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A kind of method that prepares boric acid phenyl ester modified high ortho phenolic fiber by wet spinning

A technology of phenyl borate and wet spinning, applied in the manufacture of rayon, chemical characteristics of fibers, manufacture of fire-retardant and flame-retardant filaments, etc., can solve problems such as difficulty in mass production, pollution of electrospinning, etc.

Active Publication Date: 2020-10-20
ZHONGYUAN ENGINEERING COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In view of the serious pollution in the solidification process of melt spinning and the difficulty of large-scale production of electrospinning in the prior art, the present invention proposes a heat-resistant and flame-retardant phenyl borate modified high The preparation method of ortho phenolic fiber

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A method for preparing phenyl borate modified high ortho phenolic fiber by wet spinning, specifically comprising the following steps:

[0029] (1) Mix phenol, ethanol, boric acid and oxalic acid in a mass ratio of 100:50:45:2, heat up to boiling, condense and reflux for 1 hour, dehydrate under reduced pressure and gradually heat up to 130°C to obtain phenyl borate;

[0030] (2) Phenyl borate, phenol, and formaldehyde (the molar ratio of phenol to formaldehyde is 1:0.8, and the mass ratio of phenol to phenyl borate is 100:4) in zinc acetate (the mass of phenol is calculated as 100, and the mass ratio of zinc acetate is 1 ), heated to boiling for 2 hours, added dropwise concentrated sulfuric acid (the mass ratio of phenol to concentrated sulfuric acid was 100:0.2), continued the reaction for 0.5 hours, dehydrated under reduced pressure, and lowered the temperature to 40°C within 1 hour, then The temperature was raised to 105°C within 5 hours, the vacuum degree was 8500Pa,...

Embodiment 2

[0036] A method for preparing phenyl borate modified high ortho phenolic fiber by wet spinning, specifically comprising the following steps:

[0037](1) Mix phenol, ethanol, boric acid and oxalic acid in a mass ratio of 100:50:45:2, heat up to boiling, condense and reflux for 7 hours, dehydrate under reduced pressure and gradually heat up to 200°C to obtain phenyl borate;

[0038] (2) Phenyl borate, phenol, acetaldehyde (the molar ratio of phenol to acetaldehyde is 1:1, the mass ratio of phenol to phenyl borate is 100:20) in cadmium acetate (phenol is calculated as 100, cadmium acetate is 3) Under the action of the reaction, heat to boiling for 6 hours, add dropwise hydrochloric acid (the mass ratio of phenol to hydrochloric acid is 100:2), continue the reaction for 4 hours, carry out dehydration under reduced pressure, and reduce the temperature to 60°C within 1 hour, and then within 5 hours Heat up to 170°C, vacuum degree is 8500Pa, react for 4h until the solution is viscous...

Embodiment 3

[0044] A method for preparing phenyl borate modified high ortho phenolic fiber by wet spinning, specifically comprising the following steps:

[0045] (1) Mix phenol, ethanol, boric acid and oxalic acid in a mass ratio of 100:50:45:2, heat up to boiling, condense and reflux for 3 hours, dehydrate under reduced pressure and gradually heat up to 180°C to obtain phenyl borate;

[0046] (2) Phenyl borate, phenol, furfural (the molar ratio of phenol to furfural is 1:0.85, the mass ratio of phenol to phenyl borate is 100:6) in cobalt acetate (phenol is 100, cobalt acetate is 2) Under the action of the reaction, heat to boiling for 3 hours, add dropwise phosphoric acid (the mass ratio of phenol to phosphoric acid is 100:1), continue the reaction for 2 hours, carry out dehydration under reduced pressure, and reduce the temperature to 50°C within 1 hour, and then within 5 hours Raise the temperature to 130°C, the vacuum degree is 8500Pa, and react for 3 hours until the solution is visco...

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Abstract

The invention discloses a method for preparing borophenylic acid-modified high-ortho phenolic fibers through wet spinning. The method comprises the following steps: mixing phenol compounds, ethanol and oxalic acid for reaction so as to obtain borophenylic acid, and reacting by virtue of the phenol compounds, aldehyde compounds and borophenylic acid, so as to generate borophenylic acid-modified high-ortho thermoplastic phenolic resin; dissolving the obtained borophenylic acid-modified high-ortho thermoplastic phenolic resin into absolute ethyl alcohol to react with aldehyde, so as to obtain borophenylic acid-modified high-ortho thermosetting phenolic resin; and uniformly mixing the borophenylic acid-modified high-ortho thermosetting phenolic resin with absolute ethyl alcohol, polyvinyl butyral and the like, and carrying out wet spinning and thermosetting, so as to obtain the borophenylic acid-modified high-ortho phenolic fibers. According to the method, the borophenylic acid-modified high-ortho thermosetting phenolic resin is taken as the raw materials and is sequentially subjected to wet spinning and thermosetting so as to generate the phenolic fibers, and the borophenylic acid-modified high-ortho phenolic fibers with good mechanical property and high limit oxygen index and heat resistance can be obtained without solution solidification; and the method is simple in process andhas an environment-friendly preparation process.

Description

technical field [0001] The invention belongs to the field of preparation of flame-retardant and temperature-resistant special fibers, and in particular relates to a method for preparing phenyl borate-modified high-ortho-position phenolic fibers by wet spinning. Background technique [0002] Phenolic fiber has less smoke during combustion, is non-toxic, has no melt dripping phenomenon, has instant high temperature resistance, high limiting oxygen index, heat resistance and flame retardancy and other properties. [0003] Although the preparation of phenolic fibers is suitable for the melt-spinning process, this method has been recognized and industrialized. However, due to the low molecular weight of the precursor phenolic resin, the nascent fiber is extremely brittle, and the subsequent process is difficult to operate; and how to make the fiber into an insoluble and infusible polycondensate with a three-dimensional crosslinked structure is the difficulty of this process. On ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/94D01F1/10D01F1/07C08G8/10C08G8/32C08G8/04C08G8/06C08G8/12
CPCC08G8/04C08G8/06C08G8/10C08G8/12C08G8/32D01F1/07D01F1/10D01F6/94
Inventor 杨凯焦明立任东雪宋梦刁泉张彩云李洁曹健刘红燕
Owner ZHONGYUAN ENGINEERING COLLEGE