Soft modified composite short fiber and production method thereof

Abstract

The invention relates to the technical field of fiber materials, in particular to a soft modified composite short fiber and a production method thereof, which are used for solving the problem that the application of the existing composite short fiber in some scenes is limited due to poor softness, mechanical property and antibacterial property of the existing composite short fiber. According to the production method, PET resin is used as a core layer raw material of the composite short fiber, the composite short fiber is endowed with high strength and toughness, the mechanical property of the composite short fiber can be further improved after modified graphene oxide is added, PE resin is used as a skin layer raw material of the composite short fiber, and the composite short fiber is endowed with good flexibility and wear resistance. After the quaternary ammonium polysiloxane is added, the antibacterial property of the material can be greatly improved, and meanwhile, the flexibility of the material is further improved; the composite short fiber keeps soft and comfortable, has high mechanical properties and antibacterial properties, and is very suitable for manufacturing high-quality home textiles, clothes and other products, and the production method is simple in process, easy to operate and suitable for large-scale industrial production.

Description

Technical Field

[0001] The 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 has mechanical strength. Although they have their own advantages, a single material is difficult to meet the multifunctional needs 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 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, limiting 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 short 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 skin layer 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: Add graphite powder, concentrated sulfuric acid and concentrated nitric acid to a three-necked flask equipped with a stirrer and a thermometer, stir for 20-30 minutes at a temperature of -5-0°C and a stirring rate of 300-400r / min, then add potassium permanganate and continue stirring the reaction for 1-1.5 hours, then heat the temperature to 35-40°C and continue stirring the reaction for 2-3 hours, then heat the temperature to 90-100°C and continue stirring the reaction for 6-8 hours, pour the reaction product into ice water after the reaction is completed, then add hydrogen peroxide, then centrifuge, wash the precipitate with hydrochloric acid solution and distilled water for 3-5 times in sequence, then place it in a vacuum drying oven, and dry it at a temperature of 50-55°C for 3-4 hours 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 for 20-30 minutes at a temperature of 25-30°C and a stirring rate of 300-400r / min, then add isophorone diisocyanate and continue to stir and react for 20-30 minutes, then adjust the pH to 9-10 with ammonia water, then continue to stir and react for 10-12 hours at a temperature of 85-90°C, and after the reaction is completed, cool the reaction product to room temperature, then centrifuge, wash the precipitate with distilled water for 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 1g:25-30mL:10-15mL:4-6g:10-15mL.

[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 1g:50-60mL:2-6g.

[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 solution of the present invention: the quaternary ammonium polysiloxane is prepared by the following steps:

[0022] Step b1: Add hydrogen-containing silicone oil, allyl alcohol glycidyl ether, Karstedt catalyst and isopropanol into a three-necked flask equipped with a stirrer and a thermometer, stir for 20-30 minutes at a temperature of 25-30° C. and a stirring rate of 300-400 r / min, then heat to 80-85° 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 epoxy polysiloxane;

[0023] Step b2: Add epoxy polysiloxane, triethanolamine, acetic acid and isopropanol into a three-necked flask equipped with a stirrer and a thermometer, stir for 20-30 minutes at a temperature of 25-30°C and a stirring rate of 300-400 r / min, then heat 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 solution of the present invention: the usage ratio of the hydrogen-containing silicone oil, allyl alcohol glycidyl ether, Karstedt catalyst and isopropanol in step b1 is 10g:1.1-2.5g:0.02-0.06g:20-25mL.

[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 isopropanol in step b2 is 10g:1.3-2.1g:2.5-3.5g:40-50mL.

[0027] As a further solution of the present invention: a method for producing soft modified composite short 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: Mix the PE resin and the quaternary ammonium polysiloxane evenly, then add them into the single screw extruder II, and melt extrude them 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 soft modified composite staple fiber and the production method thereof are as follows: PET resin and modified graphene oxide are uniformly mixed, and then added to a single screw extruder I for melt extrusion to obtain a core layer melt; PE resin and quaternary ammonium polysiloxane are uniformly mixed, and then added to a single screw extruder II for melt extrusion to obtain a skin layer melt; the core layer melt and the skin layer melt are combined and uniformly extruded through a skin-core composite spinning assembly, and then cooled, oiled and wound 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, gives it higher strength and toughness, adds modified oxide Graphene can further improve its mechanical properties. PE resin is used as the cortex raw material of the composite short fiber, which gives it good softness and wear resistance. Adding quaternary ammonium polysiloxane thereto can greatly improve its antibacterial properties and further improve its softness. Therefore, the composite short 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 needs of modern society 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 short fibers, a modified graphene oxide is first prepared. First, graphite powder is used as a raw material to prepare graphene oxide, and then the graphene oxide is treated with isophorone diisocyanate, and organic matter is grafted onto the surface of the graphene oxide to encapsulate it, thereby improving its dispersibility, making it less likely to agglomerate and able to be evenly distributed in the matrix, and the introduced isocyanate groups enable it to be combined with the matrix in the form of chemical bonds, thereby greatly improving the mechanical properties of the composite short fibers;

[0035] In the process of preparing the soft modified composite staple fibers, a quaternary ammonium polysiloxane is also prepared. First, hydrogen-containing silicone oil and allyl alcohol glycidyl ether are reacted, and the SiH on the hydrogen-containing silicone oil reacts with the alkenyl on the allyl alcohol glycidyl ether to undergo a silylation reaction, and an epoxy group is introduced at the same time 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, thereby greatly improving 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 described embodiments 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 creative work are within the scope of protection of the present invention.

[0037] Embodiment 1:

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

[0039] Step S1: 1g of graphite powder, 25mL of concentrated sulfuric acid with a mass fraction of 96% and 10mL of concentrated nitric acid with a mass fraction of 66% are added to a three-necked flask equipped with a stirrer and a thermometer, and stirred for 20min at a temperature of -5°C and a stirring rate of 300r / min, then 4g of potassium permanganate is added and the stirring reaction is continued for 1h, then the temperature is raised to 35°C and the stirring reaction is continued for 2h, then the temperature is raised to 90°C and the stirring reaction is continued for 6h, and after the reaction is completed, the reaction product is poured into ice water, and then 10mL of hydrogen peroxide with a mass fraction of 25% is added, and then centrifuged, and the precipitate is washed 3 times with a hydrochloric acid solution with a mass fraction and distilled water in turn, and then placed in a vacuum drying oven and dried at a temperature of 50°C for 3h 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 for 20 min at a temperature of 25 ° C and a stirring rate of 300 r / min, and then 2 g of isophorone diisocyanate was added and the stirring reaction was continued for 20 min, and then the pH was adjusted to 9 with 20% ammonia water by mass, 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, and 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 for 20 min at a temperature of 25° C. and a stirring rate of 300 r / min, and then the temperature was raised to 80° C. and the stirring reaction was continued for 3 h. 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 for 20 min at a temperature of 25 ° C and a stirring rate of 300 r / min, and then the temperature was 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 then the solvent was removed by rotary evaporation to obtain quaternary ammonium polysiloxane;

[0043] Step S5: 100 parts of PET resin, 0.2 parts of modified graphene oxide, 100 parts of PE resin and 3 parts of quaternary ammonium polysiloxane are weighed in parts by weight for later use; 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 then uniformly extruded through a core-skin composite spinning assembly, and then cooled, oiled and wound to obtain soft modified composite staple fibers.

[0047] Embodiment 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 for 25 min at a temperature of -3 ° C and a stirring rate of 350 r / min, then 5 g of potassium permanganate was added and the stirring reaction was continued for 1.2 h, and then the temperature was raised to 38 ° C and the stirring reaction was continued for 2.5 h, and 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, and then centrifuged. The precipitate was washed 4 times with a hydrochloric acid solution and distilled water with a mass fraction, 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 for 25 min at a temperature of 28 ° C and a stirring rate of 350 r / min, and then 4 g of isophorone diisocyanate was added and the stirring reaction was continued for 25 min, and then the pH was adjusted to 9.5 with 22% ammonia water by mass, 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, and the precipitate was washed with distilled water 4 times, and then placed in a vacuum drying oven, and dried at a temperature of 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 alcohol 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 for 25 min at a temperature of 28° C. and a stirring rate of 350 r / min, and then the temperature was raised to 82° 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 then the solvent was removed by rotary evaporation to obtain epoxy polysiloxane;

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

[0053] Step S5: weighing 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 for standby use; 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 then uniformly extruded through a core-skin composite spinning assembly, and then cooled, oiled and wound to obtain soft modified composite staple fibers.

[0057] Embodiment 3:

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

[0059] Step S1: 1g of graphite powder, 30mL of concentrated sulfuric acid with a mass fraction of 98% and 15mL of concentrated nitric acid with a mass fraction of 68% are added to a three-necked flask equipped with a stirrer and a thermometer, and stirred for 30min at a temperature of 0°C and a stirring rate of 400r / min, then 6g of potassium permanganate is added and the stirring reaction is continued for 1.5h, then the temperature is raised to 40°C and the stirring reaction is continued for 3h, then the temperature is raised to 100°C and the stirring reaction is continued for 8h, and after the reaction is completed, the reaction product is poured into ice water, and then 15mL of hydrogen peroxide with a mass fraction of 30% is added, and then centrifuged, and the precipitate is washed 5 times with a hydrochloric acid solution with a mass fraction and distilled water in turn, and then placed in a vacuum drying oven and dried at a temperature of 55°C for 4h 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 for 30 min at a temperature of 30 ° C and a stirring rate of 400 r / min, and then 6 g of isophorone diisocyanate was added and the stirring reaction was continued for 30 min, and then the pH was adjusted to 10 with 25% ammonia water by mass, 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, and the precipitate was washed with distilled water 5 times, and then placed in a vacuum drying oven and dried at a temperature of 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 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 for 30 min at a temperature of 30° C. and a stirring rate of 400 r / min, and then the temperature was raised to 85° C. and the stirring reaction was continued for 4 h. 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;

[0062] Step S4: 10 g of epoxy polysiloxane, 2.1 g of triethanolamine, 3.5 g of acetic acid and 50 mL of isopropanol were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred for 30 min at a temperature of 30 ° C and a stirring rate of 400 r / min, and then the temperature was 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 then the solvent was removed by rotary evaporation to obtain quaternary ammonium polysiloxane;

[0063] Step S5: 100 parts of PET resin, 2.2 parts of modified graphene oxide, 100 parts of PE resin and 15 parts of quaternary ammonium polysiloxane are weighed in parts by weight for later use; 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 soft modified composite staple fibers.

[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 for standby use; 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 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;

[0071] Step S3: The PE resin is 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;

[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 soft modified composite short fibers.

[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: 1g of graphite powder, 30mL of concentrated sulfuric acid with a mass fraction of 98% and 15mL of concentrated nitric acid with a mass fraction of 68% are added to a three-necked flask equipped with a stirrer and a thermometer, and stirred for 30min at a temperature of 0°C and a stirring rate of 400r / min, then 6g of potassium permanganate is added and the stirring reaction is continued for 1.5h, then the temperature is raised to 40°C and the stirring reaction is continued for 3h, then the temperature is raised to 100°C and the stirring reaction is continued for 8h, and after the reaction is completed, the reaction product is poured into ice water, and then 15mL of hydrogen peroxide with a mass fraction of 30% is added, and then centrifuged, and the precipitate is washed 5 times with a hydrochloric acid solution with a mass fraction and distilled water in turn, and then placed in a vacuum drying oven and dried at a temperature of 55°C for 4h 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 for 30 min at a temperature of 30 ° C and a stirring rate of 400 r / min, and then 6 g of isophorone diisocyanate was added and the stirring reaction was continued for 30 min, and then the pH was adjusted to 10 with 25% ammonia water by mass, 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, and the precipitate was washed with distilled water 5 times, and then placed in a vacuum drying oven and dried at a temperature of 65 ° C for 3 h to obtain modified graphene oxide;

[0077] Step S3: weighing 100 parts of PET resin, 2.2 parts of modified graphene oxide and 100 parts of PE resin according to weight for standby use; 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 uniformly extruded through a core-skin composite spinning assembly, and then cooled, oiled and wound to obtain soft modified composite staple fibers.

[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 for 30 min at a temperature of 30° C. and a stirring rate of 400 r / min, and then the temperature was raised to 85° C. and the stirring reaction was continued for 4 h. 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;

[0084] Step S2: 10 g of epoxy polysiloxane, 2.1 g of triethanolamine, 3.5 g of acetic acid and 50 mL of isopropanol were added to a three-necked flask equipped with a stirrer and a thermometer, and stirred for 30 min at a temperature of 30 ° C and a stirring rate of 400 r / min, and then the temperature was 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 then the solvent was removed by rotary evaporation to obtain quaternary ammonium polysiloxane;

[0085] Step S3: weighing 100 parts of PET resin, 100 parts of PE resin and 15 parts of quaternary ammonium polysiloxane according to weight for standby use; 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 uniformly extruded through a core-skin composite spinning assembly, and then cooled, oiled and wound to obtain soft modified composite staple fibers.

[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 parts for standby use; 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 soft modified composite short fibers.

[0095] The soft modified composite short fibers of Examples 1-3 and Comparative Examples 1-4 were subjected to performance tests, and the test results are as follows:

[0096]

[0097] According to the data in the above table, based on 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 properties.

[0098] In the description of this specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.

[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 specific embodiments described or replace them in a similar manner. As long as they do not deviate from the invention or exceed the scope defined in this application, they shall all fall within the protection scope 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 skin layer 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: Add graphite powder, concentrated sulfuric acid and concentrated nitric acid to a three-necked flask equipped with a stirrer and a thermometer, stir for 20-30 minutes at a temperature of -5-0°C and a stirring rate of 300-400r / min, then add potassium permanganate and continue stirring the reaction for 1-1.5 hours, then heat the temperature to 35-40°C and continue stirring the reaction for 2-3 hours, then heat the temperature to 90-100°C and continue stirring the reaction for 6-8 hours, pour the reaction product into ice water after the reaction is completed, then add hydrogen peroxide, then centrifuge, wash the precipitate with hydrochloric acid solution and distilled water for 3-5 times in sequence, then place it in a vacuum drying oven, and dry it at a temperature of 50-55°C for 3-4 hours to obtain graphene oxide; Step a2: Add graphene oxide and N,N-dimethylformamide to a three-necked flask equipped with a stirrer and a thermometer, stir for 20-30 minutes at a temperature of 25-30°C and a stirring rate of 300-400r / min, then add isophorone diisocyanate and continue to stir and react for 20-30 minutes, then adjust the pH to 9-10 with ammonia water, then continue to stir and react for 10-12 hours at a temperature of 85-90°C, and after the reaction is completed, cool the reaction product to room temperature, then centrifuge, wash the precipitate with distilled water for 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.

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 1g:25-30mL:10-15mL:4-6g:10-15mL.

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 1g:50-60mL:2-6g.

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: Add hydrogen-containing silicone oil, allyl alcohol glycidyl ether, Karstedt catalyst and isopropanol into a three-necked flask equipped with a stirrer and a thermometer, stir for 20-30 minutes at a temperature of 25-30° C. and a stirring rate of 300-400 r / min, then heat to 80-85° 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 epoxy polysiloxane; Step b2: Add epoxy polysiloxane, triethanolamine, acetic acid and isopropanol into a three-necked flask equipped with a stirrer and a thermometer, stir for 20-30 minutes at a temperature of 25-30°C and a stirring rate of 300-400 r / min, then heat 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 hydrogen-containing 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.

8. The soft modified composite short fiber according to claim 6, characterized in that: The mass fraction of active hydrogen in 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 isopropanol in step b2 is 10g:1.3-2.1g:2.5-3.5g:40-50mL.

10. A method for producing soft modified composite short fibers, 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: Mix the PE resin and the quaternary ammonium polysiloxane evenly, then add them into the single screw extruder II, and melt extrude them 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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