CN112796009A - PAN-based carbon fiber precursor oiling agent and preparation method thereof - Google Patents
PAN-based carbon fiber precursor oiling agent and preparation method thereof Download PDFInfo
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- CN112796009A CN112796009A CN202011617029.6A CN202011617029A CN112796009A CN 112796009 A CN112796009 A CN 112796009A CN 202011617029 A CN202011617029 A CN 202011617029A CN 112796009 A CN112796009 A CN 112796009A
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- Prior art keywords
- pan
- carbon fiber
- based carbon
- fiber precursor
- emulsion
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 48
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 48
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000002243 precursor Substances 0.000 title claims abstract description 29
- 239000008041 oiling agent Substances 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000000839 emulsion Substances 0.000 claims abstract description 49
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 25
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims abstract description 15
- 239000000080 wetting agent Substances 0.000 claims abstract description 15
- 239000004593 Epoxy Substances 0.000 claims abstract description 13
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 13
- 229920000570 polyether Polymers 0.000 claims abstract description 13
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims abstract description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 18
- 229910052710 silicon Inorganic materials 0.000 claims description 18
- 239000010703 silicon Substances 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 18
- -1 ester quaternary ammonium salt Chemical class 0.000 claims description 10
- 238000004806 packaging method and process Methods 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 239000002736 nonionic surfactant Substances 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 14
- 230000003647 oxidation Effects 0.000 abstract description 7
- 238000007254 oxidation reaction Methods 0.000 abstract description 7
- 238000003763 carbonization Methods 0.000 abstract description 4
- 230000007547 defect Effects 0.000 abstract description 3
- 239000011148 porous material Substances 0.000 abstract description 3
- 238000009987 spinning Methods 0.000 abstract description 3
- 229920002239 polyacrylonitrile Polymers 0.000 description 26
- 239000000835 fiber Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000010959 steel Substances 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
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 229920006231 aramid fiber Polymers 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 229920002313 fluoropolymer Polymers 0.000 description 1
- 239000004811 fluoropolymer Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 229920006253 high performance fiber Polymers 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229920001558 organosilicon polymer Polymers 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000012360 testing method Methods 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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/10—Chemical after-treatment of artificial filaments or the like during manufacture of carbon
- D01F11/14—Chemical after-treatment of artificial filaments or the like during manufacture of carbon with organic compounds, e.g. macromolecular compounds
Abstract
The invention relates to the technical field of spinning oil, in particular to PAN-based carbon fiber precursor oil and a preparation method thereof. The PAN-based carbon fiber precursor oiling agent comprises the following components in percentage by mass: 5 to 50 percent of amino and epoxy modified organosilicon emulsion, 5 to 35 percent of polyether modified organosilicon emulsion, 0.5 to 10 percent of quaternary ammonium salt, 0.1 to 5 percent of wetting agent and deionized water. When the modified silicone emulsion is prepared, firstly, the amino-modified silicone emulsion, the epoxy-modified silicone emulsion and the polyether-modified silicone emulsion are added into a variable speed mixer according to the proportion and are uniformly stirred, then, the quaternary ammonium salt is added according to the proportion and is stirred, finally, the wetting agent and the deionized water are slowly added according to the proportion and are uniformly stirred and are subpackaged. The PAN-based carbon fiber precursor oiling agent has good quality stability and heat resistance, can effectively prevent PAN precursor from being adhered and doubled in the pre-oxidation process, reduces the pore defect in the high-temperature carbonization process, and reduces the amount of the filament.
Description
Technical Field
The invention belongs to the technical field of carbon fiber additives, and particularly relates to a PAN (polyacrylonitrile) -based carbon fiber precursor oiling agent for playing anti-sticking and isolating roles in a fiber processing process and a preparation method thereof.
Background
The carbon fiber is a high-strength high-modulus fiber composed of carbon elements, is fired at a high temperature of more than 1000 ℃, has a carbon content of more than 90 percent, and has a series of advantages of light weight, high strength, high temperature resistance, low creep deformation, corrosion resistance and the like. The relative density of the carbon fiber is only one fourth of that of steel, but the tensile strength is four times that of high-performance steel, and the carbon fiber has unique structure and mechanical property, so that the carbon fiber is widely applied to the fields of aviation, aerospace, sports, leisure and entertainment and the like.
The main raw materials for manufacturing the carbon fiber comprise viscose fiber, Polyacrylonitrile (PAN) fiber, asphalt, phenolic aldehyde and the like. Because the production process of the PAN-based carbon fiber is relatively simple and has the same performance as other precursor fibers, the PAN-based carbon fiber is more applied and dominates the market field of carbon fibers. The PAN-based carbon fiber has high strength and rigidity, can even replace metal materials such as steel, aluminum alloy and the like, has the worldwide productivity inferior to that of aramid fiber, and becomes a second-ranked world high-performance fiber material.
The preparation of PAN-based carbon fiber comprises the following processes: polymerization, spinning, pre-oxidation and carbonization. In the pre-oxidation process, due to the fact that the temperature is high (250-300 ℃), the PAN precursor can fuse, adhere and doubling, and therefore the number of carbon fiber broken filaments obtained finally is large, and the doubling phenomenon exists, and strength and usability of the carbon fiber are affected.
In order to alleviate the above situation, in the process of preparing carbon fiber precursor, there is generally an oiling process, in which a spinning oil is attached to the surface of polyacrylonitrile precursor. In the pre-oxidation process, the oil agent plays the roles of anti-sticking and isolation, thereby inhibiting fusion, adhesion and doubling among protofilaments, enabling the pre-oxidation process of the carbon fiber to be smoothly carried out, and improving the strength and quality of the carbon fiber.
Because the organic silicon polymer has excellent anti-sticking, isolating, lubricating and high temperature resistance properties, the organic silicon oil agent taking the organic silicon as the main component is the main choice of the special oil agent for manufacturing the high-performance carbon fiber. There are many foreign patents reporting on spin finishes based on functional group-modified polydimethylsiloxanes, and almost all spin finishes used for producing high-performance carbon fibers have functional group-modified polysiloxanes as the main component. The main component of the carbon fiber oil agent widely used by carbon fiber manufacturers at home and abroad at present is amino polysiloxane, which is used in the form of aqueous emulsion and contains proper emulsifier and other auxiliary agents, but the use effect is not satisfactory.
Disclosure of Invention
The invention provides a precursor oiling agent suitable for PAN-based carbon fibers and a preparation method thereof based on the research background, prevents adhesion and doubling of PAN precursors in a pre-oxidation process, reduces the defect of pores in a high-temperature carbonization process, and reduces the amount of fuzz.
The invention provides a PAN-based carbon fiber precursor oiling agent, which comprises the following components in percentage by mass: 5 to 50 percent of amino and epoxy modified organosilicon emulsion, 5 to 35 percent of polyether modified organosilicon emulsion, 0.5 to 10 percent of quaternary ammonium salt, 0.1 to 5 percent of wetting agent and the balance of deionized water.
Preferably, the optimal composition of the protofilament oiling agent is as follows by mass percent: 30% of amino and epoxy modified organic silicon emulsion, 20% of polyether modified organic silicon emulsion, 8% of quaternary ammonium salt, 0.5% of wetting agent and 41.5% of deionized water.
In the invention, the amino-epoxy modified organosilicon emulsion has the ammonia value of 2000-6000 mmol/g and the epoxy value of 1000-4000 mmol/g, and is purchased from Shanghai fluoropolymerization chemical products GmbH, and the product brand is SS 6189.
The polyether modified organic silicon emulsion is prepared from crude oil with the viscosity of 500-5000 mPa.s, and is purchased from Shanghai fluoropolymerization chemical products, Inc., and the product brand is SS 6179.
The quaternary ammonium salt is ester quaternary ammonium salt.
The wetting agent is a nonionic surfactant available from Dow chemical under the product designations Tergitol 15-s-9, Tergitol 15-s-5, Tergitol 15-s-7.
The invention provides a preparation method of a PAN-based carbon fiber precursor oiling agent, which comprises the following steps: adding amino-modified silicone emulsion, epoxy-modified silicone emulsion and polyether-modified silicone emulsion into a variable-speed mixer according to the above-mentioned proportion, uniformly stirring them, then adding quaternary ammonium salt according to the above-mentioned proportion, stirring them, finally slowly adding wetting agent and deionized water according to the above-mentioned proportion, uniformly stirring them and packaging.
Technical effects of the invention
The amino and epoxy modified organosilicon emulsion in the PAN-based carbon fiber precursor oiling agent can improve the fiber separation property and the temperature resistance of the PAN-based carbon fiber precursor; the polyether modified organic silicon emulsion can improve the convergence and antistatic property of the PAN-based carbon fiber precursor; the quaternary ammonium salt has good antistatic property, so that the yarn burst of the protofilament in the pre-oxidation process is greatly reduced, and the broken yarn is effectively reduced; the wetting agent is added to enable the oiling agent to be uniformly distributed on the surface of the protofilament, so that doubling and adhesion caused by partial lack of oiling agent protection are prevented, and the broken filament phenomenon and the pore defect caused by friction between fibers or friction between the fibers and a metal roller in the high-temperature carbonization process are reduced.
Detailed Description
The present invention is described in detail below with reference to specific examples, which are intended to illustrate the present invention and not to limit the scope of the present invention.
In the following examples, the amino-and epoxy-modified silicone emulsions were obtained from Shanghai Fluoropolymer chemical products, Inc. under the product designation SS 6189; the polyether modified organic silicon emulsion is purchased from Shanghai fluoropolymerization chemical products, Inc., and the product brand is SS 6179; esterquat was purchased from bosch Huarun oleochemical Co., Ltd; nonionic surfactants are available from Dow chemical under the product designations Tergitol 15-s-9, Tergitol 15-s-5, Tergitol 15-s-7 variable speed mixer from IKA, model RW20 digitil.
Example 1
The PAN-based carbon fiber precursor oiling agent comprises the following components in percentage by mass: 30% of amino and epoxy modified organosilicon emulsion, 20% of polyether modified organosilicon emulsion, 8% of ester quaternary ammonium salt, 0.5% of nonionic surface activity and 41.5% of deionized water. Adding amino-modified silicone emulsion, epoxy-modified silicone emulsion and polyether-modified silicone emulsion into a variable-speed mixer according to the above-mentioned proportion, uniformly stirring them, then adding quaternary ammonium salt according to the above-mentioned proportion, stirring them, finally slowly adding wetting agent and deionized water according to the above-mentioned proportion, uniformly stirring them and packaging.
Example 2
The PAN-based carbon fiber precursor oiling agent comprises the following components in percentage by mass: 5% of amino and epoxy modified organic silicon emulsion, 5% of polyether modified organic silicon emulsion, 0.5% of ester quaternary ammonium salt, 0.1% of nonionic surface activity and 89.4% of deionized water. Adding amino-modified silicone emulsion, epoxy-modified silicone emulsion and polyether-modified silicone emulsion into a variable-speed mixer according to the above-mentioned proportion, uniformly stirring them, then adding quaternary ammonium salt according to the above-mentioned proportion, stirring them, finally slowly adding wetting agent and deionized water according to the above-mentioned proportion, uniformly stirring them and packaging.
Example 3
The PAN-based carbon fiber precursor oiling agent comprises the following components in percentage by mass: 50% of amino and epoxy modified organic silicon emulsion, 35% of polyether modified organic silicon emulsion, 10% of ester quaternary ammonium salt, 5% of nonionic surface activity and 0% of deionized water. Adding amino-modified silicone emulsion, epoxy-modified silicone emulsion and polyether-modified silicone emulsion into a variable-speed mixer according to the above-mentioned proportion, uniformly stirring them, then adding quaternary ammonium salt according to the above-mentioned proportion, stirring them, finally slowly adding wetting agent and deionized water according to the above-mentioned proportion, uniformly stirring them and packaging.
Example 4
The PAN-based carbon fiber precursor oiling agent comprises the following components in percentage by mass: 30% of amino-group and epoxy-group modified organic silicon emulsion, 5% of polyether modified organic silicon emulsion, 5% of ester quaternary ammonium salt, 0.5% of nonionic surface activity and 59.5% of deionized water. Adding amino-modified silicone emulsion, epoxy-modified silicone emulsion and polyether-modified silicone emulsion into a variable-speed mixer according to the above-mentioned proportion, uniformly stirring them, then adding quaternary ammonium salt according to the above-mentioned proportion, stirring them, finally slowly adding wetting agent and deionized water according to the above-mentioned proportion, uniformly stirring them and packaging.
The oil prepared in example 1 is applied to the PAN-based T300-grade carbon fiber production process, and the obtained PAN-based T300-grade carbon fiber has the following mechanical property test data: tensile strength range 3500MPa, tensile modulus 230GPa, elongation at break: 1.8 percent, and meets the PAN-based T300-grade carbon fiber national standard.
The PAN-based T300-grade carbon fiber has the following mechanical property national standard:
tensile strength range: 3500-4500 MPa; tensile modulus: 220-260 GPa; elongation at break: 1.3 to 2.0 percent.
While the preferred embodiments of the present invention have been described in detail, it will be understood by those skilled in the art that the invention is not limited thereto, and that various changes and modifications may be made without departing from the spirit of the invention, and the scope of the appended claims is to be accorded the full scope of the invention.
Claims (7)
1. A PAN-based carbon fiber precursor oiling agent is characterized by comprising the following components in percentage by mass: 5-50% of amino and epoxy modified organic silicon emulsion, 5-35% of polyether modified organic silicon emulsion, 0.5-10% of quaternary ammonium salt, 0.1-5% of wetting agent and the balance of deionized water.
2. The PAN-based carbon fiber strand finish according to claim 1, wherein,
the PAN-based carbon fiber precursor oiling agent comprises the following components in percentage by mass: 30% of amino and epoxy modified organic silicon emulsion, 20% of polyether modified organic silicon emulsion, 8% of quaternary ammonium salt, 0.5% of wetting agent and 41.5% of deionized water.
3. The PAN-based carbon fiber precursor oiling agent according to claim 1, wherein:
wherein the amino-epoxy modified organosilicon emulsion has an ammonia value of 2000-6000 mmol/g and an epoxy value of 1000-4000 mmol/g.
4. The PAN-based carbon fiber precursor oiling agent according to claim 1, wherein:
wherein the viscosity of the polyether modified organic silicon emulsion is 500-5000 mPa.s.
5. The PAN-based carbon fiber precursor oiling agent according to claim 1, wherein:
wherein the quaternary ammonium salt is ester quaternary ammonium salt.
6. The PAN-based carbon fiber precursor oiling agent according to claim 1, wherein:
wherein the wetting agent is a nonionic surfactant.
7. The preparation method of the PAN-based carbon fiber precursor oiling agent as defined in any one of claims 1 to 6, which is characterized by comprising the following steps: adding amino-modified silicone emulsion, epoxy-modified silicone emulsion and polyether-modified silicone emulsion into a variable-speed mixer according to the above-mentioned proportion, uniformly stirring them, then adding quaternary ammonium salt according to the above-mentioned proportion, stirring them, finally slowly adding wetting agent and deionized water according to the above-mentioned proportion, uniformly stirring them and packaging.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011617029.6A CN112796009A (en) | 2020-12-30 | 2020-12-30 | PAN-based carbon fiber precursor oiling agent and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202011617029.6A CN112796009A (en) | 2020-12-30 | 2020-12-30 | PAN-based carbon fiber precursor oiling agent and preparation method thereof |
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| CN112796009A true CN112796009A (en) | 2021-05-14 |
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| CN202011617029.6A Pending CN112796009A (en) | 2020-12-30 | 2020-12-30 | PAN-based carbon fiber precursor oiling agent and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113897708A (en) * | 2021-11-18 | 2022-01-07 | 中复神鹰碳纤维股份有限公司 | Oiling agent for polyacrylonitrile carbon fiber precursor and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101280475A (en) * | 2008-05-21 | 2008-10-08 | 威海东方润德新材料有限公司 | Lubricating antistatic high-performance oil for drawing production of carbon fibre |
| JP2012102429A (en) * | 2010-11-10 | 2012-05-31 | Matsumoto Yushi Seiyaku Co Ltd | Oil agent for acrylic fiber for producing carbon fiber, acrylic fiber for producing carbon fiber and method for producing carbon fiber |
| US20140134094A1 (en) * | 2011-06-06 | 2014-05-15 | Mitsubishi Rayon Co., Ltd. | Oil agent for carbon fiber precursor acrylic fiber, oil composition for carbon fiber precursor acrylic fiber, processed-oil solution for carbon-fiber precursor acrylic fiber, and method for producing carbon-fiber precursor acrylic fiber bundle, and carbon-fiber bundle using carbon-fiber precursor acrylic fiber bundle |
-
2020
- 2020-12-30 CN CN202011617029.6A patent/CN112796009A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101280475A (en) * | 2008-05-21 | 2008-10-08 | 威海东方润德新材料有限公司 | Lubricating antistatic high-performance oil for drawing production of carbon fibre |
| JP2012102429A (en) * | 2010-11-10 | 2012-05-31 | Matsumoto Yushi Seiyaku Co Ltd | Oil agent for acrylic fiber for producing carbon fiber, acrylic fiber for producing carbon fiber and method for producing carbon fiber |
| US20140134094A1 (en) * | 2011-06-06 | 2014-05-15 | Mitsubishi Rayon Co., Ltd. | Oil agent for carbon fiber precursor acrylic fiber, oil composition for carbon fiber precursor acrylic fiber, processed-oil solution for carbon-fiber precursor acrylic fiber, and method for producing carbon-fiber precursor acrylic fiber bundle, and carbon-fiber bundle using carbon-fiber precursor acrylic fiber bundle |
Non-Patent Citations (1)
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| 李连贵等: "聚丙烯腈基碳纤维原丝用油剂的制备", 《上海纺织科技》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113897708A (en) * | 2021-11-18 | 2022-01-07 | 中复神鹰碳纤维股份有限公司 | Oiling agent for polyacrylonitrile carbon fiber precursor and preparation method thereof |
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