CN112725941A - Carbon fiber precursor oiling agent capable of bearing high-power steam drafting - Google Patents
Carbon fiber precursor oiling agent capable of bearing high-power steam drafting Download PDFInfo
- Publication number
- CN112725941A CN112725941A CN202011571929.1A CN202011571929A CN112725941A CN 112725941 A CN112725941 A CN 112725941A CN 202011571929 A CN202011571929 A CN 202011571929A CN 112725941 A CN112725941 A CN 112725941A
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- Prior art keywords
- oil
- silicone oil
- carbon fiber
- fiber precursor
- agent
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 33
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 33
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 239000002243 precursor Substances 0.000 title claims abstract description 27
- 239000008041 oiling agent Substances 0.000 title claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 30
- 229920000459 Nitrile rubber Polymers 0.000 claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 20
- 238000004132 cross linking Methods 0.000 claims abstract description 3
- 229920002545 silicone oil Polymers 0.000 claims description 59
- 239000004593 Epoxy Substances 0.000 claims description 23
- 239000000835 fiber Substances 0.000 claims description 17
- 125000004494 ethyl ester group Chemical group 0.000 claims description 15
- 150000001450 anions Chemical class 0.000 claims description 12
- 239000002736 nonionic surfactant Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000002131 composite material Substances 0.000 claims description 11
- 239000000178 monomer Substances 0.000 claims description 9
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 8
- 229920000570 polyether Polymers 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims description 6
- 229920013822 aminosilicone Polymers 0.000 claims description 6
- DLFDEDJIVYYWTB-UHFFFAOYSA-N dodecyl(dimethyl)azanium;bromide Chemical compound Br.CCCCCCCCCCCCN(C)C DLFDEDJIVYYWTB-UHFFFAOYSA-N 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 229920000136 polysorbate Polymers 0.000 claims description 6
- 238000009775 high-speed stirring Methods 0.000 claims description 5
- 238000004945 emulsification Methods 0.000 claims description 4
- 238000006116 polymerization reaction Methods 0.000 claims description 3
- 239000011550 stock solution Substances 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 2
- 238000002166 wet spinning Methods 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 3
- 229920001296 polysiloxane Polymers 0.000 claims 2
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims 2
- 239000006185 dispersion Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 125000004093 cyano group Chemical group *C#N 0.000 abstract description 2
- 229920002239 polyacrylonitrile Polymers 0.000 description 6
- 238000001035 drying Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000009987 spinning Methods 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 3
- 230000001804 emulsifying effect Effects 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material 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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/04—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
- D01F11/06—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/02—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F6/18—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolymers obtained by reactions only involving carbon-to-carbon unsaturated bonds from polymers of unsaturated nitriles, e.g. polyacrylonitrile, polyvinylidene cyanide
Abstract
The invention discloses a carbon fiber precursor oiling agent capable of bearing high-power steam drafting. The oil agent prepared by the invention has the advantages that the self-crosslinking reaction can be carried out at high temperature to form a net-shaped oil agent with high tensile toughness, and the tensile toughness of the oil film is further improved through the nano-level nitrile rubber powder, the intermolecular force of cyano groups and the oil agent and the tensile toughness of the nitrile rubber powder among chains of the net-shaped structure while forming a net-shaped structure, so that the oil film can bear the stretching force with higher multiple.
Description
Technical Field
The invention belongs to the technical field of preparation of high-performance carbon fiber precursors, and particularly relates to a carbon fiber precursor oiling agent capable of bearing high-power steam drafting.
Background
The polyacrylonitrile-based carbon fiber is the most promising precursor for producing high-performance carbon fiber, and the carbon fiber can be prepared by using polyacrylonitrile precursor as a starting raw material through pre-oxidation and carbonization processes. The oiling agent is used as a surface protective film in the protofilament process, namely the fiber is protected from being scratched in the running process and is protected in the subsequent oxidation process, so that the fiber is prevented from generating a sheath core. Uniformity of oiling on the filament surface is important. In the process of pursuing high-strength carbon fibers, steam drafting high-power orientation positively contributes to strength, the drafting multiple is increased, and the oiling agent also needs to synchronously bear the drafting multiple, so that higher requirements are made on the tensile toughness of the oiling agent.
Disclosure of Invention
The invention aims to provide a carbon fiber precursor oiling agent capable of bearing high-power steam drafting.
The purpose of the invention is realized by providing a carbon fiber precursor oiling agent capable of bearing high-power steam drafting, which comprises the following components:
in the conventional amino silicone oil with the molecular weight of 1000-1500 g/mol: epoxy silicone oil: in the polyether silicone oil mass ratio of (60-70) to (13-23) to (7-27), the epoxy polyamino silicone oil and the silicone oil ethyl ester silicone oil with the molecular weights of 1000-1500g/mol and 2100-3000g/mol are respectively added to be modified monomer silicone oil, and the composite oil agent comprises the following components: epoxy polyamino silicone oil: the mass ratio of the silicone oil ethyl ester to the silicone oil is (75-85): (5-10): (5-20), on the basis, the particle size of the nanometer-grade nitrile rubber powder is increased to be 30-120nm, the amount of the nitrile rubber powder is 0.5-2% of the total mass of the oil agent, and the nitrile rubber can be produced and used after high-speed stirring and dispersing treatment at 3000-5000 rpm in an emulsifying system in which the anion is dodecyl dimethyl ammonium bromide, the nonionic surfactant is tween or Span80 and the ratio of the anion to the nonionic surfactant is 1: 3-1: 14.
The carbon fiber precursor is spun by a polymerization stock solution, and an oil film is formed on the surface of the fiber after the carbon fiber precursor is washed by water at 30-40 ℃, drawn by water at 70-85 ℃, oiled at 25-35 ℃ and dried at 100-180 ℃. Wherein the concentration of the oil groove is controlled to be 1.8-2.5%.
Compared with the prior art, the invention has the following remarkable advantages:
1. through the addition of active monomers and high-temperature self-crosslinking reaction, a three-dimensional reticular oil film layer is formed;
2. when a net structure is formed, the tensile toughness of the oil film is further improved through the nano-grade nitrile rubber powder, the intermolecular force of cyano groups and an oil agent between chains of the net structure and the tensile toughness of the nitrile rubber powder.
3. The formed oil film and fiber are drawn by a steam drawing machine under the steam pressure of 0.4-0.65MPa, the drawing multiple of 3-6 times can be borne, and the oil agent falling rate before and after the steam drawing is 0.01-0.03%.
Detailed Description
The present invention will be further explained with reference to examples.
Example 1
In the production process of dry-jet wet-spun polyacrylonitrile carbon fibers, the composite oil agent is prepared from amino silicone oil (molecular weight of 1300 g/mol): epoxy silicone oil (molecular weight 1200 g/mol): in the polyether silicone oil (molecular weight 800g/mol) with the mass ratio of 65:25:10, the epoxy polyamino silicone oil and the silicone oil ethyl ester silicone oil with the molecular weights of 1200g/mol and 3000g/mol are added as modified monomer silicone oil, and the composite oil agent is prepared by the following steps: epoxy polyamino silicone oil: the mass ratio of the silicone oil ethyl ester to the silicone oil is 85: 5:10, on the basis, the granularity of the nanometer nitrile rubber powder is increased to 100nm, the amount of the nitrile rubber powder is 0.8 percent of the total mass of the oil agent, and the nitrile rubber can be produced and used after high-speed stirring and dispersing treatment at 4000rpm in an emulsification system with the anion of dodecyl dimethyl ammonium bromide, the nonionic surfactant of tween or Span80 and the ratio of the anion to the nonionic surfactant of 1: 8.
Spinning carbon fiber precursor with the polymer solution, washing with water at 40 deg.C, drawing with water at 85 deg.C, applying oil at 25 deg.C, and drying at 160 deg.C to form oil film on the fiber surface. Wherein the concentration of the oil groove is controlled to be 1.8 percent. The drafting can be carried out under the steam pressure of 0.55MPa, the drafting time can be 4.5 times that of the fiber synchronously, and the oil falling rate before and after the steam drafting is 0.02%.
Example 2
In the production process of dry-jet wet-spun polyacrylonitrile carbon fibers, the composite oil agent is prepared from amino silicone oil (with the molecular weight of 1000 g/mol): epoxy silicone oil (molecular weight 1500 g/mol): in the polyether silicone oil (molecular weight 1000g/mol) with the mass ratio of 70:20:10, epoxy polyamino silicone oil and silicone oil ethyl ester silicone oil with the molecular weights of 1500g/mol and 2500g/mol are added as modified monomer silicone oil, and the composite oil agent is prepared by the following steps: epoxy polyamino silicone oil: the mass ratio of the silicone oil ethyl ester to the silicone oil is 80: 10: 10, on the basis, the granularity of the nanometer nitrile rubber powder is increased to 100nm, the amount of the nitrile rubber powder is 1.0 percent of the total mass of the oil agent, and the nitrile rubber can be produced and used after high-speed stirring and dispersing treatment at 4000rpm in an emulsification system with the anion of dodecyl dimethyl ammonium bromide, the nonionic surfactant of tween or Span80 and the ratio of the anion to the nonionic surfactant of 1: 10.
Spinning carbon fiber precursor with the polymer solution, washing with water at 40 deg.C, drawing with water at 85 deg.C, applying oil at 25 deg.C, and drying at 180 deg.C to form oil film on the fiber surface. Wherein the concentration of the oil groove is controlled at 2.0%. The drafting can be carried out under the steam pressure of 0.58MPa, the drafting time and the fiber can synchronously bear the steam drafting multiple of 4.9 times, and the oil agent falling rate before and after the steam drafting is 0.01 percent.
Example 3
In the production process of dry-jet wet-spun polyacrylonitrile carbon fibers, the composite oil agent is prepared from amino silicone oil (with the molecular weight of 1500 g/mol): epoxy silicone oil (molecular weight 1500 g/mol): in the polyether silicone oil (with the molecular weight of 1500g/mol) with the mass ratio of 70:20:10, epoxy polyamino silicone oil and silicone oil ethyl ester silicone oil with the molecular weights of 1500g/mol and 2500g/mol are added as modified monomer silicone oil, and the composite oil agent is prepared by the following steps: epoxy polyamino silicone oil: the mass ratio of the silicone oil ethyl ester to the silicone oil is 80: 5: 15, on the basis, the granularity of the nanometer nitrile rubber powder is increased to 80nm, the amount of the nitrile rubber powder is 1.2 percent of the total mass of the oil agent, and the nitrile rubber can be produced and used after being stirred and dispersed at a high speed of 5000rpm in an emulsifying system with the anion of dodecyl dimethyl ammonium bromide, the nonionic surfactant of tween or Span80 and the ratio of the anion to the nonionic surfactant of 1: 12.
Spinning carbon fiber precursor with the polymer solution, washing with water at 40 deg.C, drawing with water at 85 deg.C, applying oil at 25 deg.C, and drying at 180 deg.C to form oil film on the fiber surface. Wherein the concentration of the oil groove is controlled at 2.2 percent. The drafting can be carried out under the steam pressure of 0.61MPa, the drafting time can be 5.1 times of the steam drafting time of the fiber synchronously, and the oil agent falling rate before and after the steam drafting is 0.01 percent.
Example 4
In the production process of wet spinning polyacrylonitrile carbon fiber, the composite oil agent is prepared according to the following steps of amino silicone oil (molecular weight is 1000 g/mol): epoxy silicone oil (molecular weight 1000 g/mol): in the polyether silicone oil (molecular weight 1000g/mol) with the mass ratio of 70:20:10, epoxy polyamino silicone oil and silicone oil ethyl ester silicone oil with the molecular weights of 1000g/mol and 2100g/mol are added as modified monomer silicone oil, and the composite oil agent is prepared by the following steps: epoxy polyamino silicone oil: the mass ratio of the silicone oil ethyl ester to the silicone oil is 80: 15: 5, on the basis, the granularity of the nanometer nitrile rubber powder is increased to 80nm, the amount of the nitrile rubber powder is 0.8 percent of the total mass of the oil agent, and the nitrile rubber can be produced and used after high-speed stirring and dispersing treatment at 4000rpm in an emulsification system with the anion of dodecyl dimethyl ammonium bromide, the nonionic surfactant of tween or Span80 and the ratio of the anion to the nonionic surfactant of 1: 12.
Spinning carbon fiber precursor by using a polymerization stock solution, washing by using water at 50 ℃, drawing by using water at 95 ℃, oiling at 25 ℃ and drying at 140 ℃ to form an oil film on the surface of the fiber. Wherein the concentration of the oil groove is controlled to be 2.4 percent. The drafting can be carried out under the steam pressure of 0.45MPa, the drafting time can be 3.8 times of the steam drafting time of the fiber synchronously, and the oil agent falling rate before and after the steam drafting is 0.01 percent.
It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that various changes and modifications to the invention described herein may occur to those skilled in the art upon reading the teachings herein, and that such equivalents are within the scope of the invention as defined in the appended claims.
Claims (8)
1. The carbon fiber precursor oiling agent capable of bearing high-power steam drafting is characterized in that:
the carbon fiber precursor oil is characterized in that epoxy polyamino and silicone ethyl ester are added into amino, epoxy and polyether compound oil to form an oil film, and nano-level nitrile rubber powder is added and uniformly distributed in the oil film; the oil film can bear 3.0-6.0 times of steam drafting multiple on the surface of the fiber synchronously with the fiber.
2. The carbon fiber precursor oil solution capable of withstanding high-power steam drawing according to claim 1, wherein: the amino silicone oil in the composite oil agent is as follows: epoxy silicone oil: the mass ratio of the polyether silicone oil is (60-70): 13-23): 7-27, and the molecular weight is 3000-.
3. The carbon fiber precursor oil solution capable of withstanding high-power steam drawing according to claim 1, wherein: the epoxy polyamino silicone oil and the silicone oil ethyl ester silicone oil are modified monomer silicone oil, and the molecular weights of the epoxy polyamino silicone oil and the silicone oil ethyl ester silicone oil are respectively 1500g/mol in 1000-plus range and 3000g/mol in 2100-plus range; compound oil agent: epoxy polyamino silicone oil: the mass ratio of the silicone oil ethyl ester to the silicone oil is (75-85): (5-10): (5-20).
4. The carbon fiber precursor oil solution capable of withstanding high-power steam drawing according to claim 1, wherein: the granularity of the nanometer nitrile rubber powder is 30-120nm, and the amount of the nitrile rubber powder is 0.5-2% of the total mass of the oil agent.
5. The carbon fiber precursor oil solution capable of withstanding high-power steam drawing according to claim 1, wherein: the composite oil agent, the modified monomer silicone oil and the nano-grade nitrile butadiene rubber powder are subjected to high-speed stirring dispersion treatment at 3000-5000 rpm in an emulsification system, wherein the anion is dodecyl dimethyl ammonium bromide, the nonionic surfactant is tween or Span80, and the ratio of the anion to the nonionic surfactant is 1: 3-1: 14.
6. A preparation method of the carbon fiber precursor oil agent capable of enduring high-power steam drafting based on any one of claims 1 to 5, which is characterized by comprising the following steps: firstly, adding reactive silicone oil with epoxy polyamino and silicone ethyl ester as modified monomers into amino, epoxy and polyether compound oil agent to enable the oil agent to be capable of quickly self-crosslinking into an oil film at the temperature of 100-180 ℃; adding nanometer nitrile rubber powder into the oil solution, and uniformly distributing the nitrile rubber powder in the oil film; the formed oil film can bear 3.0-6.0 times of steam drafting multiple on the surface of the fiber synchronously with the fiber.
7. A filament-making method based on the carbon fiber precursor oil agent capable of enduring high-power steam drafting according to any one of claims 1 to 5, characterized in that: the carbon fiber precursor is spun by a polymerization stock solution, and an oil film is formed on the surface of the fiber after the carbon fiber precursor is washed by water at 30-40 ℃, drawn by water at 70-85 ℃, oiled at 25-35 ℃ and dried at 180 ℃ with 100 ℃, wherein the concentration of an oil groove is controlled at 1.8-2.5%.
8. The application of the carbon fiber precursor oiling agent capable of bearing high-power steam drafting is characterized in that the oiling agent can be used in wet and dry-jet wet spinning carbon fiber precursor sections.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011571929.1A CN112725941A (en) | 2020-12-27 | 2020-12-27 | Carbon fiber precursor oiling agent capable of bearing high-power steam drafting |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011571929.1A CN112725941A (en) | 2020-12-27 | 2020-12-27 | Carbon fiber precursor oiling agent capable of bearing high-power steam drafting |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112725941A true CN112725941A (en) | 2021-04-30 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011571929.1A Pending CN112725941A (en) | 2020-12-27 | 2020-12-27 | Carbon fiber precursor oiling agent capable of bearing high-power steam drafting |
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Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5726241A (en) * | 1994-01-19 | 1998-03-10 | Hexcel Corporation | Finishing oil for precursor for high performance carbon fibers and precursor |
| JP2000136485A (en) * | 1998-08-28 | 2000-05-16 | Toray Ind Inc | Silicone straight oil finishing agent, precursor fiber for carbon fiber, carbon fiber and their production |
| JP2001172879A (en) * | 1999-10-08 | 2001-06-26 | Sanyo Chem Ind Ltd | Oil agent for production of carbon fiber |
| JP2003027378A (en) * | 2001-07-17 | 2003-01-29 | Toray Ind Inc | Silicone oil solution for carbon fiber precursor, precursor fiber for carbon fiber and method for producing carbon fiber |
| 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 |
| WO2011118791A1 (en) * | 2010-03-26 | 2011-09-29 | 日本ペイント株式会社 | Method for forming coating film |
| CN103122504A (en) * | 2011-11-18 | 2013-05-29 | 中国石油化工股份有限公司 | Oiling method for small tow PAN (Polyacrylonitrile)-based carbon fiber precursors |
| CN104179019A (en) * | 2014-08-25 | 2014-12-03 | 中复神鹰碳纤维有限责任公司 | Preparation method of carbon fiber precursor oil agent |
-
2020
- 2020-12-27 CN CN202011571929.1A patent/CN112725941A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5726241A (en) * | 1994-01-19 | 1998-03-10 | Hexcel Corporation | Finishing oil for precursor for high performance carbon fibers and precursor |
| JP2000136485A (en) * | 1998-08-28 | 2000-05-16 | Toray Ind Inc | Silicone straight oil finishing agent, precursor fiber for carbon fiber, carbon fiber and their production |
| JP2001172879A (en) * | 1999-10-08 | 2001-06-26 | Sanyo Chem Ind Ltd | Oil agent for production of carbon fiber |
| JP2003027378A (en) * | 2001-07-17 | 2003-01-29 | Toray Ind Inc | Silicone oil solution for carbon fiber precursor, precursor fiber for carbon fiber and method for producing carbon fiber |
| 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 |
| WO2011118791A1 (en) * | 2010-03-26 | 2011-09-29 | 日本ペイント株式会社 | Method for forming coating film |
| CN103122504A (en) * | 2011-11-18 | 2013-05-29 | 中国石油化工股份有限公司 | Oiling method for small tow PAN (Polyacrylonitrile)-based carbon fiber precursors |
| CN104179019A (en) * | 2014-08-25 | 2014-12-03 | 中复神鹰碳纤维有限责任公司 | Preparation method of carbon fiber precursor oil agent |
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Application publication date: 20210430 |