CN107573794A - A kind of dumb light finishing varnish acrylic emulsion and preparation method thereof - Google Patents

A kind of dumb light finishing varnish acrylic emulsion and preparation method thereof Download PDF

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Publication number
CN107573794A
CN107573794A CN201711004606.2A CN201711004606A CN107573794A CN 107573794 A CN107573794 A CN 107573794A CN 201711004606 A CN201711004606 A CN 201711004606A CN 107573794 A CN107573794 A CN 107573794A
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China
Prior art keywords
added dropwise
dumb light
acrylic emulsion
finishing varnish
emulsion
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CN201711004606.2A
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Chinese (zh)
Inventor
李明杰
赵家栋
毛雄伟
李斌
陈尧红
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Zhejiang Kelisen Chemical Co Ltd
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Zhejiang Kelisen Chemical Co Ltd
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Priority to CN201711004606.2A priority Critical patent/CN107573794A/en
Publication of CN107573794A publication Critical patent/CN107573794A/en
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Abstract

The invention discloses a kind of dumb light finishing varnish acrylic emulsion and preparation method thereof, by percentage to the quality, including following components:Methacrylic acid 0.1%~0.3%, butyl acrylate 15%~16%, methyl methacrylate 1%~2%, styrene 8%~10%, hydrophobic vinyl special type monomer 10%~12%, reactive emulsifier 0.4%~0.6%, acrylamide 0.4%~0.6%, room-temperature self crosslinking monomer 0.5%~1.0%, silane coupler 0.1%~0.3%, molecular weight regulator 0.1%~0.2%, persulfate 0.02%~0.1%, ammoniacal liquor 0.1%~0.5%, deionized water 60%~70%.The present invention need not add flatting silica, you can so that glossiness is less than 20, the present invention has the performance that glossiness is low, permeability is good, dilution stability and storage stability are good.

Description

A kind of dumb light finishing varnish acrylic emulsion and preparation method thereof
Technical field
The invention belongs to building coating field, and in particular to a kind of dumb light finishing varnish acrylic emulsion and its preparation side Method.
Background technology
Matte varnish is one kind of water paint.For dumb light paint and semigloss paint are mainly the gloss of paint film.In general partly The glossiness of lac varnish should be between 40~60 (60 degree of angles), and dumb light paint gloss should be below 20 (60 degree of angles).Semigloss paint after brushing Paint film is more plain, and dumb light paint paint film more has texture.The characteristics of dumb light paint be lacquer painting than milder, somewhat vaporific, matte varnish does not have Have strong reflective to protecting vision to be also beneficial to.
It is the current focus researched and developed in the industry and difficult point to prepare high-performance coating dumb light finishing varnish.Building coating dumb light cover Face varnish paint film will not only have the property such as stain resistance, weatherability, resistance to water-white, chemicals-resistant and the artificial spatter property of bloom varnish Low-luster and high-permeability requirement can also be met in addition.
General dumb light finishing varnish is to add appropriate flatting silica and auxiliary material blending in varnish on the market at present Form.Although the glossiness of paint film can be reduced by using flatting silica and auxiliary material, also there is gloss uneven simultaneously The problems such as even, permeability reduces, system stability difference.
The content of the invention
In order to solve the above problems, the invention provides a kind of dumb light finishing varnish acrylic emulsion, it is not necessary to adds Flatting silica, you can so that glossiness is less than 20.
The technical scheme is that:A kind of dumb light finishing varnish acrylic emulsion, by percentage to the quality, including with Lower component:
Methacrylic acid 0.1%~0.3%, butyl acrylate 15%~16%, methyl methacrylate 1%~2%, benzene Ethene 8%~10%, hydrophobic vinyl special type monomer 10%~12%, reactive emulsifier 0.4%~0.6%, acryloyl Amine 0.4%~0.6%, room-temperature self crosslinking monomer 0.5%~1.0%, silane coupler 0.1%~0.3%, molecular weight regulator 0.1%~0.2%, persulfate 0.02%~0.1%, ammoniacal liquor 0.1%~0.5%, deionized water 60%~70%.
The flat stock reasonable disposition of the present invention, obtains a kind of dumb light finishing varnish acrylic emulsion, the emulsion without flatting silica, Small with particle diameter, emulsifier is low, the features such as dilution stability and good storage stability.The base material handled through this emulsion has The characteristics such as glossiness is low, permeability is good, resistance to water-white and closure is good.
Preferably, the reactive emulsifier is allyl alkyl polyoxyethylene ether ammonium sulfate.
Preferably, the room-temperature self crosslinking monomer is DAAM.
Preferably, the silane coupler is vinyltrimethoxy silane.
Preferably, the molecular weight regulator is n-dodecyl mercaptan.
Preferably, the persulfate is potassium peroxydisulfate.
Preferably, the hydrophobic vinyl special type monomer be tert-butyl acrylate, Tert-butyl Methacrylate and One or more in allyl methacrylate.
Present invention also offers the preparation method of above-mentioned dumb light finishing varnish acrylic emulsion, comprise the following steps:
(1) emulsifying tank:According to default proportioning, by the reactive emulsifier, methacrylic acid, methacrylic acid of 9/10 weight Methyl esters, butyl acrylate, acrylamide, the 1/4 of hydrophobic vinyl special type monomer ratio weight, room-temperature self crosslinking monomer and go Ionized water, it is placed in emulsifying tank, stirs 20~30 minutes, pre-emulsion is made;
(2) reactor:According to default proportioning, the reactive emulsifier of 1/10 weight, molecular weight regulator under remainder, go from Sub- water and potassium peroxydisulfate, emulsifying agent, molecular weight regulator and deionized water are placed in reactor and are heated to temperature as 88 After DEG C, start that the potassium peroxydisulfate of 1/4 weight is added dropwise;
(3) pre-emulsion is added dropwise at 87~88 DEG C, is added dropwise 2~3 hours, is added dropwise after the 3/4 of pre-emulsion gross weight Pause is added dropwise, and silane coupler and remaining hydrophobic vinyl special type monomer added in emulsifying tank stir 10 minutes with Afterwards, continue pre-emulsion being added dropwise in reactor, be added dropwise 0.5~1 hour, and remaining potassium peroxydisulfate is added dropwise simultaneously, drip Bi Hou, 2 hours are incubated at 87~89 DEG C, it is 7.0~8.0 that ammoniacal liquor regulation pH value is added after cooling, you can filtering and discharging, is obtained The dumb light finishing varnish acrylic emulsion.
The dumb light finishing varnish acrylic emulsion is prepared via above-mentioned preparation method, viscosity is 100~ 500mPa.s, discharge the dumb light finishing varnish acrylic emulsion for producing that solid content is 38%.
Compared with prior art, beneficial effects of the present invention are embodied in:
The present invention need not add flatting silica, you can so that glossiness is less than 20, the present invention has that glossiness is low, permeability Get well, the performance that dilution stability and storage stability are good.
Embodiment
Embodiment 1
A kind of dumb light finishing varnish acrylic emulsion, by percentage to the quality, including following components:
Methacrylic acid 0.2%, butyl acrylate 15.7%, methyl methacrylate 1.0%, styrene 9.0%, methyl Tert-butyl acrylate 10.0%, allyl methacrylate 1.0%, reactive emulsifier 0.52%, acrylamide 0.4% are double Acetone acrylamide 0.5%, silane coupler 0.2%, n-dodecyl mercaptan 0.1%, potassium peroxydisulfate 0.05%, ammoniacal liquor 0.15, deionized water 61.18%;Wherein reactive emulsifier is allyl alkyl polyoxyethylene ether ammonium sulfate, silane coupler For vinyltrimethoxy silane.
(1) emulsifying tank:According to default proportioning, by the reactive emulsifier, methacrylic acid, methacrylic acid of 9/10 weight Methyl esters, butyl acrylate, acrylamide, Tert-butyl Methacrylate with weight/power ratio 1/4, room-temperature self crosslinking monomer and deionization Water, it is placed in emulsifying tank, stirs 20~30 minutes, pre-emulsion is made;
(2) reactor:According to default proportioning, the reactive emulsifier of 1/10 weight, n-dodecyl mercaptan under remainder, go Ionized water and potassium peroxydisulfate, emulsifying agent, molecular weight regulator and deionized water are placed in 1000mL reactors and are heated to After temperature is 88 DEG C, start that the potassium peroxydisulfate of 1/4 weight is added dropwise;
(3) pre-emulsion is added dropwise at 87~88 DEG C, is added dropwise 2~3 hours, is added dropwise after the 3/4 of pre-emulsion gross weight Pause is added dropwise, and silane coupler and remaining hydrophobic vinyl special type monomer added in emulsifying tank stir 10 minutes with Afterwards, continue pre-emulsion being added dropwise in reactor, be added dropwise 0.5~1 hour, and remaining potassium peroxydisulfate is added dropwise simultaneously, drip Bi Hou, 2 hours are incubated at 87~89 DEG C, it is 7.0~8.0 that ammoniacal liquor regulation pH value is added after cooling, you can filtering and discharging obtains Solid content is 38% dumb light finishing varnish acrylic emulsion.
Embodiment 2
A kind of dumb light finishing varnish acrylic emulsion, by percentage to the quality, including following components:
The invention discloses a kind of dumb light finishing varnish acrylic emulsion, by percentage to the quality, including following components: Methacrylic acid 0.25%, butyl acrylate 15.4%, methyl methacrylate 1.0%, styrene 9.05%, methacrylic acid The tert-butyl ester 9.0%, tert-butyl acrylate 1.0%, allyl methacrylate 1.0%, reactive emulsifier 0.55%, acryloyl Amine 0.6%, DAAM 0.5%, silane coupler 0.2%, n-dodecyl mercaptan 0.1%, potassium peroxydisulfate 0.05%, ammoniacal liquor 0.15, deionized water 61.15%;Wherein reactive emulsifier is allyl alkyl polyoxyethylene ether ammonium sulfate, Silane coupler is vinyltrimethoxy silane.
(1) emulsifying tank:According to default proportioning, by the reactive emulsifier, methacrylic acid, methacrylic acid of 9/10 weight Methyl esters, butyl acrylate, acrylamide, Tert-butyl Methacrylate with weight/power ratio 1/4, room-temperature self crosslinking monomer and deionization Water, it is placed in emulsifying tank, stirs 20~30 minutes, pre-emulsion is made;
(2) reactor:According to default proportioning, the reactive emulsifier of 1/10 weight, n-dodecyl mercaptan under remainder, go Ionized water and potassium peroxydisulfate, emulsifying agent, molecular weight regulator and deionized water are placed in 1000mL reactors and are heated to After temperature is 88 DEG C, start that the potassium peroxydisulfate of 1/4 weight is added dropwise;
(3) pre-emulsion is added dropwise at 87~88 DEG C, is added dropwise 2~3 hours, is added dropwise after the 3/4 of pre-emulsion gross weight Pause is added dropwise, and silane coupler and remaining hydrophobic vinyl special type monomer added in emulsifying tank stir 10 minutes with Afterwards, continue pre-emulsion being added dropwise in reactor, be added dropwise 0.5~1 hour, and remaining potassium peroxydisulfate is added dropwise simultaneously, drip Bi Hou, 2 hours are incubated at 87~89 DEG C, it is 7.0~8.0 that ammoniacal liquor regulation pH value is added after cooling, you can filtering and discharging obtains Solid content is 38% dumb light finishing varnish acrylic emulsion.
Embodiment 3
A kind of dumb light finishing varnish acrylic emulsion, by percentage to the quality, including following components:
Methacrylic acid 0.3%, butyl acrylate 15.4%, methyl methacrylate 1.0%, styrene 8.9%, methyl Tert-butyl acrylate 10.2%, allyl methacrylate 1.0%, reactive emulsifier 0.4%, acrylamide 0.5%, double third Ketone acrylamide 0.5%, silane coupler 0.2%, n-dodecyl mercaptan 0.1%, potassium peroxydisulfate 0.05%, ammoniacal liquor 0.15, Deionized water 61.3%
;Wherein reactive emulsifier is allyl alkyl polyoxyethylene ether ammonium sulfate, and silane coupler is vinyl front three TMOS.
(1) emulsifying tank:According to default proportioning, the reactive emulsifier, methacrylic acid, metering system of 9/10 weight will be taken Sour methyl esters, butyl acrylate, acrylamide, Tert-butyl Methacrylate with weight/power ratio 1/4, room-temperature self crosslinking monomer and go from Sub- water, is placed in emulsifying tank, stirs 20~30 minutes, and pre-emulsion is made;
(2) reactor:According to default proportioning, the reactive emulsifier of 1/10 weight, n-dodecyl mercaptan under remainder, go Ionized water and potassium peroxydisulfate, emulsifying agent, molecular weight regulator and deionized water are placed in 1000mL reactors and are heated to After temperature is 88 DEG C, start that the potassium peroxydisulfate of 1/4 weight is added dropwise;
(3) pre-emulsion is added dropwise at 87~88 DEG C, is added dropwise 2~3 hours, is added dropwise after the 3/4 of pre-emulsion gross weight Pause is added dropwise, and silane coupler and remaining hydrophobic vinyl special type monomer added in emulsifying tank stir 10 minutes with Afterwards, continue pre-emulsion being added dropwise in reactor, be added dropwise 0.5~1 hour, and remaining potassium peroxydisulfate is added dropwise simultaneously, drip Bi Hou, 2 hours are incubated at 87~89 DEG C, it is 7.0~8.0 that ammoniacal liquor regulation pH value is added after cooling, you can filtering and discharging obtains Solid content is 38% dumb light finishing varnish acrylic emulsion.
Embodiment 4
A kind of dumb light finishing varnish acrylic emulsion, by percentage to the quality, including following components:
Methacrylic acid 0.2%, butyl acrylate 15.8%, methyl methacrylate 1.0%, styrene 8.9%, methyl Tert-butyl acrylate 10.0%, allyl methacrylate 1.0%, reactive emulsifier 0.5%, acrylamide 0.4%, double third Ketone acrylamide 0.5%, silane coupler 0.2%, n-dodecyl mercaptan 0.1%, potassium peroxydisulfate 0.05%, ammoniacal liquor 0.15, Deionized water 61.2%;Wherein reactive emulsifier is allyl alkyl polyoxyethylene ether ammonium sulfate, and silane coupler is ethene Base trimethoxy silane.
(1) emulsifying tank:According to default proportioning, by the reactive emulsifier, methacrylic acid, methacrylic acid of 9/10 weight Methyl esters, butyl acrylate, acrylamide, Tert-butyl Methacrylate with weight/power ratio 1/4, room-temperature self crosslinking monomer and deionization Water, it is placed in emulsifying tank, stirs 20~30 minutes, pre-emulsion is made;
(2) reactor:According to default proportioning, the reactive emulsifier of 1/10 weight, n-dodecyl mercaptan under remainder, go Ionized water and potassium peroxydisulfate, emulsifying agent, molecular weight regulator and deionized water are placed in 1000mL reactors and are heated to After temperature is 88 DEG C, start that the potassium peroxydisulfate of 1/4 weight is added dropwise;
(3) pre-emulsion is added dropwise at 87~88 DEG C, is added dropwise 2~3 hours, is added dropwise after the 3/4 of pre-emulsion gross weight Pause is added dropwise, and silane coupler and remaining hydrophobic vinyl special type monomer added in emulsifying tank stir 10 minutes with Afterwards, continue pre-emulsion being added dropwise in reactor, be added dropwise 0.5~1 hour, and remaining potassium peroxydisulfate is added dropwise simultaneously, drip Bi Hou, 2 hours are incubated at 87~89 DEG C, it is 7.0~8.0 that ammoniacal liquor regulation pH value is added after cooling, you can filtering and discharging obtains Solid content is 38% dumb light finishing varnish acrylic emulsion.
Embodiment 5
A kind of dumb light finishing varnish acrylic emulsion, by percentage to the quality, including following components:
Methacrylic acid 0.25%, butyl acrylate 15.4%, methyl methacrylate 1.0%, styrene 9.05%, first Base tert-butyl acrylate 10.0%, tert-butyl acrylate 1.0%, reactive emulsifier 0.52%, acrylamide 0.4%, double third Ketone acrylamide 0.5%, silane coupler 0.2%, n-dodecyl mercaptan 0.1%, potassium peroxydisulfate 0.05%, ammoniacal liquor 0.15, Deionized water 61.22%;Wherein reactive emulsifier is allyl alkyl polyoxyethylene ether ammonium sulfate, and silane coupler is ethene Base trimethoxy silane.
(1) emulsifying tank:According to default proportioning, by the reactive emulsifier, methacrylic acid, methacrylic acid of 9/10 weight Methyl esters, butyl acrylate, acrylamide, Tert-butyl Methacrylate with weight/power ratio 1/4, room-temperature self crosslinking monomer and deionization Water, it is placed in emulsifying tank, stirs 20~30 minutes, pre-emulsion is made;
(2) reactor:According to default proportioning, the reactive emulsifier of 1/10 weight, n-dodecyl mercaptan under remainder, go Ionized water and potassium peroxydisulfate, emulsifying agent, molecular weight regulator and deionized water are placed in 1000mL reactors and are heated to After temperature is 88 DEG C, start that the potassium peroxydisulfate of 1/4 weight is added dropwise;
(3) pre-emulsion is added dropwise at 87~88 DEG C, is added dropwise 2~3 hours, is added dropwise after the 3/4 of pre-emulsion gross weight Pause is added dropwise, and silane coupler and remaining hydrophobic vinyl special type monomer added in emulsifying tank stir 10 minutes with Afterwards, continue pre-emulsion being added dropwise in reactor, be added dropwise 0.5~1 hour, and remaining potassium peroxydisulfate is added dropwise simultaneously, drip Bi Hou, 2 hours are incubated at 87~89 DEG C, it is 7.0~8.0 that ammoniacal liquor regulation pH value is added after cooling, you can filtering and discharging obtains Solid content is 38% dumb light finishing varnish acrylic emulsion.
Test glossiness effective evaluation:
Emulsion prepared by the present invention is prepared into film on a glass with 120 μm of wet film makers, it is small in drying at room temperature 24 When after determine glossiness.Operation equipment:BYK micro~gloss 4442.E measurement technology:1.567 refraction coefficient black glass On-gauge plate, reflected value are 100 gloss units.Light-source structure:60 ° of incident angles.Measuring method:Continuous measure 5 times is averaged. Test result is shown in Table 1.
The glossiness test result of the embodiment 1~5 of table 1
Embodiment 1 2 3 4 5
Glossiness 12 18 16 12 19

Claims (8)

  1. A kind of 1. dumb light finishing varnish acrylic emulsion, it is characterised in that by percentage to the quality, including following components:
    Methacrylic acid 0.1%~0.3%, butyl acrylate 15%~16%, methyl methacrylate 1%~2%, styrene 8%~10%, hydrophobic vinyl special type monomer 10%~12%, reactive emulsifier 0.4%~0.6%, acrylamide 0.4%~0.6%, room-temperature self crosslinking monomer 0.5%~1.0%, silane coupler 0.1%~0.3%, molecular weight regulator 0.1%~0.2%, persulfate 0.02%~0.1%, ammoniacal liquor 0.1%~0.5%, deionized water 60%~70%.
  2. 2. dumb light finishing varnish acrylic emulsion as claimed in claim 1, it is characterised in that the reactive emulsifier is Allyl alkyl polyoxyethylene ether ammonium sulfate.
  3. 3. dumb light finishing varnish acrylic emulsion as claimed in claim 1, it is characterised in that the room-temperature self crosslinking monomer For DAAM.
  4. 4. dumb light finishing varnish acrylic emulsion as claimed in claim 1, it is characterised in that the silane coupler is second Alkenyl trimethoxy silane.
  5. 5. dumb light finishing varnish acrylic emulsion as claimed in claim 1, it is characterised in that the molecular weight regulator is N-dodecyl mercaptan.
  6. 6. dumb light finishing varnish acrylic emulsion as claimed in claim 1, it is characterised in that the persulfate is over cure Sour potassium.
  7. 7. dumb light finishing varnish acrylic emulsion as claimed in claim 1, it is characterised in that the hydrophobic vinyl is special Kind monomer is the one or more in tert-butyl acrylate, Tert-butyl Methacrylate and allyl methacrylate.
  8. 8. the preparation method of the dumb light finishing varnish acrylic emulsion as described in claim 1~7 is any, it is characterised in that Comprise the following steps:
    (1) emulsifying tank:According to default proportioning, by the reactive emulsifier, methacrylic acid, methyl methacrylate of 9/10 weight Ester, butyl acrylate, acrylamide, the 1/4 of hydrophobic vinyl special type monomer ratio weight, room-temperature self crosslinking monomer and go from Sub- water, is placed in emulsifying tank, stirs 20~30 minutes, and pre-emulsion is made;
    (2) reactor:According to default proportioning, the reactive emulsifier of 1/10 weight, molecular weight regulator, deionized water under remainder And potassium peroxydisulfate, emulsifying agent, molecular weight regulator and deionized water are placed in reactor be heated to temperature for 88 DEG C it Afterwards, the potassium peroxydisulfate of 1/4 weight of dropwise addition is started;
    (3) pre-emulsion is added dropwise at 87~88 DEG C, is added dropwise 2~3 hours, pause after the 3/4 of pre-emulsion gross weight is added dropwise It is added dropwise, and after silane coupler and remaining hydrophobic vinyl special type monomer added in emulsifying tank stirring 10 minutes, after It is continuous that pre-emulsion is added dropwise in reactor, it is added dropwise 0.5~1 hour, and remaining potassium peroxydisulfate is added dropwise simultaneously, after being added dropwise, 2 hours are incubated at 87~89 DEG C, it is 7.0~8.0 that ammoniacal liquor regulation pH value is added after cooling, you can filtering and discharging, is obtained described Dumb light finishing varnish acrylic emulsion.
CN201711004606.2A 2017-10-23 2017-10-23 A kind of dumb light finishing varnish acrylic emulsion and preparation method thereof Pending CN107573794A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109265625A (en) * 2018-09-25 2019-01-25 赵家栋 A kind of dedicated acrylic emulsion of lacquer and its preparation method and application
CN109337023A (en) * 2018-09-26 2019-02-15 上海乘鹰新材料有限公司 A kind of PVDC composite membrane primary coat lotion and its synthetic method
CN111205387A (en) * 2020-03-12 2020-05-29 广东巴德富新材料有限公司 Zero-additive odor-free super stain-resistant acrylate emulsion and preparation method thereof
CN112300318A (en) * 2020-11-10 2021-02-02 三棵树(上海)新材料研究有限公司 Environment-friendly room-temperature self-crosslinking acrylate emulsion, preparation method and application thereof
CN113265020A (en) * 2021-06-22 2021-08-17 广东金万联防水材料有限公司 Preparation method of gloss oil finishing emulsion

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104045761A (en) * 2014-06-16 2014-09-17 张家港康得新光电材料有限公司 Matte scratch-resistant water-based resin and preparation method thereof
CN106608943A (en) * 2016-11-22 2017-05-03 佛山市顺德区巴德富实业有限公司 One-component acrylic ester matte core-shell emulsions with good anti-water-white performance and preparation method and application thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104045761A (en) * 2014-06-16 2014-09-17 张家港康得新光电材料有限公司 Matte scratch-resistant water-based resin and preparation method thereof
CN106608943A (en) * 2016-11-22 2017-05-03 佛山市顺德区巴德富实业有限公司 One-component acrylic ester matte core-shell emulsions with good anti-water-white performance and preparation method and application thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109265625A (en) * 2018-09-25 2019-01-25 赵家栋 A kind of dedicated acrylic emulsion of lacquer and its preparation method and application
CN109265625B (en) * 2018-09-25 2021-02-26 浙江科力森化学有限公司 Acrylic emulsion special for real stone paint and preparation method and application thereof
CN109337023A (en) * 2018-09-26 2019-02-15 上海乘鹰新材料有限公司 A kind of PVDC composite membrane primary coat lotion and its synthetic method
CN111205387A (en) * 2020-03-12 2020-05-29 广东巴德富新材料有限公司 Zero-additive odor-free super stain-resistant acrylate emulsion and preparation method thereof
CN112300318A (en) * 2020-11-10 2021-02-02 三棵树(上海)新材料研究有限公司 Environment-friendly room-temperature self-crosslinking acrylate emulsion, preparation method and application thereof
CN113265020A (en) * 2021-06-22 2021-08-17 广东金万联防水材料有限公司 Preparation method of gloss oil finishing emulsion

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