CN116641158A - Composite carbon fiber preparation process - Google Patents
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 26
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 26
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 239000002131 composite material Substances 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000011282 treatment Methods 0.000 claims abstract description 41
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 26
- 230000003647 oxidation Effects 0.000 claims abstract description 20
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000004140 cleaning Methods 0.000 claims abstract description 13
- 239000002243 precursor Substances 0.000 claims abstract description 10
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 7
- 238000003763 carbonization Methods 0.000 claims description 26
- 239000007788 liquid Substances 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 238000002791 soaking Methods 0.000 claims description 11
- 238000009987 spinning Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000011248 coating agent Substances 0.000 claims description 8
- 238000000576 coating method Methods 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 239000012153 distilled water Substances 0.000 claims description 6
- 238000007654 immersion Methods 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 239000006185 dispersion Substances 0.000 claims description 5
- 238000002166 wet spinning Methods 0.000 claims description 5
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 239000005011 phenolic resin Substances 0.000 claims description 4
- 229920001568 phenolic resin Polymers 0.000 claims description 4
- 239000003495 polar organic solvent Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 238000010000 carbonizing Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 9
- 239000000835 fiber Substances 0.000 description 8
- 230000008901 benefit Effects 0.000 description 6
- 238000002156 mixing Methods 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 229920002972 Acrylic fiber Polymers 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005674 electromagnetic induction Effects 0.000 description 1
- 238000005338 heat storage Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/77—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof
- D06M11/79—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with silicon or compounds thereof with silicon dioxide, silicic acids or their salts
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/39—Aldehyde resins; Ketone resins; Polyacetals
- D06M15/41—Phenol-aldehyde or phenol-ketone resins
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Inorganic Fibers (AREA)
Abstract
Description
技术领域technical field
本发明涉及复合型碳纤维制备技术领域，具体为一种复合型碳纤维制备工艺。The invention relates to the technical field of composite carbon fiber preparation, in particular to a composite carbon fiber preparation process.
背景技术Background technique
碳纤维指的是含碳量在90％以上的高强度高模量纤维。耐高温居所有化纤之首。用腈纶和粘胶纤维做原料，经高温氧化碳化而成。碳纤维主要由碳元素组成，具有耐高温、抗摩擦、导热及耐腐蚀等特性外形呈纤维状、柔软、可加工成各种织物，由于其石墨微晶结构沿纤维轴择优取向，因此沿纤维轴方向有很高的强度和模量。而现有技术中的碳纤维其功能性过于单一，缺少一种复合型多功能式碳纤维。Carbon fiber refers to high-strength and high-modulus fibers with a carbon content of more than 90%. High temperature resistance ranks first among all chemical fibers. It is made of acrylic fiber and viscose fiber, which is oxidized and carbonized at high temperature. Carbon fiber is mainly composed of carbon elements. It has the characteristics of high temperature resistance, friction resistance, heat conduction and corrosion resistance. Orientation has high strength and modulus. And its function of the carbon fiber in the prior art is too single, lacks a kind of composite multifunctional carbon fiber.
发明内容Contents of the invention
针对现有技术不足，本发明提供了一种复合型碳纤维制备工艺，为解决现有技术中碳纤维功能性单一的问题。Aiming at the deficiencies of the prior art, the present invention provides a composite carbon fiber preparation process to solve the problem of single functionality of the carbon fiber in the prior art.
为达到上述目的，本发明提供了一种复合型碳纤维制备工艺，包括以下步骤：In order to achieve the above object, the invention provides a composite carbon fiber preparation process, comprising the following steps:
步骤一，将纺丝液通过干喷湿纺法制备原丝；Step 1, the spinning solution is prepared by a dry jet wet spinning method;
步骤二，将原丝进行预氧化处理，预氧化过程中的温度控制在240度，预氧化反应时间为80分钟；Step 2, carrying out pre-oxidation treatment on the precursor, the temperature in the pre-oxidation process is controlled at 240 degrees, and the pre-oxidation reaction time is 80 minutes;
步骤三，将原丝进行热辊牵伸处理；Step 3, the raw silk is subjected to hot roller drafting treatment;
步骤四，将原丝进行二次预氧化处理，预氧化过程中的温度控制在260度，预氧化反应时间为100分钟；Step 4, carrying out secondary pre-oxidation treatment on the precursor, the temperature in the pre-oxidation process is controlled at 260 degrees, and the pre-oxidation reaction time is 100 minutes;
步骤五，将原丝进行二次牵伸，牵伸采用蒸汽加热方式处理；Step 5, the raw silk is subjected to secondary drafting, and the drafting is processed by steam heating;
步骤六，将原丝放入由抗菌整理剂制备成的浸轧液中进行浸轧处理，浸泡温度为30度，浸泡时间为20分钟，浸泡后经蒸馏水反复清洗；Step 6, put the raw silk into the padding solution prepared by antibacterial finishing agent for padding treatment, the soaking temperature is 30 degrees, the soaking time is 20 minutes, and it is washed repeatedly with distilled water after soaking;
步骤七，将原丝放入由纳米二氧化硅和丙酮溶剂制备成的分散液中进行浸轧，浸轧处理次数为2次，浸轧完成后经蒸馏水反复清洗，清洗后做烘干处理；Step 7, put the raw silk into the dispersion liquid prepared by nano-silica and acetone solvent for padding, the number of padding treatments is 2 times, after the padding is completed, it is repeatedly washed with distilled water, and dried after cleaning;
步骤八，将原丝置入低温碳化炉做初步碳化反应处理，碳化温度为400度，初步碳化反应处理后置入高温碳化炉做碳化反应处理，碳化温度为1000度；Step 8, put the raw silk into a low-temperature carbonization furnace for preliminary carbonization reaction treatment, the carbonization temperature is 400 degrees, after the preliminary carbonization reaction treatment, put it into a high-temperature carbonization furnace for carbonization reaction treatment, the carbonization temperature is 1000 degrees;
步骤九，将碳化处理后的原丝进行清洗，清洗后进行干燥；Step 9, cleaning the raw silk after the carbonization treatment, and drying after cleaning;
步骤十，干燥后进行收丝得到碳纤维。Step 10, drying and collecting to obtain carbon fibers.
采用上述技术方案有益的是：将原材料制备成纺丝液后通过干喷湿纺法制备成原丝，将原丝进行初步预氧化处理，处理后进行热辊牵伸处理，而后再进行二次氧化和二次牵伸，将原丝放入由抗菌整理剂制备成的浸轧液中进行浸轧处理，浸轧和清洗后再置入分散液中进行浸轧，在清洗和烘干后进行碳化处理，直至干燥后收丝得到碳纤维；上述技术中通过干喷湿纺所制备有利于形成细特化、致密化和均质化的原丝，同时纺出的纤维体密度较高，表面平滑无沟槽，且可实现速纺丝，用于生产高性能、高质量的碳纤维原丝；上述技术中通过热辊牵伸——提升纺速，而传统纺丝线的牵伸和烘干流程中均采用蒸汽加热，由于蒸汽传导热能效率较低，因此牵伸的线速度较慢，大致为80～240m/min，而热辊牵伸采用电磁感应直接加热导丝辊，在同等辊径条件下热效率增加，能有效提升基础纺速；上述技术中在浸轧液中进行浸轧处理，能够提高原丝的抗菌性能，使得纤维功能多样化；上述技术中在分散液中进行浸轧处理，能够提高纤维的耐温蓄热性，即使得纤维保温效果提高，进而使得限位功能多样化；上述技术中通过不同温度进行的碳化处理，以此保证碳纤维的成品和强度。The advantage of adopting the above-mentioned technical scheme is: the raw materials are prepared into spinning solution and then prepared into raw silk by dry-jet wet spinning method, the raw silk is subjected to preliminary pre-oxidation treatment, and after the treatment, hot roll drawing treatment is carried out, and then a second Oxidation and secondary drawing, put the raw silk into the padding liquid prepared by antibacterial finishing agent for padding treatment, padding and cleaning, then put it into the dispersion liquid for padding, after cleaning and drying Carbonization treatment until the fibers are collected after drying to obtain carbon fibers; in the above-mentioned technology, the preparation of dry-jet wet spinning is conducive to the formation of finely specialized, densified and homogenized precursors, and the spun fibers have a high density and a smooth surface There are no grooves, and fast spinning can be achieved, which is used to produce high-performance and high-quality carbon fiber precursors; in the above-mentioned technology, hot roller drafting is used to increase the spinning speed, while the drafting and drying process of traditional spinning lines Both are heated by steam. Due to the low efficiency of steam conduction heat energy, the linear speed of drafting is relatively slow, roughly 80-240m/min, while hot roll drafting uses electromagnetic induction to directly heat the godet roll. Under the same roll diameter condition The increase of thermal efficiency can effectively improve the basic spinning speed; the padding treatment in the padding liquid in the above technology can improve the antibacterial performance of the raw silk and make the fiber function diversified; the padding treatment in the dispersion liquid in the above technology can Improving the temperature resistance and heat storage of the fiber means improving the thermal insulation effect of the fiber and diversifying the limit function; in the above technology, the carbonization treatment is carried out at different temperatures to ensure the finished product and strength of the carbon fiber.
本发明进一步设置：所述步骤三中的热辊牵伸倍数为2.8至3.0倍数。The present invention further sets: the draft ratio of the hot roller in the third step is 2.8 to 3.0 times.
采用上述技术方案有益的是：上述技术中热辊牵伸倍数为2.8至3.0倍数，提高热效率的同时进一步的提高基础纺速。The benefit of adopting the above-mentioned technical solution is that: in the above-mentioned technology, the draft ratio of the hot roller is 2.8 to 3.0 times, which improves the thermal efficiency and further improves the basic spinning speed.
本发明进一步设置：所述步骤四中预氧化含氧量为25％-90％。The present invention further sets: the pre-oxidation oxygen content in the step 4 is 25%-90%.
采用上述技术方案有益的是：上述技术中预氧化含氧量为25％-90％，使得原丝能够进一步的到氧化，提高后续收丝能力。The benefit of adopting the above technical solution is that the pre-oxidation oxygen content in the above technology is 25%-90%, so that the raw silk can be further oxidized and the subsequent spinning ability can be improved.
本发明进一步设置：所述步骤六中的浸液率保持在70％。The present invention further sets: the liquid immersion rate in the sixth step is kept at 70%.
采用上述技术方案有益的是：上述技术中浸液率保持在70％，提高原丝在浸液率中的浸泡程度，同时提高抗菌整理剂于原丝上的覆盖率。The benefit of adopting the above technical solution is that: in the above technology, the immersion rate is kept at 70%, the degree of immersion of the original silk in the immersion rate is improved, and the coverage rate of the antibacterial finishing agent on the original silk is improved at the same time.
本发明进一步设置：所述步骤七中烘干前的原丝可置入涂覆液中，所述涂覆液由银粉、镍粉、酚醛树脂和极性有机溶剂超声混合制成，所述原丝浸泡完成后进行烘干处理。The present invention further sets: the raw silk before drying in the step 7 can be put into the coating liquid, and the coating liquid is made by ultrasonic mixing of silver powder, nickel powder, phenolic resin and polar organic solvent, and the raw silk After the silk soaking is completed, it is dried.
采用上述技术方案有益的是：上述技术中涂覆液由银粉、镍粉、酚醛树脂和极性有机溶剂超声混合制成，使得原丝在浸入涂覆液后形成覆膜，该覆膜能够有效提升原丝抗静电性，进而实现碳纤维功能多样化。The advantage of adopting the above-mentioned technical scheme is that the coating liquid in the above-mentioned technology is made by ultrasonically mixing silver powder, nickel powder, phenolic resin and polar organic solvent, so that the raw silk forms a film after being immersed in the coating liquid, and the film can effectively Improve the antistatic property of raw silk, and realize the function diversification of carbon fiber.
具体实施方式Detailed ways
本发明提供一种复合型碳纤维制备工艺，包括以下步骤：The invention provides a composite carbon fiber preparation process, comprising the following steps:
步骤一，将纺丝液通过干喷湿纺法制备原丝；Step 1, the spinning solution is prepared by a dry jet wet spinning method;
步骤二，将原丝进行预氧化处理，预氧化过程中的温度控制在240度，预氧化反应时间为80分钟；Step 2, carrying out pre-oxidation treatment on the precursor, the temperature in the pre-oxidation process is controlled at 240 degrees, and the pre-oxidation reaction time is 80 minutes;
步骤三，将原丝进行热辊牵伸处理；Step 3, the raw silk is subjected to hot roller drafting treatment;
步骤四，将原丝进行二次预氧化处理，预氧化过程中的温度控制在260度，预氧化反应时间为100分钟；Step 4, carrying out secondary pre-oxidation treatment on the precursor, the temperature in the pre-oxidation process is controlled at 260 degrees, and the pre-oxidation reaction time is 100 minutes;
步骤五，将原丝进行二次牵伸，牵伸采用蒸汽加热方式处理；Step 5, the raw silk is subjected to secondary drafting, and the drafting is processed by steam heating;
步骤六，将原丝放入由抗菌整理剂制备成的浸轧液中进行浸轧处理，浸泡温度为30度，浸泡时间为20分钟，浸泡后经蒸馏水反复清洗；Step 6, put the raw silk into the padding solution prepared by antibacterial finishing agent for padding treatment, the soaking temperature is 30 degrees, the soaking time is 20 minutes, and it is washed repeatedly with distilled water after soaking;
步骤七，将原丝放入由纳米二氧化硅和丙酮溶剂制备成的分散液中进行浸轧，浸轧处理次数为2次，浸轧完成后经蒸馏水反复清洗，清洗后做烘干处理；Step 7, put the raw silk into the dispersion liquid prepared by nano-silica and acetone solvent for padding, the number of padding treatments is 2 times, after the padding is completed, it is repeatedly washed with distilled water, and dried after cleaning;
步骤八，将原丝置入低温碳化炉做初步碳化反应处理，碳化温度为400度，初步碳化反应处理后置入高温碳化炉做碳化反应处理，碳化温度为1000度；Step 8, put the raw silk into a low-temperature carbonization furnace for preliminary carbonization reaction treatment, the carbonization temperature is 400 degrees, after the preliminary carbonization reaction treatment, put it into a high-temperature carbonization furnace for carbonization reaction treatment, the carbonization temperature is 1000 degrees;
步骤九，将碳化处理后的原丝进行清洗，清洗后进行干燥；Step 9, cleaning the raw silk after the carbonization treatment, and drying after cleaning;
步骤十，干燥后进行收丝得到碳纤维。Step 10, drying and collecting to obtain carbon fibers.
本发明进一步设置：所述步骤三中的热辊牵伸倍数为2.8至3.0倍数，所述步骤四中预氧化含氧量为25％-90％，所述步骤六中的浸液率保持在70％，所述步骤七中烘干前的原丝可置入涂覆液中，所述涂覆液由银粉、镍粉、酚醛树脂和极性有机溶剂超声混合制成，所述原丝浸泡完成后进行烘干处理。The present invention further sets: the draft ratio of the hot roll in the step three is 2.8 to 3.0 times, the pre-oxidation oxygen content in the step four is 25%-90%, and the immersion rate in the step six remains at 70%, the raw silk before drying in the step 7 can be placed in the coating solution, the coating solution is made by ultrasonically mixing silver powder, nickel powder, phenolic resin and polar organic solvent, and the raw silk is soaked Drying is done after completion.
以上显示和描述了本发明的基本原理和主要特征及本发明的优点，本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内，本发明要求保护范围由所附的权利要求书及其等效物界定。Above shows and described basic principle of the present invention and main feature and the advantage of the present invention, those skilled in the art should understand that, the present invention is not limited by above-mentioned embodiment, what described in above-mentioned embodiment and description just illustrates the present invention Principle, under the premise of not departing from the spirit and scope of the present invention, the present invention also has various changes and improvements, and these changes and improvements all fall within the claimed scope of the present invention, and the claimed scope of the present invention is defined by the appended claims Requirements and their equivalents are defined.
Claims (5)
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| CN202310585006.9A CN116641158A (en) | 2023-05-23 | 2023-05-23 | Composite carbon fiber preparation process |
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