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Acetoacetyl modified ethylene-vinyl alcohol copolymer and preparation method thereof

A vinyl alcohol copolymer and acetoacetyl group technology is applied in the field of polymer chemical materials to achieve the effects of improving processability, good fresh-keeping and good water solubility

Inactive Publication Date: 2015-02-11
石家庄万尚医药科技有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] There is no report on modifying ethylene-vinyl alcohol copolymer with acetoacetyl group

Method used

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  • Acetoacetyl modified ethylene-vinyl alcohol copolymer and preparation method thereof
  • Acetoacetyl modified ethylene-vinyl alcohol copolymer and preparation method thereof
  • Acetoacetyl modified ethylene-vinyl alcohol copolymer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 50.0 g of ethylene-vinyl alcohol copolymer (EVOH) to 450 ml of dimethyl sulfoxide, heat and stir to dissolve. After the solution was cooled to room temperature, 0.1 ml of triethylamine was added dropwise to the reaction system, and then diketene (16 g, 0.190 mol) was added dropwise to the reaction system, and the dropwise was completed in 10 minutes. A large number of bubbles will be generated during the dropwise addition. After the dropwise addition, stir and react at room temperature for 8 hours. After the reaction, slowly add 3000ml butanone dropwise to the reaction solution, reflux for 2 hours after the dropwise addition, filter after cooling, and reflux the filter cake with butanone for 4 hours (400ml ×2), the resulting white powder was vacuum-dried at 80°C to obtain an acetoacetate-modified ethylene-vinyl alcohol copolymer with a mass of 49.6 g. Analysis by IR external standard method showed that the content of acetoacetyl group was 1.21mol / kg (the external s...

Embodiment 2

[0031]Add 50.0 g of ethylene-vinyl alcohol copolymer (EVOH) to 450 ml of dimethyl sulfoxide, heat and stir to dissolve. After dissolving, it was lowered to room temperature, and 0.1 ml of triethylamine was added dropwise to the reaction system, and then diketene (26 g, 0.309 mol) was added dropwise to the reaction system, and the dropwise was completed in 10 minutes. A large number of bubbles will be generated during the dropwise addition. After the dropwise addition, stir and react at room temperature for 8 hours. After the reaction, slowly add 3000ml butanone dropwise to the reaction solution, reflux for 2 hours after the dropwise addition, filter after cooling, and reflux the filter cake with butanone for 4 hours (400ml ×2), the resulting white powder was vacuum-dried at 80°C to obtain acetoacetyl-modified ethylene-vinyl alcohol copolymer with a mass of 53.6 g. According to IR external standard analysis, the content of acetoacetyl group was 2.20 mol / kg.

Embodiment 3

[0033] Add 50.0 g of ethylene-vinyl alcohol copolymer (EVOH) to 450 ml of dimethyl sulfoxide, heat and stir to dissolve. After the solution was cooled to room temperature, 0.1 ml of triethylamine was added dropwise to the reaction system, and then diketene (5.5 g, 0.065 mol) was added dropwise to the reaction system, and the dropwise was completed in 10 minutes. A large number of bubbles will be generated during the dropwise addition. After the dropwise addition, stir and react at room temperature for 8 hours. After the reaction, slowly add 3000ml butanone dropwise to the reaction solution, reflux for 2 hours after the dropwise addition, filter after cooling, and reflux the filter cake with butanone for 4 hours (400ml ×2), the resulting white powder was vacuum-dried at 80°C to obtain acetoacetyl-modified ethylene-vinyl alcohol copolymer with a mass of 46.2 g. The content of acetoacetyl group was 0.60 mol / kg by IR external standard analysis.

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Abstract

The invention discloses a preparation method of an acetoacetyl modified ethylene-vinyl alcohol copolymer. Commercial ethylene vinyl alcohol (EVOH) is used as a raw material, the ethylene content in the EVOH is 20%-40%, the vinyl alcohol content in the EVOH is 60%-80%, and by virtue of the modification by diketene, the acetoacetyl content in the obtained modified copolymer is 0.60-2.20mol / kg. The preparation method disclosed by the invention comprises the following two steps of: (1) dissolving the ethylene-vinyl alcohol copolymer in an organic solvent to react with the diketene under the catalytic action of an organic base; and (2) adding an organic solvent after the reaction is ended to precipitate the product. The acetoacetyl modified ethylene-vinyl alcohol copolymer obtained prepared the invention is white solid powder, and is good in product quality and water solubility.

Description

technical field [0001] The invention belongs to the field of polymer chemical materials, and in particular relates to an acetoacetyl-modified ethylene-vinyl alcohol copolymer and a preparation method thereof. Background technique [0002] The copolymer of ethylene and vinyl alcohol (EVOH) is composed of vinyl segment (E) and vinyl alcohol segment (VA), and its ratio is usually 20% to 40% of E segment and 60% to 80% of VA segment . Therefore, EVOH not only has the excellent gas barrier properties of polyvinyl alcohol, but also has the good moisture resistance and processability of polyethylene. Its most notable feature is its barrier effect on gas, which can effectively block the penetration of oxygen, carbon dioxide or nitrogen and other gases, so it is widely used as packaging materials for food, medicine, cosmetics and so on. In the use of air-filled packaging technology, EVOH resin can also effectively retain carbon dioxide or nitrogen used to protect products. EVOH re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F216/06C08F210/02C08F8/00
Inventor 李玮赵世炜霍竹林尚慕宏
Owner 石家庄万尚医药科技有限公司
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