CN115991814A - Application of increasing monomer concentration in micelle in increasing molecular weight of ethylene-vinyl acetate copolymer emulsion - Google Patents
Application of increasing monomer concentration in micelle in increasing molecular weight of ethylene-vinyl acetate copolymer emulsion Download PDFInfo
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- CN115991814A CN115991814A CN202111221244.9A CN202111221244A CN115991814A CN 115991814 A CN115991814 A CN 115991814A CN 202111221244 A CN202111221244 A CN 202111221244A CN 115991814 A CN115991814 A CN 115991814A
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- Prior art keywords
- vinyl acetate
- molecular weight
- ethylene
- increasing
- copolymer emulsion
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- 239000000839 emulsion Substances 0.000 title claims abstract description 27
- 239000005038 ethylene vinyl acetate Substances 0.000 title claims abstract description 18
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 title claims abstract description 18
- 239000000178 monomer Substances 0.000 title claims abstract description 15
- 239000000693 micelle Substances 0.000 title claims abstract description 9
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 claims abstract description 17
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 5
- 239000005977 Ethylene Substances 0.000 claims description 5
- 238000006116 polymerization reaction Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000007334 copolymerization reaction Methods 0.000 claims 1
- 229920000642 polymer Polymers 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 239000012065 filter cake Substances 0.000 description 6
- 239000004372 Polyvinyl alcohol Substances 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 239000007800 oxidant agent Substances 0.000 description 5
- 230000001590 oxidative effect Effects 0.000 description 5
- 229920002451 polyvinyl alcohol Polymers 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 238000000944 Soxhlet extraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 229940017705 formaldehyde sulfoxylate Drugs 0.000 description 2
- SBGKURINHGJRFN-UHFFFAOYSA-N hydroxymethanesulfinic acid Chemical compound OCS(O)=O SBGKURINHGJRFN-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 2
- 229910052939 potassium sulfate Inorganic materials 0.000 description 2
- 235000011151 potassium sulphates Nutrition 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 230000006978 adaptation Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000006136 alcoholysis reaction Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000011895 specific detection Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
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- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention belongs to the technical field of vinyl acetate polymers, and particularly relates to an application of increasing monomer concentration in micelles in increasing molecular weight of ethylene-vinyl acetate copolymer emulsion. The invention obviously improves the molecular weight of the prepared ethylene-vinyl acetate copolymer emulsion by improving the monomer concentration.
Description
Technical Field
The invention belongs to the technical field of vinyl acetate polymers, and particularly relates to an application of increasing monomer concentration in micelles in increasing molecular weight of ethylene-vinyl acetate copolymer emulsion.
Background
The EVA emulsion has the advantages of internal plasticity, alkali resistance, creep resistance, wettability, adhesiveness, high temperature resistance, storage stability, good compatibility with other chemicals and the like, and is mainly used in the fields of adhesives, coatings, packaging, carpet backing, wallpaper coatings and the like ("modification and application of EVA emulsion", zhang Xinya and the like, rubber industry, 2003, 50 th coil 6, 379 left column 3 rd section 1 line to right column 1 st line, publication date 2003, 12 months 31 days, "modification and application of EVA emulsion", zhang Jiangbin, printing and dyeing auxiliary, 1998, 15 th coil 6, 29 left column 1 st line to 2 nd section 12 line, 1998, publication date 12 months 31 days).
However, the viscosity average molecular weight of existing VAE emulsions is relatively low, ranging from 20 to 24 tens of thousands.
Disclosure of Invention
In view of the above, the present invention aims to provide an application of increasing the monomer concentration in micelles in increasing the molecular weight of an ethylene-vinyl acetate copolymer emulsion.
In order to solve the technical problems, the inventor has conducted intensive research, and found that increasing the monomer concentration during polymerization can significantly increase the molecular weight of the ethylene-vinyl acetate copolymer emulsion.
Therefore, the invention aims to protect the application of increasing the monomer concentration in the micelle in increasing the molecular weight of the ethylene-vinyl acetate copolymer emulsion.
The monomer concentration in the micelle refers to the content of vinyl acetate in the polyvinyl alcohol micelle.
Further, the monomer includes a vinyl acetate monomer.
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 as monomers, wherein the initial use amount of the vinyl acetate is 40-50 wt% in the polymerization process, and the residual vinyl acetate is dropwise added at a constant speed within 30-35 minutes.
The invention has the beneficial effects that:
the invention effectively improves the viscosity average molecular weight of the ethylene-vinyl acetate copolymer emulsion by improving the monomer concentration in the polymerization process.
The invention obviously improves the viscosity average molecular weight of the ethylene-vinyl acetate copolymer emulsion, thereby improving the viscosity of the ethylene-vinyl acetate copolymer emulsion and meeting the application requirements of the fields of wood, plastics and the like.
The method is simple, does not need to change the existing process route, and is beneficial to industrial production.
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; after emulsion breaking, standing for 15min, 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 for 24h in a water bath at 90 ℃; filtering the liquid, weighing 1g of filter cake, adding 100g of acetone, and refluxing in a Soxhlet extraction tube for 72 hours; filtering the extract, and testing the viscosity average molecular weight by using a viscosity method. The specific detection method 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 is prepared from 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),
formaldehyde sulfoxylate or 0.2 part;
3.46 parts of hydrogen peroxide (with the concentration of 1.8 percent by weight),
and proper amount of deionized water.
The preparation method of the copolymer emulsion comprises the following specific steps:
A. preparation of raw materials
1) Preparing an oxidant solution system: adding 4.4 parts of deionized water and 3.46 parts of oxidant into the oxidant tank, and uniformly stirring;
2) Preparing polyvinyl alcohol emulsion: 2.0 parts of polyvinyl alcohol and 40 parts of deionized water are weighed and poured into a reaction kettle, stirred for 15 minutes at normal temperature, then heated to 80 ℃ and dissolved for 30 minutes at the temperature;
B. feeding production
Pumping polyvinyl alcohol emulsion, formaldehyde sulfoxylate 0.2 parts and deionized water 5.6 parts into a reaction kettle, pumping vinyl acetate (initial dosage) accounting for 50% of the total amount into the reaction kettle, uniformly stirring, adding ethylene and boosting to a set pressure of 3.0MPa;
heating the reaction kettle, dropwise adding an oxidant solution when the temperature is increased to 60 ℃, and dropwise adding the rest vinyl acetate at a constant speed within 25 minutes when the temperature in the reaction kettle reaches 72 ℃ and the pressure reaches 5.0MPa, wherein the temperature of the reaction kettle is controlled at 72 ℃;
cutting off ethylene after the addition of the vinyl acetate is completed;
and (3) controlling the rest oxidant solution to drop completely at a constant speed within 45min, cooling to 60 ℃, defoaming, filtering, cooling and discharging to obtain the emulsion.
Comparative example 1
This comparative example was the same as the other parameter settings of example 1 except that the initial amount of vinyl acetate was 20% (mass ratio) and the constant-speed dropping time of the remaining vinyl acetate was 120 minutes.
Performance detection
The viscosity average molecular weight of the emulsions obtained in example 1 and comparative example 1 was measured, and the results are shown in Table 1.
TABLE 1 Performance test results
| Source | Viscosity average molecular weight |
| Example 1 | 45 ten thousand (ten thousand) |
| Comparative example 1 | 26 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 (4)
1. The application of increasing the monomer concentration in the micelle in increasing the molecular weight of the ethylene-vinyl acetate copolymer emulsion.
2. The use of claim 1, wherein the monomer comprises a vinyl acetate monomer.
3. The use according to claim 1 or 2, wherein the molecular weight is a viscosity average molecular weight.
4. The preparation method of the ethylene-vinyl acetate copolymer emulsion takes vinyl acetate and ethylene as monomers and is obtained by copolymerization, and is characterized in that the initial use amount of the vinyl acetate is 40-50 wt% in the polymerization process, and the residual vinyl acetate is dropwise added at a constant speed within 30-35 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111221244.9A CN115991814A (en) | 2021-10-20 | 2021-10-20 | Application of increasing monomer concentration in micelle in increasing molecular weight of ethylene-vinyl acetate copolymer emulsion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111221244.9A CN115991814A (en) | 2021-10-20 | 2021-10-20 | Application of increasing monomer concentration in micelle in increasing molecular weight of ethylene-vinyl acetate copolymer emulsion |
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| Publication Number | Publication Date |
|---|---|
| CN115991814A true CN115991814A (en) | 2023-04-21 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111221244.9A Pending CN115991814A (en) | 2021-10-20 | 2021-10-20 | Application of increasing monomer concentration in micelle in increasing molecular weight of ethylene-vinyl acetate copolymer emulsion |
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| Country | Link |
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| CN (1) | CN115991814A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02274707A (en) * | 1989-03-23 | 1990-11-08 | Air Prod And Chem Inc | Manufacture of high-solid emulsion of vinyl acetate/ethylene copolymer containing water-soluble monomer |
| JPH04272902A (en) * | 1990-11-07 | 1992-09-29 | Air Prod And Chem Inc | Vinyl acetate/ethylene copolymer emulsion improved in wet viscosity |
| CN103626910A (en) * | 2013-11-29 | 2014-03-12 | 西南化工研究设计院有限公司 | Solid ethylene-vinyl acetate copolymer and preparation method thereof |
| CN109651556A (en) * | 2017-10-11 | 2019-04-19 | 中国石油化工集团公司 | Monodisperse vinyl acetate-ethylene copolymerization emulsions and preparation method thereof |
-
2021
- 2021-10-20 CN CN202111221244.9A patent/CN115991814A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02274707A (en) * | 1989-03-23 | 1990-11-08 | Air Prod And Chem Inc | Manufacture of high-solid emulsion of vinyl acetate/ethylene copolymer containing water-soluble monomer |
| JPH04272902A (en) * | 1990-11-07 | 1992-09-29 | Air Prod And Chem Inc | Vinyl acetate/ethylene copolymer emulsion improved in wet viscosity |
| CN103626910A (en) * | 2013-11-29 | 2014-03-12 | 西南化工研究设计院有限公司 | Solid ethylene-vinyl acetate copolymer and preparation method thereof |
| CN109651556A (en) * | 2017-10-11 | 2019-04-19 | 中国石油化工集团公司 | Monodisperse vinyl acetate-ethylene copolymerization emulsions and preparation method thereof |
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