Method for preparing phenolic resin fiber of high molecular weight

A technology of phenolic resin fibers and high molecular weight, which is applied in the fields of fiber chemical characteristics, single-component synthetic polymer rayon, textiles and papermaking, and can solve problems such as high free phenol content, easy gelation, and metal impurities, and achieve High mechanical strength, short reaction time, and high degree of curing

Inactive Publication Date: 2013-03-20
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The patent number is 4299947, and the invention title is "High Molecular Weight Phenolic Resin". The divalent metal salt is used as the ortho-position induction catalyst, but the phenolic condensation process is easy to gel, the content of free phenol is high, and the resin contains metal impurities, which affects Ablation resistance and heat insulation performance of products

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Take m-cresol 0.5 mole as an example to prepare other raw materials used for high ortho position thermoplastic phenolic resin and the preparation method comprises the following steps:

[0032] 1. Ingredients

[0033] Take 54g of m-cresol and 10.5g of paraformaldehyde and add them to the autoclave, that is, the molar ratio of m-cresol and paraformaldehyde with the same quality of formaldehyde is 1:0.7, and paraformaldehyde is a low-grade polyformaldehyde with a polymerization degree of 8-100. Molecular weight pom.

[0034] 2. Chemical reaction

[0035] The temperature of the reactant was raised to 210°C under stirring, the pressure was 6.0MPa, and the reaction was carried out at constant temperature for 50 minutes.

[0036] 3. Preparation of phenolic resin

[0037] After the reaction, put the product into a vacuum drying oven, dry at 180°C for 5 hours, and control the pressure at -0.07MPa to prepare a phenolic resin.

[0038] The prepared phenolic resin adopts gel pe...

Embodiment 2

[0050] Take m-cresol 0.5 mole as an example to prepare other raw materials used for high ortho position thermoplastic phenolic resin and the preparation method comprises the following steps:

[0051]In batching process step 1, 54 g of m-cresol and 13.51 g of paraformaldehyde are taken, that is, the molar ratio of m-cresol to formaldehyde having the same quality as paraformaldehyde is 1:0.9. In step 2 of the chemical reaction process, the temperature of the reactants was raised to 210° C. under stirring, the pressure was 2.0 MPa, and the reaction was carried out at a constant temperature for 50 minutes. In step 3 of the process for preparing the phenolic resin, after the reaction, the product was put into a vacuum drying oven, dried at 180° C. for 5 hours, and the pressure was controlled at -0.07 MPa to prepare the phenolic resin. The measurement of the molecular weight of the phenolic resin is the same as in Example 1, and a phenolic resin with a molecular weight of 14,000 is ...

Embodiment 3

[0053] Take m-cresol 0.5 mole as an example to prepare other raw materials used for high ortho position thermoplastic phenolic resin and the preparation method comprises the following steps:

[0054] In batching process step 1, 54 g of m-cresol and 7.51 g of paraformaldehyde are taken, that is, the molar ratio of m-cresol and formaldehyde having the same quality as paraformaldehyde is 1:0.5. In step 2 of the chemical reaction process, the temperature of the reactants was raised to 210° C. under stirring, the pressure was 6.0 MPa, and the reaction was carried out at constant temperature for 50 minutes. In step 3 of the process for preparing the phenolic resin, after the reaction, the product was put into a vacuum drying oven, dried at 180° C. for 5 hours, and the pressure was controlled at -0.07 MPa to prepare the phenolic resin. The determination of the molecular weight of the phenolic resin and the calculation of the ortho-to-para ratio are the same as in Example 1, and a phe...

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Abstract

The invention relates to a method for preparing high molecular weight phenolic resin fibers, comprising the following processing steps of: mixture making, chemical reaction, preparation of phenolic resins, preparation of nascent fibers, preparation of solidifying liquid, solidification reaction, and washing and drying. The method adopts phenol and aldehyde as raw materials which are prepared into the high molecular weight phenolic resins under the condition of high temperature and high pressure; after melt-spinning, the solidification reaction is performed in the solidifying liquid and the high molecular weight phenolic resin fibers are prepared. The method has the advantages of short reaction time, high curing degree and so on; the high molecular weight phenolic resin fibers prepared by adoption of the method have high mechanical strength via test and are characterized by antiflamming, flame resistance, heat insulation, corrosion resistance and so on; the materials can be used as heat-insulating, insulating and corrosion resistant materials of an aerial aerocraft, as materials of fireproof and corrosion resistant clothes and also as materials of an acid and corrosion resistant filter, and are also raw materials of special fibers such as carbon fibers, graphite fibers, active carbon fibers, ion exchangers and so on.

Description

technical field [0001] The invention belongs to the technical field of polymer phenolic resin fiber materials, and in particular relates to a preparation method of highly cross-linked phenolic resin fibers. Background technique [0002] Phenolic fibers can be used as thermal insulation, insulation and corrosion-resistant materials in aerospace, national defense and aviation industries due to their flame-proof, flame-resistant, heat-insulating and corrosion-resistant properties. At the same time, it is also the primary raw material for special fibers such as carbon fiber, graphite fiber, activated carbon fiber and ion exchange. [0003] The U.S. Patent No. 3714111 discloses a method for preparing phenolic fibers, which is prepared by melt-spinning thermoplastic phenolic resins and then solidified in a bath of hydrochloric acid and formaldehyde. In this method, the as-spun fibers have to undergo several hours of reaction at 40°C and 60°C before the temperature is raised to 10...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): D01F6/76D01F11/08
Inventor董文生刘春玲殷勇刚梁冼朱丛星
OwnerSHAANXI NORMAL UNIV