Method of producing carbon fibrous material

FIELD: process engineering.

SUBSTANCE: proposed method comprises processing initial cellulose fibrous material by liquid-phase composition containing silanol groups with molecular weight varying from 900 to 2400 and viscosity varying from 520 to 1700 cPs, and 2-7%-water solution of fire retardant. Processed material is dried to 105-125°C for 60-120 min. Then, carbonisation is performed in air at 140-170°C for 25-40 min. Carbonisation is terminated at 700°C to proceed with high-temperature processing at, at least, 2200°C.

EFFECT: high physical properties and yield.

4 cl, 6 ex

 

The invention relates to the field of production of carbon fibrous materials used as reinforcing fillers for composite materials, and is intended for the modification of the original cellulosic fibrous materials.

Known continuous method for the production of carbon fiber material, comprising processing the hydrated cellulose fiber material with solutions of silicone resins in an organic solvent and subsequent carbonization and graphitization in the conditions of deformation, in which the carbonization of hydrate cellulose fibrous material is subjected to relaxation by heating it to 120-300°C for 0.4 to 2.0 h and cooling to 18-30°C for 0.05 to 0.2 h, after which the heating is repeated in the specified mode when the degree of deformation of this material 0-(-10)%, the carbonization is carried out at a high temperature from 180°C to 600°C, while in the range of 300-400°C, the material is subjected to a deformation degree(-25)-(+30)%, graphitization lead when 900-2800°C when the degree of deformation(-10)-(+25)%, and formed during carbonization products of pyrolysis are removed from the working zone with a temperature of 350-450°C; graphitization carried out in the presence of carborundorum compounds (see RF patent №2045472, IPC SW 31/02, 10.10.1995).

This method has the disadvantage that provides for the processing of fibrous material before the study is th relaxation solution polymethylsiloxane in acetone, which is easily inflammable toxic substance.

In addition, carbon fibers and materials based on it have increased values of the coefficient of variation in physico-mechanical characteristics.

Closest to the claimed method is the production of carbon fiber material by processing the original cellulosic fibrous material 5-20%aqueous solution of the flame retardant, heat treatment in air, carbonization at a gradual increase in temperature up to 600°C and the subsequent high-temperature treatment in an inert atmosphere up to 2200°C (U.S. Pat. RU # 2047674, IPC D01F 9/12, 10.11.1995).

The known method has the disadvantage that you can get carbon fiber materials, physico-acid and the performance of which is not high enough.

The technical result when using the claimed invention is the production of carbon fibrous materials with high physical and mechanical properties while maintaining a uniformly high values of the yield of carbon residue.

This technical result is achieved by a method for production of carbon fiber material, characterized by the processing of the original cellulosic fibrous material in a liquid-phase composition comprising an aqueous solution of a flame retardant, a heat treatment in air, the carbonation in post the foam temperature rise and subsequent high-temperature treatment in an inert atmosphere, according to the invention, the liquid-phase composition for the treatment of raw fibrous material additionally contains 10-20%water emulsion of the oligomeric resin containing 7-13,4% silanol groups corresponding to the General formula

HO{[MeSi(OH)O][Me2SiO]m}nH,

where Me is methyl; m and n are integers or fractional numbers: m=1-3, n=3-10 with a molecular weight of from 900 to 2400 and a viscosity in the range from 520 to 1700 SP, using 2-7%aqueous solution of the flame retardant, and the treated liquid-phase composition of the fibrous material is dried at a temperature of 105-125°C for 60-120 min, heat treatment in air is carried out at a temperature of 140-170°C for 25-40 min, carbonation finish at 700°C, and subsequent high-temperature treatment is carried out at temperatures of at least 2200°C.

In addition, the technical result is achieved by the fact that, as a flame retardant used substance from the group comprising haloesters, solfataras, phosphorus, boron salt of ammonium, potassium, sodium, urea or mixtures thereof; processing the original pulp of fibrous materials is carried out by dipping in a liquid composition or by spraying the liquid-phase composition; as a source of cellulose fibrous materials using various textile structures, such as fabrics or knitted fabric, whether or not the adjusted material of viscose technical threads.

The achievement of the technical result became possible after the conduct of scientific experimental research and field testing. It was found that to achieve the desired characteristics of carbon fibers and materials when applying silicone resin with a high content of silanol groups, namely from 7% to 13.4%. Such resins have been selected from the subclass hydroxypoly(oligo)methylsiloxanes and synthesized by the method described in the book. Lmonukili "Chemistry and technology of Organoelement monomers and polymers", M., Chemistry, 1998, str-313.

The method includes the following stages:

1. Partial etherification mixture methylchlorosilanes butyl alcohol.

2. Hydrolytic deposition of partially esterified methylchlorosilanes.

3. Distillation of the solvent.

The method is as follows.

In a reactor equipped with a stirrer, thermometer and reflux condenser, load estimated number of methyltrichlorosilane (MTHS), clear (DMDCS) and toluene. Under stirring, the reactor type butanol T≤60°C. the resulting product was incubated for 3 hours. Then the reaction mixture was hydrolized with water at T≤30°C. Toluene-butanolic solution oligomerisation resin is washed with water until neutral and the solvent is distilled off under a pressure of 133 PA at 45-50 is C.

The obtained resin belong to the category of low viscosity oligomers with hydroxyl groups at the silicon atom, which correspond to the General chemical formula

HO{[MeSi(OH)O][Me2SiO]m}nH,

where Me is methyl; m and n are integers or fractional numbers: m=1-3, n=3-10.

The presence in the resin of the polar groups and the low viscosity give the ability to evenly moisten viscose textile patterns. Due to the high content of silanol groups (7-13,4%) with a further heat treatment, is their interaction, including the hydroxyl viscose fibers with the formation of cross-linked structures, chemically related to fiber in the course of polycondensation processes. Essentially these structures protect the fiber from unwanted reactions with the products of pyrolysis.

To identify pitches and determine the chemical and physical properties used the following methods and instruments. The reaction products were investigated by NMR-1H and29Si spectroscopy spectrometer Broker AM 360 operating frequency 360.13 MHz. The content of silanol groups in the resins was determined by volumetric method on the device Servicenow the amount of released N2in the reaction product with LiAlH4. The molecular weight of the resins was determined by gel chromatograph firm "Knauer", storagereview columns Shodex" (calibrated relative to polystyrene). Viscosity productionprocess using Brookfield viscometer firm "Anton Paar", model DV-1P.

Synthesis is carried out by the above method.

Example A. Take 149 g MTHS, 232 g DMDS, 190 ml of toluene, 76 g of butanol and 120 ml of water. Get 174 g of the oligomeric resin with the content of silanol groups 10,91 wt.%, the corresponding General formula: HO{[MeSi(OH)O][Me2SiO]m}nH, where Me is methyl; m=1,8, n=5. M.M. resin 1170, the viscosity of 690 SP.

Example B. Take 149 g MTHS, 387 g DMDS, 270 ml of toluene, 108 ml of butanol and 162 ml of water. Receive 250 g of the oligomeric resin with the content of silanol groups to 9.32 wt.%, the corresponding General formula: HO{[MeSi(OH)O][Me2SiO]m}nH, where Me is methyl; m=3, n=3,1. M.M. resin 900, the viscosity of 520 SP.

Example Century. Take 149 g MTHS, 374 g DMDS, 260 ml of toluene, 106 ml of butanol and 158 ml of water. Get 244 g of the oligomeric resin, containing silanol groups 7 wt.%, the corresponding General formula: HO{[MeSi(OH)O][Me2SiO]m}nH, where Me is methyl, m=2,9, n=8,2. M.M. resin 2400, the viscosity of 1700 CPs.

Example, Take 300 g MTHS, 258 g DMDS, 280 ml of toluene, 109 ml of butanol and 180 ml of water. Get 246 g of the oligomeric resin with the content of silanol groups of 13.4 wt.%, the corresponding General formula: HO{[MeSi(OH)O][Me2SiO]m}nH, where Me is methyl where m=1, n=10. M.M. resin 1518, the viscosity of 1040 SP.

As a source of cellulose fibrous material used textile structure in the form of viscose industrial single-layer fabric brand TVs-2P or knitwear brand P Is T-3/2, or non-woven viscose material, or a multilayer fabric brand ET-4.

The claimed method of production of carbon fibrous materials is carried out in a continuous mode as follows.

The original cellulosic fibrous material - viscose industrial single-layer fabric brand TVs-2P or knitwear brand OEM-3/2, or non-woven viscose material, or a multilayer fabric brand ET-4, produced on a textile machine, is fed into a bath of liquid-phase composition that contains 10-20%water emulsion of the oligomeric resin containing 7-13,4% silanol groups corresponding to the General formula HO{[MeSi(OH)O][Me2SiO]m}nH, where

Me is methyl; m and n are integers or fractional numbers: m=1-3, n=3-10 with a molecular weight of from 900 to 2400 and a viscosity in the range from 520 to 1700 SP, and 2-7%aqueous solution of the flame retardant. To remove moisture treated material is dried in air at a temperature of 105-125°C for 60-120 minutes. When carrying out the subsequent stage of the process - heat treatment in air (thermo relaxation) at a temperature of 140-170°C for 25-40 minutes is the reduction of internal stresses formed in the viscose technical threads in forming and subsequent textile processing, as well as by thermal oxidation of chemical compounds deposited on the viscose materials by okunan the I in the liquid-phase composition or spraying of liquid-phase composition and forming on the surface of the fibers "protective layer". The carbonization is carried out at a gradual increase in temperature and finish at 700°C and a high temperature treatment is carried out in an inert atmosphere at temperatures of at least 2200°C. the Processing of the original cellulosic fibrous material is carried out by spraying the liquid-phase composition.

The claimed method is illustrated by examples.

Example 1. Fabric viscose technical TVs-2P treated by dipping in liquid-phase composition containing 20%water emulsion-based oligomeric resin obtained in example As and 5%aqueous solution of diammonium phosphate. To remove moisture treated viscose fabric is dried at a temperature of 125°C for 60 minutes. Heat treatment of the material in air is carried out at a temperature of 170°C for 25 minutes. Then carry out carbonation with a gradual increase in temperature, which finished at a temperature of 700°C, and subsequent heat treatment at a temperature of 2200°C. in an inert atmosphere. The obtained carbon fibrous material has the following characteristics:

the breaking load on the basis of wide strips of 5 cmN
the yield of carbon residue31,1%
5,8%

Example 2. Fabric viscose knitted HTP-3/2 treated by dipping in liquid-phase composition containing 15%water emulsion-based oligomeric resin obtained in example B, and 7%aqueous solution of triethanolamine lauryl sulphate. To remove moisture treated viscose knitted fabric is dried at 110°C for 80 minutes. Heat treatment of the material in air is carried out at a temperature of 140°C for 40 minutes. Then carry out carbonation with a gradual increase in temperature, which finished at a temperature of 700°C, and subsequent heat treatment at a temperature of 2300°C. in an inert atmosphere. The obtained carbon fibrous material has the following characteristics:

the breaking load on the basis of wide strips of 5 cmN
the yield of carbon residue30,3%
the coefficient of variation for the yield of carbon residue5,4%

Example 3. Non-woven viscose material is treated by spraying liquid compositions containing a 10%aqueous emulsion-based oligomeric resin obtained in example C, and 2%nybody solution of ammonium chloride. To remove moisture treated non-woven viscose material is dried at 105°C for 120 minutes. Heat treatment of the material in air is carried out at a temperature of 150°C for 40 minutes. Carbonization and subsequent high-temperature treatment is carried out as in example 1. The obtained carbon fibrous material has the following characteristics:

the breaking load of a strip width of 5 cmN
the yield of carbon residue32,0%
the coefficient of variation for the yield of carbon residue6,7%

Example 4. Layered viscose technical fabric TVM-4 treated by spraying a liquid composition containing 13%water emulsion-based oligomeric resin obtained in example G, and 3%aqueous solution of urea. To remove moisture treated fabric is dried at a temperature of 115°C for 120 minutes. Heat treatment of the material in air is carried out at a temperature of 170°C for 40 minutes. Carbonization and subsequent high-temperature treatment is carried out according to example 2. The obtained carbon fibrous material has the following characteristics:

the breaking load on the basis of wide strips of 5 cmN
the yield of carbon residue28,9%
the coefficient of variation for the yield of carbon residue7,1%

Example 5. Fabric viscose technical single-layer FA-2P treated by spraying a liquid composition containing 14%water emulsion-based oligomeric resin obtained in example B, and 5%aqueous solution tetraborate sodium. All thermal processing: drying, heat treatment in air, and high temperature carbonization treatment is carried out as in example 1. The obtained carbon fibrous material has the following characteristics:

the breaking load on the basis of wide strips of 5 cmN
the yield of carbon residue29,9%
the coefficient of variation for the yield of carbon residue6,2%

Example 6. Layered viscose technical fabric ET-4 is treated by dipping in liquid-phase composition containing 12%water emulsion oligomers the second resin, obtained in example C, and 4%aqueous solution of ammonium sulfate. All thermal processing: drying, heat treatment in air, and high temperature carbonization treatment is carried out according to example 2. The obtained carbon fibrous material has the following characteristics:

the breaking load on the basis of wide strips of 5 cmN
the yield of carbon residue29,6%
the coefficient of variation for the yield of carbon residue6,8%.

1. Method for the production of carbon fiber material, characterized by the processing of the original cellulosic fibrous material in a liquid-phase composition comprising an aqueous solution of a flame retardant, a heat treatment in air, the carbonation with a gradual increase in temperature and subsequent high-temperature treatment in an inert atmosphere, wherein the liquid composition further comprises 10-20%aqueous emulsion of the oligomeric resin containing 7-13,4% silanol groups corresponding to the General formula:
HO{[MeSi(OH)O][Me2SiO]m}nH, where
Me is methyl; m and n are integers or fractional numbers: m=1-3, n=3-10, with a molecular weight of from 900 to 2400 and viscosity in before the crystals from 520 to 1700 SP, using 2-7%aqueous solution of the flame retardant, and the treated liquid-phase composition of the fibrous material is dried at a temperature of 105-125°C for 60-120 min, heat treatment in air is carried out at a temperature of 140-170°C for 25-40 min, carbonation finish at 700°C, and subsequent high-temperature treatment is carried out at temperatures of at least 2200°C.

2. The method according to claim 1, characterized in that as a flame retardant used substance selected from the group comprising haloesters, solfataras, phosphorus, boron salt of ammonium, potassium, sodium, urea or mixtures thereof.

3. The method according to claim 1, characterized in that the processing of the original pulp of fibrous materials is carried out by dipping in a liquid composition or by spraying the liquid-phase composition.

4. The method according to claim 1, characterized in that as the source of cellulose fibrous materials using various textile structures, such as fabrics or knitted fabric, or nonwoven viscose technical yarns.



 

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