A process for the antistatic treatment of resin-based polyester fibres
By in-situ polymerization of modified quercetin with zein and aniline monomers, combined with low-temperature plasma treatment and multi-stage thermal stretching, a stable "ion-electron-hydrophilic" triple conductive network was constructed, which solved the problem of unstable antistatic properties of polyester fibers and improved the mechanical properties and durability of the fibers.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- ZHEJIANG HAILI ENVIRONMENTAL TECH CO LTD
- Filing Date
- 2025-10-16
- Publication Date
- 2026-05-12
AI Technical Summary
Existing antistatic technologies for polyester fibers suffer from poor compatibility and durability, unstable performance, and decreased mechanical properties. In particular, it is difficult to achieve effective all-round static dissipation under different humidity environments.
In-situ polymerization of modified quercetin with zein and aniline monomers was employed, combined with low-temperature plasma treatment and multi-stage dynamic thermal stretching, to form a zein/polyaniline core-shell conductive structure. A triple synergistic conductive network of "ions-electrons-hydrophiles" was constructed through bacterial cellulose nanolayers.
It achieves stable antistatic properties under different humidity environments, improves the mechanical properties of the fiber as well as its washability and abrasion resistance, and conforms to the trend of green and sustainable development.
Smart Images
Figure CN121046980B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the field of polymer materials and fiber manufacturing technology, and particularly relates to an antistatic treatment process for resin-based polyester fibers. Background Technology
[0002] Polyester fibers (such as PET and PBT) are widely used in textiles, electronics, medical and protective products due to their excellent mechanical properties, chemical resistance and cost advantages. However, the inherent high insulation and hydrophobicity of polyester fibers make them prone to generating and accumulating static charges, leading to fabrics easily attracting dust, discomfort when worn, safety accidents in flammable and explosive environments, and damage to precision components in the electronics industry.
[0003] Existing antistatic technologies are mainly divided into two categories: one is the internal blending method, which involves blending the antistatic agent with polyester chips before melt spinning; the other is the surface treatment method, such as spraying and impregnation coating. Commonly used antistatic agents in the internal blending method include small-molecule quaternary ammonium salts, esters, ethers, or conductive fillers such as carbon nanotubes and graphene. However, these methods have the following limitations in certain application scenarios:
[0004] Poor compatibility and durability: Most small molecule antistatic agents have poor compatibility with polyester matrix and are prone to migration and precipitation during processing and use (i.e., "blooming"), which leads to rapid decay of antistatic performance.
[0005] Limited performance: Single-type antistatic agents (pure ionic or pure electronic) often have unstable performance under different humidity conditions, making it difficult to achieve comprehensive and effective static dissipation.
[0006] Impact on mechanical properties: If conductive fillers (such as CNTs) are not dispersed evenly or are added in excessive amounts, they will act as stress concentration points, severely degrading the strength, elongation and spinnability of the fiber. Summary of the Invention
[0007] This invention provides an antistatic treatment process for resin-based polyester fibers, aiming to solve the above-mentioned problems.
[0008] This invention is achieved through an antistatic treatment process for resin-based polyester fibers, comprising the following steps:
[0009] S1 involves blending dried polyester chips (viscosity 0.60-0.68 dl / g) with modified quercetin (mass ratio 100:1-5) and then performing melt spinning (screw temperature set at 260-275℃, chamber temperature not exceeding 280℃, spinning speed 1200-1800m / min).
[0010] S2 passes the melt stream through a first treatment liquid containing zein and aniline monomer, and then through a second treatment liquid containing an oxidant to carry out an in-situ polymerization reaction to obtain nascent fibers;
[0011] S3 performs low-temperature plasma treatment on nascent fibers;
[0012] S4 performs multi-stage dynamic thermal stretching and heat setting on the fibers.
[0013] Preferably, the preparation method of the modified quercetin includes the following steps:
[0014] By weight, 1 part quercetin is dispersed in 20-50 parts anhydrous N,N-dimethylformamide (DMF), and 0.5-1.5 parts anhydrous potassium carbonate is added as a catalyst. The mixture is then stirred and activated at 60-80°C under nitrogen protection for 0.5-1 hours.
[0015] Slowly add 1-3 parts of 3-chloro-1,2-propanediol, heat to 90-110℃ and react for 6-12 hours to obtain the intermediate;
[0016] After the reaction is complete, cool, precipitate, wash, and dry.
[0017] One part of the obtained epoxy-modified quercetin intermediate was redissolved in 15-30 parts of DMF, and 2-5 parts of 1-carboxyethyl-3-methylimidazolium tetrafluoroborate ionic liquid and 0.1-0.3 parts of tetrabutylammonium bromide catalyst were added. The reaction was carried out at 100-120℃ for 8-16 hours.
[0018] The reaction solution was precipitated, washed, and vacuum dried to obtain modified quercetin.
[0019] Preferably, the first treatment solution comprises the following raw materials in parts by weight: 1-5 parts of zein, 0.5-3 parts of aniline monomer, and a solvent consisting of 70-90 parts of a 70%-90% volume-concentration aqueous solution of ethanol and 0.5-2 parts of glacial acetic acid; the residence time of the fiber in the first treatment solution is 2-6 seconds.
[0020] Preferably, the preparation method of the first treatment solution includes the following steps:
[0021] Dissolve zein in the mixed solvent and stir until completely dissolved;
[0022] Add aniline monomer and stir continuously for 0.5-2 hours to obtain the first treatment solution.
[0023] Preferably, the second treatment solution is a 0.1-0.5 mol / L ammonium persulfate aqueous solution, and the residence time of the fiber in the second treatment solution is 2-4 seconds.
[0024] Zein self-assembles on the fiber surface under phase transition and acts as a template to guide aniline monomers to undergo in-situ oxidative polymerization with ammonium persulfate, forming a zein / polyaniline core-shell conductive structure on the fiber surface.
[0025] Preferably, the plasma treatment uses a low-temperature plasma treatment device, and the treatment atmosphere is a mixture of ammonia and argon, wherein the volume percentage of ammonia is 10%-40%. The treatment power is 300-800W, the treatment time is 30-120 seconds, and the chamber pressure is 20-100Pa.
[0026] Plasma treatment introduces nitrogen-containing active groups and generates active free radicals on the fiber surface, inducing the formation of a covalent cross-linking network between the epoxy / hydroxyl groups in the modified quercetin and the polyester molecular chains, zein molecules, and polyaniline.
[0027] Preferably, the multi-stage dynamic thermal stretching and heat setting specifically refers to:
[0028] The first stage of stretching is carried out in a hot water bath or on hot rollers at 85-95℃, with a stretching ratio of 2.0-3.5 times.
[0029] The second stage of stretching is carried out in a heat-setting chamber at 105-120℃, with a stretching ratio of 1.2-1.8 times. The stretching speed fluctuates periodically at a frequency of 1-5Hz and an amplitude of 10%-30%. The total stretching ratio is controlled between 3.5-5.5 times.
[0030] Finally, perform relaxation heat setting at 125-135℃ for 1-5 seconds.
[0031] Preferably, the plasma-treated fibers are guided through or immersed in a bioreactor containing fermentation medium and Acetobacter xylinum (inoculum size 1%-5% v / v). Subsequently, they are statically cultured at 28-30°C for 24-72 hours. After fermentation, the fibers are washed sequentially with a mild alkaline aqueous solution (e.g., 0.1M NaOH, used to terminate the reaction and remove bacterial cells) and deionized water, and then dried at 60-80°C.
[0032] Fermentation medium formula (parts by weight): 20-50 parts glucose, 5-10 parts peptone, 5-10 parts yeast extract, 1-3 parts disodium hydrogen phosphate, 0.5-1.5 parts citric acid, with the remainder being water, and adjust the pH to 5.0-6.0.
[0033] Acetobacter xylinum uses the fiber surface as a growth template to synthesize and deposit bacterial cellulose nanofibers, forming a dense BC nano-reinforcement layer.
[0034] The hydrophilic channels provided by BC, combined with the internal modified quercetin and the surface zein / polyaniline, construct a triple synergistic conductive network of "ions-electrons-hydrophiles". This enables the fiber to maintain stable antistatic properties under different humidity environments, with BC particularly ensuring basic antistatic capabilities under low humidity conditions.
[0035] The three-dimensional nanonetwork of BC acts as a reinforcement, bonding with the polyester matrix through physical entanglement and hydrogen bonding, significantly improving the modulus and strength of the composite fiber. Its nanoscale effect avoids stress concentration, toughening the fiber without causing embrittlement.
[0036] Plasma pretreatment provides an active substrate for BC synthesis. BC combines with the fiber surface in a "symbiotic" manner through biosynthesis, further improving the water resistance and abrasion resistance of the entire functional layer.
[0037] When stretched at high temperatures, the in-situ generated BC network constrains and guides the movement of polyester molecular chains, causing the polyester chains to arrange and crystallize more orderly in the gaps between BC nanofibers, thereby further improving mechanical properties.
[0038] Compared with the prior art, the embodiments of this application have the following main advantages:
[0039] The antistatic treatment process for resin-based polyester fibers provided by this invention utilizes internally modified quercetin to provide ionic conductivity, surface zein / polyaniline to provide electronic conductivity, and in-situ synthesized bacterial cellulose nanolayers to provide hydrophilic channels and ion adsorption sites. These three components are cross-linked by plasma to form a stable "electron-ion-hydrophilic" triple conductive network, resulting in a comprehensive, efficient, and long-lasting antistatic effect.
[0040] By using plasma-induced covalent crosslinking, modified quercetin and zein / polyaniline conductive networks are "welded" to the fiber surface and near-surface region, improving the washability and abrasion resistance of the antistatic layer.
[0041] The functional components quercetin, zein, and bacterial cellulose are all derived from biomass, which aligns with the trend of green and sustainable development. Attached Figure Description
[0042] Figure 1 This is a flowchart of an antistatic treatment process for resin-based polyester fibers provided by the present invention.
[0043] Figure 2 This is a flowchart of the preparation method of modified quercetin provided by the present invention;
[0044] Figure 3 This is a flowchart of the preparation method of the first treatment liquid provided by the present invention. Detailed Implementation
[0045] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs; the terminology used herein in the specification of the application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application; the terms "comprising" and "having," and any variations thereof, in the specification, claims, and foregoing drawings of this application are intended to cover non-exclusive inclusion. The terms "first," "second," etc., in the specification, claims, or foregoing drawings of this application are used to distinguish different objects, not to describe a particular order.
[0046] In this document, the term "embodiment" means that a particular feature, structure, or characteristic described in connection with an embodiment may be included in at least one embodiment of this application. The appearance of this phrase in various places throughout the specification does not necessarily refer to the same embodiment, nor is it a separate or alternative embodiment mutually exclusive with other embodiments. It will be explicitly and implicitly understood by those skilled in the art that the embodiments described herein can be combined with other embodiments.
[0047] Example 1
[0048] This invention provides an antistatic treatment process for resin-based polyester fibers, such as... Figures 1-3 As shown, it includes the following steps:
[0049] S1 involves blending dried polyester chips (viscosity 0.65 dl / g) with modified quercetin (mass ratio 100:1) and then melt spinning them.
[0050] The preparation method of the modified quercetin includes the following steps:
[0051] By weight, 1 part of quercetin was dispersed in 20 parts of anhydrous N,N-dimethylformamide (DMF), and 0.5 parts of anhydrous potassium carbonate was added as a catalyst. The mixture was then activated by stirring at 60°C under nitrogen protection for 0.5 hours.
[0052] One part of 3-chloro-1,2-propanediol was slowly added dropwise, and the mixture was heated to 90°C and reacted for 6 hours to obtain the intermediate.
[0053] After the reaction is complete, cool, precipitate, wash, and dry.
[0054] One part of the obtained epoxy-modified quercetin intermediate was redissolved in 15 parts of DMF, and two parts of 1-carboxyethyl-3-methylimidazolium tetrafluoroborate ionic liquid and 0.1 parts of tetrabutylammonium bromide catalyst were added. The mixture was reacted at 100°C for 8 hours.
[0055] The reaction solution was precipitated, washed, and vacuum dried to obtain modified quercetin.
[0056] S2 passes the melt stream through a first treatment liquid containing zein and aniline monomer. The fiber stays in the first treatment liquid for 2 seconds and is then immediately guided through a second treatment liquid to obtain nascent fiber.
[0057] The preparation method of the first treatment solution includes the following steps:
[0058] Dissolve 1 part of zein in a mixed solvent of 70 parts of 80% (v / v) aqueous ethanol and 0.5 parts of glacial acetic acid, and stir until completely dissolved;
[0059] Add 0.5 parts of aniline monomer and stir continuously for 0.5 hours to obtain the first treatment solution.
[0060] The second treatment solution is a 0.1 mol / L ammonium persulfate aqueous solution, and the fiber residence time in the second treatment solution is 2 seconds.
[0061] S3 performs low-temperature plasma treatment on nascent fibers;
[0062] The plasma treatment employs a low-temperature plasma treatment device, with a treatment atmosphere consisting of a mixture of ammonia and argon, wherein ammonia accounts for 10% of the volume. The treatment power is 300W, the treatment time is 30 seconds, and the chamber pressure is 20Pa.
[0063] S4 performs multi-stage dynamic thermal stretching and heat setting on the fibers.
[0064] The first stage of stretching is carried out in a hot water bath or on a hot roller at 85°C, with a stretching ratio of 3.0 times.
[0065] The second stage of stretching was carried out in a heat-setting chamber at 105℃, with a stretching ratio of 1.5 times and a stretching speed that fluctuated periodically at a frequency of 1Hz and an amplitude of 10%. The total stretching ratio was controlled at 4.5 times.
[0066] Finally, perform relaxation heat setting at 125℃ for 1 second.
[0067] Example 2
[0068] This invention provides an antistatic treatment process for resin-based polyester fibers, such as... Figures 1-3 As shown, it includes the following steps:
[0069] S1 involves blending dried polyester chips (viscosity 0.65 dl / g) with modified quercetin (mass ratio 100:2) and then melt spinning them.
[0070] The preparation method of the modified quercetin includes the following steps:
[0071] By weight, 1 part of quercetin was dispersed in 30 parts of anhydrous N,N-dimethylformamide (DMF), and 0.8 parts of anhydrous potassium carbonate was added as a catalyst. The mixture was then activated by stirring at 65°C under nitrogen protection for 0.6 hours.
[0072] 1.5 parts of 3-chloro-1,2-propanediol were slowly added dropwise, and the mixture was heated to 95°C and reacted for 7 hours to obtain the intermediate.
[0073] After the reaction is complete, cool, precipitate, wash, and dry.
[0074] One part of the obtained epoxy-modified quercetin intermediate was redissolved in 18 parts of DMF, and three parts of 1-carboxyethyl-3-methylimidazolium tetrafluoroborate ionic liquid and 0.15 parts of tetrabutylammonium bromide catalyst were added. The mixture was reacted at 105°C for 10 hours.
[0075] The reaction solution was precipitated, washed, and vacuum dried to obtain modified quercetin.
[0076] S2 passes the melt stream through a first treatment liquid containing zein and aniline monomer. The fiber stays in the first treatment liquid for 3 seconds and is then immediately guided through a second treatment liquid to obtain nascent fiber.
[0077] The preparation method of the first treatment solution includes the following steps:
[0078] Dissolve 2 parts of zein in a mixed solvent of 75 parts of 80% (v / v) aqueous ethanol and 1 part of glacial acetic acid, and stir until completely dissolved.
[0079] Add 1.5 parts of aniline monomer and stir continuously for 1 hour to obtain the first treatment solution.
[0080] The second treatment solution is a 0.2 mol / L ammonium persulfate aqueous solution, and the fiber residence time in the second treatment solution is 2 seconds.
[0081] S3 performs low-temperature plasma treatment on nascent fibers;
[0082] The plasma treatment employs a low-temperature plasma treatment device, with a treatment atmosphere consisting of a mixture of ammonia and argon, wherein ammonia accounts for 20% of the volume. The treatment power is 400W, the treatment time is 50 seconds, and the chamber pressure is 40Pa.
[0083] S4 performs multi-stage dynamic thermal stretching and heat setting on the fibers.
[0084] The first stage of stretching is carried out in a hot water bath or on a hot roller at 85°C, with a stretching ratio of 3.0 times.
[0085] The second stage of stretching was carried out in a heat-setting chamber at 105°C, with a stretching ratio of 1.5 times and a stretching speed that fluctuated periodically at a frequency of 1 Hz and an amplitude of 15%. The total stretching ratio was controlled at 4.5 times.
[0086] Finally, perform relaxation heat setting at 125℃ for 2 seconds.
[0087] Example 3
[0088] This invention provides an antistatic treatment process for resin-based polyester fibers, such as... Figures 1-3 As shown, it includes the following steps:
[0089] S1 involves blending dried polyester chips (viscosity 0.65 dl / g) with modified quercetin (mass ratio 100:3) and then melt spinning them.
[0090] The preparation method of the modified quercetin includes the following steps:
[0091] By weight, 1 part of quercetin was dispersed in 35 parts of anhydrous N,N-dimethylformamide (DMF), and 1 part of anhydrous potassium carbonate was added as a catalyst. The mixture was then activated by stirring at 70°C under nitrogen protection for 0.75 hours.
[0092] Two parts of 3-chloro-1,2-propanediol were slowly added dropwise, and the mixture was heated to 100°C and reacted for 9 hours to obtain the intermediate.
[0093] After the reaction is complete, cool, precipitate, wash, and dry.
[0094] One part of the obtained epoxy-modified quercetin intermediate was redissolved in 22.5 parts of DMF, and 3.5 parts of 1-carboxyethyl-3-methylimidazolium tetrafluoroborate ionic liquid and 0.2 parts of tetrabutylammonium bromide catalyst were added. The reaction was carried out at 110°C for 12 hours.
[0095] The reaction solution was precipitated, washed, and vacuum dried to obtain modified quercetin.
[0096] S2 passes the melt stream through a first treatment liquid containing zein and aniline monomer. The fiber stays in the first treatment liquid for 4 seconds and is then immediately guided through a second treatment liquid to obtain nascent fiber.
[0097] The preparation method of the first treatment solution includes the following steps:
[0098] Dissolve 3 parts of zein in a mixed solvent of 80 parts of 80% (v / v) ethanol aqueous solution and 1.25 parts of glacial acetic acid, and stir until completely dissolved;
[0099] Add 1.75 parts of aniline monomer and stir continuously for 1.25 hours to obtain the first treatment solution.
[0100] The second treatment solution is a 0.3 mol / L ammonium persulfate aqueous solution, and the fiber residence time in the second treatment solution is 3 seconds.
[0101] S3 performs low-temperature plasma treatment on nascent fibers;
[0102] The plasma treatment employs a low-temperature plasma treatment device, with a treatment atmosphere consisting of a mixture of ammonia and argon, wherein ammonia accounts for 25% of the volume. The treatment power is 550W, the treatment time is 75 seconds, and the chamber pressure is 60Pa.
[0103] S4 performs multi-stage dynamic thermal stretching and heat setting on the fibers.
[0104] The first stage of stretching is carried out in a hot water bath or on a hot roller at 90°C, with a stretching ratio of 3.0 times.
[0105] The second stage of stretching was carried out in a heat-setting chamber at 115°C, with a stretching ratio of 1.5 times and a stretching speed that fluctuated periodically at a frequency of 3 Hz and an amplitude of 20%. The total stretching ratio was controlled at 4.5 times.
[0106] Finally, perform relaxation heat setting at 130℃ for 3 seconds.
[0107] Example 4
[0108] This invention provides an antistatic treatment process for resin-based polyester fibers, such as... Figures 1-3 As shown, it includes the following steps:
[0109] S1 involves blending dried polyester chips (viscosity 0.65 dl / g) with modified quercetin (mass ratio 100:4) and then melt spinning them.
[0110] The preparation method of the modified quercetin includes the following steps:
[0111] By weight, 1 part of quercetin was dispersed in 45 parts of anhydrous N,N-dimethylformamide (DMF), and 1.2 parts of anhydrous potassium carbonate was added as a catalyst. The mixture was then activated by stirring at 75°C under nitrogen protection for 0.8 hours.
[0112] 2.5 parts of 3-chloro-1,2-propanediol were slowly added dropwise, and the mixture was heated to 105°C and reacted for 10 hours to obtain the intermediate.
[0113] After the reaction is complete, cool, precipitate, wash, and dry.
[0114] One part of the obtained epoxy-modified quercetin intermediate was redissolved in 26 parts of DMF, and four parts of 1-carboxyethyl-3-methylimidazolium tetrafluoroborate ionic liquid and 0.25 parts of tetrabutylammonium bromide catalyst were added. The mixture was reacted at 115°C for 14 hours.
[0115] The reaction solution was precipitated, washed, and vacuum dried to obtain modified quercetin.
[0116] S2 passes the melt stream through a first treatment liquid containing zein and aniline monomer. The fiber stays in the first treatment liquid for 5 seconds and is then immediately guided through a second treatment liquid to obtain nascent fiber.
[0117] The preparation method of the first treatment solution includes the following steps:
[0118] Dissolve 4 parts of zein in a mixed solvent of 85 parts of 80% (v / v) ethanol aqueous solution and 1.5 parts of glacial acetic acid, and stir until completely dissolved;
[0119] Add 2.5 parts of aniline monomer and stir continuously for 1.5 hours to obtain the first treatment solution.
[0120] The second treatment solution is a 0.4 mol / L ammonium persulfate aqueous solution, and the fiber residence time in the second treatment solution is 4 seconds.
[0121] S3 performs low-temperature plasma treatment on nascent fibers;
[0122] The plasma treatment employs a low-temperature plasma treatment device, with a treatment atmosphere consisting of a mixture of ammonia and argon, wherein ammonia accounts for 30% of the volume. The treatment power is 700W, the treatment time is 100 seconds, and the chamber pressure is 80Pa.
[0123] S4 performs multi-stage dynamic thermal stretching and heat setting on the fibers.
[0124] The first stage of stretching is carried out in a hot water bath or on a hot roller at 95°C, with a stretching ratio of 3.0 times.
[0125] The second stage of stretching was carried out in a heat-setting chamber at 120°C, with a stretch ratio of 1.5 times and a stretching speed that fluctuated periodically at a frequency of 4 Hz and an amplitude of 25%. The total stretch ratio was controlled at 4.5 times.
[0126] Finally, perform relaxation heat setting at 135℃ for 4 seconds.
[0127] Example 5
[0128] This invention provides an antistatic treatment process for resin-based polyester fibers, such as... Figures 1-3 As shown, it includes the following steps:
[0129] S1 involves blending dried polyester chips (viscosity 0.65 dl / g) with modified quercetin (mass ratio 100:5) and then melt spinning them.
[0130] The preparation method of the modified quercetin includes the following steps:
[0131] By weight, 1 part of quercetin was dispersed in 50 parts of anhydrous N,N-dimethylformamide (DMF), and 1.5 parts of anhydrous potassium carbonate was added as a catalyst. The mixture was then activated by stirring at 80°C for 1 hour under nitrogen protection.
[0132] Three parts of 3-chloro-1,2-propanediol were slowly added dropwise, and the mixture was heated to 110°C and reacted for 12 hours to obtain the intermediate.
[0133] After the reaction is complete, cool, precipitate, wash, and dry.
[0134] One part of the obtained epoxy-modified quercetin intermediate was redissolved in 30 parts of DMF, and 5 parts of 1-carboxyethyl-3-methylimidazolium tetrafluoroborate ionic liquid and 0.3 parts of tetrabutylammonium bromide catalyst were added. The mixture was reacted at 120°C for 16 hours.
[0135] The reaction solution was precipitated, washed, and vacuum dried to obtain modified quercetin.
[0136] S2 passes the melt stream through a first treatment liquid containing zein and aniline monomer. The fiber stays in the first treatment liquid for 6 seconds and is then immediately guided through a second treatment liquid to obtain nascent fiber.
[0137] The preparation method of the first treatment solution includes the following steps:
[0138] Dissolve 5 parts of zein in a mixed solvent of 90 parts of 80% ethanol aqueous solution and 2 parts of glacial acetic acid, and stir until completely dissolved.
[0139] Add 3 parts of aniline monomer and stir continuously for 2 hours to obtain the first treatment solution.
[0140] The second treatment solution is a 0.5 mol / L ammonium persulfate aqueous solution, and the fiber residence time in the second treatment solution is 4 seconds.
[0141] S3 performs low-temperature plasma treatment on nascent fibers;
[0142] The plasma treatment employs a low-temperature plasma treatment device, with a treatment atmosphere consisting of a mixture of ammonia and argon, wherein ammonia accounts for 40% of the volume. The treatment power is 800W, the treatment time is 120 seconds, and the chamber pressure is 100Pa.
[0143] S4 performs multi-stage dynamic thermal stretching and heat setting on the fibers.
[0144] The first stage of stretching is carried out in a hot water bath or on a hot roller at 95°C, with a stretching ratio of 3.0 times.
[0145] The second stage of stretching was carried out in a heat-setting chamber at 120℃, with a stretching ratio of 1.5 times and a stretching speed that fluctuated periodically at a frequency of 5Hz and an amplitude of 30%. The total stretching ratio was controlled at 4.5 times.
[0146] Finally, perform relaxation heat setting at 135℃ for 5 seconds.
[0147] Example 6
[0148] The difference between this embodiment and embodiment 3 is that:
[0149] The plasma-treated fibers are guided through or immersed in a bioreactor containing fermentation medium and Acetobacter xylinum (inoculum 3% v / v).
[0150] Subsequently, it was statically cultured at 29°C for 48 hours.
[0151] After fermentation, the fiber is washed sequentially with a mild alkaline aqueous solution (such as 0.1M NaOH, used to terminate the reaction and remove the cells) and deionized water, and then dried at 70°C.
[0152] Finally, multi-stage dynamic thermal stretching and heat setting are performed.
[0153] The fermentation medium formula (parts by weight) is as follows: 35 parts glucose, 7.5 parts peptone, 7.5 parts yeast extract, 2 parts disodium hydrogen phosphate, 1 part citric acid, and the remainder is water, adjusted to pH 5.0-6.0.
[0154] Blank control group: Pure polyester chips (100 parts by weight) were used without adding any antistatic agents or performing any surface treatment, and only conventional melt spinning and hot stretching were performed.
[0155] Comparative Example 1: Pure polyester chips (100 parts by weight) were blended with 1.5 parts by weight of commercially available quaternary ammonium salt antistatic agents (such as stearoyl lactate quaternary ammonium salt) and subjected to conventional melt spinning and hot stretching.
[0156] Comparative Example 2: The difference from Example 3 is that the first treatment solution does not contain zein.
[0157] Comparative Example 3: The difference from Example 3 is that no plasma treatment was performed.
[0158] Comparative Example 4: The difference from Example 3 is that the modified quercetin was replaced with an equal amount of ordinary quercetin.
[0159] Performance tests were conducted on the fibers from Examples 1-6, the blank control group, and Comparative Examples 1-4.
[0160] Test methods and standards
[0161] Surface resistivity: GB / T 12703.4-2010, standard environment (20±2℃, RH 35±5%).
[0162] Washability: The resistivity was tested after 50 equivalent washes using the AATCC 61-2020 rapid method.
[0163] Mechanical properties: GB / T 14344-2008, measurement of breaking strength and elongation.
[0164] Water contact angle: seat drop method, to assess hydrophilicity.
[0165] The test results are shown in Table 1 below:
[0166]
[0167] The results above show that the fiber prepared by this invention has good durable antistatic properties and high mechanical strength.
[0168] It should be noted that, for the sake of simplicity, the foregoing embodiments are all described as a series of actions. However, those skilled in the art should understand that the present invention is not limited to the described order of actions, as some steps may be performed in other orders or simultaneously according to the present invention. Furthermore, those skilled in the art should also understand that the embodiments described in the specification are preferred embodiments, and the actions and modules involved are not necessarily essential to the present invention.
[0169] It should be understood that the disclosed apparatus can be implemented in other ways, as illustrated in the embodiments provided in this application. For example, the apparatus embodiments described above are merely illustrative; the division of units described above is only a logical functional division, and in actual implementation, there may be other division methods. For example, multiple units or components may be combined or integrated into another system, or some features may be ignored or not executed. Furthermore, the coupling or communication connections shown or discussed may be through some interfaces; the indirect coupling or communication connections between devices or units may be telecommunications or other forms.
[0170] The units described above as separate components may or may not be physically separate. The components shown as units may or may not be physical units; that is, they may be located in one place or distributed across multiple network units. Some or all of the units can be selected to achieve the purpose of this embodiment according to actual needs.
[0171] The above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit the scope of protection of the invention. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on these embodiments, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art can still combine, add, delete, or otherwise adjust the features of the various embodiments of the present invention according to the circumstances without conflict or creative effort, thereby obtaining different technical solutions that do not fundamentally depart from the concept of the present invention. These technical solutions also fall within the scope of protection of the present invention.
Claims
1. An antistatic treatment process for resin-based polyester fibers, characterized in that, Includes the following steps: S1 involves blending dried polyester chips with modified quercetin and then performing melt spinning. The mass ratio of polyester chips to modified quercetin is 100:1-5. S2 passes the melt stream through a first treatment solution containing zein and aniline monomer, and then through a second treatment solution containing an oxidant to obtain nascent fibers; S3 performs low-temperature plasma treatment on nascent fibers; S4 performs multi-stage dynamic thermal stretching and thermal setting on the fibers; The preparation method of the modified quercetin is as follows: By weight, 1 part quercetin is dispersed in 20-50 parts anhydrous N,N-dimethylformamide (DMF), and 0.5-1.5 parts anhydrous potassium carbonate is added as a catalyst. The mixture is then stirred and activated at 60-80°C under nitrogen protection for 0.5-1 hours. Slowly add 1-3 parts of 3-chloro-1,2-propanediol, heat to 90-110℃ and react for 6-12 hours to obtain the intermediate; After the reaction is complete, cool, precipitate, wash, and dry. One part of the obtained epoxy-modified quercetin intermediate was redissolved in 15-30 parts of DMF, and 2-5 parts of 1-carboxyethyl-3-methylimidazolium tetrafluoroborate ionic liquid and 0.1-0.3 parts of tetrabutylammonium bromide catalyst were added. The reaction was carried out at 100-120℃ for 8-16 hours. The reaction solution was precipitated, washed, and vacuum dried to obtain modified quercetin.
2. The antistatic treatment process for resin-based polyester fibers as described in claim 1, characterized in that, The first treatment solution comprises the following raw materials in parts by weight: 1-5 parts of zein, 0.5-3 parts of aniline monomer, and a solvent consisting of 70-90 parts of a 70%-90% volume-concentration aqueous solution of ethanol and 0.5-2 parts of glacial acetic acid.
3. The antistatic treatment process for resin-based polyester fibers as described in claim 2, characterized in that, The preparation method of the first treatment solution includes the following steps: Dissolve zein in a mixed solvent consisting of a 70%-90% (v / v) aqueous ethanol solution and glacial acetic acid, and stir until completely dissolved; Add aniline monomer and stir continuously for 0.5-2 hours to obtain the first treatment solution.
4. The antistatic treatment process for resin-based polyester fibers as described in claim 1, characterized in that, The second treatment solution is a 0.1-0.5 mol / L ammonium persulfate aqueous solution.
5. The antistatic treatment process for resin-based polyester fibers as described in claim 1, characterized in that, The atmosphere for plasma treatment is a mixture of ammonia and argon with a volume ratio of 10%-40%; the treatment power is 300-800W, and the treatment time is 30-120 seconds.
6. The antistatic treatment process for resin-based polyester fibers as described in claim 1, characterized in that, The multi-stage dynamic thermal stretching and heat setting specifically refers to: The first stage of tensile testing was conducted at 85-95℃, with a tensile ratio of 2.0-3.5 times. The second stage of stretching is carried out at 105-120℃, with a stretching ratio of 1.2-1.8 times. During the second stage of stretching, the stretching speed fluctuates periodically at a frequency of 1-5Hz and an amplitude of 10%-30%. The total stretching ratio is 3.5-5.5 times.
7. The antistatic treatment process for resin-based polyester fibers as described in claim 1, characterized in that, The fibers after step S3 were immersed in Acetobacter xylinum fermentation medium and statically cultured at 28-30°C for 24-72 hours; after fermentation, the fibers were washed and dried.
8. The antistatic treatment process for resin-based polyester fibers as described in claim 7, characterized in that, The fermentation medium comprises the following raw materials in parts by weight: 20-50 parts glucose, 5-10 parts peptone, 5-10 parts yeast extract, 1-3 parts disodium hydrogen phosphate, 0.5-1.5 parts citric acid, and the balance being water.