阅读说明：本技术 一种涤纶纺丝用fdy油剂 (FDY oil agent for polyester spinning ) 是由 王金雪 俞中锋 郝凌霄 杨佳伟 吴亚清 高宏飞 申宝兵 于 2021-01-22 设计创作，主要内容包括：本发明提供一种涤纶纺丝用FDY油剂,属于涤纶长丝加工领域。该涤纶纺丝用FDY油剂,含有40-60重量份的聚乙二醇烷基酸酯,5-15重量份的甘油酯乙氧基化物,4-6重量份的甘油酯乙氧基化物磷酸酯钾盐,5-25重量份的共聚PO/EO聚醚多元醇,15-25重量份的脂肪酸甲酯乙氧基化物,8-12重量份水,0.1-1重量份添加剂。本发明旨涤纶纺丝用FDY油剂,具有可纺性好,断头率低,发烟温度较高的特点。(The invention provides an FDY oiling agent for polyester spinning, belonging to the field of polyester filament yarn processing. The FDY oil agent for polyester spinning comprises 40-60 parts by weight of polyethylene glycol alkyl acid ester, 5-15 parts by weight of glyceride ethoxylate, 4-6 parts by weight of glyceride ethoxylate phosphate potassium salt, 5-25 parts by weight of copolymerized PO/EO polyether polyol, 15-25 parts by weight of fatty acid methyl ester ethoxylate, 8-12 parts by weight of water and 0.1-1 part by weight of additive. The FDY oiling agent for polyester spinning has the characteristics of good spinnability, low end breakage rate and higher fuming temperature.)

1. An FDY oil agent for polyester spinning comprises 40-60 parts by weight of polyethylene glycol alkyl acid ester, 5-15 parts by weight of glyceride ethoxylate, 4-6 parts by weight of glyceride ethoxylate phosphate potassium salt, 5-25 parts by weight of copolymerized PO/EO polyether polyol, 15-25 parts by weight of fatty acid methyl ester ethoxylate, 8-12 parts by weight of water and 0.1-1 part by weight of additive.

2. FDY oil according to claim 1, characterized in that the polyethylene glycol alkyl acid ester is a monoester or diester of polyethylene glycol having a number average molecular weight of 200-1200 and an unsaturated fatty acid.

3. FDY oil according to claim 1 or 2, characterized in that the number average molecular weight of the glycerol ester ethoxylate is 1500-.

4. FDY oil according to claim 3, characterized in that the potassium salt of the glycerol ester ethoxylate phosphate is obtained after esterification of the glycerol ester ethoxylate with diphosphorus pentoxide.

5. FDY finish according to claim 4, characterized in that the number average molecular weight of the copolymerized PO/EO polyether polyol is 800-2200.

6. FDY oil according to claim 5, characterized in that the fatty acid methyl ester ethoxylate has a number average molecular weight of 300-500 and the fatty acid is an unsaturated fatty acid.

7. FDY finish according to claim 6, characterized in that the fatty acid methyl ester ethoxylate is the same as one or more of the unsaturated fatty acids used in the polyethylene glycol alkyl acid ester.

8. FDY oil according to claim 7, characterized in that the additive is a mixture of a defoamer and polyethylene glycol in a mass ratio of 1: 1-2.

9. A process for preparing an FDY finish as claimed in claim 1 comprising the steps of: uniformly mixing polyethylene glycol alkyl acid ester to obtain a mixture 1; uniformly mixing the glyceride ethoxylate and phosphate potassium salt of the glyceride ethoxylate to obtain a mixture 2; uniformly mixing fatty acid methyl ester ethoxylate to obtain a mixture 3; uniformly mixing the copolymerized PO/EO polyether polyol to obtain a mixture 4; and under the stirring state, sequentially adding the mixtures 2, 3 and 4 into the mixture 1, uniformly stirring, placing at 55-65 ℃ for 40-50 hours, adding water and additives, stirring, performing centrifugal separation, and removing precipitates to obtain the FDY oil agent.

Technical Field

The invention belongs to the field of polyester filament yarn processing, and particularly relates to an FDY oil agent for polyester spinning.

Background

Various industrial fibers generate static electricity due to friction during spinning and accumulate. The chargeability of the fiber is mainly determined by the chemical properties and structure of the fiber. The polyester fiber is one of the fibers with the largest industrial use amount at present, and is a macromolecular compound taking a covalent bond as a main chain, and because the macromolecular compound cannot be ionized and can not transfer electrons or ions, and the molecules of the macromolecular compound have hydrophobicity and small polarity of molecular groups, the charge is not easy to escape in the processing process. In the spinning process, static electricity can be generated in the system due to continuous friction between the yarns or between the yarns and the rolling shaft, and because the insulation property of the terylene is good and the resistance is large, the static electricity is released very slowly, so that charge accumulation can be caused, and further danger is caused.

The chemical fiber oil, especially high speed spinning oil, is prepared with main surfactant including antistatic agent, smoothing agent, bundling agent, emulsifier, etc. The existing FDY oil agent for polyester spinning has lower fuming temperature and higher end breakage rate.

Disclosure of Invention

The invention aims to provide an FDY oil agent for polyester spinning, which has the characteristics of good spinnability, low end breakage rate and higher smoke temperature.

The purpose of the invention is realized by adopting the following technical scheme:

an FDY oil agent for polyester spinning comprises 40-60 parts by weight of polyethylene glycol alkyl acid ester, 5-15 parts by weight of glyceride ethoxylate, 4-6 parts by weight of glyceride ethoxylate phosphate potassium salt, 5-25 parts by weight of copolymerized PO/EO polyether polyol, 15-25 parts by weight of fatty acid methyl ester ethoxylate, 8-12 parts by weight of water and 0.1-1 part by weight of additive.

In the present invention, the polyethylene glycol alkyl acid ester is a monoester or diester of polyethylene glycol having a number average molecular weight of 200-1200 and an unsaturated fatty acid.

In the present invention, the number average molecular weight of the glyceride ethoxylate is 1500-.

In the invention, the potassium glyceride ethoxylate phosphate is obtained after the glyceride ethoxylate is esterified with the diphosphorus pentoxide.

In the present invention, the number average molecular weight of the copolymerized PO/EO polyether polyol is 800-.

In the present invention, the number average molecular weight of the fatty acid methyl ester ethoxylate is 300-500, and the fatty acid is an unsaturated fatty acid.

In the present invention, one or more of the unsaturated fatty acids used in the fatty acid methyl ester ethoxylate and the polyethylene glycol alkyl acid ester are the same, so that the stability is good.

In the invention, the additive is a mixture of a defoaming agent and polyethylene glycol according to a mass ratio of 1: 1-2.

The invention also provides a preparation method of the FDY oiling agent, which comprises the following steps: uniformly mixing polyethylene glycol alkyl acid ester to obtain a mixture 1; uniformly mixing the glyceride ethoxylate and phosphate potassium salt of the glyceride ethoxylate to obtain a mixture 2; uniformly mixing fatty acid methyl ester ethoxylate to obtain a mixture 3; uniformly mixing the copolymerized PO/EO polyether polyol to obtain a mixture 4; and under the stirring state, sequentially adding the mixtures 2, 3 and 4 into the mixture 1, uniformly stirring, placing at 55-65 ℃ for 40-50 hours, adding water and additives, stirring, performing centrifugal separation, and removing precipitates to obtain the FDY oil agent.

The FDY oiling agent for polyester spinning has the characteristics of good stability, good spinnability, low end breakage rate and higher fuming temperature.

Detailed Description

Example 1

The preparation method of the FDY oiling agent 1 comprises the following steps:

(1) weighing the following components: 10g of polyethylene glycol oleic acid diester A, 20g of polyethylene glycol oleic acid diester B, 10g of polyethylene glycol oleic acid monoester C, 10g of polyethylene glycol oleic acid diester D, 8g of glycerol ethoxylate A, 5g of potassium phosphate salt of glycerol ethoxylate A, 3g of copolymerized PO/EO polyether polyol B, 10g of fatty acid methyl ester ethoxylate A, 10g of fatty acid methyl ester ethoxylate B, 10g of deionized water and 0.5g of additives. Wherein the additives are: the defoaming agent ZS-2802 (Jiangsu clock hill chemical industry Co., Ltd.) and the polyethylene glycol 400 are mixed according to the mass ratio of 1: 1.

(2) Uniformly mixing polyethylene glycol oleic acid diester A, polyethylene glycol oleic acid diester B, polyethylene glycol oleic acid monoester C and polyethylene glycol oleic acid diester D to obtain a mixture 1; uniformly mixing the glyceride ethoxylate A and phosphate potassium salt of the glyceride ethoxylate A to obtain a mixture 2; uniformly mixing the fatty acid methyl ester ethoxylate A and the fatty acid methyl ester ethoxylate B to obtain a mixture 3; uniformly mixing the copolymerized PO/EO polyether polyol A and the copolymerized PO/EO polyether polyol B to obtain a mixture 4;

(3) adding the mixture 2 into the mixture 1 under the stirring state, and uniformly stirring; then, under the stirring state, adding the mixture 3, and uniformly stirring; under stirring, the mixture 4 was added and stirred uniformly. Then, the mixture was stirred for two hours and stored in an oven at 60 ℃ for 48 hours. And after the thermal storage is finished, adding water and the additive, stirring for 60 minutes, then carrying out centrifugal separation, discarding precipitates (impurities), and taking the liquid as the FDY oil agent 1.

Example 2

The preparation method of the FDY oiling agent 2 comprises the following steps:

(1) weighing the following components: 10g polyethylene glycol oleic acid diester A; 25g of polyethylene glycol oleic acid diester D; 15g of polyethylene glycol oleic acid monoester E; 8g of glycerol ester ethoxylate A; 3g of glycerol ester ethoxylate C; 3g potassium phosphate salt of glycerol ester ethoxylate A; 3g potassium phosphate salt of glycerol ester ethoxylate C; 3g of copolymerized PO/EO polyether polyol E; 3g of copolymerized PO/EO polyether polyol F. 6g of fatty acid methyl ester ethoxylate A; 10g of fatty acid methyl ester ethoxylate B; 10g of deionized water; 0.2g of additive. Wherein the additives are: the defoaming agent ZS-2802 (Jiangsu clock hill chemical industry Co., Ltd.) and the polyethylene glycol 400 are mixed according to the mass ratio of 1: 2, or a mixture thereof.

(2) Uniformly mixing polyethylene glycol oleic acid diester A, polyethylene glycol oleic acid diester D and polyethylene glycol oleic acid monoester E to obtain a mixture 1; uniformly mixing glyceride ethoxylate A, glyceride ethoxylate C, phosphate potassium salt of glyceride ethoxylate A and phosphate potassium salt of glyceride ethoxylate C to obtain a mixture 2; uniformly mixing the fatty acid methyl ester ethoxylate A and the fatty acid methyl ester ethoxylate B to obtain a mixture 3; uniformly mixing the copolymerized PO/EO polyether polyol E and the copolymerized PO/EO polyether polyol F to obtain a mixture 4;

(3) adding the mixture 2 into the mixture 1 under the stirring state, and uniformly stirring; then, under the stirring state, adding the mixture 3, and uniformly stirring; under stirring, the mixture 4 was added and stirred uniformly. Then, the mixture was stirred for two hours and stored in an oven at 60 ℃ for 48 hours. And after the thermal storage is finished, adding water and the additive, stirring for 60 minutes, then carrying out centrifugal separation, discarding precipitates (impurities), and taking the liquid as the FDY oil agent 2.

Example 3

The preparation method of the FDY oiling agent 3 comprises the following steps:

(1) weighing the following components: 5g polyethylene glycol oleic acid diester A; 15g of polyethylene glycol oleic acid diester F; 15G polyethylene glycol oleic acid monoester G; 10g of polyethylene glycol oleic acid monoester E; 3g of glycerol ester ethoxylate A; 5g of glycerol ester ethoxylate B; 2g potassium phosphate salt of glycerol ester ethoxylate A; 2g potassium phosphate salt of glycerol ester ethoxylate B; 12g of copolymerized PO/EO polyether polyol C; 8g of copolymerized PO/EO polyether polyol D; 5g of fatty acid methyl ester ethoxylate C; 5g of fatty acid methyl ester ethoxylate D; 5g of fatty acid methyl ester ethoxylate E; 10g of deionized water; 0.1g of additive. Wherein the additives are: the defoaming agent ZS-2802 (Jiangsu clock hill chemical industry Co., Ltd.) and the polyethylene glycol 600 are mixed according to the mass ratio of 1: 1.

(2) Uniformly mixing polyethylene glycol oleic acid diester A, polyethylene glycol oleic acid diester F, polyethylene glycol oleic acid monoester G and polyethylene glycol oleic acid monoester E to obtain a mixture 1; uniformly mixing glyceride ethoxylate A, glyceride ethoxylate B, potassium phosphate salt of glyceride ethoxylate A and potassium phosphate salt of glyceride ethoxylate B to obtain a mixture 2; uniformly mixing fatty acid methyl ester ethoxylate C, fatty acid methyl ester ethoxylate D and fatty acid methyl ester ethoxylate E to obtain a mixture 3; uniformly mixing the copolymerized PO/EO polyether polyol C and the copolymerized PO/EO polyether polyol D to obtain a mixture 4;

(3) adding the mixture 2 into the mixture 1 under the stirring state, and uniformly stirring; then, under the stirring state, adding the mixture 3, and uniformly stirring; under stirring, the mixture 4 was added and stirred uniformly. Then, the mixture was stirred for two hours and stored in an oven at 60 ℃ for 48 hours. And after the thermal storage is finished, adding water and the additive, stirring for 60 minutes, then carrying out centrifugal separation, discarding precipitates (impurities), and taking the liquid as the FDY oil agent 3.

The ingredients of examples 1-3 were prepared by the methods of examples 4-8.

EXAMPLE 4 preparation of Mono-and diesters of Polyethyleneglycol oleic acid

The following methods are respectively adopted to prepare polyethylene glycol oleic acid monoester and polyethylene glycol oleic acid diester: adding polyethylene glycol into a kettle, adding citric acid (catalyst), starting a stirrer, replacing with nitrogen for 3 times, heating to 130 ℃, and dehydrating at 130 ℃ under vacuum for 1.5 hours. Heating to 180 ℃, vacuumizing to the pressure of-0.095 MPa, closing the vacuum, introducing oleic acid, heating to 210 ℃, preserving the heat at 210 ℃ for 7 hours, vacuumizing and keeping the vacuum state for 0.5 hour. Cooling to 100 ℃, and pressing the materials into a treatment kettle. In a treatment kettle, when the temperature of the materials is 70-80 ℃, adding water accounting for 5% of the mass of the materials and phosphoric acid accounting for 0.1% of the mass of the materials, stirring for 1 hour, then adding silicate clay (refining agent) accounting for 0.5% of the mass of the materials, stirring for 0.5 hour, heating to 120-130 ℃ for dehydration, filtering until the water content is qualified, and discharging to obtain the polyethylene glycol oleic acid monoester and diester. The number average molecular weight (Mn) and the addition amount of polyethylene glycol, the amount of catalyst and the addition amount (g) of oleic acid in the preparation of polyethylene glycol oleic acid monoester and diester are shown in Table 1.

TABLE 1

Example 5 glyceride ethoxylate preparation

Adding oleum ricini into kettle, adding catalyst (MgO, Al)₂O₃And TiO₂And the molar ratio of Mg, Al and Ti is 1: 3: 0.5), starting the stirrer, replacing the stirrer with nitrogen for 3 times, heating to 135 ℃, and then dehydrating for 2 hours at 135 ℃ under a vacuum condition. Heating to 140 ℃, vacuumizing until the pressure is-0.095 MPa, closing the vacuum, introducing ethylene oxide, heating to 160 ℃, aging at 160 ℃ for 2 hours after the ethylene oxide is introduced, vacuumizing, maintaining the vacuum state for 0.5 hour, cooling to 80 ℃, and pressing into a treatment kettle. When the temperature of the materials is reduced to 70-80 ℃, 160g of water and 20.2g of phosphoric acid are added, stirred for 1 hour, and thenAdding 8g of argil (refining agent), stirring for 0.5 hour, heating to 120-130 ℃, dehydrating until the water content is qualified, filtering and discharging.

TABLE 2

EXAMPLE 6 preparation of a copolymerized PO/EO polyether polyol

The starter and catalyst (KOH) were charged to a 0.5L autoclave. The autoclave was connected to a storage tank containing a mixed gas of ethylene oxide and propylene oxide. Heating to 80 deg.C under stirring, vacuumizing to remove trace water and other low-boiling-point substances, and adding N₂The residual air in the kettle was replaced. Heating to 140 deg.C, maintaining the temperature, controlling the pressure to 0.35Mpa, and continuously and stably introducing the mixture of ethylene oxide and propylene oxide. And after the mixture of ethylene oxide and propylene oxide is introduced, aging for 30min, introducing cooling water for cooling, releasing pressure, removing the product, and removing the catalyst by a conventional method to obtain the copolymerized PO/EO polyether polyol.

TABLE 3 products and raw materials and amounts thereof used in their preparation

In table 3: EO is an abbreviation for ethylene oxide and PO is an abbreviation for propylene oxide.

Example 7 fatty acid methyl ester ethoxylate preparation

Mixing a certain amount of fatty acid methyl ester and proper amount of catalyst (MgO, Al)₂O₃And TiO₂And the molar ratio of Mg, Al and Ti is 1: 3: 0.5) into the autoclave. An ethylene oxide tank was connected to the autoclave. Heating to 80 deg.C under stirring in high-pressure autoclave, and vacuumizing to remove reactionTrace water and other low boiling point substances in the system are used for replacing the residual air in the kettle by N2. The autoclave is heated to 160 ℃, the pressure is controlled to be 0.3Mpa, and the ethylene oxide is continuously and stably introduced to the required amount. And after the introduction of the ethylene oxide is finished, aging for 30min, introducing cooling water for cooling, releasing pressure, removing the product, and filtering out the catalyst to obtain the fatty acid methyl ester ethoxylate. The amounts of the products and the fatty acid methyl esters, ethylene oxide and catalyst used during the reaction are shown in Table 4.

TABLE 4 specific raw material usage for each product and preparation

EXAMPLE 8 preparation of Potassium salt of Glycerol Ether ethoxylate phosphate

The glycerol ester ethoxylate A, glycerol ester ethoxylate B and glycerol ester ethoxylate C obtained in example 5 were each reacted with phosphorus pentoxide to prepare the corresponding potassium salts of glycerol ester ethoxylate phosphate esters. The specific method comprises the following steps: adding the glyceride ethoxylate into a round-bottom flask, keeping the temperature at 60 ℃ under normal pressure, and mixing the glyceride ethoxylate and phosphorus pentoxide in a molar ratio of 1:1 adding phosphorus pentoxide powder, stirring, and keeping the temperature at 60 ℃ for 1 hour. Adding water accounting for 30 percent of the total mass of the glyceride ethoxylate and the phosphorus pentoxide, continuously stirring and preserving the temperature for 3 hours, and finally adding KOH to adjust the pH value to 6-7. Cooling, filtering and removing the product.

Example 9 test results of spin finish

The smoke temperature test method specifically comprises the following steps: 20g of each of the FDY oil solutions of examples 1 to 3 and a commercially available sample GXM-100 (rosin oil and fat) was placed in an evaporation pan having a diameter of 10cm, heated on a heating plate, and the smoking phenomenon was captured by a camera to determine the smoking temperature.

Smoke emission test: 20g of FDY oil solution obtained in examples 1 to 3 and a commercially available sample GXM-100 (rosin oil and fat) were put in a 50ml beaker, placed in an oven for 1 hour, and then taken out and cooled. The difference between the front and the back quality is the smoke amount of each product. The temperature at which each product is placed in the oven is the smoking temperature of each product.

The FDY oil solution and the commercially available sample GXM-100 (rosin oil and fat) in examples 1 to 3 were tried on terylene 200D/144F, and the breakage rate, the full bobbin rate and the waste silk rate were examined.

The results of the above tests are shown in Table 5. The FDY oiling agents in the examples 1-3 have good spinnability, low end breakage rate, high full bobbin ratio, low waste silk rate, higher smoking temperature, no smoke or trace smoke and no corrosion.

TABLE 5FDY oil and commercial sample GXM-100 (rosin oil) Properties