A polyester staple fiber oil agent and preparation method thereof

By using modified flake graphite powder and carboxy-butadiene butadiene latex to form an antistatic film layer in polyester staple fiber oil agent, the problem of insufficient antistatic properties of the existing oil agent is solved, and the long-term antistatic effect on the fiber surface and the stability of the film layer are achieved.

CN118345530BActive Publication Date: 2025-04-15TAICANG LONGFANG OIL CO LTD
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Patent Information

Application Number
CN202410659504.8
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-05-27
Publication Date
2025-04-15
Estimated Expiration
2044-05-27

AI Technical Summary

Technical Problem

The existing polyester staple fiber oil agent has insufficient antistatic properties, which leads to high resistance on the fiber surface, which easily leads to difficulties in non-woven fabrics forming and hydrospinning.

Method used

Modified scale graphite powder and carboxylic styrene butadiene latex are used as conductive components to form an antistatic film layer through double bond addition reaction, reducing the resistance of the fiber surface, and firmly adhering the film layer to the fiber surface through hydrogen bonding.

Benefits of technology

The long-term antistatic film layer is formed on the surface of polyester staple fibers, which significantly reduces the resistance of the fiber surface and improves the antistatic property and the integrity of the film layer.

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Abstract

The invention discloses a polyester staple fiber oil agent and a preparation method thereof. The invention first performs surface modification treatment on flake graphite powder, introduces amino groups and double bonds on the surface of the flake graphite powder, then, under the action of an initiator, potassium persulfate, performs double bond addition reaction on the 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 polyester staple fiber is treated with the oil agent to form an antistatic film layer on the surface of the polyester staple fiber, wherein the antistatic film layer contains flake graphite powder and carboxyl styrene butadiene structure, both of which 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.
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Description

Technical Field

[0001] The invention relates to the technical field of oil preparation, and in particular to a polyester staple fiber oil and a preparation method thereof. Background Art

[0002] Polyester staple fiber oil is a surfactant specially prepared for polyester staple fibers. It is mainly composed of fatty acid esters, polyols, polymers, etc. It has excellent lubricity, antistatic properties, softness and durability. This oil plays a very important role in spinning, stretching, spinning, weaving and other processing procedures. It can improve the smoothness of the fiber, maintain the appropriate friction coefficient between fibers and between fibers and other contact parts, and reduce the static electricity generated during fiber production and processing and make it disappear quickly.

[0003] Polyester staple fiber oil not only has an antistatic effect on polyester staple fiber production, but also has an important antistatic effect on textile processing. In textile processing, polyester staple fibers go through processes such as cleaning, carding, and drawing. When passing through various textile machines, the friction static electricity between fibers and fibers, and between fibers and equipment has a great impact on textile processing. The staple fiber oil agent gives the staple fibers different friction characteristics and bundling properties according to different processes, so that the spinning and weaving of polyester staple fibers can proceed smoothly.

[0004] 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 have uniform color, soft and smooth feel, good antistatic property, clustering property and smoothness, and is suitable for the production of various polyester staple fibers.

[0005] In recent years, the research on polyester staple fiber oils has also made significant progress, including the development of new polyester staple fiber oils, the synthesis and application of high-carbon alkyl phosphate potassium salts (PK), the development of alkylamine polyoxyethylene ether (APEO) substitutes, the optimization and screening of oil formulations, and the research and practice of green production. In recent years, the oils developed and manufactured have poor antistatic properties, high fiber specific resistivity, and are prone to difficulties in non-woven web formation and spunlace due to the types and ratios of the selected compositions.

[0006] 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 salts, 20 to 40 parts of fatty alcohol phosphate polyoxyethylene ethers, 10 to 30 parts of fatty acid polyoxyethylene esters, and 10 to 30 parts of fatty amine polyoxyethylene polyoxypropylene ethers. Although the antistatic properties of the prepared polyester staple fiber oil agent are improved, further improvement is still needed. Summary of the invention

[0007] In view of the deficiencies in the prior art, the object 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.

[0008] In order to achieve the above object, the present invention adopts the following technical scheme:

[0009] A polyester staple fiber oil agent 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 parts of a defoaming agent.

[0010] Specifically, the preparation method of the antistatic liquid is as follows:

[0011] S1. Ultrasonic dispersion of flake graphite powder in ethanol aqueous solution, then adding dimethyl (dimethylamino) vinyl silane thereto, stirring at 40-60° C. for 1-3 h, followed by filtering, washing and drying to obtain modified flake graphite powder;

[0012] S2. Add modified flake graphite powder, sodium dodecyl sulfate and tert-dodecyl mercaptan into 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 2-3h, and after the reaction is completed, an antistatic liquid is obtained.

[0013] 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 it is not limited to the listed values, and other unlisted values ​​within the numerical range are also applicable.

[0014] 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 unlisted values ​​within the numerical range are also applicable.

[0015] 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 the present application is potassium persulfate, and other commonly used initiators in the art are also applicable.

[0016] Specifically, the lubricant 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 lubricant 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.

[0017] Specifically, the sizing agent is selected from at least one of polyoxyethylene laurate, glycerol random polyether, and N-acyl amino acid salt.

[0018] 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.

[0019] 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.

[0020] 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 generation of sediment in the oil bath and reduce the frequency of cleaning the oil bath.

[0021] The present invention also provides a method for preparing the 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 reaction kettle, 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.

[0022] Compared with the prior art, the present invention has the following beneficial effects:

[0023] (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 dopes the flake graphite powder in the molecular chain of carboxylated styrene butadiene latex through chemical action, introduces it into oil agent as a conductive component, and uses the oil agent to treat polyester staple fibers, thereby forming an antistatic film layer on the surface of the polyester staple fibers, wherein the antistatic film layer contains flake graphite powder and carboxylated styrene butadiene structure, and both flake graphite powder and carboxylated styrene butadiene structure 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 fibers have good antistatic effect.

[0024] (2) The flake graphite powder in the antistatic film layer has a layered structure. Due to the weak interlayer van der Waals force of the layered structure, 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 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 lasting antistatic effect of the polyester staple fiber. DETAILED DESCRIPTION

[0025] The present invention is further described in detail below through specific preferred embodiments, but the present invention is not limited to the following embodiments.

[0026] It should be noted that, unless otherwise specified, the chemical reagents involved in the present invention were purchased through commercial channels.

[0027] The mesh size of the flake graphite powder used in the present invention is 400 mesh.

[0028] Example 1

[0029] A method for preparing a polyester staple fiber oil agent comprises the following steps:

[0030] 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 into a reactor, stirred at 200 r / min for 40 min at 50°C, then 40 parts of smoothing agent glycerol monooleate were added, stirred at 600 r / min for 30 min, then 0.5 parts of defoaming agent tributyl phosphate were added, stirred at 120 r / min for 30 min, and cooled to room temperature to obtain polyester staple fiber oil;

[0031] Wherein, the preparation method of the antistatic liquid is as follows:

[0032] S1. Ultrasonic dispersion of 10 g of flake graphite powder in 100 mL of 75 wt% ethanol aqueous solution, and then adding 1 g of dimethyl (dimethylamino) vinyl silane thereto, stirring at 40 ° C for 2 h, followed by filtering, washing, and drying to obtain modified flake graphite powder;

[0033] 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.

[0034] Example 2

[0035] A method for preparing a polyester staple fiber oil agent comprises the following steps:

[0036] 15 parts of emulsifier sodium N-methylamide carboxylate, 1 part of sizing agent propylene glycol 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 propylene glycol monostearate were added, stirred at 600 r / min for 30 min, and then 0.8 parts of defoaming agent polydimethylsiloxane were added, stirred at 150 r / min for 15 min, and cooled to room temperature to obtain a polyester staple fiber oil agent;

[0037] Wherein, the preparation method of the antistatic liquid is as follows:

[0038] S1. 8 g of flake graphite powder was ultrasonically dispersed in 100 mL of 75 wt% ethanol aqueous solution, and then 1 g of dimethyl (dimethylamino) vinyl silane was added thereto, and the mixture was stirred at 60 ° C for 1 h, and then filtered, washed, and dried to obtain modified flake graphite powder;

[0039] 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.

[0040] Example 3

[0041] A method for preparing a polyester staple fiber oil agent comprises the following steps:

[0042] 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 are added into a reactor, stirred at 200 r / min for 30 min at 60°C, then 50 parts of smoothing agent glycerol monostearate are added, stirred at 800 r / min for 30 min, and then 1 part of defoaming agent polydimethylsiloxane is added, stirred at 100 r / min for 30 min, and cooled to room temperature to obtain a polyester staple fiber oil agent;

[0043] Wherein, the preparation method of the antistatic liquid is as follows:

[0044] S1. Ultrasonic dispersion of 12 g of flake graphite powder in 100 mL of 75 wt% ethanol aqueous solution, and then adding 3 g of dimethyl (dimethylamino) vinyl silane thereto, stirring at 40 ° C for 3 h, followed by filtering, washing and drying to obtain modified flake graphite powder;

[0045] 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.

[0046] Example 4

[0047] A method for preparing a polyester staple fiber oil agent comprises the following steps:

[0048] 12 parts of emulsifier sodium N-methylamide carboxylate, 2 parts of sizing agent propylene glycol 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 min at 60°C, then 45 parts of smoothing agent propylene glycol monostearate were added, stirred at 800 r / min for 30 min, and then 0.5 parts of defoaming agent polydimethylsiloxane were added, stirred at 100 r / min for 30 min, and cooled to room temperature to obtain a polyester staple fiber oil agent;

[0049] Wherein, the preparation method of the antistatic liquid is as follows:

[0050] S1. Ultrasonic dispersion of 10 g of flake graphite powder in 100 mL of 75 wt% ethanol aqueous solution, and then adding 3 g of dimethyl (dimethylamino) vinyl silane thereto, stirring at 40 ° C for 3 h, followed by filtering, washing and drying to obtain modified flake graphite powder;

[0051] 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.

[0052] Comparative Example 1

[0053] A method for preparing a polyester staple fiber oil agent comprises the following steps:

[0054] 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 into a reactor, stirred at 200 r / min for 40 min at 50°C, then 40 parts of smoothing agent glycerol monooleate were added, stirred at 600 r / min for 30 min, then 0.5 parts of defoaming agent tributyl phosphate were added, stirred at 120 r / min for 30 min, and cooled to room temperature to obtain polyester staple fiber oil;

[0055] Wherein, the preparation method of the antistatic liquid is as follows:

[0056] 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.

[0057] Compared with Example 1, no flake graphite powder is added to the antistatic liquid in this comparative example.

[0058] Comparative Example 2

[0059] A method for preparing a polyester staple fiber oil agent comprises the following steps:

[0060] 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 into a reactor, stirred at 200 r / min for 40 min at 50°C, then 40 parts of smoothing agent glycerol monooleate were added, stirred at 600 r / min for 30 min, then 0.5 parts of defoaming agent tributyl phosphate were added, stirred at 120 r / min for 30 min, and cooled to room temperature to obtain polyester staple fiber oil;

[0061] Wherein, the preparation method of the antistatic liquid is as follows:

[0062] Add 4g of 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.

[0063] Compared with Example 1, the flake graphite powder in this comparative example is not modified.

[0064] The oil-free polyester staple fibers were immersed in the oil prepared in Examples 1-4 and Comparative Examples 1-2 for 5 minutes, spun dry, and dried in an oven at 100° C. for 6 hours to prepare test fiber samples, which were tested as follows:

[0065] Friction coefficient measurement: measured 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:

[0066] Table 1

[0067]

[0068] Antistatic test: The prepared fiber sample to be tested is woven in plain weave to obtain fabric, and the test is conducted with reference to GB / T 12703.5-2010 Evaluation of electrostatic properties of textiles Part 5: Triboelectric charging voltage;

[0069] Retention rate of antistatic property after washing 10 times: the prepared fabric was cut into square specimens with a length and width of 10 cm from the fabric according to GB / T 12490 standard, the water temperature was 40°C, detergent (AATCC1993 standard detergent WOB) was added, the washing time was 2 hours, and after drying, the antistatic property retention rate was tested after the washing and drying process was cycled 10 times; the test results are shown in Table 2:

[0070] Table 2

[0071]

[0072] Finally, it should be noted that the above embodiments do not limit the present invention in any form. For those skilled in the art, some modifications and improvements can be made to the present invention. Therefore, any modification or improvement made without departing from the spirit of the present invention belongs to the scope of protection claimed in the present invention.

Claims

1. A 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 parts of defoaming agent; Wherein, the preparation method of the antistatic liquid is as follows: S1. Ultrasonic dispersion of flake graphite powder in ethanol aqueous solution, then adding dimethyl (dimethylamino) vinyl silane thereto, stirring at 40-60° C. for 1-3 h, 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 into 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 2-3h, and after the reaction is completed, an antistatic liquid is obtained.

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

3. The polyester staple fiber oil according to claim 1, characterized in that: 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.

4. The polyester staple fiber oil according to claim 1, characterized in that: The lubricant is selected from at least one of glycerol monooleate, glycerol monostearate, glycerol monopalmitate, lauryl oleate, isooctyl stearate, and trihydroxypropane isooctyl alcohol ester.

5. The polyester staple fiber oil according to claim 1, characterized in that: The sizing agent is selected from at least one of polyoxyethylene laurate, glycerol random polyether, and N-acyl amino acid salt.

6. The polyester staple fiber oil according to claim 1, characterized in that: The emulsifier is selected from at least one of stearate, N-methylamide carboxylate, and sorbitan fatty acid ester polyoxyethylene ether.

7. The polyester staple fiber oil according to claim 1, characterized in that: The antioxidant is selected from at least one of antioxidant 1076 and antioxidant 1035.

8. The polyester staple fiber oil according to claim 1, characterized in that: The defoaming agent is selected from at least one of tributyl phosphate and polydimethylsiloxane.

9. The method for preparing the polyester staple fiber oil agent according to any one of claims 1 to 8, 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, then adding a smoothing agent, stirring at 600-800 r / min for 30-60 min, then adding a defoaming agent, stirring at 100-150 r / min for 15-30 min, cooling to room temperature, and obtaining a polyester staple fiber oil agent.

Citation Information

Patent Citations

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  • Polyester FDY oiling agent and preparation method thereof

    CN117721555A