CN113818106B - Environment-friendly degradable polyester FDY (fully drawn yarn) oiling agent and preparation method thereof - Google Patents
Environment-friendly degradable polyester FDY (fully drawn yarn) oiling agent and preparation method thereof Download PDFInfo
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/04—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
- D01F11/08—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The invention relates to the field of spinning auxiliaries, and discloses an environment-friendly degradable polyester FDY oiling agent which comprises the following raw materials in parts by weight: 40-50 parts of high-temperature resistant smoothing agent, 44.5-55 parts of degradable environment-friendly emulsifier, 5-7 parts of degradable antistatic agent and 0.1-0.5 part of oil stabilizer; the high-temperature-resistant smoothing agent comprises the components of polyol ester, fatty acid ester and refined vegetable oil; the degradable environment-friendly emulsifier comprises plant polyene phenol polyoxyethylene ether; the degradable antistatic agent comprises plant polyene phenol polyoxyethylene ether phosphate. The components in the oil agent adopt degradable raw materials, so that the produced oil agent not only meets the requirements of on-machine production, but also can improve the degradation degree of the oil agent, reduce the treatment cost of the oil agent and greatly improve the environmental protection property of the oil agent.
Description
Technical Field
The invention relates to the technical field of spinning auxiliaries, in particular to an environment-friendly degradable polyester FDY oiling agent and a preparation method thereof.
Background
The polyester FDY oiling agent is an indispensable chemical fiber auxiliary agent in the polyester filament yarn production process, and the quality and the use effect of the oiling agent directly influence the quality of the polyester filament yarn and the smooth production, so that the oiling agent must be carefully considered when the oiling agent is selected. At present, most of domestic chemical fiber industries use imported oil agents with the brands of Japanese bamboo book, german Dakoch and the like; the domestic oil agent is developed by scientific research for decades, products with excellent performances can be produced at present, such as Zhejiang chemical, tung Kun and Tiangong large-brand oil agent at present shows good development trend, gradually replaces imported oil agent, and occupies domestic market.
The polyester FDY oiling agent is mainly prepared from mineral oil, an emulsifier, an antistatic agent and other auxiliary agents, for example, the viscose spinning oiling agent and a preparation method thereof disclosed in China patent literature, the publication number CN108755141A of the oiling agent comprises a lubricant, an antistatic agent and an emulsifier, wherein the lubricant is one or more of white oil, liquid paraffin, vaseline, spindle oil, stearate and oleate, the emulsifier is one or more of fatty alcohol polyoxyethylene ether, fatty acid polyoxyethylene ester, polyol fatty acid ester, nonylphenol polyoxyethylene ether and polyethylene glycol, and the antistatic agent is one or more of alkyl phosphate, alkyl sulfate, alkyl phosphate and higher alcohol sulfate.
In the existing spinning oil, all raw materials are generally undegradable or have low degradation degree in a short period, so that the oil is directly high in treatment cost, large in treatment period and high in treatment technical requirement, and the environment-friendly performance of the oil also has a large improvement space.
Disclosure of Invention
The invention aims to solve the problems of high treatment cost, large treatment period and high treatment technical requirements of the oiling agent caused by generally nondegradable raw materials or low degradation degree in a short period in the prior art, and provides the environment-friendly degradable terylene FDY oiling agent and the preparation method thereof, wherein the components in the oiling agent adopt degradable raw materials, so that the produced oiling agent meets the requirements of on-machine production, the degradation degree of the oiling agent can be improved, the treatment cost of the oiling agent is reduced, and the environment-friendly property of the oiling agent is greatly improved.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the environment-friendly degradable polyester FDY oiling agent comprises the following raw materials in parts by weight: 40-50 parts of high-temperature resistant smoothing agent, 44.5-55 parts of degradable environment-friendly emulsifier, 5-7 parts of degradable antistatic agent and 0.1-0.5 part of oil stabilizer;
the high-temperature-resistant smoothing agent comprises the components of polyol ester, fatty acid ester and refined vegetable oil; in the terylene FDY oiling agent, the high temperature resistant smoothing agent mainly has the functions of reducing friction, improving the oil film strength, preventing the problems of broken ends, broken filaments and the like caused by fiber scratch, and reducing the abrasion and corrosion to equipment; the invention selects the polyol ester, the fatty acid ester and the refined vegetable oil as the smoothing agent, does not contain mineral oil which is difficult to degrade, has no toxicity, low smell and strong biodegradability, and simultaneously has excellent lubricity and stability, high flash point, high temperature resistance, low volatility and good abrasion resistance;
the degradable environment-friendly emulsifier comprises plant polyene phenol polyoxyethylene ether; the invention selects the plant polyene phenol polyoxyethylene ether as the degradable environment-friendly emulsifier, and compared with the traditional fatty alcohol polyoxyethylene ether emulsifier, the plant polyene phenol polyoxyethylene ether has the advantages of equivalent emulsifying power and hard water resistance, higher cloud point, lower foam performance, better detergency, lower toxicity and easier biodegradation;
the degradable antistatic agent comprises plant polyene phenol polyoxyethylene ether phosphate. The invention selects the plant polyene phenol polyoxyethylene ether phosphate as the degradable antistatic agent, compared with the traditional alkyl phosphate and fatty alcohol polyoxyethylene ether phosphate antistatic agent, the biodegradability of the antistatic agent is improved, so that the oiling agent is more environment-friendly, and meanwhile, the antistatic agent in the invention can increase the hygroscopicity of fibers, can better adjust the dynamic friction coefficient between the fibers, can be adsorbed on the surfaces of the fibers in the high-speed spinning process, improves the conductivity and reduces the accumulation of static electricity.
Therefore, most of the components in the polyester FDY oiling agent have the characteristic of easy biodegradation, so that the produced oiling agent not only meets the requirement of on-machine production, but also can improve the degradation degree of the oiling agent, has high degradation rate and short degradation period, reduces the treatment cost of the oiling agent, and greatly improves the environmental protection property of the oiling agent.
Preferably, the mass ratio of the polyol ester to the fatty acid ester to the refined vegetable oil in the high-temperature resistant smoothing agent is 17-20:15-20:5-10; the polyol ester is selected from one or two of neopentyl glycol dioleate and pentaerythritol; the fatty acid ester is one or more selected from isooctyl stearate, trimethylolpropane oleate and fatty acid isopropyl ester.
Preferably, the degradable environment-friendly emulsifier comprises cardanol polyoxyethylene ether, and the degradable antistatic agent comprises cardanol polyoxyethylene ether phosphate. The cardanol polyoxyethylene ether has the advantages of cheap and easily available raw materials and easily regulated HLB value, and can be used as the components in the emulsifier and the antistatic agent to improve the degradability of the oil agent and the usability of the oil agent.
Preferably, the components of the degradable environment-friendly emulsifier comprise cardanol polyoxyethylene ether with HLB values of 4.5, 7, 7.5, 9, 9.5 and 13 respectively.
Preferably, the mass ratio of cardanol polyoxyethylene ether with HLB value of 4.5, 7, 7.5, 9, 9.5 and 13 is 7-9:14-17:4.5-5:4-5:7-9:8-11.
According to the invention, the research shows that the HLB value of the cardanol polyoxyethylene ether has a great influence on the stability of the oiling agent, when the cardanol polyoxyethylene ether with a single HLB value is adopted as an emulsifier, the oiling agent cannot have good stability, and the oiling agent with good stability can be obtained only by proportioning the cardanol polyoxyethylene ethers with different HLB values according to a specific proportion, so that the oiling agent meets the spinning requirement.
Preferably, the preparation method of the cardanol polyoxyethylene ether comprises the following steps: pressing cashew nut shells to obtain cashew nut shell oil; refining the cashew nut shell oil to obtain cardanol; mixing cardanol with sodium hydroxide solution, decompressing, pumping out water vapor and air, and then introducing nitrogen to replace air; then adding ethylene oxide, heating to 130-140 ℃ for reaction for 4-6 hours, cooling to 75-85 ℃ after the reaction is completed, and neutralizing the product with acetic acid to obtain the cardanol polyoxyethylene ether. The cardanol polyoxyethylene ethers with different HLB values can be obtained by adjusting the adding proportion of the ethylene oxide and the cardanol.
Preferably, the preparation method of the cardanol polyoxyethylene ether phosphate comprises the following steps: (1) Heating cardanol polyoxyethylene ether to 40-50 ℃, then adding phosphorus pentoxide under stirring, and reacting for 2-4 h at 60-70 ℃; adding water and hydrogen peroxide, reacting for 1-3 h at 70-80 ℃, and cooling to room temperature to obtain an intermediate; (2) Heating the intermediate to 40-50 ℃, then dropwise adding phosphorus pentoxide and cardanol polyoxyethylene ether in a stirring state, and reacting for 2-4 h at 60-70 ℃; and then adding water and hydrogen peroxide, reacting for 1-3 hours at 70-80 ℃, and cooling to room temperature to obtain the cardanol polyoxyethylene ether phosphate.
The conventional polyoxyethylene ether phosphate is generally prepared by directly carrying out phosphorylation reaction on polyoxyethylene ether and phosphorus pentoxide, but the reaction releases a large amount of heat, so that the product is easy to coke and has a deep color, and the color of the prepared polyester FDY can be influenced when the polyoxyethylene ether phosphate is used in a spinning oil, so that the polyester FDY is unfavorable for the subsequent use of polyester. The preparation method comprises the steps of carrying out two-step reaction in the preparation of the cardanol polyoxyethylene ether phosphate, firstly reacting a part of cardanol polyoxyethylene ether with phosphorus pentoxide to obtain an intermediate, and then reacting the intermediate with cardanol polyoxyethylene ether and phosphorus pentoxide to finally obtain the cardanol polyoxyethylene ether phosphate. The cardanol polyoxyethylene ether phosphate monoester prepared by the method has the content of 77%, the conversion rate of 97%, and can effectively avoid coking of products and control the color of the products, thereby avoiding the influence of the color of the oiling agent on the color of polyester FDY.
Preferably, the mass ratio of the cardanol polyoxyethylene ether to the phosphorus pentoxide added in the step (1) is 58-62:11-12; the mass volume ratio of the cardanol polyoxyethylene ether to the added water is 58-62 kg:4L; the mass fraction of the hydrogen peroxide is 20-30%, and the volume ratio of the added water to the hydrogen peroxide is 4:2.5-3.8.
Preferably, the mass ratio of the intermediate, phosphorus pentoxide and cardanol polyoxyethylene ether added in the step (2) is 34-36:21-22:97-98; the mass volume ratio of the intermediate to the added water is 34-36 kg:3L; the mass fraction of the hydrogen peroxide is 20-30%, and the volume ratio of the added water to the hydrogen peroxide is 3:2-3.
Preferably, the oil stabilizer is one or two selected from triethanolamine and long-chain fatty alcohol.
The invention also provides a preparation method of the polyester FDY oiling agent, which comprises the following steps: uniformly stirring the degradable environment-friendly emulsifier at 35-40 ℃; then adding a degradable antistatic agent and uniformly stirring; adding a high-temperature resistant smoothing agent, and uniformly stirring; and finally adding an oil stabilizer, uniformly stirring, and filtering to obtain the oil stabilizer.
Therefore, the invention has the following beneficial effects:
(1) The raw materials used in the invention do not contain substances such as APEO and the like, most of the raw materials have the characteristic of easy biodegradation, and the raw materials are mainly characterized by high degradation rate and short degradation period.
(2) The raw materials of the cardanol polyoxyethylene ether are extracted from plants, so that waste resources can be fully utilized, market application is developed, and the development of the environment-friendly industry is promoted.
(3) Compared with the existing oil, the oil produced by the invention has the advantages of excellent performances, strong detergency, low foam, excellent emulsifying power, extremely low toxicity and easy degradation, and reduces the treatment cost of the waste oil.
(4) The invention has low cost of raw materials and simple preparation method, and is suitable for mass production.
Detailed Description
The invention is further described below in connection with the following detailed description.
In the present invention, all the equipment and raw materials are commercially available or commonly used in the industry, and the methods in the following examples are conventional in the art unless otherwise specified.
Example 1:
the environment-friendly degradable polyester FDY oiling agent comprises the following raw materials in parts by weight:
40 parts of high-temperature resistant smoothing agent, wherein 20 parts of environment-friendly polyol ester (Shandong Rui, neopentyl glycol dioleate), 15 parts of fatty acid ester (sea-safe petrochemical, isooctyl stearate) and 5 parts of refined vegetable oil (Shanghai Chen-expensive canola oil);
54.9 parts of degradable environment-friendly emulsifier, 8.6 parts of cardanol polyoxyethylene ether with an HLB value of 4.5 and 17 parts of cardanol polyoxyethylene ether with an HLB value of 7; 5 parts of cardanol polyoxyethylene ether with an HLB value of 7.5; 5 parts of cardanol polyoxyethylene ether with an HLB value of 9, 8.6 parts of cardanol polyoxyethylene ether with an HLB value of 9.5 and 10.7 parts of cardanol polyoxyethylene ether with an HLB value of 13;
the preparation method of the cardanol polyoxyethylene ether comprises the following steps: pressing cashew nut shells to obtain cashew nut shell oil; refining the cashew nut shell oil to obtain cardanol; 157kg of cardanol is put into a stainless steel reaction kettle, and 2.5kg of sodium hydroxide solution prepared by dissolving sodium hydroxide in 30kg of water is added; after the materials are added, electric induction heating is used, and after water vapor and air are pumped out under reduced pressure, nitrogen is introduced to replace the air in the kettle; and (3) filling nitrogen into the kettle, pressing ethylene oxide into the kettle, uniformly heating the kettle to 135 ℃, reacting the kettle at 135 ℃ for 5 hours, cooling the kettle to 80 ℃ after the reaction is finished, and neutralizing the product with acetic acid to obtain the cardanol polyoxyethylene ether. The cardanol polyoxyethylene ether with different HLB values is obtained by adjusting the adding proportion of the ethylene oxide and the cardanol;
7 parts of degradable antistatic agent, namely cardanol polyoxyethylene ether phosphate is adopted as the degradable antistatic agent, and the preparation method comprises the following steps: (1) Heating 60kg of cardanol polyoxyethylene ether to 45 ℃, then adding 11.7kg of phosphorus pentoxide under stirring, and reacting for 3 hours at 65 ℃; then adding 4L of water and 30wt% of hydrogen peroxide solution 2.5L, carrying out hydrolysis reaction for 2 hours at 75 ℃, and cooling to room temperature to obtain an intermediate; (2) Heating 35kg of intermediate to 45 ℃, then dropwise adding 21.3kg of phosphorus pentoxide and 97.8kg of cardanol polyoxyethylene ether under stirring, and reacting for 3h at 65 ℃; adding 3L of water and 30wt% of hydrogen peroxide 2L, reacting for 2 hours at 75 ℃, and cooling to room temperature to obtain the cardanol polyoxyethylene ether phosphate;
0.1 part of oil stabilizer (Dow chemical, triethanolamine).
The preparation method of the environment-friendly degradable polyester FDY oiling agent comprises the following steps: setting the water bath temperature of the stirring kettle, and ensuring the temperature in the stirring kettle to be 37 ℃; the components of the degradable environment-friendly emulsifier are added into a stirring kettle according to the proportion and stirred uniformly; adding the degradable antistatic agent into the kettle, and uniformly stirring; sequentially adding the components of the high-temperature-resistant smoothing agent, and uniformly stirring; and finally adding an oil stabilizer, uniformly stirring, and filtering to obtain the oil stabilizer.
Example 2:
the environment-friendly degradable polyester FDY oiling agent comprises the following raw materials in parts by weight:
44 parts of high-temperature resistant smoothing agent, wherein 17 parts of environment-friendly polyol ester (Shandong Rui Jie, pentaerythritol), 20 parts of fatty acid ester (sea-Anpetrifaction, trimethylolpropane oleate) and 7 parts of refined vegetable oil (Shanghai Chen-expensive canola oil);
49.9 parts of degradable environment-friendly emulsifier, wherein 7.8 parts of cardanol polyoxyethylene ether with an HLB value of 4.5 and 15.5 parts of cardanol polyoxyethylene ether with an HLB value of 7; 4.7 parts of cardanol polyoxyethylene ether with an HLB value of 7.5; 4.7 parts of cardanol polyoxyethylene ether with an HLB value of 9, 7.7 parts of cardanol polyoxyethylene ether with an HLB value of 9.5 and 9.5 parts of cardanol polyoxyethylene ether with an HLB value of 13; the preparation method of cardanol polyoxyethylene ether was the same as in example 1;
7 parts of degradable antistatic agent, namely cardanol polyoxyethylene ether phosphate is adopted as the degradable antistatic agent, and the preparation method comprises the following steps: (1) 58kg of cardanol polyoxyethylene ether is heated to 40 ℃, then 11kg of phosphorus pentoxide is added under stirring, and the mixture reacts for 4 hours at 60 ℃; then adding 4L of water and 25wt% of hydrogen peroxide solution 3L, carrying out hydrolysis reaction for 3 hours at 70 ℃, and cooling to room temperature to obtain an intermediate; (2) 34kg of intermediate is heated to 40 ℃, 21kg of phosphorus pentoxide and 97kg of cardanol polyoxyethylene ether are then added dropwise under stirring, and the mixture is reacted for 4 hours at 60 ℃; adding 3L of water and 25wt% of hydrogen peroxide solution 2.4L, reacting for 3 hours at 70 ℃, and cooling to room temperature to obtain the cardanol polyoxyethylene ether phosphate;
0.3 part of oil stabilizer (Dow chemical, triethanolamine).
The preparation method of the environment-friendly degradable polyester FDY oiling agent comprises the following steps: setting the water bath temperature of the stirring kettle, and ensuring the temperature in the stirring kettle to be 35 ℃; the components of the degradable environment-friendly emulsifier are added into a stirring kettle according to the proportion and stirred uniformly; adding the degradable antistatic agent into the kettle, and uniformly stirring; sequentially adding the components of the high-temperature-resistant smoothing agent, and uniformly stirring; and finally adding an oil stabilizer, uniformly stirring, and filtering to obtain the oil stabilizer.
Example 3:
the environment-friendly degradable polyester FDY oiling agent comprises the following raw materials in parts by weight:
47 parts of high-temperature resistant smoothing agent, wherein 20 parts of environment-friendly polyol ester (Shandong Rui, neopentyl glycol dioleate), 20 parts of fatty acid ester (sea-safe petrochemical, isooctyl stearate) and 7 parts of refined vegetable oil (Shanghai Chen-expensive canola oil);
47.9 parts of degradable environment-friendly emulsifier, wherein 7.5 parts of cardanol polyoxyethylene ether with an HLB value of 4.5 and 15 parts of cardanol polyoxyethylene ether with an HLB value of 7; 4.5 parts of cardanol polyoxyethylene ether with an HLB value of 7.5; 5 parts of cardanol polyoxyethylene ether with an HLB value of 9, 7.5 parts of cardanol polyoxyethylene ether with an HLB value of 9.5 and 8.4 parts of cardanol polyoxyethylene ether with an HLB value of 13; the preparation method of cardanol polyoxyethylene ether was the same as in example 1;
5 parts of degradable antistatic agent, wherein the degradable antistatic agent adopts cardanol polyoxyethylene ether phosphate, and the preparation method comprises the following steps: (1) 62kg of cardanol polyoxyethylene ether is heated to 50 ℃, then 12kg of phosphorus pentoxide is added under stirring, and the mixture reacts for 2 hours at 70 ℃; then adding 4L of water and 3.8L of 20wt% hydrogen peroxide, carrying out hydrolysis reaction for 1h at 80 ℃, and cooling to room temperature to obtain an intermediate; (2) 36kg of intermediate is heated to 50 ℃, 22kg of phosphorus pentoxide and 98kg of cardanol polyoxyethylene ether are then added dropwise under stirring, and the mixture is reacted for 2 hours at 70 ℃; adding 3L of water and 20wt% of hydrogen peroxide solution 3L, reacting for 1h at 80 ℃, and cooling to room temperature to obtain the cardanol polyoxyethylene ether phosphate;
0.5 part of oil stabilizer (Dow chemical, triethanolamine).
The preparation method of the environment-friendly degradable polyester FDY oiling agent comprises the following steps: setting the water bath temperature of the stirring kettle, and ensuring the temperature in the stirring kettle to be 40 ℃; the components of the degradable environment-friendly emulsifier are added into a stirring kettle according to the proportion and stirred uniformly; adding the degradable antistatic agent into the kettle, and uniformly stirring; sequentially adding the components of the high-temperature-resistant smoothing agent, and uniformly stirring; and finally adding an oil stabilizer, uniformly stirring, and filtering to obtain the oil stabilizer.
Example 4:
the environment-friendly degradable polyester FDY oiling agent comprises the following raw materials in parts by weight:
50 parts of high-temperature resistant smoothing agent, wherein 20 parts of environment-friendly polyol ester (Shandong Rui, neopentyl glycol dioleate), 20 parts of fatty acid ester (sea-safe petrochemical, isooctyl stearate) and 10 parts of refined vegetable oil (Shanghai Chen-expensive canola oil);
44.9 parts of degradable environment-friendly emulsifier, wherein 7 parts of cardanol polyoxyethylene ether with an HLB value of 4.5 and 14 parts of cardanol polyoxyethylene ether with an HLB value of 7; 4.5 parts of cardanol polyoxyethylene ether with an HLB value of 7.5; 4 parts of cardanol polyoxyethylene ether with an HLB value of 9, 7 parts of cardanol polyoxyethylene ether with an HLB value of 9.5 and 8.4 parts of cardanol polyoxyethylene ether with an HLB value of 13; the preparation method of cardanol polyoxyethylene ether was the same as in example 1;
5 parts of degradable antistatic agent, namely cardanol polyoxyethylene ether phosphate is adopted as the degradable antistatic agent, and the preparation method is the same as that in the example 1;
0.1 part of oil stabilizer (Dow chemical, triethanolamine).
The preparation method of the environment-friendly degradable polyester FDY oiling agent comprises the following steps: setting the water bath temperature of the stirring kettle, and ensuring the temperature in the stirring kettle to be 40 ℃; the components of the degradable environment-friendly emulsifier are added into a stirring kettle according to the proportion and stirred uniformly; adding the degradable antistatic agent into the kettle, and uniformly stirring; sequentially adding the components of the high-temperature-resistant smoothing agent, and uniformly stirring; and finally adding an oil stabilizer, uniformly stirring, and filtering to obtain the oil stabilizer.
Comparative example 1:
in the oiling agent of comparative example 1, the degradable environment-friendly emulsifier was cardanol polyoxyethylene ether with HLB value of 4.5, and the rest was the same as in example 1.
Comparative example 2:
in the oiling agent of comparative example 1, the degradable environment-friendly emulsifier was cardanol polyoxyethylene ether with HLB value of 7.5, and the rest was the same as in example 1.
Comparative example 3 (change of HLB value match of cardanol polyoxyethylene ether in emulsifier):
in the oiling agent of the comparative example 3, the components of the degradable environment-friendly emulsifier are as follows: 8.6 parts of cardanol polyoxyethylene ether with an HLB value of 9; 17 parts of cardanol polyoxyethylene ether with an HLB value of 13; 5 parts of cardanol polyoxyethylene ether with an HLB value of 4.5; 5 parts of cardanol polyoxyethylene ether with an HLB value of 7, 8.6 parts of cardanol polyoxyethylene ether with an HLB value of 7.5 and 10.7 parts of cardanol polyoxyethylene ether with an HLB value of 9.5; the remainder was the same as in example 1.
Comparative example 4 (one-step preparation of cardanol polyoxyethylene ether phosphate):
the preparation method of cardanol polyoxyethylene ether phosphate as a degradable antistatic agent in comparative example 4 comprises the following steps: 97.8kg of cardanol polyoxyethylene ether is heated to 45 ℃, then 21.3kg of phosphorus pentoxide is added under stirring, and the mixture reacts for 3 hours at 65 ℃; then adding 3L of water and 30wt% of hydrogen peroxide solution to perform hydrolysis reaction for 2 hours at 75 ℃, and cooling to room temperature to obtain the cardanol polyoxyethylene ether phosphate; the remainder was the same as in example 1.
Comparative example 5:
commercial polyester spinning oil agent: bamboo book 1946.
The performance indexes of the oils prepared in the above examples and comparative examples were tested and the results are shown in table 1.
Table 1: and (5) testing the performance index of the oiling agent.
As can be seen from Table 1, the polyester FDY oiling agent prepared by the formulation in examples 1 to 4 has good performance indexes and meets the condition of spinning test. In contrast, in comparative examples 1 and 2, cardanol polyoxyethylene ether with a single HLB value is used as an emulsifier, and in comparative example 3, the HLB value of cardanol polyoxyethylene ether in the emulsifier is changed to match, so that the stability of the oil agent is reduced and the oil agent cannot be stably stored; in comparative example 4, cardanol polyoxyethylene ether phosphate is prepared by a one-step method as an antistatic agent, and the prepared oiling agent has darker color and can influence the spinning color.
The performance index of the obtained polyester FDY was tested by on-machine test spinning using the oiling agents in the above examples and comparative examples, and the results are shown in table 2.
Table 2: and (5) testing the performance of the polyester FDY.
| Performance index | Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 5 |
| Spinning specification | 83dtex/48f | 83dtex/48f | 83dtex/48f | 83dtex/48f | 83dtex/48f |
| Fiber oil content% | 0.983 | 0.990 | 0.995 | 0.981 | 1.000 |
| Breaking strength cN/dtex | 4.58 | 4.62 | 4.69 | 4.65 | 4.60 |
| Elongation at break% | 25.79 | 25.49 | 27.67 | 27.20 | 26.23 |
| Uniformity of dyeing | Uniformity of | Uniformity of | Uniformity of | Uniformity of | Uniformity of |
| Specific resistance of fiber omega cm | 26.7×10 8 | 28.3×10 8 | 27.6×10 8 | 26.5×10 8 | 31.5×10 8 |
| Coefficient of friction mu d | 0.437 | 0.427 | 0.435 | 0.437 | 0.427 |
| Winding tension cN | 18 | 18 | 17 | 18 | 18 |
| Static voltage V | 160 | 170 | 170 | 160 | 160 |
| Shrinkage in boiling water% | 7.28 | 7.28 | 7.65 | 7.56 | 7.56 |
As can be seen from table 2, the oil in the present invention has good spinnability.
The oil solutions in the above examples and comparative example 5 were tested for biodegradability, and the results were as followsTable 3 shows (BOD was measured using working fluid concentration of 15% of the effective oil content 5 Value method).
Table 3: results of biodegradability test.
| Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 5 | |
| O 2 ，mg/L | 61.6 | 60.5 | 59.6 | 57.9 | 42.8 |
As can be seen from Table 3, examples 1 to 4 show BOD of the polyester FDY oil prepared by the formulation and method of the present invention 5 The value is almost 1.5 times that of the commercial oil in comparative example 5, which shows that the oil in the present invention is more suitable for microbial growth, i.e., the biodegradability of the oil in the present invention is significantly better than that of the commercial oil in comparative example.
Claims (6)
1. The environment-friendly degradable polyester FDY oiling agent is characterized by comprising the following raw materials in parts by weight: 40-50 parts of high-temperature resistant smoothing agent, 44.5-55 parts of degradable environment-friendly emulsifier, 5-7 parts of degradable antistatic agent and 0.1-0.5 part of oil stabilizer;
the high-temperature-resistant smoothing agent comprises the components of polyol ester, fatty acid ester and refined vegetable oil;
the components of the degradable environment-friendly emulsifier comprise cardanol polyoxyethylene ether with HLB values of 4.5, 7, 7.5, 9, 9.5 and 13 respectively; the mass ratio of cardanol polyoxyethylene ether with the HLB value of 4.5, 7, 7.5, 9, 9.5 and 13 is 7-9:14-17:4.5-5:4-5:7-9:8-11;
the components of the degradable antistatic agent are cardanol polyoxyethylene ether phosphate, and the preparation method of the cardanol polyoxyethylene ether phosphate comprises the following steps:
(1) Heating cardanol polyoxyethylene ether to 40-50 ℃, adding phosphorus pentoxide in a stirring state, and reacting for 2-4 hours at 60-70 ℃; adding water and hydrogen peroxide, reacting for 1-3 hours at 70-80 ℃, and cooling to room temperature to obtain an intermediate; the mass ratio of the added cardanol polyoxyethylene ether to the phosphorus pentoxide is 58-62:11-12;
(2) Heating the intermediate to 40-50 ℃, and then dropwise adding phosphorus pentoxide and cardanol polyoxyethylene ether in a stirring state, wherein the mass ratio of the added intermediate to the phosphorus pentoxide to the cardanol polyoxyethylene ether is 34-36:21-22:97-98; reacting for 2-4 hours at 60-70 ℃; and adding water and hydrogen peroxide, reacting for 1-3 hours at 70-80 ℃, and cooling to room temperature to obtain the cardanol polyoxyethylene ether phosphate.
2. The environment-friendly degradable polyester FDY oiling agent according to claim 1, wherein the mass ratio of polyol ester, fatty acid ester and refined vegetable oil in the high-temperature resistant smoothing agent is 17-20:15-20:5-10; the polyol ester is selected from one or two of neopentyl glycol dioleate and pentaerythritol; the fatty acid ester is one or more selected from isooctyl stearate, trimethylolpropane oleate and fatty acid isopropyl ester.
3. The environment-friendly degradable polyester FDY oiling agent disclosed by claim 1 is characterized in that the mass volume ratio of the added cardanol polyoxyethylene ether to the added water in the step (1) is 58-62 kg:4L; the mass fraction of the hydrogen peroxide is 20-30%, and the volume ratio of the added water to the hydrogen peroxide is 4:2.5-3.8.
4. The environment-friendly degradable polyester FDY oiling agent according to claim 1, wherein the mass-volume ratio of the intermediate added in the step (2) to the water added is 34-36 kg/3L; the mass fraction of the hydrogen peroxide is 20-30%, and the volume ratio of the added water to the hydrogen peroxide is 3:2-3.
5. The environmentally-friendly degradable polyester FDY oiling agent according to claim 1, wherein the oiling agent is one or two selected from triethanolamine and long-chain fatty alcohol.
6. A method for preparing the polyester FDY oiling agent according to any one of claims 1 to 5, characterized by comprising the steps of: uniformly stirring the degradable environment-friendly emulsifier at 35-40 ℃; then adding a degradable antistatic agent and uniformly stirring; adding a high-temperature resistant smoothing agent, and uniformly stirring; and finally adding an oil stabilizer, uniformly stirring, and filtering to obtain the oil stabilizer.
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| CN101629383A (en) * | 2009-08-27 | 2010-01-20 | 上虞市皇马化学有限公司 | Terylene FDY spinning oil and preparation process thereof |
| JP2011196000A (en) * | 2010-03-23 | 2011-10-06 | Sanyo Chem Ind Ltd | Treating agent for synthetic fiber |
| CN102978934B (en) * | 2012-11-28 | 2014-12-31 | 浙江天圣控股集团有限公司 | Low-smoke FDY (Fully Drawn Yarn) oiling agent and preparation method thereof |
| CN103147168B (en) * | 2013-03-06 | 2017-06-16 | 常州市灵达化学品有限公司 | A kind of spinning oil and preparation method |
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| CN107955152A (en) * | 2017-11-27 | 2018-04-24 | 山东诺威新材料有限公司 | Cardanol polyoxyethylene ether, its preparation method and its preparation method of the without phosphorus laundry sheet of preparation and without phosphorus laundry sheet |
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| CN108642880A (en) * | 2018-05-18 | 2018-10-12 | 杭州华春化纤染织有限公司 | A kind of high-strength polyester POY finishes and preparation method thereof |
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