An environment-friendly weather-resistant polyester oil agent and its preparation method

Abstract

The present invention relates to an environment-friendly weather-resistant polyester oil agent and a preparation method thereof, belonging to the technical field of textile fiber auxiliaries. The polyester oil agent comprises, by weight: 30-40 parts of high-addition polyoxyethylene hydrogenated castor oil, 1-2 parts of antistatic agent, 3-5 parts of stabilizer, 7-10 parts of wetting agent, 12-15 parts of bundling agent, and 38-45 parts of deionized water; the high-addition polyoxyethylene hydrogenated castor oil uses hydrogenated castor oil as a raw material, modifies the castor oil through highly active phosphorus oxychloride to introduce a phosphorus-containing group, and improves the temperature resistance of the addition product; the phosphorus-containing group has a good chelating effect on the metal-based catalyst, enabling the catalyst to be enriched at the addition site, fully exerting the catalytic effect with a small addition amount, effectively increasing the addition amount of ethylene oxide and hydrogenated castor oil, and the prepared addition product shows excellent temperature and weather resistance in tests.

Description

Technical Field

[0001] The present invention belongs to the technical field of textile fiber auxiliaries, and specifically relates to an environmentally friendly weather-resistant polyester spinning oil and a preparation method thereof. Background Art

[0002] Polyester fully drawn yarn (FDY) is a main variety of synthetic fibers. In the process of producing polyester FDY, a spinning oil must be used, and its function is to endow the fibers with good smoothness, bundling property, and antistatic property to meet the requirements of fiber processing. At present, the FDY spinning oils used by major polyester filament production enterprises are almost provided by Japanese and German manufacturers.

[0003] Polyoxyethylene hydrogenated castor oil is a macromolecular emulsifier, which is prepared by the addition of hydrogenated castor oil and ethylene oxide. It is generally used in the cosmetics industry and the printing and dyeing industry. There are also studies on adding it to polyester spinning oils to improve the smoothness. However, during the polyester spinning process, when the speed reaches 2500 - 3500 m / min, the filament is subjected to high-speed shearing by the friction disk, generating a large amount of heat. The existing polyoxyethylene hydrogenated castor oil as a smoothing agent has poor temperature and weather resistance to meet the production requirements. Therefore, this application aims to develop a polyoxyethylene hydrogenated castor oil with high addition and compound it with other auxiliaries to prepare a polyester spinning oil. Summary of the Invention

[0004] In order to solve the technical problems mentioned in the background art, the purpose of the present invention is to provide an environmentally friendly weather-resistant polyester spinning oil and a preparation method thereof.

[0005] The purpose of the present invention can be achieved by the following technical solutions:

[0006] An environmentally friendly weather-resistant polyester spinning oil, comprising the following components by weight:

[0007] 30 - 40 parts of high-addition polyoxyethylene hydrogenated castor oil, 1 - 2 parts of antistatic agent, 3 - 5 parts of stabilizer, 7 - 10 parts of wetting agent, 12 - 15 parts of bundling agent, and 38 - 45 parts of deionized water;

[0008] The high-addition polyoxyethylene hydrogenated castor oil is prepared by the following method:

[0009] Step A1: Mix hydrogenated castor oil with acetone, keep it at a constant temperature of 5 - 8 °C, apply high-speed stirring at 400 - 500 rpm, slowly add phosphorus oxychloride, control the overall addition reaction time to be 2 - 3 h, and let phosphorus oxychloride react with the hydroxyl groups in the molecular structure of hydrogenated castor oil to introduce a phosphorus-containing group. After the reaction, add deionized water for washing and rotary evaporation under reduced pressure to remove the solvent and decompose phosphorus oxychloride to obtain phosphorus-modified castor oil;

[0010] Further, the dosage ratio of hydrogenated castor oil, phosphorus oxychloride and acetone is 100 g: 1.8 - 2.1 mL: 240 - 280 mL.

[0011] Step A2: Mix the phosphorus-modified castor oil, metal-based catalyst and sulfolane, introduce nitrogen protection, heat up to 160 - 180 °C, introduce ethylene oxide and sodium hydroxide and increase the pressure to 0.7 - 0.9 MPa, react until the system pressure is constant, cool down to 100 °C, release the pressure and dropwise add glacial acetic acid for neutralization, discharge the material into boiling water for washing, cooling and drying, and slicing to obtain high-addition polyoxyethylene hydrogenated castor oil;

[0012] Further, the dosage ratio of phosphorus-modified castor oil, metal-based catalyst, sodium hydroxide and sulfolane is 100 g: 0.45 - 0.55 g: 3 - 5 g: 120 - 150 mL.

[0013] The metal-based catalyst is prepared by the following method:

[0014] Step B1: Dissolve cerium nitrate and ferric chloride in deionized water, heat up to 60 - 70 °C, introduce hot ammonia for aeration, and slowly add titanium dioxide at the same time, control the aeration reaction time to be 45 - 50 min, after the reaction ends, centrifuge to take the bottom precipitate and dry it to constant weight, heat up to 520 - 550 °C under nitrogen protection and calcine for 4 - 5 h, cool and then grind to obtain the composite matrix;

[0015] Further, the dosage ratio of cerium nitrate, ferric chloride and titanium dioxide is 10 mmol: 20 - 35 mmol: 8 - 12 mg, and the aeration ratio of hot ammonia is 0.12 - 0.15 vvm.

[0016] Step B2: Stir and hydrolyze (N,N-dimethyl-3-aminopropyl)trimethoxysilane and alkaline ethanol solution, add the composite matrix and stir at high speed, let it stand for 12 h, take the bottom precipitate, wash it with deionized water and dry it, then add methyl iodide and tetrahydrofuran, apply mechanical stirring at 200 - 300 rpm, heat up to 70 - 75 °C and reflux for 24 h, cool and then centrifuge to separate the precipitate, wash it with methanol and dry it to obtain the metal-based catalyst;

[0017] Further, the dosage ratio of the composite matrix, (N,N-dimethyl-3-aminopropyl)trimethoxysilane and methyl iodide is 1 g: 1.5 - 1.8 mL: 20 - 25 mL.

[0018] A preparation method of an environmentally friendly weather-resistant polyester oil agent specifically includes the following steps:

[0019] Step S1: Mix the high-addition polyoxyethylene hydrogenated castor oil and deionized water, heat up to 60 °C and stir at high speed for emulsification to obtain an emulsion;

[0020] Step S2: Mix other raw materials, add them to the emulsion under stirring, mix well, cool and filter to obtain an environment-friendly weather-resistant polyester finishing oil.

[0021] Advantages of the present invention:

[0022] The present invention synthesizes an iron-titanium oxide-cerium hydroxide composite material by a hydrothermal method. It is found in long-term experimental studies that it has good catalytic effects on the addition of polyoxyethylene castor oil. Through coupling with (N,N-dimethyl-3-aminopropyl)trimethoxysilane and then treating with methyl iodide for quaternary ammonium modification on the surface, the compatibility with the oil phase is improved, and at the same time, the ring-opening reaction of the epoxy group is promoted, so that the catalytic effect can be fully exerted, which is beneficial to improving the degree of addition.

[0023] In addition, in the present invention, hydrogenated castor oil is used as a raw material, and the castor oil is modified by highly active phosphorus oxychloride to introduce a phosphorus-containing group, thereby improving the temperature resistance of the addition product. At the same time, the phosphorus-containing group has a good chelating effect on the metal-based catalyst, enabling the catalyst to be enriched at the addition site, fully exerting the catalytic effect with a small addition amount, effectively increasing the addition amount of ethylene oxide and hydrogenated castor oil, and thus improving its temperature and weather resistance. Specific embodiments

[0024] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art without creative efforts based on the embodiments of the present invention belong to the scope of protection of the present invention.

[0025] Example 1

[0026] In this example, an environment-friendly weather-resistant polyester finishing oil is prepared, and the specific implementation process is as follows:

[0027] 1) Preparation of metal-based catalyst

[0028] 1.1. Take cerium nitrate and ferric chloride and mix them, add 5 times the mass of deionized water and stir to dissolve. Heat the solution to 70 °C, and introduce ammonia gas preheated to 70 °C from the bottom through an air diffuser at an aeration ratio of 0.15 vvm. Slowly add titanium dioxide (with a fineness of 0.15 μm, the same below) from above, control the aeration reaction time to be 45 min, and the addition time of titanium dioxide is half of the aeration time. The dosage ratio of cerium nitrate, ferric chloride and titanium dioxide is 10 mmol: 35 mmol: 8 mg. After the aeration is completed, centrifuge to take the bottom precipitate and dry it to constant weight in an 80 °C drying oven, and then place it in an atmosphere furnace. Roast it at 550 °C for 4 h under a nitrogen atmosphere, and cool and dry-grind it to a fineness of not less than 1200 mesh to make a composite matrix.

[0029] 1.2. Prepare an alkaline ethanol solution with a volume concentration of 30% and a pH value of 8.5. Take (N,N-dimethyl-3-aminopropyl)trimethoxysilane and the alkaline ethanol solution and mix them in a volume ratio of 1:40. Assist with mechanical stirring for hydrolysis for 1 h. Then, control the stirring rate at 800 rpm, and uniformly add the composite matrix to the hydrolysis solution and stir at high speed until it becomes a suspension state. After standing for 12 h, remove the supernatant. Take the bottom precipitate and wash it repeatedly with deionized water until it is neutral. Then, place it in a drying oven at 60 °C and dry for 2 h. Take iodomethane and tetrahydrofuran and mix them in a volume ratio of 1:1.5. Then, add the dried product, apply mechanical stirring at 300 rpm, and heat up to 75 °C for reflux reaction for 24 h. Among them, the dosage ratio of the composite matrix, (N,N-dimethyl-3-aminopropyl)trimethoxysilane, and iodomethane is 1 g:1.8 mL:25 mL. After the reaction, cool it, centrifuge to separate the precipitate, wash it with methanol, and dry it to constant weight to prepare a metal-based catalyst.

[0030] 2) Prepare highly adducted polyoxyethylene hydrogenated castor oil

[0031] 2.1. Take hydrogenated castor oil (commercially available: Beijing Huawei Ruike Chemical Co., Ltd., AR grade reagent, CAS: 8001-78-3, the same below), add acetone, and apply mechanical stirring to mix and dilute. Keep it at a constant temperature of 8 °C, apply high-speed stirring at 500 rpm, and slowly add phosphorus oxychloride within 1.5 h. After adding, continue to stir and react, and control the overall addition and reaction time to 2 h. Among them, the dosage ratio of hydrogenated castor oil, phosphorus oxychloride, and acetone is 100 g:2.1 mL:280 mL. After the reaction, add deionized water with a mass 0.4 times that of the reaction system to wash, and remove the solvent and the decomposed phosphorus oxychloride by rotary evaporation under reduced pressure to prepare phosphorus-modified castor oil;

[0032] 2.2. Take phosphorus-modified castor oil, metal-based catalyst, and sulfolane, add them, and apply mechanical stirring to mix evenly. Introduce nitrogen for protection, heat up to 180 °C, introduce ethylene oxide and sodium hydroxide, and increase the pressure to 0.7 MPa. Among them, the dosage ratio of phosphorus-modified castor oil, metal-based catalyst, sodium hydroxide, and sulfolane is 100 g:0.55 g:5 g:150 mL. Keep the temperature for reaction until the pressure of the reaction system is constant, cool down to 100 °C, release the pressure, and add glacial acetic acid dropwise to neutralize. Drain the material and wash it in boiling water, cool it, remove the aqueous phase, and dry it with hot air. Take the dried product and cut it into slices to prepare highly adducted polyoxyethylene hydrogenated castor oil.

[0033] 3) Compound polyester finishing agent

[0034] This polyester finishing agent uses highly adducted polyoxyethylene hydrogenated castor oil as a leveling material, and the compounded auxiliaries include:

[0035] An antistatic agent, selected from potassium lauryl phosphate, chemical pure reagent;

[0036] Stabilizers, selected from coconut oil-modified alkyd resin (model: COS-2830X70) and aqueous silicone (BYK-024), are mixed at a mass ratio of 3:1;

[0037] Wetting agents, selected from linear alcohol polyoxyethylene ethers, SOFTANOL 90;

[0038] Bundle agents, selected from polyoxyethylene glycerol ether and polyoxyethylene pentaerythritol ether mixed at a mass ratio of 5:1;

[0039] The following examples use raw materials of the same batch.

[0040] 3.1. Weigh 360 g of highly adducted polyoxyethylene hydrogenated castor oil and 380 g of deionized water, heat up to 60 °C, and apply high-speed stirring at 800 rpm to make an emulsion;

[0041] 3.2. Weigh 20 g of antistatic agent, 30 g of stabilizer, 70 g of wetting agent and 140 g of bundle agent, mix them with a stirrer, stir the emulsion at 360 rpm, add the mixture to the emulsion at a uniform speed and stir evenly. After cooling to room temperature, filter through an 800-mesh filter to make an environmentally friendly weather-resistant polyester oil agent.

[0042] Example 2

[0043] The specific implementation process for preparing the environmentally friendly weather-resistant polyester oil agent in this example is as follows:

[0044] 1) Preparation of metal-based catalyst

[0045] 1.1. Mix cerium nitrate and ferric chloride, add 5 times the mass of deionized water and stir to dissolve. Heat the solution to 60 °C, and introduce ammonia preheated to 60 °C from the bottom through an air diffuser at an aeration ratio of 0.12 vvm. Slowly add titanium dioxide from above, control the aeration reaction time to be 50 min, and the addition time of titanium dioxide is half of the aeration time. The dosage ratio of cerium nitrate, ferric chloride and titanium dioxide is 10 mmol: 20 mmol: 12 mg. After the aeration is completed, centrifuge to obtain the bottom precipitate, place it in an 80 °C drying oven and dry to constant weight, then place it in a muffle furnace, heat it to 520 °C in a nitrogen atmosphere and calcine for 5 h. After cooling, grind it dry to a fineness of not less than 1200 mesh to make a composite matrix;

[0046] 1.2. Prepare an alkaline ethanol solution with a volume concentration of 30% and a pH value of 8.5. Take (N,N-dimethyl-3-aminopropyl)trimethoxysilane and the alkaline ethanol solution and mix them at a volume ratio of 1:40, and hydrolyze with mechanical stirring for 1 h. Then, control the stirring rate at 800 rpm, and uniformly add the composite matrix to the hydrolyzate and stir at high speed until it becomes a suspension state. After standing for 12 h, remove the supernatant. Take the bottom precipitate and wash it repeatedly with deionized water until it is neutral, then place it in a drying oven at 60 °C and dry for 2 h. Take methyl iodide and tetrahydrofuran and mix them at a volume ratio of 1:1, then add the dried product, apply mechanical stirring at 200 rpm, and heat up to 70 °C for reflux reaction for 24 h. Among them, the dosage ratio of the composite matrix, (N,N-dimethyl-3-aminopropyl)trimethoxysilane, and methyl iodide is 1 g:1.5 mL:20 mL. After the reaction, cool it, centrifuge to separate the precipitate, wash it with methanol, and dry it to a constant weight to prepare a metal-based catalyst.

[0047] 2) Prepare high-addition polyoxyethylene hydrogenated castor oil

[0048] 2.1. Take hydrogenated castor oil, add acetone, and mix and dilute it with mechanical stirring. Keep it at a constant temperature of 5 °C, apply high-speed stirring at 400 rpm, and slowly add phosphorus oxychloride within 2 h. After adding, continue to stir and react, and control the overall addition and reaction time to be 3 h. Among them, the dosage ratio of hydrogenated castor oil, phosphorus oxychloride, and acetone is 100 g:1.8 mL:240 mL. After the reaction, add deionized water with a mass 0.3 times that of the reaction system for washing, and remove the solvent and the decomposed phosphorus oxychloride by rotary evaporation under reduced pressure to prepare phosphorus-modified castor oil;

[0049] 2.2. Take phosphorus-modified castor oil, metal-based catalyst, and sulfolane, add them and mix them evenly with mechanical stirring, introduce nitrogen for protection, heat up to 160 °C, introduce ethylene oxide and sodium hydroxide and increase the pressure to 0.9 MPa. Among them, the dosage ratio of phosphorus-modified castor oil, metal-based catalyst, sodium hydroxide, and sulfolane is 100 g:0.45 g:3 g:120 mL. Keep the temperature for reaction until the pressure of the reaction system is constant, cool down to 100 °C, release the pressure, add glacial acetic acid dropwise for neutralization, discharge the material and wash it in boiling water, cool down to remove the aqueous phase, and dry it with hot air. Take the dried product and slice it to prepare high-addition polyoxyethylene hydrogenated castor oil.

[0050] 3) Compound polyester finishing agent

[0051] 3.1. Take 400 g of high-addition polyoxyethylene hydrogenated castor oil and 450 g of deionized water, add them, heat up to 60 °C, and apply high-speed stirring at 800 rpm to prepare an emulsion;

[0052] 3.2. Take 14 g of antistatic agent, 50 g of stabilizer, 90 g of wetting agent and 120 g of bundling agent, mix them with a stirrer, stir the emulsion at 240 rpm, add the mixture to the emulsion evenly and stir well. After cooling to room temperature, filter it through an 800-mesh filter to prepare an environmentally friendly weather-resistant polyester oil agent.

[0053] Example 3

[0054] In this example, an environmentally friendly weather-resistant polyester oil agent was prepared, and the specific implementation process is as follows:

[0055] 1) Prepare a metal-based catalyst

[0056] 1.1. Take cerium nitrate and ferric chloride and mix them. Add 5 times the mass of deionized water and stir to dissolve. Heat the dissolved solution to 66 °C, and introduce ammonia preheated to 70 °C from the bottom through an air supply pipe at an aeration ratio of 0.14 vvm. Slowly add titanium dioxide from above, control the aeration reaction time to be 48 min, and the addition time of titanium dioxide is half of the aeration time. The dosage ratio of cerium nitrate, ferric chloride and titanium dioxide is 10 mmol: 28 mmol: 10 mg. After the aeration ends, centrifuge to take the bottom precipitate and dry it to constant weight in an 80 °C drying oven. Then place it in an atmosphere furnace, heat it to 520 °C in a nitrogen atmosphere and calcine for 5 h. After cooling, grind it dry to a fineness of not less than 1200 mesh to prepare a composite matrix;

[0057] 1.2. Prepare an alkaline ethanol solution with a volume concentration of 30% and a pH value of 8.5. Take (N,N-dimethyl-3-aminopropyl) trimethoxysilane and the alkaline ethanol solution and mix them according to a volume ratio of 1:40. Assist with mechanical stirring and hydrolyze for 1 h. Then control the stirring rate to be 800 rpm, add the composite matrix to the hydrolyzate evenly and stir at high speed until it is in a suspension state. After standing for 12 h, remove the supernatant. Take the bottom precipitate and wash it repeatedly with deionized water until it is neutral. Then place it in a 60 °C drying oven and dry it for 2 h. Take iodomethane and tetrahydrofuran and mix them according to a volume ratio of 1:1.2, and then add the dried product. Apply mechanical stirring at 240 rpm and heat it to 72 °C for reflux reaction for 24 h. Among them, the dosage ratio of the composite matrix, (N,N-dimethyl-3-aminopropyl) trimethoxysilane and iodomethane is 1 g: 1.6 mL: 22 mL. After the reaction, cool it, centrifuge to separate the precipitate, wash it with methanol and dry it to constant weight to prepare a metal-based catalyst.

[0058] 2) Prepare highly adducted polyoxyethylene hydrogenated castor oil

[0059] 2.1. Take hydrogenated castor oil, add acetone, and apply mechanical stirring to mix and dilute. Keep it at a constant temperature of 5°C, apply high-speed stirring at 500 rpm, and slowly add phosphorus oxychloride within 2 h. After adding, continue stirring and reacting, and control the overall addition reaction time to be 2.5 h. Among them, the dosage ratio of hydrogenated castor oil, phosphorus oxychloride, and acetone is 100 g: 1.9 mL: 260 mL. After the reaction ends, add deionized water with a mass 0.4 times that of the reaction system for washing, and remove the solvent and decomposed phosphorus oxychloride by rotary evaporation under reduced pressure to prepare phosphorus-modified castor oil;

[0060] 2.2. Take phosphorus-modified castor oil, metal-based catalyst, and sulfolane, add them and apply mechanical stirring to mix evenly. Introduce nitrogen for protection, heat up to 170°C, introduce ethylene oxide and sodium hydroxide, and increase the pressure to 0.8 MPa. Among them, the dosage ratio of phosphorus-modified castor oil, metal-based catalyst, sodium hydroxide, and sulfolane is 100 g: 0.48 g: 4 g: 150 mL. Keep the temperature for reaction until the pressure of the reaction system is constant, cool down to 100°C, release the pressure, add glacial acetic acid dropwise for neutralization, discharge the material into boiling water for washing, cool to remove the aqueous phase, and dry with hot air. Take the dried product and cut it into slices to prepare highly adducted polyoxyethylene hydrogenated castor oil.

[0061] 3) Compound polyester oil agent

[0062] 3.1. Take 300 g of highly adducted polyoxyethylene hydrogenated castor oil and 420 g of deionized water, add them, heat up to 60°C, and apply high-speed stirring at 800 rpm to prepare an emulsion;

[0063] 3.2. Take 10 g of antistatic agent, 45 g of stabilizer, 100 g of wetting agent, and 150 g of bundling agent, mix them with a stirrer, stir the emulsion at 360 rpm, add the mixed solution to the emulsion evenly with constant speed, filter with an 800-mesh filter screen after cooling to room temperature to prepare an environmentally friendly weather-resistant polyester oil agent.

[0064] Comparative Example 1

[0065] This comparative example is a commercially available polyester oil agent, which is composed of TDS-A and TDS-B type polyester oil agents mixed in a volume ratio of 2:3, both produced by Tianjin Gongda Textile Auxiliary Co., Ltd., and diluted into an 18% emulsion according to the use standard.

[0066] Comparative Example 2

[0067] This comparative example is a commercially available polyester oil agent, with the model F-3788, produced by Nippon Takemoto Co., Ltd., and diluted into a 15% emulsion according to the use standard.

[0068] Friction Test: Take the polyester oil agents provided in Examples 1 - 3 and Comparative Examples 1 - 2. Using 132 dtex / 144 f round-hole polyester filaments as test materials, after oiling, conduct friction tests with an HCC μ-Meter precision friction measuring instrument. The test parameters are set as follows: temperature 25°C, humidity 60%, test speed 100 m / min. The specific test data are shown in Table 1:

[0069] Table 1

[0070] <![CDATA[μ dF / C > <![CDATA[μ dF / M > <![CDATA[μ dF / F > Example 1 0.4348 0.5167 0.4392 Example 2 0.4309 0.5029 0.4403 Example 3 0.4294 0.4962 0.4355 Comparative Example 1 0.4865 0.5476 0.4759 Comparative Example 2 0.4328 0.5017 0.4473

[0071] Note: μ dF / C is the dynamic friction coefficient between the fiber and the ceramic, μ dF / M is the dynamic friction coefficient between the fiber and the metal, μ dF / F is the dynamic friction coefficient between the fibers.

[0072] It can be seen from the data in Table 1 that the polyester oil agent prepared by the present invention has a good lubricating effect on polyester fibers, and its performance is significantly better than that of Comparative Example 1 and similar to that of Comparative Example 2. Among them, the friction coefficient between the fibers is slightly lower than that of Comparative Example 2.

[0073] Weather Resistance Test: After oiling as in the above test, take the cake of filaments, place the cake in an oven at 70°C, and bake continuously for 168 h. Referring to the GB / T 6504 - 2017 standard, using ether as the extractant, measure the oil content rate and observe the state of the cake of filaments,

[0074] The oil content rate ρ 前 before baking, the oil content rate ρ 后 after baking, the oil loss rate ΔΡ, and the state of the cake of filaments. The specific test data are shown in Table 2:

[0075] Table 2

[0076] <![CDATA[ρ 前 / %]]> <![CDATA[ρ 后 / %]]> ΔΡ / % Cake state Example 1 0.36 0.34 5.56 No obvious change Example 2 0.37 0.36 2.70 No obvious change Example 3 0.36 0.35 2.78 No obvious change Comparative Example 1 0.34 0.25 26.47 Smelly Comparative Example 2 0.38 0.31 18.42 Slightly smelly

[0077] Note: ρ 前 is the oil content rate before baking, ρ 后 is the oil content rate after baking, and ΔΡ is the oil loss rate.

[0078] It can be seen from the data in Table 2 that the oil loss rate of the polyester oil agent prepared by the present invention after baking is much lower than that of the comparative examples, and there is no obvious problem of stinking and spoilage of the cake of filaments, showing good weather resistance.

[0079] Temperature resistance test: Take the polyester oil agents provided in Examples 1 - 3 and Comparative Examples 1 - 2, place them in an oven preheated to 150 °C, heat up at a rate of 2 °C / min, observe the temperature at which smoking occurs, record it as the smoking temperature T, then perform heat treatment at T + 20 °C for 2 h, use a Y09 - 3016 type laser dust particle counter to detect the particle values within 10 μm in the oven and observe the precipitation of the polyester oil agent. The specific results are shown in Table 3 as follows:

[0080] Table 3

[0081] T / ℃ Number of soot particles / piece State of oil agent after overheating Example 1 198±2 9892 A small amount of dispersed segregation Example 2 206±2 9348 A small amount of dispersed segregation Example 3 202±2 9675 A small amount of dispersed segregation Comparative Example 1 188±2 12850 Flocculent dark segregation Comparative Example 2 196±2 10466 A large amount of dispersed segregation

[0082] As can be seen from the data in Table 3, the polyester oil agent prepared by the present invention has good temperature resistance, with less segregation after heat treatment, showing good temperature stability.

[0083] In the description of the specification, the description referring to terms such as "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in connection with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic expressions of the above terms do not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in a suitable manner in any one or more embodiments or examples.

[0084] The above content is only an example and illustration of the present invention. Those skilled in the art of this technology can make various modifications or supplements to the described specific embodiments or use similar methods for substitution, as long as they do not deviate from the invention or exceed the scope defined by the claims of the present invention, they should fall within the protection scope of the present invention.

Claims

1. An environmentally friendly weather-resistant polyester finishing oil, characterized in that, Comprising by weight parts: 30 - 40 parts of highly adducted polyoxyethylene hydrogenated castor oil, 1 - 2 parts of antistatic agent, 3 - 5 parts of stabilizer, 7 - 10 parts of wetting agent, 12 - 15 parts of bundling agent, and 38 - 45 parts of deionized water; The highly adducted polyoxyethylene hydrogenated castor oil is prepared by the following method: Step A1: Mix hydrogenated castor oil with acetone, keep at a constant temperature of 5 - 8 °C, and slowly add phosphorus oxychloride under high - speed stirring. Control the overall addition reaction time to be 2 - 3 h. After the reaction, add deionized water for washing and perform rotary evaporation under reduced pressure to obtain phosphorus - modified castor oil; Step A2: Mix phosphorus - modified castor oil, metal - based catalyst, and sulfolane, introduce nitrogen for protection, heat up to 160 - 180 °C, introduce ethylene oxide and sodium hydroxide and increase the pressure to 0.7 - 0.9 MPa. React until the system pressure is constant, cool down to 100 °C, release the pressure and add glacial acetic acid dropwise for neutralization. Drain the material into boiling water for washing, cooling and drying, and slicing to obtain highly adducted polyoxyethylene hydrogenated castor oil; Among them, the metal - based catalyst is prepared by the following method: Step B1: Dissolve cerium nitrate and ferric chloride in deionized water, heat up to 60 - 70 °C, introduce hot ammonia for aeration, and at the same time slowly add titanium dioxide. Control the aeration reaction time to be 45 - 50 min. After the reaction, centrifuge to take the bottom precipitate, dry to constant weight, roast at 520 - 550 °C for 4 - 5 h under nitrogen protection, and grind after cooling to obtain a composite matrix; Step B2: Stir - hydrolyze (N,N - dimethyl - 3 - aminopropyl) trimethoxysilane and basic ethanol solution, add the composite matrix and stir at high speed, let stand for 12 h, take the bottom precipitate, wash with deionized water and dry. Then add methyl iodide and tetrahydrofuran, stir and heat up to 70 - 75 °C for reflux reaction for 24 h. After cooling, centrifuge to separate the precipitate, wash with methanol and dry to obtain the metal - based catalyst.

2. The environmentally friendly weather-resistant polyester finishing oil agent according to claim 1, characterized in that, The dosage ratio of hydrogenated castor oil, phosphorus oxychloride and acetone is 100 g: 1.8 - 2.1 mL: 240 - 280 mL.

3. An environmentally friendly weather-resistant polyester finishing oil according to claim 2, characterized in that, The dosage ratio of phosphorus - modified castor oil, metal - based catalyst, sodium hydroxide and sulfolane is 100 g: 0.45 - 0.55 g: 3 - 5 g: 120 - 150 mL.

4. An environmentally friendly weather-resistant polyester finishing oil according to claim 1, characterized in that, The dosage ratio of cerium nitrate, ferric chloride and titanium dioxide is 10 mmol: 20 - 35 mmol: 8 - 12 mg, and the aeration ratio of hot ammonia is 0.12 - 0.15 vvm.

5. An environmentally friendly weather-resistant polyester finishing oil according to claim 4, characterized in that, The dosage ratio of the composite matrix, (N,N - dimethyl - 3 - aminopropyl) trimethoxysilane and methyl iodide is 1 g: 1.5 - 1.8 mL: 20 - 25 mL.

6. The preparation method of an environment-friendly weather-resistant polyester finishing oil agent according to any one of claims 1-5, characterized in that, Including the following steps: Step S1: Mix highly adducted polyoxyethylene hydrogenated castor oil and deionized water, heat up to 60 °C and stir at high speed for emulsification to obtain an emulsion; Step S2: Premix the remaining raw materials, add them to the emulsion under stirring and mix well, cool and filter to obtain an environment - friendly weather - resistant polyester oil agent.