CN104371607B - High-solid-content and low-viscosity acrylate emulsion stick and preparation method - Google Patents
High-solid-content and low-viscosity acrylate emulsion stick and preparation method Download PDFInfo
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Abstract
The present invention provides a kind of high-solid-content and low-viscosity acrylate emulsion stick and preparation method thereof；For acrylic acid 2 Octyl Nitrite, butyl acrylate, vinylacetate, methyl methacrylate, acrylic acid, acrylic acid 2 hydroxypropyl acrylate, vinylacetate, containing carboxyl function monomer, the many acrylate monomers of interior crosslinking use pre-emulsification semi-continuous polymerization technique synthesis polyacrylate dispersion.Compared with prior art, the present invention has high solids content (>=65%), the feature of low viscosity (＜ 800mPas, 25 DEG C, rotating speed 60rpm).Gel is few, good stability；It is substantially free of or contains on a small quantity nonyl phenol composition, belong to environmentally-friendly acrylic ester emulsion pressure-sensitive；Can use as an individually point 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.
Background technology
Emulsion pressure-sensitive is due to water as medium, and rate of drying is slow, particularly big to some glue-spreads pressure sensitive adhesive goods,
It is dried particularly problematic, therefore, in emulsion pressure-sensitive is applied, needs to improve solid content to solve its dry problem.
High solid content emulsion pressure sensitive adhesive can improve the utilization rate of production equipment, reduce transport, the expense stored, and accelerates latex
Rate of drying, glue process just can reach the thickness required by product in minimizing.But the solid content of polymer emulsion is more than 50%
Time, viscosity starts to increase with solid content and steeply rise, and viscosity increases makes the mixing of polymerization system, heat transfer become problem, therefore,
While synthesis of high solid content, viscosity can not be the highest, and synthesis difficulty is bigger.
Summary of the invention
It is an object of the invention to provide a kind of high-solid-content and low-viscosity acrylate emulsion.
The present invention also aims to provide the preparation method of above-mentioned high-solid-content and low-viscosity acrylate emulsion.
The high-solid-content and low-viscosity acrylate emulsion of the present invention is acrylic acid-2-ethyl caproite, acrylic acid fourth
Ester, vinylacetate, methyl methacrylate, acrylic acid, 2-hydroxypropyl acrylate, vinylacetate, containing carboxyl function list
Body, the many acrylate monomers of interior crosslinking use the polyacrylate dispersion of pre-emulsification semi-continuous polymerization technique synthesis.
The present invention is polymerized by each component raw material and prepares, and its composition and ratio is counted as follows by weight:
Acrylic acid-2-ethyl caproite 30～42
Butyl acrylate 16.2 ~ 30
Butyl methacrylate 1～6
Methyl methacrylate 0～4
2-hydroxypropyl acrylate 0.2～3
Vinylacetate 2～6
Containing carboxyl function monomer 0.5～2.4
The many acrylate monomers of interior crosslinking 0.05 ~ 2
Anionic emulsifier A 0.1～0.25
Reactive emulsifier B 0～0.05
Ammonium persulfate 0.3～0.6
Sodium acid carbonate 0.2～0.6
Deionized water 28 ~ 35.
The monomer containing carboxyl function of the present invention is acrylic acid, methacrylic acid or their mixture.
The many acrylate monomers of interior crosslinking of the present invention are two (methyl) many glycol esters of acrylic acid, trimethylolpropane
One or more in methacrylate.
The many acrylate monomers of interior crosslinking of the present invention are GDMA, dimethacrylate diethyl
One or more in diol ester, TEGDMA, dimethacrylate TEG ester.
Anionic emulsifier A of the present invention is the surfactant without nonyl phenol, neopelex, ten
Sodium dialkyl sulfate, sodium sulfo-succinate, preferably sodium sulfo-succinate synthetic, as Qing Te company emulsifying agent EF810,
EF800。
Reactive emulsifier B of the present invention itself participates in reaction containing double bond, such as allyloxy Nonyl pheno
(10) ether ammonium sulfate (DNS-86), allyloxy Nonyl pheno (10) ether bis phosphoric acid (ANPEO-P).
Specifically comprising the following steps that of the preparation method of the high-solid-content and low-viscosity acrylate emulsion stick of the present invention
(1) by 53% ionized water, 7/8ths to whole emulsifying agent A, the ammonium persulfate of 4/7ths, the bicarbonate of half
Sodium and whole acrylic acid-2-ethyl caproites, butyl acrylate, 2-hydroxypropyl acrylate, vinylacetate, methacrylic acid
Methyl esters and 1/3rd add in emulsifying kettle containing carboxyl function monomer and 2-hydroxypropyl acrylate and emulsify 30 minutes, prepare pre-
Emulsion 1；
(2) by 90% the deionized water of pre-emulsion 1,7%, 2/3rds containing carboxyl function monomer and 2/3rds
2-hydroxypropyl acrylate, all in cross-link many acrylate monomers and emulsifying agent B joins in emulsifying kettle and emulsifies 15 minutes,
Prepare pre-emulsion 2；
(3) by 40% deionized water, remaining ammonium persulfate, sodium acid carbonate and emulsifying agent A add in container, and start
Stirring, adds the pre-emulsion 1 of 10% when temperature rises to 65 DEG C, is warming up to 82 ± 1 DEG C, and still temperature rise to 86 ± 1 DEG C is reacted again
20 minutes, then dropping pre-emulsion 2, pre-emulsion 2 dripped complete in about 2.5 hours, kept still temperature to exist during dropping
84±1℃；
(4) drip complete, reaction temperature is raised to 90 DEG C, insulation reaction 1 hour, then it is cooled to 40 DEG C, with 60 mesh filters
Net filtration discharging, obtains high-solid-content and low-viscosity acrylate emulsion stick.
Compared with prior art, high-solid-content and low-viscosity acrylate emulsion of the present invention have high solids content (>=
65%), the feature of low viscosity (＜ 800mPas, 25 DEG C, rotating speed 60rpm)；Gel is few, good stability.
The acrylate emulsion prepared by the present invention is substantially free of or contains on a small quantity nonyl phenol composition, belongs to environmental protection
Type acrylate emulsion；Good stability in the case of not adding nertralizer, can add organic amine according to coating needs
Or ammoniacal liquor adjusts to pH value 7 ± 1；The high-solid-content and low-viscosity acrylate emulsion stick prepared by the present invention is permissible
Use as an individually point pressure sensitive adhesive.
Detailed description of the invention
Embodiment 1
The high-solid-content and low-viscosity acrylate emulsion stick of the present invention is gathered in reaction bulb by each component raw material
Closing and prepare, its composition and ratio is counted as follows by weight:
Acrylic acid-2-ethyl caproite 30
Butyl acrylate 30
Butyl methacrylate 1.5
Methyl methacrylate 0.5
2-hydroxypropyl acrylate 0.35
Vinylacetate 1.5
Acrylic acid 0.2
TEGDMA 0.05
Anionic emulsifier EF810 0.2
Reactive emulsifier DNS-86 0
Ammonium persulfate 0.4
Ammonium hydrogen carbonate 0.3
Deionized water 35
The preparation method of the high-solid-content and low-viscosity acrylate emulsion stick of the present invention, specifically comprises the following steps that
(1) by 53% ionized water, the emulsifying agent EF810 of 7/8ths, the ammonium persulfate of 4/7ths, the bicarbonate of half
Sodium and whole acrylic acid-2-ethyl caproites, butyl acrylate, 2-hydroxypropyl acrylate, vinylacetate, methacrylic acid
Methyl esters and the acrylic acid of 1/3rd and 2-hydroxypropyl acrylate add emulsification 30 minutes in emulsifying kettle, prepare pre-emulsion 1；
(2) by 40% deionized water, remaining ammonium persulfate, sodium acid carbonate and emulsifying agent EF810 add with stirring,
Condensation, in the four-hole boiling flask of thermometer and charge door, and starts stirring, adds the pre-emulsion of 10% when temperature rises to 65 DEG C
1, remaining pre-emulsion 1, whole TEGDMAs, remaining acrylic acid, 2-hydroxypropyl acrylate and
Deionized water joins in emulsifying kettle and emulsifies 15 minutes, prepares pre-emulsion 2；
(3) after pre-emulsion 1 being put into reaction bulb, being warming up to 82 DEG C, still temperature rise to 86 DEG C is reacted 20 minutes again, then drips
Adding pre-emulsion 2, pre-emulsion 2 dripped complete in about 2.5 hours, kept still temperature at 84 ± 1 DEG C during dropping；
(4) drip complete, reaction temperature is raised to 90 DEG C, insulation reaction 1 hour, then it is cooled to 40 DEG C, with 60 mesh filters
Net filtration discharging, obtains high-solid-content and low-viscosity acrylate emulsion stick.
The high-solid-content and low-viscosity acrylate emulsion stick solid content that the present invention prepares is 65%, gel fraction
0.055%, emulsion viscosity is 450mPas(25 DEG C, rotating speed 60rpm).
Embodiment 2
The high-solid-content and low-viscosity acrylate emulsion stick of the present invention is gathered in reaction bulb by each component raw material
Closing and prepare, its composition and ratio is counted as follows by weight:
Acrylic acid-2-ethyl caproite 34
Butyl acrylate 25
Butyl methacrylate 3
Methyl methacrylate 0.5
2-hydroxypropyl acrylate 0.35
Vinylacetate 1.25
Acrylic acid 0.15
GDMA 0.05
Anionic emulsifier EF800 0.15
Reactive emulsifier DNS-86 0.05
Ammonium persulfate 0.55
Sodium acid carbonate 0.25
Deionized water 35
The preparation method of the high-solid-content and low-viscosity acrylate emulsion stick of the present invention, specifically comprises the following steps that
(1) by 53% ionized water, the emulsifying agent EF800 of 7/8ths, the ammonium persulfate of 4/7ths, the bicarbonate of half
Sodium and whole acrylic acid-2-ethyl caproites, butyl acrylate, 2-hydroxypropyl acrylate, vinylacetate, methacrylic acid
Methyl esters and the acrylic acid of 1/3rd and 2-hydroxypropyl acrylate add emulsification 30 minutes in emulsifying kettle, prepare pre-emulsion 1；
(2) by 40% deionized water, remaining ammonium persulfate, sodium acid carbonate and emulsifying agent EF800 add with stirring,
Condensation, in the four-hole boiling flask of thermometer and charge door, and starts stirring, adds the pre-emulsion of 10% when temperature rises to 65 DEG C
1, remaining pre-emulsion 1, whole TEGDMAs, DNS-86, remaining acrylic acid, acrylic acid-2-
Hydroxypropyl acrylate and deionized water join in emulsifying kettle and emulsify 15 minutes, prepare pre-emulsion 2；
(3) after pre-emulsion 1 being put into reaction bulb, being warming up to 82 DEG C, still temperature rise to 87 DEG C is reacted 20 minutes again, then drips
Adding pre-emulsion 2, pre-emulsion 2 dripped complete in about 2.5 hours, kept still temperature at 84 ± 1 DEG C during dropping；
(4) drip complete, reaction temperature is raised to 90 DEG C, insulation reaction 1 hour, then it is cooled to 40 DEG C, with 60 mesh filters
Net filtration discharging, obtains high-solid-content and low-viscosity acrylate emulsion stick.
The high-solid-content and low-viscosity acrylate emulsion stick solid content that the present invention prepares is 65%, gel fraction
0.045%, emulsion viscosity is 660mPas(25 DEG C, 60rpm).
Embodiment 3
The high-solid-content and low-viscosity acrylate emulsion stick of the present invention is gathered in reaction bulb by each component raw material
Closing and prepare, its composition and ratio is counted as follows by weight:
Acrylic acid-2-ethyl caproite 42
Butyl acrylate 16.2
Butyl methacrylate 3
2-hydroxypropyl acrylate 0.35
Vinylacetate 6
Acrylic acid 2.4
GDMA 2
Anionic emulsifier EF810 0.1
Reactive emulsifier ANPEO-P 0.15
Ammonium persulfate 0.55
Sodium acid carbonate 0.25
Deionized water 28
The preparation method of the high-solid-content and low-viscosity acrylate emulsion stick of the present invention, specifically comprises the following steps that
(1) by 53% ionized water, the emulsifying agent EF810 of 7/8ths, the ammonium persulfate of 4/7ths, the bicarbonate of half
Sodium and whole acrylic acid-2-ethyl caproites, butyl acrylate, 2-hydroxypropyl acrylate, vinylacetate, methacrylic acid
Methyl esters and the acrylic acid of 1/3rd and 2-hydroxypropyl acrylate add emulsification 30 minutes in emulsifying kettle, prepare pre-emulsion 1；
(2) by 40% deionized water, remaining ammonium persulfate, sodium acid carbonate and emulsifying agent EF810 add with stirring,
Condensation, in the four-hole boiling flask of thermometer and charge door, and starts stirring, adds the pre-emulsion of 10% when temperature rises to 65 DEG C
1, remaining pre-emulsion 1, whole TEGDMAs, ANPEO-P, remaining acrylic acid, acrylic acid-2-
Hydroxypropyl acrylate and deionized water join in emulsifying kettle and emulsify 15 minutes, prepare pre-emulsion 2；
(3) putting in reaction bulb by pre-emulsion 1, be warming up to 82 DEG C, still temperature rise to 87 DEG C is reacted 20 minutes again, then drips
Adding pre-emulsion 2, pre-emulsion 2 dripped complete in about 2.5 hours, kept still temperature at 84 ± 1 DEG C during dropping；
(4) drip complete, reaction temperature is raised to 90 DEG C, insulation reaction 1 hour, then it is cooled to 40 DEG C, with 60 mesh filters
Net filtration discharging, obtains high-solid-content and low-viscosity acrylate emulsion stick.
The high-solid-content and low-viscosity acrylate emulsion stick solid content that the present invention prepares is 72%, gel fraction
0.086%, emulsion viscosity is 800mPas(25 DEG C, 60rpm).
Embodiment 4
The high-solid-content and low-viscosity acrylate emulsion stick of the present invention is gathered in reaction bulb by each component raw material
Closing and prepare, its composition and ratio is counted as follows by weight:
Acrylic acid-2-ethyl caproite 36
Butyl acrylate 20
Butyl methacrylate 6
2-hydroxypropyl acrylate 0.4
Acrylic acid 2.4
GDMA 1
Anionic emulsifier EF810 0.2
Reactive emulsifier DNS-86 0.05
Ammonium persulfate 0.6
Sodium acid carbonate 0.6
Deionized water 32.25
The preparation method of the high-solid-content and low-viscosity acrylate emulsion stick of the present invention, specifically comprises the following steps that
(1) by 53% ionized water, whole emulsifying agent EF810, the ammonium persulfate of 4/7ths, the sodium acid carbonate of half and
The acrylic acid of whole acrylic acid-2-ethyl caproite, butyl acrylate, 2-hydroxypropyl acrylate and 1/3rd and acrylic acid-
2-hydroxypropyl acrylate adds emulsification 30 minutes in emulsifying kettle, prepares pre-emulsion 1；
(2) by 40% deionized water, remaining ammonium persulfate, sodium acid carbonate add with stirring, condensation, thermometer and
In the four-hole boiling flask of charge door, and start stirring, when temperature rises to 65 DEG C, add the pre-emulsion 1 of 10%, remaining pre-breast
Change liquid 1, whole TEGDMAs, DNS-86, remaining acrylic acid, 2-hydroxypropyl acrylate and go from
Sub-water joins in emulsifying kettle and emulsifies 15 minutes, prepares pre-emulsion 2；
(3) putting in reaction bulb by pre-emulsion 1, be warming up to 83 DEG C, still temperature rise to 87 DEG C is reacted 20 minutes again, then drips
Adding pre-emulsion 2, pre-emulsion 2 dripped complete in about 2.5 hours, kept still temperature at 84 ± 1 DEG C during dropping；
(4) drip complete, reaction temperature is raised to 90 DEG C, insulation reaction 1 hour, then it is cooled to 40 DEG C, with 60 mesh filters
Net filtration discharging, obtains high-solid-content and low-viscosity acrylate emulsion stick.
The high-solid-content and low-viscosity acrylate emulsion stick solid content that the present invention prepares is 67%, gel fraction
0.076%, emulsion viscosity is 720mPas(25 DEG C, 60rpm).
Claims (7)
1. the preparation method of a high-solid-content and low-viscosity acrylate emulsion stick,
Its composition and ratio is counted as follows by weight:
Acrylic acid-2-ethyl caproite 30～42
Butyl acrylate 16.2 ~ 30
Butyl methacrylate 1～6
Methyl methacrylate 0～4
2-hydroxypropyl acrylate 0.2～3
Vinylacetate 2～6
Containing carboxyl function monomer 0.5～2.4
The many acrylate monomers of interior crosslinking 0.05 ~ 2
Anionic emulsifier A 0.1～0.25
Reactive emulsifier B 0～0.05
Ammonium persulfate 0.3～0.6
Sodium acid carbonate 0.2～0.6
Deionized water 28 ~ 35；
Prepared by the polymerization of above each component raw material；Step is as follows:
(1) by 53% deionized water, the emulsifying agent A of 7/8ths or whole, the ammonium persulfate of 4/7ths, the bicarbonate of half
Sodium and whole acrylic acid-2-ethyl caproites, butyl acrylate, vinylacetate, butyl methacrylate, 1/3rd contain
Carboxyl function monomer and 1/3rd 2-hydroxypropyl acrylate add in emulsifying kettle and emulsify 30 minutes, prepare pre-emulsion 1；
(2) by 90% the deionized water of pre-emulsion 1,7%, 2/3rds containing carboxyl function monomer and the third of 2/3rds
Olefin(e) acid-2-hydroxypropyl acrylate, the many acrylate monomers of interior crosslinking join in emulsifying kettle and emulsify 15 minutes, prepare pre-emulsion 2；
(3) by 40% deionized water, remaining ammonium persulfate, sodium acid carbonate and emulsifying agent A add in container, and start and stir
Mix, when temperature rises to 65 DEG C, add the pre-emulsion 1 of 10%, be warming up to 82 ± 1 DEG C, react again after still temperature rise to 86 ± 1 DEG C
20 minutes, then dropping pre-emulsion 2, pre-emulsion 2 dripped complete in 2.5 hours, kept still temperature 84 during dropping
±1℃；
(4) drip complete, reaction temperature is raised to 90 DEG C, insulation reaction 1 hour, then it is cooled to 40 DEG C, obtains high solids content
Low viscosity acrylate emulsion pressure-sensitive adhesive；
Described step (1) adds methyl methacrylate；
Adding reactive emulsifier B, described reactive emulsifier B in described step (2) is allyloxy Nonyl pheno
(10) ether ammonium sulfate (DNS-86) or allyloxy Nonyl pheno (10) ether bis phosphoric acid (ANPEO-P).
The preparation method of high-solid-content and low-viscosity acrylate emulsion stick the most according to claim 1, its feature
It is: the described monomer containing carboxyl function is acrylic acid, methacrylic acid or their mixture.
The preparation method of high-solid-content and low-viscosity acrylate emulsion stick the most according to claim 1, its feature
It is: the described many acrylate monomers of interior crosslinking are two (methyl) many glycol esters of acrylic acid, trimethylolpropane metering system
One or more in acid esters.
The preparation method of high-solid-content and low-viscosity acrylate emulsion stick the most according to claim 1, its feature
Be: the described many acrylate monomers of interior crosslinking be GDMA, diethyleneglycol dimethacrylate, two
One or more in methacrylic acid triglycol ester, dimethacrylate TEG ester.
The preparation method of high-solid-content and low-viscosity acrylate emulsion stick the most according to claim 1, its feature
It is: described anionic emulsifier A is the surfactant without nonyl phenol.
The preparation method of high-solid-content and low-viscosity acrylate emulsion stick the most according to claim 5, its feature
It is: described anionic emulsifier A is neopelex, lauryl sodium sulfate, sodium sulfo-succinate.
The preparation method of high-solid-content and low-viscosity acrylate emulsion stick the most according to claim 1, its feature
It is: described anionic emulsifier A is emulsifying agent EF810, EF800.
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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 |
| CN105504148B (en) * | 2016-02-25 | 2017-07-28 | 广州晶海化工有限公司 | A kind of water-borne pressure sensitive adhesive and preparation method thereof |
| CN108285508B (en) * | 2017-01-20 | 2020-10-30 | 湖北航天化学技术研究所 | Medium-high viscosity emulsion type acrylate pressure-sensitive adhesive for protective film, and preparation method and application thereof |
| CN106995676A (en) * | 2017-04-10 | 2017-08-01 | 孙小力 | A kind of zero formaldehyde wood adhesive and preparation method thereof |
| CN108084329B (en) * | 2017-12-01 | 2020-12-22 | 华南协同创新研究院 | Vinegar-acrylic emulsion with high solid content and low viscosity and preparation method thereof |
| 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 |
| CN109837046B (en) * | 2019-02-28 | 2020-11-27 | 广东星宇耐力新材料股份有限公司 | Water-based adhesive for dry compounding of plastic film and preparation method thereof |
| 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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| CN102603957A (en) * | 2012-02-29 | 2012-07-25 | 长兴化学工业(中国)有限公司 | Water-based adhesive component and preparation method of water-based pressure sensitive adhesive formed by water-based adhesive component |
| CN103205223B (en) * | 2012-08-29 | 2015-08-12 | 湖北航天化学技术研究所 | A kind of surface protection film single component emulsion pressure-sensitive and its preparation method and application |
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