Preparation method and application of plasticized melt-spun commodity-grade active PAN precursors

A commercial-grade, melt-spinning technology, which is applied in melt-spinning, rayon manufacturing, textiles and papermaking, etc., can solve the problems of low environmental friendliness, difficulty in imparting modification effect to raw silk, increasing CFs preparation cost, difficulty in CFs performance regulation, etc. question

Active Publication Date: 2021-04-23
ZHENJIANG COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are some deficiencies in the pretreatment technology of raw silk. First, the process needs to be strictly regulated to ensure the modification effect. At the same time, damage to the appearance and structure of the raw silk should be avoided as much as possible, which is difficult to control
Secondly, it is difficult to give the same modification effect to the inner and outer layers of the original silk by the pretreatment modification method after the original silk is formed, which will affect the homogenization of the stabilized fiber and the final CFs structure, and ultimately affect the CFs performance.
Finally, adding any pretreatment process will increase the preparation cost of CFs and the difficulty of controlling CFs performance.
[0004] CN101759837B discloses a method for preparing polyacrylonitrile spinning stock solution for high-performance carbon fiber in ionic liquid. The patent uses ionic liquid as a reaction solvent to polymerize polyacrylonitrile, and uses dimethyl sulfoxide as a solvent solution to prepare raw silk , but the amount of organic solvent used in this invention is large, and the degree of environmental friendliness is low

Method used

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  • Preparation method and application of plasticized melt-spun commodity-grade active PAN precursors
  • Preparation method and application of plasticized melt-spun commodity-grade active PAN precursors

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Choose the viscosity average molecular weight as 5.2×10 4 g / mol, acrylonitrile content is 88 mole percent (mol%) copolymerized PAN as raw material, high-purity commercial grade BMiMCI as plasticizer, sodium dodecylbenzenesulfonate as dispersant, the mass ratio of the three is 6 : 3.96: 0.04, using a pulverizer to fully mix the three raw materials.

[0028] The blend is made into strips and pelletized by using a twin-screw extruder, and the temperatures in each zone of the twin-screw are set to 120°C, 130°C, 140°C, 150°C, 150°C, and 140°C respectively. The material is immediately pelletized and packaged. Keep the ambient temperature not higher than 25°C and the humidity not higher than 5% during the process of mechanical blending, sliver making and pelletizing.

[0029] The prepared particles are used as raw materials in the melt spinning process, and are spun by a single-screw melt spinning machine. The number of spinneret holes is 36, the diameter is 0.3mm, the pump...

Embodiment 2

[0032] Choose the viscosity average molecular weight as 6.5×10 4g / mol, copolymerized PAN with acrylonitrile content of 90mol% as raw material, high-purity commercial grade [Bmim]Cl as plasticizer, sodium dodecylbenzenesulfonate as dispersant, the mass ratio of the three is 5:4.95 : 0.05, using a pulverizer to fully mix the three raw materials. A twin-screw extruder is used for strip making and pelletizing, and the temperature of each zone of the twin-screw is set to 130°C, 140°C, 140°C, 150°C, 150°C, and 140°C, and the strip-making material is immediately pelletized , and encapsulate. Keep the ambient temperature not higher than 25°C and the humidity not higher than 10% during the process of mechanical blending, sliver making and pelletizing.

[0033] The prepared particles are used as raw materials in the melt spinning process, the number of holes in the spinneret is 36, the diameter is 0.3mm, the pump supply is 35g / min, the spinning length is 5m, and the melt blending zone...

Embodiment 3

[0036] Choose the viscosity average molecular weight as 7×10 4 g / mol, copolymerized PAN with acrylonitrile content of 92mol% as raw material, high-purity commercial grade [Bmim]Cl as plasticizer, sodium dodecylbenzenesulfonate as dispersant, the mass ratio of the three is 6:3.96 : 0.04, using a pulverizer to fully mix the three raw materials.

[0037] A twin-screw extruder is used for strip making and pelletizing, and the temperature of each zone of the twin-screw is set to 130°C, 140°C, 150°C, 150°C, 150°C, and 140°C, and the strip-making material is immediately pelletized , and encapsulate. Keep the ambient temperature not higher than 25°C and the humidity not higher than 10% during the process of mechanical blending, sliver making and pelletizing.

[0038] The prepared particles are used as the raw material in the melt spinning process, the number of holes in the spinneret is 36, the diameter is 0.3mm, the pump supply is 35g / min, the spinning length is 4.5m, and the spinn...

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Abstract

The invention relates to a preparation method and application of plasticized melt-spun commodity-grade active PAN precursors. Copolymerized PAN with the viscosity-average molecular weight of (5-7)x10<4> g/mol is selected as a raw material, [Bmim]Cl is selected as a plasticizer, sodium dodecylbenzene sulfonate is selected as a dispersing agent, and mixing is performed in a mechanical blending mode. A single-screw spinning machine is adopted for spinning, and the temperature of a melt blending area needs to reach 270 DEG C. The number of holes in a spinneret plate is 36, the hole diameter is 0.3 mm, the pump supply amount is 35 g/min, and the screw speed is 100-200 r/min. The temperature of a spinning workshop is 10-20 DEG C, the spinning stroke is 3-5 m, a traction roller is 300-400 m/min, and the draft multiples of a bottom layer roller, a middle layer roller and an upper layer roller are 2-2.5, 1.5-2 and 1.2-1.5 respectively. The precursors are soaked in deionized water with the temperature of 20-30 DEG C for 12-24 hours, and drying is performed in a drying oven with the temperature of 40-50 DEG C. The precursors are perfect in structure and contain a large amount of active free radicals.

Description

technical field [0001] The invention belongs to the field of composite material preparation, and in particular relates to a preparation method and application of plasticized melt spinning commercial-grade active PAN precursors. Background technique [0002] Due to the unoptimized selection of the second and third comonomers of commercial-grade polyacrylonitrile (PAN) precursors, some monomers hinder the subsequent stabilization process, resulting in uncontrollable stabilized fiber structures; at the same time, higher monomer content (approximately 10mol%) has caused certain hindrance to the continuity of the cyclization behavior in the stabilization stage. Therefore, the protofilaments were stabilized for too long and the structure was uncontrollable. In order to reduce the stabilization time and improve the structure, researchers at home and abroad have focused on optimizing the structure of commercial-grade PAN precursors using new technologies to adapt to high-temperatur...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/54D01F1/10D01F9/22D01F11/06D01D1/04D01D5/098
CPCD01F6/54D01F1/10D01F9/22D01F11/06D01D1/04D01D5/098Y02P20/54
Inventor 李翔刘福杰
Owner ZHENJIANG COLLEGE
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