CN113445324A - Carbon fiber oil agent suitable for alpine regions - Google Patents
Carbon fiber oil agent suitable for alpine regions Download PDFInfo
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- CN113445324A CN113445324A CN202110741090.XA CN202110741090A CN113445324A CN 113445324 A CN113445324 A CN 113445324A CN 202110741090 A CN202110741090 A CN 202110741090A CN 113445324 A CN113445324 A CN 113445324A
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- Prior art keywords
- carbon fiber
- agent
- oil agent
- oil
- alpine
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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
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/6436—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing amino groups
-
- 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
- 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
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/647—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing polyether sequences
-
- 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
- D06M15/643—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain
- D06M15/65—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds containing silicon in the main chain containing epoxy groups
-
- 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
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
- D06M2101/28—Acrylonitrile; Methacrylonitrile
Abstract
The invention discloses a carbon fiber oil agent suitable for alpine regions. The carbon fiber oil agent suitable for alpine regions is an emulsion with the mass concentration of 20-30% prepared from an effective component and water, and is characterized in that an organic silicon oil agent with polydimethylsiloxane as a basic component is selected and subjected to graft modification by a surfactant, and components such as an antifreezing agent, a lubricating agent, an antistatic agent and the like are added, the effective component begins to be cooled at the speed of 5-10 ℃/min in an air environment, the viscosity of a dispersion system changes within the range of 7.2-25 mPa.s in the cooling process of 20-50 ℃, the light transmittance is 80-95%, the phenomena of emulsion breaking and oil floating are avoided, the oil agent emulsion still has stability in the alpine environment, and the emulsion can be stably stored for 8-12 months in the cold environment of 0-50 ℃.
Description
Technical Field
The invention relates to the technical field of carbon fiber production, in particular to a carbon fiber oiling agent suitable for alpine regions.
Background
The performance of the carbon fiber precursor oiling agent is a key technical index in carbon fiber production, and the performance of the oiling agent has direct influence on the wear resistance, the antistatic property, the surface smoothness and the structure compactness of the precursor. The market demand for carbon fiber, a high-performance material, is getting larger and larger, and in order to expand the capacity, production enterprises are not only distributed in coastal areas, but also begin to shift to various areas in China. Aiming at the problem that the severe natural environment of alpine regions easily causes the phenomena of coagulation, emulsion breaking, deterioration and the like of carbon fiber oiling agents to further influence the performance of carbon fiber precursors, the invention develops the carbon fiber oiling agent which can be suitable for the alpine regions.
Disclosure of Invention
The invention aims to provide a carbon fiber oiling agent suitable for alpine regions.
The technical scheme for realizing the purpose of the invention is as follows:
the invention provides a carbon fiber oiling agent suitable for alpine regions, wherein the effective component of the carbon fiber oiling agent is a uniform emulsion which is prepared from water and has the mass concentration of 20-30%; in the effective components of the carbon fiber oil agent, the weight ratio of functional group modified polydimethylsiloxane to the emulsifier is 4-9: 1-6 percent of assistant, and the assistant accounts for 1-10 percent of the total mass of the oil agent.
Compared with the prior art, the invention has the following remarkable advantages:
1. according to the invention, the high temperature resistance of the oil agent in the pre-oxidation and carbonization stages is ensured after the grafting modification is carried out on the components of the common silicone oil, and the oil agent can play a role in bundling and preventing protofilaments from being adhered; after the cold-resistant surfactant and the anti-freezing agent are added, the components of the oil agent have high cold resistance, the stability of components, states and performance can be kept in a high-cold environment, the smooth operation of the carbon fiber manufacturing process is ensured, and the oil agent is suitable for the production and preparation of carbon fibers in high-cold areas.
2. The carbon fiber oil starts to be cooled at a speed of 5-10 ℃/min in an air environment, the viscosity of a dispersion system is changed within a range of 7.2-25 mPa.s in the cooling process of 20-50 ℃, and the light transmittance of the oil is 80-95%.
Detailed Description
The preparation method of the carbon fiber oiling agent suitable for the alpine region comprises the steps of combining one or more of epoxy modified polysiloxane, amino modified polysiloxane and polyether modified polysiloxane to finish modification of an organic silicon oiling agent with polydimethylsiloxane as a main component, and then mixing functional group modified polydimethylsiloxane and an emulsifier according to the ratio of 4-9: 1 to 6 by weight.
The preferable emulsifier is one of fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ether or fatty amine polyglycol ether with good anti-coking capability and antistatic property and a combination thereof, and is stirred at a high speed and slowly added with deionized water in the process, and then an auxiliary agent with anti-freezing and lubricating properties accounting for 1-10% of the total mass of the oil agent is added, so that the mixture is uniformly mixed, and the uniform emulsion with the mass concentration of 20-30% prepared by the effective component and water is obtained.
The prepared oil solution starts to be cooled at the speed of 5-10 ℃/min in the air environment, the viscosity of a dispersion system is changed within the range of 7.2-25 mPa.s in the cooling process of 20-50 ℃, and the light transmittance of the oil solution is 80-95%. The carbon fiber oil agent is placed in a cold environment at the temperature of 0-50 ℃ below zero and can be stably stored for 8-12 months. The oil content of the polyacrylonitrile precursor in the oiling process is kept at 0.5-1.5%, the oil content is controlled at 0.2-1.0% in the pre-oxidation and carbonization stages in a high-temperature state, the oiling agent has lubricating and protecting effects on the surface of the fiber, the defects on the surface and the inside of the carbon fiber can be reduced, and the excellent and stable properties of the oiling agent indirectly ensure the mechanical property of the polyacrylonitrile carbon fiber.
The following structural general formula of the polydimethylsiloxane modified by multiple functional groups in the invention
a. Multiple workThe structural general formula of the molecule of the dimethyl silicone polymer modified by the radical is shown in the specification, wherein R ═ CH (CH)2) X, wherein
X＝1～3；
b. Several functional groups representing F in the general structural formula a
Example 1
Taking 3 parts of amino modified polydimethylsiloxane oil, 3 parts of epoxy modified polydimethylsiloxane oil and 3 parts of polyether modified polydimethylsiloxane oil, adding 6 parts of emulsifying agent, uniformly mixing surfactant and antifreezing agent accounting for 10% of the total mass of the silicone oil and the emulsifying agent, and adding ionized water while stirring and dispersing at a high speed of 3000r/min to prepare a uniform emulsion with the mass concentration of 30%. When the oil agent is stored in an environment of 50 ℃ below zero, the viscosity of the oil agent is 23.5mPa.s, the standing time is as long as 8 months, the appearance of the oil agent is in a blue-blue transparent state, the phenomena of emulsion breaking and layering are avoided, and the light transmittance of the oil agent is 70%.
The oil content of the polyacrylonitrile protofilament is kept at 0.6% in the oiling process in the spinning stage, the burr phenomenon on the surface of the fiber is relatively reduced, and the conditions of doubling and breaking are improved. The oil content is controlled to be 0.4% in the pre-oxidation and carbonization stages in the high-temperature state, and the defect rate of the prepared carbon fiber tows is reduced by 70% compared with that of the carbon fiber tows which are not subjected to the modified oil agent.
Example 2
Taking 3 parts of amino modified polydimethylsiloxane oil, 2 parts of epoxy modified polydimethylsiloxane oil and 1 part of polyether modified polydimethylsiloxane oil, adding 3 parts of emulsifying agent, uniformly mixing surfactant and antifreezing agent with the total mass accounting for 5% of the total mass of the silicone oil and the emulsifying agent, and adding ionized water to prepare uniform emulsion with the mass concentration of 25% while stirring and dispersing at a high speed of 3000 r/min. When the oil agent is stored in an environment with the temperature of minus 30 ℃, the viscosity of the oil agent is 17.5mPa.s, the standing time is as long as 10 months, the appearance of the oil agent is in a blue-blue transparent state, the phenomena of demulsification and floating oil delamination do not occur, and the light transmittance of the oil agent is 83%.
The oil content of the polyacrylonitrile protofilament is kept at 0.8% in the oiling process in the spinning stage, the burr phenomenon on the surface of the fiber is obviously reduced, and the conditions of doubling and breaking are improved. The oil content is controlled to be 0.6% in the pre-oxidation and carbonization stages in the high-temperature state, and the defect rate of the prepared carbon fiber tows is reduced by 85% compared with that of the carbon fiber tows which are not subjected to the modified oil agent.
Example 3
Taking 2 parts of amino modified polydimethylsiloxane oil and 1 part of epoxy modified polydimethylsiloxane oil, adding 1 part of emulsifier, uniformly mixing surfactant and antifreeze agent with the total mass accounting for 1% of the total mass of the silicone oil and the emulsifier, and adding ionized water while stirring and dispersing at a high speed of 3000r/min to prepare a uniform emulsion with the mass concentration of 20%. When the oil agent is stored in an environment at 15 ℃ below zero, the viscosity of the oil agent is 10.5mPa.s, the standing time is as long as 12 months, the appearance of the oil agent is in a blue-blue transparent state, the phenomena of demulsification and floating oil delamination do not occur, and the light transmittance of the oil agent is 95%.
The oil content of the polyacrylonitrile protofilament is kept at 1.2% in the oiling process in the spinning stage, the burr phenomenon on the surface of the fiber is obviously reduced, and the conditions of doubling and breaking are obviously improved. The oil content in the pre-oxidation and carbonization stages at high temperature is controlled to be 0.8%, and the defect rate of the prepared carbon fiber tows is reduced by 93% compared with that of the carbon fiber tows without the modified oil agent on the surface and inside.
The modified oil agent has the effects of lubricating and protecting fibers, reduces the defects on the surface and the inside of the carbon fibers, obviously improves the mechanical property of the carbon fibers, and indirectly ensures the mechanical property of the polyacrylonitrile carbon fibers. The examples prove that the modified oil agent still has stability in high and cold environments, has reliable performance and can be suitable for the production industry of carbon fibers in high and cold areas.
The oil agent is used for the polyacrylonitrile precursor in the oiling process, the oil content is kept at 0.5-1.5%, the fiber surface is lubricated and protected, the defects on the surface and inside of the carbon fiber can be reduced, and the stability of the oil agent in the high and cold environment indirectly ensures the mechanical property of the polyacrylonitrile carbon fiber.
The present invention has been described in detail with reference to the foregoing specific embodiments, but it should be understood that the invention is not limited thereto, and various changes, substitutions and alterations can be made thereto without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (8)
1. The carbon fiber oil agent is suitable for alpine regions and is characterized in that: in the carbon fiber oiling agent, the effective component of the carbon fiber oiling agent is a uniform emulsion which is prepared by water and has the mass concentration of 20-30%; in the effective components of the carbon fiber oil agent, the weight ratio of functional group modified polydimethylsiloxane to the emulsifier is 4-9: 1-6 percent of assistant, and the assistant accounts for 1-10 percent of the total mass of the oil agent.
2. The carbon fiber oiling agent suitable for the alpine region according to claim 1, characterized in that: the functional group modified polydimethylsiloxane is one of epoxy modified polysiloxane, amino modified polysiloxane or polyether modified polysiloxane which can realize self-emulsification and has enough polyether content, and the combination thereof.
3. The carbon fiber oiling agent suitable for the alpine region according to claim 2, characterized in that: the amino modified polydimethylsiloxane is one of poly [3- ((2-aminoethyl) amino) propyl ] dimethyl siloxane, methoxy-terminated poly [3- ((2-aminoethyl) amino) propyl ] dimethyl siloxane and a combination thereof; the epoxy modified polydimethylsiloxane is one of 1, 2-epoxy cyclohexyl modified polydimethylsiloxane, 1, 2-epoxy cyclopentyl modified polydimethylsiloxane and a combination thereof.
4. The carbon fiber oiling agent suitable for the alpine region according to claim 1, characterized in that: the emulsifier is one of fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ether or fatty amine polyglycol ether or their combination.
5. The carbon fiber oiling agent suitable for the alpine region according to claim 1, characterized in that: and (3) electrically stirring the carbon fiber oil agent in the alpine region at the speed of 3000-4000 r/min to obtain a uniform emulsion with the mass concentration of 20-30% prepared by the effective components and water.
6. The carbon fiber oiling agent suitable for the alpine region according to claim 1, characterized in that: the auxiliary agent is epoxy fatty methyl ester serving as an antifreezing agent, so that the oil agent component can resist lower high and cold temperatures and cannot deteriorate in a low-temperature environment.
7. A preparation method of the carbon fiber oil agent suitable for the alpine region based on any one of claims 1-6, characterized by comprising the following steps: combining one or more than one of epoxy modified polysiloxane, amino modified polysiloxane or polyether modified polysiloxane to complete the modification of the organic silicon oil agent with polydimethylsiloxane as the main component, and then mixing the functional group modified polydimethylsiloxane with an emulsifier;
stirring at high speed during mixing, slowly adding deionized water, adding adjuvant, and mixing to obtain uniform emulsion containing effective components and water.
8. The application method of the carbon fiber oil agent suitable for the alpine region based on any one of claims 1 to 6 is characterized by comprising the following steps: in the oiling process, the oiling agent is used for the polyacrylonitrile protofilament, and the oil content is kept at 0.5-1.5%.
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| CN202110741090.XA CN113445324A (en) | 2021-06-30 | 2021-06-30 | Carbon fiber oil agent suitable for alpine regions |
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| CN202110741090.XA CN113445324A (en) | 2021-06-30 | 2021-06-30 | Carbon fiber oil agent suitable for alpine regions |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103014922A (en) * | 2011-09-22 | 2013-04-03 | 中国科学院化学研究所 | Organosilicon spinning oil agent used for preparing polyacrylonitrile-based carbon fiber, and preparation method thereof |
| CN103031734A (en) * | 2011-09-29 | 2013-04-10 | 中国石油化工股份有限公司 | Preparation method of oiling agent for small-filament-bundle PAN-based carbon fiber precursor |
| CN104448811A (en) * | 2014-11-14 | 2015-03-25 | 安邦电气集团有限公司 | Low-temperature reinforced type heating cable sheathing material and preparation method thereof |
| CN104894178A (en) * | 2015-05-12 | 2015-09-09 | 华南理工大学 | Method for preparing epoxidized fatty acid methyl ester |
| CN111139555A (en) * | 2019-12-26 | 2020-05-12 | 中复神鹰碳纤维有限责任公司 | High-heat-resistance oil agent and preparation method of polyacrylonitrile carbon fiber |
-
2021
- 2021-06-30 CN CN202110741090.XA patent/CN113445324A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103014922A (en) * | 2011-09-22 | 2013-04-03 | 中国科学院化学研究所 | Organosilicon spinning oil agent used for preparing polyacrylonitrile-based carbon fiber, and preparation method thereof |
| CN103031734A (en) * | 2011-09-29 | 2013-04-10 | 中国石油化工股份有限公司 | Preparation method of oiling agent for small-filament-bundle PAN-based carbon fiber precursor |
| CN104448811A (en) * | 2014-11-14 | 2015-03-25 | 安邦电气集团有限公司 | Low-temperature reinforced type heating cable sheathing material and preparation method thereof |
| CN104894178A (en) * | 2015-05-12 | 2015-09-09 | 华南理工大学 | Method for preparing epoxidized fatty acid methyl ester |
| CN111139555A (en) * | 2019-12-26 | 2020-05-12 | 中复神鹰碳纤维有限责任公司 | High-heat-resistance oil agent and preparation method of polyacrylonitrile carbon fiber |
Non-Patent Citations (1)
| Title |
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| 施惠生等: "《混凝土外加剂实用技术大全》", 31 December 2008 * |
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