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Itaconic acid derivant for copolymerization of acrylonitrile

A technology of methylene succinic acid and derivatives, which is applied in the field of methylene succinic acid derivatives, can solve the problems of difficult mass transfer and poor guarantee of polymer structure uniformity, and achieve controllability Improved effect

Active Publication Date: 2010-07-07
KINGFA SCI & TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patents 02130021.6, 02130023.2, and 02130024.0 provide a method for passing ammonia gas into a homopolymer or a binary copolymer to indirectly obtain a terpolymer, although theoretically this method can obtain a polymerization with a uniform distribution of segment composition However, since the polymer solution is usually a very viscous system, this gas-liquid reaction is a complex heterogeneous reaction, the mass transfer is difficult, and the uniformity of the polymer structure cannot be well guaranteed.

Method used

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  • Itaconic acid derivant for copolymerization of acrylonitrile
  • Itaconic acid derivant for copolymerization of acrylonitrile
  • Itaconic acid derivant for copolymerization of acrylonitrile

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Add 0.1 mol itaconic anhydride and 0.105 mol ethanol into a 50 ml conical flask, place it on a 30 degree constant temperature shaker for 24 hours, and then add 15 ml ammonia to the flask and shake for 30 minutes. The product was distilled under reduced pressure at 60 degrees for 2 hours to obtain a white solid, namely methylene succinic acid derivative, with a yield of 98%.

Embodiment 2

[0021] Add 0.1 mol itaconic acid, 0.2 mol methanol, and 0.1 ml concentrated hydrochloric acid to a 50 ml three-necked flask, stir the reaction at 50 degrees for 2 hours, titrate the acid value of the reactant to the theoretical value, and remove excess methanol and residual hydrochloric acid under reduced pressure. Add 15ml ammonia water and shake for 30min. The product was distilled under reduced pressure at 60 degrees for 2 hours to obtain a white solid, namely methylene succinic acid derivative, with a yield of 95%.

Embodiment 3

[0023] Put 30g acrylonitrile, 0.6g methylene succinic acid derivative (Example 1), and 120g dimethyl sulfoxide into a 250ml reaction flask, let the nitrogen flow for 30 minutes and then keep the temperature at 50 degrees, add 0.15g azobisisoheptonitrile After reacting for 12 hours under the protection of nitrogen, the obtained binary copolymer has a viscosity average molecular weight of 160,000, a molecular weight distribution of 2.2, and a monomer conversion rate of 91%.

[0024]

[0025] Acrylonitrile (R 1 Is an alkyl group with 2 carbon atoms)

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Abstract

The invention discloses an itaconic acid derivant for copolymerization of acrylonitrile. The structural general formula (I) of the itaconic acid derivant is as follows: in the formula (I), R1 is alkyl. The itaconic acid derivant with both ester-base and ammonio is adopted as a comonomer for the acrylonitrile and the conventional ternary polymerization is replaced, so that the controllability of a copolymer is improved. The itaconic acid derivant is used for preparing high-performance PAN raw silks. In the copolymer of the acrylonitrile and the itaconic acid derivant, the mass ratio of the acrylonitrile is within 90 to 99.99%, and the mass ratio of the itaconic acid derivant is within 0.01 to 10%. The number-average molar mass of the copolymer is within 1 to 1 million.

Description

Technical field [0001] The invention relates to a methylene succinic acid derivative. Background technique [0002] Polyacrylonitrile-based carbon fiber has outstanding mechanical properties and is a hot spot in carbon fiber research in recent years. High-quality PAN precursor is the key to preparing high-performance PAN-based carbon fibers, and synthesis of high-quality acrylonitrile copolymer is the basis for obtaining high-quality polyacrylonitrile precursor. [0003] Acrylonitrile homopolymer has poor solubility, poor spinnability, and concentrated heat generation during pre-oxidation, which easily leads to fiber defects. In order to improve spinnability and lower the cyclization temperature, it is usually improved by adding other monomers to copolymerize. Common comonomers include methyl acrylate, methyl methacrylate, acrylamide, itaconic acid, and acrylic acid. It is generally believed that the addition of ester monomers can reduce the viscosity of the spinning solution and...

Claims

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Application Information

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IPC IPC(8): C07C69/593C07C67/08
Inventor 辛伟黄险波宋威代惊奇马雷黄有平
Owner KINGFA SCI & TECH CO LTD
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