Soft modified composite staple fiber and method of producing same

Abstract

The present application relates to the technical field of fiber materials, in particular to a soft modified composite staple fiber and a production method thereof, which is used to solve the problem that the softness, mechanical properties and antibacterial properties of the existing composite staple fiber are not good, which limits its application in some scenarios; the production method uses PET resin as the core layer raw material of the composite staple fiber, which gives it higher strength and toughness, and after adding modified graphene oxide, the mechanical properties can be further improved; PE resin is used as the skin layer raw material of the composite staple fiber, which gives it better softness and wear resistance, and after adding quaternary ammonium base polysiloxane, the antibacterial properties can be greatly improved, and the softness is further improved; the composite staple fiber has high mechanical properties and antibacterial properties while maintaining softness and comfort, and is very suitable for manufacturing high-quality home textiles, clothing and other products, and the production method is simple in process and easy to operate, and is suitable for large-scale industrial production.

Description

Technical Field

[0001] The present invention relates to the technical field of fiber materials, and in particular to a soft modified composite short fiber and a production method thereof. Background Art

[0002] With the development of modern science and technology, people have higher and higher requirements for fiber materials. Traditional fiber materials, such as PE fiber, have softness and PET fiber, have mechanical strength. Although they have their own advantages, a single material is difficult to meet the multifunctional requirements of modern fiber materials.

[0003] In recent years, the skin-core structure has become a research hotspot due to its unique performance advantages. This structure can improve the mechanical properties and softness of the fiber to a certain extent through the different designs of the inner and outer layer materials. However, although the existing skin-core structure composite staple fibers have improved in mechanical properties, the improvement effect is limited, and they often perform poorly in terms of antibacterial properties, making it difficult to meet the needs of certain application scenarios, such as medical supplies, sanitary products or advanced textiles. Therefore, it is particularly urgent to develop a composite staple fiber that has softness, excellent mechanical properties and antibacterial properties. Summary of the Invention

[0004] In order to overcome the above-mentioned technical problems, the purpose of the present invention is to provide a soft modified composite staple fiber and a production method thereof, which solves the problem that the existing composite staple fibers have poor softness, mechanical properties and antibacterial properties, which limit their application in certain scenarios.

[0005] The purpose of the present invention can be achieved through the following technical solutions:

[0006] A soft modified composite staple fiber comprises a core layer and a sheath layer;

[0007] Wherein, the core layer comprises the following components in parts by weight:

[0008] 100 parts of PET resin, 0.2-2.2 parts of modified graphene oxide;

[0009] Wherein, the cortex comprises the following components in parts by weight:

[0010] 100 parts of PE resin, 3-15 parts of quaternary ammonium polysiloxane;

[0011] Wherein, the modified graphene oxide is prepared by the following steps:

[0012] Step a1: adding graphite powder, concentrated sulfuric acid and concentrated nitric acid to a three-necked flask equipped with a stirrer and a thermometer, stirring at a temperature of -5-0°C and a stirring rate of 300-400 r / min for 20-30 min, then adding potassium permanganate and continuing to stir and react for 1-1.5 h, then heating to 35-40°C and continuing to stir and react for 2-3 h, then heating to 90-100°C and continuing to stir and react for 6-8 h, after the reaction is completed, pouring the reaction product into ice water, then adding hydrogen peroxide, and then centrifuging. The precipitate is washed with hydrochloric acid solution and distilled water 3-5 times in sequence, and then placed in a vacuum drying oven and dried at a temperature of 50-55°C for 3-4 h to obtain graphene oxide;

[0013] Step a2: Add graphene oxide and N,N-dimethylformamide to a three-necked flask equipped with a stirrer and a thermometer, stir at a temperature of 25-30°C and a stirring rate of 300-400 r / min for 20-30 minutes, then add isophorone diisocyanate and continue stirring to react for 20-30 minutes, then adjust the pH to 9-10 with ammonia water, then raise the temperature to 85-90°C and continue stirring to react for 10-12 hours, and after the reaction is completed, cool the reaction product to room temperature, then centrifuge, wash the precipitate with distilled water 3-5 times, and then place it in a vacuum drying oven and dry it at a temperature of 60-65°C for 2-3 hours to obtain modified graphene oxide.

[0014] As a further solution of the present invention: the usage ratio of the graphite powder, concentrated sulfuric acid, concentrated nitric acid, potassium permanganate and hydrogen peroxide in step a1 is 1 g: 25-30 mL: 10-15 mL: 4-6 g: 10-15 mL.

[0015] As a further solution of the present invention: the mass fraction of the concentrated sulfuric acid in step a1 is 96-98%.

[0016] As a further solution of the present invention: the mass fraction of the concentrated nitric acid in step a1 is 66-68%.

[0017] As a further solution of the present invention: the mass fraction of the hydrogen peroxide in step a1 is 25-30%.

[0018] As a further solution of the present invention: the mass fraction of the hydrochloric acid solution in step a1 is 10-15%.

[0019] As a further solution of the present invention: the usage ratio of the graphene oxide, N,N-dimethylformamide and isophorone diisocyanate in step a2 is 1 g:50-60 mL:2-6 g.

[0020] As a further solution of the present invention: the mass fraction of the ammonia water in step a2 is 20-25%.

[0021] As a further embodiment of the present invention: the quaternary ammonium polysiloxane is prepared by the following steps:

[0022] Step b1: adding hydrogen silicone oil, allyl alcohol glycidyl ether, Karstedt catalyst and isopropanol to a three-necked flask equipped with a stirrer and a thermometer, stirring at a temperature of 25-30° C. and a stirring rate of 300-400 r / min for 20-30 minutes, then heating to 80-85° C. and continuing stirring for 3-4 hours. After the reaction is completed, the reaction product is cooled to room temperature, and then the solvent is removed by rotary evaporation to obtain epoxy polysiloxane;

[0023] Step b2: Add epoxy polysiloxane, triethanolamine, acetic acid and isopropyl alcohol to a three-necked flask equipped with a stirrer and a thermometer, stir at a temperature of 25-30°C and a stirring rate of 300-400 r / min for 20-30 minutes, then raise the temperature to 65-70°C and continue stirring for 3-4 hours. After the reaction is completed, the reaction product is cooled to room temperature, and then the solvent is removed by rotary evaporation to obtain quaternary ammonium polysiloxane.

[0024] As a further embodiment of the present invention, the ratio of the hydrogenated silicone oil, allyl alcohol glycidyl ether, Karstedt catalyst and isopropanol in step b1 is 10 g: 1.1-2.5 g: 0.02-0.06 g: 20-25 mL.

[0025] As a further solution of the present invention: the mass fraction of active hydrogen in the hydrogen-containing silicone oil in step b1 is 0.06-0.08%.

[0026] As a further solution of the present invention: the usage ratio of the epoxy polysiloxane, triethanolamine, acetic acid and isopropyl alcohol in step b2 is 10g:1.3-2.1g:2.5-3.5g:40-50mL.

[0027] As a further embodiment of the present invention: a method for producing soft modified composite staple fibers comprises the following steps:

[0028] Step 1: Weigh 100 parts of PET resin, 0.2-2.2 parts of modified graphene oxide, 100 parts of PE resin, and 3-15 parts of quaternary ammonium polysiloxane according to weight, and set aside; the model of the PET resin is Sinopec Yizheng FG600; the model of the PE resin is Sinochem Quanzhou Petrochemical HDPE5502;

[0029] Step 2: PET resin and modified graphene oxide are mixed evenly, and then added into a single-screw extruder I, and melt-extruded at a temperature of 260-270° C. to obtain a core layer melt;

[0030] Step 3: PE resin and quaternary ammonium polysiloxane are mixed evenly, and then added into a single screw extruder II, and melt-extruded at a temperature of 230-250°C to obtain a skin layer melt;

[0031] Step 4: The core layer melt and the skin layer melt are combined in a mass ratio of 3:7 and uniformly extruded through the skin-core composite spinning assembly. After cooling, oiling and winding, soft modified composite short fibers are obtained.

[0032] Beneficial effects of the present invention:

[0033] The present invention discloses a soft modified composite staple fiber and a production method thereof, comprising the steps of uniformly mixing PET resin and modified graphene oxide, adding the mixture to a single screw extruder I for melt extrusion to obtain a core layer melt, uniformly mixing PE resin and quaternary ammonium polysiloxane, adding the mixture to a single screw extruder II for melt extrusion to obtain a skin layer melt, combining the core layer melt and the skin layer melt into a skin-core composite spinning assembly for uniform extrusion molding, and then cooling, oiling and winding to obtain a soft modified composite staple fiber; the production method uses PET resin as the core layer raw material of the composite staple fiber, imparting it with higher strength and toughness, and adding modified oxide to obtain a soft modified composite staple fiber; Graphene can further improve its mechanical properties. PE resin is used as the cortex raw material of the composite staple fiber, which gives it better softness and wear resistance. Adding quaternary ammonium polysiloxane thereto can greatly improve its antibacterial properties and further improve its softness. Therefore, the composite staple fiber with a skin-core structure finally obtained not only maintains softness and comfort, but also has high mechanical properties and antibacterial properties. It is very suitable for manufacturing high-quality home textiles, clothing and other products, while increasing the service life of the product, meeting the modern society's demand for environmentally friendly and healthy materials. Moreover, the production method is simple in process, easy to operate, and suitable for large-scale industrial production.

[0034] In the process of preparing the soft modified composite staple fibers, a modified graphene oxide is first prepared. Graphite powder is used as the raw material to prepare graphene oxide. Then, the graphene oxide is treated with isophorone diisocyanate. Organic matter is grafted onto the surface of the graphene oxide to encapsulate it, improving its dispersibility, making it less likely to agglomerate and allowing it to be evenly distributed in the matrix. The introduced isocyanate groups enable it to bond to the matrix in the form of chemical bonds, significantly improving the mechanical properties of the composite staple fibers.

[0035] In the process of preparing soft modified composite staple fibers, a quaternary ammonium polysiloxane is also prepared. First, hydrogenated silicone oil and allyl alcohol glycidyl ether are reacted, and the SiH on the hydrogenated silicone oil undergoes a silylation reaction with the alkenyl group on the allyl alcohol glycidyl ether, and at the same time, an epoxy group is introduced to obtain epoxy polysiloxane. Then, epoxy polysiloxane and triethanolamine are reacted, and the epoxy group on the epoxy polysiloxane reacts with the tertiary amine group on the triethanolamine to form a quaternary ammonium group to obtain quaternary ammonium polysiloxane. The SiO bond in the quaternary ammonium polysiloxane imparts excellent flexibility and elasticity, thereby improving the softness of the composite staple fibers. In addition, the introduced quaternary ammonium group has an excellent antibacterial effect, which greatly improves the antibacterial and antibacterial properties of the composite staple fibers. DETAILED DESCRIPTION

[0036] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts shall fall within the scope of protection of the present invention.

[0037] Example 1:

[0038] This embodiment is a method for producing a soft modified composite staple fiber, comprising the following steps:

[0039] Step S1: 1 g of graphite powder, 25 mL of 96% concentrated sulfuric acid, and 10 mL of 66% concentrated nitric acid were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at a temperature of -5 ° C and a stirring rate of 300 r / min for 20 min. Then, 4 g of potassium permanganate was added and the stirring reaction was continued for 1 h. Then, the temperature was raised to 35 ° C and the stirring reaction was continued for 2 h. Then, the temperature was raised to 90 ° C and the stirring reaction was continued for 6 h. After the reaction was completed, the reaction product was poured into ice water, and then 10 mL of 25% hydrogen peroxide was added. After centrifugation, the precipitate was washed three times with a 10% hydrochloric acid solution and distilled water, and then placed in a vacuum drying oven and dried at a temperature of 50 ° C for 3 h to obtain graphene oxide;

[0040] Step S2: 1 g of graphene oxide and 50 mL of N,N-dimethylformamide were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at a temperature of 25 ° C. and a stirring rate of 300 r / min for 20 min. Then, 2 g of isophorone diisocyanate was added and the stirring reaction was continued for 20 min. Then, the pH was adjusted to 9 with 20% ammonia water, and then the temperature was raised to 85 ° C. and the stirring reaction was continued for 10 h. After the reaction was completed, the reaction product was cooled to room temperature and then centrifuged. The precipitate was washed with distilled water 3 times, and then placed in a vacuum drying oven and dried at a temperature of 60 ° C. for 2 h to obtain modified graphene oxide;

[0041] Step S3: 10 g of hydrogen-containing silicone oil with an active hydrogen mass fraction of 0.06%, 1.1 g of allyl alcohol glycidyl ether, 0.02 g of Karstedt catalyst, and 20 mL of isopropanol were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at a temperature of 25° C. and a stirring rate of 300 r / min for 20 minutes. The temperature was then raised to 80° C. and the stirring reaction was continued for 3 hours. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation to obtain epoxy polysiloxane;

[0042] Step S4: 10 g of epoxy polysiloxane, 1.3 g of triethanolamine, 2.5 g of acetic acid, and 40 mL of isopropanol were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at 25° C. and a stirring rate of 300 r / min for 20 min. The temperature was then raised to 65° C. and the stirring reaction was continued for 3 h. After the reaction was completed, the reaction product was cooled to room temperature, and the solvent was then removed by rotary evaporation to obtain a quaternary ammonium polysiloxane;

[0043] Step S5: Weigh 100 parts of PET resin, 0.2 parts of modified graphene oxide, 100 parts of PE resin, and 3 parts of quaternary ammonium polysiloxane according to weight and set aside; the model of the PET resin is Sinopec Yizheng FG600; the model of the PE resin is Sinochem Quanzhou Petrochemical HDPE5502;

[0044] Step S6: PET resin and modified graphene oxide are mixed evenly, and then added into a single-screw extruder I, and melt-extruded at a temperature of 260° C. to obtain a core layer melt;

[0045] Step S7: PE resin and quaternary ammonium polysiloxane are mixed evenly, and then added into a single-screw extruder II, and melt-extruded at a temperature of 230° C. to obtain a skin layer melt;

[0046] Step S8: The core layer melt and the skin layer melt are combined in a mass ratio of 3:7 and uniformly extruded through a core-skin composite spinning assembly, and then cooled, oiled and wound to obtain a soft modified composite staple fiber.

[0047] Example 2:

[0048] This embodiment is a method for producing a soft modified composite staple fiber, comprising the following steps:

[0049] Step S1: 1 g of graphite powder, 28 mL of 97% concentrated sulfuric acid, and 12 mL of 67% concentrated nitric acid were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at a temperature of -3 ° C and a stirring rate of 350 r / min for 25 min. Then, 5 g of potassium permanganate was added and the stirring reaction was continued for 1.2 h. Then, the temperature was raised to 38 ° C and the stirring reaction was continued for 2.5 h. Then, the temperature was raised to 95 ° C and the stirring reaction was continued for 7 h. After the reaction was completed, the reaction product was poured into ice water, and then 12 mL of 28% hydrogen peroxide was added. After centrifugation, the precipitate was washed 4 times with a 12% hydrochloric acid solution and distilled water, and then placed in a vacuum drying oven and dried at a temperature of 52 ° C for 3.5 h to obtain graphene oxide;

[0050] Step S2: 1 g of graphene oxide and 55 mL of N,N-dimethylformamide were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at a temperature of 28 ° C and a stirring rate of 350 r / min for 25 min. Then, 4 g of isophorone diisocyanate was added and the stirring reaction was continued for 25 min. Then, the pH was adjusted to 9.5 with 22% ammonia water, and then the temperature was raised to 88 ° C and the stirring reaction was continued for 11 h. After the reaction was completed, the reaction product was cooled to room temperature and then centrifuged. The precipitate was washed with distilled water 4 times and then placed in a vacuum drying oven and dried at 62 ° C for 2.5 h to obtain modified graphene oxide;

[0051] Step S3: 10 g of hydrogen-containing silicone oil with an active hydrogen mass fraction of 0.07%, 1.8 g of allyl glycidyl ether, 0.04 g of Karstedt catalyst, and 22 mL of isopropanol were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at a temperature of 28° C. and a stirring rate of 350 r / min for 25 minutes. The temperature was then raised to 82° C. and the stirring reaction was continued for 3.5 hours. After the reaction was completed, the reaction product was cooled to room temperature, and then the solvent was removed by rotary evaporation to obtain epoxy polysiloxane;

[0052] Step S4: 10 g of epoxy polysiloxane, 1.7 g of triethanolamine, 3 g of acetic acid, and 45 mL of isopropanol were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at 28° C. and a stirring rate of 350 r / min for 25 min. The temperature was then raised to 68° C. and the stirring reaction was continued for 3.5 h. After the reaction was completed, the reaction product was cooled to room temperature, and the solvent was then removed by rotary evaporation to obtain a quaternary ammonium polysiloxane;

[0053] Step S5: Weigh 100 parts of PET resin, 1.2 parts of modified graphene oxide, 100 parts of PE resin, and 9 parts of quaternary ammonium polysiloxane according to weight and set aside; the model of the PET resin is Sinopec Yizheng FG600; the model of the PE resin is Sinochem Quanzhou Petrochemical HDPE5502;

[0054] Step S6: PET resin and modified graphene oxide are mixed evenly, and then added into a single-screw extruder I, and melt-extruded at a temperature of 265° C. to obtain a core layer melt;

[0055] Step S7: PE resin and quaternary ammonium polysiloxane are mixed evenly, and then added into a single-screw extruder II, and melt-extruded at a temperature of 240° C. to obtain a skin layer melt;

[0056] Step S8: The core layer melt and the skin layer melt are combined in a mass ratio of 3:7 and uniformly extruded through a core-skin composite spinning assembly, and then cooled, oiled and wound to obtain a soft modified composite staple fiber.

[0057] Example 3:

[0058] This embodiment is a method for producing a soft modified composite staple fiber, comprising the following steps:

[0059] Step S1: 1 g of graphite powder, 30 mL of 98% concentrated sulfuric acid, and 15 mL of 68% concentrated nitric acid were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at 0 ° C. and a stirring rate of 400 r / min for 30 min. Then, 6 g of potassium permanganate was added and the stirring reaction was continued for 1.5 h. Then, the temperature was raised to 40 ° C. and the stirring reaction was continued for 3 h. Then, the temperature was raised to 100 ° C. and the stirring reaction was continued for 8 h. After the reaction was completed, the reaction product was poured into ice water, and then 15 mL of 30% hydrogen peroxide was added. After centrifugation, the precipitate was washed 5 times with 15% hydrochloric acid solution and distilled water in sequence, and then placed in a vacuum drying oven and dried at a temperature of 55 ° C. for 4 h to obtain graphene oxide;

[0060] Step S2: 1 g of graphene oxide and 60 mL of N,N-dimethylformamide were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at a temperature of 30 ° C and a stirring rate of 400 r / min for 30 min. Then, 6 g of isophorone diisocyanate was added and the stirring reaction was continued for 30 min. Then, the pH was adjusted to 10 with 25% ammonia water, and then the temperature was raised to 90 ° C and the stirring reaction was continued for 12 h. After the reaction was completed, the reaction product was cooled to room temperature and then centrifuged. The precipitate was washed with distilled water 5 times and then placed in a vacuum drying oven and dried at 65 ° C for 3 h to obtain modified graphene oxide;

[0061] Step S3: 10 g of hydrogen-containing silicone oil with an active hydrogen mass fraction of 0.08%, 2.5 g of allyl glycidyl ether, 0.06 g of Karstedt catalyst, and 25 mL of isopropanol were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at a temperature of 30° C. and a stirring rate of 400 r / min for 30 minutes. The temperature was then raised to 85° C. and the stirring reaction was continued for 4 hours. After the reaction was completed, the reaction product was cooled to room temperature, and the solvent was then removed by rotary evaporation to obtain epoxy polysiloxane;

[0062] Step S4: 10 g of epoxy polysiloxane, 2.1 g of triethanolamine, 3.5 g of acetic acid, and 50 mL of isopropyl alcohol were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at 30° C. and a stirring rate of 400 r / min for 30 min. The temperature was then raised to 70° C. and the stirring reaction was continued for 4 h. After the reaction was completed, the reaction product was cooled to room temperature, and the solvent was then removed by rotary evaporation to obtain a quaternary ammonium polysiloxane;

[0063] Step S5: Weigh 100 parts of PET resin, 2.2 parts of modified graphene oxide, 100 parts of PE resin, and 15 parts of quaternary ammonium polysiloxane according to weight and set aside; the model of the PET resin is Sinopec Yizheng FG600; the model of the PE resin is Sinochem Quanzhou Petrochemical HDPE5502;

[0064] Step S6: PET resin and modified graphene oxide are mixed evenly, and then added into a single-screw extruder I, and melt-extruded at a temperature of 270° C. to obtain a core layer melt;

[0065] Step S7: PE resin and quaternary ammonium polysiloxane are mixed evenly, and then added into a single-screw extruder II, and melt-extruded at a temperature of 250° C. to obtain a skin layer melt;

[0066] Step S8: The core layer melt and the skin layer melt are combined in a mass ratio of 3:7 and uniformly extruded through a core-skin composite spinning assembly, and then cooled, oiled and wound to obtain a soft modified composite staple fiber.

[0067] Comparative Example 1:

[0068] This comparative example is a method for producing a soft modified composite staple fiber, comprising the following steps:

[0069] Step S1: Weigh 100 parts of PET resin and 100 parts of PE resin according to weight and set aside; the model of the PET resin is Sinopec Yizheng FG600; the model of the PE resin is Sinochem Quanzhou Petrochemical HDPE5502;

[0070] Step S2: The PET resin is mixed uniformly, and then added into a single-screw extruder I, and melt-extruded at a temperature of 210° C. to obtain a core layer melt;

[0071] Step S3: The PE resin is mixed uniformly, and then added into the single-screw extruder II, and melt-extruded at a temperature of 250° C. to obtain a skin layer melt;

[0072] Step S4: The core layer melt and the skin layer melt are combined in a mass ratio of 3:7 and uniformly extruded through a core-skin composite spinning assembly, and then cooled, oiled and wound to obtain a soft modified composite staple fiber.

[0073] Comparative Example 2:

[0074] This comparative example is a method for producing a soft modified composite staple fiber, comprising the following steps:

[0075] Step S1: 1 g of graphite powder, 30 mL of 98% concentrated sulfuric acid, and 15 mL of 68% concentrated nitric acid were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at 0 ° C. and a stirring rate of 400 r / min for 30 min. Then, 6 g of potassium permanganate was added and the stirring reaction was continued for 1.5 h. Then, the temperature was raised to 40 ° C. and the stirring reaction was continued for 3 h. Then, the temperature was raised to 100 ° C. and the stirring reaction was continued for 8 h. After the reaction was completed, the reaction product was poured into ice water, and then 15 mL of 30% hydrogen peroxide was added. After centrifugation, the precipitate was washed 5 times with 15% hydrochloric acid solution and distilled water in sequence, and then placed in a vacuum drying oven and dried at a temperature of 55 ° C. for 4 h to obtain graphene oxide;

[0076] Step S2: 1 g of graphene oxide and 60 mL of N,N-dimethylformamide were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at a temperature of 30 ° C and a stirring rate of 400 r / min for 30 min. Then, 6 g of isophorone diisocyanate was added and the stirring reaction was continued for 30 min. Then, the pH was adjusted to 10 with 25% ammonia water, and then the temperature was raised to 90 ° C and the stirring reaction was continued for 12 h. After the reaction was completed, the reaction product was cooled to room temperature and then centrifuged. The precipitate was washed with distilled water 5 times and then placed in a vacuum drying oven and dried at 65 ° C for 3 h to obtain modified graphene oxide;

[0077] Step S3: Weigh 100 parts of PET resin, 2.2 parts of modified graphene oxide, and 100 parts of PE resin according to weight and set aside; the model of the PET resin is Sinopec Yizheng FG600; the model of the PE resin is Sinochem Quanzhou Petrochemical HDPE5502;

[0078] Step S4: PET resin and modified graphene oxide are mixed evenly, and then added into a single-screw extruder I, and melt-extruded at a temperature of 210° C. to obtain a core layer melt;

[0079] Step S5: The PE resin is mixed evenly, and then added into the single-screw extruder II, and melt-extruded at a temperature of 250° C. to obtain a skin layer melt;

[0080] Step S6: The core layer melt and the skin layer melt are combined in a mass ratio of 3:7 and then uniformly extruded through a core-skin composite spinning assembly, and then cooled, oiled and wound to obtain a soft modified composite staple fiber.

[0081] Comparative Example 3:

[0082] This comparative example is a method for producing a soft modified composite staple fiber, comprising the following steps:

[0083] Step S1: 10 g of hydrogen-containing silicone oil with an active hydrogen mass fraction of 0.08%, 2.5 g of allyl alcohol glycidyl ether, 0.06 g of Karstedt catalyst, and 25 mL of isopropanol were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at a temperature of 30° C. and a stirring rate of 400 r / min for 30 minutes. The temperature was then raised to 85° C. and the stirring reaction was continued for 4 hours. After the reaction was completed, the reaction product was cooled to room temperature, and the solvent was then removed by rotary evaporation to obtain epoxy polysiloxane;

[0084] Step S2: 10 g of epoxy polysiloxane, 2.1 g of triethanolamine, 3.5 g of acetic acid, and 50 mL of isopropyl alcohol were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred at 30° C. and a stirring rate of 400 r / min for 30 min. The temperature was then raised to 70° C. and the stirring reaction was continued for 4 h. After the reaction was completed, the reaction product was cooled to room temperature, and the solvent was then removed by rotary evaporation to obtain a quaternary ammonium polysiloxane;

[0085] Step S3: Weigh 100 parts of PET resin, 100 parts of PE resin, and 15 parts of quaternary ammonium polysiloxane according to weight and set aside; the model of the PET resin is Sinopec Yizheng FG600; the model of the PE resin is Sinochem Quanzhou Petrochemical HDPE5502;

[0086] Step S4: The PET resin is mixed evenly, and then added into a single-screw extruder I, and melt-extruded at a temperature of 210° C. to obtain a core layer melt;

[0087] Step S5: PE resin and quaternary ammonium polysiloxane are mixed evenly, and then added into a single-screw extruder II, and melt-extruded at a temperature of 250° C. to obtain a skin layer melt;

[0088] Step S6: The core layer melt and the skin layer melt are combined in a mass ratio of 3:7 and then uniformly extruded through a core-skin composite spinning assembly, and then cooled, oiled and wound to obtain a soft modified composite staple fiber.

[0089] Comparative Example 4:

[0090] This comparative example is a method for producing a soft modified composite staple fiber, comprising the following steps:

[0091] Step S1: Weigh 100 parts of PET resin, 2.2 parts of graphene oxide, 100 parts of PE resin, and 15 parts of benzalkonium chloride according to weight and set aside; the model of the PET resin is Sinopec Yizheng FG600; the model of the PE resin is Sinochem Quanzhou Petrochemical HDPE5502;

[0092] Step S2: PET resin and graphene oxide are mixed evenly, and then added into a single-screw extruder I, and melt-extruded at a temperature of 210° C. to obtain a core layer melt;

[0093] Step S3: PE resin and benzalkonium chloride are mixed evenly, and then added into a single-screw extruder II, and melt-extruded at a temperature of 250° C. to obtain a skin layer melt;

[0094] Step S4: The core layer melt and the skin layer melt are combined in a mass ratio of 3:7 and uniformly extruded through a core-skin composite spinning assembly, and then cooled, oiled and wound to obtain a soft modified composite staple fiber.

[0095] The performance of the soft modified composite staple fibers of Examples 1-3 and Comparative Examples 1-4 was tested, and the test results are shown below:

[0096]

[0097] Referring to the data in the above table, according to the comparison between Examples 1-3 and Comparative Examples 1-4, it can be seen that the addition of modified graphene oxide gives the composite staple fibers excellent mechanical properties, and the addition of quaternary ammonium polysiloxane gives the composite staple fibers excellent antibacterial properties. Therefore, the composite staple fibers of the present application have excellent comprehensive performance.

[0098] Throughout this specification, references to terms such as "one embodiment," "example," or "specific example" indicate that the specific features, structures, materials, or characteristics described in conjunction with that embodiment or example are included in at least one embodiment or example of the present invention. In this specification, schematic representations of these terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.

[0099] The above contents are merely examples and explanations of the present invention. Those skilled in the art may make various modifications or additions to the described specific embodiments or replace them in similar ways. As long as they do not deviate from the invention or exceed the scope defined in this application, they should all fall within the scope of protection of the present invention.

Claims

1. A soft modified composite short fiber, characterized in that: Includes core layer and cortex; Wherein, the core layer comprises the following components in parts by weight: 100 parts of PET resin, 0.2-2.2 parts of modified graphene oxide; Wherein, the cortex comprises the following components in parts by weight: 100 parts of PE resin, 3-15 parts of quaternary ammonium polysiloxane; Wherein, the modified graphene oxide is prepared by the following steps: Step a1: adding graphite powder, concentrated sulfuric acid and concentrated nitric acid to a three-necked flask equipped with a stirrer and a thermometer, stirring at a temperature of -5-0°C and a stirring rate of 300-400 r / min for 20-30 min, then adding potassium permanganate and continuing to stir and react for 1-1.5 h, then heating to 35-40°C and continuing to stir and react for 2-3 h, then heating to 90-100°C and continuing to stir and react for 6-8 h, after the reaction is completed, pouring the reaction product into ice water, then adding hydrogen peroxide, and then centrifuging. The precipitate is washed with hydrochloric acid solution and distilled water 3-5 times in sequence, and then placed in a vacuum drying oven and dried at a temperature of 50-55°C for 3-4 h to obtain graphene oxide; Step a2: adding graphene oxide and N,N-dimethylformamide to a three-necked flask equipped with a stirrer and a thermometer, stirring at a temperature of 25-30°C and a stirring rate of 300-400 r / min for 20-30 minutes, then adding isophorone diisocyanate and continuing to stir and react for 20-30 minutes, then adjusting the pH to 9-10 with ammonia water, then heating to 85-90°C and continuing to stir and react for 10-12 hours, and after the reaction is completed, the reaction product is cooled to room temperature, then centrifuged, and the precipitate is washed with distilled water 3-5 times, and then placed in a vacuum drying oven and dried at a temperature of 60-65°C for 2-3 hours to obtain modified graphene oxide; The quaternary ammonium polysiloxane is prepared by the following steps: By reacting hydrogen-containing silicone oil with allyl alcohol glycidyl ether, Si-H on the hydrogen-containing silicone oil and the alkenyl on the allyl alcohol glycidyl ether undergo a silylation reaction to obtain epoxy polysiloxane, and then reacting the epoxy polysiloxane with triethanolamine to obtain quaternary ammonium polysiloxane.

2. The soft modified composite short fiber according to claim 1, characterized in that: The usage ratio of the graphite powder, concentrated sulfuric acid, concentrated nitric acid, potassium permanganate and hydrogen peroxide in step a1 is 1 g: 25-30 mL: 10-15 mL: 4-6 g: 10-15 mL.

3. The soft modified composite short fiber according to claim 1, characterized in that: The mass fraction of the concentrated sulfuric acid in step a1 is 96-98%, the mass fraction of the concentrated nitric acid is 66-68%, the mass fraction of the hydrogen peroxide is 25-30%, and the mass fraction of the hydrochloric acid solution is 10-15%.

4. The soft modified composite short fiber according to claim 1, characterized in that: The usage ratio of the graphene oxide, N,N-dimethylformamide and isophorone diisocyanate in step a2 is 1 g:50-60 mL:2-6 g.

5. The soft modified composite short fiber according to claim 1, characterized in that: The mass fraction of the ammonia water in step a2 is 20-25%.

6. The soft modified composite short fiber according to claim 1, characterized in that: The quaternary ammonium polysiloxane is prepared by the following steps: Step b1: adding hydrogen silicone oil, allyl alcohol glycidyl ether, Karstedt catalyst and isopropanol to a three-necked flask equipped with a stirrer and a thermometer, stirring at a temperature of 25-30° C. and a stirring rate of 300-400 r / min for 20-30 minutes, then heating to 80-85° C. and continuing stirring for 3-4 hours. After the reaction is completed, the reaction product is cooled to room temperature, and then the solvent is removed by rotary evaporation to obtain epoxy polysiloxane; Step b2: Add epoxy polysiloxane, triethanolamine, acetic acid and isopropyl alcohol to a three-necked flask equipped with a stirrer and a thermometer, stir at a temperature of 25-30°C and a stirring rate of 300-400 r / min for 20-30 minutes, then raise the temperature to 65-70°C and continue stirring for 3-4 hours. After the reaction is completed, the reaction product is cooled to room temperature, and then the solvent is removed by rotary evaporation to obtain quaternary ammonium polysiloxane.

7. The soft modified composite short fiber according to claim 6, characterized in that: The usage ratio of the hydrogenated silicone oil, allyl alcohol glycidyl ether, Karstedt catalyst and isopropyl alcohol in step b1 is 10 g: 1.1-2.5 g: 0.02-0.06 g: 20-25 mL.

8. The soft modified composite short fiber according to claim 6, characterized in that: The active hydrogen mass fraction of the hydrogen-containing silicone oil in step b1 is 0.06-0.08%.

9. The soft modified composite short fiber according to claim 6, characterized in that: The usage ratio of the epoxy polysiloxane, triethanolamine, acetic acid and isopropyl alcohol in step b2 is 10 g: 1.3-2.1 g: 2.5-3.5 g: 40-50 mL.

10. A method for producing the soft modified composite staple fiber according to any one of claims 1 to 9, characterized in that: The following steps are involved: Step 1: Weigh 100 parts of PET resin, 0.2-2.2 parts of modified graphene oxide, 100 parts of PE resin, and 3-15 parts of quaternary ammonium polysiloxane according to weight, and set aside; the model of the PET resin is Sinopec Yizheng FG600; the model of the PE resin is Sinochem Quanzhou Petrochemical HDPE5502; Step 2: PET resin and modified graphene oxide are mixed evenly, and then added into a single screw extruder I, and melt-extruded at a temperature of 260-270° C. to obtain a core layer melt; Step 3: PE resin and quaternary ammonium polysiloxane are mixed evenly, and then added into a single screw extruder II, and melt-extruded at a temperature of 230-250°C to obtain a skin layer melt; Step 4: The core layer melt and the skin layer melt are combined in a mass ratio of 3:7 and uniformly extruded through the skin-core composite spinning assembly. After cooling, oiling and winding, soft modified composite short fibers are obtained.

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