment 3
High-solid-content and low-viscosity acrylate emulsion stick of the present invention is polymerized by each component raw material and prepares in reaction flask, and its composition and ratio is counted as follows by weight:
Ethyl acrylate 42
Butyl acrylate 16.2
Butyl methacrylate 3
2-hydroxypropyl acrylate 0.35
Vinyl acetate 6
Vinylformic acid 2.4
Ethylene glycol dimethacrylate 2
Anionic emulsifier EF810 0.1
Reactive emulsifier ANPEO-P 0.15
Ammonium persulphate 0.55
Sodium bicarbonate 0.25
Deionized water 28
The preparation method of high-solid-content and low-viscosity acrylate emulsion stick of the present invention, concrete steps are as follows:
(1) by 53% ionized water, 7/8ths emulsifying agent EF810, the ammonium persulphate of 4/7ths, the sodium bicarbonate of half and whole ethyl acrylates, butyl acrylate, 2-hydroxypropyl acrylate, vinyl acetate, methyl methacrylate and 1/3rd vinylformic acid and 2-hydroxypropyl acrylate to add in emulsifying kettle emulsification 30 minutes, obtained pre-emulsion 1;
(2) by the deionized water of 40%, remaining ammonium persulphate, sodium bicarbonate and emulsifying agent EF810 add with stirring, condensation, in the four-hole boiling flask of thermometer and charging opening, and start stirring, when temperature rises to 65 DEG C, add the pre-emulsion 1 of 10%, remaining pre-emulsion 1, whole TEGDMAs, ANPEO-P, remaining vinylformic acid, 2-hydroxypropyl acrylate and deionized water to join in emulsifying kettle emulsification 15 minutes, obtained pre-emulsion 2;
(3) drop in reaction flask by pre-emulsion 1, be warming up to 82 DEG C, still temperature rise extremely
87 DEG Creact 20 minutes again, then drip pre-emulsion 2, pre-emulsion 2 dropwised in about 2.5 hours, kept still temperature at 84 ± 1 DEG C in dropping process;
(4) dropwise, temperature of reaction is raised to 90 DEG C, insulation reaction 1 hour, is then cooled to 40 DEG C, filters discharging, obtain high-solid-content and low-viscosity acrylate emulsion stick with 60 mesh filter screens.
The high-solid-content and low-viscosity acrylate emulsion stick solid content that the present invention obtains is 72%, and gel fraction 0.086%, emulsion viscosity is 800mP
as(25 DEG C, 60rpm).
Embodiment 4
High-solid-content and low-viscosity acrylate emulsion stick of the present invention is polymerized by each component raw material and prepares in reaction flask, and its composition and ratio is counted as follows by weight:
Ethyl acrylate 36
Butyl acrylate 20
Butyl methacrylate 6
2-hydroxypropyl acrylate 0.4
Vinylformic acid 2.4
Ethylene glycol dimethacrylate 1
Anionic emulsifier EF810 0.2
Reactive emulsifier DNS-86 0.05
Ammonium persulphate 0.6
Sodium bicarbonate 0.6
Deionized water 32.25
The preparation method of high-solid-content and low-viscosity acrylate emulsion stick of the present invention, concrete steps are as follows:
(1) by 53% ionized water, whole emulsifying agent EF810, the ammonium persulphate of 4/7ths, the sodium bicarbonate of half and whole ethyl acrylates, butyl acrylate, 2-hydroxypropyl acrylate and 1/3rd vinylformic acid and 2-hydroxypropyl acrylate to add in emulsifying kettle emulsification 30 minutes, obtained pre-emulsion 1;
(2) by the deionized water of 40%, remaining ammonium persulphate, sodium bicarbonate add with stirring, condensation, in the four-hole boiling flask of thermometer and charging opening, and start stirring, when temperature rises to 65 DEG C, add the pre-emulsion 1 of 10%, remaining pre-emulsion 1, whole TEGDMAs, DNS-86, remaining vinylformic acid, 2-hydroxypropyl acrylate and deionized water to join in emulsifying kettle emulsification 15 minutes, obtained pre-emulsion 2;
(3) drop in reaction flask by pre-emulsion 1, be warming up to 83 DEG C, still temperature rise extremely
87 DEG Creact 20 minutes again, then drip pre-emulsion 2, pre-emulsion 2 dropwised in about 2.5 hours, kept still temperature at 84 ± 1 DEG C in dropping process;
(4) dropwise, temperature of reaction is raised to 90 DEG C, insulation reaction 1 hour, is then cooled to 40 DEG C, filters discharging, obtain high-solid-content and low-viscosity acrylate emulsion stick with 60 mesh filter screens.
The high-solid-content and low-viscosity acrylate emulsion stick solid content that the present invention obtains is 67%, and gel fraction 0.076%, emulsion viscosity is 720mP
as(25 DEG C, 60rpm).
Claims (9)
1. a high-solid-content and low-viscosity acrylate emulsion stick, is characterized in that its composition and ratio is counted as follows by weight:
Ethyl acrylate 30 ~ 42
Butyl acrylate 16.2 ~ 30
Butyl methacrylate 1 ~ 6
Methyl methacrylate 0 ~ 4
2-hydroxypropyl acrylate 0.2 ~ 3
Vinyl acetate 2 ~ 6
Containing carboxyl function monomer 0.5 ~ 2.4
Interior crosslinked many acrylate monomers 0.05 ~ 2
Anionic emulsifier A 0.1 ~ 0.25
Reactive emulsifier B 0 ~ 0.05
Ammonium persulphate 0.3 ~ 0.6
Sodium bicarbonate 0.2 ~ 0.6
Deionized water 28 ~ 35;
Be polymerized by above each component raw material and prepare.
2. high-solid-content and low-viscosity acrylate emulsion stick according to claims 1, is characterized in that: described is vinylformic acid, methacrylic acid or their mixture containing carboxyl function monomer.
3. high-solid-content and low-viscosity acrylate emulsion stick according to claims 1, is characterized in that: described interior crosslinked many acrylate monomers are one or more in the many glycol esters of two (methyl) vinylformic acid, TriMethylolPropane(TMP) methacrylic ester.
4. high-solid-content and low-viscosity acrylate emulsion stick according to claims 1 or 3, is characterized in that: described interior crosslinked many acrylate monomers are one or more in Ethylene glycol dimethacrylate, diethyleneglycol dimethacrylate(DEGDMA), TEGDMA, dimethacrylate TEG ester.
5. high-solid-content and low-viscosity acrylate emulsion stick according to claims 1, it is characterized in that: described anionic emulsifier A is not containing the tensio-active agent of nonyl phenol, Sodium dodecylbenzene sulfonate, sodium lauryl sulphate, sodium sulfo-succinate, preferred sodium sulfo-succinate synthetics, as emulsifying agent EF810, EF800 of Qing Te company.
6. high-solid-content and low-viscosity acrylate emulsion stick according to claims 1, is characterized in that: described reactive emulsifier B is allyloxy Nonyl pheno (10) ether ammonium sulfate (DNS-86) or allyloxy Nonyl pheno (10) ether bis phosphoric acid (ANPEO-P).
7. a preparation method for the high-solid-content and low-viscosity acrylate emulsion stick described in claims 1, is characterized in that step is as follows:
(1) by 53% ionized water, 7/8ths or whole emulsifying agent A, the ammonium persulphate of 4/7ths, the sodium bicarbonate of half and whole ethyl acrylates, butyl acrylate, 2-hydroxypropyl acrylate, vinyl acetate, butyl methacrylate, 1/3rd the 2-hydroxypropyl acrylate containing carboxyl function monomer and 1/3rd to add in emulsifying kettle emulsification 30 minutes, obtained pre-emulsion 1;
(2) by the deionized water of the pre-emulsion 1,7% of 90%, 2/3rds containing carboxyl function monomer and 2/3rds 2-hydroxypropyl acrylate, all in crosslinked many acrylate monomers to join in emulsifying kettle emulsification 15 minutes, obtained pre-emulsion 2;
(3) by the deionized water of 40%, remaining ammonium persulphate, sodium bicarbonate and emulsifying agent A add in container, and start stirring, add the pre-emulsion 1 of 10%, be warming up to when temperature rises to 65 DEG C
82 ± 1dEG C, still temperature rise is extremely
86 ± 1 DEG Cafter react 20 minutes again, then drip pre-emulsion 2, pre-emulsion 2 dropwised in about 2.5 hours, kept still temperature at 84 ± 1 DEG C in dropping process;
(4) dropwise, temperature of reaction is raised to 90 DEG C, insulation reaction 1 hour, is then cooled to 40 DEG C, obtains high-solid-content and low-viscosity acrylate emulsion stick.
8. the preparation method of the high-solid-content and low-viscosity acrylate emulsion stick according to claims 7, is characterized in that adding methyl methacrylate in step (1).
9. the preparation method of the high-solid-content and low-viscosity acrylate emulsion stick according to claims 7, is characterized in that adding reactive emulsifier B in step (2).
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105504148A (en) * | 2016-02-25 | 2016-04-20 | 广州晶海化工有限公司 | Waterborne pressure-sensitive adhesive and preparation method thereof |
| TWI554526B (en) * | 2015-05-22 | 2016-10-21 | 四維精密材料股份有限公司 | The process for preparing high solid content emulsion pressure sensitive adhesive |
| CN106995676A (en) * | 2017-04-10 | 2017-08-01 | 孙小力 | A kind of zero formaldehyde wood adhesive and preparation method thereof |
| CN108084329A (en) * | 2017-12-01 | 2018-05-29 | 华南协同创新研究院 | A kind of vinegar-acrylic emulsion of high-solid-content and low-viscosity and preparation method thereof |
| CN108285508A (en) * | 2017-01-20 | 2018-07-17 | 湖北航天化学技术研究所 | Protective film high viscous development of Acrylate Emulsion Pressure-Sensitive Adhesive and preparation method and application in using |
| CN108912262A (en) * | 2018-05-28 | 2018-11-30 | 浙江万宝龙胶粘制品有限公司 | A kind of water-borne pressure sensitive adhesive lotion and its synthetic method with double grains gauge structure |
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| CN109929075A (en) * | 2017-12-18 | 2019-06-25 | 万华化学（宁波）有限公司 | The preparation method and polyacrylate microspheric pressure sensitive adhesive of the modified polyacrylic acid ester microsphere suspension liquid of aqueous phase in surface and its application |
| CN112143421A (en) * | 2020-09-01 | 2020-12-29 | 许贵真 | Preparation method of flame-retardant high-solid-content acrylic pressure-sensitive adhesive |
| CN113980170A (en) * | 2021-11-18 | 2022-01-28 | 南京科开新材料有限公司 | Preparation method of high-solid-content low-viscosity acrylate emulsion |
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Cited By (13)
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| TWI554526B (en) * | 2015-05-22 | 2016-10-21 | 四維精密材料股份有限公司 | The process for preparing high solid content emulsion pressure sensitive adhesive |
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| CN105504148A (en) * | 2016-02-25 | 2016-04-20 | 广州晶海化工有限公司 | Waterborne pressure-sensitive adhesive and preparation method thereof |
| CN108285508A (en) * | 2017-01-20 | 2018-07-17 | 湖北航天化学技术研究所 | Protective film high viscous development of Acrylate Emulsion Pressure-Sensitive Adhesive and preparation method and application in using |
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| CN106995676A (en) * | 2017-04-10 | 2017-08-01 | 孙小力 | A kind of zero formaldehyde wood adhesive and preparation method thereof |
| CN108084329A (en) * | 2017-12-01 | 2018-05-29 | 华南协同创新研究院 | A kind of vinegar-acrylic emulsion of high-solid-content and low-viscosity and preparation method thereof |
| CN109929075A (en) * | 2017-12-18 | 2019-06-25 | 万华化学（宁波）有限公司 | The preparation method and polyacrylate microspheric pressure sensitive adhesive of the modified polyacrylic acid ester microsphere suspension liquid of aqueous phase in surface and its application |
| CN109929075B (en) * | 2017-12-18 | 2021-12-14 | 万华化学（宁波）有限公司 | Preparation method of surface-modified polyacrylate microsphere aqueous suspension, polyacrylate microsphere pressure-sensitive adhesive and application thereof |
| CN108912262A (en) * | 2018-05-28 | 2018-11-30 | 浙江万宝龙胶粘制品有限公司 | A kind of water-borne pressure sensitive adhesive lotion and its synthetic method with double grains gauge structure |
| CN109837046A (en) * | 2019-02-28 | 2019-06-04 | 广东星宇耐力新材料股份有限公司 | A kind of compound aqueous adhesive and preparation method thereof of plastic film dry type |
| CN112143421A (en) * | 2020-09-01 | 2020-12-29 | 许贵真 | Preparation method of flame-retardant high-solid-content acrylic pressure-sensitive adhesive |
| CN113980170A (en) * | 2021-11-18 | 2022-01-28 | 南京科开新材料有限公司 | Preparation method of high-solid-content low-viscosity acrylate emulsion |
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