A kind of preparation method and application of plasticized melt spinning commercial grade active pan precursor

A commercial-grade, melt-spinning technology, used in melt-spinning, rayon manufacturing, textiles and papermaking, etc., can solve the problems of difficulty in imparting modification effects to the precursor, affecting the performance of CFs, and the effect of structural homogenization. The melt viscosity increases too fast, the stabilization reaction is accelerated, and the environmental pollution is small.

Active Publication Date: 2022-07-08
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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  • A kind of preparation method and application of plasticized melt spinning commercial grade active pan precursor
  • A kind of preparation method and application of plasticized melt spinning commercial grade active pan precursor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Choose the viscosity average molecular weight as 5.2×10 4 g / mol, the copolymerized PAN with acrylonitrile content of 88 mole percent (mol%) is used as raw material, high-purity commercial grade BMiMCI is used as plasticizer, and sodium dodecylbenzene sulfonate is used as dispersant, and 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 a twin-screw extruder, and the temperature of each zone of the twin-screw is set to be 120°C, 130°C, 140°C, 150°C, 150°C, and 140°C, respectively. The material is immediately diced and packaged. The ambient temperature should not be higher than 25℃ and the humidity should not be higher than 5% during the process of mechanical blending, bar making and pelletizing.

[0029] The prepared pellets are used as raw materials in the melt spinning process, and are spun by a single-screw melt spinning machine. The number of spinneret ho...

Embodiment 2

[0032] Choose the viscosity average molecular weight as 6.5×10 4g / mol, copolymerized PAN with acrylonitrile content of 90 mol% is used as raw material, high-purity commercial grade [Bmim]Cl is used as plasticizer, and sodium dodecylbenzene sulfonate is used as dispersant, and the mass ratio of the three is 5:4.95 : 0.05, use a pulverizer to fully mix the three raw materials. The twin-screw extruder is used to make bars and pelletize, and the temperature of each zone of the twin-screw is set to be 130°C, 140°C, 140°C, 150°C, 150°C, and 140°C, respectively. , and packaged. The ambient temperature should not be higher than 25℃ and the humidity should not be higher than 10% during the process of mechanical blending, bar making and pelletizing.

[0033] The prepared pellets were used as the raw material in the melt spinning process. The number of spinneret holes was 36, the diameter was 0.3 mm, the pump supply was 35 g / min, the spinning distance was 5 m, and the spinning machine ...

Embodiment 3

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

[0037] A twin-screw extruder is used to make bars and pelletize, and the temperature of each zone of the twin-screw is set to be 130°C, 140°C, 150°C, 150°C, 150°C, and 140°C, respectively. , and packaged. The ambient temperature should not be higher than 25℃ and the humidity should not be higher than 10% during the process of mechanical blending, bar making and pelletizing.

[0038] The prepared pellets were used as raw materials in the melt spinning process, the number of spinneret holes was 36, the diameter was 0.3 mm, the pump supply was 35 g / min, the spinning distance was 4.5 m, and the spinning mach...

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Abstract

The invention relates to a preparation method and application of plasticized melt-spun commercial-grade active PAN raw silk. Choose a viscosity average molecular weight of 5‑7×10 4 g / mol copolymerized PAN is used as raw material, [Bmim]Cl is used as plasticizer, and sodium dodecylbenzene sulfonate is used as dispersant, which is mixed by mechanical blending. Using a single screw spinning machine for spinning, the temperature of the melt blending zone should reach 270 °C. The number of spinneret holes is 36, the hole diameter is 0.3mm, the pump supply is 35g / min, and the screw speed is 100‑200r / min. The temperature of the spinning workshop is 10-20℃, the spinning distance is 3-5m, the pulling roller is 300-400m / min, and the draft ratios of the bottom, middle and upper rollers are 2-2.5, 1.5-2, 1.2-1.5 respectively. Soak the raw silk in deionized water at 20-30°C for 12-24h, and dry it in an oven at 40-50°C. The protofilament has a perfect structure and contains a lot 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 precursor. Background technique [0002] Commercial grade polyacrylonitrile (PAN) precursors are not optimally selected for the second and third comonomers, and some monomers hinder the subsequent stabilization process, resulting in uncontrollable stabilized fiber structure; at the same time, high monomer content (approximately 10 mol%) hindered the continuation of the cyclization behavior during the stabilization phase. Therefore, the stabilization time of the precursor is too long, and the structure is uncontrollable. In order to reduce the stabilization time and improve the structure, domestic and foreign researchers have focused on using new technologies to optimize the structure of commercial-grade PAN precursors to adapt to high-temperature erosion in the ...

Claims

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Application Information

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Patent Type & Authority Patents(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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