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Method for preparing isotactic polyacrylonitrile and application thereof

An isotactic, polyacrylonitrile technology, which is applied in the field of preparing isotactic polyacrylonitrile, can solve the problems of low isotacticity of polyacrylonitrile triads, and achieves improved stereoregularity, Keep the arrangement neat

Active Publication Date: 2014-04-16
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Chen Hou et al. (201010603348) applied for a patent to prepare polyacrylonitrile with triad isotacticity of 0.35~0.42 by atom transfer radical active polymerization method using electron transfer regeneration catalyst, and the polyacrylonitrile synthesized by this method Acrylonitrile triads have low isotacticity

Method used

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  • Method for preparing isotactic polyacrylonitrile and application thereof
  • Method for preparing isotactic polyacrylonitrile and application thereof
  • Method for preparing isotactic polyacrylonitrile and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Mix 2.2 grams of 280um urea (produced by Sinopharm Group) and 0.8 ml of acrylonitrile (produced by Sinopharm Group) into the reaction bottle (ratio of substances: acrylonitrile: urea = 1:3), and freeze at -60 degrees Celsius for 150 hour, add liquid nitrogen in the reaction bottle afterwards, carry out gamma ray irradiation, the irradiation dose is 28.8kGy, after the irradiation, the reaction bottle is moved into the environment of -60 degrees Celsius, and the nitrogen gas of -60 degrees Celsius is passed into the reaction bottle, The flow rate was 400 L / h, and after the polymerization was carried out for 4 hours, it was repeatedly washed with water, filtered, and dried.

[0035] The polymerization yield is 48%, and the number-average molecular weight of the obtained isotactic polyacrylonitrile is 30580, and the molecular weight distribution is 1.28, and the three-unit isotacticity is 98% (see figure 1 ).

[0036] The abscissa in the figure is the chemical shift (ppm),...

Embodiment 2

[0038] Mix 2.2 grams of 150um urea (produced by Sinopharm Group) and 0.8 ml of acrylonitrile (produced by Sinopharm Group) into the reaction bottle (ratio of substances: acrylonitrile: urea = 1:3), and freeze at -45 degrees Celsius for 100 After that, liquid nitrogen was added to the reaction bottle, and Co60γ-ray irradiation was carried out. The irradiation dose was 72kGy. After the irradiation, the reaction bottle was moved into the environment of -110 degrees Celsius, and the nitrogen gas of -110 degrees Celsius was passed into the reaction bottle. After polymerization at 300 L / h for 8 hours, washing with water, filtration, and drying were repeated.

[0039] The polymerization yield is 68%, and the number-average molecular weight of the obtained isotactic polyacrylonitrile is 19470, and the molecular weight distribution is 1.41, and the three-unit isotacticity is 99% (see figure 2 ).

Embodiment 3

[0041] Mix 0.61 g of 150um urea (produced by Sinopharm Group) and 0.8 ml of acrylonitrile (produced by Sinopharm Group) into the reaction bottle (ratio of substances: acrylonitrile: urea = 1:0.83), freeze at -60 degrees Celsius for 400 hour, add liquid nitrogen in the reaction bottle afterwards, carry out Co60 gamma ray irradiation, irradiation dose is 66.6kGy, after irradiation, move the reaction bottle into the environment of -95 degrees centigrade, pass into the nitrogen of -95 degrees Celsius in the reaction bottle, The flow rate was 50 L / h, and after the polymerization was carried out for 5 hours, it was repeatedly washed with water, filtered, and dried.

[0042] The polymerization yield is 62.5%, and the number-average molecular weight of the obtained isotactic polyacrylonitrile is 18280, and the molecular weight distribution is 1.31, and the three-unit isotacticity is 99% (see image 3 ).

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Abstract

The invention provides a method for preparing isotactic polyacrylonitrile, which comprises the following steps: (1) proportionally and evenly mixing acrylonitrile and urea; (2) freezing the mixture obtained in the step (1) under low-temperature condition to form a urea-acrylonitrile compound; (3) dispersing the urea-acrylonitrile compound obtained in the step (2) in liquid nitrogen, and carrying out gamma-ray irradiation; and (4) carrying out polymerization reaction on the irradiated substance obtained in the step (3) in a low-temperature environment. The isotactic triad (mm) content in the isotactic polyacrylonitrile prepared by the method is greater than or equal to 98%; and the polymerization yield and the molecular weight of polyacrylonitrile can be regulated by controlling the gamma-ray irradiation time and polymerization reaction time.

Description

technical field [0001] The invention relates to the field of polymer material preparation, in particular to a method for preparing isotactic polyacrylonitrile and its application. Background technique [0002] Polyacrylonitrile is an important precursor in polymer materials and has attracted extensive attention in many fields. [0003] A nitrile group is attached to every other carbon atom on the polyacrylonitrile backbone. According to the position of the nitrile group, polyacrylonitrile has three stereochemical configurations: isotactic polyacrylonitrile, syndiotactic polyacrylonitrile, and atactic polyacrylonitrile. [0004] The size of the molecular weight of the polymer, its molecular weight distribution, and the stereoregularity of the molecular chain have a great influence on its performance, molding process and final product performance. [0005] Many attempts have been made in the past to prepare isotactic polyacrylonitrile, but none have an isotactic triad (mm) c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F120/44C08F2/46C08F2/44C08K5/21
Inventor 邹均庭王雨松庞文民石磊鲁非
Owner UNIV OF SCI & TECH OF CHINA
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