A high temperature resistant spinning oil and preparation method thereof

By adding a specific amount of low-molecular-weight polymers to the spinning oil and rationally designing the emulsifier, the problems of stratification, turbidity, and poor heat resistance of the spinning oil are solved, and the spinning stability and dyeing uniformity at high temperatures are improved without any harm to the environment.

CN117947635BActive Publication Date: 2025-09-09ZHEJIANG SCI-TECH UNIV
View PDF 2 Cites 0 Cited by

Patent Information

Application Number
CN202410114819.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-01-26
Publication Date
2025-09-09
Estimated Expiration
2044-01-26

AI Technical Summary

Technical Problem

Existing spinning oils have serious stratification and turbidity problems, poor heat resistance and high-temperature smoothness, severe volatility, contain heavy metal ions or are harmful to the ecological environment, leading to spinning abnormalities such as hairy yarns, broken ends, white powder and tension fluctuations during the spinning process, and are prone to problems such as difficulty in dyeing and uneven dyeing in subsequent dyeing.

Method used

A low-molecular-weight polymer with a specific content is used as a smoothing agent. The type and content of the emulsifier are reasonably designed, and the HLB value of the spinning oil is controlled at 12-18. A high-temperature resistant spinning oil is prepared, which includes 40-60% of a smoothing agent, 6-10% of an antistatic agent, 15-30% of an emulsifier, 3-10% of a sizing agent, 3-10% of a dispersant, 0.1-1.5% of an antioxidant, 1-3% of a humectant and 10-20% of a diluent. The low-molecular-weight polymer is prepared through a specific reaction process.

Benefits of technology

It improves the stability and high-temperature smoothness of the spinning oil, reduces the friction between fibers, reduces spinning abnormalities, improves dyeing properties, is environmentally friendly and harmless, and has better performance than commercially available oils.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure QLYQS_1
    Figure QLYQS_1
  • Figure BDA0004684793770000021
    Figure BDA0004684793770000021
  • Figure BDA0004684793770000061
    Figure BDA0004684793770000061
Patent Text Reader

Abstract

The present invention relates to the field of chemical fiber, and the present invention discloses a high temperature resistant spinning oil and a preparation method thereof. The spinning oil includes: smoothing agent 40-60%, antistatic agent 6-10%, emulsifier 15-30%, bunching agent 3-10%, dispersant 3-10%, antioxidant 0.1-1.5%, humectant 1-3%, diluting solvent 10-20%, pH regulator 0.1-0.5%; the smoothing agent contains 10-30wt% of the total amount of spinning oil. The spinning oil of the present invention contains a self-developed low molecular weight polymer, which can give the spinning oil excellent stability, heat resistance and high temperature smoothing performance. After oiling, the friction force between various fibers can be fully reduced, the oil film strength of the spinning oil on the fiber surface is increased, and the occurrence of spinning abnormalities such as hair, broken ends and tension fluctuations and entanglement is prevented or reduced.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The present invention relates to the field of chemical fibers, and in particular to a high-temperature resistant spinning oil and a preparation method thereof. Background Art

[0002] Most chemical fibers have a low dielectric constant, low moisture regain, and a high coefficient of friction, especially for polyester industrial yarn. Therefore, the use of a spinning oil is essential. Spinning oils, primarily surfactants, form a directional adsorption layer, or oil film, on the surface of chemical fibers. The hydrophilic groups in the oil film are oriented toward the air, absorbing moisture from the air and forming a continuous water film on the fiber surface. This allows charged ions to migrate across the film, reducing the accumulation of static charge caused by friction, thereby lowering the fiber's surface resistance and increasing its conductivity. The oil film also creates a certain affinity for the fibers, maintaining a certain degree of bundledness and preventing them from becoming disorganized. It also imparts a certain smoothness to the fibers, protecting them from damage during friction and providing a pleasant feel. This ensures smooth spinning, stretching, and drying processes. It also eliminates static electricity during the textile process, preventing undesirable problems such as winding around aprons, rollers, and cylinders, reducing lint and broken ends, and ensuring the quality of the fiber product. Although the dosage of chemical fiber oil in chemical fiber production is only 0.15%-2.5%, it plays a vital role in the quality of the fiber.

[0003] With the rapid development of the chemical fiber industry, the trend of high-speed spinning and industrial application growth is obvious, and the production demand for improving spinning stability and fiber performance is also growing. For example, polyester industrial yarn, which is often used for skeleton reinforcement, needs to undergo high-temperature heat stretching and shaping (above 200°C) during post-processing. During this period, the fiber aggregation structure changes significantly and the mechanical properties are greatly improved. Spinning oil is one of the factors affecting spinning stability and the uniformity of fiber physical and mechanical properties. Therefore, the spinning oil is required to have good heat resistance, low volatility and no decomposition when heated, and no fiber coloring; at the same time, the fiber must have good smoothness and high oil film strength. There must be no broken ends or lint during fiber production and post-processing, and precipitates and white powder must be minimized. The oil must also be able to give the fiber excellent antistatic properties. Therefore, chemical fibers have high requirements for the performance of spinning oils. After the fibers are oiled, some need to be stretched and dried at high temperatures. The finished yarns must also undergo post-processing, stretching, weaving and other processes.

[0004] Existing spinning oils generally have serious problems such as severe stratification and turbidity during actual preparation, poor heat resistance and high-temperature smoothness, high volatility, and the presence of heavy metal ions or substances harmful to the ecological environment. In addition, in spinning applications, they are prone to spinning anomalies such as lint, broken ends, white powder, tension fluctuations, and entanglement. In subsequent dyeing, dyeing is prone to difficulty and uneven dyeing, which seriously reduces the quality of the fiber. Summary of the Invention

[0005] The present invention aims to overcome the problems of current spinning oils, such as serious stratification and turbidity, poor heat resistance and high-temperature smoothness, severe volatility, and the presence of heavy metal ions or substances harmful to the ecological environment. In addition, in spinning applications, the present invention generally easily leads to spinning abnormalities such as lint, broken ends, white powder, tension fluctuations, and entanglement. In subsequent dyeing, the present invention easily causes difficulties in dyeing and uneven dyeing. A high-temperature resistant spinning oil and a preparation method thereof are proposed.

[0006] The specific technical solutions of the present invention are:

[0007] In a first aspect, the present invention provides a high-temperature resistant spinning oil, comprising the following components in mass percentage: 40-60% smoothing agent, 6-10% antistatic agent, 15-30% emulsifier, 3-10% sizing agent, 3-10% dispersant, 0.1-1.5% antioxidant, 1-3% humectant, 10-20% diluent solvent, and 0.1-0.5% pH regulator.

[0008] The smoothing agent contains a low molecular weight polymer accounting for 10-30 wt% of the total amount of the spinning oil and having the following molecular structure:

[0009]

[0010] wherein x+y+z=8-30; R and R' are C2-C5 alkane groups.

[0011] Unlike conventional spin finishes, the present invention's spin finish contains the aforementioned low-molecular-weight polymer as a core component of the smoothing agent. The present inventors discovered that adding a specific amount of this low-molecular-weight polymer to the spin finish imparts excellent stability, heat resistance, and high-temperature smoothness. This, combined with the ability to significantly reduce friction between fibers and increase the strength of the oil film on the fiber surface, prevents or reduces spinning anomalies such as lint, broken ends, tension fluctuations, and entanglement. Furthermore, the probability of subsequent dyeing, such as difficulty dyeing and uneven dyeing, can be reduced.

[0012] In the molecular structure of the aforementioned low molecular weight polymer, x+y+z should be limited to a range of 8-30. The present invention has discovered that as x+y+z gradually increases, the stability of the resulting low molecular weight polymer gradually improves, effectively reducing volatility. However, the larger the x+y+z, the better. The present invention has further discovered that when x+y+z exceeds 30, the molecular structure instability increases significantly, resulting in a significant decrease in the high-temperature stability and tarring properties of the resulting low molecular weight polymer.

[0013] Furthermore, it's important to emphasize that the present invention has discovered that the content of low-molecular-weight polymers is crucial to the performance of the spinning oil. Too little can reduce the oil's smoothness and heat resistance, rendering it incapable of protecting the chemical fiber during post-processing, such as high-temperature stretching and shaping (above 200°C). Conversely, excessively high levels can increase the overall HLB value of the spinning oil, potentially causing stratification and turbidity during compounding, and also affecting the subsequent dyeing and hygroscopic properties of the chemical fiber. Preferably, the high-temperature-resistant spinning oil has an HLB value of 12-18.

[0014] Conventional spinning finishes are difficult to form due to significant differences in the hydrophilic-lipophilic balance (HLB) values ​​of smoothing agents, sizing agents, and antistatic agents. Therefore, the formulation requires careful consideration of the type and content of emulsifiers to ensure a uniform and stable finish with a small emulsion particle size. Furthermore, spinning finishes are typically formulated into emulsions for use, requiring a more hydrophilic profile. The present invention controls the HLB value of the spin finish to between 12 and 18, ensuring a long-lasting, uniform dispersion without stratification.

[0015] Preferably, the preparation method of the low molecular weight polymer is as follows: a diol and a tribasic acid with an acid-alcohol molar ratio of 1:1.8-5.2, or a triol and a dibasic acid with an acid-alcohol molar ratio of 1.8-5.2:1, and a catalyst dosage of 0.01-0.03%, first under catalysis and N2 protection, heating to 150-200 ° C for reaction for 0.5-1h, then adding 1-3wt% petroleum ether, vacuum reaction for 1-2h, and cooling to obtain a low molecular weight polymer.

[0016] The low molecular weight polymer is successfully obtained by the above-mentioned method of the present invention. Petroleum ether is added during the reaction process, which can form a binary or ternary azeotrope with water or one of the reactants, thereby promptly removing water from the reaction system, thereby shifting the equilibrium in a positive direction and significantly accelerating the reaction rate. Furthermore, it should be emphasized that the present invention has found that the amount of petroleum ether should not be excessive, as otherwise it can easily lead to an excessively low reaction temperature, which in turn reduces the reaction rate.

[0017] Preferably, the smoothing agent comprises, in addition to the low molecular weight polymer, one or a mixture of trimethylolpropane oleate, pentaerythritol oleate, diisooctyl sebacate, isooctyl oleate and polyethylene glycol citrate.

[0018] Preferably, the emulsifier is one or a mixture of fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, fatty acid polyoxyethylene ester, sorbitan oleate polyoxyethylene ether and sorbitan stearate.

[0019] Preferably, the sizing agent is one or a mixture of hydrogenated castor oil polyoxyethylene ether, castor oil polyoxyethylene ether, polyoxyethylene laurate, fatty acid triethanolamine ester and oleic acid triethanolamine soap.

[0020] Preferably, the antistatic agent is one or a mixture of several of propylene glycol block polyether, sodium secondary alkyl sulfonate, C12-C14 polyoxyethylene ether phosphate potassium salt and C12-C14 alkyl phosphate potassium / sodium salt.

[0021] Preferably, the dilution solvent is an oil-soluble solvent, which is one or a mixture of industrial white oil, liquid paraffin, C10 solvent oil, D100 cycloalkane solvent, and normal C15 alkane solvent.

[0022] Preferably, the pH regulating stabilizer is one or two of sodium carbonate, sodium bicarbonate, sodium hydroxide, laurylamine polyoxyethylene ether, and T151.

[0023] Preferably, the moisturizing agent is an alcohol substance with high boiling point and good heat resistance, specifically one or a mixture of glycerol, propylene glycol, sorbitol, ethylene glycol, ethylene glycol, polyethylene glycol with Mw=100-1000.

[0024] In a second aspect, the present invention provides a method for preparing a spinning oil, comprising the following steps:

[0025] 1) Add emulsifier, sizing agent and antistatic agent into the reactor in order according to the ratio, heat to 40-70°C, and stir evenly for 0.5-1h;

[0026] 2) Add the smoothing agent into the reactor according to the ratio and continue stirring for 0.5-1h;

[0027] 3) Stop heating the reactor and allow it to cool naturally. Add the moisturizer, diluent, and dispersant to the reactor according to the ratio and continue stirring for 30 minutes.

[0028] 4) When the solution temperature drops to 25-30°C, add antioxidant and pH stabilizer according to the ratio, stir evenly, cool and filter to obtain the finished product.

[0029] In a third aspect, the present invention provides the use of the above-mentioned spinning oil in the preparation of industrial polyester yarn.

[0030] Compared with the prior art, the present invention has the following technical effects:

[0031] (1) The spinning oil of the present invention contains a self-developed low-molecular-weight polymer as the core component of the smoothing agent. After adding a specific amount of the low-molecular-weight polymer to the spinning oil, the spinning oil can be given excellent stability, heat resistance and high-temperature smoothing properties. After oiling, the friction between various fibers can be fully reduced, and the strength of the oil film of the spinning oil on the fiber surface can be increased, thereby preventing or reducing the occurrence of spinning abnormalities such as lint, broken ends, tension fluctuations, and entanglement. Furthermore, in subsequent dyeing, the probability of the occurrence of phenomena such as difficult dyeing and uneven dyeing can be reduced.

[0032] (2) The present invention limits the x+y+z in the molecular structure of the low molecular weight polymer to 8 to 30. Low molecular weight polymers within this range have low volatility and excellent high temperature stability.

[0033] (3) The raw material cost of the spinning oil of the present invention is low, no harmful ingredients such as APEO (alkylphenol polyoxyethylene ether) are used, and the spinning oil is green and environmentally friendly. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 This is the hydrogen nuclear magnetic resonance spectrum of the low molecular weight polymer prepared in Example 4;

[0035] Figure 2 This is the infrared spectrum of the low molecular weight polymer obtained in Example 4. DETAILED DESCRIPTION

[0036] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the specific embodiments of the present invention are described in detail below.

[0037] In the following description, many specific details are set forth to facilitate a full understanding of the present invention. However, the present invention may also be implemented in other ways different from those described herein. Those skilled in the art may make similar generalizations without violating the connotation of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.

[0038] Preparation case of low molecular weight polymer smoothing agent

[0039] Example 1

[0040] Low molecular weight polymer smoothing agent (M w =1000-2500): Triol (1,1,1-(trihydroxymethyl)-ethane) is reacted with a dibasic acid (adipic acid) at a molar ratio of 1:2. The catalyst (antimony glycol) is used at a level of 0.02%. Under nitrogen protection, the temperature is raised to 170°C for 1 hour. Then, 3% petroleum ether is added, the reaction is carried out under vacuum for 0.5 hour, and the temperature is lowered to obtain the finished product.

[0041] Example 2

[0042] Low molecular weight polymer smoothing agent (M w =2000-3500): Triol (1,1,1-(trihydroxymethyl)-ethane) is reacted with a dibasic acid (adipic acid) at an acid-to-alcohol molar ratio of 1:2 and a catalyst (antimony glycol) at a level of 0.02%. Under nitrogen protection, the reaction is heated to 180°C for 1 hour. Then, 3% petroleum ether is added, the reaction is carried out under vacuum for 1 hour, and the temperature is lowered to obtain the finished product.

[0043] Comparative Example 1

[0044] Preparation of a low molecular weight polymer smoothing agent (Mw>3500): Triol (1,1,1-(trimethylol)-ethane) was reacted with a dibasic acid (adipic acid) at a molar ratio of 1:2. The catalyst (antimony glycol) was used at a level of 0.02%. Under nitrogen protection, the reaction was heated to 190°C for 1.5 hours. Then, 3% petroleum ether was added, the reaction was vacuum-treated for 1 hour, and the temperature was lowered to yield the finished product.

[0045] Comparative Example 2

[0046] Low molecular weight polymer smoothing agent (M w =2000-3500): Triol (1,1,1-(trihydroxymethyl)-ethane) is reacted with a dibasic acid (adipic acid) at a molar ratio of 1:2 and a catalyst (antimony glycol) of 0.02%. Under nitrogen protection, the temperature is raised to 180°C for 1 hour. Then, 5% petroleum ether is added, the reaction is carried out under vacuum for 1 hour, and the temperature is lowered to obtain the finished product.

[0047] Example 3

[0048] Low molecular weight polymer smoothing agent (M w =1000-2500): A diol (neopentyl glycol) is reacted with a tribasic acid (citric acid) at a molar ratio of 1:2 and a catalyst (ethylene glycol antimony) at 0.02%. Under nitrogen protection, the reaction is heated to 170°C for 1 hour. Then, 3% petroleum ether is added, the reaction is carried out under vacuum for 0.5 hour, and the temperature is lowered to obtain the finished product.

[0049] Example 4

[0050] Low molecular weight polymer smoothing agent (M w =1000-2500): A diol (polyethylene glycol) is reacted with a tribasic acid (citric acid) at a molar ratio of 1:2. The catalyst (antimony glycol) is used at a level of 0.02%. Under nitrogen protection, the reaction is heated to 170°C for 1 hour. Then, 3% petroleum ether is added, the reaction is carried out under vacuum for 0.5 hour, and the temperature is lowered to obtain the finished product.

[0051] Figure 1This is the infrared spectrum of the low molecular weight polymer. The stretching vibration of hydroxyl group -OH has an absorption peak at 3455.92cm-1, and the absorption peak of methylene CH is at 2865.43cm-1. -1 and 1453.14cm -1 1732.58cm -1 、1247.62cm -1 and 1090.90cm -1 The absorption peak at 520.87 cm is the stretching vibration of C=O and CO. -1 The absorption peak is caused by the out-of-plane bending vibration of CH.

[0052] Figure 2 This is the H NMR spectrum of a low molecular weight polymer. Its molecular structure has five hydrogen atoms in different environments. The resonance peak of the hydrogen atom on the hydroxyl group (-OH) is 6.62 ppm, the resonance peak of the hydrogen atom at the end of polyethylene glycol is 4.89 ppm, the resonance peak of the hydrogen atom of the methylene group (-CH2-) is 4.22 ppm, the resonance peak of the hydrogen atom of the carbonyl group (-C=O) is 3.54 ppm, and the resonance peak of the hydrogen atom of the methylene group (-CH2-) is 2.73 ppm.

[0053] The heat resistance performance of Examples 1-4, Comparative Examples 1-2 and common smoothing agents on the market were tested, and the test data are shown in the following table.

[0054]

[0055] From the data in the above table we can see that:

[0056] The x+y+z in the low molecular weight molecular structure obtained in Examples 1 and 2 is between 8 and 30, M w =1000-3500, the heat resistance of the product is significantly better than that of comparative example 3 (x+y+z>30, M w >3500), indicating that the low molecular weight polymer in the preferred range of the present invention has better heat resistance.

[0057] Comparative Example 2 differs from Example 2 in that a higher amount of petroleum ether (5%) was used during the preparation process. The results show that excessive petroleum ether also leads to a decrease in the heat resistance of the polymer. In addition, the heat resistance of the low molecular weight polymers obtained in each example is also significantly better than that of conventional commercially available smoothing agents.

[0058] Spinning oil preparation case

[0059] Example 5

[0060] The mass percentages of the components of the high temperature resistant spinning oil for polyester industrial yarn are as follows:

[0061] (Smoothing agent) pentaerythritol oleate 26%, (Example 2) low molecular weight polymer 20%; (Emulsifier) ​​hydrogenated castor oil polyoxyethylene ether 18%; (Antistatic agent) propylene glycol block polyether 6%; (Dispersant) polyisobutylene succinimide 5%; (Blocking agent) triethanolamine oleate soap 3%; (Dilution solvent) normal C15 alkane solvent 18%; (Moisturizer) ethylene glycol 3%; (Antioxidant) triphenyl phosphite 0.8%; (pH adjuster) lauramine polyoxyethylene ether 0.2%.

[0062] Example 6

[0063] The mass percentages of the components of the high temperature resistant spinning oil for polyester industrial yarn are as follows:

[0064] (Smoothing agent) pentaerythritol oleate 25%, (Example 2) low molecular weight polymer 15%, (Smoothing agent) trimethylolpropane oleate 10%; (Emulsifier) ​​hydrogenated castor oil polyoxyethylene ether 15%; (Antistatic agent) propylene glycol block polyether 6%, secondary alkyl sodium sulfonate 2%; (Dispersant) polyisobutylene succinimide 4%; (Blocking agent) triethanolamine oleate soap 2%, hydrogenated castor oil polyoxyethylene ether 7%; (Diluting solvent) 32# white oil 10%; (Moisturizing agent) ethylene glycol 2%; (Antioxidant) triphenyl phosphite 1.5%; (pH adjuster) laurylamine polyoxyethylene ether 0.5%.

[0065] Example 7

[0066] The mass percentages of the components of the high temperature resistant spinning oil for polyester industrial yarn are as follows:

[0067] (Smoothing agent) pentaerythritol oleate 15%, (Example 2) low molecular weight polymer 10%, (Smoothing agent) trimethylolpropane oleate 20%; (Emulsifier) ​​hydrogenated castor oil polyoxyethylene ether 12%, sorbitan stearate 10%; (Antistatic agent) lauryl alcohol polyoxyethylene alkyl phosphate potassium 3%, secondary alkyl sodium sulfonate 5%; (Dispersant) polyisobutylene succinimide 4%; (Blocking agent) castor oil polyoxyethylene ether 8%; (Dilution solvent) 32# white oil 8%; (Moisturizer) ethylene glycol 2%; (Antioxidant) triphenyl phosphite 2%; (pH adjuster) lauramine polyoxyethylene ether 1%.

[0068] Example 8

[0069] The mass percentages of the components of the high temperature resistant spinning oil for polyester industrial yarn are as follows:

[0070] (Example 2) Low molecular weight polymer 30%; (Emulsifier) ​​Span S80 20%, Tween T80 17%; (Antistatic agent) Sodium secondary alkyl sulfonate 8%; (Dispersant) Polyisobutylene succinimide 2%; (Blocking agent) Triethanolamine oleate soap 4%; (Dilution solvent) Normal C15 alkane solvent 15%; (Moisturizer) Ethylene glycol 2%; (Antioxidant) Triphenyl phosphite 0.5%; (pH adjuster) Laurylamine polyoxyethylene ether 1.5%.

[0071] Comparative Example 3

[0072] The mass percentages of the components of the high temperature resistant spinning oil for polyester industrial yarn are as follows:

[0073] (Smoothing agent) trimethylolpropane oleate 45%; (Emulsifier) ​​hydrogenated castor oil polyoxyethylene ether 12%, sorbitan stearate 10%; (Antistatic agent) lauryl alcohol polyoxyethylene alkyl phosphate potassium 3%, secondary alkyl sodium sulfonate 5%; (Dispersant) polyisobutylene succinimide 4%; (Blocking agent) castor oil polyoxyethylene ether 8%; (Diluent) 32# white oil 8%; (Moisturizer) ethylene glycol 2%; (Antioxidant) triphenyl phosphite 2%; (pH adjuster) lauramine polyoxyethylene ether 1%.

[0074] Comparative Example 4

[0075] The mass percentages of the components of the high temperature resistant spinning oil for polyester industrial yarn are as follows:

[0076] (Smoothing agent) Pentaerythritol oleate 25%, (Smoothing agent) Trimethylolpropane oleate 20%; (Emulsifier) ​​Hydrogenated castor oil polyoxyethylene ether 12%, Sorbitan stearate 10%; (Antistatic agent) Lauryl alcohol polyoxyethylene alkyl phosphate potassium 3%, Sodium secondary alkyl sulfonate 5%; (Dispersant) Polyisobutylene succinimide 4%; (Blocking agent) Castor oil polyoxyethylene ether 8%; (Diluting solvent) 32# white oil 8%; (Moisturizer) Ethylene glycol 2%; (Antioxidant) Triphenyl phosphite 2%; (pH adjuster) Lauramine polyoxyethylene ether 1%.

[0077] Comparative Example 5

[0078] The mass percentages of the components of the high temperature resistant spinning oil for polyester industrial yarn are as follows:

[0079] (Smoothing agent) pentaerythritol oleate 40%, (Example 2) low molecular weight polymer 6%; (Emulsifier) ​​hydrogenated castor oil polyoxyethylene ether 18%; (Antistatic agent) propylene glycol block polyether 6%; (Dispersant) polyisobutylene succinimide 5%; (Blocking agent) triethanolamine oleate soap 3%; (Dilution solvent) normal C15 alkane solvent 18%; (Moisturizer) ethylene glycol 3%; (Antioxidant) triphenyl phosphite 0.8%; (pH adjuster) laurylamine polyoxyethylene ether 0.2%.

[0080] Comparative Example 6

[0081] The mass percentages of the components of the high temperature resistant spinning oil for polyester industrial yarn are as follows:

[0082] (Smoothing agent) pentaerythritol oleate 6%, (Example 2) low molecular weight polymer 40%; (Emulsifier) ​​hydrogenated castor oil polyoxyethylene ether 18%; (Antistatic agent) propylene glycol block polyether 6%; (Dispersant) polyisobutylene succinimide 5%; (Blocking agent) triethanolamine oleate soap 3%; (Dilution solvent) normal C15 alkane solvent 18%; (Moisturizer) ethylene glycol 3%; (Antioxidant) triphenyl phosphite 0.8%; (pH adjuster) laurylamine polyoxyethylene ether 0.2%.

[0083] According to the mass percentage of each component in Examples 5-8 and Comparative Examples 3-6, the emulsifier, sizing agent and antistatic agent were put into the reactor in sequence, the temperature was raised to 50°C, and the mixture was stirred evenly for 1 hour; the smoothing agent was added to the reactor according to the ratio, and the stirring was continued for 0.5 hours; the heating of the reactor was stopped, the temperature was naturally cooled, and the moisturizing agent, diluting solvent and dispersant were added to the reactor according to the ratio, and the stirring was continued for 30 minutes; when the solution temperature dropped to 25°C, the antioxidant, pH stabilizer and water were added according to the ratio, and finally the mixture was stirred evenly, cooled and filtered to obtain the finished product.

[0084] The spinning oils obtained in Examples 5-8 and Comparative Examples 3-6 were tested, and the specific test items are shown in the following table.

[0085] Test items Detection method or instrument Moisture Karl Fischer titrator pH Leiji Benchtop pH Meter PHS-25 Viscosity Rotational rheometer Heat resistance Thermogravimetric analyzer surface tension High Temperature Contact Angle Tester DM2700P Wetting time GB / T 11983-2008 Oil film strength MRS-1J Mechanical Four-ball Long-time Anti-wear Testing Machine Volatile loss rate 140℃, 2h; 250℃, 2h Conductivity Ultra-high resistance micro-current tester ST2643

[0086] The spinning oils of Examples 5-8, Comparative Examples 3-6 and imported oils were compared, and the test data of their basic performance indicators are shown in the following table.

[0087]

[0088]

[0089] Note: *Imported oil comes from Zhejiang Guxiandao Green Fiber Co., Ltd.

[0090] From the data in the above table, we can see that:

[0091] The spin finishes of various embodiments of the present invention exhibit significant advantages over commercially available imported finishes in terms of volatility loss rate and friction coefficient, demonstrating improved heat resistance and smoothness. Surface tension, electrical conductivity, and other basic properties are comparable to or better than those of imported finishes, demonstrating that the spin finishes of the present invention are fully comparable in overall performance to imported finishes.

[0092] The smoothing agent in the formulations of Comparative Examples 3 and 4 was not compounded with a low molecular weight polymer, and the other components were the same as those in Example 7. The results showed that the various properties of Comparative Examples 3 and 4 were significantly inferior to those in Example 7. The formulation of Comparative Example 5 contained only 6% of a low molecular weight polymer, and the formulation of Comparative Example 6 contained 40% of a low molecular weight polymer, and the other components were the same as those in Example 5. The results showed that when the content of the low molecular weight polymer was less than 10% or greater than 30%, various properties would be poor.

[0093] The above describes the specific embodiments of the present invention, but does not impose any form of limitation on the technical solutions of the present invention. The protection content of the present invention is not limited to the above embodiments. In the technical field to which the present invention belongs, all changes and modifications within the technical spirit of the present invention are within the protection scope of the present invention.

Claims

1. A high temperature resistant spinning oil, characterized in that: The invention comprises the following components in mass percentage: smoothing agent 40-60%, antistatic agent 6-10%, emulsifier 15-30%, sizing agent 3-10%, dispersant 3-10%, antioxidant 0.1-1.5%, moisturizing agent 1-3%, diluting solvent 10-20%, pH regulator 0.1-0.5%; The smoothing agent contains a low molecular weight polymer accounting for 10-30 wt% of the total amount of the spinning oil and having the following molecular structure: wherein x+y+z=8-30; R and R' are C2-C5 alkane groups; The HLB value of the high temperature resistant spinning oil is 12-18; The emulsifier is one or a mixture of fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, castor oil polyoxyethylene ether, fatty acid polyoxyethylene ester, sorbitan oleate polyoxyethylene ether and sorbitan stearate.

2. The spinning oil according to claim 1, wherein: The preparation method of the low molecular weight polymer comprises the following steps: reacting a diol and a tribasic acid with an acid-alcohol molar ratio of 1:1.8-5.2, or a triol and a dibasic acid with an acid-alcohol molar ratio of 1.8-5.2:1, firstly heating the mixture to 150-200°C under catalysis and N2 protection for 0.5-1h, then adding 1-3wt% petroleum ether, vacuumizing the mixture for 1-2h, and cooling the mixture to obtain the low molecular weight polymer.

3. The spinning oil according to claim 1, wherein: In addition to the low molecular weight polymer, the smoothing agent also includes one or a mixture of trimethylolpropane oleate, pentaerythritol oleate, diisooctyl sebacate, isooctyl oleate and polyethylene glycol citrate.

4. The spinning oil according to claim 1, wherein: The sizing agent is one or a mixture of hydrogenated castor oil polyoxyethylene ether, castor oil polyoxyethylene ether, polyoxyethylene laurate, fatty acid triethanolamine ester and oleic acid triethanolamine soap.

5. The spinning oil according to claim 1, wherein: The antistatic agent is one or a mixture of several of propylene glycol block polyether, sodium secondary alkyl sulfonate, C12-C14 polyoxyethylene ether phosphate potassium salt and C12-C14 alkyl phosphate potassium / sodium salt.

6. The spinning oil according to claim 1, wherein: The dilution solvent is an oil-soluble solvent, which is one or a mixture of industrial white oil, liquid paraffin, C10 solvent oil, D100 cycloalkane solvent, and normal C15 alkane solvent.

7. The spinning oil according to claim 1, wherein: The moisturizing agent is one or a mixture of glycerin, propylene glycol, sorbitol, ethylene glycol, ethylene glycol, and polyethylene glycol with Mw=200-1000.

8. A method for preparing the spinning oil according to any one of claims 1 to 7, characterized in that The following steps are involved: 1) Add emulsifier, sizing agent and antistatic agent into the reactor in order according to the ratio, heat to 40-70°C, and stir evenly for 0.5-1h; 2) Add the smoothing agent into the reactor according to the ratio and continue stirring for 0.5-1h; 3) Stop heating the reactor and allow it to cool naturally. Add the moisturizer, diluent, and dispersant to the reactor according to the ratio and continue stirring for 30 minutes. 4) When the solution temperature drops to 25-30°C, add antioxidant and pH stabilizer according to the ratio, stir evenly, cool and filter to obtain the finished product.

9. Use of the spinning oil according to any one of claims 1 to 7 in the preparation of industrial polyester yarn.

Citation Information

Patent Citations

  • Process for lubricating synthetic fibre material

    CH619989A5

  • Super-hydrophilic yarn smoothing agent and preparation method thereof

    CN108442103A