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Method and device for polymerizing polyacrylonitrile spinning stock solution

A polymerization method and spinning dope technology, which are applied in the field of polymer solution polymerization, can solve the problems of short material residence time, difficult spinning dope, not universal application, etc., and achieve lower operating costs, stable product quality, and small footprint. Effect

Active Publication Date: 2012-05-09
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the diversity and complexity of polymer polymerization systems, general hypergravity reaction methods and devices are not generally applicable to the polymerization processes of different systems, and it is necessary to conduct research and development according to the characteristics of different polymerization processes, such as for polyacrylonitrile spinning The synthesis system of stock solution has high viscosity and the polymerization process takes a certain amount of time. If the general supergravity reaction method is adopted, the residence time of the material in the equipment is very short, and it is difficult to complete the polymerization process of the spinning stock solution well.

Method used

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  • Method and device for polymerizing polyacrylonitrile spinning stock solution
  • Method and device for polymerizing polyacrylonitrile spinning stock solution
  • Method and device for polymerizing polyacrylonitrile spinning stock solution

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Example 1: 2323.2g of acrylonitrile, 48.4g of itaconic acid, 48.4g of methyl acrylate and 9900g of dimethyl sulfoxide were added to the mixing zone, powered by a gear pump, and the materials entered from the upper material inlet through a heat exchanger The rotor returns to the stirring area, so that the material circulates between the integrated supergravity polymerization reactor and the heat exchanger at a circulation rate of 50L / h, and is controlled by adjusting the flow rate of the temperature control jacket and the circulating water of the heat exchanger The temperature is at 60°C, and nitrogen is blown to drive oxygen for 20 minutes. Dissolve 21.68g of azobisisobutyronitrile into 1100g of dimethyl sulfoxide, add it into the material inlet pipe through the branch pipe on the material inlet, and spray it to the inner edge of the rotor with a speed of 1000 rpm through the liquid distributor. The rotor is installed concentrically The 5-layer porous plate with an open...

Embodiment 2

[0033] Embodiment 2: As described in Embodiment 1, the rotor speed is 500 rev / min, and other conditions remain unchanged. The measured product conversion rate is 95.1%, and the molecular weight distribution coefficient is 2.7.

Embodiment 3

[0034] Embodiment 3: As described in Embodiment 1, the initiator solution addition rate is 0.04 times of the material circulation flow rate, and other conditions remain unchanged, and the product conversion rate recorded is 95.6%, and the molecular weight distribution coefficient is 2.5.

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Abstract

The invention relates to a method and device for polymerizing polyacrylonitrile spinning stock solution. In the polymerization process, polymerization is initiated step by step under the actions of hypergravity and normal gravity fields; in the polymerization device integrating a hypergravity revolving bed, a stirring reactor and a heat exchanger, the mixture of acrylonitrile, comonomer and solvent, and an initiator are mixed at the micro level; after the initiator is added, the materials in the stirring reactor continue to complete the polymerization process, thereby enhancing the mixing efficiency in the whole polymerization process; and thus, the molecular weight distribution of the polymerized spinning stock solution is controllable and narrow. Compared with the traditional single-kettle polymerization method, under the conditions of the same treatment scale and equivalent product quality of the polymerized polyacrylonitrile spinning stock solution, the invention can reduce the operating cost by 20% and save the energy by 30%, the product quality is stable, and the obtained polyacrylonitrile spinning stock solution can be used for preparing high-performance polyacrylonitrile-based carbon fiber.

Description

Technical field: [0001] The invention relates to a method and device for polymer solution polymerization, in particular to a polymerization method and a polymerization reaction device for polyacrylonitrile spinning stock solution, and also relates to the application of supergravity technology in the polymerization reaction of polyacrylonitrile spinning stock solution. The polymerized spinning dope can prepare high-performance polyacrylonitrile-based carbon fibers through spinning, pre-oxidation and carbonization processes. Background technique: [0002] The most commonly used synthetic method of polyacrylonitrile is free radical polymerization, and the specific implementation methods include solution polymerization, suspension polymerization and aqueous phase precipitation polymerization. In industrial applications, solution polymerization is the main method. At present, most of the methods used in solution polymerization are to carry out stirring reaction polymerization in ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/44C08F2/01C08F2/04D01F9/22
Inventor 陈建峰李沃源初广文徐梁华邹海魁毋伟
Owner BEIJING UNIV OF CHEM TECH
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