Polyether for polyester DTY (Draw Textured Yarn) oiling agent as well as preparation method and application thereof
The polyester DTY oiling agent prepared under specific conditions uses polyether as an emulsifier, which solves the stability and thermal stability problems of existing DTY oiling agents, improves the anti-yellowing performance and fiber bundle properties of the oiling agent, and achieves good processing results.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-19
- Publication Date
- 2026-04-03
AI Technical Summary
Existing DTY oils suffer from insufficient stability, poor thermal stability, easy yellowing, and poor smoothness, which affect the fiber processing effect.
A polyether for polyester DTY oiling was prepared by using a compound containing active hydrogen groups as an initiator and a bimetallic cyanide (DMC) as a catalyst to polymerize with propylene oxide and ethylene oxide under specific pressure and temperature. This polyether was then used as an emulsifier in combination with base oil, antistatic agent, and antisplatter agent to prepare polyester DTY oiling.
The prepared polyester DTY oil has good stability, anti-yellowing properties, smoothness and bundling properties, and good washability, which improves the stability and quality of fiber processing.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of polyester DTY oiling technology, specifically to a polyether for polyester DTY oiling, its preparation method, and its uses. Background Technology
[0002] Polyester filament is the largest branch of the chemical fiber industry. With its easy-washing and quick-drying properties, durability, good elasticity, light resistance, and corrosion resistance, it is widely used in clothing, home textiles, and industrial textiles. During the spinning process of polyester products after monomer polymerization, DTY oil can adjust the friction between fibers and between fibers and metal, reducing the coefficient of friction and minimizing static electricity generated by friction. This results in fibers with good bundle properties, smoothness, and splitting ability, meeting the needs of subsequent fiber processing.
[0003] However, existing DTY oils still have some problems in practical applications. Some oils lack stability and are prone to stratification during storage, leading to uneven distribution of active ingredients and affecting their performance. Some oils have poor thermal stability and are prone to yellowing at high temperatures. Others have poor smoothness, which can easily cause filament breakage, monofilament breakage, or fraying. Therefore, it is necessary to find a polyester DTY oil with good stability and excellent performance. Summary of the Invention
[0004] This invention provides a polyether for polyester DTY oiling agents, a preparation method thereof, and its uses. DTY oiling agents using the polyether prepared by this invention as emulsifiers are odorless and have good stability, anti-yellowing properties, smoothness, clumping properties, and washability.
[0005] In a first aspect, this application provides a method for preparing polyether for polyester DTY oiling agents, comprising the following steps: A compound containing active hydrogen groups was used as an initiator, and a bimetallic cyanide (DMC) was used as a catalyst. The mixture was polymerized with an epoxy mixture at a pressure of 0~0.3MPa and a temperature of 120℃~150℃ to obtain the polyether for polyester DTY oiling agent. The epoxy mixture comprises propylene oxide (PO) and ethylene oxide (EO), wherein the mass ratio of propylene oxide to ethylene oxide is 1:(1.2~3).
[0006] In one possible implementation, the mass of the bimetallic cyanide accounts for 20 to 50 ppm of the sum of the mass of the initiator and the epoxy mixture, preferably 30 ppm; In one possible implementation, the bimetallic cyanide includes zinc-cobalt bimetallic cyanide (Zn-CoDMC).
[0007] In one possible implementation, the mass ratio of propylene oxide to ethylene oxide is 1:(1.5~1.8). In one possible implementation, the pressure is 0.18~0.22 MPa; In one possible implementation, the temperature is 130°C to 150°C.
[0008] In one possible implementation, the mass of the initiator added is 25% to 35% of the total mass of the initiator and epoxy mixture.
[0009] In one possible implementation, the compound containing an active hydrogen group includes one or more of isooctanol, C8-10 mixed alcohols, C12-14 mixed alcohols, lauryl alcohol, isodecanol, and isodecanool, preferably isodecanool.
[0010] In one possible implementation, after the polymerization reaction is completed, the product is refined to obtain the polyester DTY oiling polyether.
[0011] In one possible implementation, the purification includes one or both of filtration and centrifugation, preferably, the supernatant is collected after centrifugation.
[0012] Secondly, this application provides a polyether for polyester DTY oil prepared according to the preparation method described above.
[0013] Thirdly, this application provides a polyester DTY oiling agent, comprising, by weight percentage: 85.0%~92.7% base oil, 0.1%~1.0% antistatic agent, 0.2%~1.0% antisplatter agent, and 6.0%~14.7% emulsifier; The emulsifier includes the polyether for polyester DTY oiling.
[0014] In one possible implementation, the base oil comprises 87.0% to 92.7%; In one possible implementation, the antistatic agent is 0.1% to 0.5%; In one possible implementation, the anti-splatter agent is 0.2% to 0.5%; In one possible implementation, the emulsifier is 7% to 12%; In one possible implementation, the base oil comprises one or more of industrial white oil, dioctyl sebacate, and trimethylolpropane tris(3-mercaptopropionate); In one possible implementation, the antistatic agent includes one or more of potassium phenolate phosphate and potassium dodecyl phosphate. In one possible implementation, the anti-splatter agent includes one or more of EPDM rubber and polymethacrylate.
[0015] The technical solution of this invention has the following advantages: 1. The preparation method of the polyester DTY oiling agent polyether provided by the present invention includes the following steps: using a compound containing an active hydrogen group as an initiator, using a bimetallic cyanide as a catalyst, and performing a polymerization reaction with an epoxy mixture at a pressure of 0~0.3MPa and a temperature of 120℃~150℃ to obtain the polyester DTY oiling agent polyether; the epoxy mixture includes propylene oxide and ethylene oxide, and the mass ratio of propylene oxide to ethylene oxide is 1:(1.2~3).
[0016] Polyether is one of the main components in the preparation of polyester DTY oil. As an emulsifier in DTY oil, the quality of polyether directly affects the product quality of DTY oil. This application combines a specific ratio of PO / EO with a specific type of catalyst to prepare a polyether that, when used in DTY oil, results in good stability, excellent anti-yellowing properties, good binding and washability, and is also environmentally friendly and biodegradable. Detailed Implementation
[0017] The following embodiments are provided to better understand the present invention, but the following embodiments do not constitute a limitation on the content and scope of protection of the present invention. Any product that is the same as or similar to the present invention, derived by any person under the guidance of the present invention or by combining the features of the present invention with other prior art, falls within the scope of protection of the present invention.
[0018] Unless otherwise specified, all experimental steps or conditions in the examples were performed according to conventional experimental procedures and conditions in the art. Reagents or instruments whose manufacturers are not specified are all commercially available products.
[0019] Raw material source: C8-C10 fatty alcohols were purchased from Maclean's, catalog number A913421, analytical grade; Propylene oxide and ethylene oxide were purchased from Wanhua Chemical, industrial grade. DMC (zinc-cobalt bimetallic cyanide) was purchased from Jiangsu Bade Polyurethane Co., Ltd., industrial grade; Industrial white oil was purchased from Chuanhua Chemical Co., Ltd., industrial grade. Potassium phenol ether phosphate salt, purchased from KBT Chemical, industrial grade; Trimethylolpropane tris(3-mercaptopropionate), dioctyl sebacate, potassium dodecyl phosphate, and polymethacrylate were all purchased from Aladdin and were of analytical grade. EPDM rubber, purchased from Shenyang Elapex Chemical Co., Ltd., industrial grade.
[0020] Example 1 This embodiment provides a method for preparing polyether for polyester DTY oiling agents, including the following steps: 144g of C8-C10 fatty alcohol and 30ppm of DMC (i.e., DMC accounts for 30ppm of the total mass of the C8-C10 fatty alcohol and epoxy mixture) were added to a 5L stainless steel reactor. Nitrogen purging was performed, and the oxygen content inside the reactor was measured to be below 100ppm. The reactor was heated to 130℃ and the pressure was set to 0.2±0.02MPa. An epoxy mixture (containing 145g of propylene oxide and 218g of ethylene oxide) was continuously added for random copolymerization. The reaction temperature was maintained at 130℃ until the pressure inside the reactor stopped decreasing (because the addition of the epoxy mixture generates gaseous epoxy, causing the pressure inside the reactor to rise; when the pressure inside the reactor stops decreasing, the gaseous epoxy mixture is considered to be completely consumed, and the reaction ends). After the reaction is stopped, the temperature is lowered to 80°C, acetic acid is added to neutralize to pH 6-8, vacuum degassing is performed, the material is cooled and discharged, and the product undergoes two-step purification: first, filtration is performed to remove salts, and then the supernatant is collected by centrifugation to obtain the polyether for polyester DTY oiling.
[0021] The polyether prepared in this embodiment has the following characteristics: number average molecular weight: 505 g / mol, moisture content: <1 wt%, hydroxyl value: 101 mg KOH / g, pH: 6.3.
[0022] This embodiment also provides a polyester DTY oiling agent, which, by weight percentage, consists of the following components: 90% base oil industrial white oil, 0.1% antistatic agent potassium phenol ether phosphate, 0.2% antisplatter agent EPDM rubber, and 9.7% emulsifier (polyether obtained in Example 1).
[0023] The above-mentioned method for preparing polyester DTY oil is as follows: Emulsifier, antistatic agent and antisplatter agent are added to the reaction vessel in proportion and stirred at 500 r / min for 1 h at 60℃; then the base oil is added to the reaction vessel and stirred for another 50 min. After stirring evenly, the mixture is naturally cooled to obtain polyester DTY oil.
[0024] Example 2 This embodiment provides a method for preparing polyether for polyester DTY oiling agents, including the following steps: 158g of isomeric decaol and 30ppm of DMC were added to a 5L stainless steel reactor, and nitrogen purging was performed. The oxygen content inside the reactor was measured to be below 100ppm. The reactor was heated to 130℃ and the pressure was 0.2±0.01MPa. An epoxy mixture (containing 145g of propylene oxide and 261g of ethylene oxide) was continuously added for random copolymerization. The reaction temperature was maintained at 130℃ until the pressure inside the reactor no longer decreased. After the reaction was stopped, the temperature was lowered to 80℃, acetic acid was added to neutralize to pH 6-8, vacuum degassing was performed, and the product was discharged after cooling. The product underwent two-step purification: first, filtration was performed to remove salts, and then the supernatant was collected by centrifugation to obtain the polyether for DTY oils.
[0025] The polyether prepared in this embodiment has a number average molecular weight of 567 g / mol, moisture content of <1 wt%, hydroxyl value of 92 mg KOH / g, and pH of 6.
[0026] A polyester DTY oiling agent, by weight percentage, is composed of the following components: 89% base oil dioctyl sebacate, 0.3% antistatic agent potassium phenol ether phosphate, 0.5% antisplatter agent polymethyl methacrylate, and 10.2% emulsifier (polyether obtained in Example 2).
[0027] The above-mentioned method for preparing polyester DTY oil is as follows: Emulsifier, antistatic agent and antisplatter agent are added to the reaction vessel in proportion and stirred at 500 r / min for 1 h at 60℃; then the base oil is added to the reaction vessel and stirred for another 50 min. After stirring evenly, the mixture is naturally cooled to obtain polyester DTY oil.
[0028] Example 3 This embodiment provides a method for preparing polyether for polyester DTY oiling agents, including the following steps: 186g of lauryl alcohol and 30ppm of DMC were added to a 5L stainless steel reactor, and nitrogen purging was performed. The oxygen content inside the reactor was measured to be below 100ppm. The reactor was heated to 130℃ and the pressure was 0.2±0.01MPa. An epoxy mixture (containing 145g of propylene oxide and 290g of ethylene oxide) was continuously added for random copolymerization. The reaction temperature was maintained at 130℃ until the pressure inside the reactor no longer decreased. After the reaction was stopped, the temperature was lowered to 80℃, acetic acid was added to neutralize to pH 6-8, vacuum degassing was performed, and the product was discharged after cooling. The product underwent two-step purification: first, filtration was performed to remove salts, and then the supernatant was collected by centrifugation to obtain the polyether for DTY oils.
[0029] The polyether prepared in this embodiment has a number average molecular weight of 619 g / mol, a moisture content of <1 wt%, a hydroxyl value of 91 mg KOH / g, and a pH of 6.
[0030] A polyester DTY oiling agent, by weight percentage, is composed of the following components: The base oil is trimethylolpropane tris(3-mercaptopropionate) 91%, the antistatic agent is potassium dodecyl phosphate 0.5%, the antisplatter agent is ethylene propylene diene monomer (EPDM) 0.5%, and the emulsifier (polyether obtained in Example 3) is 8.0%.
[0031] The above-mentioned method for preparing polyester DTY oil is as follows: Emulsifier, antistatic agent and antisplatter agent are added to the reaction vessel in proportion and stirred at 500 r / min for 1 h at 60℃; then the base oil is added to the reaction vessel and stirred for another 50 min. After stirring evenly, the mixture is naturally cooled to obtain polyester DTY oil.
[0032] Comparative Example 1 This comparative example provides a method for preparing polyether for polyester DTY oiling agents, which is basically the same as that in Example 1, except that the amount of propylene oxide added is 191g and the amount of ethylene oxide added is 172g, that is, the mass ratio of propylene oxide to ethylene oxide is 1:0.9.
[0033] The content of polyester DTY oil components and the preparation method in this comparative example are the same as in Example 1.
[0034] Comparative Example 2 This comparative example provides a method for preparing polyether for polyester DTY oiling agents, which is basically the same as that in Example 1, except that the amount of propylene oxide added is 72.6g and the amount of ethylene oxide added is 290.4g, that is, the mass ratio of propylene oxide to ethylene oxide is 1:4.
[0035] The content of polyester DTY oil components and the preparation method in this comparative example are the same as in Example 1.
[0036] The polyester DTY oil prepared in this comparative example is a pale yellow, turbid, oily liquid.
[0037] Comparative Example 3 This comparative example provides a method for preparing polyether for polyester DTY oiling agents, which is basically the same as that in Example 1, except that the catalyst used is the alkali metal catalyst sodium methoxide.
[0038] The content of polyester DTY oil components and the preparation method in this comparative example are the same as in Example 1.
[0039] Comparative Example 4 The imported oil is selected from Matsumoto's polyester DTY oil from Japan.
[0040] Test case The polyester DTY oiling agents of each embodiment and comparative example were tested: stability: (1) Appearance: Turbidity measured by a turbidity meter is less than 3 NTU, which is considered to be clear and transparent.
[0041] (2) High temperature stability: After baking the oil at 160℃ for 0h, 6h, 12h and 24h respectively, observe whether the color of the oil changes.
[0042] Smoke temperature: Thermogravimetric analysis is used to determine the thermal decomposition initiation temperature (i.e. the initial smoke temperature) of the oil by monitoring the mass change of the oil during the heating process.
[0043] Volatilization loss: Bake in an oven at 160℃ for 6 hours, compare the weight difference before and after baking, and calculate the percentage of weight loss.
[0044] Surface tension: The surface tension of 1 g / L polyether emulsifier at 25°C was tested using the platinum plate method.
[0045] Breakage rate: refers to the number of times a filament breaks per unit time (or per unit output) during DTY production. It is mainly affected by the smoothness (reducing friction between the filament and the equipment), antistatic properties (preventing breakage caused by static electricity), and cohesion (preventing monofilament dispersion) of the oil. The production process is simulated using a small texturing test machine to test the effect of the oil on the breakage rate.
[0046] Filament count: refers to the number of broken or detached monofilaments on the surface of DTY yarn (e.g., the number of filaments per meter of yarn). It is mainly affected by the lubricating properties of the oil (reducing friction between fibers), film-forming properties (forming a uniform oil film to coat the monofilaments), and anti-entanglement properties (preventing yarns from sticking together). The number of broken monofilaments (filament count) is counted by observing the cross-section or longitudinal section of the yarn under a microscope.
[0047] Bundling property refers to the cohesive force of the oiling agent on the fibers, reflecting the fiber's ability to maintain the integrity of the fiber bundle during processing (such as stretching and texturing) and post-processing (such as weaving). Its core principle is to assess the bundling effect of the oiling agent by evaluating the degree of fiber cross-section dispersion. Using an industry-standard testing method, oil-free fibers are immersed in an oiling agent solution, ensuring the oiling agent adheres evenly to the fiber surface. Subsequently, the fiber bundle is sheared under tension, and the dispersion of the cross-section is observed. The less dispersion, the better the bundling property.
[0048] Washability refers to the ease with which oil can be removed from the fiber surface, directly affecting the efficiency of subsequent processing (such as dyeing and finishing) and product quality (such as dyeing uniformity). Its core principle is to assess the washability of oil by measuring the difference in oil content before and after washing. A soap washing device (such as a small laboratory washing machine) is used, with neutral soap solution (2g / L) added at a liquor ratio of 1:50, and the washing process lasting 10 minutes. The oil content before and after washing is then observed.
[0049] The test results are shown in Table 1.
[0050] Table 1
[0051] The appearance is clear and not cloudy, proving that it does not separate into layers.
[0052] As can be seen from the table, the polyester DTY oil prepared by the polyether emulsifier provided by the present invention has no odor, good stability, anti-yellowing properties, and clumping properties, and good washability.
[0053] The oil in Comparative Example 1 was pale yellow when baked at 160℃ for 0 hours, turned yellow after 12 hours, and turned brownish-yellow after 24 hours, indicating poor high-temperature thermal stability.
[0054] In Comparative Example 2, after increasing the specific gravity of ethylene oxide, the prepared oil became cloudy and uneven, making it unusable.
[0055] The oil agent in Comparative Example 3 showed good high-temperature stability, but during use, the breakage rate and the number of filaments increased significantly, indicating that the oil agent was not very effective for polyester.
[0056] Comparative Example 4 is a DTY polyester oiling agent imported from Matsumoto, Japan. As can be seen from Table 1, the performance of this patented embodiment is superior to that of the imported oiling agent in many aspects, especially in the process of use, where it exhibits excellent performance.
[0057] Obviously, the above embodiments are merely illustrative examples for clear explanation and are not intended to limit the implementation. Those skilled in the art will recognize that other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all possible implementations here. However, obvious variations or modifications derived therefrom are still within the scope of protection of this invention.
Claims
1. A method for preparing a polyether for polyester DTY oiling agents, characterized in that, Includes the following steps: A compound containing active hydrogen groups was used as an initiator and a bimetallic cyanide was used as a catalyst. The mixture was polymerized with an epoxy compound at a pressure of 0~0.3MPa and a temperature of 120℃~150℃ to obtain the polyether for polyester DTY oiling agent. The epoxy mixture includes propylene oxide and ethylene oxide, wherein the mass ratio of propylene oxide to ethylene oxide is 1:(1.2~3).
2. The method for preparing polyether for polyester DTY oiling agents according to claim 1, characterized in that, The mass of the bimetallic cyanide accounts for 20-50 ppm of the sum of the mass of the initiator and the epoxy mixture; and / or The bimetallic cyanides include zinc-cobalt bimetallic cyanides.
3. The method for preparing polyether for polyester DTY oiling agents according to claim 1, characterized in that, At least one of the following conditions must be met: (1) The mass ratio of propylene oxide to ethylene oxide is 1:(1.5~1.8); (2) The pressure is 0.18~0.22MPa; (3) The temperature is 130℃~150℃.
4. The method for preparing the polyether for polyester DTY oiling agents according to claim 1, characterized in that, The mass of the initiator added is 25% to 35% of the total mass of the initiator and epoxy mixture.
5. The method for preparing the polyether for polyester DTY oiling agents according to any one of claims 1-4, characterized in that, The compound containing an active hydrogen group includes one or more of isooctanol, C8-10 mixed alcohols, C12-14 mixed alcohols, lauryl alcohol, isododecyl alcohol, and isodecayl alcohol, preferably isodecayl alcohol.
6. The method for preparing the polyether for polyester DTY oiling agents according to any one of claims 1-4, characterized in that, After the polymerization reaction is completed, the product is refined to obtain the polyester DTY oiling polyether.
7. The method for preparing the polyether for polyester DTY oiling agents according to claim 6, characterized in that, The purification process includes one or both of filtration and centrifugation, preferably, the supernatant is collected after centrifugation.
8. A polyether for polyester DTY oiling prepared by the method according to any one of claims 1-7.
9. A polyester DTY oiling agent, characterized in that, It comprises, by weight percentage: base oil 85.0%~92.7%, antistatic agent 0.1%~1.0%, antisplatter agent 0.2%~1.0%, and emulsifier 6.0%~14.7%; The emulsifier includes the polyether for polyester DTY oiling as described in claim 8.
10. The polyester DTY oiling agent according to claim 9, characterized in that, At least one of the following conditions must be met: (1) Base oil 87.0%~92.7%; (2) Antistatic agent 0.1%~0.5%; (3) Anti-splatter agent 0.2%~0.5%; (4) Emulsifier 7%~12%; (5) The base oil includes one or more of industrial white oil, dioctyl sebacate, and trimethylolpropane tris(3-mercaptopropionate); (6) The antistatic agent includes one or more of potassium salt of phenolic ether phosphate and potassium salt of dodecyl phosphate; (7) The anti-splatter agent includes one or more of EPDM rubber and polymethyl methacrylate.