Preparation method of particles of copolymer containing ethylene and vinyl alcohol structural units

A unit copolymer alcohol and structural unit technology, which is applied in the field of preparation of copolymer particles containing ethylene and vinyl alcohol structural units, can solve the problems of shape and size control, removal, high catalyst and by-products, and achieve separation efficiency improvement and reduction Effect of water consumption and improvement of product quality

Active Publication Date: 2014-08-13
BEIJING UNIV OF CHEM TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to solve the problem of shape and size control in the solid molding of the copolymer alcohol solution containing ethylene and vinyl alcohol structural units, and solve the problem of efficient removal of catalysts and by-products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Stir at 50°C (600 rev / min), carry out saponification or alcoholysis of ethylene-vinyl acetate copolymer in an alcoholic medium under the catalysis of sodium hydroxide, then add an aqueous solution containing 1.8% acetic acid at 80°C to obtain ethylene-vinyl alcohol 1.8L co-solution of copolymer (ethylene content 37mol%) / methanol / water / acetic acid and other components, wherein the mass ratio of ethylene-vinyl alcohol copolymer / methanol / water / acetic acid is 1:6.7:2.9:0.05. Adjust the temperature of the co-solution to 20°C, prepare granular ethylene-vinyl alcohol copolymer solids containing micropores within 10 minutes, with an average particle size of 1-3mm, and a micropore diameter of 0.007-0.03mm, and within 2 minutes Clear solvents and by-products can be separated. Under agitation, wash the copolymer particles containing micropores with water, and repeat once to clean the copolymer. The copolymer does not agglomerate during the drying process, dries quickly, and does ...

Embodiment 2

[0051] Stirring at 60°C (700 rpm), the preparation conditions of the copolymer / methanol / water solution are the same as in Example 1, except that an aqueous solution containing 1.5% acetic acid at 20°C is added to obtain ethylene-vinyl alcohol copolymer / methanol / water 1.7L co-solution of acetic acid and other components, wherein the mass ratio of ethylene-vinyl alcohol copolymer / methanol / water / acetic acid is 1:6.7:3.6:0.05. Adjust the temperature of the co-solution to 28°C, and add water (10°C) with a mass ratio of 1:1 to the copolymer to prepare a granular ethylene-vinyl alcohol copolymer solid containing micropores, with an average particle size of 2 ~4mm, the micropore diameter is 0.01~0.07mm, and the clear solvent and by-products can be separated within 2 minutes. The separation and washing method is the same as in Example 1, and achieves the same washing effect as in Example 1. The copolymer does not agglomerate during the drying process, dries quickly, and does not gener...

Embodiment 3

[0053] Stirring at 75°C (1000 rpm), the preparation conditions of the copolymer / methanol / water solution are the same as in Example 1, except that the aqueous solution containing 2.7% acetic acid at 20°C is added, wherein the ethylene-vinyl alcohol copolymer (ethylene content 38 %) / methanol / water / acetic acid mass ratio is 1:6.7:1.7:0.05. Adjust the temperature of the co-solution to 5°C, and add water (3°C) with a mass ratio of 0.2:1 to the copolymer to prepare a granular ethylene-vinyl alcohol copolymer solid containing micropores, with an average particle size of 0.3 ~2mm, micropore diameter is 0.006~0.02mm. The separation and washing method is the same as in Example 1, and achieves the same washing effect as in Example 1. The copolymer dries quickly and does not generate significant static electricity.

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Abstract

The invention relates to a preparation method of particles of a copolymer containing ethylene and vinyl alcohol structural units. The copolymer is an ethylene-vinyl alcohol bipolymer or an ethylene-vinyl alcohol-vinyl acetate terpolymer, and the method comprises the following steps: (1) preparing a copolymer / a solvent / a water solution, (2) preparing the particles of the copolymer, and (3) removing a residual catalyst in the particles of the copolymer. The effect of the preparation method is as follows: 1) solid particles of the copolymer which has uniform and adjustable particle size and internally contains micro channels can be obtained, the adjustable particle size is in the range of 0.1-10mm, and the micro pore diameter is 0.005-0.1mm. Compared with the prior art, filtration and separation are simple, the separation efficiency is improved by more than 30 times, and the drying process does not agglomerate, does not produce dust and static electricity; 2) by adjusting the process conditions, control on copolymer solid shape and size can be realized; and 3) the removal effect of catalyst residues and by-products can be improved, the times of washing is reduced, the water consumption is reduced by more than 1 / 3, the washing time is shortened to 1 / 10 or less, and the quality of the product is improved.

Description

technical field [0001] The invention relates to a method for preparing copolymer particles containing ethylene and vinyl alcohol structural units, in particular to a method for preparing copolymer solids containing micropores by direct precipitation of copolymer alcohol solutions containing ethylene and vinyl alcohol units particle method. Background technique [0002] Copolymers containing ethylene and vinyl alcohol structural units, such as ethylene-vinyl alcohol copolymer (EVOH for short) or ethylene-vinyl alcohol-vinyl acetate copolymer, etc., are a kind of ethylene polymer with excellent processing performance and vinyl alcohol polymer A polymer material with excellent gas barrier properties. This polymer material has the characteristics of excellent gas barrier properties, mechanical strength, stretchability, abrasion resistance, antistatic properties, solvent resistance, processability and transparency. It is widely used in packaging materials, textile materials, me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F210/02C08F218/08C08F8/00C08J9/28C08J3/14C08J3/09C08J3/07C08L23/08
Inventor 吴一弦华炜张树张佩君薛晓贤李铁慧段常青冯克
Owner BEIJING UNIV OF CHEM TECH
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