CN116876117B - Preparation method of acrylic fiber-based carbon fiber - Google Patents
Preparation method of acrylic fiber-based carbon fiber Download PDFInfo
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- CN116876117B CN116876117B CN202310898394.6A CN202310898394A CN116876117B CN 116876117 B CN116876117 B CN 116876117B CN 202310898394 A CN202310898394 A CN 202310898394A CN 116876117 B CN116876117 B CN 116876117B
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 25
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 25
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 229920002972 Acrylic fiber Polymers 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000835 fiber Substances 0.000 claims abstract description 35
- 229920002239 polyacrylonitrile Polymers 0.000 claims abstract description 23
- 229910052802 copper Inorganic materials 0.000 claims abstract description 20
- 239000010949 copper Substances 0.000 claims abstract description 20
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 18
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000009987 spinning Methods 0.000 claims abstract description 18
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910000077 silane Inorganic materials 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 12
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000004246 zinc acetate Substances 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 8
- 238000010000 carbonizing Methods 0.000 claims abstract description 7
- 230000003647 oxidation Effects 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 11
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 6
- 239000004094 surface-active agent Substances 0.000 claims description 6
- 238000003763 carbonization Methods 0.000 claims description 5
- JZCCFEFSEZPSOG-UHFFFAOYSA-L copper(II) sulfate pentahydrate Chemical compound O.O.O.O.O.[Cu+2].[O-]S([O-])(=O)=O JZCCFEFSEZPSOG-UHFFFAOYSA-L 0.000 claims description 5
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 5
- 239000000244 polyoxyethylene sorbitan monooleate Substances 0.000 claims description 5
- 229920000053 polysorbate 80 Polymers 0.000 claims description 5
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 5
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 claims description 4
- 238000001125 extrusion Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 claims description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical group [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- 239000004744 fabric Substances 0.000 abstract description 9
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 10
- 239000003063 flame retardant Substances 0.000 description 10
- 239000000463 material Substances 0.000 description 10
- 238000005303 weighing Methods 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
- 229920002821 Modacrylic Polymers 0.000 description 1
- 101100005280 Neurospora crassa (strain ATCC 24698 / 74-OR23-1A / CBS 708.71 / DSM 1257 / FGSC 987) cat-3 gene Proteins 0.000 description 1
- 241000168254 Siro Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- -1 acrylonitrile compound Chemical class 0.000 description 1
- 239000004760 aramid Substances 0.000 description 1
- 229920003235 aromatic polyamide Polymers 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
Classifications
-
- 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
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
-
- 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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Inorganic Fibers (AREA)
- Artificial Filaments (AREA)
Abstract
The application provides a preparation method of acrylic fiber-based carbon fibers, and belongs to the technical field of polyacrylonitrile fiber manufacturing. Adding silane modified nano copper and zinc acetate into polyacrylonitrile, stirring to obtain a spinning solution, carrying out electrostatic spinning to obtain modified polyacrylonitrile fibers, placing the modified polyacrylonitrile fibers in a tubular resistance furnace, carrying out pre-oxidation treatment in an air medium, and carbonizing in a nitrogen medium to obtain the modified acrylic fiber-based carbon fibers. The acrylic carbon fiber obtained by the method has the advantages of greatly improved heat resistance and softness, higher flame retardance (LOI value), convenience in spinning, and improved hydrophilicity and soft hand feeling of the manufactured fabric.
Description
Technical Field
The application relates to a preparation method of acrylic fiber-based carbon fiber, and belongs to the technical field of polyacrylonitrile fiber manufacturing.
Background
Flame retardance of textiles is one of the current global challenges. Currently, the major flame retardant fabrics on the market fall into two categories: the first is a medium-low grade flame-retardant fabric, which mainly uses modified chemical fiber flame retardance, has poor effect, is easy to generate melt drops after combustion, and causes secondary scalding; the second is high-grade flame-retardant fabric, which mainly comprises high-performance flame-retardant fibers (Du Bangfang fibers 1313, 1414 and the like), is monopoly of DuPont, japanese emperor and other companies in the United states, and has high cost, high-temperature resistance, bottleneck in certain occasions and poor softness. In the market, the oxygen index LOI of the high-end flame-retardant main stream product aramid 1313 is only about 29 (B2 grade), belongs to a combustible material (refer to standard GB 8624-2012, namely, classification of combustion performance of building materials and products), starts to decompose at a high temperature exceeding 370 ℃, starts to carbonize at 400 ℃, and is difficult to meet special requirements. In special occasions, a domestic high-performance flame-retardant material with more excellent flame retardant property, better softness and secondary harm such as molten drops is urgently needed.
The carbon fiber is made of special acrylonitrile compound, can resist for more than 3 minutes in an aerobic environment at about 1000 ℃, can keep the original characteristics of the material, can be called as a non-combustible material (LOI value is more than 32, and other high-temperature resistant materials are called as flame-retardant materials), and is the material with the lowest cost and the best flame retardance in the existing high-performance flame-retardant materials, but the material has the problems of strong rigidity, less curling, poor fiber cohesion and the like in the spinning process at present, so that the material is more difficult to process into strips, comb and weave than other fibers. The invention develops the incombustible acrylic carbon fiber.
Disclosure of Invention
In view of the above, the present application provides a method for preparing acrylic carbon fiber, which can improve the flexibility and cohesion of the fiber, and the fiber has high fire resistance (LOI value) and soft touch.
Specifically, the application is realized by the following scheme:
The preparation method of the acrylic fiber-based carbon fiber comprises the following steps:
1) Spinning: adding silane modified nano copper and zinc acetate into polyacrylonitrile, stirring to obtain a spinning solution, and carrying out electrostatic spinning to obtain modified polyacrylonitrile fibers, wherein the electrostatic spinning parameters are as follows: the extrusion speed of the solution is 0.5-0.8 mL/h, and the voltage is 15-25 kV;
2) Pre-oxidation treatment: placing the modified polyacrylonitrile fiber in a tubular resistance furnace, performing pre-oxidation treatment in an air medium, and raising the temperature from room temperature to 200-260 ℃ at 3 ℃/min, and keeping the temperature for 1-2 hours to obtain pre-oxidized yarns;
3) Carbonizing: carbonizing the preoxidized fiber in nitrogen medium, and heating from the preoxidation temperature to 600-900 ℃ for 20-40 min to obtain the modified acrylic fiber.
The scheme mainly comprises two steps of preparing the modified polyacrylonitrile fiber and preparing the acrylic fiber-based carbon fiber by pre-oxidizing the modified polyacrylonitrile fiber, and introducing metal particles such as zinc, copper and the like into the modified acrylic fiber-based carbon fiber, so that the heat resistance and the softness of the modified acrylic fiber-based carbon fiber are greatly improved, spinning is facilitated, and the prepared fabric has soft touch feeling and is endowed with high fire resistance (LOI value) at the same time.
Further, as preferable:
in the step (1) of the process,
Preparation of silane modified nano copper particles: and (3) weighing polyoxyethylene sorbitan monooleate and hexamethyldisiloxane, adding a proper amount of sodium dithionite into a four-necked flask, fully stirring at a stirring speed of 500 revolutions per minute, heating to 80 ℃, measuring copper sulfate pentahydrate in a separating funnel, continuously stirring for reacting for 2-3 hours after the dripping of 60-80 drops per minute at 80 ℃ is completed, and filtering to obtain silane modified nano-copper particles. In the preparation process, 100mL of polyoxyethylene sorbitan monooleate and 10mL of hexamethyldisiloxane with the concentration of 0.05mol/L and 100-200 mL of copper sulfate pentahydrate with the concentration of 0.5mol/L can be weighed first.
In the spinning solution, the addition mass ratio of the silane modified nano copper is 1-12%. The adding mass ratio of the zinc acetate is 1-6%. The addition mass ratio of the polyacrylonitrile is 5-15%.
The spinning solution also comprises tetrahydrofuran, N-dimethylformamide and a surfactant, wherein the adding ratio of the tetrahydrofuran, the N, N-dimethylformamide to the surfactant is 3-5: 3-4: 0.5 to 1.5.
In the scheme, the surfactant and the silane are added into the acrylic fiber spinning solution to modify nano copper and zinc acetate, so that the tensile strength, softness and hydrophilicity of the polyacrylonitrile fiber after pre-oxidation are improved.
In the step 3) of the method,
The carbonization temperature is firstly increased from the pre-oxidation temperature to 600 ℃ at 5 ℃/min, then the heating speed is adjusted to 10 ℃/min, the carbonization temperature is directly increased to 900 ℃, and the carbonization temperature is treated for 30 to 40min.
The modified acrylic fiber-based carbon fiber has excellent performance, limiting oxygen index LOI of 40, soft hand feeling, good hydrophilicity, better breaking strength and low price.
Drawings
FIG. 1 is an XRD pattern of unmodified polyacrylonitrile and modacrylic fibers;
FIG. 2 is a scanning electron microscope image of the polyacrylonitrile yarn before and after modification in example 1.
Detailed Description
Example 1
The preparation method of the acrylic fiber-based carbon fiber comprises the following steps:
(1) Preparing a spinning solution: respectively weighing 45mL of tetrahydrofuran, 35mL of N, N-dimethylformamide, adding 4% by mass of zinc acetate, 8% by mass of silane modified nano copper particles and 4% by mass of sodium dodecyl benzene sulfonate, uniformly mixing, adding 12.00g of polyacrylonitrile, and stirring on a magnetic stirrer for 3-4 hours at 80 ℃ to obtain an acrylonitrile spinning solution.
The preparation process of the silane modified nano copper particles comprises the following steps: weighing 100mL of polyoxyethylene sorbitan monooleate with the concentration of 0.05mol/L and 10mL of hexamethyldisiloxane in a four-necked flask, adding a proper amount of sodium dithionite, fully stirring, heating to the temperature of 80 ℃ at the stirring speed of 500 r/min, weighing 200mL of copper sulfate pentahydrate with the concentration of 0.5mol/L in a separating funnel, continuously stirring for reacting for 2 hours at the speed of 60 drops per minute at the temperature of 80 ℃ after the complete dropwise addition, and filtering to obtain the silane modified nano-copper particles.
(2) And (3) electrostatic spinning: adopting a high-voltage electrostatic spinning machine, wherein the electrostatic spinning process parameters are as follows: the extrusion speed of the solution is 0.6mL/h, the receiving distance is 20cm, and the voltage is 21kV, so that the modified polyacrylonitrile fiber is prepared.
(3) Pre-oxidation: and (3) pre-oxidizing the prepared modified polyacrylonitrile fiber in an air medium in a tubular resistance furnace. The temperature was raised from room temperature to 260℃at 3℃per minute, and then the mixture was treated at this temperature for 1 hour to obtain a pre-oxidized yarn.
(4) Carbonizing: carbonizing the preoxidized fiber in nitrogen medium, heating from 260 ℃ to 600 ℃ at 5 ℃/min, heating to 900 ℃ at 10 ℃/min, and treating at 900 ℃ for 30min to obtain the modified acrylic fiber-based carbon fiber.
The modified polyacrylonitrile fiber obtained by the method is woven after being spun by compact siro spinning.
The fibers before and after modification were tested and the results are shown in fig. 1 and 2: as can be seen from fig. 1, in the XRD curve of the modified polyacrylonitrile fiber, the series of weak diffraction peaks appearing in the vicinity of 29.8 ° and 34.4 ° for 2θ represent the characteristic diffraction peaks of copper and zinc, respectively. The surface of the unmodified front fiber (left graph) is smoother and flatter, the longitudinal grooves on the surface of the fiber are increased after modification (right graph), and a small amount of granular substances exist on the surface of the fiber.
Example 2
The present example was the same as example 1, but the zinc acetate was added in different mass percentages, and the results are shown in table 1.
Table 1: influence of different zinc acetate addition amounts on fiber properties
Conclusion: with the addition of zinc acetate in the spinning solution, the breaking strength and breaking elongation of the modified acrylic carbon fiber are improved, the hydrophilicity of the fiber is improved, the fabric is soft in hand feeling, and the zinc acetate addition amount is 4% (namely example 1) and is optimal.
Example 3
The present example was the same as example 1, but the silane modified nano copper was added in different mass ratios, and the results are shown in table 2.
Table 2: influence of different modified nano copper addition amounts on fiber properties
Conclusion: with the addition of silane modified nano copper in the spinning solution, the breaking strength and breaking elongation of the modified acrylic carbon fiber are improved, the hydrophilicity of the fiber is improved, the fabric is soft in hand feeling, and the addition of the modified nano copper is optimal when the addition amount of the modified nano copper is 8% (namely example 1).
Meanwhile, the applicant also compares the modified acrylic carbon fiber fabric with a commercially available representative flame retardant fabric, and the result is shown in table 3.
Table 3: performance comparison of modified acrylic-based carbon fiber with Du Bangfang (commercially available) fiber 1313
Comparison of table 3 shows that: the modified acrylic fiber based carbon fiber prepared by the embodiment has excellent performance, limiting oxygen index LOI of 40, soft hand feeling, better spray burning experimental result than market products, high safety and difficult occurrence of safety problems caused by molten drops; and the price is low.
Claims (4)
1. The preparation method of the acrylic fiber-based carbon fiber is characterized by comprising the following steps of:
1) Spinning: adding silane modified nano copper and zinc acetate into polyacrylonitrile, stirring to obtain a spinning solution, and carrying out electrostatic spinning to obtain modified polyacrylonitrile fibers, wherein the electrostatic spinning parameters are as follows: the extrusion speed of the solution is 0.5-0.8 mL/h, the voltage is 15-25 kV,
The spinning solution also comprises tetrahydrofuran, N-dimethylformamide and a surfactant, the adding ratio of the tetrahydrofuran, the N, N-dimethylformamide and the surfactant is 3-5:3-4:0.5-1.5,
The preparation method of the silane modified nano copper comprises the following steps: adding sodium dithionite into polyoxyethylene sorbitan monooleate and hexamethyldisiloxane, stirring thoroughly, heating to 80 ℃, dripping copper sulfate pentahydrate at the speed of 60-80 drops/min, continuing stirring to react for 2-3 hours, filtering to obtain silane modified nano copper,
In the spinning solution, the mass ratio of zinc acetate is 1-6%, the mass ratio of polyacrylonitrile is 5-15%, and the mass ratio of silane modified nano copper particles is 1-12%;
2) Pre-oxidation treatment: placing the modified polyacrylonitrile fiber in a tubular resistance furnace, performing pre-oxidation treatment in an air medium, and raising the temperature from room temperature to 200-260 ℃ at 3 ℃/min, and keeping the temperature for 1-2 hours to obtain pre-oxidized yarns;
3) Carbonizing: carbonizing the preoxidized fiber in nitrogen medium, and heating from the preoxidation temperature to 600-900 ℃ for 20-40 min to obtain the modified acrylic fiber.
2. The method for preparing acrylic-based carbon fiber according to claim 1, characterized in that: in the step 1), the surfactant is sodium dodecyl benzene sulfonate.
3. The method for preparing acrylic-based carbon fiber according to claim 1, characterized in that: the adding mole ratio of the polyoxyethylene sorbitan monooleate to the copper sulfate pentahydrate is 1:10-20.
4. The method for preparing acrylic-based carbon fiber according to claim 1, characterized in that: in the step 3), the carbonization temperature is firstly increased from the pre-oxidation temperature to 600 ℃ at a speed of 5 ℃/min, then the temperature is directly increased to 900 ℃ at a speed of 10 ℃/min, and the carbonization temperature is treated for 30-40 min at the temperature.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310898394.6A CN116876117B (en) | 2023-07-21 | 2023-07-21 | Preparation method of acrylic fiber-based carbon fiber |
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| CN202310898394.6A CN116876117B (en) | 2023-07-21 | 2023-07-21 | Preparation method of acrylic fiber-based carbon fiber |
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| CN116876117A CN116876117A (en) | 2023-10-13 |
| CN116876117B true CN116876117B (en) | 2024-04-23 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL6919555A (en) * | 1968-12-31 | 1970-07-02 | ||
| CN101348952A (en) * | 2008-09-17 | 2009-01-21 | 天津工业大学 | Active carbon fibre and preparation thereof |
| CN102465453A (en) * | 2010-11-16 | 2012-05-23 | 晓健科技（大连）有限公司 | Radiation-proof warming carbon fiber and production method of same |
| CN105798320A (en) * | 2014-12-31 | 2016-07-27 | 中国科学院化学研究所 | Method for preparing nanometer copper powder at low temperature |
| CN108532029A (en) * | 2018-04-17 | 2018-09-14 | 浙江理工大学 | Using taking or the discarded method taken acrylic fibers and prepare carbon nano-fiber |
| JP2021075679A (en) * | 2019-11-06 | 2021-05-20 | 寧波瑞凌新能源科技有限公司Ｎｉｎｇｂｏ Ｒａｄｉ−Ｃｏｏｌ Ａｄｖａｎｃｅｄ Ｅｎｅｒｇｙ Ｔｅｃｈｎｏｌｏｇｉｅｓ Ｃｏ．， Ｌｔｄ． | Cooling coating material and method for preparing the same |
| CN115851071A (en) * | 2022-10-25 | 2023-03-28 | 辽宁科技大学 | Preparation method of environment-friendly super-hydrophobic anti-biological fouling self-repairing coating |
-
2023
- 2023-07-21 CN CN202310898394.6A patent/CN116876117B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| NL6919555A (en) * | 1968-12-31 | 1970-07-02 | ||
| CN101348952A (en) * | 2008-09-17 | 2009-01-21 | 天津工业大学 | Active carbon fibre and preparation thereof |
| CN102465453A (en) * | 2010-11-16 | 2012-05-23 | 晓健科技（大连）有限公司 | Radiation-proof warming carbon fiber and production method of same |
| CN105798320A (en) * | 2014-12-31 | 2016-07-27 | 中国科学院化学研究所 | Method for preparing nanometer copper powder at low temperature |
| CN108532029A (en) * | 2018-04-17 | 2018-09-14 | 浙江理工大学 | Using taking or the discarded method taken acrylic fibers and prepare carbon nano-fiber |
| JP2021075679A (en) * | 2019-11-06 | 2021-05-20 | 寧波瑞凌新能源科技有限公司Ｎｉｎｇｂｏ Ｒａｄｉ−Ｃｏｏｌ Ａｄｖａｎｃｅｄ Ｅｎｅｒｇｙ Ｔｅｃｈｎｏｌｏｇｉｅｓ Ｃｏ．， Ｌｔｄ． | Cooling coating material and method for preparing the same |
| CN115851071A (en) * | 2022-10-25 | 2023-03-28 | 辽宁科技大学 | Preparation method of environment-friendly super-hydrophobic anti-biological fouling self-repairing coating |
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