CN117866138A - Mica powder modified emulsion and preparation method and application thereof - Google Patents
Mica powder modified emulsion and preparation method and application thereof Download PDFInfo
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- CN117866138A CN117866138A CN202311800216.1A CN202311800216A CN117866138A CN 117866138 A CN117866138 A CN 117866138A CN 202311800216 A CN202311800216 A CN 202311800216A CN 117866138 A CN117866138 A CN 117866138A
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- 239000000839 emulsion Substances 0.000 title claims abstract description 174
- 239000010445 mica Substances 0.000 title claims abstract description 44
- 229910052618 mica group Inorganic materials 0.000 title claims abstract description 44
- 239000000843 powder Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 238000004945 emulsification Methods 0.000 title description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 67
- 239000000178 monomer Substances 0.000 claims abstract description 65
- 239000003999 initiator Substances 0.000 claims abstract description 61
- ISXSCDLOGDJUNJ-UHFFFAOYSA-N tert-butyl prop-2-enoate Chemical compound CC(C)(C)OC(=O)C=C ISXSCDLOGDJUNJ-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000004132 cross linking Methods 0.000 claims abstract description 26
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 12
- 230000009477 glass transition Effects 0.000 claims abstract 2
- 239000000463 material Substances 0.000 claims description 30
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 26
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 20
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 17
- 239000003995 emulsifying agent Substances 0.000 claims description 16
- DBCAQXHNJOFNGC-UHFFFAOYSA-N 4-bromo-1,1,1-trifluorobutane Chemical compound FC(F)(F)CCCBr DBCAQXHNJOFNGC-UHFFFAOYSA-N 0.000 claims description 15
- STVZJERGLQHEKB-UHFFFAOYSA-N ethylene glycol dimethacrylate Substances CC(=C)C(=O)OCCOC(=O)C(C)=C STVZJERGLQHEKB-UHFFFAOYSA-N 0.000 claims description 15
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 14
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 14
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 13
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 9
- GOXQRTZXKQZDDN-UHFFFAOYSA-N 2-Ethylhexyl acrylate Chemical compound CCCCC(CC)COC(=O)C=C GOXQRTZXKQZDDN-UHFFFAOYSA-N 0.000 claims description 6
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 5
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 5
- LCPVQAHEFVXVKT-UHFFFAOYSA-N 2-(2,4-difluorophenoxy)pyridin-3-amine Chemical compound NC1=CC=CN=C1OC1=CC=C(F)C=C1F LCPVQAHEFVXVKT-UHFFFAOYSA-N 0.000 claims description 4
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 4
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 4
- 239000004641 Diallyl-phthalate Substances 0.000 claims description 4
- QUDWYFHPNIMBFC-UHFFFAOYSA-N bis(prop-2-enyl) benzene-1,2-dicarboxylate Chemical compound C=CCOC(=O)C1=CC=CC=C1C(=O)OCC=C QUDWYFHPNIMBFC-UHFFFAOYSA-N 0.000 claims description 4
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 4
- CIHOLLKRGTVIJN-UHFFFAOYSA-N tert‐butyl hydroperoxide Chemical compound CC(C)(C)OO CIHOLLKRGTVIJN-UHFFFAOYSA-N 0.000 claims description 3
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical compound OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 2
- CFVWNXQPGQOHRJ-UHFFFAOYSA-N 2-methylpropyl prop-2-enoate Chemical compound CC(C)COC(=O)C=C CFVWNXQPGQOHRJ-UHFFFAOYSA-N 0.000 claims description 2
- FYRWKWGEFZTOQI-UHFFFAOYSA-N 3-prop-2-enoxy-2,2-bis(prop-2-enoxymethyl)propan-1-ol Chemical compound C=CCOCC(CO)(COCC=C)COCC=C FYRWKWGEFZTOQI-UHFFFAOYSA-N 0.000 claims description 2
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 2
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 2
- 239000002202 Polyethylene glycol Substances 0.000 claims description 2
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 2
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 2
- OKKRPWIIYQTPQF-UHFFFAOYSA-N Trimethylolpropane trimethacrylate Chemical compound CC(=C)C(=O)OCC(CC)(COC(=O)C(C)=C)COC(=O)C(C)=C OKKRPWIIYQTPQF-UHFFFAOYSA-N 0.000 claims description 2
- 229930003268 Vitamin C Natural products 0.000 claims description 2
- IBVAQQYNSHJXBV-UHFFFAOYSA-N adipic acid dihydrazide Chemical compound NNC(=O)CCCCC(=O)NN IBVAQQYNSHJXBV-UHFFFAOYSA-N 0.000 claims description 2
- 125000004386 diacrylate group Chemical group 0.000 claims description 2
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 2
- OMNKZBIFPJNNIO-UHFFFAOYSA-N n-(2-methyl-4-oxopentan-2-yl)prop-2-enamide Chemical compound CC(=O)CC(C)(C)NC(=O)C=C OMNKZBIFPJNNIO-UHFFFAOYSA-N 0.000 claims description 2
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 claims description 2
- 229920001223 polyethylene glycol Polymers 0.000 claims description 2
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 2
- 229920000053 polysorbate 80 Polymers 0.000 claims description 2
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 2
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 2
- 235000019154 vitamin C Nutrition 0.000 claims description 2
- 239000011718 vitamin C Substances 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims 1
- 230000004888 barrier function Effects 0.000 abstract description 10
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 6
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 239000002861 polymer material Substances 0.000 abstract description 2
- 238000003786 synthesis reaction Methods 0.000 abstract description 2
- 239000008367 deionised water Substances 0.000 description 44
- 229910021641 deionized water Inorganic materials 0.000 description 44
- 239000000123 paper Substances 0.000 description 19
- 239000003513 alkali Substances 0.000 description 12
- 239000002585 base Substances 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 12
- 238000001816 cooling Methods 0.000 description 12
- 238000006386 neutralization reaction Methods 0.000 description 12
- 239000002518 antifoaming agent Substances 0.000 description 11
- 238000004090 dissolution Methods 0.000 description 11
- 239000003755 preservative agent Substances 0.000 description 11
- 230000002335 preservative effect Effects 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 9
- 230000000903 blocking effect Effects 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 7
- 238000000576 coating method Methods 0.000 description 7
- 239000004698 Polyethylene Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011436 cob Substances 0.000 description 2
- 239000007888 film coating Substances 0.000 description 2
- 238000009501 film coating Methods 0.000 description 2
- 150000002632 lipids Chemical class 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 125000003011 styrenyl group Chemical group [H]\C(*)=C(/[H])C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Polymerisation Methods In General (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a mica powder modified emulsion and a preparation method and application thereof. Relates to the technical field of high polymer material synthesis. The modified emulsion comprises the following components: monomers containing unsaturated double bonds; a crosslinking monomer; mica powder; an initiator; an auxiliary agent; water; the unsaturated double bond-containing monomer comprises tert-butyl acrylate, and the glass transition temperature of the modified emulsion is less than 25 ℃. According to the invention, an environment-friendly formula is adopted, substances such as acrylamide food safety hidden trouble are not added, and the problem of adhesion in the application process of the high-barrier emulsion is solved by adding the mica powder modified emulsion while the excellent barrier property of the emulsion is ensured. In addition, the invention further improves the barrier property of the emulsion through optimizing the components and the dosage.
Description
Technical Field
The invention relates to the technical field of high polymer material synthesis, in particular to a mica powder modified emulsion and a preparation method and application thereof.
Background
As the pace of life increases, the need for disposable paper containers in daily life increases. At present, a PE film coating process is generally adopted on the surface of a paper carrier of a paper container so as to provide good oil and water resistance. However, the PE film coating container is difficult to pulp and recycle, PE materials are difficult to degrade, and the abandoned PE container becomes white garbage, so that plastic pollution is caused. In recent years, with the increasing environmental awareness, the trend of replacing PE coated paper products with coated paper products has become large.
The coated paper product is prepared by coating a layer of special coating material on the surface of common paper to improve the glossiness, smoothness, stiffness, water resistance, oil resistance and the like of the paper. Such coating materials are typically made from emulsions. An emulsion is a colloidal substance formed from solid particles suspended in a liquid. Emulsions are typically composed of colloidal particles, dispersants, stabilizers, water, and the like. In the production of coated paper products, the emulsion is coated onto the surface of the paper and then converted to a coating by drying and curing processes. The solid particles in the emulsion can fill the tiny pits on the surface of the paper to form a barrier coating, so that the paper is smoother, and the properties of water resistance, oil resistance and the like are provided.
There are problems associated with the emulsions used in coated paper products in the prior art, including the addition of acrylamide-based materials and blocking in high barrier emulsion applications.
To improve the properties of the coated paper products, acrylamide-based substances are often added to the emulsion. Acrylamide is a chemical substance commonly used to increase emulsion stability and oil resistance. However, acrylamide can cause food safety hazards, especially when harmful substances are released under high temperature conditions.
The high-barrier emulsion is an emulsion with excellent water resistance, oil resistance and gas resistance, and is commonly used in the fields of packaging materials and the like. However, blocking sometimes occurs during the application of high barrier emulsions. This is because the polymers of the high barrier emulsions are generally relatively sticky and tend to stick during the winding of the paper roll.
Based on this, there is a need to develop a novel modified emulsion to solve the above problems.
Disclosure of Invention
The first technical problem to be solved by the invention is as follows:
a modified emulsion is provided.
The second technical problem to be solved by the invention is as follows:
a method of preparing the modified emulsion is provided.
The third technical problem to be solved by the invention is:
the application of the modified emulsion.
The invention also provides a coated white cardboard.
In order to solve the first technical problem, the invention adopts the following technical scheme:
a modified emulsion comprising the following components:
monomers containing unsaturated double bonds;
a crosslinking monomer;
mica powder;
an initiator;
an auxiliary agent;
water;
the unsaturated double bond-containing monomer comprises tert-butyl acrylate.
According to the embodiments of the present invention, one of the technical solutions has at least one of the following advantages or beneficial effects:
according to the invention, an environment-friendly formula is adopted, substances such as acrylamide food safety hidden trouble are not added, and the problem of adhesion in the application process of the high-barrier emulsion is solved by adding the mica powder modified emulsion while the excellent barrier property of the emulsion is ensured. In addition, the invention further improves the barrier property of the emulsion through optimizing the components and the dosage.
The modified emulsion provided by the invention has excellent water and oil blocking capability and excellent anti-adhesion performance, meets the food safety requirement, and can be widely used in various coating packaging food papers.
According to one embodiment of the invention, the modified emulsion comprises the following components in parts by weight:
420-650 parts of unsaturated double bond-containing monomer;
0.05-1 part of crosslinking monomer;
10-50 parts of mica powder;
0.5-10 parts of initiator;
5-15 parts of an auxiliary agent;
400-800 parts of water.
According to one embodiment of the invention, the modified emulsion comprises the following components in parts by weight:
440-630 parts of unsaturated double bond-containing monomer;
0.1-0.9 part of crosslinking monomer;
15-45 parts of mica powder;
1-8 parts of an initiator;
6-14 parts of an auxiliary agent;
400-800 parts of water.
According to one embodiment of the invention, the modified emulsion comprises the following components in parts by weight:
470-600 parts of unsaturated double bond-containing monomer;
0.2-0.8 part of crosslinking monomer;
20-40 parts of mica powder;
1.5-6 parts of initiator;
7-13 parts of an auxiliary agent;
400-800 parts of water.
According to one embodiment of the invention, the effect of t-butyl acrylate is to improve the hydrophobicity of the emulsion.
According to one embodiment of the present invention, the unsaturated double bond-containing monomer further includes at least one of styrene, methyl methacrylate, n-butyl acrylate, n-butyl methacrylate, isobutyl acrylate, 2-ethylhexyl acrylate, ethyl acrylate, acrylic acid, methacrylic acid, and hydroxyethyl acrylate.
According to one embodiment of the present invention, the crosslinking monomer includes at least one of diallyl phthalate, N' N methylene bisacrylamide, ethylene glycol dimethacrylate, pentaerythritol triallyl ether, polyethylene glycol diacrylate, ethylene glycol dimethacrylate, trimethylolpropane trimethacrylate, diacetone acrylamide, and adipic acid dihydrazide.
According to one embodiment of the present invention, the initiator comprises at least one of potassium persulfate, sodium persulfate, ammonium persulfate, sodium bisulfite, vitamin C, and t-butyl hydroperoxide.
According to one embodiment of the invention, the adjuvant comprises an emulsifier comprising at least one of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, DOWFAX 2A1, SR-10 Ai Dike, ER-10 Ai Dike, LCN287 Craien, COPS-1 Soxhlet and Tween 80.
In order to solve the second technical problem, the invention adopts the following technical scheme:
a method of preparing the modified emulsion comprising the steps of:
s1, mixing mica powder and part of auxiliary agent in part of water to obtain a base material A;
s2, mixing a monomer containing unsaturated double bonds, a crosslinking monomer and the balance of auxiliary agent in the balance of water to obtain a pre-emulsion B;
s3, mixing the primer A, the pre-emulsion B and the initiator, and heating to obtain the modified emulsion.
According to one embodiment of the invention, a method for preparing the modified emulsion comprises the steps of:
mixing mica powder and part of auxiliary agent in part of water to obtain a base material A;
q2, mixing a monomer containing unsaturated double bonds, a crosslinking monomer and the balance of auxiliary agent in the balance of water to obtain a pre-emulsion B;
q3, mixing the bottom material A, part of the pre-emulsion B and part of the initiator, and heating to obtain flaky seed emulsion;
and Q4, adding the residual pre-emulsion B and the residual initiator C into the flaky seed emulsion, heating, preserving heat after the reaction is finished, cooling to 50 ℃ after the heat preservation is finished, and adding alkali liquor for neutralization to obtain the modified emulsion.
In the step Q3, since the mica powder is in a flake shape, the polymerized monomer is polymerized on the basis of the mica powder to form a flake seed emulsion, and the flake emulsion can be stacked more densely in the film forming process, so that the barrier property of the modified emulsion is improved.
According to one embodiment of the invention, in step Q3, the heating temperature is 80-90℃and the reaction time is 20-30min.
According to one embodiment of the invention, in the step Q4, the temperature of heat preservation is 80-90 ℃ and the heat preservation time period is 1h;
according to one embodiment of the present invention, in the step Q4, the residual pre-emulsion B and the residual initiator C are added dropwise for 3 to 4 hours.
In another aspect of the present invention, a coated white cardboard is also provided. Comprising a modified emulsion as described in the example of aspect 1 above. The application adopts all the technical schemes of the modified emulsion, so that the modified emulsion has at least all the beneficial effects brought by the technical schemes of the embodiment.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Detailed Description
The words "preferably," "more preferably," and the like in the present invention refer to embodiments of the invention that may provide certain benefits in some instances. However, other embodiments may be preferred under the same or other circumstances. Furthermore, the recitation of one or more preferred embodiments does not imply that other embodiments are not useful, nor is it intended to exclude other embodiments from the scope of the invention.
When a range of values is disclosed herein, the range is considered to be continuous and includes both the minimum and maximum values for the range, as well as each value between such minimum and maximum values. Further, when a range refers to an integer, each integer between the minimum and maximum values of the range is included. Further, when multiple range description features or characteristics are provided, the ranges may be combined. In other words, unless otherwise indicated, all ranges disclosed herein are to be understood to include any and all subranges subsumed therein.
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to fall within the scope of the invention.
The reagents, methods and apparatus employed in the present invention, unless otherwise specified, are all conventional in the art.
Example 1
The modified emulsion comprises the following components in parts by weight:
510 parts of unsaturated double bond-containing monomer;
0.4 parts of a crosslinking monomer;
20 parts of mica powder;
3 parts of an initiator;
8 parts of emulsifying agent;
deionized water, 700 parts;
the unsaturated double bond-containing monomer comprises 20 parts of tert-butyl acrylate.
The preparation of the modified emulsion comprises the following steps:
s1, adding 250 parts of deionized water, 2 parts of DOWFAX 2A1 and 1 part of LCN287 into a reaction kettle, adding 20 parts of nano mica powder after complete dissolution, uniformly dispersing, and heating to 80 ℃ to form a base material A;
s2, 6 parts of DOWFAX 2A1 and 2 parts of LCN287 are dissolved in 400 parts of deionized water, 280 parts of n-butyl acrylate, 200 parts of methyl methacrylate, 10 parts of acrylic acid, 20 parts of tert-butyl acrylate and 0.4 part of ethylene glycol dimethacrylate are added respectively to prepare a pre-emulsion B;
s3, 3 parts of ammonium persulfate is dissolved in 50 parts of deionized water to prepare an initiator solution C. Taking 4% by weight of the pre-emulsion B and 8% by weight of the initiator solution C, adding the pre-emulsion B into the bottom material A, and preserving heat at 85 ℃ for 25min to form flaky seed emulsion;
s4, dropwise adding the residual pre-emulsion B and the residual initiator solution C into the flaky seed emulsion, dropwise adding for 3 hours, keeping the temperature at 80 ℃, preserving the heat for 1 hour, cooling to 50 ℃, adding alkali liquor for neutralization, and then adding a defoaming agent with a conventional dosage and a preservative with a conventional dosage to obtain the modified emulsion.
Example 2
Example 2 differs from example 1 in that: the amounts of methyl methacrylate and n-butyl acrylate vary. Wherein, the amount of methyl methacrylate in example 1 is 200 parts and the amount of n-butyl acrylate is 280 parts; in example 2, the amount of methyl methacrylate was 260 parts and the amount of n-butyl acrylate was 220 parts.
The modified emulsion comprises the following components in parts by weight:
510 parts of unsaturated double bond-containing monomer;
0.4 parts of a crosslinking monomer;
20 parts of mica powder;
3 parts of an initiator;
8 parts of emulsifying agent;
deionized water, 700 parts;
the unsaturated double bond-containing monomer comprises 20 parts of tert-butyl acrylate.
The preparation of the modified emulsion comprises the following steps:
s1, adding 250 parts of deionized water, 2 parts of DOWFAX 2A1 and 1 part of LCN287 into a reaction kettle, adding 20 parts of nano mica powder after complete dissolution, uniformly dispersing, and heating to 80 ℃ to form a base material A;
s2, 6 parts of DOWFAX 2A1 and 2 parts of LCN287 are dissolved in 400 parts of deionized water, and then 220 parts of n-butyl acrylate, 260 parts of methyl methacrylate, 10 parts of acrylic acid, 20 parts of tert-butyl acrylate and 0.4 part of ethylene glycol dimethacrylate are added respectively to prepare a pre-emulsion B;
s3, 3 parts of ammonium persulfate is dissolved in 50 parts of deionized water to prepare an initiator solution C. Taking 4% by weight of the pre-emulsion B and 8% by weight of the initiator solution C, adding the pre-emulsion B into the bottom material A, and preserving heat at 85 ℃ for 25min to form flaky seed emulsion;
s4, dropwise adding the residual pre-emulsion B and the residual initiator solution C into the flaky seed emulsion, dropwise adding for 3 hours, keeping the temperature at 80 ℃, preserving the heat for 1 hour, cooling to 50 ℃, adding alkali liquor for neutralization, and then adding a defoaming agent with a conventional dosage and a preservative with a conventional dosage to obtain the modified emulsion.
Example 3
Example 3 differs from example 1 in that: the amounts of methyl methacrylate and n-butyl acrylate vary. Wherein, the amount of methyl methacrylate in example 1 is 200 parts and the amount of n-butyl acrylate is 280 parts; in example 3, the amount of methyl methacrylate was 290 parts and the amount of n-butyl acrylate was 190 parts.
The modified emulsion comprises the following components in parts by weight:
510 parts of unsaturated double bond-containing monomer;
0.4 parts of a crosslinking monomer;
20 parts of mica powder;
3 parts of an initiator;
8 parts of emulsifying agent;
deionized water, 700 parts;
the unsaturated double bond-containing monomer comprises 20 parts of tert-butyl acrylate.
The preparation of the modified emulsion comprises the following steps:
s1, adding 250 parts of deionized water, 2 parts of DOWFAX 2A1 and 1 part of LCN287 into a reaction kettle, adding 20 parts of nano mica powder after complete dissolution, uniformly dispersing, and heating to 80 ℃ to form a base material A;
s2, 6 parts of DOWFAX 2A1 and 2 parts of LCN287 are dissolved in 400 parts of deionized water, and then 190 parts of n-butyl acrylate, 290 parts of methyl methacrylate, 10 parts of acrylic acid, 20 parts of tert-butyl acrylate and 0.4 part of ethylene glycol dimethacrylate are added respectively to prepare a pre-emulsion B;
s3, 3 parts of ammonium persulfate is dissolved in 50 parts of deionized water to prepare an initiator solution C. Taking 4% by weight of the pre-emulsion B and 8% by weight of the initiator solution C, adding the pre-emulsion B into the bottom material A, and preserving heat at 85 ℃ for 25min to form flaky seed emulsion;
s4, dropwise adding the residual pre-emulsion B and the residual initiator solution C into the flaky seed emulsion, dropwise adding for 3 hours, keeping the temperature at 80 ℃, preserving the heat for 1 hour, cooling to 50 ℃, adding alkali liquor for neutralization, and then adding a defoaming agent with a conventional dosage and a preservative with a conventional dosage to obtain the modified emulsion.
Example 4
Example 4 differs from example 1 in that: in example 4, methyl methacrylate and n-butyl acrylate in example 1 were replaced with styrene and 2-ethylhexyl acrylate, and the amount of styrene was 238 parts and the amount of 2-ethylhexyl acrylate was 242 parts.
The modified emulsion comprises the following components in parts by weight:
510 parts of unsaturated double bond-containing monomer;
0.4 parts of a crosslinking monomer;
20 parts of mica powder;
3 parts of an initiator;
8 parts of emulsifying agent;
deionized water, 700 parts;
the unsaturated double bond-containing monomer comprises 20 parts of tert-butyl acrylate.
The preparation of the modified emulsion comprises the following steps:
s1, adding 250 parts of deionized water, 2 parts of DOWFAX 2A1 and 1 part of LCN287 into a reaction kettle, adding 20 parts of nano mica powder after complete dissolution, uniformly dispersing, and heating to 80 ℃ to form a base material A;
s2, 6 parts of DOWFAX 2A1 and 2 parts of LCN287 are dissolved in 400 parts of deionized water, and then 242 parts of acrylic acid-2-ethylhexyl ester, 238 parts of styrene, 10 parts of acrylic acid, 20 parts of tert-butyl acrylate and 0.4 part of ethylene glycol dimethacrylate are respectively added to prepare a pre-emulsion B;
s3, 3 parts of ammonium persulfate is dissolved in 50 parts of deionized water to prepare an initiator solution C. Taking 4% by weight of the pre-emulsion B and 8% by weight of the initiator solution C, adding the pre-emulsion B into the bottom material A, and preserving heat at 85 ℃ for 25min to form flaky seed emulsion;
s4, dropwise adding the residual pre-emulsion B and the residual initiator solution C into the flaky seed emulsion, dropwise adding for 3 hours, keeping the temperature at 80 ℃, preserving the heat for 1 hour, cooling to 50 ℃, adding alkali liquor for neutralization, and then adding a defoaming agent with a conventional dosage and a preservative with a conventional dosage to obtain the modified emulsion.
Example 5
Example 5 differs from example 1 in that: the amount of mica powder varies. Wherein, the use amount of the mica powder in the example 1 is 20 parts; in example 5, the amount of mica powder used was 30 parts.
The modified emulsion comprises the following components in parts by weight:
510 parts of unsaturated double bond-containing monomer;
0.4 parts of a crosslinking monomer;
30 parts of mica powder;
3 parts of an initiator;
8 parts of emulsifying agent;
deionized water, 700 parts;
the unsaturated double bond-containing monomer comprises 20 parts of tert-butyl acrylate.
The preparation of the modified emulsion comprises the following steps:
s1, adding 250 parts of deionized water, 2 parts of DOWFAX 2A1 and 1 part of LCN287 into a reaction kettle, adding 30 parts of nano mica powder after complete dissolution, uniformly dispersing, and heating to 80 ℃ to form a base material A;
s2, 6 parts of DOWFAX 2A1 and 2 parts of LCN287 are dissolved in 400 parts of deionized water, 280 parts of n-butyl acrylate, 200 parts of methyl methacrylate, 10 parts of acrylic acid, 20 parts of tert-butyl acrylate and 0.4 part of ethylene glycol dimethacrylate are added respectively to prepare a pre-emulsion B;
s3, 3 parts of ammonium persulfate is dissolved in 50 parts of deionized water to prepare an initiator solution C. Taking 4% by weight of the pre-emulsion B and 8% by weight of the initiator solution C, adding the pre-emulsion B into the bottom material A, and preserving heat at 85 ℃ for 25min to form flaky seed emulsion;
s4, dropwise adding the residual pre-emulsion B and the residual initiator solution C into the flaky seed emulsion, dropwise adding for 3 hours, keeping the temperature at 80 ℃, preserving the heat for 1 hour, cooling to 50 ℃, adding alkali liquor for neutralization, and then adding a defoaming agent with a conventional dosage and a preservative with a conventional dosage to obtain the modified emulsion.
Example 6
Example 6 differs from example 5 in that: the amount of t-butyl acrylate varies. Wherein the amount of t-butyl acrylate used in example 5 was 20 parts; in example 6, the amount of t-butyl acrylate was 30 parts.
The modified emulsion comprises the following components in parts by weight:
510 parts of unsaturated double bond-containing monomer;
0.4 parts of a crosslinking monomer;
20 parts of mica powder;
3 parts of an initiator;
8 parts of emulsifying agent;
deionized water, 700 parts;
the unsaturated double bond-containing monomer comprises 30 parts of tert-butyl acrylate.
The preparation of the modified emulsion comprises the following steps:
s1, adding 250 parts of deionized water, 2 parts of DOWFAX 2A1 and 1 part of LCN287 into a reaction kettle, adding 30 parts of nano mica powder after complete dissolution, uniformly dispersing, and heating to 80 ℃ to form a base material A;
s2, 6 parts of DOWFAX 2A1 and 2 parts of LCN287 are dissolved in 400 parts of deionized water, 280 parts of n-butyl acrylate, 200 parts of methyl methacrylate, 10 parts of acrylic acid, 30 parts of tert-butyl acrylate and 0.4 part of ethylene glycol dimethacrylate are added respectively to prepare a pre-emulsion B;
s3, 3 parts of ammonium persulfate is dissolved in 50 parts of deionized water to prepare an initiator solution C. Taking 4% by weight of the pre-emulsion B and 8% by weight of the initiator solution C, adding the pre-emulsion B into the bottom material A, and preserving heat at 85 ℃ for 25min to form flaky seed emulsion;
s4, dropwise adding the residual pre-emulsion B and the residual initiator solution C into the flaky seed emulsion, dropwise adding for 3 hours, keeping the temperature at 80 ℃, preserving the heat for 1 hour, cooling to 50 ℃, adding alkali liquor for neutralization, and then adding a defoaming agent with a conventional dosage and a preservative with a conventional dosage to obtain the modified emulsion.
Example 7
Example 7 differs from example 1 in that: in example 7, the crosslinking monomer ethylene glycol dimethacrylate of example 1 was replaced with diallyl phthalate.
The modified emulsion comprises the following components in parts by weight:
510 parts of unsaturated double bond-containing monomer;
0.4 parts of a crosslinking monomer;
20 parts of mica powder;
3 parts of an initiator;
8 parts of emulsifying agent;
deionized water, 700 parts;
the unsaturated double bond-containing monomer comprises 20 parts of tert-butyl acrylate.
The preparation of the modified emulsion comprises the following steps:
s1, adding 250 parts of deionized water, 2 parts of DOWFAX 2A1 and 1 part of LCN287 into a reaction kettle, adding 20 parts of nano mica powder after complete dissolution, uniformly dispersing, and heating to 80 ℃ to form a base material A;
s2, 6 parts of DOWFAX 2A1 and 2 parts of LCN287 are dissolved in 400 parts of deionized water, 280 parts of n-butyl acrylate, 200 parts of methyl methacrylate, 10 parts of acrylic acid, 20 parts of tert-butyl acrylate and 0.4 part of diallyl phthalate are respectively added to prepare a pre-emulsion B;
s3, 3 parts of ammonium persulfate is dissolved in 50 parts of deionized water to prepare an initiator solution C. Taking 4% by weight of the pre-emulsion B and 8% by weight of the initiator solution C, adding the pre-emulsion B into the bottom material A, and preserving heat at 85 ℃ for 25min to form flaky seed emulsion;
s4, dropwise adding the residual pre-emulsion B and the residual initiator solution C into the flaky seed emulsion, dropwise adding for 3 hours, keeping the temperature at 80 ℃, preserving the heat for 1 hour, cooling to 50 ℃, adding alkali liquor for neutralization, and then adding a defoaming agent with a conventional dosage and a preservative with a conventional dosage to obtain the modified emulsion.
Example 8
Example 8 differs from example 1 in that: in example 8, the emulsifier DOWFAX 2A1 of example 1 was replaced with sodium dodecylbenzenesulfonate.
The modified emulsion comprises the following components in parts by weight:
510 parts of unsaturated double bond-containing monomer;
0.4 parts of a crosslinking monomer;
20 parts of mica powder;
3 parts of an initiator;
8 parts of emulsifying agent;
deionized water, 700 parts;
the unsaturated double bond-containing monomer comprises 20 parts of tert-butyl acrylate.
The preparation of the modified emulsion comprises the following steps:
s1, adding 250 parts of deionized water, 2 parts of sodium dodecyl benzene sulfonate and 1 part of LCN287 into a reaction kettle, adding 20 parts of nano mica powder after complete dissolution, uniformly dispersing, and heating to 80 ℃ to form a base material A;
s2, 6 parts of sodium dodecyl benzene sulfonate and 2 parts of LCN287 are dissolved in 400 parts of deionized water, 280 parts of n-butyl acrylate, 200 parts of methyl methacrylate, 10 parts of acrylic acid, 20 parts of tert-butyl acrylate and 0.4 part of ethylene glycol dimethacrylate are added respectively to prepare a pre-emulsion B;
s3, 3 parts of ammonium persulfate is dissolved in 50 parts of deionized water to prepare an initiator solution C. Taking 4% by weight of the pre-emulsion B and 8% by weight of the initiator solution C, adding the pre-emulsion B into the bottom material A, and preserving heat at 85 ℃ for 25min to form flaky seed emulsion;
s4, dropwise adding the residual pre-emulsion B and the residual initiator solution C into the flaky seed emulsion, dropwise adding for 3 hours, keeping the temperature at 80 ℃, preserving the heat for 1 hour, cooling to 50 ℃, adding alkali liquor for neutralization, and then adding a defoaming agent with a conventional dosage and a preservative with a conventional dosage to obtain the modified emulsion.
Example 9
Example 9 differs from example 1 in that: in example 9, the initiator ammonium persulfate in example 1 was replaced with sodium persulfate.
The modified emulsion comprises the following components in parts by weight:
510 parts of unsaturated double bond-containing monomer;
0.4 parts of a crosslinking monomer;
20 parts of mica powder;
3 parts of an initiator;
8 parts of emulsifying agent;
deionized water, 700 parts;
the unsaturated double bond-containing monomer comprises 20 parts of tert-butyl acrylate.
The preparation of the modified emulsion comprises the following steps:
s1, adding 250 parts of deionized water, 2 parts of DOWFAX 2A1 and 1 part of LCN287 into a reaction kettle, adding 20 parts of nano mica powder after complete dissolution, uniformly dispersing, and heating to 80 ℃ to form a base material A;
s2, 6 parts of DOWFAX 2A1 and 2 parts of LCN287 are dissolved in 400 parts of deionized water, 280 parts of n-butyl acrylate, 200 parts of methyl methacrylate, 10 parts of acrylic acid, 20 parts of tert-butyl acrylate and 0.4 part of ethylene glycol dimethacrylate are added respectively to prepare a pre-emulsion B;
s3, 3 parts of sodium persulfate is dissolved in 50 parts of deionized water to prepare an initiator solution C. Taking 4% by weight of the pre-emulsion B and 8% by weight of the initiator solution C, adding the pre-emulsion B into the bottom material A, and preserving heat at 85 ℃ for 25min to form flaky seed emulsion;
s4, dropwise adding the residual pre-emulsion B and the residual initiator solution C into the flaky seed emulsion, dropwise adding for 3 hours, keeping the temperature at 80 ℃, preserving the heat for 1 hour, cooling to 50 ℃, adding alkali liquor for neutralization, and then adding a defoaming agent with a conventional dosage and a preservative with a conventional dosage to obtain the modified emulsion.
Comparative example 1
Comparative example 1 differs from example 1 in that: the mica powder was not contained in comparative example 1.
The modified emulsion comprises the following components in parts by weight:
510 parts of unsaturated double bond-containing monomer;
0.4 parts of a crosslinking monomer;
3 parts of an initiator;
8 parts of emulsifying agent;
deionized water, 700 parts;
the unsaturated double bond-containing monomer comprises 20 parts of tert-butyl acrylate.
The preparation of the modified emulsion comprises the following steps:
s1, adding 250 parts of deionized water, 2 parts of DOWFAX 2A1 and 1 part of LCN287 into a reaction kettle, and heating to 80 ℃ after complete dissolution to form a bottom material A;
s2, 6 parts of DOWFAX 2A1 and 2 parts of LCN287 are dissolved in 400 parts of deionized water, 280 parts of n-butyl acrylate, 200 parts of methyl methacrylate, 10 parts of acrylic acid, 20 parts of tert-butyl acrylate and 0.4 part of ethylene glycol dimethacrylate are added respectively to prepare a pre-emulsion B;
s3, 3 parts of ammonium persulfate is dissolved in 50 parts of deionized water to prepare an initiator solution C. Taking 4% by weight of the pre-emulsion B and 8% by weight of the initiator solution C, adding the pre-emulsion B into the bottom material A, and preserving heat at 85 ℃ for 25min to form flaky seed emulsion;
s4, dropwise adding the residual pre-emulsion B and the residual initiator solution C into the flaky seed emulsion, dropwise adding for 3 hours, keeping the temperature at 80 ℃, preserving the heat for 1 hour, cooling to 50 ℃, adding alkali liquor for neutralization, and then adding a defoaming agent with a conventional dosage and a preservative with a conventional dosage to obtain the modified emulsion.
Comparative example 2
Comparative example 2 differs from example 1 in that: comparative example 2 does not contain t-butyl acrylate.
The modified emulsion comprises the following components in parts by weight:
490 parts of unsaturated double bond-containing monomer;
0.4 parts of a crosslinking monomer;
20 parts of mica powder;
3 parts of an initiator;
8 parts of emulsifying agent;
deionized water, 700 parts.
The preparation of the modified emulsion comprises the following steps:
s1, adding 250 parts of deionized water, 2 parts of DOWFAX 2A1 and 1 part of LCN287 into a reaction kettle, adding 20 parts of nano mica powder after complete dissolution, uniformly dispersing, and heating to 80 ℃ to form a base material A;
s2, 6 parts of DOWFAX 2A1 and 2 parts of LCN287 are dissolved in 400 parts of deionized water, 280 parts of n-butyl acrylate, 200 parts of methyl methacrylate, 10 parts of acrylic acid and 0.4 part of ethylene glycol dimethacrylate are added respectively to prepare a pre-emulsion B;
s3, 3 parts of ammonium persulfate is dissolved in 50 parts of deionized water to prepare an initiator solution C. Taking 4% by weight of the pre-emulsion B and 8% by weight of the initiator solution C, adding the pre-emulsion B into the bottom material A, and preserving heat at 85 ℃ for 25min to form flaky seed emulsion;
s4, dropwise adding the residual pre-emulsion B and the residual initiator solution C into the flaky seed emulsion, dropwise adding for 3 hours, keeping the temperature at 80 ℃, preserving the heat for 1 hour, cooling to 50 ℃, adding alkali liquor for neutralization, and then adding a defoaming agent with a conventional dosage and a preservative with a conventional dosage to obtain the modified emulsion.
Performance test:
the emulsions obtained in examples 1 to 6 and comparative examples 1 to 2 were coated on white cardboard with a coating amount of 6 to 8g, and the coated films were tested for lipid resistance, water absorption (cobb value 10 min) and blocking resistance according to the group standard aqueous coated paper cup (aqueous coated paper cup paper) T/CPA 001-2021 test method, and the results are shown in table 1.
TABLE 1
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Wherein st=styrene;
mma=methyl methacrylate;
ba=n-butyl acrylate;
2-EHA = 2-ethylhexyl acrylate;
aa=acrylic acid;
t-ba=tert-butyl acrylate.
From table 1, it can be known that: it can be seen from examples 1-3 that the higher the TG of the emulsion, the progressively lower the lipid resistance, the progressively lower the Cobb, and the lower the blocking number, i.e. the higher the TG the lower the oil and water blocking properties and the improved anti-blocking properties.
Example 4 is compared with example 1, and shows that under the condition of adopting different main monomers and keeping other components unchanged, the barrier property and the anti-tackiness of the emulsion are not obviously changed like TG.
Example 5, comparative example 1, and example 1 are compared, demonstrating that nano-mica can significantly improve the blocking resistance.
Example 6 and example 5, and comparative example 2 and example 1, demonstrate that t-butyl acrylate can improve the water resistance of the emulsion.
Examples 7-9 replaced crosslinking monomer, emulsifier and initiator, respectively, and the application test results were substantially the same as in example 1, and the test results were not shown one by one in table 1 to avoid redundancy.
The foregoing is merely exemplary embodiments of the present invention and are not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention or direct or indirect application in the relevant art are intended to be included in the scope of the present invention.
Claims (10)
1. A modified emulsion characterized in that: the composition comprises the following components:
monomers containing unsaturated double bonds;
a crosslinking monomer;
mica powder;
an initiator;
an auxiliary agent;
water;
the unsaturated double bond-containing monomer comprises tert-butyl acrylate;
the glass transition temperature of the modified emulsion is less than 25 ℃.
2. A modified emulsion according to claim 1, characterized in that: the modified emulsion comprises the following components in parts by weight:
420-650 parts of unsaturated double bond-containing monomer;
0.05-1 part of crosslinking monomer;
10-50 parts of mica powder;
0.5-10 parts of initiator;
5-15 parts of an auxiliary agent;
400-800 parts of water.
3. A modified emulsion according to claim 2, characterized in that: the modified emulsion comprises the following components in parts by weight:
440-630 parts of unsaturated double bond-containing monomer;
0.1-0.9 part of crosslinking monomer;
15-45 parts of mica powder;
1-8 parts of an initiator;
6-14 parts of an auxiliary agent;
400-800 parts of water.
4. A modified emulsion according to claim 1, characterized in that: the unsaturated double bond-containing monomer further comprises at least one of styrene, methyl methacrylate, n-butyl acrylate, n-butyl methacrylate, isobutyl acrylate, 2-ethylhexyl acrylate, ethyl acrylate, acrylic acid, methacrylic acid and hydroxyethyl acrylate.
5. A modified emulsion according to claim 1, characterized in that: the crosslinking monomer comprises at least one of diallyl phthalate, N' N methylene bisacrylamide, ethylene glycol dimethacrylate, pentaerythritol triallyl ether, polyethylene glycol diacrylate, ethylene glycol dimethacrylate, trimethylolpropane trimethacrylate, diacetone acrylamide and adipic acid dihydrazide.
6. A modified emulsion according to claim 1, characterized in that: the initiator comprises at least one of potassium persulfate, sodium persulfate, ammonium persulfate, sodium bisulfite, vitamin C and tert-butyl hydroperoxide.
7. A modified emulsion according to claim 1, characterized in that: the auxiliary agent comprises an emulsifier, wherein the emulsifier comprises at least one of sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, DOWFAX 2A1, SR-10 Ai Dike, ER-10 Ai Dike, LCN287 Craien, COPS-1 Sodel and Tween 80.
8. A method of preparing a modified emulsion according to any one of claims 1 to 7, characterized in that: the method comprises the following steps:
s1, mixing mica powder and part of auxiliary agent in part of water to obtain a base material A;
s2, mixing a monomer containing unsaturated double bonds, a crosslinking monomer and the balance of auxiliary agent in the balance of water to obtain a pre-emulsion B;
s3, mixing the primer A, the pre-emulsion B and the initiator, and heating to obtain the modified emulsion.
9. The method according to claim 8, wherein: in step S3, the heating temperature is 80-90 ℃.
10. A coated white cardboard, characterized in that: a modified emulsion comprising the modified emulsion of any one of claims 1 to 7.
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