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Preparation method of acrylic nitrile homopolymer (copolymer)

A technology of acrylonitrile and copolymer, which is applied in the field of preparation of acrylonitrile homopolymer to achieve the effect of high yield and easy storage

Inactive Publication Date: 2007-05-16
CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Based on the above studies, the three most important controllable / living free radical polymerization methods (ATRP, NMP and RAFT) have been used to regulate the polymerization of acrylonitrile, but the maximum number average molecular weight of the obtained polymer is limited to about 50,000

Method used

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  • Preparation method of acrylic nitrile homopolymer (copolymer)
  • Preparation method of acrylic nitrile homopolymer (copolymer)

Examples

Experimental program
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Effect test

Embodiment 1

[0027] The preparation of embodiment 1 acrylonitrile homopolymer

[0028] The first step preparation of dithiobenzoyl dithio

[0029] 12.6 grams of benzyl chloride were added dropwise to the system containing 6.4 grams of sulfur, 10 grams of sodium methylate, and 70 grams of methanol within one hour using a dropping funnel. The resulting brown solution was heated to 80° C. and refluxed overnight. After cooling to room temperature, the mixture was filtered to remove white sodium chloride solid, and then methanol was removed on a rotary evaporator. The resulting solid was redissolved in 100 ml of distilled water and washed three times with ether (3 x 50 ml). Add 50ml of diethyl ether to the solution, acidify the biphasic mixture with 30% hydrochloric acid until the aqueous layer loses its characteristic brown color and the upper layer appears dark purple, separate the ether layer solution, add 120ml of distilled water, and extract disulfide with 240ml of 30% sodium hydroxide s...

Embodiment 2

[0034] The preparation of embodiment 2 acrylonitrile homopolymer

[0035] The first step preparation of dithiophenylacetyl dithio

[0036] In a three-neck flask with a reflux condenser and a dropping funnel, under nitrogen protection, add 7.7 grams of magnesium chips, 150 ml of anhydrous ether, and drop 40 grams of benzyl chloride into the system within 30 minutes under an ice-water bath , continued to stir for 1 hour, and then refluxed for 0.5 hours. After cooling, 24 g of carbon disulfide was added dropwise within 15 minutes at 0° C., and the reaction was continued for 3 hours. The mixture was poured into 150 ml of ice water, the organic layer was separated, and the aqueous layer was washed three times with ether (3 x 50 ml). The aqueous layer was acidified with 30% hydrochloric acid and extracted with ether until it became colorless, and the ether layer solutions were combined. 100 ml of distilled water was added, extracted with 30% sodium hydroxide solution, and washed ...

Embodiment 3

[0039] The preparation of embodiment 3 acrylonitrile homopolymer

[0040] With 2.5mg of azobisisobutyronitrile, 5.1mg of dithiophenylacetyl disulfide replaces azobisisobutyronitrile and dithiophenylacetyl dithio in Example 2, and others are the same as in Example 2, 0.5 g of acrylonitrile homopolymer was obtained, and the monomer conversion rate was 61.7%. As determined by GPC, the number average molecular weight of the acrylonitrile homopolymer was 212,000, and the molecular weight distribution was 1.72.

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Abstract

The invention discloses a preparing method of acrylon even (co-) polymer with high molecule and narrow molecular distribution, which is characterized by the following: the carbamodithioic material can be moduling agent of free acrylon radical, wherein Z is phenyl or benzyl, which can produce RAFT chain transmitting agent acted by azo-diisobutyronitrile at original position, which copolymerizes acrylon with other monomers; when Z is benzyl, the number average molecular weight is about 230000 with molecular distribution under 2.0 (1.70 as minimum value).

Description

technical field [0001] The invention relates to a method for preparing an acrylonitrile homopolymer (co)polymer, in particular to a method for preparing an acrylonitrile homopolymer or copolymer with high molecular weight and narrow molecular weight distribution. technical background [0002] Because polyacrylonitrile has excellent properties such as good hardness and strength, good chemical resistance, excellent compatibility with polar substances, and low air tightness, the polymer plays an important role in industry. An important commercial polymer, especially for carbon fibers. at the same time. This also makes many polymer chemists and research groups have been full of strong interest in the synthesis of polyacrylonitrile with clear structure (controllable molecular size and molecular weight distribution). However, the living / controlled free-radical polymerization of acrylonitrile represents a particular challenge because of its high reactivity and the poor solubility...

Claims

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Application Information

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IPC IPC(8): C08F20/44C08F2/38C08K5/372
Inventor 李悦生刘晓辉张贵宝李百祥
Owner CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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