Preparing method of phenolic fibers

A technology of phenolic fiber and phenolic resin, which is 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., and achieve stable and continuous spinning and high spinning efficiency High and uniform fiber fineness

Active Publication Date: 2020-08-07
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 s

Method used

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  • Preparing method of phenolic fibers
  • Preparing method of phenolic fibers

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

The invention discloses a preparing method of phenolic fibers. The method comprises the steps that phenolic resin and a spinning improver are evenly mixed, a mixed material is subjected to melt blending through a dual-screw extruder to form a melt, the melt enters a single-screw extruder, the fibers are sprayed out through a fiber spraying assembly, the fibers are sucked through a fiber sucking device, the fibers are conveyed to a fiber collecting device by a fiber conveying pipe, and phenolic fiber protofilaments are obtained; and the prepared phenolic fiber protofilaments are subjected to apre-crosslinking reaction in a solidifying solution composed of formaldehyde, hydrochloric acid and deionized water, a ladder type heating manner is adopted for carrying out a second-time crosslinkingreaction, and finally, at the high temperature, third-time crosslinking treatment is carried out. The spinning efficiency of the phenolic fiber protofilaments can be effectively improved, the phenolic fiber crosslinking reaction time can be shortened, and the phenolic fibers which are excellent in mechanical property, and high in char yield can be prepared.

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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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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