High-wetting heat-resistant carbon fiber precursor oiling agent as well as preparation and application thereof

By using silicone oil protectants and polyether esters to prepare carbon fiber precursor oils, the problems of insufficient heat resistance and film-forming properties of existing oils are solved, the wettability and mechanical properties of carbon fibers are improved, and the ash content is reduced.

CN120989769AActive Publication Date: 2025-11-21DONGHUA UNIV
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Patent Information

Application Number
CN202511534842.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-10-27
Publication Date
2025-11-21
Estimated Expiration
2045-10-27

AI Technical Summary

Technical Problem

Existing carbon fiber oils have problems such as poor heat resistance, poor film-forming properties, and high ash content, and cannot effectively protect carbon fiber precursors.

Method used

Using silicone oil protectant and polyether esters as the main components, along with emulsifiers, antistatic agents and defoamers, carbon fiber precursor oil is prepared by phase inversion method to form a stable emulsion, thereby improving wettability and heat resistance.

Benefits of technology

It achieves excellent wettability and film-forming properties of carbon fiber precursor, reduces ash content, and improves the mechanical properties of carbon fiber.

✦ Generated by Eureka AI based on patent content.

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Patent Text Reader

Abstract

The invention relates to a high-wettability heat-resistant carbon fiber precursor oiling agent as well as preparation and application thereof. The high-wettability heat-resistant carbon fiber precursor oiling agent is prepared from the following components: a silicone oil protective agent, polyether ester, an emulsifier, an antistatic agent, a de-foaming agent and de-ionized water. The carbon fiber precursor oiling agent disclosed by the invention has excellent lubricity, heat resistance and film-forming property, meanwhile, the oiling agent has high wettability and excellent fiber wetting effect, and can effectively protect fibers, reduce the ash content and improve the performance of carbon fibers.
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Description

TECHNICAL FIELD

[0001] The present application belongs to the field of precursor oil, and particularly relates to a high-wetting heat-resistant carbon fiber precursor oil as well as preparation and application thereof. BACKGROUND

[0002] Carbon fiber is a kind of fiber material with excellent properties such as high strength, high modulus, heat corrosion resistance and corrosion resistance. It is widely used in aerospace, railway transportation, wind power generation, medical devices, leisure and entertainment and other fields. Among them, polyacrylonitrile-based carbon fiber has the most optimal performance and relatively low price, and accounts for the largest proportion in the carbon fiber market.

[0003] Carbon fiber oil is an important auxiliary agent used in the production of carbon fiber precursor, and plays an important role in the production of high-performance carbon fiber. The carbon fiber oil generates a uniform oil film on the surface of each single fiber, which isolates the single fibers from each other to prevent adhesion and fiber combination. Since the generated oil film has softness and self-lubricating property, it can also prevent friction and wear between the fiber bundle and the roller during production. In the pre-oxidation process, it can prevent heat accumulation or overheating, causing local thermal adhesion or thermal combination between single fibers, which helps to form homogeneous fibers. The oil film still has a protective effect on the fiber surface during low-temperature carbonization.

[0004] Most carbon fiber oils use silicon-based oils, mainly modified silicon oils with amino, epoxy and polyether groups. Carbon fiber oil is an oil agent prepared by compounding silicon oil, deionized water and additives. Currently, domestic oil agents have many problems, such as poor heat resistance, poor film formation and high ash content. The current patents of carbon fiber oil mainly focus on improving the heat resistance and film formation of the oil agent. For example: Chinese patent CN118773778A uses low molecular weight polysiloxane and phosphate-modified polysiloxane as the main component to obtain a high protective carbon fiber oil with self-crosslinking and film-forming properties; Chinese patent CN116657287A introduces phenyl-modified silicon oil into the carbon fiber oil system with amino-polyether-modified silicon oil as the main component to improve the heat resistance of the oil agent. The oil agents of the above patents are all modified silicon oils with different functional groups to improve the performance of the oil agent, but only improve the performance of the oil agent on one side, and the silicon oil is modified by short chain groups, and the ash content of the oil agent is high. SUMMARY

[0005] In view of the defects of the prior art, the technical problem to be solved by the present application is to provide a high-wetting heat-resistant carbon fiber precursor oil and its preparation and application. The oil agent has excellent wettability, film formation and heat resistance, and has good protection performance for the fiber.

[0006] The present application provides a carbon fiber precursor oil, the components of which include, by weight fraction:

[0007] 10-30 parts of silicone oil protectant;

[0008] 10-30 parts of polyether esters;

[0009] 1-5 parts emulsifier;

[0010] 1-5 parts of antistatic agent;

[0011] 1-5 parts of defoamer;

[0012] 60-80 parts deionized water;

[0013] The structural formula of the silicone oil protective agent is:

[0014] ;

[0015] Where a is an integer from 5 to 50, b is an integer from 5 to 50, c is an integer from 20 to 200, d is an integer from 5 to 50, and R is... R3 and R4 are selected from C1 to C2 respectively. 10 Alkyl groups.

[0016] Preferably, the molecular weight of the silicone oil protectant is 5000 to 30000.

[0017] Preferably, the silicone oil protectant is obtained by mixing and reacting phenyl hydrogen silicone oil, unsaturated alcohol ether, solvent and catalyst;

[0018] The unsaturated alcohol ether mentioned above is:

[0019] R3 and R4 are selected from C1 to C2 respectively. 10 Alkyl groups.

[0020] The solvent includes one or more of toluene, isopropanol, dichloromethane, chloroform, methanol, acetone, acetonitrile, and dimethyl sulfoxide; the catalyst is chloroplatinic acid.

[0021] The reaction in the preparation of silicone oil protective agent: under nitrogen protection, pre-activation at 50-70℃ for 1-2 h, reaction at 90-110℃ for 3-6 h, and finally de-oxidation under reduced pressure at 120-150℃.

[0022] Preferably, the preparation of the phenyl hydrogen-containing silicone oil includes: mixing octamethylcyclotetrasiloxane, benzene-containing siloxane, hydrogen-containing siloxane, end-capping agent and catalyst, reacting to obtain phenyl hydrogen-containing silicone oil;

[0023] The benzene-containing siloxane is one or more of octaphenylcyclotetrasiloxane, hexaphenylcyclotrisiloxane, diphenyldimethoxysilane, and diphenyldiethoxysilane; the hydrogen-containing siloxane is one or more of tetramethylcyclotetrasiloxane, polymethylhydrosiloxane, pentamethylcyclopentasiloxane, heptamethyltrisiloxane, and octamethyltrisiloxane.

[0024] The end-capping agent is one or more of hexamethyldisiloxane and tetramethyldisiloxane; the catalyst is concentrated sulfuric acid.

[0025] The reaction in the preparation of phenyl hydrogen silicone oil is carried out under nitrogen protection at 40-70°C for 5-9 hours, and finally depressurized at 150-200°C.

[0026] Preferably, the polyether ester has the following structural formula: Where m is an integer from 1 to 10, and R5 is a integer from C2 to C5. 15 Alkyl groups.

[0027] Preferably, the mass ratio of the silicone oil protectant to the polyether ester is (0.5~6):1, and more preferably, the mass ratio is (0.5~2):1.

[0028] Preferably, the emulsifier includes one or more of nonylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, isomeric alcohol polyoxyethylene ether, polyvinyl alcohol, sodium dodecylbenzene sulfonate, and trihydroxymethane polyoxyethylene ether.

[0029] Preferably, the antistatic agent comprises one or more of polyoxyethylene laurate, polyoxyethylene fatty alcohol phosphate, sorbitan fatty acid ester, dodecyltrimethylammonium chloride, and hexadecyltrimethylammonium sulfonate.

[0030] Preferably, the defoamer includes one or more of diisobutylmethanol, ethylene glycol monostearate, isoamyl alcohol, and trialkylmelamine;

[0031] Preferably, the average particle size of the raw silk oil is 150–300 nm.

[0032] This invention provides a method for preparing any of the carbon fiber precursor oils, comprising:

[0033] Weigh each component according to the mass fraction, mix the silicone oil protectant, polyether ester, emulsifier, antistatic agent, and defoamer, then add deionized water and reverse the phase to form an emulsion, thus obtaining the carbon fiber precursor oil.

[0034] This invention provides the application of any of the carbon fiber precursor oiling agents in the preparation of polyacrylonitrile-based carbon fibers.

[0035] Beneficial effects

[0036] The carbon fiber precursor oil of this invention, with silicone oil protectant and polyether esters as the main components, has excellent wettability, film-forming properties and heat resistance, and can effectively protect carbon fiber precursor, improve the mechanical properties of carbon fiber, and reduce the ash content of carbon fiber. Detailed Implementation

[0037] The present invention will be further illustrated below with reference to specific embodiments. It should be understood that these embodiments are for illustrative purposes only and are not intended to limit the scope of the invention. Furthermore, it should be understood that after reading the teachings of this invention, those skilled in the art can make various alterations or modifications to the invention, and these equivalent forms also fall within the scope defined by the appended claims.

[0038] I. The pre-oxidation and carbonization conditions in the examples and comparative examples are as follows:

[0039] Pre-oxidation was carried out in an air atmosphere, and the temperature was maintained at 240℃, 250℃, and 260℃ for 15 min respectively. Carbonization was carried out in a nitrogen atmosphere using a gradient heating method, with the duration of passing through the low-temperature carbonization zone (400℃, 500℃, 600℃, 700℃, 800℃) and the high-temperature carbonization zone (1000℃, 1100℃, 1200℃, 1300℃, 1400℃) both being 2 min.

[0040] II. The testing standards and characterization methods are as follows:

[0041] The particle size of the oil was tested using a particle size analyzer.

[0042] The contact angle was tested using a contact angle measuring instrument to measure the contact angle of the oil on the PAN film;

[0043] The residual heat rate was tested using a thermogravimetric analyzer under nitrogen conditions, and the residual heat rate at 300℃ was used for comparison.

[0044] Mechanical properties were tested according to national standard GB / T 31290-2022, with a clamping distance of 20 mm and a moving speed of 2 mm / min;

[0045] Ash content was tested according to industry standard FZ / T 50044-2018.

[0046] III. Structural formula of the silicone oil protective agent in the examples:

[0047] ,

[0048] Where R is (a): ,or

[0049] (b):

[0050] The structural formula of polyether esters is:

[0051] .

[0052] Example 1

[0053] Highly wettable and heat-resistant carbon fiber precursor oil, comprising the following components by weight:

[0054] 20 parts silicone oil protectant;

[0055] 10 parts of polyether esters;

[0056] 5 parts of fatty alcohol polyoxyethylene ether;

[0057] 3 parts of dodecyltrimethylammonium chloride;

[0058] 2 parts of diisobutylmethanol;

[0059] 60 parts of deionized water.

[0060] The preparation steps of the silicone oil protective agent are as follows:

[0061] (1) Preparation of phenyl hydrogen-containing silicone oil:

[0062] Weigh 106.76 g of octamethylcyclotetrasiloxane, 60 g of diphenyldimethoxysilane, 30 g of polymethylhydrosiloxane, 3.24 g of hexamethyldisiloxane and 3 g of concentrated sulfuric acid, add each component to a reaction vessel and mix evenly. Under nitrogen protection, react at 60°C for 7 h, and then remove the phenyl hydrogen silicone oil by depressurization at 150°C.

[0063] (2) Preparation of silicone oil protective agent:

[0064] Take 200 g of phenyl hydrogen silicone oil, 98.19 g of unsaturated alcohol ether, 74.55 g of isopropanol and 0.018 g of chloroplatinic acid, mix them evenly, pre-activate at 70 °C for 1 h under nitrogen protection, react at 90 °C for 4 h, and then remove the impurities under reduced pressure at 120 °C to obtain the product.

[0065] The R group in the silicone oil protectant is (b), R3 is a C1 alkyl group, R4 is a C2 alkyl group, the molecular weight of the silicone oil protectant is 13682, a is 16, b is 37, c is 25, and d is 36.

[0066] In the polyether esterified compound, m is 2 and R5 is a C5 alkyl group.

[0067] The preparation process and performance testing of the oil are as follows:

[0068] The components, excluding deionized water, were mixed evenly in proportion, and then deionized water was added and stirred for 4 hours. After phase inversion, an emulsion with an average particle size of 194 nm was obtained. The emulsion has excellent stability, a contact angle of 8°, and a thermal residual rate of 98% at 300°C.

[0069] When this oil was applied to the preparation of T700 grade carbon fiber precursor, the resulting precursor was free of fuzz and had good film-forming effect. The carbon fiber obtained after pre-oxidation and carbonization treatment had a tensile strength of 5093 MPa and an ash content of 0.15%.

[0070] Example 2

[0071] Highly wettable and heat-resistant carbon fiber precursor oil, comprising the following components by weight:

[0072] 10 parts silicone oil protectant;

[0073] 20 parts of polyether esters;

[0074] 5 parts of fatty alcohol polyoxyethylene ether;

[0075] 3 parts of dodecyltrimethylammonium chloride;

[0076] 2 parts of diisobutylmethanol;

[0077] 60 parts of deionized water.

[0078] The silicone oil protectant and polyether ester are the same as in Example 1.

[0079] The preparation process and performance testing of the oil are as follows:

[0080] The components, excluding deionized water, were mixed evenly in proportion, and then deionized water was added and stirred for 4 hours. After phase inversion, an emulsion with an average particle size of 173 nm was obtained. The emulsion has excellent stability, a contact angle of 17°, and a thermal residual rate of 94% at 300°C.

[0081] When this oil agent is applied to the preparation of T700 grade carbon fiber precursor, the resulting precursor is free of fuzz and has good film-forming effect. After pre-oxidation and carbonization treatment, the carbon fiber obtained has a tensile strength of 4798 MPa and an ash content of 0.11%.

[0082] Example 3

[0083] Highly wettable and heat-resistant carbon fiber precursor oil, comprising the following components by weight:

[0084] 15 parts silicone oil protectant;

[0085] 15 parts of polyether esters;

[0086] 5 parts of fatty alcohol polyoxyethylene ether;

[0087] 3 parts of dodecyltrimethylammonium chloride;

[0088] 2 parts of diisobutylmethanol;

[0089] 60 parts of deionized water.

[0090] The silicone oil protectant and polyether ester are the same as in Example 1.

[0091] The preparation process and performance testing of the oil are as follows:

[0092] The components, excluding deionized water, were mixed evenly in proportion, and then deionized water was added and stirred for 4 hours. After phase inversion, an emulsion with an average particle size of 185 nm was obtained. The emulsion has excellent stability, a contact angle of 12°, and a thermal residual rate of 96% at 300°C.

[0093] When this oil agent is applied to the preparation of T700 grade carbon fiber precursor, the resulting precursor is free of fuzz and has good film-forming effect. The carbon fiber obtained after pre-oxidation and carbonization treatment has a tensile strength of 4896 MPa and an ash content of 0.13%.

[0094] Example 4

[0095] Highly wettable and heat-resistant carbon fiber precursor oil, with the same mass fractions of each component as in Example 1.

[0096] The preparation steps of the silicone oil protectant are the same as in Example 1, wherein the R group in the silicone oil protectant is (b), R3 is a C3 alkyl group, and R4 is a C6 alkyl group.

[0097] Polyether esters are the same as in Example 1.

[0098] The preparation process and performance testing of the oil are as follows:

[0099] The components, excluding deionized water, were mixed evenly in proportion, and then deionized water was added and stirred for 4 hours. After phase inversion, an emulsion with an average particle size of 197 nm was obtained. The emulsion has excellent stability, a contact angle of 9°, and a thermal residual rate of 98% at 300°C.

[0100] When this oil was applied to the preparation of T700 grade carbon fiber precursor, the resulting precursor was free of fuzz and had good film-forming effect. After pre-oxidation and carbonization treatment, the carbon fiber obtained had a tensile strength of 4932 MPa and an ash content of 0.15%.

[0101] Example 5

[0102] Highly wettable and heat-resistant carbon fiber precursor oil, with the same mass fractions of each component as in Example 1.

[0103] The preparation steps of the silicone oil protectant are the same as in Example 1, wherein the R group in the silicone oil protectant is (b), R3 is a C5 alkyl group, and R4 is a C8 alkyl group.

[0104] The polyether esterification is the same as in Example 1.

[0105] The preparation process and performance testing of the oil are as follows:

[0106] The components, excluding deionized water, were mixed evenly in proportion, and then deionized water was added and stirred for 4 hours. After phase inversion, an emulsion with an average particle size of 193 nm was obtained. The emulsion has excellent stability, a contact angle of 8°, and a thermal residual rate of 98% at 300°C.

[0107] When this oil was applied to the preparation of T700 grade carbon fiber precursor, the resulting precursor was free of fuzz and had good film-forming effect. The carbon fiber obtained after pre-oxidation and carbonization treatment had a tensile strength of 4967 MPa and an ash content of 0.14%.

[0108] Example 6

[0109] Highly wettable and heat-resistant carbon fiber precursor oil, with the same mass fractions of each component as in Example 1.

[0110] The silicone oil protectant is the same as in Example 1.

[0111] In the polyether ester, m is 5 and R5 is C. 10 alkyl.

[0112] The preparation process and performance testing of the oil are as follows:

[0113] The components, excluding deionized water, were mixed evenly in proportion, and then deionized water was added and stirred for 4 hours. After phase inversion, an emulsion with an average particle size of 191 nm was obtained. The emulsion has excellent stability, a contact angle of 8°, and a thermal residual rate of 98% at 300°C.

[0114] When this oil was applied to the preparation of T700 grade carbon fiber precursor, the resulting precursor was free of fuzz and had good film-forming effect. The carbon fiber obtained after pre-oxidation and carbonization treatment had a tensile strength of 4923 MPa and an ash content of 0.15%.

[0115] Example 7

[0116] Highly wettable and heat-resistant carbon fiber precursor oil, with the same mass fractions of each component as in Example 1.

[0117] The silicone oil protectant is the same as in Example 1.

[0118] In the polyether ester, m is 7 and R5 is C. 12 alkyl.

[0119] The preparation process and performance testing of the oil are as follows:

[0120] The components, excluding deionized water, were mixed evenly in proportion, and then deionized water was added and stirred for 4 hours. After phase inversion, an emulsion with an average particle size of 186 nm was obtained. The emulsion has excellent stability, a contact angle of 8°, and a thermal residual rate of 97% at 300°C.

[0121] When this oil agent is applied to the preparation of T700 grade carbon fiber precursor, the resulting precursor is free of fuzz and has good film-forming effect. After pre-oxidation and carbonization treatment, the carbon fiber obtained has a tensile strength of 4931 MPa and an ash content of 0.14%.

[0122] Comparative Example 1

[0123] Highly wettable and heat-resistant carbon fiber precursor oil, comprising the following components by weight:

[0124] 30 parts silicone oil protectant;

[0125] 5 parts of fatty alcohol polyoxyethylene ether;

[0126] 3 parts of dodecyltrimethylammonium chloride;

[0127] 2 parts of diisobutylmethanol;

[0128] 60 parts of deionized water.

[0129] The silicone oil protectant is the same as in Example 1.

[0130] The preparation process and performance testing of the oil are as follows:

[0131] The components, excluding deionized water, were mixed evenly in proportion, and then deionized water was added and stirred for 4 hours. After phase inversion, an emulsion with an average particle size of 267 nm was obtained. The emulsion had good stability, a contact angle of 6°, and a thermal residual rate of 99% at 300°C.

[0132] When this oil was applied to the preparation of T700 grade carbon fiber precursor, the resulting precursor was free of fuzz and had good film-forming effect. The carbon fiber obtained after pre-oxidation and carbonization treatment had a tensile strength of 4827 MPa and an ash content of 0.21%.

[0133] Comparative Example 2

[0134] Highly wettable and heat-resistant carbon fiber precursor oil, with the same mass fractions of each component as in Example 1.

[0135] The preparation steps of the silicone oil protectant are the same as in Example 1, wherein the R group in the silicone oil protectant is (a), R1 is a C1 alkyl group, and R2 is a C2 alkyl group.

[0136] The polyether esterification is the same as in Example 1.

[0137] The preparation process and performance testing of the oil are as follows:

[0138] The components, excluding deionized water, were mixed evenly in proportion, and then deionized water was added and stirred for 4 hours. After phase inversion, an emulsion with an average particle size of 187 nm was obtained. The emulsion exhibited excellent stability, a contact angle of 21°, and a thermal residual rate of 96% at 300°C.

[0139] When this oil agent is applied to the preparation of T700 grade carbon fiber precursor, the resulting precursor is free of fuzz and has good film-forming effect. The carbon fiber obtained after pre-oxidation and carbonization treatment has a tensile strength of 4728 MPa and an ash content of 0.19%.

[0140] Comparative Example 3

[0141] Highly wettable and heat-resistant carbon fiber precursor oil, with the same mass fractions of each component as in Example 1.

[0142] The preparation steps of the silicone oil protectant are the same as in Example 1, wherein the R group in the silicone oil protectant is (a), R1 is a C3 alkyl group, and R2 is a C6 alkyl group.

[0143] The polyether esterification is the same as in Example 1.

[0144] The preparation process and performance testing of the oil are as follows:

[0145] The components, excluding deionized water, were mixed evenly in proportion, and then deionized water was added and stirred for 4 hours. After phase inversion, an emulsion with an average particle size of 184 nm was obtained. The emulsion has excellent stability, a contact angle of 19°, and a thermal residual rate of 97% at 300°C.

[0146] When this oil agent is applied to the preparation of T700 grade carbon fiber precursor, the resulting precursor is free of fuzz and has good film-forming effect. After pre-oxidation and carbonization treatment, the carbon fiber obtained has a tensile strength of 4785 MPa and an ash content of 0.18%.

[0147] In summary, this invention synthesizes a highly wettable and heat-resistant carbon fiber precursor oil, which is composed of silicone oil protectant, polyether ester, emulsifier, antistatic agent, and defoamer.

[0148] Data from Example 1 shows that the carbon fiber precursor oiling agent of the present invention has excellent performance, protecting the fiber and improving its properties. Comparison of data from Examples 1-3 shows that changing the ratio of silicone oil protectant to polyether esters affects fiber performance; more silicone oil protectant results in better wettability and higher heat resistance, but also higher ash content. Comparison of data from Example 1 and Comparative Example 1 shows that polyether esters can improve the emulsification effect of the oiling agent. Comparison of data from Examples 4-5 shows that changing R3 and R4 in group (b) of the silicone oil protectant has no significant effect on fiber performance. Comparison of data from Examples 6-7 shows that changing m and R5 in the polyether ester has no significant effect on oiling agent performance. Comparison of data from Example 1 and Comparative Examples 2-3 shows that replacing the R group in the silicone oil protectant with (a) reduces fiber performance and increases ash content. The present invention proposes a high-wetting and heat-resistant carbon fiber precursor oiling agent, which is of great significance for improving oiling agent wettability, heat resistance, reducing ash content, and enhancing carbon fiber performance.

Claims

1. A carbon fiber precursor oiling agent, characterized in that, By weight, the components include: 10-30 parts of silicone oil protectant; 10-30 parts of polyether esters; 1-5 parts emulsifier; 1-5 parts of antistatic agent; 1-5 parts of defoamer; 60-80 parts deionized water; The structural formula of the silicone oil protective agent is: ; Where a is an integer from 5 to 50, b is an integer from 5 to 50, c is an integer from 20 to 200, d is an integer from 5 to 50, and R is... R3 and R4 are selected from C1 to C2 respectively. 10 Alkyl groups.

2. The carbon fiber precursor oiling agent according to claim 1, characterized in that, The molecular weight of the silicone oil protectant is 5000 to 30000.

3. The carbon fiber precursor oiling agent according to claim 1, characterized in that, The silicone oil protectant is obtained by mixing and reacting phenyl hydrogen-containing silicone oil, unsaturated alcohol ether, solvent, and catalyst; wherein the unsaturated alcohol ether is... R3 and R4 are selected from C1 to C2 respectively. 10 Alkyl groups.

4. The carbon fiber precursor oiling agent according to claim 3, characterized in that, The solvent includes one or more of toluene, isopropanol, dichloromethane, chloroform, methanol, acetone, acetonitrile, and dimethyl sulfoxide; the catalyst is chloroplatinic acid.

5. The carbon fiber precursor oiling agent according to claim 3, characterized in that, The preparation of the phenyl hydrogen-containing silicone oil includes: mixing octamethylcyclotetrasiloxane, benzene-containing siloxane, hydrogen-containing siloxane, end-capping agent and catalyst, reacting to obtain phenyl hydrogen-containing silicone oil; The benzene-containing siloxane is one or more of octaphenylcyclotetrasiloxane, hexaphenylcyclotrisiloxane, diphenyldimethoxysilane, and diphenyldiethoxysilane; the hydrogen-containing siloxane is one or more of tetramethylcyclotetrasiloxane, polymethylhydrosiloxane, pentamethylcyclopentasiloxane, heptamethyltrisiloxane, and octamethyltrisiloxane. The end-capping agent is one or more of hexamethyldisiloxane and tetramethyldisiloxane; the catalyst is concentrated sulfuric acid.

6. The carbon fiber precursor oiling agent according to claim 1, characterized in that, The structural formula of the polyether ester is: Where m is an integer from 1 to 10, and R5 is a integer from C2 to C5. 15 Alkyl groups.

7. The carbon fiber precursor oiling agent according to claim 1, characterized in that, The emulsifier includes one or more of nonylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, isomeric alcohol polyoxyethylene ether, polyvinyl alcohol, sodium dodecylbenzene sulfonate, and trihydroxymethane polyoxyethylene ether. The antistatic agent includes one or more of polyoxyethylene laurate, polyoxyethylene fatty alcohol phosphate, sorbitan fatty acid ester, dodecyltrimethylammonium chloride, and hexadecyltrimethyl quaternary ammonium sulfonate. The defoamer includes one or more of diisobutylmethanol, ethylene glycol monostearate, isoamyl alcohol, and trialkylmelamine; The average particle size of the raw silk oil is 150–300 nm.

8. A method for preparing the carbon fiber precursor oiling agent according to any one of claims 1 to 7, characterized in that, include: Weigh each component according to the mass fraction, mix the silicone oil protectant, polyether ester, emulsifier, antistatic agent, and defoamer, then add deionized water and reverse the phase to form an emulsion, thus obtaining the carbon fiber precursor oil.

9. The use of the carbon fiber precursor oiling agent according to any one of claims 1 to 7 in the preparation of polyacrylonitrile-based carbon fibers.

Citation Information

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