CN102587066B - Mucilage glue-based graphitized carbon fiber felt production process - Google Patents
Mucilage glue-based graphitized carbon fiber felt production process Download PDFInfo
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- CN102587066B CN102587066B CN201210053726.2A CN201210053726A CN102587066B CN 102587066 B CN102587066 B CN 102587066B CN 201210053726 A CN201210053726 A CN 201210053726A CN 102587066 B CN102587066 B CN 102587066B
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Abstract
The present invention relates to a kind of Mucilage glue-based graphitized carbon fiber felt production process, including following process: 1) viscose glue base fiber felt is passed sequentially through tank and catalyst tank by pulling device tractive, 2) moisture in fiber felt is extruded, and be dried；3) dried fiber felt carries out pre-oxidation treatment；4) carbon fiber felt after pre-oxidation treatment adds N2Protection successively enters low-temperature carbonization room and high temperature cabonization room, and the fiber felt after high temperature cabonization is through N2Protection clot, is cooled to room temperature；Complete the clot fiber felt after continuous prodution operation through enter graphitization process equipment, through stage heat up after, complete graphitization process, then pass through post processing, detect and pack after complete produce.Operation by pipelining, achieve carbon fiber felt from be catalyzed to pre-oxidize again to low temperature, high temperature cabonization procedure produce, overcome the properties of product existing for original interval metaplasia production. art uncontrollable, the inhomogenous deficiency of gram density of product, carbonizing degree.
Description
Technical field
The present invention relates to the production method of a kind of macromolecular fibre felt, specifically, relating to a kind of employing viscose glue base fiber felt is raw material, it is achieved the production method of the Novel viscose base graphitization carbon fiber felt of continuous prodution.
Background technology
China started to develop viscose-based carbon fiber from the eighties in last century, and its product applies all to military project aspect, through development for many years, developed into seriation, diversified carbon fiber series of products from the single product started most.Wherein apply most commonly used be C/C composite, it has lightweight, Gao Biqiang, high ratio mould and the property of superhigh temperature resistant, and along with the development of material preparation technology, C/C composite plays an important role in field of aerospace.Mucilage glue-based graphitized carbon fiber felt is the most increasingly subject to the people's attention as the basic material producing C/C composite, Mucilage glue-based graphitized carbon fiber felt selects viscose glue base chopped fiber, through shredding, comb net, acupuncture processing, make each to collude with forming parent felt to fiber frictionally each other together, through dipping (catalyst treatment), be dried, pre-oxidation, low-temperature carbonization and high temperature cabonization, after form through high temperature graphitization.Compared with braiding C/C composite, the intensity of the C/C composite that Mucilage glue-based graphitized carbon fiber felt is made is relatively low, but processing technique is simple, cycle is short, low cost, the highest in requirement of strength and require the position of thermal stress resistance, the larynx such as middle-size and small-size solid rocket motor nozzle serves as a contrast, and the C/C composite that Mucilage glue-based graphitized carbon fiber felt is made is successfully applied.It addition, the C/C composite that Mucilage glue-based graphitized carbon fiber felt is made has the loose structure of relatively lower thermal conductivity, thus also it is commonly used for ablating heat shield material.Although China is the biggest to the demand of this product, but owing to production technology is grasped by overseas enterprise, the enterprise of domestic production viscose-based carbon fiber felt is little, production technology is the most not mature enough, and a large amount of enterprises producing PAN fiber and activated carbon fiber do not produce ability and the maturation process of Mucilage glue-based graphitized carbon fiber felt.Cause China's a large amount of import of this series products.
Summary of the invention:
The purpose of the present invention is aiming at that China's current viscose-based carbon fiber felt production technology is immature, cannot realize continuous prodution, the carbon fiber felt poor-performing simultaneously produced is not enough, there is provided one can realize continuous prodution, the Novel viscose base graphitization carbon fiber felt that properties of product are identical with same kind of products at abroad simultaneously.
The technical scheme is that a kind of Mucilage glue-based graphitized carbon fiber felt production process, including the continuous production process of fiber felt carbonization, fiber felt graphitization process, postprocessing working procedures and detection packaging process, wherein the continuous production process of fiber felt carbonization includes following process:
1) viscose glue base fiber felt is passed sequentially through tank and catalyst tank by pulling device tractive, remove the sodium ion in the middle of viscose glue base fiber felt, and fiber felt is carried out carbonization protection；
2) pulling device continues tractive fiber felt, by pressure roller, is extruded by the moisture in fiber felt by pressure roller, then utilizes drying equipment to be dried fiber felt；
3), during dried fiber felt is pulled entrance and oxidation furnaces, pre-oxidation treatment is carried out；
4) carbon fiber felt after pre-oxidation treatment adds N2Protection enters low-temperature carbonization room and carries out low-temperature carbonization, and carbonization indoor temperature controls at 600 DEG C, and the carbon fiber felt after low-temperature carbonization is pulled entrance high temperature cabonization room, adds N2After protection, carrying out high temperature cabonization, carburizing temperature controls at 1100 DEG C, and the fiber felt after high temperature cabonization is through N2Protection clot, is cooled to room temperature；
Complete the clot fiber felt after continuous prodution operation through N2Protection, gets rid of in felt after air, enters graphitization process equipment, after stage heats up, complete graphitization process, then pass through post processing, detect and pack after complete to produce.
Preferably, the described catalyst in catalyst tank is ammonium bromide, ammonium dihydrogen phosphate and diammonium phosphate, and wherein ammonium bromide is that 2%-4%, ammonium dihydrogen phosphate and diammonium phosphate are respectively 4%-6%, and surplus is water.
In preferably described low-temperature carbonization and high temperature cabonization operation, carry out N2During protection, the N added2Preheat.
Preferably, the protection N being passed through2Admission line from one end of carbonizing chamber access, gas outlet is positioned at the other end of carbonizing chamber, and spiral pipeline shape hovers above in carbonizing chamber；The two ends of carbonizing chamber are provided with the most independent protection N2Gas outlet.
Preferably, after described high temperature cabonization terminates, carry out drop condensate prevention protection operation when coming out of the stove, utilize water vapour to cool down for the high-temperature carbon fiber felt come out of the stove, add N simultaneously2Protect, and the lower section of fiber felt arranges tank auxiliary temperature-reducing.
The invention have the benefit that first, operation by pipelining, achieve carbon fiber felt from be catalyzed to pre-oxidize again to low temperature, high temperature cabonization procedure produce, more conventional interval is changed production technology and is compared, production time shortens, production efficiency is greatly improved, production cost is significantly reduced, and overcomes the properties of product existing for original interval metaplasia production. art uncontrollable, the inhomogenous deficiency of gram density of product, carbonizing degree.Secondly; utilize catalyst to be catalyzed, can effectively reject be purchased from domestic fibre manufacturer at present the fiber precursor bought when present in metal ion, and fiber is protected by; make its slow reaction in low and high temperature carbonisation, it is ensured that the performance of fiber felt.Meanwhile, the processing step of preheating protection gas is used so that when being filled with protection gas, the cracked gas in carbonizing chamber will not be met condensation and be connect, it is to avoid the condensation impurity of generation pollutes fiber felt.It addition, the product after high temperature cabonization is protected through drop condensate prevention, by steam and N2Duplicate protection, it is ensured that the performance of product and quality.
Summary of the invention:
The specific embodiment of the present invention, a kind of Mucilage glue-based graphitized carbon fiber felt production process, including the continuous production process of fiber felt carbonization, fiber felt graphitization process, postprocessing working procedures and detection packaging process, wherein the continuous production process of fiber felt carbonization includes following process:
1) viscose glue base fiber felt is passed sequentially through tank and catalyst tank by pulling device tractive, remove the sodium ion in the middle of viscose glue base fiber felt, and fiber felt is carried out carbonization protection；The described catalyst in catalyst tank is ammonium bromide, ammonium dihydrogen phosphate and diammonium phosphate, and wherein ammonium bromide is that 2%-4%, ammonium dihydrogen phosphate and diammonium phosphate are respectively 4%-6%, and surplus is water.
2) pulling device continues tractive fiber felt, by pressure roller, is extruded by the moisture in fiber felt by pressure roller, then utilizes drying equipment to be dried fiber felt；
3), during dried fiber felt is pulled entrance and oxidation furnaces, pre-oxidation treatment is carried out；
4) carbon fiber felt after pre-oxidation treatment adds N2Protection enters low-temperature carbonization room and carries out low-temperature carbonization, and carbonization indoor temperature controls at 600 DEG C, and the carbon fiber felt after low-temperature carbonization is pulled entrance high temperature cabonization room, adds N2After protection, carrying out high temperature cabonization, carburizing temperature controls at 1100 DEG C, and the fiber felt after high temperature cabonization is through N2Protection clot, is cooled to room temperature；In described low-temperature carbonization and high temperature cabonization operation, carry out N2During protection, to the N added2Preheat, the protection N being passed through2Admission line from one end of carbonizing chamber access, gas outlet is positioned at the other end of carbonizing chamber, and spiral pipeline shape hovers above in carbonizing chamber；The two ends of carbonizing chamber are provided with the most independent protection N2Gas outlet.After described high temperature cabonization terminates, carry out drop condensate prevention protection operation when coming out of the stove, utilize water vapour to cool down for the high-temperature carbon fiber felt come out of the stove, add N simultaneously2Protect, and the lower section of fiber felt arranges tank auxiliary temperature-reducing.
Complete the clot fiber felt after continuous prodution operation through N2Protection, gets rid of in felt after air, enters graphitization process equipment, after stage heats up, complete graphitization process, then pass through post processing, detect and pack after complete to produce.
Claims (4)
1. a Mucilage glue-based graphitized carbon fiber felt production process, it is characterized in that, including the continuous production process of fiber felt carbonization, fiber felt graphitization process, postprocessing working procedures and detection packaging process, wherein the continuous production process of fiber felt carbonization includes following process:
1) viscose glue base fiber felt is passed sequentially through tank and catalyst tank by pulling device tractive, remove the sodium ion in the middle of viscose glue base fiber felt, and fiber felt is carried out carbonization protection；
2) pulling device continues tractive fiber felt, by pressure roller, is extruded by the moisture in fiber felt by pressure roller, then utilizes drying equipment to be dried fiber felt；
3), during dried fiber felt is pulled entrance pre-oxidation equipment, pre-oxidation treatment is carried out；
4) carbon fiber felt after pre-oxidation treatment adds N2Protection enters low-temperature carbonization room and carries out low-temperature carbonization, and carbonization indoor temperature controls at 600 DEG C, and the carbon fiber felt after low-temperature carbonization is pulled entrance high temperature cabonization room, adds N2After protection, carrying out high temperature cabonization, carburizing temperature controls at 1100 DEG C, and the fiber felt after high temperature cabonization is through N2Protection clot, is cooled to room temperature；After described high temperature cabonization terminates, carry out drop condensate prevention protection operation when coming out of the stove, utilize water vapour to cool down for the high-temperature carbon fiber felt come out of the stove, add N simultaneously2Protect, and the lower section of fiber felt arranges tank auxiliary temperature-reducing；
Complete the clot fiber felt after continuous prodution operation through N2Protection, gets rid of in felt after air, enters graphitization process equipment, after stage heats up, complete graphitization process, then pass through post processing, detect and pack after complete to produce.
2. Mucilage glue-based graphitized carbon fiber felt production process as claimed in claim 1, it is characterized in that, the described catalyst in catalyst tank is ammonium bromide, ammonium dihydrogen phosphate and diammonium phosphate, wherein ammonium bromide is 2%-4%, ammonium dihydrogen phosphate and diammonium phosphate are respectively 4%-6%, and surplus is water.
3. Mucilage glue-based graphitized carbon fiber felt production process as claimed in claim 1, it is characterised in that in described low-temperature carbonization and high temperature cabonization operation, carry out N2During protection, the N added2Preheat.
4. Mucilage glue-based graphitized carbon fiber felt production process as claimed in claim 3, it is characterised in that the protection N being passed through2Admission line from one end of carbonizing chamber access, gas outlet is positioned at the other end of carbonizing chamber, and spiral pipeline shape hovers above in carbonizing chamber；The two ends of carbonizing chamber are provided with the most independent protection N2Gas outlet.
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| CN201210053726.2A CN102587066B (en) | 2012-03-05 | 2012-03-05 | Mucilage glue-based graphitized carbon fiber felt production process |
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| CN103668831B (en) * | 2013-12-11 | 2015-10-28 | 杨学斌 | Active carbon fiber felt, cloth continuous production technique |
| CN103696195A (en) * | 2013-12-11 | 2014-04-02 | 杨学斌 | Secondary carbonization technology for producing activated carbon fibers |
| CN105064031A (en) * | 2015-08-20 | 2015-11-18 | 北京化工大学 | Method for preparing high-modulus carbon fibers at low temperature |
| CN109457430A (en) * | 2018-11-08 | 2019-03-12 | 嘉兴纳科新材料有限公司 | A kind of preparation method of electric heating carbon fibre fabric |
| CN109957860B (en) * | 2019-04-01 | 2021-10-22 | 梁继选 | Preparation method of viscose high-temperature graphite carbon fiber |
| CN110512414A (en) * | 2019-08-30 | 2019-11-29 | 四川骏瑞碳纤维材料有限公司 | A kind of anti-oxidant viscose-based graphite felt and its preparation process |
| CN113249825A (en) * | 2021-05-10 | 2021-08-13 | 深圳市华鼎星科技有限公司 | High-conductivity carbon fiber applied to touch screen and preparation method and application thereof |
| CN113684639B (en) * | 2021-08-23 | 2022-06-14 | 安徽弘昌新材料有限公司 | Pre-oxidation furnace, processing equipment and processing technology for processing non-woven felt |
| CN113774604A (en) * | 2021-09-17 | 2021-12-10 | 安徽弘昌新材料有限公司 | Preparation process of viscose-based carbon fiber composite graphite felt and prepared graphite felt |
| CN113862942B (en) * | 2021-09-29 | 2023-08-15 | 因达孚先进材料(苏州)股份有限公司 | Pre-oxidation furnace system for producing viscose-based carbon felt |
| CN113972024A (en) * | 2021-10-29 | 2022-01-25 | 吉林聚能新型炭材料股份有限公司 | Carbon-based high-length-diameter-ratio flexible conductive material and preparation method thereof |
| CN115182154B (en) * | 2022-07-22 | 2024-01-26 | 江苏米格新材料股份有限公司 | Ultra-high-purity viscose-based graphite felt and preparation method and application thereof |
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