A kind of preparation method of acrylonitrile-based carbon fiber spinning liquid and its polymerization reaction equipment

An acrylonitrile-based carbon fiber, polymerization reaction technology, applied in the chemical characteristics of fibers, textiles and papermaking, etc., can solve the problems of uneven material properties and structure, and achieve the effect of good mixing effect, improved reaction degree and reliable mass transfer.

Active Publication Date: 2012-02-08
KINGFA SCI & TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a method for preparing acrylonitrile-based carbon fiber spinning solution, so as to solve the problem of inhomogeneous material properties and structure in the existing preparation method

Method used

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  • A kind of preparation method of acrylonitrile-based carbon fiber spinning liquid and its polymerization reaction equipment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1: Weigh 20Kg dimethyl sulfoxide, 6.336Kg acrylonitrile, 132g acrylamide and 66g itaconic acid, and pour them into a 50L reaction kettle in turn, after stirring and dissolving completely, bubbling with argon for 20min to remove the solution and There is air in the kettle, and at the same time, 50°C hot water is passed through the jacket of the reaction kettle. When the temperature of the material is 50°C, add 36.3g of azobisisoheptanonitrile, the reaction starts, and after 30min, the twin-screw reaction extruder is opened to circulate the material, and the output of the extruder is 50Kg / h, and the temperature of the jacket of the extruder is kept at 50 ℃. At the same time, 3.4 kg of dimethyl sulfoxide and 66 g of itaconic acid were added to the feeding tank of the extruder, and the feeding was completed within 3 hours with a metering pump. Discharging after 15 hours of polymerization. The conversion rate is 92.6%, the weight average molecular weight is 158,000...

Embodiment 2

[0027] Example 2: Weigh 20Kg dimethyl sulfoxide, 6.336kg acrylonitrile, 132g acrylamide and 66g itaconic acid, and pour them into a 50L reaction kettle in turn, after stirring and dissolving completely, bubbling with argon for 20min to remove the solution and Air in the kettle, while hot water at 45°C was passed through the jacket of the reaction kettle. When the temperature of the material is 50°C, add 46.2g of azobisisoheptanonitrile, the reaction begins, and after 30min, two sets of twin-screw reaction extruders in series are opened to circulate the material, and the output of the extruder is 50Kg / h, and the extruder is kept The jacket temperature was 45°C. At the same time, 3.4 kg of dimethyl sulfoxide and 66 g of itaconic acid were added to the feeding tank of the extruder, and the feeding was completed within 3 hours with a metering pump. Discharging after 20 hours of polymerization. The conversion rate is 95.1%, the weight average molecular weight is 135,000, and the ...

Embodiment 3

[0028] Example 3: Weigh 17.5Kg dimethyl sulfoxide, 4.85kg acrylonitrile, 75g methyl acrylate and 30g itaconic acid, pour them into a 50L reaction kettle in turn, stir and dissolve completely, and then bubble with argon for 20min to remove solution and the air in the kettle, and at the same time, hot water at 60°C was passed through the jacket of the reaction kettle. When the temperature of the material is 60°C, add 30.0g of azobisisobutyronitrile, the reaction starts, and after 30 minutes, open two series-connected twin-screw reaction extruders to circulate the material, and the output of the extruders is 50Kg / h. The jacket temperature was 60°C. At the same time, 2.5kg of dimethyl sulfoxide and 35g of itaconic acid were added to the feeding tank of the extruder, and the feeding was completed within 4 hours with a metering pump. Discharging after 12 hours of polymerization. The conversion rate is 91.6%, the weight average molecular weight is 132,000, and the molecular weight ...

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Abstract

The invention discloses a preparation method of acrylonitrile-based carbon fiber spinning solution and polymerization reaction equipment thereof. The preparation method of the present invention carries out solution polymerization reaction in the polymerization reaction equipment, and described polymerization reaction equipment comprises reaction kettle and reaction extruder, and reaction kettle is connected with reaction extruder, and reaction kettle and reaction extruder are respectively provided with temperature control device . In the present invention, a reaction extruder is connected to the reaction kettle, and the screw extrusion structure adopted by the reaction extruder not only has the function of mixing materials of a traditional extruder, but also can introduce a reaction medium and a chemical reaction in the extrusion process, and has the advantages of The function of the synthesis reactor, the reaction extruder is better able to handle high-viscosity materials, and can continuously and rapidly produce new, very thin material surface layers, so that the surface / volume ratio of the materials increases, and the reaction medium is evenly distributed in the materials , the degree of response increases.

Description

technical field [0001] The invention relates to the preparation technology of acrylonitrile-based carbon fiber spinning solution. Background technique [0002] Because carbon fiber has excellent properties such as high strength, high modulus, high temperature resistance, corrosion resistance, fatigue resistance, creep resistance, electrical conductivity and thermal conductivity, it is an indispensable engineering material in the aerospace industry. It is also widely used in construction, and it is a high-tech fiber that belongs to both military and civilian uses. Among them, polyacrylonitrile-based carbon fiber has developed rapidly due to its simple production process and good mechanical properties, and has become the most important and absolute variety. Since the properties of polyacrylonitrile-based carbon fibers largely depend on the properties of carbon fiber precursors, the quality of spinning stock solution is the premise and basis for preparing high-quality precurso...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/44C08F2/01C08F2/06D01F9/22
Inventor 宋威黄险波代惊奇辛伟黄有平马雷
Owner KINGFA SCI & TECH CO LTD
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