Polyester staple fiber oiling agent and preparation method thereof

Abstract

According to the polyester staple fiber oiling agent and the preparation method thereof, firstly, crystalline flake graphite powder is subjected to surface modification treatment, amino and double bonds are introduced to the surface of the crystalline flake graphite powder, then, under the action of an initiator potassium persulfate, the modified crystalline flake graphite powder, butadiene, styrene and acrylic acid are subjected to a double-bond addition reaction, and the polyester staple fiber oiling agent is obtained. The crystalline flake graphite powder is doped in a molecular chain of carboxylic butadiene-styrene latex through chemical action, the crystalline flake graphite powder serves as a conductive component to be introduced into the oiling agent, the polyester staple fibers are treated through the oiling agent, an antistatic film layer is formed on the surfaces of the polyester staple fibers, and the antistatic film layer contains the crystalline flake graphite powder and a carboxylic butadiene-styrene structure, so that the antistatic property of the polyester staple fibers is improved. The crystalline flake graphite powder and the carboxylated styrene-butadiene structure both have certain conductivity and form a conductive path, so that the resistance of the surface of the fiber can be greatly reduced, and the treated polyester staple fiber has a good antistatic effect.

Description

[0001] This application is a divisional application. The application number of the original application is 202410659504.8, and the original application date is May 27, 2024. The entire content of the original application is incorporated into this application by reference. Technical Field

[0002] The invention relates to the technical field of oil preparation, in particular to a polyester staple fiber oil and a preparation method thereof. Background Art

[0003] Polyester staple fiber oil is a surfactant specifically formulated for polyester staple fibers. Composed primarily of fatty acid esters, polyols, and polymers, it exhibits excellent lubricity, antistatic properties, softness, and durability. This oil plays a crucial role in spinning, stretching, spinning, and weaving processes, primarily by improving fiber smoothness, maintaining an optimal coefficient of friction between fibers and between fibers and other contacting parts, and reducing and rapidly dissipating static electricity generated during fiber production and processing.

[0004] Polyester staple fiber oils not only have an antistatic effect on polyester staple fiber production but also play a significant role in textile processing. During textile processing, polyester staple fibers undergo processes such as blowroom, carding, and drawing. As they pass through various textile machines, frictional static electricity generated between fibers and between fibers and equipment significantly impacts the textile process. Staple fiber oils are designed to impart different frictional properties and bundle-forming properties to the staple fibers, tailored to the specific process, thereby ensuring smooth spinning and weaving.

[0005] In addition, polyester staple fiber oil agent has the characteristics of simple preparation, easy use, and wide applicability. It can make the fiber after oiling uniform in color, soft and smooth to the touch, and has good antistatic properties, bundling properties, and smoothness. It is suitable for the production of various polyester staple fibers.

[0006] In recent years, significant progress has been made in the research of polyester staple fiber lubricants, including the development of new polyester staple fiber lubricants, the synthesis and application of high-carbon alkyl phosphate potassium salts (PK), the research and development of alternatives to alkylamine polyoxyethylene ethers (APEOs), the optimization and screening of lubricant formulations, and the research and practice of green production. However, due to the type and ratio of the selected compositions, the lubricants developed in recent years often suffer from poor antistatic properties, high fiber resistivity, and difficulties in forming nonwoven webs and hydroentanglement.

[0007] Chinese patent document CN201811419659.5 discloses a polyester staple fiber oil agent, which includes the following components, in parts by weight: 20 to 40 parts of secondary alkyl phosphate salt, 20 to 40 parts of fatty alcohol phosphate polyoxyethylene ether, 10 to 30 parts of fatty acid polyoxyethylene ester, and 10 to 30 parts of fatty amine polyoxyethylene polyoxypropylene ether. Although the antistatic properties of the prepared polyester staple fiber oil agent are improved, further improvement is still needed. Summary of the Invention

[0008] In view of the shortcomings of the prior art, the purpose of the present invention is to provide a polyester staple fiber oil agent and a preparation method thereof. The prepared oil agent can form an antistatic film layer on the surface of the polyester staple fiber and has a long-lasting antistatic effect.

[0009] In order to achieve the above object, the present invention adopts the following technical solutions: A polyester staple fiber oil comprises the following raw materials in parts by weight: 40-60 parts of a smoothing agent, 1-3 parts of a sizing agent, 8-15 parts of an antistatic liquid, 10-15 parts of an emulsifier, 1-3 parts of an antioxidant, and 0.5-1 part of a defoaming agent.

[0010] Specifically, the preparation method of the antistatic liquid is as follows: S1. Ultrasonic dispersion of flake graphite powder in an ethanol aqueous solution, followed by addition of dimethyl (dimethylamino) vinyl silane, stirring at 40-60° C. for 1-3 hours, followed by filtering, washing, and drying to obtain modified flake graphite powder; S2. Add modified flake graphite powder, sodium dodecyl sulfate and tert-dodecyl mercaptan to deionized water, stir evenly, introduce nitrogen to expel the air, then add butadiene, styrene and acrylic acid, stir and heat to 60-70°C, add initiator potassium persulfate, react for 2-3 hours, and after the reaction is completed, an antistatic liquid is obtained.

[0011] Preferably, in step S1, the mass ratio of flake graphite powder and dimethyl (dimethylamino) vinyl silane is 8-12:1-3. In some embodiments of the present invention, for example, 8:1, 8:2, 8:3, 10:1, 10:2, 10:3, 12:1, 12:2, 12:3 can be selected, but is not limited to the listed values. Other values not listed within the numerical range are also applicable.

[0012] Preferably, the mass fraction of the ethanol aqueous solution is 60-80%. In some embodiments of the present invention, for example, 60%, 65%, 70%, 75%, and 80% can be selected, but it is not limited to the listed values. Other values not listed within the numerical range are also applicable.

[0013] Preferably, in step S2, the mass ratio of modified flake graphite powder, sodium dodecyl sulfate, tert-dodecyl mercaptan, deionized water, butadiene, styrene, acrylic acid and potassium persulfate is 4-6:1-2:1-2:100:15-25:20-30:10-15:0.8-1.5. It should be noted that the initiator selected in this application is potassium persulfate, and other commonly used initiators in this field are also applicable.

[0014] Specifically, the smoothing agent is selected from at least one of glycerol monooleate, glycerol monostearate, glycerol monopalmitate, lauryl oleate, isooctyl stearate, and trihydroxypropane isooctyl ester. The purpose of adding the smoothing agent is to reduce the friction coefficient between fibers and between fibers and other contact parts, and to prevent fibers from becoming fuzzy or broken during subsequent processing.

[0015] Specifically, the sizing agent is selected from at least one of polyoxyethylene laurate, glycerol random polyether, and N-acyl amino acid salt.

[0016] Specifically, the emulsifier is selected from at least one of stearate, N-methylamide carboxylate, and sorbitan fatty acid ester polyoxyethylene ether. The purpose of adding the emulsifier is to reduce the interfacial tension between the surfactant and water and maintain the relative stability of the solution.

[0017] Specifically, the antioxidant is selected from at least one of antioxidant 1076 and antioxidant 1035. The purpose of adding the antioxidant is to improve the antioxidant performance of the oil, effectively inhibit or slow down the oxidation of the smoothing agent and the bundling agent at high temperature, and at the same time reduce the generation of smoke on site and improve the working environment of the spinning site.

[0018] Specifically, the defoaming agent is selected from at least one of tributyl phosphate and polydimethylsiloxane. The purpose of adding the defoaming agent is to reduce the generation of foam, and at the same time, it can also reduce the formation of sediment in the oil bath and reduce the frequency of cleaning the oil bath.

[0019] The present invention also provides a preparation method of the above-mentioned polyester staple fiber oil agent, comprising the following steps: weighing each component by weight, then adding an emulsifier, a sizing agent, an antioxidant and an antistatic liquid into a reactor, stirring at 150-200 r / min for 30-60 min at 40-60° C., then adding a smoothing agent, stirring at 600-800 r / min for 30-60 min, then adding a defoaming agent, continuing to stir at 100-150 r / min for 15-30 min, and cooling to room temperature to obtain the polyester staple fiber oil agent.

[0020] Compared with the prior art, the present invention has the following beneficial effects: (1) The present invention first performs surface modification treatment on flake graphite powder, introduces amino groups and double bonds on the surface of flake graphite powder, and then, under the action of initiator potassium persulfate, performs double bond addition reaction on modified flake graphite powder, butadiene, styrene and acrylic acid, and the flake graphite powder is doped in the molecular chain of carboxyl styrene butadiene latex through chemical action, and is introduced into the oil agent as a conductive component, and the oil agent is used to treat polyester staple fiber, forming an antistatic film layer on the surface of polyester staple fiber, the antistatic film layer contains flake graphite powder and carboxyl styrene butadiene structure, the flake graphite powder and carboxyl styrene butadiene structure both have certain conductive properties, and the two form a conductive path, which can greatly reduce the resistance of the fiber surface, so that the treated polyester staple fiber has good antistatic effect.

[0021] (2) The flake graphite powder in the antistatic film layer has a layered structure. Since the interlayer van der Waals force of the layered structure is weak, interlayer slippage is likely to occur under external friction, which can effectively reduce the wear of the antistatic film layer and help improve the integrity of the antistatic film layer, so that the treated polyester staple fiber has a long-lasting antistatic effect; at the same time, the amino groups on the surface of the flake graphite powder and the carboxyl groups in the carboxyl butadiene structure interact with the hydroxyl groups on the surface of the polyester staple fiber through hydrogen bonding, so that the antistatic film layer can be firmly attached to the surface of the polyester staple fiber, further improving the long-lasting antistatic effect of the polyester staple fiber. DETAILED DESCRIPTION

[0022] The present invention is further described in detail below through specific preferred embodiments, but the present invention is not limited to the following embodiments.

[0023] It should be noted that, unless otherwise specified, all chemical reagents involved in the present invention were purchased through commercial channels.

[0024] The mesh size of the flake graphite powder used in the present invention is 400 mesh.

[0025] Example 1 A method for preparing a polyester staple fiber oil agent comprises the following steps: 10 parts of emulsifier sodium stearate, 2 parts of sizing agent polyoxyethylene laurate, 1 part of antioxidant 1076 and 10 parts of antistatic liquid were added to a reactor, stirred at 200 r / min for 40 minutes at 50°C, then 40 parts of smoothing agent glycerol monooleate were added, stirred at 600 r / min for 30 minutes, and then 0.5 parts of defoaming agent tributyl phosphate were added, stirred at 120 r / min for 30 minutes, and cooled to room temperature to obtain a polyester staple fiber oil. Wherein, the preparation method of the antistatic liquid is as follows: S1. Ultrasonic dispersion of 10 g of flake graphite powder in 100 mL of 75 wt% ethanol aqueous solution was followed by addition of 1 g of dimethyl (dimethylamino) vinyl silane, followed by stirring at 40 °C for 2 h, followed by filtration, washing, and drying to obtain modified flake graphite powder; S2. Add 4g of modified flake graphite powder, 1g of sodium dodecyl sulfate and 1g of tert-dodecyl mercaptan to 100g of deionized water, stir evenly, introduce nitrogen to expel the air, then add 15g of butadiene, 20g of styrene and 10g of acrylic acid, stir and heat to 60°C, add 1g of initiator potassium persulfate, react for 2h, and after the reaction is completed, an antistatic liquid is obtained.

[0026] Example 2 A method for preparing a polyester staple fiber oil agent comprises the following steps: 15 parts of emulsifier sodium N-methylamide carboxylate, 1 part of sizing agent glycerol random polyether, 1 part of antioxidant 1076 and 10 parts of antistatic liquid were added to a reactor, stirred at 150 r / min for 30 min at 60°C, then 60 parts of smoothing agent glycerol monostearate were added, stirred at 600 r / min for 30 min, and then 0.8 parts of defoaming agent polydimethylsiloxane was added, stirred at 150 r / min for 15 min, and cooled to room temperature to obtain a polyester staple fiber oil. Wherein, the preparation method of the antistatic liquid is as follows: S1. 8 g of flake graphite powder was ultrasonically dispersed in 100 mL of a 75 wt% ethanol aqueous solution, and then 1 g of dimethyl (dimethylamino) vinyl silane was added thereto. The mixture was stirred at 60 ° C for 1 h, and then filtered, washed, and dried to obtain modified flake graphite powder; S2. Add 6g of modified flake graphite powder, 2g of sodium dodecyl sulfate and 1g of tert-dodecyl mercaptan to 100g of deionized water, stir evenly, introduce nitrogen to expel the air, then add 25g of butadiene, 20g of styrene and 15g of acrylic acid, stir and heat to 60°C, add 1.2g of initiator potassium persulfate, react for 3h, and after the reaction is completed, an antistatic liquid is obtained.

[0027] Example 3 A method for preparing a polyester staple fiber oil agent comprises the following steps: 10 parts of emulsifier sorbitan fatty acid ester polyoxyethylene ether, 3 parts of sizing agent glycerol random polyether, 2 parts of antioxidant 1076 and 15 parts of antistatic liquid were added to a reactor, stirred at 200 r / min for 30 min at 60°C, then 50 parts of smoothing agent glycerol monostearate were added, stirred at 800 r / min for 30 min, and then 1 part of defoaming agent polydimethylsiloxane was added, stirred at 100 r / min for 30 min, and cooled to room temperature to obtain a polyester staple fiber oil. Wherein, the preparation method of the antistatic liquid is as follows: S1. Ultrasonic dispersion of 12 g of flake graphite powder in 100 mL of 75 wt% ethanol aqueous solution was followed by addition of 3 g of dimethyl(dimethylamino)vinylsilane, followed by stirring at 40 °C for 3 h, followed by filtration, washing, and drying to obtain modified flake graphite powder; S2. Add 5g of modified flake graphite powder, 2g of sodium dodecyl sulfate and 2g of tert-dodecyl mercaptan to 100g of deionized water, stir evenly, introduce nitrogen to expel the air, then add 25g of butadiene, 30g of styrene and 10g of acrylic acid, stir and heat to 60°C, add 1.5g of initiator potassium persulfate, react for 3h, and after the reaction is completed, an antistatic liquid is obtained.

[0028] Example 4 A method for preparing a polyester staple fiber oil agent comprises the following steps: 12 parts of emulsifier sodium N-methylamide carboxylate, 2 parts of sizing agent glycerol random polyether, 3 parts of antioxidant 1076 and 8 parts of antistatic liquid were added to a reactor, stirred at 200 r / min for 30 minutes at 60°C, then 45 parts of smoothing agent glycerol monostearate were added, stirred at 800 r / min for 30 minutes, and then 0.5 parts of defoaming agent polydimethylsiloxane were added, stirred at 100 r / min for 30 minutes, and cooled to room temperature to obtain a polyester staple fiber oil. Wherein, the preparation method of the antistatic liquid is as follows: S1. Ultrasonic dispersion of 10 g of flake graphite powder in 100 mL of 75 wt% ethanol aqueous solution was followed by addition of 3 g of dimethyl(dimethylamino)vinylsilane, followed by stirring at 40 °C for 3 h, followed by filtration, washing, and drying to obtain modified flake graphite powder; S2. Add 6g of modified flake graphite powder, 2g of sodium dodecyl sulfate and 2g of tert-dodecyl mercaptan to 100g of deionized water, stir evenly, introduce nitrogen to expel the air, then add 25g of butadiene, 30g of styrene and 15g of acrylic acid, stir and heat to 65°C, add 1.5g of initiator potassium persulfate, react for 3h, and after the reaction is completed, an antistatic liquid is obtained.

[0029] Comparative Example 1 A method for preparing a polyester staple fiber oil agent comprises the following steps: 10 parts of emulsifier sodium stearate, 2 parts of sizing agent polyoxyethylene laurate, 1 part of antioxidant 1076 and 10 parts of antistatic liquid were added to a reactor, stirred at 200 r / min for 40 minutes at 50°C, then 40 parts of smoothing agent glycerol monooleate were added, stirred at 600 r / min for 30 minutes, and then 0.5 parts of defoaming agent tributyl phosphate were added, stirred at 120 r / min for 30 minutes, and cooled to room temperature to obtain a polyester staple fiber oil. Wherein, the preparation method of the antistatic liquid is as follows: Add 1g of sodium dodecyl sulfate and 1g of tert-dodecyl mercaptan to 100g of deionized water, stir evenly, introduce nitrogen to expel the air, then add 15g of butadiene, 20g of styrene, and 10g of acrylic acid, stir and heat to 60°C, add 1g of initiator potassium persulfate, react for 2h, and after the reaction is completed, an antistatic liquid is obtained.

[0030] Compared with Example 1, in this comparative example, no flake graphite powder is added to the antistatic liquid.

[0031] Comparative Example 2 A method for preparing a polyester staple fiber oil agent comprises the following steps: 10 parts of emulsifier sodium stearate, 2 parts of sizing agent polyoxyethylene laurate, 1 part of antioxidant 1076 and 10 parts of antistatic liquid were added to a reactor, stirred at 200 r / min for 40 minutes at 50°C, then 40 parts of smoothing agent glycerol monooleate were added, stirred at 600 r / min for 30 minutes, and then 0.5 parts of defoaming agent tributyl phosphate were added, stirred at 120 r / min for 30 minutes, and cooled to room temperature to obtain a polyester staple fiber oil. Wherein, the preparation method of the antistatic liquid is as follows: Add 4 g of flake graphite powder, 1 g of sodium dodecyl sulfate and 1 g of tert-dodecyl mercaptan to 100 g of deionized water, stir evenly, introduce nitrogen to expel the air, then add 15 g of butadiene, 20 g of styrene and 10 g of acrylic acid, stir and heat to 60°C, add 1 g of initiator potassium persulfate, react for 2 h, and after the reaction is completed, an antistatic liquid is obtained.

[0032] Compared with Example 1, this comparative example does not perform modification treatment on the flake graphite powder.

[0033] Oil-free polyester staple fibers were immersed in the oils prepared in Examples 1-4 and Comparative Examples 1-2 for 5 minutes, dried, and dried in an oven at 100° C. for 6 hours to prepare test fiber samples, which were then tested as follows: Friction coefficient measurement: The test was performed using a Y151 fiber friction coefficient tester at a speed of 2 m / min and a pre-tension of 5 g. The test results are shown in Table 1: Table 1 Antistatic property test: The prepared fiber sample to be tested is woven into a fabric in a plain weave form, and the test is conducted with reference to GB / T 12703.5-2010 Textiles - Evaluation of electrostatic properties - Part 5: Triboelectric voltage. Antistatic property retention after 10 washes: The fabric was cut into 10 cm square specimens according to GB / T 12490. The samples were washed at 40°C with detergent (AATCC 1993 standard detergent WOB) for 2 hours. After drying, the antistatic property retention was tested after 10 cycles of washing and drying. The test results are shown in Table 2. Table 2 Finally, it should be noted that the above embodiments do not limit the present invention in any form. Those skilled in the art will appreciate that modifications and improvements can be made based on the present invention. Therefore, any modifications or improvements made without departing from the spirit of the present invention are intended to fall within the scope of protection claimed in the present invention.

Claims

1. Polyester staple fiber oil agent, characterized in that: The raw materials include the following components in parts by weight: 40-60 parts of smoothing agent, 1-3 parts of sizing agent, 8-15 parts of antistatic liquid, 10-15 parts of emulsifier, 1-3 parts of antioxidant, and 0.5-1 part of defoaming agent.

2. The polyester staple fiber oil according to claim 1, characterized in that The preparation method of the antistatic liquid is as follows: S1. Surface modification of flake graphite powder is performed by adding dimethyl (dimethylamino) vinyl silane to introduce amino groups and double bonds on the surface of the flake graphite powder to obtain modified flake graphite powder; S2. Under the action of initiator potassium persulfate, modified flake graphite powder, butadiene, styrene and acrylic acid undergo double bond addition reaction to obtain antistatic liquid, and the flake graphite powder is doped into the molecular chain of carboxyl styrene butadiene latex through chemical action.

3. The polyester staple fiber oil according to claim 2, characterized in that In step S1, flake graphite powder is ultrasonically dispersed in an ethanol aqueous solution, and then dimethyl (dimethylamino) vinyl silane is added, stirred at 40-60° C. for 1-3 hours, and then filtered, washed, and dried; the mass ratio of flake graphite powder to dimethyl (dimethylamino) vinyl silane is 8-12:1-3.

4. The polyester staple fiber oil according to claim 3, characterized in that In step S1, the mass fraction of the ethanol aqueous solution is 60-80%.

5. The polyester staple fiber oil according to claim 3, characterized in that In step S1, the mass ratio of flake graphite powder to dimethyl(dimethylamino)vinylsilane is selected from: 8:1, 8:2, 8:3, 10:1, 10:2, 10:3, 12:1, 12:2, 12:

3.

6. The polyester staple fiber oil according to claim 2, characterized in that In step S2, modified flake graphite powder, sodium dodecyl sulfate and tert-dodecyl mercaptan are added to deionized water, stirred evenly and the air is discharged, then butadiene, styrene and acrylic acid are added, stirred and heated to 60-70°C, initiator potassium persulfate is added, and the reaction is carried out for 2-3 hours. After the reaction is completed, an antistatic liquid is obtained; wherein, the mass ratio of modified flake graphite powder, sodium dodecyl sulfate, tert-dodecyl mercaptan, deionized water, butadiene, styrene, acrylic acid and potassium persulfate is 4-6:1-2:1-2:100:15-25:20-30:10-15:0.8-1.

5.

7. The method for preparing the polyester staple fiber oil according to any one of claims 1 to 6, characterized in that: The method comprises the following steps: weighing each component by weight, then adding an emulsifier, a sizing agent, an antioxidant and an antistatic liquid into a reaction kettle, stirring at 150-200 r / min for 30-60 min at 40-60°C, subsequently adding a smoothing agent, stirring at 600-800 r / min for 30-60 min, then adding a defoaming agent, continuing stirring at 100-150 r / min for 15-30 min, and cooling to room temperature to obtain a polyester staple fiber oil agent.

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