Process for the preparation of modified polyester fibers based on graphene

Modified polyester fibers were prepared by melt blending graphene-molybdenum disulfide composite with PET material, which solved the problems of insufficient mechanical properties and flame retardancy of traditional polyester fibers, and achieved high thermal stability and good combustion inhibition effect.

CN118639347BActive Publication Date: 2025-11-25LANDRED CO LTD
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Patent Information

Application Number
CN202410960139.4
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-07-17
Publication Date
2025-11-25
Estimated Expiration
2044-07-17

AI Technical Summary

Technical Problem

Traditional polyester fibers have shortcomings in terms of mechanical properties and thermal stability, and are highly flammable, which can easily cause fires and produce toxic gases, thus affecting the environment.

Method used

Graphene composite molybdenum disulfide was melt-blended with PET material, and graphene composite powder was prepared by hydrothermal method. Then, it was grafted with aromatic Schiff base to form modified polyester fiber, which improved the compatibility and flame retardant properties of the material.

Benefits of technology

It improves the mechanical properties and thermal stability of polyester fibers, enhances flame retardancy, reduces the generation of toxic gases during combustion, and improves the toughness and compatibility of the material.

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Abstract

The application discloses a preparation process of modified polyester fiber based on graphene and relates to the technical field of graphene modification. The composite material of graphene and molybdenum disulfide is prepared by using a hydrothermal method, is subjected to carboxyl functionalization, is grafted with an aromatic Schiff base, and brings flame retardant performance. The composite material is subjected to melt blending with pure polyester fiber melt, is subjected to spinning extrusion, wetting and oiling, and winding and bundling, so that the graphene modified polyester fiber is prepared. The graphene modified polyester fiber prepared by the application has good mechanical properties and excellent flame retardant performance, is different from traditional polyester fiber materials, novel material graphene is introduced, performance is improved, and thus the application field is widened.
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Description

Technical Field

[0001] This invention relates to the field of graphene modification technology, specifically to a preparation process for graphene-based modified polyester fibers. Background Technology

[0002] Polyester fiber has a wide range of applications due to its excellent physical properties and chemical stability, making it widely used in textiles, clothing, home furnishings, and architectural decoration, and occupying an important position in the field of chemical fibers. However, traditional polyester fibers still have some shortcomings due to technological limitations, such as the need for improvement in mechanical properties and thermal stability. Furthermore, synthetic fibers themselves are highly flammable, containing a large number of oxygen atoms in their molecules, making them prone to oxidative decomposition reactions that generate a large amount of heat, potentially causing fires and producing large amounts of toxic gases, thus polluting the environment. This is a point that deserves serious attention.

[0003] Graphene is a two-dimensional carbon nanomaterial with excellent properties such as high strength and high thermal conductivity. When combined with polymers, it can endow polymers with excellent mechanical properties and thermal conductivity, effectively improving the mechanical properties of PET materials. However, the compatibility of graphene with PET materials and the dispersion uniformity of graphene nanomaterials will affect the overall performance of composite materials. Summary of the Invention

[0004] The purpose of this invention is to provide a process for preparing graphene-based modified polyester fibers to solve the problems mentioned in the background art.

[0005] To solve the above-mentioned technical problems, the present invention provides the following technical solution:

[0006] The preparation process of graphene-modified polyester fibers involves the following steps:

[0007] Step 1: Weigh out graphene oxide, ammonium molybdate tetrahydrate, and thiourea in sequence. Place the graphene in deionized water and sonicate for 2-3 hours. Then add ammonium molybdate tetrahydrate, thiourea, and surfactant, and continue sonicating for 1-2 hours. Mix thoroughly, adjust the pH to 1-2, and heat at 220-240℃ for 12-24 hours. Remove and centrifuge, wash, and place at -20--25℃ for pre-freezing treatment. Then freeze-dry for 10-12 hours to obtain graphene composite powder.

[0008] Step 2: Weigh mercaptoacetic acid, add the graphene composite powder prepared in Step 1, mix evenly, add deionized water, sonicate for 2-3 hours, centrifuge at 2500-3000 rpm for 10-15 minutes, take the supernatant, dialyze for 2-3 hours until pH=7, and freeze dry to obtain the carboxylated composite material.

[0009] Step 3: Add the carboxylated composite material prepared in step 2, 4-benzylmethylaminophenol and alkaline catalyst to anhydrous dichloromethane, stir to dissolve, heat to 30~50℃, react for 2~3h, filter out the solid material, wash with alcohol and water alternately 3 times, dry at 80~100℃ for 6~8h, and grind to obtain the modified graphene composite material.

[0010] Step 4: Weigh the pure polyester fiber melt and the modified graphene composite material prepared in Step 3, and place them separately in a vacuum dryer at 100~120℃ for 10~12h. Cool them for later use. Mix the pure polyester fiber melt obtained from the treatment and the modified graphene composite material prepared in Step 3 evenly, and then perform melt blending, spin extrusion, wetting and oiling, and winding and bundling to obtain the graphene modified polyester fiber.

[0011] In step 1, the molar ratio of graphene oxide, ammonium molybdate tetrahydrate, and thiourea is (10~15):1:(25~30).

[0012] In step 1, the surfactant is one of sodium dodecylbenzenesulfonate, hexadecyltrimethylammonium bromide, and polyvinylpyrrolidone; it is further configured as sodium dodecylbenzenesulfonate.

[0013] In step 2, the molar ratio of thioglycolic acid and graphene composite powder is (8~10):1.

[0014] In step 3, the mass ratio of 4-benzylaminophenol to carboxylated composite material is 2:1; the alkaline catalyst is a pyridine compound, and the amount added is (8~10) wt% of 4-benzylaminophenol, and the alkaline catalyst is further set as 4-dimethylaminopyridine.

[0015] In step 4, the mass ratio of the pure polyester fiber melt to the modified graphene composite material prepared in step 3 is 100:(1~5).

[0016] Compared with existing technologies, the beneficial effects achieved by this invention are as follows: This invention uses graphene-modified molybdenum disulfide surface-grafted with aromatic Schiff bases and melt-blended with PET sheets to prepare a modified polyester fiber; the hydrothermal preparation of molybdenum disulfide exhibits agglomeration, and graphene oxide is gradually reduced to reduced graphene oxide. The graphene composite powder obtained by combining it with molybdenum disulfide not only improves the dispersibility of both, but also, different surfactants bring different structural characteristics to the synthesis of molybdenum disulfide. The layered structure of the composite of sheet-like molybdenum disulfide and reduced graphene oxide greatly increases the specific surface area of ​​the material, providing more binding sites for subsequent grafting of aromatic Schiff bases; regarding the structure of the composite material, both graphene and molybdenum disulfide are high-performance lubricant additives, possessing... The excellent friction-reducing and wear-resistant properties, combined with the interlayer bonding of the two components, provide synergistic lubrication. The graphene composite powder is carboxylated with mercaptoacetic acid to graft aromatic Schiff bases. Graphene itself, as a carbon-based flame retardant, improves the char quality and thermal stability of the polymer. Aromatic Schiff bases can form stable cross-linked networks with PET materials at melting and decomposition temperatures, which is beneficial for the formation of a protective char layer during combustion. After grafting with aromatic Schiff bases, the graphene composite material not only improves the compatibility between graphene and PET substrates but also further enhances the combustion inhibition effect of modified polyester fiber materials, improving the flame retardant effect. Simultaneously, the amount of modified graphene composite material added is fixed within a certain range to improve the toughness of the blend, thereby improving the mechanical properties of the material. Detailed Implementation

[0017] The technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0018] In the experiment, the particle size of graphene oxide was 2~3nm and it was purchased from Jiangxi Shuobang New Material Technology Co., Ltd.; the intrinsic viscosity of pure polyester fiber melt was (0.650±0.010) dL / g and it was purchased from Huzhou Zhonglei Chemical Fiber Co., Ltd.

[0019] Example 1: This example provides a preparation process for graphene-modified polyester fiber, the specific steps of which are as follows:

[0020] Step 1: Weigh out 1.25g of graphene oxide, 15.45g of ammonium molybdate tetrahydrate, and 28.5g of thiourea in sequence. Place the graphene in 200ml of deionized water and sonicate for 2 hours. Then add ammonium molybdate tetrahydrate, thiourea, and 0.18g of sodium dodecylbenzenesulfonate. Continue sonicating for another 2 hours. Mix thoroughly, adjust the pH to 1, and heat at 240℃ for 24 hours. Remove and centrifuge, wash, place at -20℃ for pre-freezing, and then freeze-dry for 12 hours to obtain graphene composite powder.

[0021] Step 2: Weigh 18.4g of mercaptoacetic acid, add 2g of graphene composite powder prepared in step 1, mix evenly, add 100ml of deionized water, sonicate for 2h, centrifuge at 3000rpm for 15min, take the supernatant, dialyze for 2h until pH=7, freeze dry to obtain carboxylated composite material.

[0022] Step 3: Add 2g of the carboxylated composite material prepared in Step 2, 1g of 4-benzylmethylaminophenol and 0.1g of 4-dimethylaminopyridine to 50ml of anhydrous dichloromethane, stir to dissolve, heat to 30℃, react for 2h, filter out the solid material, wash with alcohol and water alternately 3 times, dry at 100℃ for 8h, and grind to obtain the modified graphene composite material.

[0023] Step 4: Weigh 100g of pure polyester fiber melt and 2g of the modified graphene composite material prepared in Step 3, and place them separately in a vacuum dryer at 120℃ for 12h. Cool them for later use. Mix the pure polyester fiber melt and the modified graphene composite material prepared in Step 3 evenly, and then perform melt blending, spin extrusion, wetting and oiling, and winding and bundling to obtain the graphene modified polyester fiber.

[0024] Example 2: This example provides a preparation process for graphene-modified polyester fiber, the specific steps of which are as follows:

[0025] Step 1: Weigh out 1.25g of graphene oxide, 15.45g of ammonium molybdate tetrahydrate, and 28.5g of thiourea in sequence. Place the graphene in 200ml of deionized water and sonicate for 2 hours. Then add ammonium molybdate tetrahydrate, thiourea, and 0.18g of sodium dodecylbenzenesulfonate. Continue sonicating for another 2 hours. Mix thoroughly, adjust the pH to 1, and heat at 240℃ for 24 hours. Remove and centrifuge, wash, place at -20℃ for pre-freezing, and then freeze-dry for 12 hours to obtain graphene composite powder.

[0026] Step 2: Weigh 18.4g of mercaptoacetic acid, add 2g of graphene composite powder prepared in step 1, mix evenly, add 100ml of deionized water, sonicate for 2h, centrifuge at 3000rpm for 15min, take the supernatant, dialyze for 2h until pH=7, freeze dry to obtain carboxylated composite material.

[0027] Step 3: Add 2g of the carboxylated composite material prepared in Step 2, 1g of 4-benzylmethylaminophenol and 0.1g of 4-dimethylaminopyridine to 50ml of anhydrous dichloromethane, stir to dissolve, heat to 30℃, react for 2h, filter out the solid material, wash with alcohol and water alternately 3 times, dry at 100℃ for 8h, and grind to obtain the modified graphene composite material.

[0028] Step 4: Weigh 100g of pure polyester fiber melt and 4g of the modified graphene composite material prepared in Step 3, and place them separately in a vacuum dryer at 120℃ for 12h. Cool them for later use. Mix the pure polyester fiber melt and the modified graphene composite material prepared in Step 3 evenly, and then perform melt blending, spin extrusion, wetting and oiling, and winding and bundling to obtain the graphene modified polyester fiber.

[0029] Example 3: This example provides a preparation process for graphene-modified polyester fiber, the specific steps of which are as follows:

[0030] Step 1: Weigh out 1.5g of graphene oxide, 15.45g of ammonium molybdate tetrahydrate, and 28.5g of thiourea in sequence. Place the graphene in 200ml of deionized water and sonicate for 2 hours. Then add ammonium molybdate tetrahydrate, thiourea, and 0.18g of sodium dodecylbenzenesulfonate. Continue sonicating for another 2 hours. Mix thoroughly, adjust the pH to 1, and heat at 240℃ for 24 hours. Remove and centrifuge, wash, place at -20℃ for pre-freezing, and then freeze-dry for 12 hours to obtain graphene composite powder.

[0031] Step 2: Weigh 18.4g of mercaptoacetic acid, add 2g of graphene composite powder prepared in step 1, mix evenly, add 100ml of deionized water, sonicate for 2h, centrifuge at 3000rpm for 15min, take the supernatant, dialyze for 2h until pH=7, freeze dry to obtain carboxylated composite material.

[0032] Step 3: Add 2g of the carboxylated composite material prepared in Step 2, 1g of 4-benzylmethylaminophenol and 0.1g of 4-dimethylaminopyridine to 50ml of anhydrous dichloromethane, stir to dissolve, heat to 30℃, react for 2h, filter out the solid material, wash with alcohol and water alternately 3 times, dry at 100℃ for 8h, and grind to obtain the modified graphene composite material.

[0033] Step 4: Weigh 100g of pure polyester fiber melt and 3g of the modified graphene composite material prepared in Step 3, and place them separately in a vacuum dryer at 120℃ for 12h. Cool them for later use. Mix the pure polyester fiber melt and the modified graphene composite material prepared in Step 3 evenly, and then perform melt blending, spin extrusion, wetting and oiling, and winding and bundling to obtain the graphene modified polyester fiber.

[0034] Example 4: This example provides a preparation process for graphene-modified polyester fiber, the specific steps of which are as follows:

[0035] Step 1: Weigh out 1.5g of graphene oxide, 15.45g of ammonium molybdate tetrahydrate, and 28.5g of thiourea in sequence. Place the graphene in 200ml of deionized water and sonicate for 2 hours. Then add ammonium molybdate tetrahydrate, thiourea, and 0.18g of sodium dodecylbenzenesulfonate. Continue sonicating for another 2 hours. Mix thoroughly, adjust the pH to 1, and heat at 240℃ for 24 hours. Remove and centrifuge, wash, place at -20℃ for pre-freezing, and then freeze-dry for 12 hours to obtain graphene composite powder.

[0036] Step 2: Weigh 18.4g of mercaptoacetic acid, add 2g of graphene composite powder prepared in step 1, mix evenly, add 100ml of deionized water, sonicate for 2h, centrifuge at 3000rpm for 15min, take the supernatant, dialyze for 2h until pH=7, freeze dry to obtain carboxylated composite material.

[0037] Step 3: Add 2g of the carboxylated composite material prepared in Step 2, 1g of 4-benzylmethylaminophenol and 0.1g of 4-dimethylaminopyridine to 50ml of anhydrous dichloromethane, stir to dissolve, heat to 30℃, react for 2h, filter out the solid material, wash with alcohol and water alternately 3 times, dry at 100℃ for 8h, and grind to obtain the modified graphene composite material.

[0038] Step 4: Weigh 100g of pure polyester fiber melt and 4g of the modified graphene composite material prepared in Step 3, and place them separately in a vacuum dryer at 120℃ for 12h. Cool them for later use. Mix the pure polyester fiber melt and the modified graphene composite material prepared in Step 3 evenly, and then perform melt blending, spin extrusion, wetting and oiling, and winding and bundling to obtain the graphene modified polyester fiber.

[0039] Example 5: This example provides a preparation process for graphene-modified polyester fiber, the specific steps of which are as follows:

[0040] Step 1: Weigh out 1.5g of graphene oxide, 15.45g of ammonium molybdate tetrahydrate, and 28.5g of thiourea in sequence. Place the graphene in 200ml of deionized water and sonicate for 2 hours. Then add ammonium molybdate tetrahydrate, thiourea, and 0.18g of sodium dodecylbenzenesulfonate. Continue sonicating for another 2 hours. Mix thoroughly, adjust the pH to 1, and heat at 240℃ for 24 hours. Remove and centrifuge, wash, place at -20℃ for pre-freezing, and then freeze-dry for 12 hours to obtain graphene composite powder.

[0041] Step 2: Weigh 18.4g of mercaptoacetic acid, add 2g of graphene composite powder prepared in step 1, mix evenly, add 100ml of deionized water, sonicate for 2h, centrifuge at 3000rpm for 15min, take the supernatant, dialyze for 2h until pH=7, freeze dry to obtain carboxylated composite material.

[0042] Step 3: Add 2g of the carboxylated composite material prepared in Step 2, 1g of 4-benzylmethylaminophenol and 0.1g of 4-dimethylaminopyridine to 50ml of anhydrous dichloromethane, stir to dissolve, heat to 30℃, react for 2h, filter out the solid material, wash with alcohol and water alternately 3 times, dry at 100℃ for 8h, and grind to obtain the modified graphene composite material.

[0043] Step 4: Weigh 100g of pure polyester fiber melt and 5g of the modified graphene composite material prepared in Step 3, and place them separately in a vacuum dryer at 120℃ for 12h. Cool them for later use. Mix the pure polyester fiber melt and the modified graphene composite material prepared in Step 3 evenly, and then perform melt blending, spin extrusion, wetting and oiling, and winding and bundling to obtain the graphene modified polyester fiber.

[0044] Comparative Example 1: Comparative Example 1 is a control experiment for Example 4, which does not include graphene oxide. The specific steps are as follows:

[0045] Step 1: Weigh 15.45g of ammonium molybdate tetrahydrate and 28.5g of thiourea in sequence. Place the graphene in 200ml of deionized water and sonicate for 2 hours. Then add ammonium molybdate tetrahydrate, thiourea and 0.18g of sodium dodecylbenzenesulfonate. Continue sonicating for 2 hours, mix evenly, adjust the pH to 1, heat at 240℃ for 24 hours, remove and centrifuge, wash, place at -20℃ for pre-freezing, and then freeze-dry for 12 hours to obtain molybdenum disulfide powder.

[0046] Step 2: Weigh 18.4g of mercaptoacetic acid, add 2g of molybdenum disulfide powder prepared in Step 1, mix well, add 100ml of deionized water, sonicate for 2h, centrifuge at 3000rpm for 15min, take the supernatant, dialyze for 2h until pH=7, freeze dry to obtain carboxylated composite material.

[0047] Step 3: Add 2g of the carboxylated composite material prepared in step 2, 1g of 4-benzylmethylaminophenol and 0.1g of 4-dimethylaminopyridine to 50ml of anhydrous dichloromethane, stir to dissolve, heat to 30℃, react for 2h, filter out the solid material, wash with alcohol and water alternately 3 times, dry at 100℃ for 8h, and grind to obtain the modified composite material.

[0048] Step 4: Weigh 100g of pure polyester fiber melt and 4g of the modified composite material prepared in Step 3, and place them separately in a vacuum dryer at 120℃ for 12h. Cool them for later use. Mix the pure polyester fiber melt and the modified composite material prepared in Step 3 evenly, and then perform melt blending, spin extrusion, wetting and oiling, and winding and bundling to obtain the modified polyester fiber.

[0049] Comparative Example 2: Comparative Example 2 is a control experiment of Example 4, except that sodium dodecylbenzenesulfonate was replaced with hexadecyltrimethylammonium bromide. The specific steps are as follows:

[0050] Step 1: Weigh out 1.5g of graphene oxide, 15.45g of ammonium molybdate tetrahydrate, and 28.5g of thiourea in sequence. Place the graphene in 200ml of deionized water and sonicate for 2 hours. Then add ammonium molybdate tetrahydrate, thiourea, and 0.18g of cetyltrimethylammonium bromide and sonicate for another 2 hours. Mix well, adjust the pH to 1, heat at 240℃ for 24 hours, remove and centrifuge, wash, place at -20℃ for pre-freezing, and then freeze-dry for 12 hours to obtain graphene composite powder.

[0051] Step 2: Weigh 18.4g of mercaptoacetic acid, add 2g of graphene composite powder prepared in step 1, mix evenly, add 100ml of deionized water, sonicate for 2h, centrifuge at 3000rpm for 15min, take the supernatant, dialyze for 2h until pH=7, freeze dry to obtain carboxylated composite material.

[0052] Step 3: Add 2g of the carboxylated composite material prepared in Step 2, 1g of 4-benzylmethylaminophenol and 0.1g of 4-dimethylaminopyridine to 50ml of anhydrous dichloromethane, stir to dissolve, heat to 30℃, react for 2h, filter out the solid material, wash with alcohol and water alternately 3 times, dry at 100℃ for 8h, and grind to obtain the modified graphene composite material.

[0053] Step 4: Weigh 100g of pure polyester fiber melt and 4g of the modified graphene composite material prepared in Step 3, and place them separately in a vacuum dryer at 120℃ for 12h. Cool them for later use. Mix the pure polyester fiber melt and the modified graphene composite material prepared in Step 3 evenly, and then perform melt blending, spin extrusion, wetting and oiling, and winding and bundling to obtain the graphene modified polyester fiber.

[0054] Comparative Example 3: Comparative Example 3 serves as a control experiment for Example 4. The amount of modified graphene composite material was adjusted compared to Example 4. The specific steps are as follows:

[0055] Step 1: Weigh out 1.5g of graphene oxide, 15.45g of ammonium molybdate tetrahydrate, and 28.5g of thiourea in sequence. Place the graphene in 200ml of deionized water and sonicate for 2 hours. Then add ammonium molybdate tetrahydrate, thiourea, and 0.18g of sodium dodecylbenzenesulfonate. Continue sonicating for another 2 hours. Mix thoroughly, adjust the pH to 1, and heat at 240℃ for 24 hours. Remove and centrifuge, wash, place at -20℃ for pre-freezing, and then freeze-dry for 12 hours to obtain graphene composite powder.

[0056] Step 2: Weigh 18.4g of mercaptoacetic acid, add 2g of graphene composite powder prepared in step 1, mix evenly, add 100ml of deionized water, sonicate for 2h, centrifuge at 3000rpm for 15min, take the supernatant, dialyze for 2h until pH=7, freeze dry to obtain carboxylated composite material.

[0057] Step 3: Add 2g of the carboxylated composite material prepared in Step 2, 1g of 4-benzylmethylaminophenol and 0.1g of 4-dimethylaminopyridine to 50ml of anhydrous dichloromethane, stir to dissolve, heat to 30℃, react for 2h, filter out the solid material, wash with alcohol and water alternately 3 times, dry at 100℃ for 8h, and grind to obtain the modified graphene composite material.

[0058] Step 4: Weigh 100g of pure polyester fiber melt and 10g of the modified graphene composite material prepared in Step 3, and place them separately in a vacuum dryer at 120℃ for 12h. Cool them for later use. Mix the pure polyester fiber melt and the modified graphene composite material prepared in Step 3 evenly, and then perform melt blending, spin extrusion, wetting and oiling, and winding and bundling to obtain the graphene modified polyester fiber.

[0059] Testing and Experiment

[0060] 1. Perform tensile property tests according to GB / T 9997: Take the modified polyester fiber filaments prepared in Examples 1-5 and Comparative Examples 1-3, and take a 1m long filament as a sample on a telescopic cylinder. After ensuring that the jaws of the moving clamp are aligned and parallel, clamp the sample and test with a spacing of 20mm and a moving clamp speed of 40mm / min. Each set of examples is tested 3 times. Calculate and record the average values ​​of tensile strength and elongation at break.

[0061] 2. Flame retardant performance test: According to the vertical burning test method, the modified polyester fibers prepared in Examples 1-5 and Comparative Examples 1-3 were vertically suspended on the burning rack, the lower end of the sample was ignited, the burning situation of the sample was observed, and the rating was recorded according to the UL94 standard.

[0062]

[0063] Based on the above experimental data: Example 4 shows that the modified polyester fiber prepared in Examples 1-5 has relatively excellent comprehensive mechanical properties and flame retardant properties; Comparative Example 1, which does not add graphene oxide compared to Example 4, has a certain impact on both mechanical and flame retardant properties; Comparative Example 2, which changes the surfactant in the hydrothermal method compared to Example 4, replacing sodium dodecylbenzenesulfonate with hexadecyltrimethylammonium bromide and changing the molybdenum disulfide structure, has a slight impact on both flame retardant and mechanical properties; Comparative Example 3, which adjusts the amount of modified graphene composite material compared to Example 4, has the greatest impact on mechanical and flame retardant properties because the amount of modified graphene composite material exceeds the weight range.

[0064] Conclusion: This experiment yielded a graphene-modified polyester fiber. By melt-blending graphene-molybdenum disulfide-grafted aromatic Schiff base with PET sheets, a polyester fiber with flame retardant effect and good mechanical properties was obtained.

[0065] Finally, it should be noted that the above descriptions are merely preferred embodiments of the present invention and are not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent substitutions for some of the technical features. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A preparation process for graphene-modified polyester fiber, characterized in that, The specific steps are as follows: Step 1: Weigh out graphene oxide, ammonium molybdate tetrahydrate, and thiourea in sequence. Place the graphene in deionized water and sonicate for 2-3 hours. Then add ammonium molybdate tetrahydrate, thiourea, and surfactant, and continue sonicating for 1-2 hours. Mix thoroughly, adjust the pH to 1, and heat at 220-240℃ for 24 hours. Remove and centrifuge, wash, place at -20℃ for pre-freezing, and then freeze-dry for 10-12 hours to obtain graphene composite powder. Step 2: Weigh mercaptoacetic acid, add the graphene composite powder prepared in Step 1, mix evenly, add deionized water, sonicate for 2-3 hours, centrifuge to collect the supernatant, dialyze for 2-3 hours until pH=7, and freeze dry to obtain the carboxylated composite material. Step 3: Add the carboxylated composite material prepared in step 2, 4-benzylmethylaminophenol and alkaline catalyst to anhydrous dichloromethane, stir to dissolve, heat to 30°C, react for 2 hours, filter out the solid material, wash and dry, and grind to obtain the modified graphene composite material. Step 4: Weigh the pure polyester fiber melt and the modified graphene composite material prepared in Step 3, and place them in vacuum drying at 100~120℃ for 10~12h respectively. Cool them for later use. Mix the pure polyester fiber melt obtained by the treatment and the modified graphene composite material prepared in Step 3 evenly, and carry out melt blending, spin extrusion, wetting and oiling, and winding and bundling to obtain the graphene modified polyester fiber. In step 1, the molar ratio of graphene oxide, ammonium molybdate tetrahydrate, and thiourea is (10~15):1:(25~30); In step 1, the surfactant is one of sodium dodecylbenzenesulfonate, hexadecyltrimethylammonium bromide, and polyvinylpyrrolidone.

2. The preparation process of graphene-modified polyester fiber according to claim 1, characterized in that, In step 2, the molar ratio of thioglycolic acid and graphene composite powder is (8~10):

1.

3. The preparation process of graphene-modified polyester fiber according to claim 1, characterized in that, In step 2, centrifugation is performed at 2500~3000 rpm for 10~15 min.

4. The preparation process of graphene-modified polyester fiber according to claim 1, characterized in that, In step 3, the mass ratio of 4-benzylaminophenol to the carboxylated composite material is 2:

1.

5. The preparation process of graphene-modified polyester fiber according to claim 1, characterized in that, In step 3, the alkaline catalyst is a pyridine compound, and the amount of alkaline catalyst added is (8~10) wt% of 4-benzylmethylaminophenol.

6. The preparation process of graphene-modified polyester fiber according to claim 1, characterized in that, In step 3, the solid material is filtered out by suction filtration. The specific steps for washing and drying in step 3 are as follows: wash with alcohol and water alternately 3 times, and dry at 80~100℃ for 6~8 hours.

7. The preparation process of graphene-modified polyester fiber according to claim 1, characterized in that, In step 4, the mass ratio of pure polyester fiber melt to modified graphene composite material is 100:(1~5).

Citation Information

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