CN100497773C - Method for preparing glue-based carbon fiber - Google Patents
Method for preparing glue-based carbon fiber Download PDFInfo
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- CN100497773C CN100497773C CNB2007100563162A CN200710056316A CN100497773C CN 100497773 C CN100497773 C CN 100497773C CN B2007100563162 A CNB2007100563162 A CN B2007100563162A CN 200710056316 A CN200710056316 A CN 200710056316A CN 100497773 C CN100497773 C CN 100497773C
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- carbon fiber
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- based carbon
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Abstract
A preparation method of viscose-based carbon fiber is characterized in that a. viscose precursor fiber after being stranded and twisted is taken as raw material and is soaked and rinsed for one hour with 95-100 DEG C hot water; b. the raw material is dried in a drier at a temperature of 75-80 DEG C; c. the dried material is soaked again in diammonium hydrogenorthophosphate solution with 5 percent concentration for half an hour at 60 DEG C; d. then the material is dried again in the drier at 75-80 DEG C; e. the dried material is loaded to a composite bracket of iron-chrome and phenolic aldehyde fiber and then placed for carbonization into a shaft-shaped carbonization furnace, the temperature of which is gradually raised to 930 DEG C, the temperature of which is kept for 30 minutes. The material in the furnace is carbonized for 27 hours; f. the carbon fiber is cooled naturally to ambient temperature in the furnace and then taken out for production of viscose-based carbon fiber product. The invention removes impurity remained in raw material and has carbonization rate as high as 33.5 percent, tensile strength 453MPa, which is one time as much as the previous product.
Description
Technical field
The present invention relates to a kind of method for preparing viscose-based carbon fiber.
Background technology
The tensile strength of existing viscose-based carbon fiber product is about 200Mpa, product contains impurity, because the fast development of application technology is more and more higher to the tensile strength requirement of this product, harsh more to impure requirement, therefore new problem has been proposed to manufacturing enterprise.The problem such as tensile strength, impurity that influences carbon fiber has all multifactor in technical process, more as the medicine that can make antiscorching, diammonium hydrogen phosphate, ammonium chloride, ammonium sulfate, ammonium bromide, sodium tetraborate, zinc chloride, urea or glacial acetic acid etc. all can, antiscorching drug concentration commonly used and the isoparametric range of choice of temperature be broad also, therefore based on prior art, improve technology, select optimum process condition, be realize improving the quality of products, performance and yield is most economical, one of method fast.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of viscose-based carbon fiber, this method can improve tensile strength and yield based on prior art, reduce the impurity of viscose carbon fibres.
The present invention adopts following method to realize: a kind of preparation method of viscose-based carbon fiber is characterized in that: a, be raw material with the rayon fiber behind the doubling twisting, with 95-100 ℃ of hot-water soak 20 minutes, change water and soaked 30 minutes again that rinsing is 10 minutes then; B, use oven for drying, temperature is 75-80 ℃ in the baking oven; It is in 5% the ammonium dibasic phosphate aqueous solution that c, the material after will drying are immersed in concentration again, 60 ℃ of soaking temperatures, soak time 30 minutes; D, use oven for drying, temperature is 75-80 ℃ in the baking oven; E, the material of oven dry is packed in siderochrome aluminium and phenolic aldehyde cloth compound basket, compound basket is put into flue, and flue is put into well formula carbide furnace body of heater and is carried out carbonization, and furnace temperature rises to 930 ℃ gradually, constant temperature is 30 minutes in the time of 930 ℃, begins to finish carbonization altogether 27 hours to constant temperature from intensification; F, flue is hung out body of heater, carbon fiber naturally cools to room temperature in flue, takes out then and makes the viscose-based carbon fiber product.
Draw through repetition test, rayon fiber is with 95-100 ℃ of hot wash 1 hour, removes that remaining impurities improves yield simultaneously in the raw material, and the carbonization yield reaches 33.5%.The viscose-based carbon fiber tensile strength of producing with present technique reaches 453Mpa, doubles than the tensile strength 200Mpa of existing product.Experiment shows that the ammonium dibasic phosphate aqueous solution of selection 5% is made antiscorching in this technology, is the optium concentration scheme that improves tensile strength.The material surface recombination of packing into has in the siderochrome aluminium basket of phenolic aldehyde cloth, falls in the material because phenolic aldehyde cloth can prevent basket, flue, the iron sheet that comes off, and can prevent to collapse in the body of heater iron scale.Present technique washes with water has removed remaining impurities in the raw material, and with compound basket of impurity that has prevented to bring in the carbonisation, so the impurity level in the product reduces to minimum or do not have impurity.Because each position temperature stabilization of well formula carbide furnace, compound basket blobs can not occur, so quality is stablized, improved to properties of product.The effect of making antiscorching with diammonium hydrogen phosphate is: the thermal decomposition that can make viscose is carried out under wideer temperature range and relatively low temperature, makes the oxidation Decomposition time lengthening, and the fiber surface hole defect reduces.In addition, the existence of antiscorching also helps the deposition of carbon at fiber surface, can remedy the blemish of fiber, improves the mechanical property of viscose-based carbon fiber, thereby has improved the tensile strength of viscose-based carbon fiber.Antiscorching suppresses the effect that the laevoglucose tar material produces in addition, and the tar content when making the fiber carbonization reduces, thereby has reduced the decomposition loss of carbon, has finally improved the carbonization yield.
Table 1 is the influence to the carbonization yield of washing temperature in this technology, time
Experiment shows: 100 ℃ of 14# sample water temperatures, and wash time 1 hour, carbonization yield 33.5%, effect is best.
Table 2 be in this technology diammonium hydrogen phosphate concentration to the viscose-based carbon fiber effects of tensile strength
| Sample number | Concentration % | Tensile strength MPa |
| 1# | 0 | 100.5 |
| 2# | 0.5 | 170 |
| 3# | 1.5 | 212 |
| 4# | 3.0 | 312 |
| 5# | 4.0 | 375 |
| 6# | 5.0 | 453 |
| 7# | 10 | 358 |
| 8# | 20 | 349 |
Experiment shows: the diammonium hydrogen phosphate of 6# sample concentration 5% improves the tensile strength of viscose carbon fibres, and effect is best.
The specific embodiment
Get 60 kilograms of the rayon fibers of 120D doubling twisting, putting into water temperature 95-100 ℃ of pond soaked 20 minutes, changing water soaked 30 minutes again, rinsing was taken out in 10 minutes then, impurity in the material is stayed in the water, material washing back oven for drying, temperature is 75-80 ℃ in the baking oven, with at least 2 hours, with being immersed in concentration behind the dry materials again is in 5% the ammonium dibasic phosphate aqueous solution, 60 ℃ of soaking temperatures, soak time at least 30 minutes, take out the back oven for drying, be warming up to 75-80 ℃ in the baking oven, be incubated at least 10 hours, again material is packed in the compound basket that siderochrome aluminium and phenolic aldehyde cloth makes, compound basket is put into flue, flue is put into the carbonization of well formula carbide furnace body of heater, and carbide furnace was warming up to 930 ℃ gradually from room temperature, with 27 hours, constant temperature is 30 minutes in the time of 930 ℃, then flue is hung out body of heater, carbon fiber is cooling taking-up in 8 hours naturally in flue, produces 20.1 kilograms of viscose-based carbon fiber products, tensile strength 450Mpa, originally the viscose-based carbon fiber product tensile strength of Sheng Chaning is 200Mpa, and the carbonization yield reaches 33.5%, the product free from admixture.
Claims (1)
1, a kind of preparation method of viscose-based carbon fiber is characterized in that: a, be raw material with the rayon fiber behind the doubling twisting, with 95-100 ℃ of hot-water soak 20 minutes, change water and soaked 30 minutes again that rinsing is 10 minutes then; B, use oven for drying, temperature is 75-80 ℃ in the baking oven; It is in 5% the ammonium dibasic phosphate aqueous solution that c, the material after will drying are immersed in concentration again, 60 ℃ of soaking temperatures, soak time 30 minutes; D, use oven for drying, temperature is 75-80 ℃ in the baking oven; E, the material of oven dry is packed in siderochrome aluminium and phenolic aldehyde cloth compound basket, compound basket is put into flue, and flue is put into well formula carbide furnace body of heater and is carried out carbonization, and furnace temperature rises to 930 ℃ gradually, constant temperature is 30 minutes in the time of 930 ℃, begins to finish carbonization altogether 27 hours to constant temperature from intensification; F, flue is hung out body of heater, carbon fiber naturally cools to room temperature in flue, takes out then and makes the viscose-based carbon fiber product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100563162A CN100497773C (en) | 2007-11-05 | 2007-11-05 | Method for preparing glue-based carbon fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007100563162A CN100497773C (en) | 2007-11-05 | 2007-11-05 | Method for preparing glue-based carbon fiber |
Publications (2)
| Publication Number | Publication Date |
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| CN101158063A CN101158063A (en) | 2008-04-09 |
| CN100497773C true CN100497773C (en) | 2009-06-10 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2007100563162A Active CN100497773C (en) | 2007-11-05 | 2007-11-05 | Method for preparing glue-based carbon fiber |
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| CN (1) | CN100497773C (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105064031A (en) * | 2015-08-20 | 2015-11-18 | 北京化工大学 | Method for preparing high-modulus carbon fibers at low temperature |
| CN109957860B (en) * | 2019-04-01 | 2021-10-22 | 梁继选 | Preparation method of viscose high-temperature graphite carbon fiber |
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2007
- 2007-11-05 CN CNB2007100563162A patent/CN100497773C/en active Active
Non-Patent Citations (4)
| Title |
|---|
| 粘胶基炭纤维毡的制备. 徐洪新等.辽宁化工，第30卷第11期. 2001 |
| 粘胶基炭纤维毡的制备. 徐洪新等.辽宁化工，第30卷第11期. 2001 * |
| 粘胶活性碳纤维预浸剂的热分解作用及效能评选. 曾凡龙等.材料科学与工程学报，第22卷第5期. 2004 |
| 粘胶活性碳纤维预浸剂的热分解作用及效能评选. 曾凡龙等.材料科学与工程学报，第22卷第5期. 2004 * |
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| CN101158063A (en) | 2008-04-09 |
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Owner name: JIYAN HIGH SCIENCE FIBRE CO., LTD., JILIN CITY Free format text: FORMER OWNER: JILIN HANGYUAN CARBON FIBRES CO., LTD. Effective date: 20080516 |
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Effective date of registration: 20080516 Address after: Postal code nine, 516-1 Street station, Jilin economic and Technological Development Zone, Jilin, China: 132101 Applicant after: Jilin Jiyan High-tech Fibers Co., Ltd. Address before: Postal code nine, 516-1 Street station, Jilin economic and Technological Development Zone, Jilin, China: 132101 Applicant before: Jilin Hangyuan Carbon Fibres Co., Ltd. |
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