A kind of full-dull polyester high-speed spinning POY oil agent and preparation method thereof

Abstract

The invention belongs to the technical field of polyester oil, and specifically relates to a full-dull polyester high-speed spinning POY oil and a preparation method thereof. The full-dull polyester high-speed spinning POY oil comprises the following components by weight: 60-70 parts of a smoothing agent; 10-15 parts of an emulsifier; 5-8 parts of an antistatic agent; 3-5 parts of a sizing agent; and 8-10 parts of an additive. The full-dull polyester high-speed spinning POY oil prepared by the invention has good smooth wetting performance, heat resistance, antistatic performance and stability. When applied to the full-dull polyester POY, no abnormal phenomena such as hairy fibers and broken ends occur, and the high-quality rate of the full-dull polyester fiber is high.

Description

Technical Field

[0001] The invention belongs to the technical field of polyester oil agents, and in particular relates to a full-dull polyester high-speed spinning POY oil agent and a preparation method thereof. Background Art

[0002] Polyester fiber, also known as polyester fiber, is made from polyethylene terephthalate (PET) or its copolymers through a spinning process. It has high strength, wear resistance, heat resistance and corrosion resistance, and is easy to clean and maintain. It is widely used in textile clothing, household goods, industry and many other fields; the polyester high-speed spinning production process is an efficient polyester fiber production method. During the high-speed spinning, drawing and post-processing of polyester fibers, it is necessary to spray oil on the fiber surface to improve the smoothness, bundling and antistatic properties of the fibers, improve the drawing, curling, winding and textile processing properties of the fibers, avoid the occurrence of lint and broken ends in the production process, and ensure the smooth progress of the production process. Therefore, oil becomes an indispensable processing aid in the polyester spinning process.

[0003] Polyester POY oil is an oil specially used for the production of polyester pre-oriented yarn (POY). Its main components include base oil, emulsifier, antistatic agent, smoothing agent and sizing agent, etc.; Chinese patent application number CN202310062228.2 discloses a polyester POY oil and its preparation method. The polyester POY oil includes: 50-80 parts of smoothing agent; 5-12 parts of antistatic agent; 7-10 parts of sizing agent; 20-30 parts of emulsifier; 8-25 parts of additives, wherein the smoothing agent includes mineral oil, polyether, trimethylolpropane ester, oleic acid (i.e., modified ricinoleic acid), and phosphate ester, and the additives include flake graphite and nano-silicon dioxide particles. The prepared POY oil has good heat resistance and is formed. The advantages of high oil film strength and good antistatic performance; Chinese patent application number CN202311846792.X also discloses a polyester POY oil agent and its preparation method, which includes the following raw material components by weight: 40-50 parts of smoothing agent; 10-20 parts of emulsifier; 5-8 parts of antistatic agent; 1-3 parts of clustering agent; 3-6 parts of stabilizer; 5-10 parts of viscosity-temperature-viscosity characteristic regulator; 20-30 parts of deionized water; wherein the viscosity-temperature-viscosity characteristic regulator has a sustained release function, which can gradually release the viscosity regulator, viscosity regulating auxiliary agent and water locking agent therein during use, thereby alleviating the problem of unstable viscosity-temperature-viscosity characteristics caused by phase separation of the oil agent, and improving the performance of the oil agent at high temperature.

[0004] Although the above patents have obtained polyester POY oil agents with better performance through different improvements, they are not suitable for the processing of full-dull polyester fibers. Since at least 1.5% of matting agent titanium dioxide is added to the full-dull polyester fibers, titanium dioxide is easy to agglomerate and precipitate on the melt surface during high-speed spinning, increasing the friction between fibers and fibers, and between fibers and equipment, thereby causing white powder and abnormal spinning phenomena such as tension fluctuations and entanglement, which affect the superior quality rate of full-dull polyester fiber products; therefore, it is necessary to develop a POY oil agent suitable for full-dull polyester fibers. Summary of the invention

[0005] The purpose of the present invention is to provide a full-dull polyester high-speed spinning POY oil agent and a preparation method thereof in view of the deficiencies in the prior art. The prepared full-dull polyester high-speed spinning POY oil agent has good smooth wetting performance, heat resistance, antistatic performance and stability. When applied to the full-dull polyester POY, no abnormal phenomena such as hairy fibers and broken ends occur, and the high-quality rate of the full-dull polyester fiber is high.

[0006] The technical solution adopted by the present invention to achieve the above-mentioned purpose is:

[0007] A full-dull polyester high-speed spinning POY oil agent comprises the following components by weight: 60-70 parts of a smoothing agent; 10-15 parts of an emulsifier; 5-8 parts of an antistatic agent; 3-5 parts of a bundling agent; and 8-10 parts of an additive.

[0008] Furthermore, the smoothing agent is composed of fatty acid ester and polyether in a mass ratio of 1-1.5:6; the fatty acid ester is any one of glycerol monopalmitate, glycerol monooleate, and glycerol monostearate, or a mixture of several of them; the polyether is any one of fatty acid random polyoxyethylene polyoxypropylene ether, fatty alcohol random polyoxyethylene polyoxypropylene ether, and fatty acid polyoxyethylene ether, or a mixture of several of them.

[0009] Furthermore, the emulsifier is any one of stearate, N-methylamide carboxylate, and sorbitan fatty acid ester polyoxyethylene ether, or a mixture of several of them.

[0010] Furthermore, the antistatic agent is composed of an alkyl phosphate salt and an alkyl sodium sulfonate derivative in a mass ratio of 1:1.

[0011] Furthermore, the sizing agent is any one of lauryl polyoxyethylene ether, sulfated castor oil, and coconut oil fatty acid diethanolamide, or a mixture of several of them.

[0012] Furthermore, the additive consists of modified titanium dioxide and ethylene glycol in a mass ratio of 1:3-4.

[0013] In the technical solution of the present invention, the preparation method of the modified titanium dioxide is:

[0014] S1. Disperse nano titanium dioxide into 50% ethanol solution, add 3-aminopropyltriethoxysilane, mix well, adjust the pH value of the solution to about 6.5, heat to 40-50°C, stir and react for 4-5h, filter after the reaction is complete, wash the filter residue repeatedly with ethanol, and dry to obtain amino titanium dioxide;

[0015] S2. Disperse the amino titanium dioxide in ethanol, add sodium alkyl sulfonate derivatives and triethylamine, mix well, heat to 60-65°C, react for 6-7 hours, filter after the reaction is completed, wash the filter residue repeatedly with ethanol, and dry to obtain modified nano titanium dioxide.

[0016] Furthermore, the mass ratio of the nano titanium dioxide and 3-aminopropyltrimethoxysilane in step S1 is 1:0.05-0.07; the mass ratio of the amino titanium dioxide, sodium alkyl sulfonate derivative and triethylamine in step S2 is 1:0.1-0.2:0.02-0.04.

[0017] In the technical solution of the present invention, the preparation method of the sodium alkyl sulfonate derivative is:

[0018] (1) Add N,N-dimethylformamide, 5-chlorobenzotriazole, 8-chloro-1-octanol and sodium hydroxide to a reaction vessel, mix well, heat to 90-100°C, stir and react for 3-4 hours. After the reaction is completed, cool, extract with water and ethyl acetate, and concentrate the organic phase under reduced pressure to obtain an octanol derivative with the chemical formula:

[0019] ;

[0020] (2) Add acetonitrile, octanol derivative and 1,3-propyl sultone into a reaction container, mix well, and add 30% sodium methoxide methanol solution dropwise while stirring. After the addition is complete, heat to 70-80°C and react for 5-6 hours. After the reaction is complete, filter to remove insoluble matter, add sodium hydroxide to the filtrate, stir for 0.5 hours, remove acetonitrile, extract with water and ethyl acetate, and concentrate the aqueous phase under reduced pressure to obtain a sodium alkyl sulfonate derivative with the chemical formula:

[0021] .

[0022] Furthermore, the molar ratio of 5-chlorobenzotriazole, 8-chloro-1-octanol and sodium hydroxide in step (1) is 1:1-1.1:1.1-1.2; the molar ratio of octanol derivative, 1,3-propyl sultone and sodium methoxide in step (2) is 1:1.1-1.2:0.1-0.2; the molar amount of sodium hydroxide is the same as that of 1,3-propyl sultone.

[0023] The present invention also provides a method for preparing a fully matte polyester high-speed spinning POY oil agent, comprising the following steps: adding a smoothing agent, an emulsifier, an antistatic agent, and a sizing agent into a reaction kettle according to a mass ratio, stirring for 1-1.5 hours at 50-60° C. and a rotation speed of 600-800 r / min, then adding an additive, stirring evenly, and cooling to obtain the fully matte polyester high-speed spinning POY oil agent.

[0024] The present invention has the following beneficial effects:

[0025] In order to improve the heat resistance of alkyl sulfonate sodium salt, the present invention uses 5-chlorobenzotriazole as a raw material, and sequentially reacts with 8-chloro-1-octanol, 1,3-propyl sultone and sodium hydroxide to obtain an alkyl sodium sulfonate derivative, which contains a benzotriazole group with good heat resistance in its structure, and can improve the heat resistance of the alkyl sodium sulfonate derivative. The structure of the alkyl sodium sulfonate derivative prepared by the present invention also contains a long-chain alkyl sodium sulfonate group, which belongs to anionic surfactant compounds and has good antistatic effect and dispersing and wetting properties. The present invention uses the alkyl sodium sulfonate derivative and alkyl phosphate ester salt as an antistatic agent, which can not only jointly improve the antistatic performance of the oil, but also the alkyl sodium sulfonate derivative is helpful to improve the heat resistance of the oil.

[0026] In order to improve the dispersibility of nano titanium dioxide in oil, the present invention first introduces -NH2 on the surface of 3-aminopropyl triethoxysilane, and then reacts with phenyl chloride in alkyl sodium sulfonate derivatives to prepare modified titanium dioxide. The modified titanium dioxide has alkyl sodium sulfonate derivative molecules grafted on the surface, can be fully and evenly dispersed in the oil, improves the high temperature stability, heat resistance and antistatic performance of the oil, and has better compatibility with full-dull polyester fibers. The friction coefficients between the full-dull polyester fibers and between the fibers and metals after oiling are smaller, and the precipitation of matting agent titanium dioxide in the full-dull polyester fibers can be effectively prevented, which helps to ensure the performance of the full-dull polyester fibers and the stability of production, thereby improving the high-quality rate of the full-dull polyester fibers.

[0027] The full-dull polyester high-speed spinning POY oil agent provided by the present invention comprises a smoothing agent, an emulsifier, an antistatic agent composed of alkyl phosphate salts and alkyl sodium sulfonate derivatives, a sizing agent, and an additive composed of modified titanium dioxide and ethylene glycol. The oil agent has good smooth wetting performance, heat resistance, antistatic performance and stability. When applied to the full-dull polyester POY, no abnormal phenomena such as hairy fibers and broken ends occur, and the high-quality rate of the full-dull polyester fiber is high. DETAILED DESCRIPTION

[0028] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present application will be clearly and completely described below in combination with the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, rather than all the embodiments; the technical features designed in different implementation modes of the present invention described below can be combined with each other as long as they do not conflict with each other; based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.

[0029] In the technical scheme of the present invention, the chemical reagents used are all commercially available, among which 3-aminopropyltriethoxysilane CAS No. 919-30-2; triethylamine CAS No. 121-44-8; 5-chlorobenzotriazole CAS No. 94-97-3; 8-chloro-1-octanol CAS No. 23144-52-7; sodium hydroxide CAS No. 1310-73-2; 1,3-propyl sultone CAS No. 1120-71-4; sodium methoxide CAS No. 124-41- 4; ethylene glycol CAS No. 107-21-1; ethanol CAS No. 64-17-5; N,N-dimethylformamide CAS No. 68-12-2; acetonitrile CAS No. 75-05-8; fatty acid random polyoxyethylene polyoxypropylene ether is stearic acid random polyoxyethylene polyoxypropylene ether 1500; fatty alcohol random polyoxyethylene polyoxypropylene ether is glycerol random polyoxyethylene polyoxypropylene ether 3000; fatty acid polyoxyethylene ether is lauric acid polyoxyethylene ether (the average addition number of polyoxyethylene is 9).

[0030] This embodiment provides a method for preparing a sodium alkyl sulfonate derivative, specifically:

[0031] (1) Add 650 mL of N,N-dimethylformamide, 20.0 g of 5-chlorobenzotriazole, 23.6 g of 8-chloro-1-octanol and 6.3 g of sodium hydroxide into a reaction container, mix well, heat to 90°C, stir and react for 4 hours. After the reaction is completed, cool, extract with water and ethyl acetate, and concentrate the organic phase under reduced pressure to obtain 31.4 g of octanol derivative; the molar ratio of 5-chlorobenzotriazole, 8-chloro-1-octanol and sodium hydroxide is 1:1.1:1.2; the reaction process is:

[0032] ;

[0033] Octanol derivative: ESI (m / z): 282.7 [M+H] + , 1H-NMR (600MHz, DMSO-d6, δppm): 7.99 (s, 1H), 7.90 (d, J=8.4Hz, 1H), 7.46 (d, J=8.4Hz, 1H), 4.70 (s, 1H), 4.46-4.49 (m, 2H), 3.62-3.66 (m, 2H), 1.95-2.01 (m, 2H), 1.46-1.52 (m, 4H), 1.26-1.31 (m, 6H).

[0034] (2) Add 500 mL of acetonitrile, 30.0 g of octanol derivative and 15.6 g of 1,3-propyl sultone into a reaction container, mix well, and add 3.8 g of 30% sodium methoxide methanol solution dropwise while stirring. After the addition is complete, heat the mixture to 80°C and react for 5 h. After the reaction is complete, filter and remove insoluble matter. Add 5.1 g of sodium hydroxide to the filtrate and stir for 0.5 h to remove acetonitrile. Extract the mixture with water and ethyl acetate, and concentrate the aqueous phase under reduced pressure to obtain 38.6 g of sodium alkyl sulfonate derivative. The molar ratio of octanol derivative, 1,3-propyl sultone and sodium methoxide is 1:1.2:0.2. The molar amount of sodium hydroxide is the same as that of 1,3-propyl sultone. The reaction process is as follows:

[0035] ;

[0036] Sodium alkyl sulfonate derivative: ESI (m / z): 426.9 [M+H] + , 1 H-NMR (600MHz, DMSO-d6, δppm): 8.01 (s, 1H), 7.92 (d, J=8.4Hz, 1H), 7.45 (d, J=8.4Hz, 1H), 4.46-4.50 ( m, 2H), 3.35-3.38 (m, 4H), 3.01-3.10 (m, 2H), 1.90-1.95 (m, 4H), 1.45-1.50 (m, 4H), 1.25-1.31 (m, 6H).

[0037] A full-dull polyester high-speed spinning POY oil agent comprises the following components in parts by weight: 70 parts of a smoothing agent; 15 parts of an emulsifier; 7 parts of an antistatic agent; 5 parts of a bundling agent; and 10 parts of an additive.

[0038] The lubricant is composed of fatty acid ester and polyether in a mass ratio of 1.5:6; the fatty acid ester is glycerol monopalmitate; the polyether is fatty alcohol random polyoxyethylene polyoxypropylene ether; the emulsifier is stearate; the antistatic agent is composed of alkyl phosphate salt and alkyl sodium sulfonate derivative in a mass ratio of 1:1; the sizing agent is coconut oil fatty acid diethanolamide; the additive is composed of modified titanium dioxide and ethylene glycol in a mass ratio of 1:3.

[0039] The preparation method of modified titanium dioxide is:

[0040] S1. Disperse nano titanium dioxide into 50% ethanol solution, add 3-aminopropyltriethoxysilane, mix well, adjust the pH value of the solution to about 6.5, heat to 50°C, stir and react for 4 hours, filter after the reaction is completed, wash the filter residue repeatedly with ethanol, and dry to obtain amino titanium dioxide; the mass ratio of nano titanium dioxide to 3-aminopropyltrimethoxysilane is 1:0.07;

[0041] S2. Disperse the aminated titanium dioxide in ethanol, add sodium alkyl sulfonate derivatives and triethylamine, mix well, heat to 65°C, react for 7 hours, filter after the reaction is completed, wash the filter residue repeatedly with ethanol, and dry to obtain modified nano titanium dioxide; the mass ratio of aminated titanium dioxide, sodium alkyl sulfonate derivatives, and triethylamine is 1:0.2:0.04.

[0042] A method for preparing a fully matte polyester high-speed spinning POY oil agent comprises the following steps: adding a smoothing agent, an emulsifier, an antistatic agent and a sizing agent into a reaction kettle according to a mass ratio, stirring for 1.5 hours at 60° C. and a rotation speed of 700 r / min, then adding an additive, stirring evenly, and cooling to obtain a fully matte polyester high-speed spinning POY oil agent.

[0043] A full-dull polyester high-speed spinning POY oil agent comprises the following components in parts by weight: 65 parts of a smoothing agent; 13 parts of an emulsifier; 8 parts of an antistatic agent; 3 parts of a bundling agent; and 9 parts of an additive.

[0044] The lubricant is composed of fatty acid ester and polyether in a mass ratio of 1.3:6; the fatty acid ester is glycerol monostearate; the polyether is fatty acid random polyoxyethylene polyoxypropylene ether; the emulsifier is sorbitan fatty acid ester polyoxyethylene ether; the antistatic agent is composed of alkyl phosphate salt and alkyl sodium sulfonate derivative in a mass ratio of 1:1; the sizing agent is lauryl polyoxyethylene ether; the additive is composed of modified titanium dioxide and ethylene glycol in a mass ratio of 1:3.5.

[0045] The preparation method of modified titanium dioxide is:

[0046] S1. Disperse nano titanium dioxide into 50% ethanol solution, add 3-aminopropyltriethoxysilane, mix well, adjust the pH value of the solution to about 6.5, heat to 40°C, stir and react for 5 hours, filter after the reaction is completed, wash the filter residue repeatedly with ethanol, and dry to obtain amino titanium dioxide; the mass ratio of nano titanium dioxide to 3-aminopropyltrimethoxysilane is 1:0.06;

[0047] S2. Disperse the aminated titanium dioxide in ethanol, add sodium alkyl sulfonate derivatives and triethylamine, mix well, heat to 60°C, react for 6.5 hours, filter after the reaction is completed, wash the filter residue repeatedly with ethanol, and dry to obtain modified nano titanium dioxide; the mass ratio of aminated titanium dioxide, sodium alkyl sulfonate derivatives, and triethylamine is 1:0.1:0.03.

[0048] A method for preparing a fully matte polyester high-speed spinning POY oil agent comprises the following steps: adding a smoothing agent, an emulsifier, an antistatic agent and a sizing agent into a reaction kettle according to a mass ratio, stirring for 1 hour at 55° C. and a rotation speed of 800 r / min, then adding additives, stirring evenly, and cooling to obtain a fully matte polyester high-speed spinning POY oil agent.

[0049] A full-dull polyester high-speed spinning POY oil agent comprises the following components in parts by weight: 60 parts of a smoothing agent; 10 parts of an emulsifier; 5 parts of an antistatic agent; 4 parts of a bundling agent; and 8 parts of an additive.

[0050] The lubricant is composed of fatty acid ester and polyether in a mass ratio of 1:6; the fatty acid ester is glycerol monooleate; the polyether is fatty acid polyoxyethylene ether; the emulsifier is N-methylamide carboxylate; the antistatic agent is composed of alkyl phosphate salt and alkyl sodium sulfonate derivative in a mass ratio of 1:1; the sizing agent is sulfated castor oil; and the additive is composed of modified titanium dioxide and ethylene glycol in a mass ratio of 1:4.

[0051] The preparation method of modified titanium dioxide is:

[0052] S1. Disperse nano titanium dioxide into 50% ethanol solution, add 3-aminopropyltriethoxysilane, mix well, adjust the pH value of the solution to about 6.5, heat to 45°C, stir and react for 4.5 hours, filter after the reaction is completed, wash the filter residue repeatedly with ethanol, and dry to obtain amino titanium dioxide; the mass ratio of nano titanium dioxide to 3-aminopropyltrimethoxysilane is 1:0.05;

[0053] S2. Disperse the aminated titanium dioxide in ethanol, add sodium alkyl sulfonate derivatives and triethylamine, mix well, heat to 65°C, react for 6 hours, filter after the reaction is completed, wash the filter residue repeatedly with ethanol, and dry to obtain modified nano titanium dioxide; the mass ratio of aminated titanium dioxide, sodium alkyl sulfonate derivatives, and triethylamine is 1:0.15:0.02.

[0054] A method for preparing a fully matte polyester high-speed spinning POY oil agent comprises the following steps: adding a smoothing agent, an emulsifier, an antistatic agent and a sizing agent into a reaction kettle according to a mass ratio, stirring for 1.5 hours at 50° C. and a rotation speed of 600 r / min, then adding an additive, stirring evenly, and cooling to obtain a fully matte polyester high-speed spinning POY oil agent.

[0055] Comparative Example 1

[0056] Compared with Example 2, the antistatic agent in this comparative example is an alkyl phosphate salt.

[0057] A full-dull polyester high-speed spinning POY oil agent comprises the following components in parts by weight: 70 parts of a smoothing agent; 15 parts of an emulsifier; 7 parts of an antistatic agent; 5 parts of a bundling agent; and 10 parts of an additive.

[0058] The lubricant is composed of fatty acid ester and polyether in a mass ratio of 1.5:6; the fatty acid ester is glycerol monopalmitate; the polyether is fatty alcohol random polyoxyethylene polyoxypropylene ether; the emulsifier is stearate; the antistatic agent is alkyl phosphate; the sizing agent is coconut oil fatty acid diethanolamide; the additive is composed of modified titanium dioxide and ethylene glycol in a mass ratio of 1:3.

[0059] The preparation methods of modified titanium dioxide and full-dull polyester high-speed spinning POY oil agent are the same as those in Example 2.

[0060] Comparative Example 2

[0061] Compared with Example 2, the additive in this comparative example consists of nano titanium dioxide and ethylene glycol in a mass ratio of 1:3.

[0062] A full-dull polyester high-speed spinning POY oil agent comprises the following components in parts by weight: 70 parts of a smoothing agent; 15 parts of an emulsifier; 7 parts of an antistatic agent; 5 parts of a bundling agent; and 10 parts of an additive.

[0063] The lubricant is composed of fatty acid ester and polyether in a mass ratio of 1.5:6; the fatty acid ester is glycerol monopalmitate; the polyether is fatty alcohol random polyoxyethylene polyoxypropylene ether; the emulsifier is stearate; the antistatic agent is composed of alkyl phosphate salt and alkyl sodium sulfonate derivative in a mass ratio of 1:1; the sizing agent is coconut oil fatty acid diethanolamide; the additive is composed of nano titanium dioxide and ethylene glycol in a mass ratio of 1:3.

[0064] The preparation method of a fully matte polyester high-speed spinning POY oil agent is the same as that of Example 2.

[0065] Comparative Example 3

[0066] Compared with Example 2, the antistatic agent in this comparative example is an alkyl phosphate salt; and the additive is composed of nano titanium dioxide and ethylene glycol in a mass ratio of 1:3.

[0067] A full-dull polyester high-speed spinning POY oil agent comprises the following components in parts by weight: 70 parts of a smoothing agent; 15 parts of an emulsifier; 7 parts of an antistatic agent; 5 parts of a bundling agent; and 10 parts of an additive.

[0068] The lubricant is composed of fatty acid ester and polyether in a mass ratio of 1.5:6; the fatty acid ester is glycerol monopalmitate; the polyether is fatty alcohol random polyoxyethylene polyoxypropylene ether; the emulsifier is stearate; the antistatic agent is alkyl phosphate; the sizing agent is coconut oil fatty acid diethanolamide; the additive is composed of nano titanium dioxide and ethylene glycol in a mass ratio of 1:3.

[0069] The preparation method of a fully matte polyester high-speed spinning POY oil agent is the same as that of Example 2.

[0070] Performance Testing

[0071] The performance tests were conducted on the full matte polyester high-speed spinning POY oils prepared in Examples 2-4 and Comparative Examples 1-3, wherein the viscosity (25°C) test was conducted in accordance with GB / T 265-88 standard; the surface tension test was conducted in accordance with GB / T 22237-2008 standard; Smoke point test: heat 10g of sample respectively, and record the temperature when continuous smoke appears; Volatilization reduction test: heat 10g of sample at 170℃ for 1h, then cool to 25℃, weigh and record as m, volatility reduction % = (10-m) / 10×100%; Room temperature stability test: place 10% aqueous solution emulsion in a constant temperature water bath at 25℃ for 72h, and it is stable if there is no stratification; High temperature stability test: place 10% aqueous solution emulsion in a constant temperature water bath at 80℃ for 8h, and observe whether demulsification and wall hanging occur; Wetting speed test: use canvas sedimentation method to test 10% aqueous solution emulsion at 30℃; Oiling rate test refers to GB / T 6504-2017 standard.

[0072] The oil agent was applied to the full-dull polyester POY and spun at high speed to make the full-dull polyester fiber. The abnormal phenomena such as hairy fibers and broken ends and the rate of superior products were observed. The XCF-1A fiber friction coefficient tester was used to determine the fiber-metal friction coefficient μ1 and the fiber-fiber friction coefficient μ2. Antistatic performance test: The YG321 fiber resistivity meter was used to determine the resistivity under the conditions of 25°C and 60% relative humidity for 24 hours. The results are shown in Table 1 below.

[0073] Table 1 Performance test results

[0074]

[0075] From the results in Table 1, it can be seen that the viscosity of the polyester high-speed spinning POY oil prepared in Examples 2-4 of the present invention is 123-128 cP, the oiling rate is 0.43-0.45%, the stability is good, the surface tension is low, the wetting speed is fast, the friction coefficient is small, the smoke point is high, the volatile loss is low, and the specific resistivity is low, indicating that it has good smooth wetting performance, heat resistance and antistatic performance. It is used on full-dull polyester POY, and the full-dull polyester fiber is made by high-speed spinning without abnormal phenomena such as hairy silk and broken ends, and the rate of excellent products reaches 99%; compared with Comparative Examples 1-3, the sodium alkyl sulfonate derivative in the antistatic agent of Example 2 of the present invention and the modified titanium dioxide in the additive can jointly improve the smooth wetting performance, heat resistance and antistatic performance of the oil.

[0076] It should be noted that, in this article, terms such as "comprises", "includes" or any other variations thereof are intended to cover non-exclusive inclusion, so that a process, method, article or apparatus that includes a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or apparatus.

[0077] Although the embodiments of the present application have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present application, and that the scope of the present application is defined by the appended claims and their equivalents.

Claims

1. A full-dull polyester high-speed spinning POY oil agent, characterized in that: The invention comprises the following components by weight: 60-70 parts of a smoothing agent; 10-15 parts of an emulsifier; 5-8 parts of an antistatic agent; 3-5 parts of a sizing agent; and 8-10 parts of an additive; wherein the antistatic agent is composed of an alkyl phosphate salt and an alkyl sodium sulfonate derivative in a mass ratio of 1:1; and the additive is composed of modified titanium dioxide and ethylene glycol in a mass ratio of 1:3-4. The preparation method of the modified titanium dioxide is: S1. Disperse nano titanium dioxide into 50% ethanol solution, add 3-aminopropyltriethoxysilane, mix well, adjust the pH value of the solution to about 6.5, heat to 40-50°C, stir and react for 4-5h, filter after the reaction is complete, wash the filter residue repeatedly with ethanol, and dry to obtain amino titanium dioxide; S2, dispersing the aminated titanium dioxide in ethanol, adding sodium alkyl sulfonate derivatives and triethylamine, mixing evenly, heating to 60-65°C, reacting for 6-7h, filtering after the reaction is completed, washing the filter residue repeatedly with ethanol, and drying to obtain modified nano titanium dioxide; The sodium alkyl sulfonate derivatives described in the preparation methods of the antistatic agent and modified titanium dioxide are all obtained by reacting 5-chlorobenzotriazole as a raw material with 8-chloro-1-octanol, 1,3-propyl sultone and sodium hydroxide in sequence; the sodium alkyl sulfonate derivatives described in the preparation methods of the antistatic agent and modified titanium dioxide are all: 。 2. A full matte polyester high-speed spinning POY oil according to claim 1, characterized in that: The preparation method of the sodium alkyl sulfonate derivative is: (1) Add N,N-dimethylformamide, 5-chlorobenzotriazole, 8-chloro-1-octanol and sodium hydroxide to a reaction vessel, mix well, heat to 90-100° C., stir and react for 3-4 hours. After the reaction is completed, cool, extract with water and ethyl acetate, and concentrate the organic phase under reduced pressure to obtain an octanol derivative; (2) Add acetonitrile, octanol derivative and 1,3-propyl sultone into a reaction vessel, mix well, and add 30% sodium methoxide methanol solution dropwise while stirring. After the addition is complete, raise the temperature to 70-80°C and react for 5-6 hours. After the reaction is completed, filter to remove insoluble matter, add sodium hydroxide to the filtrate, stir for 0.5 hours, remove acetonitrile, extract with water and ethyl acetate, and concentrate the aqueous phase under reduced pressure to obtain a sodium alkyl sulfonate derivative.

3. A full matte polyester high-speed spinning POY oil according to claim 2, characterized in that: The molar ratio of 5-chlorobenzotriazole, 8-chloro-1-octanol and sodium hydroxide in step (1) is 1:1-1.1:1.1-1.2; the molar ratio of octanol derivative, 1,3-propyl sultone and sodium methoxide in step (2) is 1:1.1-1.2:0.1-0.2; the molar amount of sodium hydroxide is the same as that of 1,3-propyl sultone.

4. The full matt polyester high-speed spinning POY oil according to claim 1, characterized in that: In the preparation method of modified titanium dioxide, the mass ratio of nano titanium dioxide and 3-aminopropyltrimethoxysilane in step S1 is 1:0.05-0.07; the mass ratio of amination titanium dioxide, sodium alkyl sulfonate derivative and triethylamine in step S2 is 1:0.1-0.2:0.02-0.

04.

5. The full matt polyester high-speed spinning POY oil according to claim 1, characterized in that: The smoothing agent consists of fatty acid ester and polyether in a mass ratio of 1-1.5:

6.

6. A full matt polyester high-speed spinning POY oil according to claim 5, characterized in that: The fatty acid ester is any one of glycerol monopalmitate, glycerol monooleate, and glycerol monostearate, or a mixture of several of them.

7. The full matt polyester high-speed spinning POY oil according to claim 5, characterized in that: The polyether is any one of fatty acid random polyoxyethylene polyoxypropylene ether, fatty alcohol random polyoxyethylene polyoxypropylene ether, fatty acid polyoxyethylene ether, or a mixture of several of them.

8. The full matt polyester high-speed spinning POY oil according to claim 1, characterized in that: The emulsifier is any one of stearate, N-methylamide carboxylate, and sorbitan fatty acid ester polyoxyethylene ether, or a mixture of several of them.

9. The full matt polyester high-speed spinning POY oil according to claim 1, characterized in that: The sizing agent is any one of lauryl polyoxyethylene ether, sulfated castor oil, and coconut oil fatty acid diethanolamide, or a mixture of several of them.

10. A method for preparing the full-dull polyester high-speed spinning POY oil according to any one of claims 1 to 9, characterized in that: The method comprises the following steps: adding a smoothing agent, an emulsifier, an antistatic agent and a sizing agent into a reaction kettle according to a mass ratio, stirring for 1-1.5 hours at 50-60° C. and a rotation speed of 600-800 r / min, then adding additives, stirring evenly, and obtaining a full-dull polyester high-speed spinning POY oil agent after cooling.

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