Crude oil direct oiling type spinning oil, preparation method and application

Abstract

The invention provides a crude oil direct oiling type spinning oil agent, a preparation method and application, the crude oil direct oiling type spinning oil agent comprises 65-75% of a composite smoothing agent, and the composite smoothing agent is composed of 25-35 parts of tetradecyl tetradecane-9-olefine acid ester and 65-75 parts of PEG-12 dipalmitate. Specific compounds are selected to form the composite smoothing agent, so that the spinning oil agent has smoothness, oil film strength and heat resistance at the same time; meanwhile, the friction coefficient of the yarn can be reduced, the uniformity of the yarn is improved, and the yarn quality is good.

Description

Technical Field

[0001] The present invention relates to the technical field of spinning, and in particular to a crude oil direct oiling type spinning oil, a preparation method and an application thereof. Background Art

[0002] Polyester, the synthetic fiber category with the largest production capacity and the most widespread application in the world, is mainly produced by integrating high-speed spinning (spinning speeds of up to 2600-3500 m / min) and ultra-high-speed stretching and winding (winding speeds of up to 5100-5500 m / min) into a one-step spinning and stretching process. This not only significantly reduces production costs, but also excels in product quality stability, providing strong support for the efficient and high-quality development of the polyester industry.

[0003] Throughout the entire spinning process, spinning oils must not only ensure smooth and unimpeded progress across all manufacturing steps, but also ensure that fiber quality is not compromised. Traditional spinning processes typically utilize an emulsion-based oil, based on mineral oil. Before use, the base oil must be mixed with water to form an emulsion. During the actual spinning process, the temperature of the fiber as it passes through the heated rollers must be increased to promote evaporation of the water in the oil. This operation consumes significant energy and results in significant waste. As the water evaporates, the oil film is easily damaged, leading to ruptures on the fiber surface and ultimately uneven oiling, severely impacting fiber quality.

[0004] To this end, Chinese patent application number 202311223821.7 discloses a crude oil-based FDY spinning oil comprising 40-60 wt% of a smoothing agent, 15-40 wt% of an emulsifier, 1-5 wt% of an antistatic agent, 1-10 wt% of a wetting and penetrating agent, and 5-10 wt% of water. The wetting and penetrating agent has an average molecular weight of less than or equal to 2000, an HLB value of less than or equal to 6, and an HLB value of 3-15. The crude oil-based FDY spinning oil of the present invention, through the synergistic effect of the wetting and penetrating agent and the emulsifier, reduces the surface tension of the crude oil-based FDY spinning oil, resulting in excellent wetting, spreading, and permeability. However, this spinning oil has difficulty maintaining the required thermal stability during high-speed spinning, resulting in poor yarn uniformity and smoothness, and prone to yarn breakage.

[0005] In view of this, the present invention is proposed. Summary of the Invention

[0006] The problem solved by the present invention is that the existing crude oil direct oiling type spinning oil is difficult to maintain the required thermal stability and emulsion stability, resulting in poor quality of the produced yarn.

[0007] To solve the above problems, the present invention provides a crude oil direct oiling type spinning oil, comprising 65-75% of a composite smoothing agent, wherein the composite smoothing agent is composed of 25-35 parts of tetradecyl tetradec-9-enoate and 65-75 parts of PEG-12 dipalmitate.

[0008] Preferably, the crude oil direct oiling type spinning oil consists of 65-75 parts of a composite smoothing agent, 10-15 parts of an emulsifier, 2-4 parts of a penetrant, 2-6 parts of an antistatic agent, and 6-10 parts of a solvent, wherein the composite smoothing agent consists of 25-35 parts of tetradecyl tetradec-9-enoate and 65-75 parts of PEG-12 dipalmitate, and the solvent is water.

[0009] Preferably, the emulsifier is selected from at least one of fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ether, cardanol polyoxyethylene ether, castor oil polyoxyethylene ether, sorbitan fatty acid ester, sorbitan polyoxyethylene ether fatty acid ester or polyethylene glycol fatty acid ester.

[0010] Preferably, the penetrant is at least one of fatty alcohol polyoxyethylene ether, potassium perfluorooctane sulfonate, and sodium perfluorooctane sulfonate. Preferably, the penetrant is composed of sodium perfluorooctane sulfonate and potassium perfluorooctane sulfonate in a mass ratio of 1:2.

[0011] Preferably, the antistatic agent is selected from at least one of alkyl alcohol phosphate polyoxyethylene ether, alkyl alcohol phosphate, alkyl alcohol sulfonate, alkyl alcohol polyoxyethylene ether sulfonate, alkyl alcohol sulfate, alkyl alcohol ether sulfate salt and alkyl alcohol ether carboxylate fatty amine polyoxyethylene ether, alkyl alcohol ammonium oxide or betaine.

[0012] Preferably, the pH of the crude oil direct oiling type spinning oil is 7.5-8.0.

[0013] The present invention also provides a method for preparing a crude oil direct oiling type spinning oil, comprising the following steps: adjusting the temperature in a reaction kettle to 38-45°C, adding a composite smoothing agent in appropriate amounts, stirring at 800-1400 rad / min for 10-50 minutes, then adding an antistatic agent and stirring for 10-40 minutes, then adding a solvent and a penetrant and stirring for 20-50 minutes, and finally adding an emulsifier and stirring for 30-90 minutes, cooling to room temperature, and filtering to obtain the product.

[0014] Preferably, the preparation method of the crude oil direct oiling type spinning oil comprises the following steps: adjusting the temperature in the reactor to 40-45°C, adding a composite smoothing agent in amount, stirring at 800-1200 rad / min for 10-30 minutes, then adding an antistatic agent and stirring for 10 minutes, then adding a solvent and a penetrant and stirring for 20-40 minutes, and finally adding an emulsifier and stirring for 30-60 minutes, cooling to room temperature and filtering to obtain the product.

[0015] The invention also discloses the application of the crude oil-oiled spinning oil in a spinning production process.

[0016] Compared with the prior art, the crude oil direct oiling type spinning oil, preparation method and application described in the present invention have the following beneficial effects: 1) The present application optimizes the components of the composite smoothing agent from the perspectives of carbon atom number, saturation, and hydroxyl number, so that the spinning oil can take into account smoothness, oil film strength and heat resistance; 2) PEG-12 dipalmitate is used instead of mineral oil, thereby reducing the friction coefficient of the yarn and improving its uniformity, and the yarn quality is good; 3) By selecting a specific addition sequence, the spinning oil can have good light transmittance and good emulsion stability; 4) By selecting a specific penetrant, the surface tension of the final spinning oil can be significantly reduced, thereby effectively avoiding the accumulation of oil stains generated under high temperature conditions on the radiant heat heater, significantly reducing the yarn breakage rate and extending the cleaning cycle of the heater, and ensuring strong production continuity. DETAILED DESCRIPTION

[0017] Below in conjunction with specific embodiment, further elaborate the present invention.Should be understood that these embodiments are used to illustrate the present invention and are not used to limit the scope of the present invention.In addition, should be understood that after reading the content of the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms fall equally within the scope limited by the appended claims of the application.

[0018] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art in the art of the present invention. The terms used in the present specification are only for the purpose of describing specific embodiments or examples and are not intended to limit the present invention. The raw materials, reagents, and equipment involved in the examples of the present invention can be obtained through commercial channels unless otherwise specified.

[0019] The traditional FDY spinning process mainly uses emulsion-type spinning oil. Since the spinning oil crude oil needs to be mixed with water to form an emulsion before use, the temperature of the hot roller needs to be increased during the spinning process to evaporate the water in the oil. This has disadvantages such as high energy consumption, reduced yarn thermal conductivity, water dilution limiting the composition of the spinning emulsion, and changes in the physical properties of the yarn due to water input and output.

[0020] For this purpose, a direct oiling type spinning oil was developed, which not only requires fiber adhesion comparable to that of traditional emulsions, but also the ability to maintain the required thermal stability and emulsion stability during high-speed spinning to ensure that the quality of the final yarn is stable and controllable. The smoothing agent in the spinning oil is mainly used to reduce the friction resistance between the fiber and the spinning equipment. The emulsifier mainly balances the monomers in the oil through physical and chemical processes to ensure that it can become a uniform and stable emulsion when used. The penetrant is the main component that reduces the surface tension of the oil, so that the oil can be more evenly covered on the fiber surface. The antistatic agent is used to reduce charge accumulation and prevent the fiber from generating static electricity during the weaving process. The above ingredients together determine the high temperature stability and emulsion stability of the oil, which are also important factors in ensuring the stability of the yarn quality. To this end, the applicant proposed the following technical solution: Experimental example: Optimization of composite smoothing agent Smoothing agents are a core component of spinning oils. They not only reduce or control friction generated during fiber contact and operation on textile equipment made of various materials, including metal, but also affect the final oil's smoothness, oil film strength, heat resistance, and even viscosity. Current smoothing agents are typically selected based on a single metric, failing to comprehensively consider multiple performance parameters. The applicants experimentally optimized component A of the composite smoothing agent based on Table 1 and prepared the spinning oil according to the method of Example 1.

[0021] The oil film strength and thermal stability of the spinning oil, as well as the static friction coefficient of the filaments prepared, were determined according to the following methods. The oil film strength was characterized by testing the maximum no-bite force using a four-ball friction tester. The thermal stability was characterized by dropping 1.0 ml of the oil sample onto a steel test piece, baking it in an oven at 230°C for 40 minutes, and then measuring the residual percentage. The static friction coefficient between the filaments and the metal was measured under a load of 300 g and a speed of 0.2 rpm. The specific testing methods are prior art and will not be repeated here.

[0022] Table 1 Effect of composite lubricant composition on lubricant performance As shown in Table 1, when the carbon number of the straight-chain alcohol in component A is more or less, the static friction coefficient of the final filament is higher, indicating that the smoothness of the oil agent is poor; when the number of hydroxyl groups of the straight-chain alcohol in component A is 2, the volatility loss is lower at this time, indicating that thermal stability is poor; in addition, for the fatty acid in component A, when the carbon number is less, the oil film strength is lower at this time, and the yarn breakage problem is prone to occur; and when the carbon number is more, the static friction coefficient of the final filament is higher, indicating that the smoothness of the oil agent is poor, and when saturated fatty acids are used, the volatility loss is lower, indicating that thermal stability is poor. In summary, in the present application, tetradecyl tetradec-9-enoate is used as one of the components of the composite smoothing agent, and the oil agent prepared can take into account both oil film strength and thermal stability and has good smoothness.

[0023] Example 1 A crude oil direct oiling type spinning oil comprises the following components: 75 parts of a composite smoothing agent, 10 parts of an emulsifier, 4 parts of a penetrant, 2 parts of an antistatic agent, and 9 parts of a solvent, wherein the composite smoothing agent comprises 35 parts of tetradecyl tetradec-9-enoate and 65 parts of PEG-12 dipalmitate, the emulsifier is PEG-400 monooleate, the penetrant is fatty alcohol polyoxyethylene ether, the antistatic agent is alkyl alcohol phosphate polyoxyethylene ether, and the solvent is water.

[0024] The preparation method is as follows: after adjusting the temperature in the reactor to 40° C., tetradecyl tetradec-9-enoate and PEG-12 dipalmitate are added, and stirred at 1000 rad / min for 10 minutes, then alkyl alcohol phosphate polyoxyethylene ether is added and stirred for 10 minutes, then water and fatty alcohol polyoxyethylene ether are added and stirred for 20 minutes, and finally, emulsifier PEG-400 monooleate is added and stirred for 30 minutes, and the mixture is cooled to room temperature and filtered to obtain the product; Tetradecyl tetradec-9-enoate (myristyl myristoleate) was prepared by the following method: myristyl alcohol (C 14 H 29 OH) and myristoleic acid (tetradec-9-enoic acid, C 14 H 26 O2) was added into the reactor at a molar ratio of 1:1.05, and p-toluenesulfonic acid was used as a reaction catalyst. The temperature was raised to 160°C under nitrogen flow for reaction for 4 hours, and the reaction catalyst and unreacted oleic acid were removed to obtain.

[0025] Example 2 A crude oil direct oiling type spinning oil, comprising the following ingredients: 70 parts of a composite smoothing agent, 15 parts of an emulsifier, 4 parts of a penetrant, 6 parts of an antistatic agent, and 5 parts of a solvent, wherein the composite smoothing agent comprises 25 parts of tetradecyl tetradec-9-enoate and 75 parts of PEG-12 dipalmitate, the emulsifier is sodium dioctyl sulfosuccinate, the penetrant is potassium perfluorooctane sulfonate, the antistatic agent is an alkyl alcohol phosphate, and the solvent is water; The preparation method is as follows: after adjusting the temperature in the reactor to 45° C., tetradecyl tetradec-9-enoate and PEG-12 dipalmitate are added, and the mixture is stirred at 800 rad / min for 20 minutes. Then, alkyl alcohol phosphate is added and stirred for 15 minutes. Thereafter, water and potassium perfluorooctane sulfonate are added and stirred for 30 minutes. Finally, an emulsifier, sodium dioctyl sulfosuccinate, is added and stirred for 20 minutes. The mixture is cooled to room temperature and filtered to obtain the product.

[0026] Example 3 A crude oil direct oiling type spinning oil, comprising the following ingredients: 65 parts of a composite smoothing agent, 15 parts of an emulsifier, 4 parts of a penetrant, 6 parts of an antistatic agent, and 10 parts of a solvent, wherein the composite smoothing agent comprises 30 parts of tetradecyl tetradec-9-enoate and 70 parts of PEG-12 dipalmitate, the emulsifier is sodium dodecylbenzenesulfonate, the penetrant is composed of sodium perfluorooctane sulfonate and potassium perfluorooctane sulfonate in a mass ratio of 1:2, the antistatic agent is an alkyl alcohol polyoxyethylene ether sulfonate, and the solvent is water; The preparation method is as follows: after adjusting the temperature in the reactor to 42° C., tetradecyl tetradec-9-enoate and PEG-12 dipalmitate are added, and the mixture is stirred at 1200 rad / min for 20 minutes. Then, alkyl alcohol polyoxyethylene ether sulfonate is added and stirred for 20 minutes. Thereafter, water and sodium perfluorooctane sulfonate and potassium perfluorooctane sulfonate are added and stirred for 40 minutes. Finally, an emulsifier, sodium dodecylbenzene sulfonate, is added and stirred for 60 minutes. The mixture is cooled to room temperature and filtered to obtain the product.

[0027] Comparative Example 1 The same technical solution as Example 1 is adopted, except that the composite smoothing agent is composed of 20 parts of tetradecyl tetradec-9-enoate and 80 parts of PEG-12 dipalmitate.

[0028] Comparative Example 2 The same technical solution as Example 1 is adopted, except that the composite smoothing agent is composed of 40 parts of tetradecyl tetradec-9-enoate and 60 parts of PEG-12 dipalmitate.

[0029] Comparative Example 3 The same technical solution as Example 1 is adopted, except that the composite smoothing agent is composed of 35 parts of tetradecyl tetradec-9-enoate and 65 parts of mineral oil.

[0030] Comparative Example 4 The same technical solution as Example 1 is adopted, except that the composite lubricant is composed of a mixture of white oil and fatty acid ester in a mass ratio of 1:1.

[0031] Comparative Example 5 The same technical scheme as Example 1 was adopted, except that the following method was adopted for preparation: the temperature in the reaction kettle was adjusted to 40°C, and tetradecyl tetradec-9-enoate, PEG-12 dipalmitate, alkyl alcohol phosphate polyoxyethylene ether, fatty alcohol polyoxyethylene ether, and monooleate were mixed, stirred at 1000 rad / min for 60 min, then water was added and stirred for 20 min, and the mixture was cooled to room temperature and filtered to obtain the product.

[0032] Comparative Example 6 Spinning oil TMT-217L imported from Japan.

[0033] The spin finishes prepared in Examples 1-3 and Comparative Examples 1-5, as well as commercially available finishes, were tested using the following methods: a) Light transmittance: Using a UV / Vis spectrometer at 660 nm, the particle uniformity and stability of a 15% emulsion were examined; b) Volatility loss: 1.0 ml of the finish sample was dropped onto a steel test piece, the sample was baked in an oven at 230°C for 40 minutes, and the residue was measured by the percentage of residue remaining; c) The spin finish was heated in a sand bath at 300°C for 3 hours, followed by further heating at 500°C in an electric furnace for 5 hours. The heating residue rate was calculated based on the weight change before and after heating. The results are shown in Table 2.

[0034] The polyester polymer was melted and the spinning oils prepared in Examples 1-3 and Comparative Examples 1-5 and a commercially available oil were applied at a rate of 0.8% using a guided oiling method. The resulting filaments were then stretched using a hot roller at 140°C to obtain polyethylene terephthalate (FDY) filaments having a fineness of 83d / 36f (number of filaments). The uniformity and static friction coefficient of the produced filaments were tested, and the results are shown in Table 2. The uniformity of the filaments was characterized by measuring the change in capacitance when the filaments were driven at 50 cm / min through a parallel plate capacitance sensor, using the prior art method.

[0035] Table 2 Physical and chemical properties of spinning oils and their impact on yarn production As can be seen from Table 2, compared with Comparative Examples 1 and 2, due to the specific ratio of the composite smoothing agent in Examples 1-3 of the present application, the final transmittance is relatively high and is basically equivalent to that of Comparative Example 4, indicating that the spinning oil prepared by the present invention has good emulsion stability; relative to Example 1, in Examples 2 and 3, an anionic fluorinated anionic surfactant is selected as the penetrant, in which the negatively charged sulfonate group is adsorbed on the interface through electrostatic action, which can significantly reduce the surface tension of the final spinning oil, effectively avoiding the accumulation of oil stains on the 500°C radiant heat heater, and also enables the oil to form a more uniform lubricating film layer on the fiber surface, thereby significantly reducing the yarn breakage rate; in addition, the reduction of oil stains can significantly extend the cleaning cycle of the heater, while ensuring that the heater has good heat conduction efficiency.

[0036] For Comparative Examples 3 and 4, when conventional mineral oil is used, although the thermal stability, % and 500°C heating residue rate of the spinning oil are comparable to those of Examples 1-3, the transmittance is significantly reduced, indicating that the emulsion stability of the final spinning oil is poor. At the same time, the uniformity of the prepared yarn is reduced, and the static friction coefficient is increased, indicating that the yarn quality is not ideal. For Comparative Example 5, although the only difference from Example 1 is the order of adding materials in the preparation method, there are also significant differences in the physical and chemical properties of the final spinning oil, especially the transmittance, indicating that changing the process sequence will affect the emulsion stability of the final oil. In fact, even if the order of adding materials is slightly adjusted, the final transmittance will be affected. Due to space limitations, this will not be repeated. The friction coefficient of the yarn produced using the spinning oil prepared in Examples 1-3 of the present application is reduced and the uniformity is improved, even better than imported oils, and the quality and performance of the yarn are improved.

[0037] Although the present invention is disclosed as above, the present invention is not limited thereto. Any person skilled in the art can make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, the scope of protection of the present invention should be based on the scope defined by the claims.

Claims

1. A crude oil direct oiling type spinning oil, characterized in that: The invention comprises 65-75% of a composite smoothing agent, wherein the composite smoothing agent is composed of 25-35 parts of tetradecyl tetradec-9-enoate and 65-75 parts of PEG-12 dipalmitate.

2. The crude oil direct oiling type spinning oil according to claim 1, characterized in that The crude oil direct oiling type spinning oil comprises 65-75 parts of a composite smoothing agent, 10-15 parts of an emulsifier, 2-4 parts of a penetrant, 2-6 parts of an antistatic agent, and 6-10 parts of a solvent, wherein the composite smoothing agent comprises 25-35 parts of tetradecyl tetradec-9-enoate and 65-75 parts of PEG-12 dipalmitate, and the solvent is water.

3. The crude oil direct oiling type spinning oil according to claim 2, characterized in that: The emulsifier is selected from at least one of fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ether, cardanol polyoxyethylene ether, castor oil polyoxyethylene ether, sorbitan fatty acid ester, sorbitan polyoxyethylene ether fatty acid ester or polyethylene glycol fatty acid ester.

4. The crude oil direct oiling type spinning oil according to claim 2, characterized in that: The penetrant is at least one of fatty alcohol polyoxyethylene ether, potassium perfluorooctane sulfonate, and sodium perfluorooctane sulfonate.

5. The crude oil direct oiling type spinning oil according to claim 2, characterized in that: The antistatic agent is selected from at least one of alkyl alcohol phosphate polyoxyethylene ether, alkyl alcohol phosphate, alkyl alcohol sulfonate, alkyl alcohol polyoxyethylene ether sulfonate, alkyl alcohol sulfate, alkyl alcohol ether sulfate salt and alkyl alcohol ether carboxylate fatty amine polyoxyethylene ether, alkyl alcohol ammonium oxide or betaine.

6. The crude oil direct oiling type spinning oil according to claim 1, characterized in that The pH value of the crude oil direct oiling type spinning oil is 7.5-8.

0.

7. The method for preparing the crude oil direct oiling type spinning oil according to any one of claims 1 to 6, characterized in that: The method comprises the following steps: adjusting the temperature in the reaction kettle to 38-45 DEG C, adding a composite smoothing agent in appropriate amount, stirring at 800-1400 rad / min for 10-50 minutes, then adding an antistatic agent and stirring for 10-40 minutes, then adding a solvent and a penetrant and stirring for 20-50 minutes, and finally adding an emulsifier and stirring for 30-90 minutes, cooling to room temperature and filtering to obtain the product.

8. The method for preparing a crude oil direct oiling type spinning oil according to claim 7, characterized in that: The method comprises the following steps: adjusting the temperature in the reaction kettle to 40-45° C., adding a composite smoothing agent in appropriate amount, stirring at 800-1200 rad / min for 10-30 minutes, then adding an antistatic agent and stirring for 10-20 minutes, then adding a solvent and a penetrant and stirring for 20-40 minutes, and finally adding an emulsifier and stirring for 30-60 minutes, cooling to room temperature, and filtering to obtain the product.

9. Use of the crude oil-based spinning oil according to any one of claims 1 to 6 in a spinning production process.

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