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High molecular weight acrylonitrile terpolymer and preparation method thereof

A technology of acrylonitrile copolymer and acrylonitrile, which is applied to the chemical characteristics of fibers, textiles and papermaking, etc. It can solve the problems of narrow exothermic peak width, wide molecular weight distribution, and inability to solve exothermic peaks, and achieve high molecular weight and narrow molecular weight distribution. Effect

Active Publication Date: 2011-09-28
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

The reactivity rate of this monomer is close to that of acrylonitrile and it is a bifunctional monomer with the functions of unsaturated carboxylic acid and unsaturated carboxylic acid ester comonomer. Its purpose is to reduce the cyclization temperature, widen the exothermic peak, and improve Spinnability, but our experiments have proved that although the above characteristics can improve spinnability, the exothermic peak width is still relatively narrow, and the molecular weight distribution is wider during terpolymerization
The patent (application number: 200710056083.6) discloses the use of azobisisoheptanonitrile instead of azobisisobutyronitrile, adding a chain transfer agent, and adopting acrylonitrile / acrylate / itaconic acid (or acrylic acid, methacrylic acid), which can be prepared A copolymer with high molecular weight and narrow molecular weight distribution can be obtained, but the shortcoming of narrow exothermic peak cannot be solved

Method used

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  • High molecular weight acrylonitrile terpolymer and preparation method thereof
  • High molecular weight acrylonitrile terpolymer and preparation method thereof

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Experimental program
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Effect test

Embodiment 1

[0017] Weigh dimethyl sulfoxide, acrylonitrile, acrylamide, β-butyl itaconate, and azobisisoheptanonitrile at a weight ratio of 800:196:1.5:2.5:1, and replace with nitrogen three times at room temperature, Polymerize at 35°C for 24 hours, remove residual monomers and air bubbles under vacuum to obtain acrylonitrile / acrylamide / β-butyl itaconate terpolymer, which is confirmed to be the ternary structure by infrared spectroscopy and elemental analysis, m= 2778, n=30, k=50; the weight average molecular weight of the copolymer is 258,000, and the molecular weight distribution index is 1.72. Thermal analysis DSC shows exothermic onset temperature T 1 =215°C, exothermic end temperature T 2 =308°C, ΔT=T 2 -T 1 =93°C, with a broad exothermic peak.

Embodiment 2

[0019] Weigh dimethyl sulfoxide, acrylonitrile, acrylamide, β-butyl itaconate, and azobisisoheptanonitrile at a weight ratio of 800:196:3:1:1, and replace them with nitrogen four times at room temperature , polymerized at 40°C for 24 hours, vacuum removed residual monomers and air bubbles, and obtained acrylonitrile / acrylamide / β-butyl itaconate terpolymer, which was confirmed by infrared spectroscopy and elemental analysis to be the ternary structure, copolymerization The weight average molecular weight is 182,000, m=1995, n=75, k=25 and the molecular weight distribution index is 1.69. Thermal analysis DSC shows exothermic onset temperature T 1 =214℃, exothermic end temperature T 2 =304°C, ΔT=T 2 -T 1 = 90°C.

Embodiment 3

[0021] Weigh dimethyl sulfoxide, acrylonitrile, acrylamide, β-ethyl itaconate, and azobisisoheptanonitrile at a weight ratio of 800:196:2:2:1, and replace them with nitrogen five times at room temperature , polymerized at 50°C for 24 hours, vacuum removed residual monomers and air bubbles, and obtained acrylonitrile / acrylamide / β-ethyl itaconate terpolymer, which was confirmed by infrared spectroscopy and elemental analysis to be the ternary structure, m =1556, n=25, k=25 The weight average molecular weight of the copolymer is 156,000, and the molecular weight distribution index is 1.87. Thermal analysis DSC shows exothermic onset temperature T 1 =212°C, exothermic end temperature T 2 =306°C, ΔT=T 2 -T 1 = 94°C.

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Abstract

The invention relates to acrylonitrile terpolymer and a preparation method thereof, which mainly solves the problem that acrylonitrile / acrylamide / beta-acrylonitrileitaconic acid ester terpolymer is not related in the prior art. The general formula is shown as the description, wherein m=2,001-4,000; n=5-400; k=5-400; the weight-average molecular weight of the terpolymer is between 150,000 and 400,000; and the molecular weight distribution index is between 1.5 and 2.5. By the technical scheme of the terpolymer and the preparation method thereof, the problem is better solved, and the invention can be applied to industrial production of high performance polyacrylonitrile spinning solution.

Description

technical field [0001] The invention relates to a high molecular weight terpolymer of acrylonitrile and a preparation method thereof. Background technique [0002] Polyacrylonitrile (PAN)-based carbon fiber is a new type of material developed rapidly in the 1960s. It has both the inherent nature of carbon materials and the softness and processability of textile fibers. It is a new generation of new military and civilian materials. The key to the performance of carbon fiber lies in the quality of the raw silk. Carbon fiber manufacturers all over the world regard the production technology of polyacrylonitrile raw silk as the top secret technology for producing carbon fiber. It is precisely because of the backward production technology of polyacrylonitrile raw silk in China that the output and quality of carbon fiber are far behind the foreign level. Therefore, high-performance carbon fiber copolymer is the premise of producing high-performance carbon fiber. [0003] As a hig...

Claims

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Application Information

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IPC IPC(8): C08F220/48C08F220/56C08F222/16D01F9/22
Inventor 沈志刚屠晓萍吴粮华
Owner CHINA PETROLEUM & CHEM CORP
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