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Acrylonitrile ternary interpolymer and preparation method thereof

A technology of acrylonitrile copolymer and acrylonitrile, which is applied in the fields of fiber chemical characteristics, textiles and paper making, and can solve problems such as inability to solve exothermic peaks, exothermic peak widths, and lower cyclization temperatures

Active Publication Date: 2012-11-14
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • Acrylonitrile ternary interpolymer and preparation method thereof
  • Acrylonitrile ternary interpolymer 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 azobisisobutyronitrile at a weight ratio of 800:196:1.5:2.5:1, and replace with nitrogen three times at room temperature, Polymerize at 50°C for 10 hours, remove residual monomers and air bubbles in vacuum to obtain acrylonitrile / acrylamide / β-butyl itaconate terpolymer, which is confirmed to be the ternary structure by infrared spectroscopy and elemental analysis, m= 1235, n=10, k=20; the weight average molecular weight of the copolymer is 148,000, and the molecular weight distribution index is 2.22. Thermal analysis DSC shows exothermic onset temperature T 1 =213°C, exothermic end temperature T 2 =309°C, ΔT=T 2 -T 1 =96°C, the exothermic peak is broad.

Embodiment 2

[0019] Weigh dimethyl sulfoxide, acrylonitrile, acrylamide, β-butyl itaconate, and azobisisobutyronitrile at a weight ratio of 800:196:3:1:1, and replace the two with helium at room temperature. The second time, polymerize at 55°C for 16 hours, remove residual monomers and air bubbles in vacuum, and obtain acrylonitrile / acrylamide / β-butyl itaconate terpolymer, which is confirmed to be the ternary structure by infrared spectroscopy and elemental analysis. The weight average molecular weight of the copolymer is 132,000, m=1034, n=34, k=12, and the molecular weight distribution index is 2.39. Thermal analysis DSC shows exothermic onset temperature T 1 =216°C, exothermic end temperature T 2 =307°C, ΔT=T 2 -T 1 = 91°C.

Embodiment 3

[0021] Weigh dimethyl sulfoxide, acrylonitrile, acrylamide, β-ethyl itaconate, and azobisisobutyronitrile at a weight ratio of 800:196:2:2:1, and replace them with nitrogen four times at room temperature , polymerized at 60°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 =1016, n=15, k=15, the weight average molecular weight of the copolymer is 116,000, and the molecular weight distribution index is 2.47. 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 an acrylonitrile ternary interpolymer and a preparation method thereof, and mainly relates to a beta-itaconic acid ester-acrylamide-acrylonitrile ternary interpolymer. A general formula of the beta-itaconic acid ester-acrylamide-acrylonitrile ternary interpolymer is expressed in the specification, wherein m, n and k in the general formula respectively express a number in a range of 500 to 1999, a number in a range of 5 to 400 and a number in a range of 5 to 400. A weight average molecular weight of the beta-itaconic acid ester-acrylamide-acrylonitrile ternary interpolymer is in a range of 60000 to 149000 and a molecular weight distribution index is in a range of 2 to 3. The beta-itaconic acid ester-acrylamide-acrylonitrile ternary interpolymer can be utilized in the industrial production of high performance polyacrylonitrile spinning stock solutions.

Description

technical field [0001] The invention relates to a ternary acrylonitrile copolymer 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 high-performance carb...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/48C08F220/56C08F222/16D01F9/22
Inventor 周文乐吴粮华赵微微沈志刚
Owner CHINA PETROLEUM & CHEM CORP
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