Spandex spinning oil and preparation method thereof

Abstract

The present invention relates to the technical field of spandex spinning oils, and more specifically to a spandex spinning oil and a preparation method thereof. The spinning oil comprises polyether-modified silicone oil, liquid paraffin, a conditioning agent, an anti-blocking agent, a dispersant, and an antistatic agent. The preparation method comprises: adding the polyether-modified silicone oil and conditioning agent to a reactor and mixing them uniformly; then adding the liquid paraffin, anti-blocking agent, dispersant, and antistatic agent; heating and stirring; and continuing stirring for a period of time until the color of the system changes from a white milky state to a colorless, transparent liquid. After the liquid cools, a colorless, transparent liquid is obtained, which is the spinning oil. The spinning oil can impart excellent antistatic properties, smoothness, bundling properties, and unwinding properties to spandex yarns, effectively resolving problems such as adhesion, edge collapse, and yarn breakage during the spandex spinning process.

Description

Technical Field

[0001] The invention relates to a spandex spinning oil and a preparation method thereof, belonging to the technical field of spandex spinning oils. Background Art

[0002] Polyurethane fiber, also known as spandex, is a type of elastic fiber. Spandex has excellent elasticity, allowing it to be stretched to 5 to 8 times its original length. It also quickly returns to its original shape after the force is released, with a resilience of up to 90%. This means it retains its shape and function even after repeated stretching and compression.

[0003] Spandex offers excellent comfort. Its soft feel makes it incredibly comfortable to wear, contouring to the body for a comfortable, non-compressive fit. Its lightweight construction also adds no extra weight. Spandex also boasts excellent durability and abrasion resistance, allowing it to withstand prolonged use without wear and tear. It also exhibits excellent acid and alkali resistance and anti-aging properties. Due to its numerous advantages, spandex has been actively developed in the textile industry, primarily for use in swimwear, sportswear, tights, and stretch pants.

[0004] Spandex molecules contain both soft and hard segments, allowing them to relax (bend and curl) when unstressed, giving spandex a certain elasticity. However, spandex yarns are prone to sticking, so lubricants are crucial in the spandex spinning process. A good lubricant ensures smoothness and bundling during the spinning process, making unwinding easier, preventing edge collapse, and minimizing bottom breakage during later use. It also imparts excellent antistatic properties to the spandex yarns.

[0005] In recent years, spandex finishing agents have developed rapidly, achieving large-scale production. However, some problems still exist in the spandex spinning process. For example, patent application publication number US3717575A discloses a spandex finishing agent composed of mineral oil, silicone oil, and amino-modified silicone oil. This finishing agent is characterized by a smooth and pleasant hand feel for the spun spandex yarn, but poor antistatic properties. Patent publication number CN111206422B discloses a dry-process antistatic spandex spinning finishing agent and its preparation method. The finishing agent comprises a composite high-temperature smoothing agent, a composite antistatic agent, a phenolic antioxidant, an aniline antioxidant, an olefinic antioxidant, a high-temperature dispersant, a softener, an environmentally friendly emulsifier, a metal stearate, a preservative, and a defoaming agent. While this finishing agent exhibits excellent antistatic properties, it suffers from poor bundling and unwinding properties. Therefore, developing a high-quality finishing agent that enhances spandex yarn antistatic properties, smoothness, bundling, and unwinding properties is of great value. Summary of the Invention

[0006] In view of the deficiencies in the prior art, the present invention provides a spandex spinning oil and a preparation method thereof. The spinning oil can make the spandex yarn have good antistatic properties, smoothness, bundling properties and unwinding properties, and can well solve the problems of adhesion, edge collapse and yarn breakage in the spandex spinning process.

[0007] The technical solution of the present invention to solve the above technical problems is as follows: a spandex spinning oil, the spinning oil comprising polyether-modified silicone oil, liquid paraffin, a regulator, an anti-blocking agent, a dispersant and an antistatic agent;

[0008] The structural formula of the polyether modified silicone oil is as follows:

[0009] ;

[0010] Wherein, m, n, a, and b are natural numbers greater than 0, and the kinematic viscosity of the polyether-modified silicone oil is 20-100 cp;

[0011] R1 is selected from 、 Any one of: R2 is selected from any one of -H, -CH3.

[0012] On the basis of the above technical solution, the present invention can also be improved as follows:

[0013] Furthermore, the spinning oil comprises, by weight, 35-50 parts of polyether-modified silicone oil, 30-45 parts of liquid paraffin, 2-10 parts of a regulator, 0.1-3 parts of an anti-blocking agent, 0.1-5 parts of a dispersant, and 1-10 parts of an antistatic agent.

[0014] Furthermore, in the structural formula of the polyether-modified silicone oil, 50≤m≤250, 30≤n≤300, 20≤a≤100, and 25≤b≤120.

[0015] Furthermore, the kinematic viscosity of the liquid paraffin is 20-50 cp; and the regulator is stearic acid alcohol.

[0016] Furthermore, the anti-adhesion agent is at least one of oleamide, cellulose acetate, and polyvinyl alcohol;

[0017] The dispersant is at least one of polyoxyethylene fatty acid ester and castor oil polyoxyethylene ether.

[0018] Furthermore, the structural formula of the antistatic agent is as follows:

[0019] ;

[0020] R is selected from any one of -H, -CH3, -CH2CH3, and -CH=CH2, and c is a natural number and 20≤c≤50.

[0021] The present invention also discloses a method for preparing a spandex spinning oil, which comprises:

[0022] Add polyether-modified silicone oil and a regulator into a reactor and mix them evenly; then add liquid paraffin, an anti-blocking agent, a dispersant, and an antistatic agent, heat and stir, and continue stirring for a period of time after the color of the system changes from a white milky state to a colorless transparent liquid. After the liquid cools, a colorless transparent liquid is obtained, which is the spinning oil.

[0023] On the basis of the above technical solution, the present invention can also be improved as follows:

[0024] Furthermore, the heating temperature is 90-100° C.; and the stirring speed is 2000-2500 rpm.

[0025] Furthermore, the preparation method of the polyether-modified silicone oil is:

[0026] Under inert gas conditions, hydrogen-containing silicone oil and polyether modifier are heated to react in the presence of a catalyst, and after the reaction is completed, polyether-modified silicone oil is obtained through post-processing and purification;

[0027] The polyether modifier is at least one selected from allyl polyoxyethylene polyoxypropylene ether, methyl allyl polyoxyethylene ether, and allyl polyoxyethylene methyl ether.

[0028] Furthermore, the molar ratio of Si-H in the hydrogenated silicone oil to C=C in the polyether modifier is 1:(1.0-1.4).

[0029] Furthermore, the catalyst is any one of a Speier catalyst and a Karstedt catalyst.

[0030] Furthermore, the heating reaction temperature is 90-130° C., and the reaction time is 6-10 h.

[0031] The beneficial effects of the present invention are:

[0032] In the spinning oil of the present invention, high-branched segment polyether-modified silicone oil is used instead of dimethyl silicone oil and low-branched segment polyether-modified silicone oil, which not only has better lubricity and better temperature resistance, but also prevents turbidity during the preparation process. The spinning oil can make the spandex yarn have good antistatic properties, smoothness, bundling properties, and unwinding properties, and can effectively solve the problems of adhesion, edge collapse, and yarn breakage in the spandex spinning process.

[0033] More specifically, the spinning oil described herein uses a diammonium salt-terminated organic linear silicone polymer as an antistatic agent, effectively forming a conductive permeable network to prevent static electricity accumulation, significantly enhancing the oil's antistatic properties. Oleamide, cellulose acetate, and polyvinyl alcohol are also used as anti-blocking agents, which complement the highly branched polyether-modified silicone oil to enhance anti-sticking properties, preventing sticking of spandex yarns.

[0034] The present invention performs appropriate polyether modification on hydrogenated silicone oil, so that when the polyether-modified silicone oil is used in a spinning oil, the spinning oil has appropriate viscosity, and oiling of spandex is more conducive to obtaining spandex with excellent performance. DETAILED DESCRIPTION

[0035] The present invention can be implemented in many other ways than those described herein, and those skilled in the art can make similar improvements without violating the scope of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed.

[0036] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art to which the present invention belongs. The terms used are only for describing specific embodiments and are not intended to limit the present invention.

[0037] A spandex spinning oil, comprising polyether-modified silicone oil, liquid paraffin, a conditioning agent, an anti-blocking agent, a dispersant, and an antistatic agent;

[0038] The structural formula of the polyether modified silicone oil is as follows:

[0039] ;

[0040] Wherein, m, n, a, and b are natural numbers greater than 0, and the kinematic viscosity of the polyether-modified silicone oil is 20-100 cp (25° C.);

[0041] R1 is selected from 、 Any one of: R2 is selected from any one of -H, -CH3.

[0042] Specifically, in parts by weight, the spinning oil includes 35-50 parts of polyether modified silicone oil, 30-45 parts of liquid paraffin, 2-10 parts of a regulator, 0.1-3 parts of an anti-blocking agent, 0.1-5 parts of a dispersant, and 1-10 parts of an antistatic agent.

[0043] Specifically, in the structural formula of the polyether-modified silicone oil, 50≤m≤250, 30≤n≤300, 20≤a≤100, and 25≤b≤120.

[0044] Specifically, the kinematic viscosity of the liquid paraffin is 20-50 cp (25° C.); and the regulator is stearic acid alcohol.

[0045] Specifically, the anti-adhesion agent is at least one of oleamide, cellulose acetate, and polyvinyl alcohol;

[0046] The dispersant is at least one of polyoxyethylene fatty acid ester and castor oil polyoxyethylene ether.

[0047] Specifically, the structural formula of the antistatic agent is as follows:

[0048] ;

[0049] R is selected from any one of -H, -CH3, -CH2CH3, and -CH=CH2, and c is a natural number and 20≤c≤50.

[0050] More specifically, the antistatic agent used in the embodiments of the present invention is POLYA AT purchased from Weihai Nuowei Xinhe New Materials Co., Ltd.

[0051] A method for preparing a spandex spinning oil, comprising:

[0052] Add polyether-modified silicone oil and a regulator into a reactor and mix them evenly; then add liquid paraffin, an anti-blocking agent, a dispersant, and an antistatic agent, heat and stir, and continue stirring for a period of time after the color of the system changes from a white milky state to a colorless transparent liquid. After the liquid cools, a colorless transparent liquid is obtained, which is the spinning oil.

[0053] Specifically, the heating temperature is 90-100° C.; and the stirring speed is 2000-2500 rpm.

[0054] Specifically, the preparation method of the polyether-modified silicone oil is:

[0055] Under inert gas conditions, hydrogen-containing silicone oil and polyether modifier are heated to react in the presence of a catalyst, and after the reaction is completed, polyether-modified silicone oil is obtained through post-processing and purification;

[0056] The polyether modifier is at least one selected from allyl polyoxyethylene polyoxypropylene ether, methyl allyl polyoxyethylene ether, and allyl polyoxyethylene methyl ether.

[0057] Specifically, the molar ratio of Si-H in the hydrogenated silicone oil to C=C in the polyether modifier is 1:(1.0-1.4).

[0058] Specifically, the catalyst is any one of a Speier catalyst and a Karstedt catalyst.

[0059] More specifically, the amount of the catalyst added to the system is 5-25 ppm (calculated based on the total mass of the hydrogen-containing silicone oil).

[0060] Specifically, the heating reaction temperature is 90-130° C., and the reaction time is 6-10 hours.

[0061] More specifically, the post-treatment purification method is as follows: after the reaction is completed, low-boiling substances are distilled off at 60°C and 0.099 MPa, and then unreacted silicon-hydrogen bonds in the system are removed at 250°C and 0.099 MPa to obtain a light yellow transparent viscous liquid, which is the polyether-modified silicone oil. The vinyl conversion rate is measured by iodine titration to be 85-90%.

[0062] Example 1

[0063] (1) Preparation of polyether modified silicone oil:

[0064] A mechanical stirrer, a three-way connector (for connecting to a nitrogen cylinder), and a thermometer were placed on the stand of a 1 L three-necked jacketed reactor.

[0065] To a reactor, add 25g of hydrogenated silicone oil (SH-18, Jiangsu Keqi Polymer Materials Co., Ltd.) and 18g of allyl polyoxyethylene polyoxypropylene ether (F-6, Jiangsu Hai'an Petrochemical Plant). Simultaneously, add 10ppm of chloroplatinic acid. After addition, evacuate the system to remove air. The molar ratio of Si-H in the hydrogenated silicone oil to C=C in the polyether modifier is 1:1.0.

[0066] The reaction system was heated to 100°C and reacted for 8 hours.

[0067] After the reaction, the product was subjected to rotary evaporation (60°C, 0.099 MPa) to remove low-boiling substances, and then subjected to high-temperature rotary evaporation (250°C, 0.099 MPa) to remove unreacted silicon-hydrogen bonds to obtain a light yellow, transparent, viscous liquid. The vinyl conversion rate was measured by iodine titration to be 86.74%, which was polyether-modified silicone oil.

[0068] (2) Preparation of spinning oil:

[0069] According to parts by weight, 2 parts of stearic acid alcohol (ST-18 Jiangsu Shengtai Chemical Technology Co., Ltd.) and 50 parts of polyether-modified silicone oil were added to a three-necked jacketed reactor and stirred to mix evenly.

[0070] Then, add 0.5 parts of oleic acid amide, 1 part of castor oil polyoxyethylene ether (HMEL-10 Zhejiang Huangma Technology Co., Ltd.), 10 parts of POLYA AT-1, and 36.5 parts of liquid paraffin (5# China Petrochemical Group Beijing Yanshan Petrochemical Co., Ltd.), turn on the stirring speed to 2500 r / min, heat to 90°C, and react for 2 hours.

[0071] The color changes from white milky to colorless transparent liquid. Continue stirring for 2 hours. Pour out the liquid after it cools down. The appearance is colorless transparent liquid, which is spandex spinning oil.

[0072] Example 2

[0073] (1) Preparation of polyether modified silicone oil:

[0074] A mechanical stirrer, a three-way connector (for connecting a nitrogen cylinder) and a thermometer were placed on the stand of a 1 L three-necked jacketed reactor.

[0075] 25g of hydrogenated silicone oil and 18g of allyl polyoxyethylene polyoxypropylene ether were added to a three-mouth reaction kettle, and 10ppm of chloroplatinic acid was added at the same time. After the addition, the system was ventilated to make it air-free. The molar ratio of Si-H in the hydrogenated silicone oil to C=C in the polyether modifier was 1:1.0.

[0076] The reaction system was heated to 100°C and reacted for 8 hours.

[0077] After the reaction, the product was subjected to rotary evaporation (60°C, 0.099 MPa) to remove low-boiling substances, and then subjected to high-temperature rotary evaporation (250°C, 0.099 MPa) to remove unreacted silicon-hydrogen bonds to obtain a light yellow, transparent, viscous liquid. The vinyl conversion rate was measured by iodine titration to be 86.74%, which was polyether-modified silicone oil.

[0078] (2) Preparation of spinning oil:

[0079] According to parts by weight, 10 parts of stearic acid alcohol and 45 parts of polyether modified silicone oil were added to a three-necked jacketed reactor and stirred and mixed uniformly.

[0080] Then, 0.1 parts of oleic acid amide, 5 parts of castor oil polyoxyethylene ether, 1 part of POLYA AT-1, and 38.9 parts of liquid paraffin were added, stirred at 2500 r / min, heated to 90° C., and reacted for 2 hours.

[0081] The color changes from white milky to colorless transparent liquid. Continue stirring for 2 hours. Pour out the liquid after it cools down. The appearance is colorless transparent liquid, which is spandex spinning oil.

[0082] Example 3

[0083] (1) Preparation of polyether modified silicone oil:

[0084] A mechanical stirrer, a three-way connector (for connecting a nitrogen cylinder) and a thermometer were placed on the stand of a 1 L three-necked jacketed reactor.

[0085] 25g of hydrogenated silicone oil and 18g of allyl polyoxyethylene polyoxypropylene ether were added to a three-mouth reaction kettle, and 10ppm of chloroplatinic acid was added at the same time. After the addition, the system was ventilated to make it air-free. The molar ratio of Si-H in the hydrogenated silicone oil to C=C in the polyether modifier was 1:1.0.

[0086] The reaction system was heated to 100°C and reacted for 8 hours.

[0087] After the reaction, the product was subjected to rotary evaporation (60°C, 0.099 MPa) to remove low-boiling substances, and then subjected to high-temperature rotary evaporation (250°C, 0.099 MPa) to remove unreacted silicon-hydrogen bonds to obtain a light yellow, transparent, viscous liquid. The vinyl conversion rate was measured by iodine titration to be 86.74%, which was polyether-modified silicone oil.

[0088] (2) Preparation of spinning oil:

[0089] According to parts by weight, 6.9 parts of stearic acid alcohol and 35 parts of polyether-modified silicone oil were added to a three-necked jacketed reactor and stirred to mix evenly.

[0090] Then, 3 parts of oleamide, 0.1 parts of castor oil polyoxyethylene ether, 10 parts of POLYA AT-1, and 45 parts of liquid paraffin were added, stirred at 2500 r / min, heated to 90° C., and reacted for 2 h.

[0091] The color changes from white milky to colorless transparent liquid. Continue stirring for 2 hours. Pour out the liquid after it cools down. The appearance is colorless transparent liquid, which is spandex spinning oil.

[0092] Example 4

[0093] (1) Preparation of polyether modified silicone oil:

[0094] A mechanical stirrer, a three-way connector (for connecting a nitrogen cylinder) and a thermometer were placed on the stand of a 1 L three-necked jacketed reactor.

[0095] 25g of hydrogenated silicone oil and 18g of allyl polyoxyethylene polyoxypropylene ether were added to a three-mouth reaction kettle, and 10ppm of chloroplatinic acid was added at the same time. After the addition, the system was ventilated to make it air-free. The molar ratio of Si-H in the hydrogenated silicone oil to C=C in the polyether modifier was 1:1.0.

[0096] The reaction system was heated to 100°C and reacted for 8 hours.

[0097] After the reaction, the product was subjected to rotary evaporation (60°C, 0.099 MPa) to remove low-boiling substances, and then subjected to high-temperature rotary evaporation (250°C, 0.099 MPa) to remove unreacted silicon-hydrogen bonds to obtain a light yellow, transparent, viscous liquid. The vinyl conversion rate was measured by iodine titration to be 86.74%, which was polyether-modified silicone oil.

[0098] (2) Preparation of spinning oil:

[0099] According to parts by weight, 5 parts of stearic acid alcohol and 40 parts of polyether-modified silicone oil were added to a three-necked jacketed reactor and stirred to mix evenly.

[0100] Then, 2.5 parts of oleic acid amide, 5 parts of castor oil polyoxyethylene ether, 7.5 parts of POLYA AT-1, and 40 parts of liquid paraffin were added, stirred at 2500 r / min, heated to 90° C., and reacted for 2 h.

[0101] The color changes from white milky to colorless transparent liquid. Continue stirring for 2 hours. Pour out the liquid after it cools down. The appearance is colorless transparent liquid, which is spandex spinning oil.

[0102] Example 5

[0103] (1) Preparation of polyether modified silicone oil:

[0104] A mechanical stirrer, a three-way connector (for connecting a nitrogen cylinder) and a thermometer were placed on the stand of a 1 L three-necked jacketed reactor.

[0105] 25g of hydrogenated silicone oil and 25.2g of methyl allyl polyoxyethylene ether (HPEG, Jiangsu Runfeng Synthetic Technology Co., Ltd.) were added to a three-well reactor, along with 25ppm of Karstedt catalyst. After the addition, the system was ventilated to make it air-free. The molar ratio of Si-H in the hydrogenated silicone oil to C=C in the polyether modifier was 1:1.4.

[0106] The reaction system was heated to 90°C and reacted for 10 h.

[0107] After the reaction is completed, the product is rotary evaporated (60℃, 0.099Mpa) to remove low-boiling substances, and then high-temperature rotary evaporated (250℃, 0.099Mpa) to remove unreacted silicon-hydrogen bonds to obtain a light yellow transparent viscous liquid, which is polyether modified silicone oil.

[0108] (2) Preparation of spinning oil:

[0109] According to parts by weight, 5 parts of stearic acid alcohol and 35 parts of polyether-modified silicone oil were added to a three-necked jacketed reactor and stirred to mix evenly.

[0110] Then add 3 parts of cellulose acetate (240-460-0 Jiangsu Bosite Chemical Co., Ltd.), 5 parts of polyoxyethylene fatty acid ester (PEG-400 Liaoning Kelong Fine Chemical Co., Ltd.), 7 parts of POLYA AT-1, and 45 parts of liquid paraffin, turn on the stirring speed to 2000 r / min, heat to 100°C, and react for 2 hours.

[0111] The color changes from white milky to colorless transparent liquid. Continue stirring for 2 hours. Pour out the liquid after it cools down. The appearance is colorless transparent liquid, which is spandex spinning oil.

[0112] Example 6

[0113] (1) Preparation of polyether modified silicone oil:

[0114] A mechanical stirrer, a three-way connector (for connecting a nitrogen cylinder) and a thermometer were placed on the stand of a 1 L three-necked jacketed reactor.

[0115] In a three-mouth reaction kettle, add 25g of hydrogenated silicone oil and 21.6g of allyloxy polyoxyethylene polyoxypropylene ether, and at the same time add 5ppm of chloroplatinic acid. After the addition, ventilate the system to make it air-free. The molar ratio of Si-H in the hydrogenated silicone oil to C=C in the polyether modifier is 1:1.2.

[0116] The reaction system was heated to 130°C and reacted for 6 hours.

[0117] After the reaction is completed, the product is rotary evaporated (60℃, 0.099Mpa) to remove low-boiling substances, and then high-temperature rotary evaporated (250℃, 0.099Mpa) to remove unreacted silicon-hydrogen bonds to obtain a light yellow transparent viscous liquid, which is polyether modified silicone oil.

[0118] (2) Preparation of spinning oil:

[0119] According to parts by weight, 7 parts of stearic acid alcohol and 45 parts of polyether-modified silicone oil were added to a three-necked jacketed reactor and stirred to mix evenly.

[0120] Then add 0.5 parts of polyvinyl alcohol (PVA17-88 Anhui Wanwei High-tech Materials Co., Ltd.), 1 part of castor oil polyoxyethylene ether, 10 parts of POLYA AT-1, and 36.5 parts of liquid paraffin (5# China Petrochemical Group Beijing Yanshan Petrochemical Co., Ltd.), turn on the stirring speed to 2500r / min, heat to 90℃, and react for 2h.

[0121] The color changes from white milky to colorless transparent liquid. Continue stirring for 2 hours. Pour out the liquid after it cools down. The appearance is colorless transparent liquid, which is spandex spinning oil.

[0122] Comparative Example 1

[0123] The same method as in Example 1 was used to prepare a spandex spinning oil, except that the polyether-modified silicone oil in Example 1 was replaced with dimethyl silicone oil. The specific preparation process was as follows:

[0124] (1) Preparation of polyether modified silicone oil:

[0125] Same as Example 1.

[0126] (2) Preparation of spinning oil:

[0127] According to parts by weight, 2 parts of stearic acid alcohol and 50 parts of dimethyl silicone oil were added to a three-necked jacketed reactor and stirred to mix evenly.

[0128] Then, add 0.5 parts of oleic acid amide, 1 part of castor oil polyoxyethylene ether, 10 parts of POLYA AT-1, and 36.5 parts of liquid paraffin, turn on the stirring speed to 2500 r / min, heat to 90°C, and react for 2 hours.

[0129] The color changes from white milky to colorless transparent liquid and continue stirring for 2 hours. After the liquid cools down, pour it out. The appearance is colorless transparent liquid, which is spandex spinning oil.

[0130] Comparative Example 2

[0131] The same method as in Example 1 was used to prepare a spandex spinning oil, except that the anti-blocking agent oleamide was replaced with magnesium stearate. The specific preparation process was as follows:

[0132] (1) Preparation of polyether modified silicone oil:

[0133] Same as Example 1.

[0134] (2) Preparation of spinning oil:

[0135] According to parts by weight, 2 parts of stearic acid alcohol and 50 parts of polyether-modified silicone oil were added into a three-necked jacketed reactor and stirred to mix evenly.

[0136] Then, 0.5 parts by weight of magnesium stearate, 1 part by weight of castor oil polyoxyethylene ether, 10 parts by weight of POLYA AT-1, and 36.5 parts by weight of liquid paraffin were added, stirred at 2500 r / min, heated to 90° C., and reacted for 2 h.

[0137] The color changes from white milky to colorless transparent liquid and continue stirring for 2 hours. After the liquid cools down, pour it out. The appearance is colorless transparent liquid, which is spandex spinning oil.

[0138] Comparative Example 3

[0139] The same method as in Example 1 was used to prepare a spandex spinning oil, except that the antistatic agent POLYAAT-1 was replaced with potassium fatty alcohol polyoxyethylene ether phosphate (MOA-3Pk-40, Nantong Hengrun New Material Technology Co., Ltd.). The specific preparation process is as follows:

[0140] (1) Preparation of polyether modified silicone oil:

[0141] Same as Example 1.

[0142] (2) Preparation of spinning oil:

[0143] According to parts by weight, 2 parts of stearic acid alcohol and 50 parts of polyether-modified silicone oil were added into a three-necked jacketed reactor and stirred to mix evenly.

[0144] Then add 0.5 parts of oleic acid amide, 1 part of castor oil polyoxyethylene ether, 10 parts of fatty alcohol polyoxyethylene ether potassium phosphate, and 36.5 parts of liquid paraffin, turn on the stirring speed to 2500r / min, heat to 90℃, and react for 2h.

[0145] The color changes from white milky to colorless transparent liquid and continue stirring for 2 hours. After the liquid cools down, pour it out. The appearance is colorless transparent liquid, which is spandex spinning oil.

[0146] Comparative Example 4

[0147] A spandex spinning oil was prepared using the same method as in Example 1, except that in Comparative Example 4, when preparing the polyether-modified silicone oil, the amount of allyl polyoxyethylene polyoxypropylene ether was increased so that the molar ratio of Si—H in the hydrogenated silicone oil to C=C in the polyether modifier was 1:2. The specific preparation process is as follows:

[0148] (1) Preparation of polyether modified silicone oil:

[0149] A mechanical stirrer, a three-way connector (for connecting to a nitrogen cylinder), and a thermometer were placed on the stand of a 1 L three-necked jacketed reactor.

[0150] Add 25g of hydrogenated silicone oil and 36g of allyl polyoxyethylene polyoxypropylene ether to a reactor, along with 10ppm of chloroplatinic acid. After the additions are complete, evacuate the system to remove air. The molar ratio of Si-H in the hydrogenated silicone oil to C=C in the polyether modifier is 1:2.

[0151] The reaction system was heated to 100°C and reacted for 8 hours.

[0152] After the reaction is completed, the product is rotary evaporated (60℃, 0.099Mpa) to remove low-boiling substances, and then high-temperature rotary evaporated (250℃, 0.099Mpa) to remove unreacted silicon-hydrogen bonds to obtain a light yellow transparent viscous liquid, which is polyether modified silicone oil.

[0153] (2) Preparation of spinning oil:

[0154] Same as Example 1.

[0155] Comparative Example 5

[0156] The same method as in Example 1 was used to prepare a spandex spinning oil, except that no anti-blocking agent was added to the spinning oil formulation of Comparative Example 5. The specific preparation process was as follows:

[0157] (1) Preparation of polyether modified silicone oil:

[0158] Same as Example 1.

[0159] (2) Preparation of spinning oil:

[0160] According to parts by weight, 2 parts of stearic acid alcohol and 50.5 parts of polyether-modified silicone oil were added to a three-necked jacketed reactor and stirred to mix evenly.

[0161] Then, add 1 part of castor oil polyoxyethylene ether, 10 parts of POLYA AT-1, and 36.5 parts of liquid paraffin, turn on the stirring speed to 2500 r / min, heat to 90°C, and react for 2 hours.

[0162] The color changes from white milky to colorless transparent liquid. Continue stirring for 2 hours. Pour out the liquid after it cools down. The appearance is colorless transparent liquid, which is spandex spinning oil.

[0163] The spinning oils prepared in the above examples and comparative examples were subjected to performance tests. The specific test results are shown in Table 1 below. The detection methods involved are as follows:

[0164] (1) Viscosity test: Use a rotational viscometer for testing. Model: ChemTron Viscolead (imported from Germany).

[0165] (2) Surface tension test: Use contact angle meter model: OCA 25 (imported from Germany).

[0166] (3) Moisture content test: Use moisture meter model: SFY-20A (Shenzhen Guanya Moisture Meter Instrument Co., Ltd.).

[0167] (4) Resistance test: Use conductivity meter model S470 SevenExcellence (imported from Switzerland)

[0168] Table 1 Spinning oil performance test results

[0169]

[0170] The above-mentioned spinning oils of the embodiment and the comparative example were used to oil the spandex. The spandex used was Taihe Newstar. ® The specific oiling process for 20D spandex is as follows: the spandex passes through two oiling rollers, which rotate in the oil tank and carry the oil on their surfaces. The spandex moves on the surfaces of the two intersecting rollers, contacting the oil on the roller surface, and the oil is applied to the spandex. The performance of the oiled spandex was tested. The specific test results are shown in Table 2 below. The test methods involved are as follows:

[0171] Oil pick-up rate test: The oil pick-up rate tester MQA7020 (Oxford Instruments Technology (Shanghai) Co., Ltd.) was used for testing.

[0172] Breaking strength test: Use a constant rate of elongation tester to test, test standard: FZ / T 50006-1994.

[0173] Elongation at break test: Tested using a constant rate of elongation strength tester, test standard: FZ / T 50006-1994.

[0174] Elastic recovery rate test: Use XN-type elastic strength tester, test standard: FZ / T 50007-2012.

[0175] Unwinding Test: Using an electronic constant tension transmission system, at a specified input speed, the output speed is recorded until the spandex yarn adheres to the surface of the roll. The unwinding performance of the spandex yarn is expressed as output speed / input speed. The smaller the ratio, the better the unwinding performance. Surface unwinding performance refers to the unwinding of the spandex yarn above the middle of the roll, while inner unwinding performance refers to the unwinding of the spandex yarn below the middle of the roll.

[0176] Table 2 Test results of spandex performance after oiling

[0177]

[0178] The data in Tables 1 and 2 above demonstrate that the spin finishes prepared using the methods of the present invention in Examples 1-6 exhibit more suitable viscosity, improved antistatic properties, and lower surface tension, thereby achieving a higher oil uptake rate on spandex. The spandex treated with the spin finishes of the present invention exhibits improved smoothness, higher breaking strength and elongation, and significantly reduces the breakage rate of the spandex yarn. Furthermore, the spandex yarn exhibits reduced stickiness and improved unwinding properties.

[0179] From the comparison of the experimental results of Comparative Example 1 and Example 1, it can be seen that compared with using polyether-modified silicone oil and dimethyl silicone oil in the spinning oil, the oil prepared using polyether-modified silicone oil has lower surface tension, is more conducive to improving the oiling rate, and has higher resistance and better antistatic effect.

[0180] From the comparison of the experimental results of Comparative Example 2 and Example 1, it can be seen that if the anti-blocking agent oleamide is replaced with magnesium stearate, the viscosity of the oil agent is high and the surface tension is high, the oiling rate is low, and the lubrication performance is reduced, the adhesion becomes stronger, and the unwinding property of the spandex yarn becomes worse.

[0181] From the comparison of the experimental results of Comparative Example 3 and Example 1, it can be seen that when the antistatic agent POLYA AT-1 is replaced with potassium fatty alcohol polyoxyethylene ether phosphate, the resistance of the oil becomes larger, the charge accumulates on the silk, and the antistatic performance deteriorates.

[0182] From the comparison of the experimental results of Comparative Example 4 and Example 1, it can be seen that when preparing polyether-modified silicone oil, increasing the usage ratio of allyl polyoxyethylene polyoxypropylene ether will result in an excess of propyl polyoxyethylene polyoxypropylene ether, which will increase the viscosity and surface tension of the oil, making it difficult to apply the oil, and will increase the friction between the spandex yarns, making them prone to breakage.

[0183] From the comparison of the experimental results of Comparative Example 5 and Example 1, it can be seen that if no anti-blocking agent is added to the spinning oil formulation, the lubricating ability of the oil decreases, the unwinding property of the spandex yarn deteriorates, and the edge collapses easily.

[0184] The various technical features of the embodiments can be combined arbitrarily. To make the description concise, not all possible combinations of the various technical features in the above embodiments are exhaustively listed. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0185] For those skilled in the art, several variations and improvements may be made without departing from the scope of the present invention, which all fall within the scope of protection of the present invention. The scope of protection of the present invention shall be based on the appended claims.

Claims

1. A spandex spinning oil, characterized in that: The spinning oil comprises, by weight, 35-50 parts of polyether-modified silicone oil, 30-45 parts of liquid paraffin, 2-10 parts of a regulator, 0.1-3 parts of an anti-blocking agent, 0.1-5 parts of a dispersant, and 1-10 parts of an antistatic agent. The structural formula of the polyether modified silicone oil is as follows: ； Wherein, 50≤m≤250, 30≤n≤300, 20≤a≤100, 25≤b≤120; the kinematic viscosity of the polyether modified silicone oil is 20-100cp; R1 is selected from ; R2 is selected from -H; The anti-adhesion agent is at least one of oleamide, cellulose acetate, and polyvinyl alcohol; The preparation method of the polyether modified silicone oil is: Under inert gas conditions, hydrogen-containing silicone oil and polyether modifier are heated to react in the presence of a catalyst, and after the reaction is completed, polyether-modified silicone oil is obtained through post-processing and purification; The polyether modifier is allyl polyoxyethylene polyoxypropylene ether; The molar ratio of Si-H in the hydrogenated silicone oil to C=C in the polyether modifier is 1:(1.0-1.4).

2. The spandex spinning oil according to claim 1, characterized in that: The kinematic viscosity of the liquid paraffin is 20-50 cp; and the regulator is stearic acid alcohol.

3. The spandex spinning oil according to claim 1, characterized in that: The dispersant is at least one of polyoxyethylene fatty acid ester and castor oil polyoxyethylene ether; The structural formula of the antistatic agent is as follows: ； R is selected from any one of -H, -CH3, -CH2CH3, and -CH=CH2, and c is a natural number and 20≤c≤50.

4. The spandex spinning oil according to claim 1, characterized in that: The catalyst is any one of a Speier catalyst and a Karstedt catalyst.

5. The spandex spinning oil according to claim 1, characterized in that: The heating reaction temperature is 90-130° C., and the reaction time is 6-10 h.

6. A method for preparing a spandex spinning oil according to any one of claims 1 to 5, characterized in that: The preparation method is: Add polyether-modified silicone oil and a regulator into a reactor and mix them evenly; then add liquid paraffin, an anti-blocking agent, a dispersant, and an antistatic agent, heat and stir, and continue stirring for a period of time after the color of the system changes from a white milky state to a colorless transparent liquid. After the liquid cools, a colorless transparent liquid is obtained, which is the spinning oil.

7. The method for preparing a spandex spinning oil according to claim 6, wherein: The heating temperature is 90-100° C.; the stirring speed is 2000-2500 rpm.

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