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A kind of preparation method of phenolic fiber

A technology of phenolic fiber and phenolic resin, applied in the field of melt spinning, can solve the problems of low efficiency of phenolic resin melt spinning process, long curing and crosslinking time, complicated preparation process, etc. Difficult, uniform effect of fiber fineness

Active Publication Date: 2021-08-10
TANGSHAN KAILUAN CHEM TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Aiming at the existing problems such as complicated preparation process of spinnable phenolic resin, low efficiency of phenolic resin melt-spinning process, long curing and cross-linking time, and difficulty in industrialization, this patent uses general-purpose phenolic resin as raw material without increasing the process steps. Next, through the preparation of raw silk and the design of post-processing technology, the spinnability of phenolic resin can be improved, the problems of high brittleness and easy broken filaments can be overcome, the spinning speed can be increased, the post-processing time can be reduced, and the production efficiency of phenolic fiber can be greatly improved, which is suitable for industrial production

Method used

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  • A kind of preparation method of phenolic fiber
  • A kind of preparation method of phenolic fiber

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] The phenolic resin with a mass fraction of 99% and 1% copolymerized nylon are uniformly mixed, and the mixed material enters the twin-screw extruder for melting and blending to form a melt, and then the melt enters the single-screw connected to the head of the twin-screw extruder Extruder, and then enter the spinning assembly through the metering pump, the pressure of the assembly is 0.1MPa, the ejected silk enters the aspirator at 0.5m below the outlet hole, the aspirating speed is 300m / min, and the silk is conveyed The pipeline is transported to the fiber collection device to obtain the phenolic fiber precursor.

[0027] Soak the phenolic fiber precursors at 5°C into a solidification solution with a mass content of 20% formaldehyde, 16% hydrochloric acid, and 64% deionized water, and stay for 15 minutes; heat up to 40°C at 2°C / min , stay for 10min; then raise the temperature to 60℃ at 2℃ / min, stay for 20min; then raise the temperature to 80℃ at 2℃ / min, stay for 20min;...

Embodiment 2

[0029]Mix the phenolic resin with a mass fraction of 85% and 15% copolymerized nylon evenly, and the mixed material enters the twin-screw extruder to melt and blend to form a melt, and then the melt enters the single-screw connected to the head of the twin-screw extruder Extruder, and then enter the spinning assembly through the metering pump, the assembly pressure is 1.5MPa, the ejected silk enters the silk suction device at 1m below the silk outlet hole, the suction speed is 800m / min, and passes through the silk pipeline Transport to the collection device to obtain phenolic fiber precursors.

[0030] Soak the phenolic fiber precursors at 30°C in a solidification solution with a mass content of 20% formaldehyde, 16% hydrochloric acid, and 64% water, and stay for 30 minutes; heat up to 40°C at 2°C / min, and stay 10min; then heat up to 60°C at 2°C / min and stay for 20min; then heat up to 80°C at 2°C / min and stay for 20min; continue to heat up to boiling at 3°C / min and stay for 30...

Embodiment 3

[0032] Mix the phenolic resin with a mass fraction of 90% and 10% copolymerized nylon evenly, and the mixed material enters the twin-screw extruder to melt and blend to form a melt, and then the melt enters the single-screw connected to the head of the twin-screw extruder Extruder, and then enter the spinning assembly through the metering pump, the assembly pressure is 1.2MPa, the ejected silk enters the silk suction device at 1m below the silk outlet hole, the suction speed is 1800m / min, and passes through the silk delivery pipeline Transport to the collection device to obtain phenolic fiber precursors.

[0033] Soak the phenolic fiber precursors at 15°C into a solidification solution with a mass content of 20% formaldehyde, 16% hydrochloric acid, and 64% water, and stay for 30 minutes; heat up to 40°C at 3°C / min, and stay 10min; then heat up to 60°C at 3°C / min and stay for 20min; then heat up to 80°C at 3°C / min and stay for 20min; continue to heat up to boiling at 3°C / min an...

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Abstract

A preparation method of phenolic fiber, comprising the steps of uniformly mixing phenolic resin and spinning improver, the mixed materials are melted and blended by a twin-screw extruder to form a melt, and then the melt enters a single-screw extruder, The fiber is sprayed out through the spinneret assembly, sucked through the aspirator, and transported to the fiber collection device by the wire feeding pipeline to obtain the phenolic fiber precursor; the prepared phenolic fiber precursor is cured in formaldehyde, hydrochloric acid, and deionized water. The pre-crosslinking reaction is carried out first in the solution, and then the second crosslinking reaction is carried out by adopting a stepwise heating method, and finally the third crosslinking treatment is carried out at high temperature. This patent effectively improves the spinning efficiency of the phenolic fiber precursor, shortens the crosslinking reaction time of the phenolic fiber, and prepares the phenolic fiber with excellent mechanical properties and high char formation rate.

Description

technical field [0001] The invention belongs to the field of melt spinning, and in particular relates to a preparation method of phenolic fiber. Background technique [0002] Phenolic fiber is a highly cross-linked organic fiber prepared from thermoplastic phenolic resin or thermosetting phenolic resin, which can withstand 2500 o C high temperature, long-term use temperature 150-180 o C, good thermal insulation. In 1968, the American Emery Company successfully developed phenolic fiber for the development of flame-resistant and fire-resistant materials for aerospace. Because phenolic fiber has excellent flame retardancy and flame resistance, it can be used to make heat insulation and insulation materials for rocket nozzles, airplanes, trains, ships, and automobiles. In addition, phenolic fiber pure spinning or blended with other fibers can also be widely used as heat-resistant clothing, racing clothing, high-temperature furnace work clothing, fire-fighting clothing, acid-r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01D5/08D01D1/06D01D13/02D01F6/94D01F1/10D01F11/08
CPCD01D1/065D01D5/08D01D13/02D01F1/10D01F6/94D01F11/08
Inventor 李建华王亚涛马小丰金旺刘莉莉李洪娟董金明
Owner TANGSHAN KAILUAN CHEM TECH CO LTD
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