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Spinning dope containing ultra-high molecular weight polyacrylonitrile and its preparation method and application

An ultra-high molecular weight, spinning dope technology, used in textiles and papermaking, fiber chemical characteristics, etc., can solve the problems of difficult filtration, easy to generate gel, low viscosity of spinning dope, achieve good technical effect and maintain stability Effect

Active Publication Date: 2018-09-14
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] One of the technical problems to be solved by the present invention is that when the acrylonitrile copolymer is prepared by a one-step method in the prior art, the polyacrylonitrile stock solution of general molecular weight has a relatively small viscosity of the spinning stock solution, which cannot meet the requirements of high-power drafting during spinning, and cannot Meet the requirements of dry-jet wet spinning process; ultra-high molecular weight polyacrylonitrile stock solution has too high viscosity, difficult to filter, and unstable spinning; when two-step method prepares spinning stock solution containing ultra-high molecular weight polyacrylonitrile, the dissolution process is not easy to control , it is easy to produce gel, and the ultra-high molecular weight component can only be controlled within a small range. A preparation method for spinning stock solution containing ultra-high molecular weight acrylonitrile copolymer is provided. In this method, the stock solution is prepared from the solution in one step Polymerized by the method, containing ultra-high molecular weight copolymer components and ordinary molecular weight copolymer components, it is suitable for high-strength drafting, and maintains the viscosity of the stock solution suitable for spinning, so that high-density, high-strength, high-modulus carbon fiber precursors can be obtained The advantages

Method used

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  • Spinning dope containing ultra-high molecular weight polyacrylonitrile and its preparation method and application
  • Spinning dope containing ultra-high molecular weight polyacrylonitrile and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032]Add 90 g of distilled acrylonitrile (AN), 5 g of methyl methacrylate, 5 g of isobutyl acrylic acid, 100 g of N,N-dimethylformamide, and 0.001 g of azobisisoheptanonitrile (ABVN) into the reactor , under the protection of nitrogen, react at a constant temperature of 30°C for 1 hour, and then continue to add 300g of N,N-dimethylformamide and 0.5g of azobisisobutyronitrile (AIBN), at a constant temperature of 60°C The reaction was carried out under low temperature for 20 hours, and then the spinning solution was decompressed to remove residual monomers and air bubbles to obtain a spinning solution containing an ultra-high molecular weight acrylonitrile copolymer. After testing, the viscosity-average molecular weight of the ultra-high molecular weight copolymer component is 4.85 million, the molecular weight distribution is 2.34, the viscosity of the polyacrylonitrile spinning stock solution is 487Pa·S at 50°C, and the stock solution is easy to filter through 5μm during the s...

Embodiment 2

[0034] Add 92g of distilled acrylonitrile (AN), 2g of itaconic acid, 6g of acrylamide, 150g of N,N-dimethylformamide, and 0.01g of azobisisoheptanonitrile (ABVN) into the reactor, Under protection, react at a constant temperature of 40°C for 2 hours, then continue to add 300g of N,N-dimethylformamide and 0.8g of azobisisobutyronitrile (AIBN), and react at a constant temperature of 50°C for 24 hours , and then the spinning solution is decompressed to remove residual monomers and air bubbles to obtain a spinning solution containing an ultra-high molecular weight acrylonitrile copolymer. After testing, the viscosity-average molecular weight of the ultra-high molecular weight copolymer component is 4.59 million, the molecular weight distribution is 3.49, the viscosity of the polyacrylonitrile spinning stock solution is 455Pa·S at 50°C, and the stock solution is easy to filter through 5μm during the spinning process Filtration of materials, after 27 times of stretching, no broken f...

Embodiment 3

[0036] Add 93g of distilled acrylonitrile (AN), 3.5g of butyl β-itaconate, 3.5g of acrylamide oxime, 186g of N,N-dimethylacetamide, and 0.1g of azobisisoheptanonitrile (ABVN) In the reactor, under the protection of nitrogen, react at a constant temperature of 50°C for 3 hours, then continue to add N,N-dimethylformamide 100g and azobisisobutyronitrile (AIBN) 0.6g, at 55°C React at a constant temperature for 22 hours, and then the spinning solution is decompressed to remove residual monomers and air bubbles to obtain a spinning solution containing an ultra-high molecular weight acrylonitrile copolymer. After testing, the viscosity-average molecular weight of the copolymer component containing ultra-high molecular weight is 3 million, and the molecular weight distribution is 4.97. The viscosity-average molecular weight of the copolymer component B is 130,000, and the molecular weight distribution is 5.66. The viscosity of the polyacrylonitrile spinning stock solution is 50 ℃ The ...

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Abstract

The invention relates to an ultrahigh-molecular-weight acrylonitrile copolymer-containing spinning stock solution and a preparation method and an application thereof, and aims to solve the technical problems that in the prior art, when a one-step method is adopted for preparing a polyacrylonitrile spinning stock solution, the spinning stock solution has relatively small viscosity and is unable to meet requirements of high-magnification drafting and dry spraying wet spinning processes, or the viscosity is too large, filtration is difficult and the precursor quality is unstable. The problems are relatively well solved through adopting the technical schemes comprising that the preparation method comprises the steps: mixing a first part solvent, a copolymerization component and a first part initiator, then polymerizing the reactive substances for 10 minutes-4 hours at the temperature of 30-50 DEG C and under the protection of gas inert with the reactive substances, followed by additionally adding a second part solvent and a second part initiator, polymerizing for 20-30 hours at the temperature of 50-70 DEG C, and thus obtaining a spinning solution I; and carrying out decompression removal of residual monomers and bubbles of the spinning solution I, and thus obtaining the ultrahigh-molecular-weight acrylonitrile copolymer-containing spinning stock solution which can be used in industrial production of carbon fiber precursors.

Description

technical field [0001] The invention relates to a spinning dope containing ultra-high molecular weight polyacrylonitrile and its preparation method and application. Background technique [0002] Polyacrylonitrile (PAN)-based carbon fiber is a new type of material developed rapidly in the 1960s, because of its light weight, high specific strength, high specific modulus, high temperature resistance, corrosion resistance, wear resistance, fatigue resistance, electrical conductivity, thermal conductivity, etc. It is widely used in military industries such as satellites, launch vehicles, tactical missiles, and spacecraft, and has become an indispensable material in the aerospace industry. Excellent carbon fiber precursors should have the characteristics of high heat resistance, less pore structure, less surface defects, dense structure, and good stretchability. [0003] The strength of carbon fiber has a good linear dependence on the product of the strength of PAN precursor and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F220/46C08F220/48C08F220/14C08F220/04C08F222/02C08F220/56C08F222/16C08F220/18C08F2/06D01F9/22
Inventor 屠晓萍缪金根沈志刚李磊肖士洁
Owner CHINA PETROLEUM & CHEM CORP