阅读说明：本技术 一种涤纶全拉伸丝油剂 (Polyester fully drawn yarn oiling agent ) 是由 杨海涛 李成达 于 2021-08-06 设计创作，主要内容包括：本发明公开了一种涤纶全拉伸丝油剂,按质量份数计,包括5～10份有机硅磷酸酯盐高分子聚合物,20～30份聚乙二醇脂肪酸酯,15～20份脂肪醇无规聚醚,3～8份磺酸盐,10～20份精制矿物油,10～15份油酸酯和10份去离子水。本发明采用的有机硅磷酸酯盐高分子聚合物具有良好的抗静电性以及耐热性,能有效降低油剂发烟量、结焦性,并与精制矿物油、多元醇脂肪酸酯、聚醚、烷基磺酸钠等原料复配,还具有油膜强度高、附着性好、上油均匀稳定的特点,能保证纤维具有较好的抗静电性、平滑性、耐热性和柔软性,能适应涤纶FDY纺丝工艺的加工要求,保证纤维生产的顺利进行。(The invention discloses a polyester fully drawn yarn oiling agent which comprises, by mass, 5-10 parts of organic silicon phosphate salt high-molecular polymer, 20-30 parts of polyethylene glycol fatty acid ester, 15-20 parts of fatty alcohol random polyether, 3-8 parts of sulfonate, 10-20 parts of refined mineral oil, 10-15 parts of oleate and 10 parts of deionized water. The organic silicon phosphate salt high molecular polymer adopted by the invention has good antistatic property and heat resistance, can effectively reduce the smoke generation amount and coking property of an oil agent, is compounded with raw materials such as refined mineral oil, polyol fatty acid ester, polyether, alkyl sodium sulfonate and the like, has the characteristics of high oil film strength, good adhesiveness and uniform and stable oiling, can ensure that the fiber has better antistatic property, smoothness, heat resistance and softness, can meet the processing requirements of a polyester FDY spinning process, and ensures the smooth production of the fiber.)

1. The polyester fully drawn yarn oiling agent is characterized in that: the components comprise, by mass, 5-10 parts of organic silicon phosphate salt high-molecular polymer, 20-30 parts of polyethylene glycol fatty acid ester, 15-20 parts of fatty alcohol random polyether, 3-8 parts of sulfonate, 10-20 parts of refined mineral oil, 10-15 parts of oleate and 10 parts of deionized water;

the structural formula of the organic silicon phosphate salt high molecular polymer is one of a formula (I) or a formula (II),

（Ⅰ），

（Ⅱ）；

wherein n is an integer of 20 to 80, a is an integer of 10 to 20, b is an integer of 5 to 20, and M is a potassium ion K⁺Or sodium ion Na⁺；

The structural formula of the polyethylene glycol fatty acid ester is R₁COO(C₂H₄O)_pH, wherein R₁Is C₁₁～C₁₇P is an integer of 6-20;

the fatty alcohol random polyether has a structural formula of R₂O(C₂H₄O)_x(C₃H₆O)_yR_3；Wherein R is₂Is C₄～C₁₂Alkyl of R₃Is C₁～C₄X, y are integers of 1 to 50, and x: y =3: 2;

the above-mentionedOf formula R₄CH₂SO₃Na; wherein R is₄Is C₁₁～C₁₇Linear or branched alkyl groups.

2. The finish for polyester fully drawn yarn according to claim 1, wherein: the kinematic viscosity of the refined mineral oil at the temperature of 40 ℃ is 5-100 mm²/s。

3. The finish for polyester fully drawn yarn according to claim 1, wherein: the oleic acid ester is one of trimethylolpropane oleate, pentaerythritol oleate and sorbitan oleate.

Technical Field

The invention relates to a polyester fiber Fully Drawn Yarn (FDY) oiling agent, belonging to the technical field of chemical fiber spinning oil.

Background

The spinning process of the polyester Fully Drawn Yarn (FDY) greatly improves the spinning production efficiency due to the high spinning speed (4200 m-5500 m/min), and occupies an increasingly large proportion in the existing polyester spinning process. However, since the polyester fiber is a hydrophobic polymer compound, in the full-drawn polyester spinning process, friction between fiber tows and between the fiber and metal equipment can generate a large amount of static electricity, which causes problems of fiber breakage, loosening and the like, and in severe cases, fiber production cannot be performed at all, thereby bringing serious economic loss to chemical fiber manufacturers. In order to ensure the smooth production of the polyester fiber, the oiling of the fiber tows becomes the necessary condition for ensuring the normal production. The spinning oil agent has the function of enabling the performances of the friction property, the antistatic property, the cohesion property and the like of the polyester fiber to be in a proper range in the spinning process so as to ensure the normal production of the fiber.

Because the hydrophilicity of the polyester fiber is poor, the critical surface tension of the polyester is 43dyn/cm, and the spinning speed of the polyester FDY is generally 4200 m/min-5500 m/min, the high spinning speed, the poor hydrophilicity and the low surface tension of the polyester fiber are added, and the oiling process is finished instantly, so that the uniform oiling of the fiber is difficult to achieve. In addition, in the high-speed spinning process, the setting temperature of the second hot roller is as high as 130-150 ℃, so that the oiling agent is required to have good thermal decomposition resistance in addition to excellent performances such as smoothness, antistatic property and the like, and if the heat resistance of the oiling agent is poor, the oiling agent on the fiber is contacted with high temperature during stretching and setting, and is decomposed into precipitates such as oil stains, oil residues and the like, and the precipitates are attached to the setting hot roller, so that the friction force is increased, and the production problems such as broken ends of fiber filaments and the like are caused. In addition, the smoke generated by the pyrolysis of the oil agent greatly deteriorates the working environment of a production workshop and seriously damages the health of production personnel, so that the terylene FDY oil agent has excellent thermal decomposition resistance. In the prior art, mineral oil, fatty acid ester, polyether, fatty alcohol-polyoxyethylene ether phosphate and other monomers are mostly adopted to compound an oil agent, and the monomer is used for compounding the oil agent, so that the performances of smoothness, cohesion, antistatic property and the like of the oil agent can meet the requirements, but the fatty alcohol-polyoxyethylene ether phosphate is not high-temperature resistant and is easy to decompose and coke on a shaping hot roller due to heating, so that the friction force is increased, and the fiber breakage and other problems are caused. The invention discloses a terylene high-speed spinning oil agent and a manufacturing method thereof in China patent CN99124724, a terylene FDY spinning oil agent and a manufacturing method thereof in CN101629383, an FDY oiling agent and a manufacturing method thereof in CN101392458, and an FDY oiling agent and a manufacturing method thereof in CN 101392458B.

The existing literature reports that silicon element has better heat resistance, and is nontoxic, cheap and easily available. However, reports and products for improving the heat resistance of the oil by adding organic silicon phosphate serving as an antistatic agent into a polyester spinning oil are not found at present.

Disclosure of Invention

The invention aims to overcome the defects in the prior art, provides a terylene FDY oil agent with strong antistatic property and stable performance, and can better solve the problem of smoke and coking of the oil agent caused by the fact that fatty alcohol polyoxyethylene ether phosphate cannot resist high temperature.

The technical scheme for achieving the purpose of the invention is to provide a polyester fully drawn yarn oiling agent which comprises, by mass, 5-10 parts of organic silicon phosphate salt high-molecular polymer, 20-30 parts of polyethylene glycol fatty acid ester, 15-20 parts of fatty alcohol random polyether, 3-8 parts of sulfonate, 10-20 parts of refined mineral oil, 10-15 parts of oleate and 10 parts of deionized water;

the structural formula of the organic silicon phosphate salt high molecular polymer is one of a formula (I) or a formula (II),

（Ⅰ） ，

（Ⅱ）；

wherein n is an integer of 20 to 80, a is an integer of 10 to 20, b is an integer of 5 to 20, and M is a potassium ion K⁺Or sodium ion Na⁺；

The structural formula of the polyethylene glycol fatty acid ester is R₁COO(C₂H₄O)_pH, wherein R₁Is C₁₁～C₁₇P is an integer of 6-20;

the fatty alcohol random polyether has a structural formula of R₂O(C₂H₄O)_x(C₃H₆O)_yR_3；Wherein R is₂Is C₄～C₁₂Alkyl of R₃Is C₁～C₄X, y are integers of 1 to 50, and x: y =3: 2;

the structural formula of the sulfonate is R₄CH₂SO₃Na; wherein R is₄Is C₁₁～C₁₇Linear or branched alkyl of (a);

the kinematic viscosity of the refined mineral oil at the temperature of 40 ℃ is 5-100 mm²/s；

The oleic acid ester is one of trimethylolpropane oleate, pentaerythritol oleate and sorbitan oleate.

The terylene FDY oil agent provided by the invention is prepared by compounding raw materials of each component with water, wherein the component organic silicon phosphate salt high molecular polymer has good antistatic property and heat resistance, and can effectively reduce the smoke volume and coking property of the oil agent; the polyethylene glycol fatty acid ester has the functions of good emulsibility and proper smoothness; the fatty alcohol random polyether can effectively improve the heat resistance and proper smoothness of the oil agent, has low foam and also has the function of reducing the foam of oil agent emulsion; the component sulfonate has good permeability, can obviously improve the wettability of the oil agent, and ensures that the oil agent is quickly spread on the fiber when the fiber is spun at high speed, thereby reducing the friction force between the fiber and metal and between the fiber and the fiber; the refined mineral oil has the advantages that the refined mineral oil has good smoothness, the fiber has good intermiscibility with slurry in the subsequent sizing procedure, the sizing is facilitated, and in addition, the mineral oil is low in price; the component oleate has good smoothness and can obviously improve the heat resistance of the oil agent.

According to the invention, hydroxyl silicone oil, hydroxyl polyether silicone oil and phosphorus pentoxide are selected to carry out a phosphorylation reaction to synthesize the silicon-containing phosphate ester antistatic agent and carry out a heat resistance experiment, and the result shows that the organic silicon phosphate ester can not be decomposed and coked at a high temperature of 150 ℃ and has good antistatic property. Therefore, the invention selects the organic silicon phosphate as the antistatic agent, and compounds the organic silicon phosphate with the raw materials of refined mineral oil, polyol fatty acid ester, polyether, alkyl sodium sulfonate and the like and deionized water to prepare the terylene FDY oil agent.

Compared with the prior art, the invention has the advantages that: the organic silicon phosphate is selected as the antistatic agent, so that the antistatic property of the oil agent can be effectively improved, and the problem that the oil agent smokes and cokes due to the fact that the traditional fatty alcohol polyoxyethylene ether phosphate is not high-temperature resistant can be effectively solved. Meanwhile, the oil agent has high oil film strength, good adhesiveness and uniform and stable oiling, can ensure that the fiber has better antistatic property, smoothness, heat resistance and softness, can meet the processing requirements of a polyester FDY spinning process, and ensures the smooth production of the fiber.

Detailed Description

The technical solution of the present invention is further described with reference to the following specific examples.

Example 1:

the embodiment provides a terylene FDY oiling agent which comprises the following components in parts by weight:

1. 5 kg of hydroxyl organic silicon phosphate potassium salt

2. 30 kg of polyethylene glycol 400 oleic acid monoester

3. Butanol-terminated atactic polyether (number-average molecular weight Mn 1000) 20 kg

4.32# refined mineral oil 20 kg

5. 10 kg of trimethylolpropane monooleate

6. Secondary sodium alkylsulfonate SAS 605 kg

7. 10 kg of deionized water

In this example, the potassium salt of a hydroxy silicone phosphate has the formula:

wherein n is 20 and the number average molecular weight Mn is 1600.

The specific method and the steps for preparing the terylene FDY oiling agent are as follows:

weighing the components according to the mass of the components, adding the weighed components into a reaction kettle, starting stirring, heating to 40-50 ℃, stirring for 2-3 hours, cooling, filtering and discharging after the components are fully and uniformly mixed to obtain the yellow and transparent terylene FDY oiling agent.

The basic performance technical indexes of the polyester FDY oiling agent prepared by the embodiment are tested by adopting the following method:

1. appearance: the appearance color and state of the oil agent were visually observed.

2. Effective content: and testing by using a drying method.

pH value: the oil was diluted to 1% concentration with deionized water and tested with a PH meter.

4. Stability of oil stock solution: by observation, the oil stock solution is stored in a colorless transparent container in a sealed manner, and is placed in a cool and dry place to observe whether the oil is layered or not.

5. Emulsion stability: the oil crude oil was diluted to 15% concentration with deionized water and observed to see if the emulsion broke within 48 hours.

6. Specific resistance: testing according to a GB/T14342-93 test method. The temperature is 25 ℃ and the relative humidity is 65 percent by adopting a YG321 type fiber specific resistance instrument for testing.

7. Coefficient of friction: the test was carried out on a model R-1053 friction coefficient apparatus.

8. Oil film strength: preparing 15% emulsion with deionized water, and testing the maximum rupture pressure of the oil film on MRS-10 type four-ball friction instrument.

9. Heat resistance: accurately weighing 1g of oil agent, drying at 120 ℃ for 2 hours, and measuring the weight loss rate, smoke point and flash point of the oil agent. The test was carried out on a SYP1001 open flash tester for petroleum products.

10. Surface tension: the prepared 15% emulsion is tested on a JZHY-80 type surface tensiometer.

11. Emulsion wettability: a 15% emulsion was formulated and tested using standard canvas sedimentation.

12. Sizing property: and (3) uniformly mixing the slurry of the water jet loom with 8% and the 15% oil emulsion, putting the mixture into a watch glass, drying the mixture for 3 hours at the temperature of 60 ℃, then drying the mixture for 2 hours at the temperature of 85 ℃, and observing the film forming condition of the slurry.

Tests show that the terylene FDY oil agent compounded according to the formula of the embodiment has the following technical performance indexes:

1. appearance: light yellow transparent liquid

2. Effective content (%) 90. + -.1

3.PH (1% aqueous solution): 6 to 8

4. Solubility: is easy to disperse in water

5. Stock solution stability: stable for one year without layering and deterioration

6. Emulsion stability (15% aqueous solution): transparent with blue light, does not break emulsion for 48 hours at normal temperature

7. Specific resistance: 3.8X 10⁸Ω

8. Coefficient of dynamic friction mu_d：0.1142

9. Coefficient of static friction mu_s：0.3825

10. Oil film strength/(kgf): 95

11. Heat resistance: no coking at 150 deg.C and slight smoking

12. Emulsion surface tension (cn/cm): 31

13. Emulsion wettability (S): 8

14. Sizing property: has good compatibility with various sizing agents.

The emulsion is prepared from 15% by mass according to the mass ratio of oil to water of 1: 5.

Example 2:

according to the operation method and the steps provided by the embodiment 1, the terylene FDY oiling agent is prepared by adopting the following components and dosage:

1. 8 kg of hydroxyl polyether organic silicon phosphate potassium salt

2. 30 kg of polyethylene glycol 400 lauric acid monoester

3. Butanol-terminated atactic polyether (number-average molecular weight Mn 1000) 12 kg

4.32# refined mineral oil 20 kg

5. Quaternary tetraol monooleate 15 kg

6. Secondary sodium alkylsulfonate SAS 605 kg

7. 10 kg of deionized water

In this example, the potassium salt of a hydroxy polyether organosilicate has the formula:

，

wherein n is 20, a is 10, b is 5, and the number average molecular weight Mn is 3000.

According to the test method provided by the embodiment 1, the terylene FDY oil agent compounded according to the formula of the embodiment has the following technical performance indexes:

1. appearance: light yellow transparent liquid

2. Effective content (%) 90. + -.1

3.PH (1% aqueous solution): 6 to 8

4. Solubility: is easy to disperse in water

5. Stock solution stability: stable for one year without layering and deterioration

6. Emulsion stability (15% aqueous solution): transparent with blue light, does not break emulsion for 48 hours at normal temperature

7. Specific resistance: 1.6X 10⁸Ω

8. Coefficient of dynamic friction mu_d：0.1208

9. Coefficient of static friction mu_s：0.3945

10. Oil film strength/(kgf): 94.5

11. Heat resistance: no coking at 150 deg.C and slight smoking

12. Emulsion surface tension (cn/cm): 31

13. Emulsion wettability (S): 8

14. Sizing property: has good compatibility with various sizing agents.

The emulsion is prepared from 15% by mass according to the mass ratio of oil to water of 1: 5.

Example 3:

in the spinning process of the terylene FDY oiling agent provided by the embodiment 1 and 2 of the invention used for producing the terylene FDY with the fineness of 150D/72f, 150D/96f, 75D/48f and the like in a chemical fiber factory, the spinning speed is 4800m/min, the temperature of a second shaping hot roller is 140 ℃, fiber oiling is respectively carried out in an oiling way of an oil nozzle and an oil tanker, and the fiber oiling rate is 0.8 percent. The fiber spun by the oil agent has good performance in subsequent processing such as warping, sizing, dyeing, weaving and the like.