Preparation Method and Application of a Polyester FDY Spinning Finish

Abstract

The invention discloses a preparation method and application of polyester FDY spinning oil, and relates to the technical field of spinning oil. The preparation method comprises the following steps: adding a smoothing agent and an emulsifier into a reaction kettle, heating to 50-70°C and stirring for 1-2 hours; adding an antistatic agent and water, and stirring for 0.5-1 hour; adding a wetting and penetrating agent and an antioxidant, stirring and mixing evenly; cooling to room temperature, filtering, and obtaining a polyester FDY spinning oil; the raw materials of the polyester FDY spinning oil include the following components: by mass, 40-60 parts of a smoothing agent, 15-40 parts of an emulsifier, 1-5 parts of an antistatic agent, 1-10 parts of a wetting and penetrating agent, 0.3-2 parts of an antioxidant, and 5-10 parts of water. In the scheme, an oil-based oiling agent is prepared, which effectively enhances the oil film strength of the polyester FDY spinning oil; and further improves the efficiency and product quality of the polyester FDY spinning process.

Description

Technical Field

[0001] The present invention relates to the technical field of spinning finishes, and specifically to a preparation method and application of a polyester FDY spinning finish. Background Art

[0002] In the chemical fiber industry of our country, the output of polyester accounts for more than 80% of the total industrial output; among them, the annual output of polyester fully drawn yarn (polyester FDY) exceeds 15 million tons, which is one of the main products of the polyester industry. Polyester FDY belongs to continuous fiber, which is a fully drawn fiber with the characteristics of high strength and high modulus. Its structure is compact and it is suitable for use in knitted fabrics and textiles, etc., and has a very wide range of applications.

[0003] At present, the main preparation method of polyester FDY is the one-step spinning and drawing method that combines high-speed spinning (the spinning speed is generally 2600 - 3500 m / min) and ultra-high-speed drawing and winding (the speed is generally 5100 - 5500 m / min). Compared with the traditional low-speed spinning combined with high-speed drawing and winding process, this method has the advantages of low cost and stable product quality. However, since synthetic fibers do not have the natural gum and oil film that natural fibers have, they have the disadvantages of poor hygroscopicity and poor antistatic performance; as a result, they are prone to generate antistatic electricity due to continuous friction during the spinning process, and it is necessary to use additives to inhibit or prevent and eliminate the accumulation of static electricity, and at the same time endow the fibers with characteristics such as softness and smoothness to enable them to pass through the subsequent processes smoothly. The additives used in the process are generally spinning finishes. In general processes, the spinning process of polyester FDY generally has high speed and large friction, and has extremely high requirements for the quality and performance of the spinning finish; and during the stretching deformation process, the temperature of the polyester filament can be as high as about 200 °C, so it is necessary for the spinning finish to have good high-temperature resistance and oxidation resistance to improve the phenomena of smoking and coking. In addition, in the spinning industry, the traditional manufacturing process of polyester FDY mainly relies on emulsion-type oiling agents, and their high water content brings problems of energy consumption and water resource waste during the spinning process.

[0004] In summary, to solve the above problems, it is of great significance to prepare a polyester FDY spinning finish and use it to prepare polyester FDY to improve the spinnability. Summary of the Invention

[0005] The purpose of the present invention is to provide a preparation method and application of a polyester FDY spinning finish to solve the problems raised in the above background art.

[0006] To solve the above technical problems, the present invention provides the following technical solutions:

[0007] A preparation method of a polyester FDY spinning finish, comprising the following steps:

[0008] Add the smoothing agent and emulsifier into the reaction kettle, heat to 50-70°C and stir for 1-2 hours; add the antistatic agent and water, stir thoroughly for 0.5-1 hour; add the wetting penetrant and antioxidant, stir and mix evenly; cool to room temperature, filter, and obtain the polyester FDY spinning oil;

[0009] The raw materials of the polyester FDY spinning oil include the following components: by weight, 40-60 parts of a smoothing agent, 15-40 parts of an emulsifier, 1-5 parts of an antistatic agent, 1-10 parts of a wetting and penetrating agent, 0.3-2 parts of an antioxidant, and 5-10 parts of water.

[0010] More optimally, the lubricant includes one or more of natural oils, synthetic esters, polyols, polymer polyethers, and industrial white oils; the antistatic agent includes one or more of quaternary ammonium salts, alkyl alcohol phosphate polyoxyethylene ethers, alkyl alcohol phosphates, and alkyl sulfates; the wetting and penetrating agent includes one or more of silicone surfactants, alkyl alcohol block polyethers, and isomeric alcohol polyoxyethylene ethers; the antioxidant includes one or more of antioxidant 1010, antioxidant 2246, antioxidant 425, antioxidant 2246-S, and antioxidant 330.

[0011] Among them, the molecular weight of bisphenol hindered phenol antioxidant is larger, the volatility and thermal stability of the antioxidant are higher, and the anti-aging effect of bisphenol hindered phenol antioxidant in the FDY spinning process will be better;

[0012] More optimally, the antistatic agent comprises the following raw materials, in parts by weight: 3 to 5 parts of alkyl alcohol phosphate polyoxyethylene ether and 0.5 to 1.5 parts of alkyl sulfate.

[0013] More optimally, the wetting and penetrating agent comprises the following raw materials, by weight: 2 to 4 parts of isomeric tridecanol polyoxyethylene ether, 1 to 3 parts of alkyl glycoside, 2 to 4 parts of alkyl alcohol block polyether, and 1 to 3 parts of silicone surfactant.

[0014] More optimally, the kinematic viscosity of the smoothing agent at 40° C. is 0.1-0.4 St, and the smoothing agent comprises the following components: by weight, 28-32 parts of synthetic ester, 4-6 parts of copolyether, and 4-6 parts of industrial white oil.

[0015] More optimally, the emulsifier is a composition of a POSS-derived emulsifier and other emulsifiers; the other emulsifiers include one or more of polyoxyethylene lauryl ester, sorbitan fatty acid ester, fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ether, castor oil polyoxyethylene ether, and polyethylene glycol fatty acid ester.

[0016] Preferably, the emulsifier comprises the following raw materials: by mass, 8-12 parts of POSS-derived emulsifier, 8-12 parts of fatty alcohol polyoxyethylene ether, 4-6 parts of sorbitan fatty acid ester, 8-12 parts of polyethylene glycol fatty acid ester, and 4-6 parts of castor oil polyoxyethylene ether.

[0017] Preferably, the preparation method of the POSS-derived emulsifier is as follows:

[0018] Step 1: Under an inert gas atmosphere, POSS heptaisobutyltrisilanol and triethylamine are successively added to tetrahydrofuran. Under an ice bath, chlorodimethylsilane is added dropwise, and the mixture is stirred for 1-1.5 hours; stirred at room temperature for 2-3 hours, and water is added; aftertreatment is carried out to obtain POSS heptaisobutyltrisilane hydride;

[0019] Step 2: Under an inert gas atmosphere, POSS heptaisobutyltrisilane hydride, modified allyl polyethylene glycol methyl ether, and a platinum catalyst are successively added to tetrahydrofuran, and reflux reaction is carried out for 5-7 hours, and aftertreatment is carried out to obtain a POSS-derived emulsifier.

[0020] Preferably, the raw materials of the POSS heptaisobutyltrisilane hydride include the following substances: by mass, 5 parts of POSS heptaisobutyltrisilanol, 7-8 parts of triethylamine, 0.8-0.9 part of chlorodimethylsilane, and 20-25 parts of tetrahydrofuran;

[0021] The raw materials of the POSS-derived emulsifier include the following substances: by mass, 5 parts of POSS heptaisobutyltrisilane hydride, 6-7 parts of modified allyl polyethylene glycol methyl ether, 0.001-0.002 part of platinum catalyst, and 10-15 parts of tetrahydrofuran.

[0022] Preferably, the preparation method of the modified allyl polyethylene glycol methyl ether is as follows: (1) Under an inert gas atmosphere, aminopolyethylene glycol methyl ether and allyl glycidyl ether with a molar ratio of 1-1.2:1 are successively added to tetrahydrofuran, and the temperature is set at 50-60 °C and stirred for 6-8 hours, and aftertreatment is carried out to obtain allyl polyethylene glycol methyl ether; (2) Allyl polyethylene glycol methyl ether is added to an alkali solution of 1.8-2 wt%, 3-chloro-2-hydroxypropyltrimethylammonium chloride is added, and the pH is adjusted to 10-10.5; stirred at room temperature for 8-12 hours, and the pH is adjusted to 6.5-7, and aftertreatment is carried out to obtain modified allyl polyethylene glycol methyl ether; wherein, the mass ratio of allyl polyethylene glycol methyl ether to 3-chloro-2-hydroxypropyltrimethylammonium chloride is 1:0.15-0.2.

[0023] In a further embodiment, there is provided an application of a polyester FDY spinning finish. The application process is as follows: directly spinning PET raw materials, with a feeding temperature of 270 - 290 °C, a spinning rate of 3000 - 3500 m / min, an oiling method of nozzle oiling, a drawing and winding rate of 5100 - 5500 m / min, a temperature of the first hot roll of 100 - 120 °C, and a temperature of the second hot roll of 150 - 200 °C.

[0024] In a more optimized embodiment, the PET raw materials include silicon-containing PET, and its preparation method is as follows: (1) Under an inert gas atmosphere, POSS heptaisobutyltrisilane and 1-pyridylpentenol with a mass ratio of 5:4 - 5 are added to tetrahydrofuran, and a platinum catalyst is added, followed by reflux reaction for 5 - 7 hours to obtain modified alcohol-based POSS; (2) Part of terephthalic acid and part of ethylene glycol are mixed evenly, and under vacuum, the temperature is set to 265 - 270 °C for pre-reaction for 1 - 2 hours; modified alcohol-based POSS, the remaining part of terephthalic acid, and the remaining part of ethylene glycol are added, and the temperature is raised to 275 - 280 °C for continued polycondensation for 1 - 2 hours, and then cooled to obtain silicon-containing PET; the silicon-containing PET includes the following raw materials, by weight, 60 - 70 parts of terephthalic acid, 120 - 150 parts of ethylene glycol, and 10 - 15 parts of triol-based POSS.

[0025] Compared with the prior art, the beneficial effects achieved by the present invention are as follows:

[0026] (1) In the present application, through optimized raw material components and ratios, an oil-based polyester FDY spinning finish is configured; compared with common emulsion-type oiling agents, the water content is significantly reduced to about 10%, and the effective concentration is significantly increased.

[0027] (2) In the present application, due to the high viscosity of the oil-based oiling agent, during the spinning process, the wet spreading and penetration ability on the surface of the fiber filaments are limited, which may cause some problems in the spun polyester FDY, affecting the use performance of the fiber filaments and the quality of the final product. Therefore, in the solution, based on incompletely condensed POSS heptaisobutyltrisilanol, a POSS-derived emulsifier with amphiphilicity is obtained through two-step graft modification, effectively improving the disadvantages and enhancing the performance of the polyester FDY spinning finish.

[0028] Among them, the POSS-derived emulsifier is prepared by first reacting chlorine with silanol to graft chlorodimethylsilane onto POSS heptaisobutyltrisilanol to introduce silicon hydride; then using the reaction of silicon hydride with an olefin group to graft-modify allyl polyethylene glycol methyl ether; and the graft-modified allyl polyethylene glycol methyl ether is based on amino polyethylene glycol methyl ether, using the reaction of an amino group with an epoxy group to graft allyl glycidyl ether to make it have a reactive olefin group; and further using the hydroxyl group generated by the reaction of an amino group with an epoxy group to react with 3-chloro-2-hydroxypropyltrimethylammonium chloride for grafting to make it contain a quaternary ammonium salt group.

[0029] Among them, the introduction of POSS-derived emulsifier effectively improves the high-temperature resistance and oxidation resistance of FDY spinning finish, and has low viscosity, high storage stability, and excellent wetting and spreading properties; it has good emulsion stability, can effectively improve the oil film strength; and can increase the antistatic performance. Thus, it further improves the efficiency and product quality of the polyester FDY spinning process; in addition, from the perspective of environmental sustainability, the characteristics of low energy consumption and water conservation will have a positive impact on the green development of the textile industry. It should be noted that: the POSS-derived emulsifier needs to be optimized, as too much introduction is instead unfavorable to stability and oil film strength.

[0030] In the (3) solution, the polyester FDY spinning finish is used to prepare polyester FDY, the spinning parameters are optimized, the applicability of the finishing agent to spinning is effectively improved, and the spinning efficiency is increased. At the same time, in a further solution, silicon-containing PET is introduced into the PET raw material, mainly introducing a modified alcohol-based POSS obtained by grafting 1-pyridylpentenol with POSS heptaisobutyltrisilane; the introduction of this substance can effectively improve the mechanical properties of polyester FDY; at the same time, containing siloxane bonds and pyridine groups can promote charge transfer, improve antistatic properties, reduce static electricity generation during spinning, and improve spinnability. In addition, due to the affinity of the introduced modified alcohol-based POSS with the spinning solution, it can promote the spreading of the finishing agent on the filament, increase the oiling property, and improve the spinning performance. Specific embodiments

[0031] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0032] It should be noted that the following parts are by weight parts, and there are no special restrictions on the purchasing manufacturers of the raw materials involved in the present invention. Exemplarily, they include: in the following examples, the antioxidant is 2246 antioxidant, the fatty acid polyoxyethylene ether is AE0-3, the sorbitan fatty acid ester is S-60, the polyethylene glycol fatty acid ester is EGMS, the silicone surfactant is OFX-0309, the alkyl alcohol phosphate polyoxyethylene ether is NP-10P, the alkyl sulfate is SLES, the isomeric tridecyl alcohol polyoxyethylene ether is 1303, the alkyl glycoside is APG0810, the alkyl alcohol block polyether is EFS-630, the castor oil polyoxyethylene ether is EL-10, the synthetic ester is PANESTER8116, the copolymer ether is EO / PO random copolymer ether, and the industrial white oil is No. 5 white oil; the CAS number of POSS heptaisobutyltrisilanol is 307531-92-6; the CAS number of chlorodimethylsilane is 1066-35-9; the molecular weight of amino poly(ethylene glycol) methyl ether is 1K; the above-mentioned and other raw materials involved are all commercially available.

[0033] Preparation of POSS-derived emulsifier: Step 1: (1) Under a nitrogen atmosphere, amino poly(ethylene glycol) methyl ether and allyl glycidyl ether with a molar ratio of 1.2:1 are sequentially added to tetrahydrofuran, the temperature is set at 58 °C and stirred for 8 hours, and aftertreatment is carried out to obtain allyl poly(ethylene glycol) methyl ether; (2) 10 parts of allyl poly(ethylene glycol) methyl ether are added to a 2 wt% alkali solution, 1.6 parts of 3-chloro-2-hydroxypropyltrimethylammonium chloride are added, and the pH is adjusted to 10.2; stirred at room temperature for 10 hours, the pH is adjusted to 7, and aftertreatment is carried out to obtain modified allyl poly(ethylene glycol) methyl ether;

[0034] Step 2: Under a nitrogen atmosphere, 5 parts of POSS heptaisobutyltrisilanol and 7.6 parts of triethylamine are sequentially added to 20 parts of tetrahydrofuran. Under an ice bath, 0.83 parts of chlorodimethylsilane are added dropwise and stirred for 1.5 hours; stirred at room temperature for 2 hours, and the reaction is quenched with water; aftertreatment is carried out to obtain POSS heptaisobutyltrisilane;

[0035] Step 3: Under a nitrogen atmosphere, 5 parts of POSS heptaisobutyltrisilane, 6.9 parts of modified allyl poly(ethylene glycol) methyl ether, and 0.002 parts of platinum catalyst are sequentially added to 12 parts of tetrahydrofuran, and refluxed for 6 hours, and aftertreatment is carried out to obtain POSS-derived emulsifier.

[0036] Preparation of the PET raw material: (1) Under a nitrogen atmosphere, POSS heptaisobutyltrisilane and 1-pyridylpentenol with a mass ratio of 5:4.6 are added to tetrahydrofuran, and a platinum catalyst is added. The mixture is refluxed for 6 hours to obtain modified alcohol-based POSS; (2) 25 parts of terephthalic acid and 55 parts of ethylene glycol are mixed evenly. Under vacuum, the temperature is set at 265°C and pre-reacted for 1.5 hours; 12 parts of modified alcohol-based POSS, 40 parts of terephthalic acid, and 80 parts of ethylene glycol are added, and the temperature is raised to 275°C and polycondensed for 2 hours, then cooled to obtain silicon-containing PET; (3) 25 parts of terephthalic acid and 55 parts of ethylene glycol are mixed evenly. Under vacuum, the temperature is set at 265°C and pre-reacted for 1.5 hours; 40 parts of terephthalic acid and 75 parts of ethylene glycol are added, and the temperature is raised to 275°C and polycondensed for 2 hours, then cooled to obtain unmodified PET; (4) The silicon-containing PET and unmodified PET are mixed evenly according to a mass ratio of 1:1 to obtain the PET raw material.

[0037] Example 1: A preparation method of a polyester FDY spinning finish, comprising the following steps:

[0038] Step 1: (1) 30 parts of synthetic ester, 5 parts of copolymerized ether, and 5 parts of industrial white oil are mixed evenly to obtain a leveling agent; (2) 10 parts of POSS-derived emulsifier, 10 parts of fatty acid polyoxyethylene ether, 5 parts of sorbitan fatty acid ester, 10 parts of polyethylene glycol fatty acid ester, and 5 parts of castor oil polyoxyethylene ether are mixed evenly to obtain an emulsifier; (3) 4 parts of alkyl alcohol phosphate polyoxyethylene ether and 1 part of alkyl sulfate are mixed evenly to obtain an antistatic agent; (4) 3 parts of isomeric tridecanol polyoxyethylene ether, 2 parts of alkyl glycoside, 3 parts of alkyl alcohol block polyether, and 2 parts of silicone surfactant are mixed evenly to obtain a wetting and penetrating agent;

[0039] Step 2: 40 parts of the leveling agent and 35 parts of the emulsifier are added to a reaction kettle, and the temperature is raised to 60°C and stirred for 2 hours; 3 parts of the antistatic agent and 10 parts of water are added and stirred thoroughly for 0.5 hour; 10 parts of the wetting and penetrating agent and 2 parts of antioxidant are added and stirred and mixed evenly; cooled to room temperature and filtered to obtain the polyester FDY spinning finish;

[0040] Step 3: The PET raw material is directly spun with the assistance of the polyester FDY spinning finish. During the process, the feeding temperature is 285°C, the spinning speed is 3200 m / min, the oiling method is nozzle oiling, the drawing and winding speed is 5300 m / min, the temperature of the first hot roller is 120°C, and the temperature of the second hot roller is 180°C.

[0041] Example 2: A preparation method of a polyester FDY spinning finish, comprising the following steps:

[0042] Step 1: (1) Mix 30 parts of synthetic ester, 5 parts of copolymerized ether, and 5 parts of industrial white oil evenly to obtain a leveling agent; (2) Mix 8 parts of POSS-derived emulsifier, 8 parts of fatty acid polyoxyethylene ether, 6 parts of sorbitan fatty acid ester, 8 parts of polyethylene glycol fatty acid ester, and 6 parts of castor oil polyoxyethylene ether evenly to obtain an emulsifier; (3) Mix 4 parts of alkyl alcohol phosphate polyoxyethylene ether and 1 part of alkyl sulfate evenly to obtain an antistatic agent; (4) Mix 3 parts of isomeric tridecanol polyoxyethylene ether, 2 parts of alkyl glycoside, 3 parts of alkyl alcohol block polyether, and 2 parts of silicone surfactant evenly to obtain a wetting and penetrating agent;

[0043] Step 2: Add 40 parts of the leveling agent and 35 parts of the emulsifier to a reaction kettle, heat up to 60 °C and stir for 2 hours; add 3 parts of the antistatic agent and 10 parts of water, stir well for 0.5 hour; add 10 parts of the wetting and penetrating agent and 2 parts of antioxidant, stir and mix evenly; cool to room temperature, filter, and obtain a polyester FDY spinning finish;

[0044] Step 3: Directly spin the PET raw material with the assistance of the polyester FDY spinning finish. During the process, the feeding temperature is 285 °C, the spinning speed is 3200 m / min, the oiling method is nozzle oiling, the drawing and winding speed is 5300 m / min, the temperature of the first hot roller is 120 °C, and the temperature of the second hot roller is 180 °C.

[0045] Example 3: A preparation method of a polyester FDY spinning finish, comprising the following steps:

[0046] Step 1: (1) Mix 30 parts of synthetic ester, 5 parts of copolymerized ether, and 5 parts of industrial white oil evenly to obtain a leveling agent; (2) Mix 12 parts of POSS-derived emulsifier, 12 parts of fatty acid polyoxyethylene ether, 4 parts of sorbitan fatty acid ester, 12 parts of polyethylene glycol fatty acid ester, and 4 parts of castor oil polyoxyethylene ether evenly to obtain an emulsifier; (3) Mix 4 parts of alkyl alcohol phosphate polyoxyethylene ether and 1 part of alkyl sulfate evenly to obtain an antistatic agent; (4) Mix 3 parts of isomeric tridecanol polyoxyethylene ether, 2 parts of alkyl glycoside, 3 parts of alkyl alcohol block polyether, and 2 parts of silicone surfactant evenly to obtain a wetting and penetrating agent;

[0047] Step 2: Add 40 parts of the leveling agent and 35 parts of the emulsifier to a reaction kettle, heat up to 60 °C and stir for 2 hours; add 3 parts of the antistatic agent and 10 parts of water, stir well for 0.5 hour; add 10 parts of the wetting and penetrating agent and 2 parts of antioxidant, stir and mix evenly; cool to room temperature, filter, and obtain a polyester FDY spinning finish;

[0048] Step 3: Directly spin the PET raw material with the assistance of the polyester FDY spinning finish. During the process, the feeding temperature is 285°C, the spinning speed is 3200 m / min, the oiling method is nozzle oiling, the drawing and winding speed is 5300 m / min, the temperature of the first hot roller is 120°C, and the temperature of the second hot roller is 180°C.

[0049] Comparative Example 1: Based on Example 1, without introducing the POSS-derived emulsifier, and the rest is the same as Example 1. Specifically as follows:

[0050] Step 1: (1) Mix 30 parts of synthetic ester, 5 parts of copolymerized ether, and 5 parts of industrial white oil evenly to obtain a smoothing agent; (2) Mix 15 parts of fatty acid polyoxyethylene ether, 5 parts of sorbitan fatty acid ester, 15 parts of polyethylene glycol fatty acid ester, and 5 parts of castor oil polyoxyethylene ether evenly to obtain an emulsifier; (3) Mix 4 parts of alkyl alcohol phosphate polyoxyethylene ether and 1 part of alkyl sulfate evenly to obtain an antistatic agent; (4) Mix 3 parts of isomeric tridecanol polyoxyethylene ether, 2 parts of alkyl glycoside, 3 parts of alkyl alcohol block polyether, and 2 parts of silicone surfactant evenly to obtain a wetting and penetrating agent;

[0051] Step 2: Add 40 parts of the smoothing agent and 35 parts of the emulsifier to the reaction kettle, heat up to 60°C and stir for 2 hours; add 3 parts of the antistatic agent and 10 parts of water, and stir thoroughly for 0.5 hour; add 10 parts of the wetting and penetrating agent and 2 parts of antioxidant, and stir and mix evenly; cool to room temperature and filter to obtain the polyester FDY spinning finish;

[0052] Step 3: Directly spin the PET raw material with the assistance of the polyester FDY spinning finish. During the process, the feeding temperature is 285°C, the spinning speed is 3200 m / min, the oiling method is nozzle oiling, the drawing and winding speed is 5300 m / min, the temperature of the first hot roller is 120°C, and the temperature of the second hot roller is 180°C.

[0053] Comparative Example 2: Based on Example 1, use allyl polyethylene glycol methyl ether to graft and prepare the POSS-derived emulsifier, and the rest is the same as Example 1; the specific different steps are as follows:

[0054] Step 1: Under a nitrogen gas atmosphere, sequentially add aminopolyethylene glycol methyl ether and allyl glycidyl ether with a molar ratio of 1.2:1 to tetrahydrofuran, set the temperature to 58°C and stir for 8 hours, and perform post-treatment to obtain allyl polyethylene glycol methyl ether;

[0055] Step 2: Under a nitrogen gas atmosphere, sequentially add 5 parts of POSS heptaisobutyl trisilanol and 7.6 parts of triethylamine to 20 parts of tetrahydrofuran. Under ice bath, dropwise add 0.83 parts of chlorodimethylsilane and stir for 1.5 hours; stir at room temperature for 2 hours, add water to quench the reaction; perform post-treatment to obtain POSS heptaisobutyl trisilane hydrogen;

[0056] Step 3: Under a nitrogen gas atmosphere, 5 parts of POSS heptaisobutyltrisilane, 6.5 parts of allyl polyethylene glycol methyl ether, and 0.002 parts of platinum catalyst were successively added to 12 parts of tetrahydrofuran, and the mixture was refluxed for 6 hours. After post-treatment, a POSS-derived emulsifier was obtained.

[0057] Comparative Example 3: Based on Example 1, the introduction amount of the POSS-derived emulsifier was increased, and the rest was the same as in Example 1; specifically as follows:

[0058] Step 1: (1) 30 parts of synthetic ester, 5 parts of copolymerized ether, and 5 parts of industrial white oil were mixed evenly to obtain a smoothing agent; (2) 17 parts of POSS-derived emulsifier, 8 parts of fatty acid polyoxyethylene ether, 4 parts of sorbitan fatty acid ester, 8 parts of polyethylene glycol fatty acid ester, and 4 parts of castor oil polyoxyethylene ether were mixed evenly to obtain an emulsifier; (3) 4 parts of alkyl alcohol phosphate polyoxyethylene ether and 1 part of alkyl sulfate were mixed evenly to obtain an antistatic agent; (4) 3 parts of isomeric tridecanol polyoxyethylene ether, 2 parts of alkyl glycoside, 3 parts of alkyl alcohol block polyether, and 2 parts of silicone surfactant were mixed evenly to obtain a wetting and penetrating agent;

[0059] Step 2: 40 parts of the smoothing agent and 35 parts of the emulsifier were added to a reaction kettle, and the temperature was raised to 60 °C and stirred for 2 hours; 3 parts of the antistatic agent and 10 parts of water were added, and the mixture was stirred thoroughly for 0.5 hour; 10 parts of the wetting and penetrating agent and 2 parts of antioxidant were added, and the mixture was stirred and mixed evenly; cooled to room temperature and filtered to obtain a polyester FDY spinning oil agent.

[0060] Step 3: The PET raw material was directly spun with the assistance of the polyester FDY spinning oil agent. During the process, the feeding temperature was 285 °C, the spinning speed was 3200 m / min, the oiling method was nozzle oiling, the drawing and winding speed was 5300 m / min, the temperature of the first hot roll was 120 °C, and the temperature of the second hot roll was 180 °C.

[0061] Comparative Example 4: Based on Example 1, during the direct spinning process, unmodified PET was used as the PET raw material, and silicon-containing PET was not introduced; the rest was the same as in Example 1; the specific different steps are as follows:

[0062] The unmodified PET was directly spun with the assistance of the polyester FDY spinning oil agent. During the process, the feeding temperature was 285 °C, the spinning speed was 3200 m / min, the oiling method was nozzle oiling, the drawing and winding speed was 5300 m / min, the temperature of the first hot roll was 120 °C, and the temperature of the second hot roll was 180 °C.

[0063] Performance Test 1: The polyester FDY spinning oil agent prepared in Example 1 was subjected to basic performance tests.

[0064] Results: (1) Appearance: light yellow - colorless transparent liquid; (2) Emulsion stability (15% aq, standing for 72 h): stable; (3) Active content: 90%; (4) pH (1% aq): 7.5; (5) Oil film strength / N: 1268 (detected according to GB / T3142); (6) Surface tension (1% aqueous solution, 25 °C, mN / m): 29; (7) Conductivity (μs / cm): 1187; (8) Viscosity (25 °C, mPa·s): 40.6; (9) No fuming; (10) No coking.

[0065] Performance Test 2: The polyester FDY spinning finish prepared in Example 1 and Comparative Examples 1 - 2 was subjected to relevant performance comparison; the antistatic property was characterized by the dynamic voltage value obtained by an electrostatic instrument under high - speed winding; the heat - resistant property was measured by using a laser dust particle technology instrument to record the number of soot particles at the second hot roll of the spinning hot box. The obtained data are shown in Table 1:

[0066]

[0067] Conclusion: The data in Table 1 show that: the polyester FDY spinning finish prepared in this application has excellent antistatic and heat - resistant properties; the data of Comparative Examples 1 - 2 show that: in Comparative Example 1, without introducing the POSS - derived emulsifier, the antistatic and heat - resistant properties decreased significantly; in Comparative Example 2, due to the preparation of the POSS - derived emulsifier by grafting allyl polyethylene glycol methyl ether and without introducing the quaternary ammonium salt segment, the performance decreased slightly.

[0068] Performance Test 3: Example 1 was compared with Comparative Examples 3 - 4, and the full - roll rate during the spinning process was recorded to characterize the spinnability; and the breaking strength and unevenness of yarn evenness of the spun polyester FDY were detected to evaluate the finished product quality of the spun fiber; among them, for the breaking strength, referring to the filament tensile property test method in GB / T14344 - 2022, it was detected by a full - automatic single - yarn strength tester, and the breaking strength was calculated according to Section 8.2; the unevenness of yarn evenness was detected by a yarn evenness tester with a 200 - m sample at a speed of 500 m / min and a frequency of 2000 Hz. The obtained data are shown in Table 2:

[0069]

[0070] Conclusion: The data in the above table show that the polyester FDY spinning finish prepared in this application has excellent spinnability and finished product quality, and excellent application performance. The data of Comparative Examples 3-4 show that in Comparative Example 3, due to the decrease in the introduction amount of POSS-derived emulsifier, the stability and smoothness are reduced, resulting in a decrease in the full bobbin rate and unevenness of yarn evenness; in Comparative Example 4, due to using unmodified PET as the PET raw material and not introducing silicon-containing PET, the affinity of the finish is decreased, resulting in a slight decrease in the full bobbin rate; however, due to the absence of silicon-containing materials, the fiber mechanical properties are decreased.

[0071] Finally, it should be noted that the above are only the preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, for those skilled in the art, they can still modify the technical solutions described in the foregoing embodiments, or perform equivalent replacements for some of the technical features. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention shall be included within the protection scope of the present invention.

Claims

1. A method for preparing a polyester FDY spinning oil, characterized in that: The following steps are involved: Add the smoothing agent and emulsifier into the reaction kettle, heat to 50-70°C and stir for 1-2 hours; add the antistatic agent and water, stir thoroughly for 0.5-1 hour; add the wetting penetrant and antioxidant, stir and mix evenly; cool to room temperature, filter, and obtain the polyester FDY spinning oil; The raw materials of the polyester FDY spinning oil include the following components: by weight, 40-60 parts of a smoothing agent, 15-40 parts of an emulsifier, 1-5 parts of an antistatic agent, 1-10 parts of a wetting and penetrating agent, 0.3-2 parts of an antioxidant, and 5-10 parts of water; The emulsifier comprises the following raw materials: by weight, 8 to 12 parts of POSS derived emulsifier, 8 to 12 parts of fatty acid polyoxyethylene ether, 4 to 6 parts of sorbitan fatty acid ester, 8 to 12 parts of polyethylene glycol fatty acid ester, and 4 to 6 parts of castor oil polyoxyethylene ether; The preparation method of the POSS derivative emulsifier is as follows: step 1: under an inert gas atmosphere, POSS heptaisobutyltrisilanol and triethylamine are sequentially added to tetrahydrofuran, and chlorodimethylsilane is added dropwise under an ice bath, and stirred for 1 to 1.5 hours; stirred at room temperature for 2 to 3 hours, and water is added; Post-treatment to obtain POSS heptaisobutyl trisilane; step 2: under an inert gas atmosphere, POSS heptaisobutyl trisilane, quaternary ammonium salt-modified allyl polyethylene glycol methyl ether, and platinum catalyst are sequentially added to tetrahydrofuran, refluxed for 5 to 7 hours, and post-treated to obtain a POSS-derived emulsifier; The preparation method of the quaternary ammonium salt modified allyl polyethylene glycol methyl ether is as follows: (1) under an inert gas atmosphere, amino polyethylene glycol methyl ether and allyl glycidyl ether in a molar ratio of 1 to 1.2:1 are sequentially added to tetrahydrofuran, the temperature is set to 50 to 60° C., stirred for reaction for 6 to 8 hours, and post-treated to obtain allyl polyethylene glycol methyl ether; (2) allyl polyethylene glycol methyl ether is added to 1.8 to 2 wt % alkali solution, 3-chloro-2-hydroxypropyltrimethylammonium chloride is added, and the pH is adjusted to 10 to 10.5; the reaction is stirred at room temperature for 8 to 12 hours, the pH is adjusted to 6.5 to 7, and post-treated to obtain quaternary ammonium salt modified allyl polyethylene glycol methyl ether.

2. The method for preparing a polyester FDY spinning oil according to claim 1, characterized in that: The lubricant includes one or more of natural oils, synthetic esters, polyols, polymer polyethers, and industrial white oils; the antistatic agent includes one or more of quaternary ammonium salts, alkyl alcohol phosphate polyoxyethylene ethers, alkyl alcohol phosphates, and alkyl sulfates; the wetting and penetrating agent includes one or more of silicone surfactants, alkyl alcohol block polyethers, and isomeric alcohol polyoxyethylene ethers; the antioxidant includes one or more of antioxidant 1010, antioxidant 2246, antioxidant 425, antioxidant 2246-S, and antioxidant 330.

3. The method for preparing a polyester FDY spinning oil according to claim 2, characterized in that: The kinematic viscosity of the smoothing agent at 40° C. is 0.1-0.4 St. The smoothing agent comprises the following components: by weight, 28-32 parts of synthetic ester, 4-6 parts of copolyether, and 4-6 parts of industrial white oil.

4. The method for preparing a polyester FDY spinning oil according to claim 1, characterized in that: The raw material of the POSS heptaisobutyl trisilyl hydrogen The material comprises the following substances: by weight, 5 parts of POSS heptaisobutyl trisilanol, 7-8 parts of triethylamine, 0.8-0.9 parts of chlorodimethylsilane, and 20-25 parts of tetrahydrofuran; the raw materials of the POSS-derived emulsifier comprise the following substances: by weight, 5 parts of POSS heptaisobutyl trisilane, 6-7 parts of quaternary ammonium salt-modified allyl polyethylene glycol methyl ether, 0.001-0.002 parts of platinum catalyst, and 10-15 parts of tetrahydrofuran.

5. The method for preparing a polyester FDY spinning oil according to claim 1, characterized in that: The mass ratio of allyl polyethylene glycol methyl ether to 3-chloro-2-hydroxypropyltrimethylammonium chloride is 1:0.15-0.

2.

6. An application of a polyester FDY spinning oil, characterized in that: The polyester FDY spinning oil prepared by the preparation method of a polyester FDY spinning oil according to any one of claims 1 to 5 has the following application process: directly spinning the PET raw material, the feed temperature is 270~290°C, the spinning rate is 3000~3500m / min, the oiling method is nozzle oiling, the stretching and winding rate is 5100~5500m / min, the first hot roller temperature is 100~120°C, and the second hot roller temperature is 150~200°C.

7. The use of a polyester FDY spinning oil according to claim 6, characterized in that: The PET raw material includes silicon-containing PET, and its preparation method is as follows: (1) under an inert gas atmosphere, POSS heptaisobutyl trisilane and 1-pyridine pentenol in a mass ratio of 5:4-5 are added to tetrahydrofuran, a platinum catalyst is added, and reflux reaction is carried out for 5-7 hours to obtain modified alcohol-based POSS; (2) part of terephthalic acid and part of ethylene glycol are mixed evenly, and under vacuum, the temperature is set to 265-270° C., and pre-reacted for 1-2 hours; the modified alcohol-based POSS, the remaining part of terephthalic acid and the remaining part of ethylene glycol are added, the temperature is raised to 275-280° C., polycondensation is continued for 1-2 hours, and the temperature is lowered to obtain silicon-containing PET; the silicon-containing PET includes the following raw materials, calculated by weight: 60-70 parts of terephthalic acid, 120-150 parts of ethylene glycol, and 10-15 parts of triol-based POSS.

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