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Preparation method of halogen-free flame-retardant polyacrylonitrile fiber

A technology of polyacrylonitrile fiber and flame-retardant polyacrylonitrile, which is applied in the manufacture of fire-resistant and flame-retardant filaments, fiber chemical characteristics, single-component synthetic polymer rayon, etc., and can solve the problems of high smoke generation of flame-retardant fibers , to achieve the effect of improving flame retardant effect, improving hygroscopicity, and improving flame retardant durability

Pending Publication Date: 2021-05-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Throughout the existing flame-retardant acrylic fibers for industrialized textiles, they are prepared by copolymerizing halogen-containing monomers with acrylonitrile or adding antimony compounds as synergists in the copolymerization system to obtain flame-retardant polyacrylonitrile polymers, and then through Spinning to prepare flame-retardant acrylic fiber. Although this type of flame-retardant fiber has a good flame-retardant effect, there is a large amount of smoke when the flame-retardant fiber is burned, and due to the existence of halogen components, it will release toxic gases during the combustion process. Environmental pollution problems such as hydrogen halide gas
With the upgrading of environmental regulations, the application of halogen-containing flame retardants on acrylic fibers has been limited, thus promoting the research of halogen-free flame-retardant polyacrylonitrile polymers or flame-retardant acrylic fibers

Method used

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  • Preparation method of halogen-free flame-retardant polyacrylonitrile fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Step 1: Heat and melt the halogen-free phosphorus and nitrogen-containing flame retardant vinylphosphonic acid, raise the temperature to above 85°C, and stir continuously for more than 30 minutes until it completely melts to a transparent light yellow liquid.

[0027] Step 2: In the stirring state, mix the liquid halogen-free phosphorus and nitrogen-containing flame retardant vinylphosphonic acid obtained in step (1) and polyacrylonitrile spinning stock solution in a weight ratio of 30:70, and the stirring speed is 1000r / min , and the stirring time was 30 minutes to obtain a blended flame retardant spinning stock solution;

[0028] Among them, the polyacrylonitrile spinning stock solution is prepared in two steps:

[0029] The polyacrylonitrile slurry with a concentration of 34wt% from the storage tank at a temperature of 50°C and the NaSCN solvent with a concentration of 58wt% from a concentrated solvent storage tank at a temperature of 85°C enter high-shear dissolutio...

Embodiment 2

[0033] Step 1: Heat and melt the halogen-free phosphorus and nitrogen-containing flame retardant (methyl vinyl phosphonate and ethyl vinyl phosphonate mixed at a mass ratio of 1:2), raise the temperature to above 85°C, and stir continuously for more than 30 minutes. Until completely melted to a transparent light yellow liquid.

[0034] Step 2: Under agitation, the mixture of the liquid halogen-free phosphorus and nitrogen-containing flame retardant vinyl phosphonate and ethyl vinyl phosphonate prepared in step (1) is mixed with the polyacrylonitrile spinning stock solution by weight 35:65 mixed evenly, the stirring speed was 1200r / min, and the stirring time was 40 minutes to obtain the blended flame retardant spinning stock solution;

[0035] Among them, the polyacrylonitrile spinning stock solution is prepared in two steps:

[0036]The polyacrylonitrile slurry with a concentration of 34wt% from the storage tank at a temperature of 50°C and the NaSCN solvent with a concentrat...

Embodiment 3

[0040] Step 1: Heat and melt the halogen-free phosphorus and nitrogen-containing flame retardant allyl phosphate methyl ester, raise the temperature to 42°C, and stir continuously for more than 30 minutes until it completely melts to a transparent light yellow liquid.

[0041] Step 2: The liquid halogen-free phosphorus and nitrogen-containing flame retardant allyl phosphate methyl ester that step (1) makes is passed through the high-shear dissolving machine with the polyacrylonitrile spinning stock solution by weight ratio of 25: 75 for online blending, the feed ratio is automatically cascade controlled by DSC, and the cascade ratio is adjusted at 0.3-0.45:1 to obtain a blended flame retardant spinning stock solution;

[0042] Among them, the polyacrylonitrile spinning stock solution is prepared in two steps:

[0043] The polyacrylonitrile slurry with a concentration of 34wt% from the storage tank at a temperature of 50°C and the NaSCN solvent with a concentration of 58wt% fro...

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Abstract

The invention provides a preparation method of a halogen-free flame-retardant polyacrylonitrile fiber. The method mainly comprises the following steps: heating and melting a halogen-free flame retardant containing phosphorus and nitrogen, then stirring and blending with a polyacrylonitrile spinning solution, carrying out wet spinning, and then carrying out cross-linking hydrolysis to obtain the flame-retardant polyacrylonitrile fiber. According to the preparation method disclosed by the invention, the halogen-free organic phosphorus-nitrogen flame retardant can be uniformly and stably dispersed in the spinning solution, so that a hole blocking phenomenon is effectively avoided during spinning, and the period of replacing a nozzle during spinning is greatly prolonged. Meanwhile, chemical modification of crosslinking and alkaline hydrolysis is further carried out on the surface of the fiber after a hot drafting procedure in a spinning process of the flame-retardant acrylic fiber, the flame retardance LOI of the prepared acrylic fiber is larger than or equal to 26%, and the hygroscopicity of the acrylic fiber is improved.

Description

technical field [0001] The invention relates to the technical field of acrylic fiber manufacturing, in particular to a method for preparing halogen-free flame-retardant polyacrylonitrile fibers by using a sodium thiocyanate aqueous solution as a spinning solvent through a wet spinning process. Background technique [0002] The fire caused by the burning of chemical fiber textile products has become one of the major disasters in today's society. Therefore, the research and development of flame-retardant textiles has become an urgent requirement in front of people and has attracted more and more attention. [0003] Although polyacrylonitrile fiber has many advantages and is widely used, it is still widely used in my country and many other countries. However, polyacrylonitrile fiber is a flammable fiber, and its limiting oxygen index (LOI) is only 18%. , when it burns, it will release more toxic cyanide and other substances. Therefore it is particularly important to research an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/54D01F1/07D01F11/06
CPCD01F6/54D01F1/07D01F11/06
Inventor 章毅杨雪红张超峰俞玉芳赵丹贤伍三华宋铮
Owner CHINA PETROLEUM & CHEM CORP
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