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Treatment method for increasing carbon yield of phenolic fibers

A treatment method, phenolic fiber technology, applied in fiber treatment, fiber type, fiber chemical characteristics, etc., can solve the problems of low carbon residue rate, limited application, poor heat resistance of fibers, etc., and achieve low cost, convenient operation, and carbon fiber The effect of high yield

Inactive Publication Date: 2017-09-29
颜笑宇
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the preparation of phenolic-based carbon fiber is generally made by carbonization of the above-mentioned acid-formaldehyde cross-linked and cured fiber. The disadvantage is that the heat resistance of the fiber is poor, and the carbon residue rate at high temperature is low. The carbon residue rate at 800 ° C is generally 55%-60%, the carbon residue rate at 1000°C is only 50-55%, which limits its application and cannot adapt to higher operating temperatures and harsher operating environments

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1: A phenolic resin-based cured fiber with a residual carbon rate of 58.2% at 800°C and a residual carbon rate of 54.3% at 1000°C was used. First, soak 5g of cured phenolic fibers in a small dipping kettle of 1500ml absolute ethanol for 3 hours, then discharge the solution, and then vacuum to 40-50KPa for 1 hour at room temperature. Weigh 10g of boric acid, 10g of phosphoric acid, 3g of sulfuric acid, 0.2g of butyl borate, 0.2g of triethanolamine borate and dissolve in 1000ml of ethanol, disperse and dissolve uniformly with ultrasonic waves, and then inhale into a small dipping kettle. Under normal pressure, the soaked fibers were soaked in the prepared boron-phosphorus impregnation treatment solution, and treated at 110 °C for 6 h. The fibers were taken out and treated in a vacuum oven with a vacuum degree of 40 KPa at 100° C. for 1 h, and finally rinsed with deionized water. Fiber in (N 2 Atmosphere) 800 ℃ carbon residual rate can reach 63.7%, 1000 ℃ carbon ...

Embodiment 2

[0020] Example 2: The same phenolic resin-based curing fiber was used as in Example 1. In the same way as in Example 1, 10 g of the cured phenolic fiber was soaked. Weigh 10g of boric acid, 15g of phosphoric acid, 3g of sulfuric acid, 0.1g of butyl borate, 0.2g of triethanolamine borate and dissolve in 1200ml of ethanol, disperse and dissolve uniformly with ultrasonic waves, and then inhale into a small dipping kettle. Under normal pressure, the soaked fibers were soaked in the prepared boron-phosphorus impregnation treatment solution, and treated at 130 °C for 4 h. The fibers were taken out and treated in a vacuum oven with a vacuum degree of 30 KPa at 110° C. for 1 h, and finally rinsed with deionized water. Fiber in (N 2 Atmosphere) 800 ℃ carbon residual rate can reach 67.2%, 1000 ℃ carbon residual rate 63.1%.

Embodiment 3

[0021] Example 3: The same phenolic resin-based curing fiber was used as in Example 1. First, soak 10g of cured phenolic fibers in a small dipping kettle of 1500ml methanol organic solvent for 5h, then discharge the solution, and treat the fibers in a vacuum of 40-50KPa at room temperature for 1h. An immersion treatment liquid was prepared in the same manner as in Example 1. Under normal pressure, the soaked fibers were immersed in the prepared boron-phosphorus impregnation treatment solution, and treated at 120 °C for 5 h. The fibers were taken out and treated in a vacuum oven with a vacuum degree of 30KPa at 110°C for 1 h, and finally rinsed with deionized water. fiber in (N 2 Atmosphere) 800 ℃ carbon residual rate can reach 64.7%, 1000 ℃ carbon residual rate 61.5%.

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Abstract

The invention relates to a preparation method for increasing the carbon yield of phenolic resin-based fiber carbonization. A phenolic resin-based solidified fiber first undergoes vacuum impregnation, and is then further treated by high temperature in an ethanol solution of B, P and S inorganic acids and organic borate ester, so that the heat resistance of the fiber is greatly enhanced, and thereby a carbonized phenolic resin-based fiber with high carbon yield is prepared. The method does not affect the basic properties of the solidified fiber, but can greatly increase the heat resistance of the fiber. After carbonization, the carbon yield of the fiber under 800 DEG C (under N<2> atmosphere) can reach 63 to 70 percent, the carbon yield under 1000 DEG C is more than 60 percent, and the thermal decomposition separation peak of the fiber is relatively gentle.

Description

technical field [0001] The invention belongs to a preparation method of phenolic resin-based fibers, in particular to a preparation method for improving the residual carbon rate of phenolic resin-based fibers. Background technique [0002] At home and abroad, the preparation of phenolic resin fibers is mainly based on formaldehyde and phenol thermoplastic phenolic resins as raw materials, and after melt spinning, they are cross-linked in a hydrochloric acid and formaldehyde system to obtain body-shaped structural fibers. At present, in the high-tech military, aerospace and aviation fields, phenolic resin fiber is an extremely important ablation-resistant and heat-resistant material. With the improvement of the performance requirements for ablation resistance and heat protection materials in the high-tech technical field, higher requirements are put forward for the performance of phenolic fibers, especially the residual carbon rate. At present, the preparation of phenolic-ba...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F9/24D01F6/76D06M13/503D06M11/82D06M11/70D06M11/55D06M101/30
CPCD01F9/24D01F6/76D06M11/55D06M11/70D06M11/82D06M13/503D06M2101/30
Inventor 颜笑宇
Owner 颜笑宇
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