A highly stable antistatic crude oil-type spinning oil and its preparation method
By introducing alkyl-modified titanium carbide sheets and sodium dodecyl sulfate sulfonate into the spinning oil, a highly stable antistatic spinning oil is constructed, which solves the problems of anti-coking and interface adaptability of the spinning oil in high-speed spinning and high-temperature environments, and improves the antistatic property and production stability of the fiber.
Patent Information
- Application Number
- CN202510752926.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-06
- Publication Date
- 2025-09-09
- Estimated Expiration
- 2045-06-06
AI Technical Summary
Existing spinning oils have insufficient anti-coking properties under high-speed spinning and high-temperature environments, making it difficult to meet production needs. They are also not adaptable enough to the interface characteristics of different fibers, leading to problems such as fiber surface damage, breakage, and fiber breakage.
Alkyl-modified titanium carbide sheets are used as the core component of the antistatic agent, combined with sodium dodecyl sulfate and sodium dodecyl sulfonate to form a highly stable antistatic spinning oil. A conductive network is constructed through a two-dimensional sheet structure, reducing the use of phosphate antistatic agents and improving the antistatic and stability of the oil.
It significantly improves the antistatic performance and stability of spinning oil, reduces coking deposits, ensures fiber quality and production efficiency, reduces the amount of antistatic agent used, and adapts to the interface characteristics requirements of different fibers.
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of spinning oils, and in particular relates to a highly stable antistatic crude oil-type spinning oil and a preparation method thereof. Background Art
[0002] As the textile industry accelerates its move toward high-value-added, functionalized fields, fiber material systems are demonstrating unprecedented diversity and innovative vitality. A range of differentiated products, including regenerated cellulose fibers, ultrafine denier yarns, bio-based fibers, and high-performance synthetic fibers, are rapidly emerging. These new fibers, each with its own unique performance characteristics, have greatly enriched the variety and application of textile products. However, their emergence also places extremely stringent demands on spinning processing technology.
[0003] As a crucial core additive in the spinning process, spin finishes face significant challenges. First, they must exhibit excellent anti-coking properties in the high-temperature environments of high-speed spinning. High temperatures can cause oxidation and polymerization of certain components in the finish. Inadequate anti-coking properties can easily lead to the formation of coking deposits. These deposits not only dramatically increase local friction between the fiber and equipment components but, in severe cases, can damage the fiber surface, degrade fiber quality, and even cause production accidents such as breakage and yarn breakage, significantly impacting production efficiency and product quality. For example, in some high-speed spinning lines, poor anti-coking properties can lead to noticeable coking in key areas after just a few hours of operation, necessitating frequent downtime for cleaning and severely hindering production progress. Second, the formulation of spin finishes must be precisely tailored to the unique interfacial properties of different fibers. Due to the significant differences in chemical composition, surface morphology, and physical properties of different fibers, the finish must not only enhance antistatic properties but also optimize anti-splash performance.
[0004] Chinese patent document CN117845379B discloses a process for preparing a highly effective antistatic agent for chemical fiber oils. This method combines nitrogen-sulfur-doped MXene with an antistatic agent to produce a novel antistatic agent. The resulting chemical fiber oil exhibits an electrical conductivity of approximately 0.775–0.988 mS / cm. While the patent's introduction of MXene improves the oil's antistatic properties to a certain extent, the overall performance of the oil remains a far cry from a quantum leap. On the one hand, the patented technology lacks significant improvements and optimizations in anti-coking performance, failing to meet the stringent requirements for anti-coking in high-speed spinning environments. On the other hand, the patent also fails to provide a comprehensive and systematic solution for adapting to varying fiber interface characteristics, making it difficult to optimize anti-splash performance while ensuring tight bundle formation and preventing breakage and loosening during spinning.
[0005] In summary, there is still an urgent need for solutions that can improve the overall performance of spinning oils. Summary of the Invention
[0006] The purpose of the present invention is to provide a highly stable antistatic crude oil-type spinning oil and a preparation method thereof. The use of alkyl-modified titanium carbide as a core component can not only improve the antistatic properties of the highly stable antistatic crude oil-type spinning oil and reduce the total amount of antistatic components, but also the use of alkyl-modified titanium carbide can improve the stability of the antistatic performance of the spinning oil, thereby comprehensively improving the performance of the highly stable antistatic crude oil-type spinning oil.
[0007] To achieve the above objectives, the present technical solution provides a highly stable antistatic crude oil spinning oil, comprising: a smoothing agent, an emulsifier, an antistatic agent, a sizing agent and a wetting agent, wherein the antistatic agent comprises an alkyl-modified titanium carbide sheet.
[0008] In some embodiments, the antistatic agent additionally includes one or a combination of sodium lauryl sulfate and sodium lauryl sulfonate.
[0009] In some embodiments, the mass content of the antistatic agent is 6-8 wt %.
[0010] This proposal specifically selects alkyl-modified titanium carbide sheets as the core component of the antistatic agent. These alkyl-modified titanium carbide sheets are surface-alkylated titanium carbide sheets with a two-dimensional lamellar structure, a type of alkyl-terminated lamellar Mxene. As the core component of the spinning oil, these alkyl-modified titanium carbide sheets can effectively enhance the overall performance of the spinning oil, including its antistatic properties and stability.
[0011] Furthermore, the alkyl modified titanium carbide sheet of this scheme is Ti3C2T with octyltriethoxysilane on the surface. x The alkyl-modified titanium carbide sheet is modified with octyltriethoxysilane through a silane coupling agent to react with the hydroxyl groups on the surface of the titanium carbide sheet. The antistatic properties of the alkyl-modified titanium carbide sheet are further improved because the alkyl-modified titanium carbide sheet is modified with octyltriethoxysilane.
[0012] Specifically, the preparation method of the alkyl-modified titanium carbide sheet is as follows:
[0013] S1: preparing titanium carbide slurry;
[0014] LiF was added to the HCl solution and stirred thoroughly in an ice bath to obtain a mixed solution. Ti3AlC2 was slowly poured into the mixed solution and reacted at 35℃~40℃ for 12~48 h to obtain an acidic solution. The acidic solution was repeatedly centrifuged and washed with deionized water until the pH of the supernatant was about 6~6.5. Ti3C2T was peeled off by oscillation during the centrifugation process. x lamellae;
[0015] S2: Alkyl modified titanium carbide sheet:
[0016] The Ti3C2Tx layer was centrifuged with acetone to replace the water solvent and a dispersion was prepared. The dispersion was placed in an inert range and ultrasonicated to obtain a single layer of Ti3C2Tx. x Acetone suspension, to the monolayer Ti3C2T x Octyltriethoxysilane is added to the acetone suspension and stirred at room temperature for 6 to 96 hours. The unreacted octyltriethoxysilane is washed by centrifugation with acetone to obtain alkyl-modified titanium carbide sheets.
[0017] In some specific embodiments,
[0018] 1-2 parts of LiF were added to 1-2 parts of HCl solution and stirred thoroughly in an ice bath for 30 minutes to obtain a mixed solution. 0.05-0.5 parts of Ti3AlC2 were slowly poured into the mixed solution and reacted at 35°C-40°C for 12-48 hours to obtain an acidic solution. At this time, the Al layer was etched. The acidic solution was then repeatedly centrifuged and washed with deionized water until the pH of the supernatant was about 6-6.5. The Ti3C2Tx layer was peeled off by oscillation during the centrifugation process.
[0019] 0.5~5gTi3C2T x The sheet (40 wt.%) was centrifuged with acetone to replace the water solvent and prepare 20-30 mL of dispersion. The dispersion was placed in an inert range and ultrasonicated to obtain a single layer of Ti3C2T x Acetone suspension, to the monolayer Ti3C2T x 0.5-5 mL of octyltriethoxysilane is added to the acetone suspension and stirred at room temperature for 6-96 hours. The unreacted octyltriethoxysilane is washed by centrifugation with acetone to obtain alkyl-modified titanium carbide sheets.
[0020] This scheme uses alkyl modified titanium carbide sheets, which has many advantages:
[0021] On the one hand, the spinning oil has good anti-coking properties: traditional spinning oils often use phosphate antistatic agents (including octanol phosphate, octanol polyoxyethylene ether phosphate, and dodecyl phosphate mentioned in the nitrogen-sulfur-doped MXene antistatic agent mentioned in the background above). These agents are prone to forming coking deposits on the hot rollers in the spinning process, affecting the stability of the spinning process. This solution uses titanium carbide flakes as the core component of the antistatic agent component, and the other antistatic agents are selected from one or a combination of sodium lauryl sulfate and sodium lauryl sulfonate. It does not contain phosphate antistatic agents, thus avoiding the adverse effects of phosphate esters and improving the product quality rate.
[0022] On the other hand, the antistatic property of the spinning oil is greatly improved: since the alkyl-modified titanium carbide flakes have a two-dimensional layer structure, a continuous conductive network can be formed in the spinning oil. This structural characteristic greatly improves the overall conductivity of the spinning oil. High conductivity means that only a small amount of antistatic agent is needed to achieve the target antistatic property, thus significantly reducing the amount of antistatic agent used.
[0023] Furthermore, the antistatic stability of the spinning oil is greatly improved. Because the inherent polar functional groups (such as -OH) on the surface of the titanium carbide flakes reduce direct contact with ambient oxygen and moisture, inhibiting oxidative degradation, the material itself can extend the life of the antistatic agent. However, the nitrogen-sulfur-doped MXene mentioned in the background art is susceptible to oxidation or hydrolysis over long-term use due to exposed surface active sites. Furthermore, the alkyl chains further impart hydrophobicity to the titanium carbide flakes, reducing their hygroscopicity and thus making their conductivity primarily dependent on the titanium carbide flakes' inherent conductive network rather than ambient humidity, further stabilizing their antistatic properties. Furthermore, the alkyl chains protect the titanium carbide flakes' surface from oxidation and hydrolysis (especially in hot and humid environments), maintaining long-term conductivity and thus improving the chemical stability of the spinning oil. Furthermore, the MXene flakes are stably dispersed in the spinning oil and are not easily aggregated by mechanical shear or temperature fluctuations, ensuring the durability of the conductive network.
[0024] In some embodiments, the spinning oil contains 40-55 wt % of a smoothing agent, wherein the smoothing agent is white oil.
[0025] In some embodiments, the spinning oil contains 15-19 wt % of an emulsifier, and the emulsifier is one or a combination of isotridecanol polyoxyethylene ether and sorbitan fatty acid ester.
[0026] In some embodiments, the spinning oil further contains 10-15 wt % of a wetting agent, and the wetting agent is fatty alcohol polyoxyethylene ether.
[0027] In some embodiments, the spinning oil further contains 7-10 wt% of a sizing agent, which is a compound of polyethylene glycol 400 oleate and isotridecyl polyoxyethylene polyoxypropylene ether, specifically in a ratio of 3-5:1-1.5.
[0028] In some embodiments, the spinning oil further contains 3-5 wt % of an anti-coking agent, which is a double-terminated surfactant of the fatty acid methyl ester ethoxylate type.
[0029] In some embodiments, the water content in the spin finish does not exceed 4 wt %.
[0030] In some embodiments, the total weight of the components in the spin finish is 100 wt %.
[0031] In a second aspect, the present invention provides a method for preparing a highly stable antistatic crude oil-based spinning oil, comprising the following steps:
[0032] A smoothing agent, an emulsifier, an antistatic agent, a sizing agent, and a wetting agent are added to the reactor in sequence while stirring. The antistatic agent includes an alkyl-modified titanium carbide sheet. The reaction temperature is set at 55-65°C, the reaction speed is set at 400-600 r / min, and the reaction time is set at 30-40 min.
[0033] The same contents as above in the examples of the preparation method will not be repeated.
[0034] Compared with the existing technology, this technical solution has the following characteristics and beneficial effects:
[0035] (1) The highly stable antistatic crude oil-type spinning oil of the present invention uses alkyl-modified titanium carbide sheets as the core component of the antistatic agent, which can effectively avoid and reduce the problem of the common salt-containing phosphorus-based antistatic agent components being prone to coking at high temperatures.
[0036] (2) Alkyl-modified titanium carbide sheets as highly conductive sheet materials can significantly improve the conductive properties of spinning oils and effectively reduce the total amount of antistatic agent components.
[0037] (3) The antistatic agent used in the oil of the present invention can significantly improve the stability of the antistatic performance of the spinning oil, making its antistatic performance less susceptible to fluctuations due to environmental influences. DETAILED DESCRIPTION
[0038] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field are within the scope of protection of the present invention.
[0039] The following is the performance test method in each embodiment:
[0040] Conductivity (10% aqueous solution): Water was added to the oil prepared in the following examples, with water accounting for 10% of the total solution by mass, and the conductivity was measured according to GB / T11007.
[0041] Oil film strength: Use a four-ball friction tester to measure the oil film strength of the sample to be tested in accordance with GB / T 3142-1982 "Determination of load-bearing capacity of lubricants (four-ball method)".
[0042] Surface tension (1% aqueous solution): measured at 25°C using a QBZY platinum plate surface tension meter (QBZY-1, Shanghai Fangrui Instrument Co., Ltd.).
[0043] Fiber resistivity: measured using an automatic digital fiber resistivity meter in accordance with GB / T14342-2015.
[0044] Fiber friction coefficient: measured using LFY-110 yarn dynamic friction tester (LFY-110, Shandong Textile Science Research Institute).
[0045] Oil content: The oil content was determined using a fiber grease quick extractor (YG981, Changzhou Shuanggu Dunda Electromechanical Technology Co., Ltd.) in accordance with the national standard GB / T6504-2008.
[0046] The following are the manufacturers and brands of the raw materials involved in the examples:
[0047] Sodium dodecyl sulfate: The manufacturer is Aladdin Reagent (Shanghai) Co., Ltd., and the brand number is 151-21-3.
[0048] Sodium dodecyl sulfate: The manufacturer is Aladdin Reagent (Shanghai) Co., Ltd., and the brand number is 2386-53-0.
[0049] Alkyl-terminated lamellae Mxene: homemade.
[0050] White oil (liquid paraffin): manufacturer is Shanghai McLean Biochemical Technology Co., Ltd., brand number is 8042-47-5.
[0051] Polyethylene glycol 400 oleate: The manufacturer is Aladdin Reagent (Shanghai) Co., Ltd., and the brand number is 9004-96-0.
[0052] Isotridecyl polyoxyethylene ether: Manufacturer: Aladdin Reagent (Shanghai) Co., Ltd., brand number 61827-42-7;
[0053] Isotridecyl polyoxyethylene polyoxypropylene ether: Manufacturer: Guangdong Wengjiang Chemical Reagent Co., Ltd.; Trademark: 78330-23-1
[0054] Fatty alcohol polyoxyethylene ether: Manufacturer: Aladdin Reagent (Shanghai) Co., Ltd., brand: 68131-39-5
[0055] Sorbitan fatty acid ester: The manufacturer is Nantong Ningyuan New Material Technology Co., Ltd.
[0056] Fatty acid methyl ester ethoxylate-based double-end-capped surfactant: manufacturer is Aladdin Reagent (Shanghai) Co., Ltd., brand number 65218-33-7.
[0057] Example 1:
[0058] A method for preparing a highly stable antistatic crude oil-based spinning oil comprises the following specific steps:
[0059] (1) Preparation of raw materials;
[0060] Antistatic agent: a mixture of alkyl-terminated flakes of Mxene, sodium lauryl sulfate, and sodium lauryl sulfonate in a mass ratio of 1:1:1;
[0061] Smoothing agent: white oil;
[0062] Emulsifier: polyoxyethylene isotridecanol ether;
[0063] Wetting agent: fatty alcohol polyoxyethylene ether;
[0064] Anti-coking agent: fatty acid methyl ester ethoxylate type double-end-capped surfactant;
[0065] water;
[0066] (2) Prepare the clustering agent;
[0067] Prepare a sizing agent by mixing polyethylene glycol 400 oleate and isotridecyl polyoxyethylene polyoxypropylene ether in a mass ratio of 3:1;
[0068] (3) Weigh 7 wt% of antistatic agent, 50 wt% of smoothing agent, 17 wt% of emulsifier, 12 wt% of wetting agent, 8 wt% of agglomerating agent, 4 wt% of anti-coking agent and 2 wt% of water in proportion, then add smoothing agent, emulsifier, antistatic agent, agglomerating agent, wetting agent and water in sequence while stirring; then react at a temperature of 60 ° C and a stirring speed of 550 r / min for 35 min to obtain a high-performance spinning oil.
[0069] The high-performance spinning oil finally prepared was yellow and transparent, with a conductivity of 1279μS / cm, an oil film strength of 1048.6N, and a surface tension of 32.38 mN / m.
[0070] During the spinning process, there is minimal oil splashing and almost no coking deposits.
[0071] The final polyester FDY fiber has a fiber specification of 70dtex / 48f and a fiber resistivity of 8.9×10 6 Ω.cm, the fiber friction coefficient is 0.3785, and the oil content is 0.67%.
[0072] Comparative Example 1:
[0073] A method for preparing a highly stable antistatic crude oil-based spinning oil is basically the same as that in Example 1, except that the antistatic agent is sodium lauryl sulfate.
[0074] The high-performance spinning oil finally prepared was yellow and transparent, with a conductivity of 717.3 μS / cm, an oil film strength of 862.4 N, and a surface tension of 33.79 mN / m.
[0075] During the spinning process, there is less oil splashing and less coking deposits.
[0076] The final polyester FDY fiber has a fiber specification of 68dtex / 48f and a fiber resistivity of 8.4×10 7 Ω.cm, the fiber friction coefficient is 0.4017, and the oil content is 0.47%.
[0077] Comparative Example 2:
[0078] A method for preparing a highly stable antistatic crude oil-based spinning oil is basically the same as that of Comparative Example 1, except that the antistatic agent is sodium lauryl sulfate and sodium lauryl sulfonate.
[0079] The high-performance spinning oil finally prepared was yellow and transparent, with a conductivity of 745.2μS / cm, an oil film strength of 803.6N, and a surface tension of 33.41 mN / m.
[0080] During the spinning process, there is less oil splashing and less coking deposits.
[0081] The final polyester FDY fiber has a fiber specification of 68dtex / 48f and a fiber resistivity of 6.9×10 7 Ω.cm, the fiber friction coefficient is 0.4002, and the oil content is 0.48%.
[0082] Comparative Example 3:
[0083] A method for preparing a highly stable antistatic crude oil-based spinning oil is basically the same as that of Comparative Example 1, except that the antistatic agent is sodium dodecyl sulfate.
[0084] The high-performance spinning oil finally prepared was yellow and transparent, with a conductivity of 807.3 μS / cm, an oil film strength of 921.2 N, and a surface tension of 33.71 mN / m.
[0085] During the spinning process, there is less oil splashing and less coking deposits.
[0086] The final polyester FDY fiber has a fiber specification of 68dtex / 48f and a fiber resistivity of 5.1×10 7 Ω.cm, the fiber friction coefficient is 0.3912, and the oil content is 0.58%.
[0087] Example 2:
[0088] A method for preparing a highly stable antistatic crude oil-based spinning oil comprises the following specific steps:
[0089] (1) Preparation of raw materials;
[0090] Antistatic agent: a mixture of alkyl-terminated flake Mxene and sodium lauryl sulfate in a mass ratio of 1:1;
[0091] Smoothing agent: white oil;
[0092] Emulsifier: sorbitan fatty acid ester;
[0093] Wetting agent: fatty alcohol polyoxyethylene ether;
[0094] Anti-coking agent: fatty acid methyl ester ethoxylate type double-end-capped surfactant;
[0095] water;
[0096] (2) Prepare the clustering agent;
[0097] Prepare a sizing agent by mixing polyethylene glycol 400 oleate and isotridecyl polyoxyethylene polyoxypropylene ether in a mass ratio of 5:1.5;
[0098] (3) 6 wt% of antistatic agent, 55 wt% of smoothing agent, 15 wt% of emulsifier, 10 wt% of wetting agent, 7 wt% of agglomerating agent, 3 wt% of anti-coking agent, and 4 wt% of water were weighed in proportion. Then, smoothing agent, emulsifier, antistatic agent, agglomerating agent, wetting agent, and water were added in sequence while stirring. The mixture was then reacted at a temperature of 55°C and a stirring speed of 400 r / min for 30 min to obtain a high-performance spinning oil. The high-performance spinning oil obtained was yellow and transparent, with a conductivity of 1123.7 μS / cm, an oil film strength of 921.2 N, and a surface tension of 32.54 mN / m.
[0099] During the spinning process, there is no oil splashing and no coking deposits.
[0100] The final polyester FDY fiber has a fiber specification of 69dtex / 48f and a fiber resistivity of 3.5×10 7 Ω.cm, the fiber friction coefficient is 0.3882, and the oil content is 0.64%.
[0101] Example 3:
[0102] A method for preparing a highly stable antistatic crude oil-based spinning oil comprises the following specific steps:
[0103] (1) Preparation of raw materials;
[0104] Antistatic agent: a mixture of alkyl-terminated flakes of Mxene and sodium dodecylsulfonate in a mass ratio of 1:1;
[0105] Smoothing agent: white oil;
[0106] Emulsifier: a mixture of isotridecanol polyoxyethylene ether and sorbitan fatty acid ester in a mass ratio of 1:1;
[0107] Wetting agent: fatty alcohol polyoxyethylene ether;
[0108] Anti-coking agent: fatty acid methyl ester ethoxylate type double-end-capped surfactant;
[0109] water;
[0110] (2) Prepare the clustering agent;
[0111] Prepare a sizing agent by mixing polyethylene glycol 400 oleate and isotridecyl polyoxyethylene polyoxypropylene ether in a mass ratio of 4:1.25;
[0112] (3) 8 wt% of antistatic agent, 40 wt% of smoothing agent, 19 wt% of emulsifier, 15 wt% of wetting agent, 10 wt% of agglomerating agent, 5 wt% of anti-coking agent, and 3 wt% of water were weighed in proportion. Then, smoothing agent, emulsifier, antistatic agent, agglomerating agent, wetting agent, and water were added in sequence while stirring. The mixture was then reacted at a temperature of 65°C and a stirring speed of 600 r / min for 40 min to obtain a high-performance spinning oil. The high-performance spinning oil obtained was yellow and transparent, with a conductivity of 1069.1 μS / cm, an oil film strength of 980 N, and a surface tension of 32.76 mN / m.
[0113] During the spinning process, there is no oil splashing and no coking deposits.
[0114] The final polyester FDY fiber has a fiber specification of 70dtex / 48f and a fiber resistivity of 4.7×107 Ω.cm, the fiber friction coefficient is 0.368, and the oil content is 0.51%.
[0115] The above-described embodiments are only used to illustrate the present invention and are not used to limit the scope of the present invention. In addition, it should be understood that after reading the contents taught by the present invention, those skilled in the art may make various changes or modifications to the present invention, and these equivalent forms belong to the scope of protection of the present invention.
[0116] Those skilled in the art should understand that the technical features of the above embodiments can be combined arbitrarily. In order to make the description concise, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.
[0117] The above embodiments merely illustrate several embodiments of the present application. While the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the present application. It should be noted that a person of ordinary skill in the art may make various modifications and improvements without departing from the spirit of the present application, all of which fall within the scope of protection of the present application. Therefore, the scope of protection of the present application shall be determined by the appended claims.
Claims
1. A highly stable antistatic crude oil-based spinning oil, characterized in that: include: Smoothing agent, emulsifier, antistatic agent, sizing agent and wetting agent, the mass content of antistatic agent is 6~8wt%, wherein the antistatic agent includes alkyl modified titanium carbide sheet, wherein the alkyl modified titanium carbide sheet is Ti3C2T with octyltriethoxysilane on the surface x The alkyl-modified titanium carbide sheet has a two-dimensional sheet structure, wherein octyltriethoxysilane reacts with hydroxyl groups on the surface of the titanium carbide sheet through a silane coupling agent; The preparation method of the alkyl-modified titanium carbide flakes is as follows: Ti3C2Tx flakes are centrifuged to replace the water solvent with acetone and prepared to obtain a dispersion, the dispersion is placed in an inert range and ultrasonically obtained to obtain an acetone suspension of a single-layer Ti3C2Tx, octyltriethoxysilane is added to the acetone suspension of the single-layer Ti3C2Tx and stirred at room temperature for 6 to 96 hours, and the unreacted octyltriethoxysilane is washed by centrifugation with acetone to obtain the alkyl-modified titanium carbide flakes.
2. The highly stable antistatic crude oil-based spinning oil according to claim 1, characterized in that: Antistatic agents additionally include one or a combination of sodium lauryl sulfate and sodium lauryl sulfonate.
3. The highly stable antistatic crude oil-based spinning oil according to claim 1, characterized in that: The mass content of the antistatic agent is 6~8wt%.
4. The highly stable antistatic crude oil-based spinning oil according to claim 1, characterized in that: The preparation method of alkyl modified titanium carbide sheet is as follows: S1: preparing titanium carbide slurry; LiF was added to HCl solution and stirred thoroughly in an ice bath to obtain a mixed solution. Ti3AlC2 was slowly poured into the mixed solution and reacted at 35℃~40℃ for 12~48 h to obtain an acidic solution. The acidic solution was repeatedly centrifuged and washed with deionized water until the pH of the supernatant was 6~6.
5. Ti3C2T was peeled off by oscillation during the centrifugation process. x lamellae; S2: Alkyl modified titanium carbide sheet: The Ti3C2Tx layer was centrifuged with acetone to replace the water solvent and a dispersion was prepared. The dispersion was placed in an inert range and ultrasonicated to obtain a single layer of Ti3C2Tx. x Acetone suspension, to the monolayer Ti3C2T x Octyltriethoxysilane is added to the acetone suspension and stirred at room temperature for 6 to 96 hours. The unreacted octyltriethoxysilane is washed by centrifugation with acetone to obtain alkyl-modified titanium carbide sheets.
5. The highly stable antistatic crude oil-based spinning oil according to claim 1, characterized in that: The spinning oil contains 40~55wt% of smoothing agent, 15~19wt% of emulsifier, 10~15wt% of wetting agent and 7~10wt% of sizing agent.
6. The highly stable antistatic crude oil-based spinning oil according to claim 1, characterized in that: The water content in the spinning oil does not exceed 4wt%.
7. The highly stable antistatic crude oil-based spinning oil according to claim 1, characterized in that: The lubricant is white oil, the emulsifier is one or a combination of isotridecanol polyoxyethylene ether and sorbitan fatty acid ester, the wetting agent is fatty alcohol polyoxyethylene ether, and the sizing agent is a compound of polyethylene glycol 400 oleate and isotridecanol polyoxyethylene polyoxypropylene ether.
8. The highly stable antistatic crude oil-based spinning oil according to claim 1, characterized in that: The spinning oil also contains 10-15wt% of a wetting agent, which is fatty alcohol polyoxyethylene ether.
9. A method for preparing the highly stable antistatic crude oil-based spinning oil according to any one of claims 1 to 8, characterized in that: The following steps are involved: In the reaction kettle, a smoothing agent, an emulsifier, an antistatic agent, a sizing agent, and a wetting agent are added in sequence while stirring. The antistatic agent includes an alkyl-modified titanium carbide sheet. The reaction temperature is set at 55-65°C and the reaction speed is 400-600 r / min. The reaction time is 30-40 min. The alkyl-modified titanium carbide sheet is Ti3C2T with octyltriethoxysilane on the surface. x The octyl triethoxysilane reacts with the hydroxyl group on the surface of the titanium carbide layer through a silane coupling agent, and the alkyl modified titanium carbide layer has a two-dimensional layer structure.
Citation Information
Patent Citations
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