CN115991813A - Application of emulsifier in increasing molecular weight of ethylene-vinyl acetate copolymer emulsion - Google Patents
Application of emulsifier in increasing molecular weight of ethylene-vinyl acetate copolymer emulsion Download PDFInfo
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- CN115991813A CN115991813A CN202111221157.3A CN202111221157A CN115991813A CN 115991813 A CN115991813 A CN 115991813A CN 202111221157 A CN202111221157 A CN 202111221157A CN 115991813 A CN115991813 A CN 115991813A
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- Prior art keywords
- molecular weight
- ethylene
- vinyl acetate
- emulsifier
- acetate copolymer
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- 239000000839 emulsion Substances 0.000 title claims abstract description 25
- 239000003995 emulsifying agent Substances 0.000 title claims abstract description 12
- 239000005038 ethylene vinyl acetate Substances 0.000 title claims abstract description 11
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 title claims abstract description 11
- 239000012874 anionic emulsifier Substances 0.000 claims description 8
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims description 7
- 150000008051 alkyl sulfates Chemical class 0.000 claims description 7
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 6
- 239000005977 Ethylene Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- MOTZDAYCYVMXPC-UHFFFAOYSA-N dodecyl hydrogen sulfate Chemical compound CCCCCCCCCCCCOS(O)(=O)=O MOTZDAYCYVMXPC-UHFFFAOYSA-N 0.000 claims description 4
- 229940043264 dodecyl sulfate Drugs 0.000 claims description 4
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000007334 copolymerization reaction Methods 0.000 claims description 2
- 239000000178 monomer Substances 0.000 claims description 2
- -1 alkyl sulphate Chemical compound 0.000 claims 1
- 229910021653 sulphate ion Inorganic materials 0.000 claims 1
- 229920002689 polyvinyl acetate Polymers 0.000 abstract description 2
- 239000011118 polyvinyl acetate Substances 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 5
- 229910021641 deionized water Inorganic materials 0.000 description 5
- 229920000642 polymer Polymers 0.000 description 5
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 4
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 4
- 239000007800 oxidant agent Substances 0.000 description 4
- 230000001590 oxidative effect Effects 0.000 description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 239000012065 filter cake Substances 0.000 description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 description 2
- 239000004289 sodium hydrogen sulphite Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 238000000944 Soxhlet extraction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000006136 alcoholysis reaction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229920006158 high molecular weight polymer Polymers 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
Landscapes
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention belongs to the technical field of polyvinyl acetate, and particularly relates to application of an emulsifier in improving molecular weight of ethylene-vinyl acetate copolymer emulsion. The invention obviously improves the molecular weight of the prepared emulsion through the emulsifier.
Description
Technical Field
The invention belongs to the technical field of polyvinyl acetate, and particularly relates to application of an emulsifier in improving molecular weight of ethylene-vinyl acetate copolymer emulsion.
Background
The VAE emulsion is a polymer emulsion formed by copolymerizing vinyl acetate and ethylene. The VAE emulsion has permanent flexibility, good adhesion, acid and alkali resistance and ultraviolet aging resistance, and is widely applied to the fields of buildings, building materials, cigarette adhesives, coatings and the like ("VAE emulsion environmental protection research progress", zhang Bianhua, management and science and technology of middle and small enterprises, 8 th period of 2017, 92 th left column, 1 st section, 1 st to 4 th line, public date 2017, 4 months and 25 days).
Molecular weight is an important structural parameter of the polymer chain. Research has shown that molecular weight has a significant impact on many important properties of high molecular weight polymers, such as rheological properties. In general, the higher the molecular weight, the worse the flowability of the polymer, and the higher the viscosity (the "relationship between the melt viscosity of the polymer and the molecular weight", xu Aide, etc., the polymer science and engineering, 1994, 1 st edition, 137 th page, 1 st paragraph, 1 st line to 2 nd paragraph, 3 rd line, publication date, 1994, 1 month, 31 th day).
However, existing VAE emulsions have relatively low molecular weights and viscosity average molecular weights of 20-24 ten thousand.
Disclosure of Invention
In view of the above, the present invention aims to provide the use of an emulsifier for increasing the molecular weight of an ethylene-vinyl acetate copolymer emulsion.
Unless otherwise specified, the parts in the invention are all parts by mass.
In order to solve the technical problems, the inventor conducts intensive research, and discovers that the emulsifier can obviously improve the molecular weight of the prepared ethylene-vinyl acetate copolymer emulsion in the research process.
The present invention is therefore aimed at protecting the use of emulsifiers for increasing the molecular weight of ethylene-vinyl acetate copolymer emulsions.
Further, the emulsifier comprises an anionic emulsifier.
Further, the anionic emulsifier comprises an alkyl sulfate.
Further, the alkyl sulfate includes dodecyl sulfate.
Further, the molecular weight is a viscosity average molecular weight.
The invention also aims at protecting the preparation method of the ethylene-vinyl acetate copolymer emulsion, which is prepared by copolymerizing vinyl acetate and ethylene serving as monomers, and adding an anionic emulsifier in the copolymerization process.
Further, the anionic emulsifier comprises an alkyl sulfate.
Further, the alkyl sulfate includes dodecyl sulfate.
The invention has the beneficial effects that:
the invention obviously improves the molecular weight of the prepared emulsion through the emulsifying agent.
The emulsion of the invention does not contain organic solvent, is nontoxic and harmless, and is safe and environment-friendly.
Detailed Description
The examples are presented for better illustration of the present invention, but are not intended to limit the scope of the present invention to the examples. Those skilled in the art will appreciate that various modifications and adaptations of the embodiments described above are possible in light of the above teachings and are intended to be within the scope of the invention.
In the invention, the detection method of the viscosity average molecular weight comprises the following steps: weighing 25g of a sample to be measured in a 100ml beaker, adding 50g of 10wt% potassium sulfate solution, and uniformly stirring; standing for 15min after emulsion breaking of the emulsion particles, carrying out suction filtration, washing a filter cake with 100mL of deionized water, repeatedly washing for 3 times, transferring the filter cake into a 500mL triangular flask, adding 300mL of water, and extracting in a water bath at 90 ℃ for 24h; filtering the liquid, weighing 1g of filter cake, adding 100g of acetone, and refluxing in a Soxhlet extraction tube for 72 hours; after the extract was filtered, the viscosity average molecular weight was measured by a multipoint method using a Ubbelohde viscometer at 25 ℃.
Example 1
The ethylene-vinyl acetate copolymer emulsion comprises the following raw materials:
50 parts of vinyl acetate, and the mixture is prepared from,
a proper amount of ethylene,
2.0 parts of polyvinyl alcohol (polymerization degree 1700, alcoholysis degree 85-90% mol/mol),
0.3 part of sodium dodecyl sulfate,
0.2 part of reducing agent sodium bisulphite,
3.46 parts of oxidant hydrogen peroxide (the concentration is 1.8%wt),
and proper amount of deionized water.
The preparation method of the emulsion is as follows
A. Raw material preparation
1) Preparing an oxidant solution: uniformly mixing 3.4 parts of deionized water and 3.46 parts of hydrogen peroxide with the concentration of 1.8 wt%;
2) Preparing a protective colloid solution: 2.0 parts of polyvinyl alcohol, 0.3 part of sodium dodecyl sulfate and 30 parts of deionized water are poured into a reaction kettle, stirred for 15min, heated to 80 ℃ and stirred for 30min again, so that the polyvinyl alcohol is dissolved;
B. feeding production
Pumping the prepared protective colloid emulsion, 0.2 part of sodium bisulphite and 6.6 parts of deionized water into a reaction kettle, pumping 12.5 parts of vinyl acetate into the reaction kettle, uniformly stirring, adding ethylene and boosting the pressure to 2.0MPa;
heating, when the temperature is increased to 50 ℃, beginning to dropwise add the oxidant solution, when the temperature reaches 72 ℃ and the pressure reaches 3.00MPa, dropwise adding the rest vinyl acetate at a constant speed within 2 hours, and preserving heat;
cutting off ethylene after the vinyl acetate is added;
controlling the rest oxidant solution to be dripped at a constant speed within 40 min;
cooling to 60 ℃, defoaming, filtering, cooling and discharging.
The product prepared in this example was in the form of an emulsion with a viscosity average molecular weight of 28 ten thousand.
Comparative example 1
The difference between this comparative example and example 1 is that: the raw materials do not contain sodium dodecyl sulfate, and sodium dodecyl sulfate is not added in the polymerization process.
The product prepared in this comparative example was in the form of emulsion with a viscosity average molecular weight of 22 ten thousand.
Furthermore, it should be understood that although the present disclosure describes embodiments, not every embodiment is provided with a separate embodiment, and that this description is provided for clarity only, and that the disclosure is not limited to the embodiments described in detail below, and that the embodiments described in the examples may be combined as appropriate to form other embodiments that will be apparent to those skilled in the art.
Claims (8)
1. The use of an emulsifier to increase the molecular weight of an ethylene-vinyl acetate copolymer emulsion.
2. The use according to claim 1, wherein the emulsifier comprises an anionic emulsifier.
3. The use according to claim 2, wherein the anionic emulsifier comprises an alkyl sulphate.
4. The use according to claim 3, wherein the alkyl sulfate comprises dodecyl sulfate.
5. The use according to any one of claims 1 to 4, wherein the molecular weight is a viscosity average molecular weight.
6. The preparation process of ethylene-vinyl acetate copolymer emulsion includes copolymerizing vinyl acetate and ethylene as monomer, and features that during the copolymerization, anionic emulsifier is added.
7. The method of claim 6, wherein the anionic emulsifier comprises an alkyl sulfate.
8. The method of claim 7, wherein the alkyl sulfate comprises dodecyl sulfate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111221157.3A CN115991813A (en) | 2021-10-20 | 2021-10-20 | Application of emulsifier in increasing molecular weight of ethylene-vinyl acetate copolymer emulsion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111221157.3A CN115991813A (en) | 2021-10-20 | 2021-10-20 | Application of emulsifier in increasing molecular weight of ethylene-vinyl acetate copolymer emulsion |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115991813A true CN115991813A (en) | 2023-04-21 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111221157.3A Pending CN115991813A (en) | 2021-10-20 | 2021-10-20 | Application of emulsifier in increasing molecular weight of ethylene-vinyl acetate copolymer emulsion |
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1425831A (en) * | 1964-03-03 | 1966-01-24 | Grace W R & Co | Emulsion polymerization of vinyl acetate using an anionic emulsifier and a peroxide catalyst |
| CN1306015A (en) * | 2000-12-27 | 2001-08-01 | 中国科学院长春应用化学研究所 | Process for preparing high-ethylene ethylene vinylacetate latex |
| CN102030858A (en) * | 2009-09-30 | 2011-04-27 | 中国石油化工集团公司 | Vinyl acetate-ethylene copolymer emulsion (VAE emulsion) and synthesis method thereof |
| CN103140514A (en) * | 2010-08-02 | 2013-06-05 | 瓦克化学股份公司 | Process for preparing vinyl acetate-ethylene copolymers by means of emulsion polymerization |
| CN103665231A (en) * | 2012-09-10 | 2014-03-26 | 中国石油化工集团公司 | Vinyl acetate-ethylene-vinyl versatate copolymer emulsion and synthesis method thereof |
| WO2014052144A1 (en) * | 2012-09-26 | 2014-04-03 | Wacker Chemical Corporation | Process for the preparation of an aqueous emulsifier-stabilized vinyl acetate-ethylene copolymer dispersion with fine particles size |
-
2021
- 2021-10-20 CN CN202111221157.3A patent/CN115991813A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR1425831A (en) * | 1964-03-03 | 1966-01-24 | Grace W R & Co | Emulsion polymerization of vinyl acetate using an anionic emulsifier and a peroxide catalyst |
| CN1306015A (en) * | 2000-12-27 | 2001-08-01 | 中国科学院长春应用化学研究所 | Process for preparing high-ethylene ethylene vinylacetate latex |
| CN102030858A (en) * | 2009-09-30 | 2011-04-27 | 中国石油化工集团公司 | Vinyl acetate-ethylene copolymer emulsion (VAE emulsion) and synthesis method thereof |
| CN103140514A (en) * | 2010-08-02 | 2013-06-05 | 瓦克化学股份公司 | Process for preparing vinyl acetate-ethylene copolymers by means of emulsion polymerization |
| CN103665231A (en) * | 2012-09-10 | 2014-03-26 | 中国石油化工集团公司 | Vinyl acetate-ethylene-vinyl versatate copolymer emulsion and synthesis method thereof |
| WO2014052144A1 (en) * | 2012-09-26 | 2014-04-03 | Wacker Chemical Corporation | Process for the preparation of an aqueous emulsifier-stabilized vinyl acetate-ethylene copolymer dispersion with fine particles size |
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