FDY crude oil type oil agent for high-gloss polyester fiber and preparation method thereof

Abstract

The present invention provides a FDY crude oil type oil agent for large shiny polyester fiber and a preparation method thereof, the preparation method comprising: putting a sizing agent, an antistatic agent, an emulsifier, a solid lubricant and a smoothing agent into a reactor, continuously stirring under heat preservation conditions, and obtaining a FDY crude oil type oil agent; wherein the solid lubricant is prepared by the following steps: in a buffer solution containing dopamine, graphite is intercalated by an intercalation agent to obtain modified graphite; raw materials including acrylic acid monomers, 1,3,6,8-tetrakis(4-methylphenyl)pyrene and 4'-aminodibenzo-18-crown-6 are used to prepare organic matter including crown ethers, and modified graphite is coated by organic matter to obtain a solid lubricant. The solid lubricant of the present invention can be uniformly and stably dispersed in the FDY crude oil type oil agent, and the friction coefficient of the FDY crude oil type oil agent can be reduced, and its heat resistance and storage stability can be improved.

Description

Technical Field

[0001] The invention relates to the technical field of textile auxiliaries, and in particular to an FDY crude oil type oil agent for high-gloss polyester fiber and a preparation method thereof. Background Art

[0002] Bright polyester fiber is a polyester spun from polyester chips with a titanium dioxide content of less than or equal to 0.1%, and is one of the important varieties of polyester. Bright polyester fiber has good gloss under light. Due to its good gloss and softness, it is often used to make high-end clothing, silk beds, curtains, sofa covers and other home decorations, adding comfort and texture to the home environment.

[0003] In the spinning process of bright polyester fiber, FDY (Fully Drawn Yarn) crude oil is needed. FDY crude oil can reduce the lint and broken ends in the high-speed spinning process, reduce the cost of the spinning process, save energy and improve product quality.

[0004] The main components of FDY crude oil type oil include sizing agent, antistatic agent, emulsifier, smoothing agent and water. Its function is to adjust the friction between fibers and fibers, fibers and metals, improve the smoothness of the fiber surface and reduce the charge of the fibers; on the other hand, it increases the number of ions on the fiber surface, improves hygroscopicity, and allows the generated static electricity to dissipate quickly.

[0005] The FDY crude oil type oil in the prior art has the following deficiencies: first, the heat resistance of the FDY crude oil type oil is not ideal, and the coking phenomenon is relatively serious, which easily leads to problems of lint and broken ends; second, the storage stability of the FDY crude oil type oil is not ideal, and it is easy to deteriorate, resulting in uneven oiling.

[0006] Inorganic fillers including silicon dioxide, calcium carbonate, zinc oxide, aluminum oxide, graphite, etc. can all be added to FDY crude oil type oil. These materials can be used to improve the thermal stability of FDY crude oil type oil. For example, the Chinese patent with the authorization announcement number CN116556056B proposes an oil containing graphite solid lubricant, which reduces the friction coefficient of the fiber and increases the smoothness of the polyester oil by adding flake graphite as a solid lubricant. At the same time, graphite can also increase the thermal stability and antistatic properties of the polyester oil. Although graphite materials can improve the heat resistance of FDY crude oil type oil, because graphite materials are difficult to be evenly dispersed in the oil system, and are easily agglomerated, the oil added with graphite materials is easily stratified and deteriorated, affecting the storage stability of FDY crude oil type oil. Summary of the invention

[0007] One of the problems solved by the present invention is how to provide an FDY crude oil type oil agent for high gloss polyester fiber with good lubricity, heat resistance and storage stability.

[0008] In order to solve at least one of the above problems, the present invention provides a method for preparing an FDY crude oil type oil agent for high-gloss polyester fiber, the preparation method comprising:

[0009] S100, according to the mass ratio of sizing agent: antistatic agent: emulsifier: solid lubricant: smoothing agent = (4-8): (6-12): (20-25): (10-25): (50-80), add sizing agent, antistatic agent, emulsifier, solid lubricant and smoothing agent into the first reaction kettle;

[0010] S200, raising the temperature of the first reactor to 40° C. to 60° C., turning on the stirring device of the first reactor, and continuously stirring for 20 min to 40 min under the heat preservation condition to obtain FDY crude oil type oil agent;

[0011] Wherein, the solid lubricant is prepared by the following steps:

[0012] S310, in a buffer solution containing dopamine, using an intercalation agent to intercalate graphite to obtain modified graphite;

[0013] S320, using raw materials including acrylic acid monomer, 1,3,6,8-tetrakis(4-methylphenyl)pyrene and 4'-aminodibenzo-18-crown-6 to prepare organic matter including crown ether, and using the organic matter to coat modified graphite to obtain a solid lubricant.

[0014] In any of the above technical solutions, S310 specifically includes:

[0015] S311, mixing dopamine, intercalating agent, and graphite in a phosphate buffer solution at a mass ratio of dopamine: intercalating agent: graphite: phosphate buffer solution = (5-10): (5-10): (20-30): 100, and performing intercalation treatment by an ultrasonic dispersion device;

[0016] S312. After the intercalation treatment is completed, the solid matter is extracted, washed, and dried to obtain modified graphite.

[0017] In any of the above technical solutions, in S311, the pH value of the phosphate buffer solution is 7.5-8.5; in S311, the ultrasonic frequency used in the intercalation treatment is 60kHz to 80kHz; in S311, the ultrasonic time used in the intercalation treatment is 30min to 1h.

[0018] In any of the above technical solutions, the intercalant is prepared by the following steps:

[0019] S410, mixing petroleum ether and n-dodecyl alcohol in a saturated sodium chloride solution to obtain a first mixture;

[0020] S420, according to the amount of n-dodecanol added in S410, adding a corresponding amount of poly(dibenzo-18-crown-6) to the first mixture and mixing them evenly to obtain a second mixture;

[0021] S430, heating the second mixture to reflux, adding concentrated sulfuric acid dropwise with simultaneous stirring, and continuing to stir the reaction for 4 to 6 hours after the addition is complete;

[0022] S440, after the reaction is completed, cooling to room temperature, alkali washing, drying, and distilling at normal pressure to obtain a reaction product;

[0023] S450, sending the reaction product into a second reaction kettle, heating it to 90° C. to 100° C. under vacuum, continuously introducing gaseous trimethylamine into the second reaction kettle for reaction, and controlling the pressure in the second reaction kettle to be 3 MPa to 4 MPa;

[0024] S460, after the reaction is completed, the second reactor is cooled and depressurized, and allowed to stand for 8 to 10 hours, and the solids in the second reactor are extracted to obtain an intercalation agent.

[0025] In any of the above technical solutions, in S410, the volume ratio of petroleum ether: n-dodecanol: saturated sodium chloride solution is (40-60): (40-60): 100; in S420, the mass ratio of poly(dibenzo-18-crown-6): n-dodecanol is (0.02-0.04): 1; in S430, concentrated sulfuric acid with an equal volume to the saturated sodium chloride solution and a concentration of 85% to 95% is added dropwise; in S450, the mass ratio of trimethylamine: reaction product is (30-35): 100.

[0026] In any of the above technical solutions, S320 specifically includes:

[0027] S321, mixing acetic acid, 1,3,6,8-tetrakis(4-methylphenyl)pyrene and 4'-aminodibenzo-18-crown-6 in o-dichlorobenzene whose mass is 8 to 10 times that of 4'-aminodibenzo-18-crown-6, stirring for 1 to 2 hours and then degassing to obtain a third mixture;

[0028] S322, feeding the acrylic acid monomer, modified graphite and the third mixture into a third reaction kettle for closed reaction;

[0029] S323. After the closed reaction is completed, the solid matter is extracted, washed, and dried to obtain a solid lubricant.

[0030] In any of the above technical solutions, in S321, the molar ratio of acetic acid: 1,3,6,8-tetrakis(4-methylphenyl)pyrene: 4'-aminodibenzo-18-crown-6 = (2-4): (45-55): 100.

[0031] In any of the above technical solutions, in S322, the mass ratio of acrylic monomer: modified graphite: third mixture is (5-10): (20-30): 100.

[0032] In any of the above technical solutions, in S323, the temperature condition of the closed reaction is 90°C to 100°C, and the time of the closed reaction is 60h to 70h.

[0033] The present invention also provides an FDY crude oil type oil agent for highly shiny polyester fibers. The FDY crude oil type oil agent for highly shiny polyester fibers is obtained by adopting the preparation method of any of the above technical solutions.

[0034] Beneficial Effects

[0035] The present invention provides a method for preparing a FDY crude oil type oil agent, which is mainly used in polyester production. As an indispensable auxiliary agent in the polyester spinning process, the FDY crude oil type oil agent can make the fiber have good smoothness, bundling and antistatic properties, thereby meeting the requirements of fiber processing. The preparation method of the present invention first puts a bundling agent, an antistatic agent, an emulsifier, a solid lubricant and a smoothing agent into a reactor, and then heats the reactor and continuously stirs, thereby obtaining a FDY crude oil type oil agent. Among them, the preparation method of the solid lubricant used in the present invention is: first, in a buffer solution containing dopamine, an intercalation agent is used to intercalate graphite, and then an organic matter including crown ether is used to coat the graphite, thereby obtaining a solid lubricant. Graphite has good lubrication performance and thermal stability, and can be used as a solid lubricant. Its application in the FDY crude oil type oil agent can reduce the friction coefficient of the FDY crude oil type oil agent and improve its heat resistance. Considering that graphite is an inorganic powder with high surface energy, its dispersibility in liquid phase oil is not ideal, for this reason, the present invention adopts intercalation agent and dopamine to modify graphite. Dopamine can improve the hydrophilicity of graphite, and intercalation agent can make graphite overcome interlayer adhesion, increase the interlayer distance of graphite and peel off stratification, thereby improving the dispersion stability and uniformity of graphite in liquid phase. Therefore, the graphite solid lubricant modified by intercalation agent and dopamine can be uniformly and stably dispersed in the oil, so that the FDY crude oil type oil of the present invention is not easy to be stratified and deteriorated. In addition, crown ethers or organic matter containing crown ether groups can not only improve the wetting ability of graphite, but also help graphite to be better compatible with the FDY oil system mainly composed of polyester or polyether compounds. The use of crown ether organic matter to coat graphite can further reduce the surface energy of graphite, and improve its compatibility and binding ability with other organic matter in the oil, especially between macromolecular polymers, to further improve the storage stability of FDY crude oil. Therefore, the solid lubricant of the present invention can be uniformly and stably dispersed in the FDY crude oil type oil, and can ensure that the FDY crude oil type oil has good heat resistance and storage stability. DETAILED DESCRIPTION

[0036] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the following is a detailed description of the specific embodiments of the present invention.

[0037] Unless otherwise specified, the reagents and raw materials used in the present invention can be purchased through commercial channels. The experimental methods in the following examples without specifying specific conditions are selected according to conventional methods and conditions, or according to the product specifications.

[0038] FDY crude oil type oil is mainly used in polyester production. It is an indispensable auxiliary agent in the polyester spinning process to ensure that the polyester fiber has good smoothness, bundling and antistatic properties. Because polyester spinning speed is fast and the spinning temperature is high, FDY crude oil type oil must have good heat resistance. In addition, it is also necessary to give the appropriate friction coefficient between fibers and between fibers and other components through FDY crude oil type oil. Finally, FDY crude oil type oil will lead to uneven oiling after deterioration, so whether FDY crude oil type oil can be stored for a long time is also one of the important criteria for measuring its quality.

[0039] The invention provides an FDY crude oil type oil agent using graphite as a solid lubricant, utilizing the good lubrication performance and thermal stability of graphite to reduce the friction coefficient of the fiber and improve the lubrication performance and thermal stability of the FDY crude oil type oil agent.

[0040] Since graphite has great differences in physical and chemical properties from commonly used raw materials such as sizing agents, antistatic agents, and lubricants, powdered graphite is not stable in the FDY crude oil system. If the particle size is too small, it is easy to agglomerate, and if the particle size is too large, it is easy to stratify. During long-term storage, the addition of graphite will also affect the storage stability of the oil.

[0041] The premise of using graphite as a solid lubricant is that its dispersion stability problem needs to be solved. Therefore, how to modify graphite in a suitable manner to improve the storage stability and thermal stability of FDY crude oil type oil is a technical problem that the following technical solution is dedicated to solving.

[0042] The embodiment of the present invention provides a method for preparing an FDY crude oil type oil agent for high-gloss polyester fiber, the preparation method comprising:

[0043] S100, according to the mass ratio of sizing agent: antistatic agent: emulsifier: solid lubricant: smoothing agent = (4-8): (6-12): (20-25): (10-25): (50-80), add sizing agent, antistatic agent, emulsifier, solid lubricant and smoothing agent into the first reaction kettle;

[0044] S200, raising the temperature of the first reactor to 40° C. to 60° C., turning on the stirring device of the first reactor, and continuously stirring for 20 min to 40 min under the heat preservation condition to obtain FDY crude oil type oil agent.

[0045] The purpose of the above steps is to prepare FDY crude oil type oil by uniformly mixing the raw materials. In order to achieve uniform mixing, the raw materials are fed into a reactor and stirred for a certain period of time under the condition of heating. Among them, the present invention uses graphite as a solid lubricant, and the solid lubricant is added after modification. The present invention improves the preparation process of the solid lubricant so that the solid lubricant is uniformly and stably dispersed in the FDY crude oil type oil, thereby improving the lubrication performance, thermal stability and storage stability of the FDY crude oil type oil.

[0046] Before introducing the modification process of the solid lubricant, other raw materials used in the preparation process of the FDY crude oil type oil are first explained. In the FDY crude oil type oil of the present invention, the sizing agent is a chemical auxiliary agent used in the fiber material processing process, and its main function is to improve the cohesion between fibers, so that the fibers can be bundled into bundles, thereby increasing the load-bearing capacity and tensile strength of the fibers. Exemplarily, the sizing agent used in the present invention includes at least one of lauroyl diethanolamine, coconut oil diethanolamide, oleic acid triethanolamine, polyethylene glycol oleate, and polyethylene glycol laurate.

[0047] An antistatic agent is a chemical substance that can increase the conductivity of the surface of an object and prevent static electricity accumulation. Its main function is to increase the conductivity of the material surface so that static charge can be leaked in time to avoid static electricity from affecting production. Exemplarily, the antistatic agent used in the present invention includes at least one of lauryl alcohol polyoxyethylene ether potassium phosphate, secondary alkyl sodium sulfonate, and lauryl alcohol polyoxyethylene ether.

[0048] An emulsifier is a surfactant that contains both a hydrophilic group and a lipophilic group in its molecule. Its main function is to reduce the interfacial tension of the components in the mixed system, form a relatively strong film or double electric layer on the surface of the droplets, prevent the droplets from aggregating with each other, and thus maintain a uniform emulsion. Exemplarily, the emulsifier used in the present invention includes at least one of isomeric alcohol polyoxyethylene ether, anhydrous sorbitan fatty acid ester, polyethylene glycol fatty acid ester, castor oil polyoxyethylene ether, cardanol polyoxyethylene ether, and sodium lauryl alcohol ether sulfate.

[0049] The smoothing agent can significantly improve the smoothness of the tow, making the surface of the tow smoother and more delicate, and also helps to reduce the friction coefficient between the tows, thereby reducing the entanglement and knotting of the tows during the production process. Exemplarily, the smoothing agent used in the present invention includes at least one of mineral oil, white oil, vegetable oil, silicone oil, and at least one of fatty alcohol oleate or polyol oleate.

[0050] It should be noted that those skilled in the art are capable of selecting and adjusting the specific raw materials and component contents of the sizing agent, antistatic agent, emulsifier and lubricant according to actual needs. The selection of the above raw materials and components in the present invention is a preferred solution adapted to the anti-wear agent preparation process of the present invention. The solid lubricant preparation process of the present invention will be described below.

[0051] The solid lubricant used in the present invention is prepared by the following steps:

[0052] S310, in a buffer solution containing dopamine, using an intercalation agent to intercalate graphite to obtain modified graphite;

[0053] S320, using raw materials including acrylic acid monomer, 1,3,6,8-tetrakis(4-methylphenyl)pyrene and 4'-aminodibenzo-18-crown-6 to prepare organic matter including crown ether, and using the organic matter to coat modified graphite to obtain a solid lubricant.

[0054] It can be understood that the purpose of treating graphite with dopamine is to improve its hydrophilicity, and the purpose of treating graphite with an intercalating agent is to increase the interlayer spacing of graphite and exfoliate the layers, thereby improving the dispersion stability and uniformity of graphite in the liquid phase.

[0055] In some implementations of the present invention, S310 specifically includes:

[0056] S311, mixing dopamine, intercalating agent, and graphite in a phosphate buffer solution at a mass ratio of dopamine: intercalating agent: graphite: phosphate buffer solution = (5-10): (5-10): (20-30): 100, and performing intercalation treatment by an ultrasonic dispersion device;

[0057] S312. After the intercalation treatment is completed, the solid matter is extracted, washed, and dried to obtain modified graphite.

[0058] Preferably, in S311, the pH value of the phosphate buffer solution is 7.5-8.5. The phosphate buffer solution of the present invention is prepared by dissolving sodium dihydrogen phosphate and disodium hydrogen phosphate in deionized water.

[0059] Preferably, in S311, the ultrasonic frequency used in the intercalation treatment is 60 kHz to 80 kHz.

[0060] Preferably, in S311, the ultrasonic time used in the intercalation treatment is 30 min to 1 h.

[0061] Specifically, the intercalant of the present invention is prepared by the following steps:

[0062] S410, mixing petroleum ether and n-dodecyl alcohol in a saturated sodium chloride solution to obtain a first mixture;

[0063] S420, according to the amount of n-dodecanol added in S410, adding a corresponding amount of poly(dibenzo-18-crown-6) to the first mixture and mixing them evenly to obtain a second mixture;

[0064] S430, heating the second mixture to reflux, adding concentrated sulfuric acid dropwise with simultaneous stirring, and continuing to stir the reaction for 4 to 6 hours after the addition is complete;

[0065] S440, after the reaction is completed, cooling to room temperature, alkali washing, drying, and distilling at normal pressure to obtain a reaction product;

[0066] S450, sending the reaction product into a second reaction kettle, heating it to 90° C. to 100° C. under vacuum, continuously introducing gaseous trimethylamine into the second reaction kettle for reaction, and controlling the pressure in the second reaction kettle to be 3 MPa to 4 MPa;

[0067] S460, after the reaction is completed, the second reactor is cooled and depressurized, and allowed to stand for 8 to 10 hours, and the solids in the second reactor are extracted to obtain an intercalation agent.

[0068] Preferably, in S410, the volume ratio of petroleum ether: n-dodecyl alcohol: saturated sodium chloride solution is (40-60): (40-60): 100.

[0069] Preferably, in S420, the mass ratio of poly(dibenzo-18-crown-6):n-dodecanol=(0.02-0.04):1.

[0070] Preferably, in S430, concentrated sulfuric acid having an equal volume to that of the saturated sodium chloride solution and a concentration of 85% to 95% is added dropwise.

[0071] Preferably, in S450, the mass ratio is trimethylamine:reaction product = (30-35): 100. The above reaction product is specifically chlorododecane.

[0072] Trimethylamine, as a nucleophilic reagent, can attack the chlorine atom in chlorododecane to form a chloride ion and a chlorododecyl trimethylamine intermediate. The chlorododecyl trimethylamine intermediate further combines with another chloride ion or other anion to form lauryl trimethyl ammonium chloride. The present invention uses lauryl trimethyl ammonium chloride as an intercalation agent, and its advantages are that lauryl trimethyl ammonium chloride has good chemical stability and heat resistance, and can improve the antistatic properties of graphite to a certain extent. In addition, lauryl trimethyl ammonium chloride has good water solubility. After the graphite is hydrophilically modified with dopamine, lauryl trimethyl ammonium chloride can also better exert its intercalation effect on graphite.

[0073] Crown ethers are macrocyclic polyethers containing multiple -oxy-methylene structural units in the molecule. Common crown ethers include 15-crown-5 and 18-crown-6. Crown ethers have good compatibilization and wetting ability, which can help graphite to be better compatible with the FDY oil system, which is mainly composed of polyester or polyether compounds. The raw material components commonly used in FDY crude oil oil are polyester or polyether compounds with large molecular weight and strong hydrogen bonding. Graphite coated with crown ether organic matter on the surface will be better compatible with the oil system of polyester or polyether compounds, further improving the storage stability of FDY crude oil oil.

[0074] In some implementations of the present invention, S320 specifically includes:

[0075] S321, mixing acetic acid, 1,3,6,8-tetrakis(4-methylphenyl)pyrene and 4'-aminodibenzo-18-crown-6 in o-dichlorobenzene whose mass is 8 to 10 times that of 4'-aminodibenzo-18-crown-6, stirring for 1 to 2 hours and then degassing to obtain a third mixture;

[0076] S322, feeding the acrylic acid monomer, modified graphite and the third mixture into a third reaction kettle for closed reaction;

[0077] S323. After the closed reaction is completed, the solid matter is extracted, washed, and dried to obtain a solid lubricant.

[0078] Preferably, in S321, the molar ratio of acetic acid: 1,3,6,8-tetrakis(4-methylphenyl)pyrene: 4'-aminodibenzo-18-crown-6=(2-4):(45-55):100.

[0079] Preferably, in S322 , the mass ratio of acrylic monomer: modified graphite: third mixture is (5-10): (20-30):100.

[0080] Preferably, in S323, the temperature condition of the closed reaction is 90°C to 100°C, and the time of the closed reaction is 60h to 70h.

[0081] In the above steps, ortho-dichlorobenzene is used as a solvent, acrylic acid monomer, 1,3,6,8-tetrakis(4-methylphenyl)pyrene and 4'-aminodibenzo-18-crown-6 are used as reactants, and acetic acid is used as a catalyst to perform a polymerization reaction in ortho-dichlorobenzene to obtain an acrylic acid polymer with crown ether group branches. The acrylic acid polymer with crown ether group branches is coated on the surface of graphite, thereby reducing the surface energy of graphite by using the acrylic acid polymer, and improving the compatibility of graphite with polyester or polyether compounds in the FDY oil system by using the crown ether group.

[0082] Example 1

[0083] In this example, intercalant sample 1-2 was prepared. The raw material components used in the preparation process of the intercalant are shown in Table 1. The specific preparation process is as follows.

[0084] According to the volume ratio in Table 1, petroleum ether and n-dodecanol are added to a reaction container containing a saturated sodium chloride solution (specifically, a water-saturated sodium chloride solution) and mixed evenly to obtain a first mixture; according to the mass ratio in Table 1, according to the amount of n-dodecanol added, a corresponding amount of poly(dibenzo-18-crown-6) is continued to be added to the reaction container containing the first mixture and mixed evenly again to obtain a second mixture; the reaction container is heated to reflux the second mixture, and concentrated sulfuric acid with a concentration of 90% equal to that of the saturated sodium chloride solution is gradually added dropwise and stirred simultaneously, the dropping step is completed within 2 hours, and the stirring reaction is continued for 4 hours after the dropping is completed; after the stirring reaction is completed, the reaction container is cooled to room temperature, and the reaction container is heated. The material in the reactor is washed twice with a 20% sodium hydroxide aqueous solution, dried with anhydrous calcium chloride, and distilled under normal pressure, and a fraction of 259° C. to 261° C. is collected to obtain a reaction product; the reaction product is sent to a reactor, the reactor is evacuated, and the reaction product is heated to 90° C. to 100° C., and gaseous trimethylamine is continuously introduced into the reactor according to the mass ratio in Table 1, and the pressure in the reactor is controlled to be 3 MPa to 4 MPa; wherein the pressure in the reactor is controlled by adjusting the flow meter and the pressure relief valve of the trimethylamine; after the reaction is completed, the reactor is cooled and depressurized, and the solid in the reactor is extracted after standing for 8 hours, and the solid is dissolved in distilled water, the organic layer is removed, and the reactor is spray-dried to obtain an intercalation agent.

[0085] Table 1

[0086]

[0087] Example 2

[0088] In this example, solid lubricant samples 1-6 were prepared. The raw material components used in the preparation process of the solid lubricant are shown in Table 2. The specific preparation process is as follows.

[0089] According to the source and mass ratio of the intercalant in Table 2, dopamine, intercalant and graphite were mixed in a phosphate buffer solution with a pH value of 8, and ultrasonically treated at a frequency of 60 kHz for 40 min by an ultrasonic dispersion device. After the ultrasonic treatment, the solid was extracted, washed with water twice, and infrared dried to obtain modified graphite; according to the molar ratio in Table 2, acetic acid, 1,3,6,8-tetrakis(4-methylphenyl)pyrene and 4'-aminodibenzo-18-crown-6 were mixed in a phosphate buffer solution with a pH value of 8, and ultrasonically treated at a frequency of 60 kHz for 40 min. After the ultrasonic treatment, the solid was extracted, washed with water twice, and infrared dried to obtain modified graphite. The mixture was mixed with 10 times the mass of o-dichlorobenzene, stirred for 2 hours, and then degassed by three freeze-pump-thaw cycles to obtain a third mixture; according to the mass ratio in Table 2, the acrylic acid monomer, the modified graphite and the third mixture were fed into a reactor, the reactor was evacuated, and then the reactor was heated to 95°C and kept sealed for reaction for 70 hours; after the reaction was completed, the solid matter in the reactor was extracted, washed once with N,N-dimethylacetamide and methanol respectively, and infrared dried to obtain a solid lubricant.

[0090] Table 2

[0091]

[0092] Example 3

[0093] In this example, FDY crude oil type oil samples 1-6 were prepared. The raw material components used in the preparation process of the FDY crude oil type oil are shown in Table 3. The specific preparation process is as follows.

[0094] According to the sources and mass ratios of the solid lubricants in Table 3, lauryl diethanolamine sizing agent, lauryl alcohol polyoxyethylene ether potassium phosphate antistatic agent, polyethylene glycol fatty acid ester emulsifier, solid lubricant and lubricant white oil were put into the reactor; the reactor was evacuated and heated to 50°C, and the stirring device of the reactor was turned on. Stirring was continued for 40 minutes under insulation conditions to obtain FDY crude oil type oil.

[0095] Table 3

[0096]

[0097] Comparative Example 1

[0098] In this comparative example, FDY crude oil type oil sample 7 was prepared. The specific preparation process of FDY crude oil type oil sample 7 was the same as that of Example 3, except that the solid lubricant used was prepared by the following process.

[0099] Using the intercalant sample 1 prepared in Example 1, dopamine, intercalant and graphite were mixed in a phosphate buffer solution with a pH value of 8 at a mass ratio of dopamine: intercalant: graphite: phosphate buffer solution = 5:10:25:100, and ultrasonically treated at a frequency of 60 kHz for 40 minutes by an ultrasonic dispersion device. After the ultrasonic treatment, the solid was extracted, washed with water twice, and infrared dried to obtain modified graphite; acrylic acid monomer and modified graphite were added to a reactor at a mass ratio of acrylic acid monomer: modified graphite = 20:100, and the reactor was vacuumed, and then heated to 95° C., and the reaction time was kept warm and sealed for 10 hours; after the reaction, the solid in the reactor was extracted, washed with acetone and water once each, and infrared dried to obtain a solid lubricant.

[0100] Comparative Example 2

[0101] In this comparative example, FDY crude oil type oil sample 8 was prepared. The specific preparation process of FDY crude oil type oil sample 8 was the same as that of Example 3, except that the solid lubricant used was prepared by the following process.

[0102] The intercalant sample 1 prepared in Example 1 was used. Dopamine, intercalant, and graphite were mixed in a phosphate buffer solution with a pH value of 8 according to a mass ratio of dopamine: intercalant: graphite: phosphate buffer solution = 5:10:25:100, and ultrasonically treated at a frequency of 60 kHz for 40 minutes by an ultrasonic dispersion device. After the ultrasonic treatment, the solid was extracted, washed with water twice, and infrared dried to obtain modified graphite. Acetic acid, 1,3,6,8-tetrakis(4-methylphenyl)pyrene: 4'-aminodibenzo-18-crown-6 were mixed in a molar ratio of acetic acid: 1,3,6,8-tetrakis(4-methylphenyl)pyrene: 4'-aminodibenzo-18-crown-6 = 2:55:100. Pyrene and 4'-aminodibenzo-18-crown-6 are mixed in o-dichlorobenzene whose mass is 10 times that of 4'-aminodibenzo-18-crown-6, and after stirring for 2 hours, degassing is carried out through three freeze-pump-thaw cycles to obtain a third mixture; the modified graphite and the third mixture are sent into a reactor at a mass ratio of modified graphite: the third mixture = 25:100, and the reactor is evacuated, and then the reactor is heated to 95°C, and the reaction time is kept sealed for 70 hours; after the reaction is completed, the solid in the reactor is extracted, and washed once with N,N-dimethylacetamide and methanol respectively, and infrared drying is carried out to obtain a solid lubricant.

[0103] Performance Testing

[0104] The performance parameters of FDY crude oil type oil samples 1-8 are as follows:

[0105]

[0106] Among them, the dynamic friction coefficient and oiling rate are obtained by using FDY crude oil type oil sample 1-8 on the spinning position under the same conditions for 20 days. The spinning speed is 4800m / min and the GR2 temperature is 135℃. The detection method of smoke emission is to weigh 10 grams of sample and place it in a 50ml beaker, place the beaker in an electric heating sleeve for continuous heating, and observe its smoke emission. The detection method of coking property is to measure 1.0ml of sample and drop it on a steel sheet, place the steel sheet in an oven at 220℃ for heating treatment for 3min, and observe the coking performance of the sample after cooling to 25℃. The detection method of volatility reduction is to take 2 grams of sample and place it in a 50ml beaker, place the beaker in an oven at 200℃ for heating treatment for 2h, cool to 25℃, weigh and calculate the volatility of the sample. The detection method of open flash point is carried out in accordance with GB / T3536. Although the present invention is disclosed as above, the present invention is not limited to this. Any person skilled in the art may make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, the protection scope of the present invention shall be based on the scope defined by the claims.

Claims

1. A method for preparing FDY crude oil type oil agent for high gloss polyester fiber, characterized in that: The preparation method comprises: S100, adding the bundling agent, the antistatic agent, the emulsifier, the solid lubricant and the smoothing agent into a first reaction kettle according to a mass ratio of bundling agent: antistatic agent: emulsifier: solid lubricant: smoothing agent = (4-8): (6-12): (20-25): (10-25): (50-80); S200, raising the temperature of the first reactor to 40° C. to 60° C., turning on the stirring device of the first reactor, and continuously stirring for 20 min to 40 min under the heat preservation condition to obtain the FDY crude oil type oil agent; Wherein, the solid lubricant is prepared by the following steps: S310, in a buffer solution containing dopamine, using an intercalation agent to intercalate graphite to obtain modified graphite; S320, using raw materials including acrylic acid monomer, 1,3,6,8-tetrakis(4-methylphenyl)pyrene and 4''-aminodibenzo-18-crown-6 to prepare an organic matter including crown ether, and using the organic matter to coat the modified graphite to obtain the solid lubricant; The intercalant is prepared by the following steps: S410, mixing petroleum ether and n-dodecyl alcohol in a saturated sodium chloride solution to obtain a first mixture; S420, according to the amount of n-dodecanol added in S410, adding a corresponding amount of poly(dibenzo-18-crown-6) to the first mixture and mixing them evenly to obtain a second mixture; S430, heating the second mixture to reflux, adding concentrated sulfuric acid dropwise with stirring, and continuing to stir the reaction for 4 to 6 hours after the addition is complete; S440, after the reaction is completed, cooling to room temperature, alkali washing, drying, and distilling at normal pressure to obtain a reaction product; S450, sending the reaction product into a second reaction kettle, heating it to 90° C. to 100° C. under vacuum, continuously introducing gaseous trimethylamine into the second reaction kettle for reaction, and controlling the pressure in the second reaction kettle to be 3 MPa to 4 MPa; S460, after the reaction is completed, the second reactor is cooled and depressurized, and allowed to stand for 8 to 10 hours, and the solids in the second reactor are extracted to obtain the intercalation agent.

2. The preparation method according to claim 1, characterized in that: S310 specifically includes: S311, mixing the dopamine, the intercalation agent, and the graphite in the phosphate buffer solution at a mass ratio of dopamine: intercalation agent: graphite: phosphate buffer solution = (5-10): (5-10): (20-30): 100, and performing the intercalation treatment by an ultrasonic dispersion device; S312. After the intercalation treatment is completed, the solid matter is extracted, washed, and dried to obtain the modified graphite.

3. The preparation method according to claim 2, characterized in that: In S311, the pH value of the phosphate buffer solution is 7.5-8.5; In S311, the intercalation treatment uses an ultrasonic frequency of 60 kHz to 80 kHz; In S311, the intercalation treatment is performed using ultrasound for a time period of 30 minutes to 1 hour.

4. The preparation method according to claim 1, characterized in that: In S410, the volume ratio of petroleum ether: n-dodecyl alcohol: saturated sodium chloride solution = (40-60): (40-60): 100; In S420, in terms of mass ratio, poly(dibenzo-18-crown-6):n-dodecanol=(0.02-0.04):1; In S430, adding dropwise the concentrated sulfuric acid having an equal volume to the saturated sodium chloride solution and a concentration of 85% to 95%; In S450, the mass ratio of trimethylamine:reaction product = (30-35):

100.

5. The preparation method according to any one of claims 1 to 4, characterized in that: S320 specifically includes: S321, mixing acetic acid, 1,3,6,8-tetrakis(4-methylphenyl)pyrene and 4''-aminodibenzo-18-crown-6 in o-dichlorobenzene whose mass is 8 to 10 times that of the 4''-aminodibenzo-18-crown-6, stirring for 1 to 2 hours and then degassing to obtain a third mixture; S322, sending the acrylic acid monomer, the modified graphite and the third mixture into a third reaction kettle for closed reaction; S323, after the closed reaction is completed, the solid matter is extracted, washed, and dried to obtain the solid lubricant.

6. The preparation method according to claim 5, characterized in that: In S321, the molar ratio of acetic acid: 1,3,6,8-tetrakis(4-methylphenyl)pyrene: 4''-aminodibenzo-18-crown-6 = (2-4): (45-55):

100.

7. The preparation method according to claim 5, characterized in that: In S322, the mass ratio of acrylic monomer: modified graphite: third mixture is (5-10): (20-30):

100.

8. The preparation method according to claim 5, characterized in that: In S323, the temperature condition of the closed reaction is 90°C to 100°C, and the time of the closed reaction is 60h to 70h.

9. An FDY crude oil type oil agent for high gloss polyester fiber, characterized in that: The FDY crude oil type oil agent for high-gloss polyester fiber is obtained by the preparation method as described in any one of claims 1 to 8.

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