Preparation method and application of polyester FDY spinning oil

By preparing an optimized oil-based polyester FDY spinning oil agent, the problems of poor hygroscopicity, poor antistatic properties and high moisture content in the polyester FDY spinning process are solved, and an efficient and environmentally friendly spinning process is achieved, improving the spinability and finished product quality of the fibers.

CN119777035AActive Publication Date: 2025-04-08JIANGSU RUIYANG ANTAI NEW MATERIAL TECH CO LTD
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Patent Information

Application Number
CN202510281200.7
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-03-11
Publication Date
2025-04-08
Estimated Expiration
2045-03-11

AI Technical Summary

Technical Problem

In the existing polyester FDY spinning process, the fiber has poor hygroscopicity and poor antistatic properties, and the high water content of traditional emulsion-type oiling agents leads to energy consumption and waste of water resources.

Method used

Oil-based polyester FDY spinning oil agent is prepared using optimized raw material components and proportions, including smoothing agents, emulsifiers, antistatic agents, wetting penetrants and antioxidants, and the performance of spinning oil agents is improved by POSS-derived emulsifiers.

Benefits of technology

It significantly reduces the moisture content of the spinning oil agent, improves the strength of the oil film and antistatic properties, improves the spinningability and finished product quality of the fibers, and reduces energy consumption and waste of water resources.

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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 the smoothing agent and the emulsifier into a reaction kettle, heating to 50-70 DEG C, and stirring for 1-2 hours; adding an antistatic agent and water, and fully stirring for 0.5-1 hour; adding the wetting penetrant and the antioxidant, and uniformly stirring and mixing; cooling to room temperature, and filtering to obtain the polyester FDY spinning oil; the polyester FDY spinning oil agent comprises the following raw material components in parts 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 penetrant, 0.3-2 parts of an antioxidant and 5-10 parts of water. According to the scheme, the oil-based oiling agent is prepared, so that the oil film strength of the polyester FDY spinning oil agent is effectively enhanced; and the efficiency and the product quality of the polyester FDY spinning process are further improved.
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Description

Technical Field

[0001] The invention relates to the technical field of spinning oils, in particular to a preparation method of a polyester FDY spinning oil and application thereof. Background Art

[0002] In my country's chemical fiber industry, polyester production 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 is a continuous fiber, a fully drawn fiber with high strength and high modulus. Its compact structure makes it suitable for woven products and fabrics, and its application is very wide.

[0003] At present, the preparation method of polyester FDY is mainly a one-step spinning and stretching method that combines high-speed spinning (spinning speed is generally 2600~3500m / min) and ultra-high-speed stretching and winding (speed is generally 5100~5500m / min). Compared with the traditional low-speed spinning combined with high-speed stretching and winding process, this method has the advantages of low cost and stable product quality. However, since synthetic fibers do not have the natural colloid and oil film that natural fiber ropes have, they have the disadvantages of poor hygroscopicity and poor antistatic performance; as a result, they are prone to antistatic properties due to continuous friction during the spinning process, and additives must be used to inhibit or eliminate static electricity accumulation, while giving the fiber softness, smoothness and other characteristics, so that it can pass through the subsequent processes smoothly. The additives used in the process are generally spinning oils. In general processes, the spinning process of polyester FDY generally has high speed and high friction, and has extremely high requirements on the quality and performance of the spinning oil; and during the stretching deformation process, the temperature of the polyester filament can reach about 200°C, so the spinning oil needs to have good high temperature resistance and oxidation resistance to improve the smoke and coking phenomenon. In addition, in the spinning industry, the traditional manufacturing process of polyester FDY mainly relies on emulsion oiling agents, and its high water content brings about energy consumption and water resource waste in the spinning process.

[0004] In summary, solving the above problems, preparing a polyester FDY spinning oil, and using it to prepare polyester FDY to improve spinnability are of great significance. Summary of the invention

[0005] The object of the present invention is to provide a preparation method of polyester FDY spinning oil and its application, so as to solve the problems raised in the above background technology.

[0006] In order to solve the above technical problems, the present invention provides the following technical solutions: A method for preparing a polyester FDY spinning oil comprises the following steps: 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.

[0007] 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.

[0008] 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; 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.

[0009] 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.

[0010] 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.

[0011] 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.

[0012] More optimally, the emulsifier comprises the following raw materials: by mass, 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.

[0013] More optimally, the preparation method of the POSS derived emulsifier is: Step 1: under an inert gas atmosphere, add POSS heptaisobutyltrisilanol and triethylamine to tetrahydrofuran in sequence, add chlorodimethylsilane dropwise under an ice bath, and stir for 1 to 1.5 hours; stir at room temperature for 2 to 3 hours, add water; and post-treat to obtain POSS heptaisobutyltrisilane; Step 2: Under an inert gas atmosphere, POSS heptaisobutyl trisilyl, 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.

[0014] More optimally, the raw materials of the POSS heptaisobutyl trisilane include the following substances: by mass, 5 parts of POSS heptaisobutyl trisilane, 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 include the following substances: by mass, 5 parts of POSS heptaisobutyl trisilane, 6-7 parts of modified allyl polyethylene glycol methyl ether, 0.001-0.002 parts of platinum catalyst, and 10-15 parts of tetrahydrofuran.

[0015] More optimally, the preparation method of the 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., the reaction is stirred for 6 to 8 hours, and post-treatment is performed 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-treatment is performed 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 to 0.2.

[0016] In a further scheme, a polyester FDY spinning oil agent is used, and the application process is: PET raw material is directly spun, the feed temperature is 270~290℃, 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℃, and the second hot roller temperature is 150~200℃.

[0017] In a more optimized embodiment, 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; 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, and 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, by weight: 60~70 parts of terephthalic acid, 120~150 parts of ethylene glycol, and 10~15 parts of triol-based POSS.

[0018] Compared with the prior art, the beneficial effects achieved by the present invention are: (1) In the present application, an oil-based polyester FDY spinning oil is prepared by optimizing the raw material components and proportions; compared with the common emulsion-type oiling agent, the water content is greatly reduced to about 10%, and the effective concentration is significantly improved.

[0019] (2) In this application, due to the high viscosity of the oil-based oiling agent, the wetting, spreading and penetration ability on the surface of the fiber filaments are limited during the spinning process, which will cause some problems in the spun polyester FDY, affecting the performance of the fiber filaments and the quality of the final product. Therefore, in the scheme, based on the incompletely condensed POSS heptaisobutyl trisilanol, two grafting modifications are performed to obtain an amphiphilic POSS derivative emulsifier, which effectively improves the shortcomings and improves the performance of the polyester FDY spinning oil.

[0020] Among them, the POSS derived emulsifier is prepared by first utilizing the reaction of chlorine and silanol to graft chlorodimethylsilane on POSS heptaisobutyltrisilanol to introduce silicon hydrogen; then utilizing the reaction of silicon hydrogen and alkenyl to graft modified allyl polyethylene glycol methyl ether; and the grafted modified allyl polyethylene glycol methyl ether is based on aminopolyethylene glycol methyl ether, utilizing the reaction of amino group and epoxy group to graft allyl glycidyl ether so that it has reactive alkenyl group; and further utilizing the reaction of amino group and epoxy group to generate hydroxyl group to react with 3-chloro-2-hydroxypropyltrimethylammonium chloride to graft so that it contains quaternary ammonium salt group.

[0021] Among them, the introduction of POSS-derived emulsifiers effectively improves the high temperature resistance and oxidation resistance of FDY spinning oil, and has low viscosity, high storage stability, excellent wet spreadability; it has good emulsion stability, can effectively improve the oil film strength; it can increase antistatic properties. Thereby further improving the efficiency and product quality of polyester FDY spinning process; in addition, from the perspective of environmental sustainability, the characteristics of low energy consumption and water saving will have a positive impact on the green development of the textile industry. It should be noted that: POSS-derived emulsifiers need to be optimized, and excessive introduction is not conducive to stability and oil film strength.

[0022] (3) In the scheme, polyester FDY spinning oil is used to prepare polyester FDY, the spinning parameters are optimized, the applicability of the oiling agent to spinning is effectively improved, and the spinning efficiency is increased. At the same time, in a further scheme, silicon-containing PET is introduced into the PET raw material, mainly the modified alcohol-based POSS obtained by grafting 1-pyridinepentenol with POSS heptaisobutyltrisilyl; the introduction of this substance can effectively improve the mechanical properties of polyester FDY; at the same time, the addition of siloxane and pyridine groups can promote charge transfer, improve antistatic properties, reduce static electricity generation during spinning, and improve spinnability. In addition, since the introduced modified alcohol-based POSS has affinity with the spinning solution, it can promote the spreading of the oiling agent on the filament, increase the oiling property, and improve the spinning performance. DETAILED DESCRIPTION

[0023] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0024] It should be noted that the following parts are calculated by weight, and the purchase manufacturers of all raw materials involved in the present invention include without any special restrictions: in the following embodiments, the antioxidant is 2246 antioxidant, the fatty acid polyoxyethylene ether is AE0-3, the anhydrous 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, and the isomeric tridecanol polyoxyethylene ether is 1303, the alkyl polyglycoside is APG0810, the alkyl alcohol block polyether is EFS-630, the castor oil polyoxyethylene ether is EL-10, the synthetic ester is PANESTER8116, the copolyether is EO / PO random copolyether, and the industrial white oil is No. 5 white oil; the CAS number of POSS heptaisobutyl trisilanol is 307531-92-6; the CAS number of chlorodimethylsilane is 1066-35-9; the molecular weight of aminopolyethylene glycol methyl ether is 1K; the above and other raw materials involved are commercially purchased.

[0025] Preparation of POSS-derived emulsifier: Step 1: (1) Under a nitrogen atmosphere, aminopolyethylene glycol methyl ether and allyl glycidyl ether in a molar ratio of 1.2:1 are added to tetrahydrofuran in sequence, the temperature is set to 58°C and stirred for reaction for 8 hours, and post-treated to obtain allyl polyethylene glycol methyl ether; (2) 10 parts of allyl polyethylene glycol methyl ether are added to 2wt% alkali solution, 1.6 parts of 3-chloro-2-hydroxypropyltrimethylammonium chloride are added, and the pH is adjusted to 10.2; the reaction is stirred at room temperature for 10 hours, the pH is adjusted to 7, and post-treated to obtain modified allyl polyethylene glycol methyl ether; Step 2: under nitrogen atmosphere, 5 parts of POSS heptaisobutyltrisilanol and 7.6 parts of triethylamine were added to 20 parts of tetrahydrofuran in sequence, and 0.83 parts of chlorodimethylsilane were added dropwise under ice bath, and stirred for 1.5 hours; stirred at room temperature for 2 hours, and water was added to quench the reaction; post-treatment was performed to obtain POSS heptaisobutyltrisilane; Step 3: Under nitrogen atmosphere, 5 parts of POSS heptaisobutyl trisilane, 6.9 parts of modified allyl polyethylene glycol methyl ether, and 0.002 parts of platinum catalyst were added to 12 parts of tetrahydrofuran in sequence, refluxed for 6 hours, and post-treated to obtain a POSS-derived emulsifier.

[0026] Preparation of the PET raw material: (1) under nitrogen atmosphere, POSS heptaisobutyl trisilane and 1-pyridine pentenol in a mass ratio of 5:4.6 are added to tetrahydrofuran, a platinum catalyst is added, and reflux reaction is carried out for 6 hours to obtain modified alcohol-based POSS; (2) 25 parts of terephthalic acid and 55 parts of ethylene glycol are mixed evenly, and the temperature is set to 265° C. under vacuum, 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; (3) 25 parts of terephthalic acid and 55 parts of ethylene glycol were mixed evenly, and the temperature was set to 265°C under vacuum for pre-reaction for 1.5 hours; 40 parts of terephthalic acid and 75 parts of ethylene glycol were added, the temperature was raised to 275°C, the condensation was continued for 2 hours, and the temperature was lowered to obtain unmodified PET; (4) the silicon-containing PET and the unmodified PET were mixed evenly in a mass ratio of 1:1 to obtain a PET raw material.

[0027] Embodiment 1: A method for preparing a polyester FDY spinning oil, comprising the following steps: Step 1: (1) 30 parts of synthetic ester, 5 parts of copolyether and 5 parts of industrial white oil are mixed evenly to obtain a lubricant; (2) 10 parts of POSS derivative 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; Step 2: Add 40 parts of smoothing agent and 35 parts of emulsifier into the reactor, heat to 60°C and stir for 2 hours; add 3 parts of antistatic agent and 10 parts of water, stir for 0.5 hours; add 10 parts of wetting penetrant and 2 parts of antioxidant, stir and mix evenly; cool to room temperature, filter, and obtain polyester FDY spinning oil; Step 3: Directly spin the PET raw material with the assistance of polyester FDY spinning oil. During the process, the feed temperature is 285°C, the spinning rate is 3200m / min, the oiling method is nozzle oiling, the stretching and winding rate is 5300m / min, the first hot roller temperature is 120°C, and the second hot roller temperature is 180°C.

[0028] Embodiment 2: A method for preparing a polyester FDY spinning oil, comprising the following steps: Step 1: (1) 30 parts of synthetic ester, 5 parts of copolyether and 5 parts of industrial white oil are mixed evenly to obtain a lubricant; (2) 8 parts of POSS derivative 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 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; Step 2: Add 40 parts of smoothing agent and 35 parts of emulsifier into the reactor, heat to 60°C and stir for 2 hours; add 3 parts of antistatic agent and 10 parts of water, stir for 0.5 hours; add 10 parts of wetting penetrant and 2 parts of antioxidant, stir and mix evenly; cool to room temperature, filter, and obtain polyester FDY spinning oil; Step 3: Directly spin the PET raw material with the assistance of polyester FDY spinning oil. During the process, the feed temperature is 285°C, the spinning rate is 3200m / min, the oiling method is nozzle oiling, the stretching and winding rate is 5300m / min, the first hot roller temperature is 120°C, and the second hot roller temperature is 180°C.

[0029] Embodiment 3: A method for preparing a polyester FDY spinning oil, comprising the following steps: Step 1: (1) 30 parts of synthetic ester, 5 parts of copolyether and 5 parts of industrial white oil are mixed evenly to obtain a lubricant; (2) 12 parts of POSS derivative 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 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; Step 2: Add 40 parts of smoothing agent and 35 parts of emulsifier into the reactor, heat to 60°C and stir for 2 hours; add 3 parts of antistatic agent and 10 parts of water, stir for 0.5 hours; add 10 parts of wetting penetrant and 2 parts of antioxidant, stir and mix evenly; cool to room temperature, filter, and obtain polyester FDY spinning oil; Step 3: Directly spin the PET raw material with the assistance of polyester FDY spinning oil. During the process, the feed temperature is 285°C, the spinning rate is 3200m / min, the oiling method is nozzle oiling, the stretching and winding rate is 5300m / min, the first hot roller temperature is 120°C, and the second hot roller temperature is 180°C.

[0030] Comparative Example 1: Based on Example 1, no POSS-derived emulsifier was introduced, and the rest was the same as Example 1, specifically as follows: Step 1: (1) 30 parts of synthetic ester, 5 parts of copolyether and 5 parts of industrial white oil are mixed evenly to obtain a lubricant; (2) 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 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; Step 2: Add 40 parts of smoothing agent and 35 parts of emulsifier into the reactor, heat to 60°C and stir for 2 hours; add 3 parts of antistatic agent and 10 parts of water, stir for 0.5 hours; add 10 parts of wetting penetrant and 2 parts of antioxidant, stir and mix evenly; cool to room temperature, filter, and obtain polyester FDY spinning oil; Step 3: Directly spin the PET raw material with the assistance of polyester FDY spinning oil. During the process, the feed temperature is 285°C, the spinning rate is 3200m / min, the oiling method is nozzle oiling, the stretching and winding rate is 5300m / min, the first hot roller temperature is 120°C, and the second hot roller temperature is 180°C.

[0031] Comparative Example 2: Based on Example 1, POSS derivative emulsifier was prepared by grafting with allyl polyethylene glycol methyl ether, and the rest was the same as Example 1; the specific difference steps were as follows: Step 1: under a nitrogen atmosphere, aminopolyethylene glycol methyl ether and allyl glycidyl ether in a molar ratio of 1.2:1 were added to tetrahydrofuran in sequence, the temperature was set to 58° C., stirred and reacted for 8 hours, and post-treated to obtain allyl polyethylene glycol methyl ether; Step 2: under nitrogen atmosphere, 5 parts of POSS heptaisobutyltrisilanol and 7.6 parts of triethylamine were added to 20 parts of tetrahydrofuran in sequence, and 0.83 parts of chlorodimethylsilane were added dropwise under ice bath, and stirred for 1.5 hours; stirred at room temperature for 2 hours, and water was added to quench the reaction; post-treatment was performed to obtain POSS heptaisobutyltrisilane; Step 3: Under a nitrogen atmosphere, 5 parts of POSS heptaisobutyl trisilane, 6.5 parts of allyl polyethylene glycol methyl ether, and 0.002 parts of a platinum catalyst were sequentially added to 12 parts of tetrahydrofuran, refluxed for 6 hours, and post-treated to obtain a POSS-derived emulsifier.

[0032] Comparative Example 3: Based on Example 1, the amount of POSS derived emulsifier introduced was increased, and the rest was the same as Example 1; specifically as follows: Step 1: (1) 30 parts of synthetic ester, 5 parts of copolyether and 5 parts of industrial white oil are mixed evenly to obtain a lubricant; (2) 17 parts of POSS derivative 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 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; Step 2: Add 40 parts of smoothing agent and 35 parts of emulsifier into the reactor, heat to 60°C and stir for 2 hours; add 3 parts of antistatic agent and 10 parts of water, stir for 0.5 hours; add 10 parts of wetting penetrant and 2 parts of antioxidant, stir and mix evenly; cool to room temperature, filter, and obtain polyester FDY spinning oil; Step 3: Directly spin the PET raw material with the assistance of polyester FDY spinning oil. During the process, the feed temperature is 285°C, the spinning rate is 3200m / min, the oiling method is nozzle oiling, the stretching and winding rate is 5300m / min, the first hot roller temperature is 120°C, and the second hot roller temperature is 180°C.

[0033] Comparative Example 4: Based on Example 1, in the direct spinning process, unmodified PET is used as the PET raw material, and silicon-containing PET is not introduced; the rest is the same as Example 1; the specific difference steps are as follows: Unmodified PET was directly spun with the assistance of polyester FDY spinning oil. During the process, the feed temperature was 285°C, the spinning rate was 3200m / min, the oiling method was nozzle oiling, the stretching and winding rate was 5300m / min, the first hot roller temperature was 120°C, and the second hot roller temperature was 180°C.

[0034] Performance test 1: The polyester FDY spinning oil prepared in Example 1 was subjected to basic performance test.

[0035] Results: (1) Appearance: light yellow to colorless transparent liquid; (2) Emulsion stability (15% aq, standing for 72h): stable; (3) Effective content: 90%; (4) pH (1% aq): 7.5; (5) Oil film strength / N: 1268 (tested in accordance with GB / T3142); (6) Surface tension (1% aqueous solution, 25℃, mN / m): 29; (7) Conductivity (μs / cm): 1187; (8) Viscosity (25℃, mPa·s): 40.6; (9) No smoke; (10) No coking.

[0036] Performance Test 2: The polyester FDY spinning oil prepared in Example 1 and Comparative Examples 1-2 were compared for related performance; the antistatic property was characterized by using an electrostatic meter to obtain the dynamic voltage value under high-speed winding; the heat resistance was characterized by using a laser dust particle technology instrument to record the number of smoke particles at the second hot roller of the spinning hot box. The obtained data are shown in Table 1:

[0037] Conclusion: The data in Table 1 show that the polyester FDY spinning oil prepared in the present application has excellent antistatic and heat resistance; the data in Comparative Examples 1 and 2 show that in Comparative Example 1, no POSS-derived emulsifier is introduced, which significantly reduces the antistatic and heat resistance; in Comparative Example 2, since the POSS-derived emulsifier is prepared by grafting allyl polyethylene glycol methyl ether, no quaternary ammonium salt segment is introduced, which slightly reduces the performance.

[0038] Performance Test 3: The relevant performances of Example 1 and Comparative Examples 3-4 were compared, and the full roll rate in the spinning process was recorded to characterize the spinnable performance; and the breaking strength and the unevenness of the yarn obtained by spinning of the polyester FDY were detected to detect the finished product quality of the spun fiber; wherein, the breaking strength was tested with reference to the test method for tensile properties of filaments in GB / T14344-2022, and the test was carried out with a fully automatic single yarn strength machine, and the breaking strength was calculated according to Part 8.2; the unevenness of the yarn was tested with a yarn uniformity meter, with a sample of 200m, a speed of 500m / min, and a frequency of 2000Hz; the obtained data are shown in Table 2:

[0039] Conclusion: The data in the above table show that the polyester FDY spinning oil prepared in this application has excellent spinnability and finished product quality, and has excellent applicability. The data of Comparative Examples 3 and 4 show that in Comparative Example 3, the amount of POSS-derived emulsifier introduced reduces the stability and smoothness, thereby reducing the full roll rate and the unevenness of the yarn; in Comparative Example 4, since unmodified PET is used as the PET raw material and silicon-containing PET is not introduced, the affinity of the oil is reduced, and the full roll rate is slightly reduced; but since there is no silicon-containing material, the mechanical properties of the fiber are reduced.

[0040] Finally, it should be noted that the above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art can still modify the technical solutions described in the aforementioned embodiments or replace some of the technical features therein by equivalents. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention shall be included in 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 trisilyl; Step 2: Under an inert gas atmosphere, POSS heptaisobutyl trisilyl, quaternary ammonium salt-modified allyl polyethylene glycol methyl ether, and platinum catalyst are added to tetrahydrofuran in sequence, refluxed for 5 to 7 hours, and post-treated to obtain a POSS-derived emulsifier.

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 following substances are included: by mass: 5 parts of POSS heptaisobutyltrisilanol, 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 include the following substances: by mass, 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 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., stirring and reacting for 6 to 8 hours, post-treating 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; stirring and reacting at room temperature for 8 to 12 hours, adjusting the pH to 6.5 to 7, post-treating to obtain quaternary ammonium salt 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 to 0.

2.

6. An application of a polyester FDY spinning oil, characterized in that: The polyester FDY spinning oil according to any one of claims 1 to 5 is used to prepare polyester FDY; the application process is: directly spinning the PET raw material, the feed temperature is 270-290°C, the spinning rate is 3000-3500 m / min, the oiling method is nozzle oiling, the stretching and winding rate is 5100-5500 m / 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.

Citation Information

Patent Citations

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