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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 difficulty in mass transfer, and the uniformity of polymer structure cannot be well guaranteed, and achieves controllability. improved effect

Active Publication Date: 2012-05-30
KINGFA SCI & TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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
Comparison scheme
Effect test

Embodiment 1

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

Embodiment 2

[0021] Add 0.1mol of itaconic acid, 0.2mol of methanol, and 0.1ml of concentrated hydrochloric acid into a 50ml three-neck flask, stir and react at 50°C 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 of ammonia water and shake for 30min. The product was distilled under reduced pressure at 60°C for 2 hours to obtain a white solid which was a methylene succinic acid derivative with a yield of 95%.

Embodiment 3

[0023] Put 30g of acrylonitrile, 0.6g of methylene succinic acid derivative (Example 1), and 120g of dimethyl sulfoxide into a 250ml reaction flask, pass nitrogen for 30min and then keep the temperature at 50°C, add 0.15g of azobisisoheptanonitrile , reacted for 12 hours under the protection of nitrogen, and the obtained binary copolymer had a viscosity-average molecular weight of 160,000, a molecular weight distribution of 2.2, and a monomer conversion rate of 91%.

[0024]

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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 acopolymer 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 present invention relates to a kind of 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 precursors are the key to preparing high-performance PAN-based carbon fibers, and the synthesis of high-quality acrylonitrile copolymers is the basis for obtaining high-quality polyacrylonitrile precursors. [0003] Acrylonitrile homopolymer has poor solubility, poor spinnability, and concentrated heat release during pre-oxidation, which can easily lead to fiber defects. In order to improve the spinnability and reduce the cyclization temperature, it is usually improved by adding other monomers to copolymerize. Common comonomers include methyl acrylate, methyl methacrylate, acrylamide, itaconic acid, acrylic acid, etc. It is generally believed that the addition of ester monomers can reduce the v...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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