Process for preparing regenerated antibacterial polyester from waste polyester material

Abstract

The invention relates to a process for preparing regenerated antibacterial polyester from a waste polyester material, and belongs to the technical field of polyester fiber processing. The invention provides a process for preparing regenerated antibacterial polyester from a waste polyester material. The process is summarized as follows: melting and pre-treating waste polyester bottle chips to obtain a base material A, dipping the base material A in a hydrophobic antibacterial finishing solution, treating to obtain a base material B, dipping the base material B in a hydrophobic nano antibacterial slurry, and treating to obtain the regenerated antibacterial polyester. The surface activity of the polyester fiber is improved through plasma treatment, on the basis, chitosan is introduced by means of hydrophobic antibacterial finishing liquid to achieve the antibacterial effect, meanwhile, a hydrophobic film is formed, finally, titanium dioxide is introduced by means of hydrophobic nano-antibacterial slurry to achieve the antibacterial effect in a synergistic mode, and meanwhile, a stable hydrophobic network structure is formed. In a sweating or humid environment, water is effectively repelled, bacterium breeding is prevented, and the antibacterial effect is synergistically achieved.

Description

Technical Field

[0001] The present invention belongs to the technical field of polyester fiber processing, and relates to a process for preparing regenerated antibacterial polyester fiber by using waste polyester materials. Background Art

[0002] Waste polyester materials mainly refer to waste polyester products such as poly(ethylene terephthalate) (PET). They are widely sourced. In practical applications, various ways of recycling waste polyester materials have been formed. Among them, the preparation of regenerated polyester fiber from waste polyester bottle chips has made great progress in both research and application. However, polyester fiber itself has poor air permeability. Regenerated polyester fiber is more likely to feel stuffy when worn due to the increase in surface groove structure, and hot air and sweat cannot be discharged, which is likely to breed and attach bacteria. Secondly, the acidic substances produced by microbial metabolism will accelerate the breakage of PET molecular chains, thereby affecting the service life of regenerated polyester fiber. Therefore, the antibacterial research on regenerated polyester fiber is very necessary. Summary of the Invention

[0003] The purpose of the present invention is to provide a process for preparing regenerated antibacterial polyester fiber by using waste polyester materials. The present invention improves the surface activity of polyester fiber through plasma treatment. On this basis, chitosan is introduced by means of a hydrophobic antibacterial finishing solution to exert antibacterial effects, and at the same time, a hydrophobic film is formed. Finally, titanium dioxide is introduced by means of a hydrophobic nano-antibacterial slurry to synergistically exert antibacterial effects, and at the same time, a stable hydrophobic network structure is formed, which can effectively repel water in case of sweating or in a humid environment, prevent the growth of bacteria, and synergistically exert antibacterial effects.

[0004] The purpose of the present invention can be achieved by the following technical solutions:

[0005] A process for preparing regenerated antibacterial polyester fiber by using waste polyester materials, the process comprising the following steps:

[0006] Step 1: After cleaning waste polyester bottle chips with water at 60°C, drying them at 60°C until the water content is lower than 0.5 wt%, melting and spinning, cooling, and performing plasma treatment to obtain base material A;

[0007] Step 2: Immerse base material A in a hydrophobic antibacterial finishing solution, control the temperature and stir, take it out and drain, and dry it at a low temperature to obtain base material B;

[0008] Step 3: Immerse base material B in a hydrophobic nano-antibacterial slurry, stir and process, take it out and drain, and cure it at a low temperature to obtain the product.

[0009] Further, in Step 1, the melting temperature is 260 - 280°C; the operation of the plasma treatment is as follows: under argon conditions, set the treatment power to 100 - 200 W, the gas flow rate to 20 - 30 sccm, and the treatment time to 2 - 3 min.

[0010] Further, the impregnation bath ratio of the base material A to the hydrophobic antibacterial finishing solution in step two is 1:3 - 5, the impregnation temperature is 30 - 40°C, and the impregnation time is 30 - 50 min; the temperature-controlled stirring is carried out at a speed of 100 - 140 rpm at 35 - 40°C; the temperature of the low-temperature drying is 60 - 70°C.

[0011] Further, the preparation method of the hydrophobic antibacterial finishing solution in step two includes the following steps:

[0012] Step X1: Control the stirring speed at 300 - 500 rpm, dissolve chitosan in deionized water to prepare a chitosan solution with a mass concentration of 2 - 3 wt%, after stirring evenly, add sodium lignosulfonate accounting for 8 - 12 wt% of the mass of chitosan, after stirring evenly, add cetyltrimethylammonium chloride accounting for 7.5 - 8.5 wt% of the mass of chitosan, and continue to stir evenly to obtain a basic solution;

[0013] Step X2: Mix 4 - 5 parts by weight of octamethylcyclotetrasiloxane, 0.5 - 0.6 parts by weight of vinyltriethoxysilane, 0.2 - 0.3 parts by weight of octylphenol polyoxyethylene ether and 8 - 12 parts by weight of deionized water, stir evenly at a speed of 200 - 400 rpm, then add 0.03 - 0.05 parts by weight of potassium persulfate, heat up to 75 - 85°C and treat for 4 - 6 h, during which the stirring speed is 150 - 250 rpm, and cool to room temperature to obtain a modified silicone emulsion;

[0014] Step X3: Heat 2.8 - 3.2 parts by weight of paraffin until melted, add 0.2 - 0.3 parts by weight of span 80 and 0.3 - 0.4 parts by weight of tween 80, stir evenly at a speed of 300 - 400 rpm, then add 10 - 12 parts by weight of deionized water and 0.01 - 0.02 parts by weight of sodium hydroxide, stir at 60 - 70°C for 1 - 2 h, and cool to room temperature to obtain a microemulsified paraffin emulsion;

[0015] Step X4: Control the stirring speed at 100 - 200 rpm, add the modified silicone emulsion, microemulsified paraffin emulsion, γ-aminopropyltriethoxysilane and aziridine crosslinking agent to the basic solution, perform ultrasonic treatment, add citric acid buffer solution dropwise to adjust the pH, and continue to stir for 2 - 3 h to obtain the product.

[0016] Further, the dosage of the modified silicone emulsion in step X4 accounts for 11 - 13 wt% of the mass of the basic solution; the dosage of the microemulsified paraffin emulsion accounts for 5 - 7 wt% of the mass of the basic solution; the dosage of γ-aminopropyltriethoxysilane accounts for 1.5 - 2.5 wt% of the mass of the basic solution; the dosage of the aziridine crosslinking agent accounts for 0.4 - 0.6 wt% of the mass of the hydrophobic antibacterial finishing solution.

[0017] Further, the parameters of the ultrasonic treatment in step X4 are as follows: the ultrasonic frequency is 30 - 40 kHz, the ultrasonic power is 100 - 200 W, and the ultrasonic time is 5 - 7 min; the citric acid buffer solution is a 0.1 - 0.2 mol / L citric acid buffer solution; and the pH is 5.5 - 6.5.

[0018] Further, the impregnation bath ratio of the base material B to the hydrophobic nano - ceramic antibacterial slurry in step three is 1:2 - 3, the impregnation temperature is 40 - 50 °C, and the impregnation time is 20 - 30 min; the rotation speed of the stirring is 20 - 30 rpm; the temperature and curing time of the low - temperature curing are 80 - 90 °C and 30 - 40 min, respectively.

[0019] Further, the preparation method of the hydrophobic nano - antibacterial slurry in step three comprises the following steps:

[0020] Step Y1: Mix 2 - 3 parts by weight of titanium dioxide with an average particle size of 20 nm, 0.04 - 0.06 parts by weight of sodium polyacrylate, 0.02 - 0.03 parts by weight of polyvinylpyrrolidone, and 10 - 16 parts by weight of deionized water, stir at a speed of 500 - 600 rpm for 10 - 20 min, then add 2.6 - 3 parts by weight of water - borne polyurethane, and continue to stir at the same speed for 20 - 30 min to obtain the slurry.

[0021] Further, the regenerated antibacterial polyester is a staple fiber.

[0022] Advantages of the present invention:

[0023] (1) By plasma treatment, active groups are generated on the surface of the polyester fiber, which can interact or adsorb with amino groups, hydroxyl groups and other groups in the chitosan molecule, increasing the chitosan loading amount and thus improving the antibacterial effect; in addition, the binding ability of the plasma - treated polyester fiber with the modified silicone emulsion and the micro - emulsified paraffin emulsion is improved, which helps to form a uniform and continuous hydrophobic film, effectively repelling water in case of sweating or humidity, preventing bacteria from growing, and exerting an antibacterial effect.

[0024] (2) In the hydrophobic antibacterial finishing solution of the present invention, chitosan and a part of titanium dioxide in the hydrophobic nano antibacterial slurry approach each other through electrostatic attraction, improving the adhesion of titanium dioxide and synergistically antibacterial. In addition, titanium dioxide will produce a photocatalytic effect under light to achieve the effect of killing bacteria; the amino group of γ-aminopropyltriethoxysilane, sodium polyacrylate, polyvinylpyrrolidone, etc. in the hydrophobic nano ceramic antibacterial slurry interact with each other, making the components in the hydrophobic nano antibacterial slurry interweave with each other. And the waterborne polyurethane fuses and penetrates with the hydrophobic layer formed on the surface of base material A during the treatment process. The aziridine crosslinking agent interacts with various components such as the amino group of chitosan and the hydroxyl group of waterborne polyurethane to further form a stable network structure, enabling the antibacterial components to stably adhere to the polyester fiber, while enhancing the hydrophobicity and synergistically exerting a stable antibacterial effect. Detailed implementation manners

[0025] To further illustrate the technical means and effects adopted by the present invention to achieve the predetermined invention purpose, the following combines examples to elaborate in detail on the specific implementation manners, structures, features and their effects of the present invention.

[0026] All the waste polyester bottle chips in the examples and comparative examples of the present invention are from Guangdong Yuanhui Environmental Protection Fiber Co., Ltd.; all the chitosan is directly purchased from the market and is purchased from Lanzhou Woteles Biotechnology Co., Ltd.; all the sodium lignosulfonate is directly purchased from the market and is purchased from Shanghai Macklin Biochemical Co., Ltd.; all cetyltrimethylammonium chloride, octamethylcyclotetrasiloxane, vinyltriethoxysilane, potassium persulfate, paraffin, sodium hydroxide, γ-aminopropyltriethoxysilane, sodium polyacrylate, polyvinylpyrrolidone are directly purchased from the market and are purchased from Sigma-Aldrich (Shanghai) Trading Co., Ltd.; all octylphenol polyoxyethylene ether is directly purchased from the market and is purchased from Nantong Chenrun Chemical Co., Ltd.; all Span 80 and Tween 80 are directly purchased from the market and are purchased from Shanghai Yuanye Bio-Technology Co., Ltd.; all aziridine crosslinking agents are directly purchased from the market and are purchased from Shanghai Haodeng Materials Co., Ltd.; all citrate buffer solutions are directly purchased from the market and are purchased from Thermo Fisher Scientific (China) Co., Ltd.; all titanium dioxide is directly purchased from the market and is purchased from Jiangsu Tianxing New Materials Co., Ltd.; all waterborne polyurethanes are directly purchased from the market and are purchased from Qingdao Ricos New Materials Technology Co., Ltd.

[0027] Example 1

[0028] A process for preparing regenerated antibacterial polyester from waste polyester materials. The process of this example includes the following steps:

[0029] Step 1: Clean the waste polyester bottle chips with water at 60°C, dry them at 60°C until the moisture content is lower than 0.5 wt%, melt-spin them, cool them, and perform plasma treatment to obtain base material A;

[0030] Step 2: Immerse base material A in a hydrophobic antibacterial finishing solution, control the temperature and stir, take it out and drain, and dry it at a low temperature to obtain base material B;

[0031] Step 3: Immerse base material B in a hydrophobic nano-antibacterial slurry, stir and process, take it out and drain, and cure it at a low temperature to obtain the product.

[0032] In Step 1 of this example, the melting temperature is 260°C; the operation of plasma treatment is as follows: under argon gas conditions, set the treatment power to 100 W, the gas flow rate to 20 sccm, and the treatment time to 2 min.

[0033] In Step 2 of this example, the immersion bath ratio of base material A to the hydrophobic antibacterial finishing solution is 1:3, the immersion temperature is 30°C, and the immersion time is 30 min; controlling the temperature and stirring means stirring at a speed of 100 rpm at 35°C; the temperature for low-temperature drying is 60°C.

[0034] The preparation method of the hydrophobic antibacterial finishing solution in Step 2 of this example includes the following steps:

[0035] Step X1: Control the stirring speed to 300 rpm, dissolve chitosan in deionized water to prepare a chitosan solution with a mass concentration of 2 wt%, add sodium lignosulfonate accounting for 8 wt% of the mass of chitosan after stirring evenly, and add cetyltrimethylammonium chloride accounting for 7.5 wt% of the mass of chitosan, and continue to stir evenly to obtain a basic solution;

[0036] Step X2: Mix 4 parts by weight of octamethylcyclotetrasiloxane, 0.5 part by weight of vinyltriethoxysilane, 0.2 part by weight of octylphenol polyoxyethylene ether and 8 parts by weight of deionized water, stir evenly at a speed of 200 rpm, then add 0.03 part by weight of potassium persulfate, heat up to 75°C and treat for 4 h, with the stirring speed being 150 rpm during this period, and cool to room temperature to obtain a modified silicone emulsion;

[0037] Step X3: Heat and melt 2.8 parts by weight of paraffin wax, add 0.2 part by weight of Span 80 and 0.3 part by weight of Tween 80, stir evenly at a speed of 300 rpm, then add 10 parts by weight of deionized water and 0.01 part by weight of sodium hydroxide, stir at 60°C for 1 h, and cool to room temperature to obtain a microemulsified paraffin wax emulsion;

[0038] Step X4: Control the stirring speed at 100 rpm, add modified silicone emulsion, microemulsified paraffin emulsion, γ-aminopropyltriethoxysilane and aziridine crosslinker to the base solution, perform ultrasonic treatment, add citric acid buffer solution dropwise to adjust the pH, and continue stirring for 2 h to obtain the product.

[0039] In step X4 of this example, the dosage of the modified silicone emulsion accounts for 11 wt% of the mass of the base solution; the dosage of the microemulsified paraffin emulsion accounts for 5 wt% of the mass of the base solution; the dosage of γ-aminopropyltriethoxysilane accounts for 1.5 wt% of the mass of the base solution; the dosage of the aziridine crosslinker accounts for 0.4 wt% of the mass of the hydrophobic antibacterial finishing solution.

[0040] The parameters of the ultrasonic treatment in step X4 of this example are: ultrasonic frequency is 30 kHz, ultrasonic power is 100 W, ultrasonic time is 5 min; the citric acid buffer solution is 0.1 mol / L citric acid buffer solution; the pH is 5.5.

[0041] In step three of this example, the dipping bath ratio of the base material B to the hydrophobic nano-ceramic antibacterial slurry is 1:2, the dipping temperature is 40 °C, the dipping time is 20 min; the stirring speed is 20 rpm; the temperature and curing time of low-temperature curing are 80 °C and 30 min respectively.

[0042] The preparation method of the hydrophobic nano-antibacterial slurry in step three of this example includes the following steps:

[0043] Step Y1: Mix 2 - 3 parts by weight of titanium dioxide with an average particle size of 20 nm, 0.04 part by weight of sodium polyacrylate, 0.02 part by weight of polyvinylpyrrolidone and 10 parts by weight of deionized water, stir at a speed of 500 rpm for 10 min, then add 2.6 parts by weight of waterborne polyurethane, and continue stirring at the same speed for 20 min to obtain the product.

[0044] The regenerated antibacterial polyester of this example is short fiber.

[0045] Example 2

[0046] A process for preparing regenerated antibacterial polyester from waste polyester materials. The process of this example includes the following steps:

[0047] Step one: Wash the waste polyester bottle chips with 60 °C water, dry them at 60 °C until the water content is lower than 0.5 wt%, melt-spin them, cool, and perform plasma treatment to obtain base material A;

[0048] Step two: Immerse the base material A in the hydrophobic antibacterial finishing solution, control the temperature and stir, take it out and drain, and dry it at low temperature to obtain base material B;

[0049] Step 3: Immerse the base material B in the hydrophobic nano antibacterial slurry, stir it, take it out and drain, and cure it at a low temperature to obtain the product.

[0050] In Step 1 of this embodiment, the melting temperature is 280 °C; the operation of plasma treatment is as follows: under the condition of argon gas, set the treatment power to 200 W, the gas flow rate to 30 sccm, and the treatment time to 3 min.

[0051] In Step 2 of this embodiment, the immersion bath ratio of the base material A to the hydrophobic antibacterial finishing liquid is 1:5, the immersion temperature is 40 °C, and the immersion time is 50 min; temperature-controlled stirring means stirring at a speed of 140 rpm at 40 °C; the temperature of low-temperature drying is 70 °C.

[0052] The preparation method of the hydrophobic antibacterial finishing liquid in Step 2 of this embodiment includes the following steps:

[0053] Step X1: Control the stirring speed to 500 rpm, dissolve chitosan in deionized water to prepare a chitosan solution with a mass concentration of 3 wt%, after stirring evenly, add sodium lignosulfonate accounting for 12 wt% of the mass of chitosan, and after stirring evenly, add cetyltrimethylammonium chloride accounting for 8.5 wt% of the mass of chitosan, and continue to stir evenly to obtain a basic solution;

[0054] Step X2: Mix 5 parts by weight of octamethylcyclotetrasiloxane, 0.6 parts by weight of vinyltriethoxysilane, 0.3 parts by weight of octylphenol polyoxyethylene ether and 12 parts by weight of deionized water, stir evenly at a speed of 400 rpm, then add 0.05 parts by weight of potassium persulfate, heat up to 85 °C and treat for 6 h, during which the stirring speed is 250 rpm, and cool to room temperature to obtain a modified silicone emulsion;

[0055] Step X3: Heat 3.2 parts by weight of paraffin to melt, add 0.3 parts by weight of Span 80 and 0.4 parts by weight of Tween 80, stir evenly at a speed of 400 rpm, then add 12 parts by weight of deionized water and 0.02 parts by weight of sodium hydroxide, stir at 70 °C for 2 h, and cool to room temperature to obtain a microemulsified paraffin emulsion;

[0056] Step X4: Control the stirring speed to 200 rpm, add the modified silicone emulsion, microemulsified paraffin emulsion, γ-aminopropyltriethoxysilane and aziridine crosslinking agent to the basic solution, perform ultrasonic treatment, dropwise add a citric acid buffer solution to adjust the pH, and continue to stir for 2 - 3 h to obtain the product.

[0057] In this embodiment, the dosage of the modified silicone emulsion in step X4 accounts for 13 wt% of the mass of the base solution; the dosage of the microemulsified paraffin emulsion accounts for 7 wt% of the mass of the base solution; the dosage of γ-aminopropyltriethoxysilane accounts for 2.5 wt% of the mass of the base solution; the dosage of the aziridine crosslinking agent accounts for 0.6 wt% of the mass of the hydrophobic antibacterial finishing solution.

[0058] The parameters of the ultrasonic treatment in step X4 of this embodiment are as follows: the ultrasonic frequency is 40 kHz, the ultrasonic power is 200 W, and the ultrasonic time is 7 min; the citric acid buffer solution is a 0.2 mol / L citric acid buffer solution; the pH is 6.5.

[0059] In step three of this embodiment, the impregnation bath ratio of the base material B to the hydrophobic nano-ceramic antibacterial slurry is 1:3, the impregnation temperature is 50 °C, and the impregnation time is 30 min; the stirring speed is 30 rpm; the temperature and curing time of the low-temperature curing are 90 °C and 40 min, respectively.

[0060] The preparation method of the hydrophobic nano-antibacterial slurry in step three of this embodiment includes the following steps:

[0061] Step Y1: Mix 3 parts by weight of titanium dioxide with an average particle size of 20 nm, 0.06 parts by weight of sodium polyacrylate, 0.03 parts by weight of polyvinylpyrrolidone, and 16 parts by weight of deionized water, stir at a speed of 600 rpm for 20 min, then add 3 parts by weight of waterborne polyurethane, and continue to stir at the same speed for 30 min to obtain.

[0062] The regenerated antibacterial polyester of this embodiment is short fiber.

[0063] Example 3

[0064] A process for preparing regenerated antibacterial polyester using waste polyester materials. The process of this embodiment includes the following steps:

[0065] Step one: After cleaning the waste polyester bottle chips with 60 °C water, dry them at 60 °C until the water content is lower than 0.5 wt%, melt-spin, cool, and perform plasma treatment to obtain the base material A;

[0066] Step two: Immerse the base material A in the hydrophobic antibacterial finishing solution, control the temperature and stir, take it out and drain, and dry it at low temperature to obtain the base material B;

[0067] Step three: Immerse the base material B in the hydrophobic nano-antibacterial slurry, stir and process, take it out and drain, and cure it at low temperature to obtain.

[0068] In step one of this embodiment, the melting temperature is 270 °C; the operation of the plasma treatment is as follows: under argon gas conditions, set the treatment power to 150 W, the gas flow rate to 25 sccm, and the treatment time to 2.5 min.

[0069] In step two of this embodiment, the impregnation bath ratio of base material A to the hydrophobic antibacterial finishing solution is 1:4, the impregnation temperature is 35 °C, and the impregnation time is 40 min; temperature-controlled stirring means stirring at a speed of 120 rpm at 37.5 °C; the temperature for low-temperature drying is 65 °C.

[0070] The preparation method of the hydrophobic antibacterial finishing solution in step two of this embodiment includes the following steps:

[0071] Step X1: Control the stirring speed to 400 rpm, dissolve chitosan in deionized water to prepare a chitosan solution with a mass concentration of 2.5 wt%, after stirring evenly, add sodium lignosulfonate accounting for 10 wt% of the mass of chitosan, after stirring evenly, add cetyltrimethylammonium chloride accounting for 8 wt% of the mass of chitosan, and continue to stir evenly to obtain a basic solution;

[0072] Step X2: Mix 4.5 parts by weight of octamethylcyclotetrasiloxane, 0.55 parts by weight of vinyltriethoxysilane, 0.25 parts by weight of octylphenol polyoxyethylene ether and 10 parts by weight of deionized water, stir evenly at a speed of 300 rpm, then add 0.04 parts by weight of potassium persulfate, heat up to 80 °C and treat for 5 h, during which the stirring speed is 200 rpm, and cool to room temperature to obtain a modified silicone emulsion;

[0073] Step X3: Heat 3 parts by weight of paraffin to melt it, add 0.25 parts by weight of Span 80 and 0.35 parts by weight of Tween 80, stir evenly at a speed of 350 rpm, then add 11 parts by weight of deionized water and 0.015 parts by weight of sodium hydroxide, stir at 65 °C for 1.5 h, and cool to room temperature to obtain a microemulsified paraffin emulsion;

[0074] Step X4: Control the stirring speed to 150 rpm, add the modified silicone emulsion, microemulsified paraffin emulsion, γ-aminopropyltriethoxysilane and aziridine crosslinking agent to the basic solution, perform ultrasonic treatment, dropwise add a citric acid buffer solution to adjust the pH, and continue to stir for 2.5 h to obtain it.

[0075] In step X4 of this embodiment, the dosage of the modified silicone emulsion accounts for 12 wt% of the mass of the basic solution; the dosage of the microemulsified paraffin emulsion accounts for 6 wt% of the mass of the basic solution; the dosage of γ-aminopropyltriethoxysilane accounts for 2 wt% of the mass of the basic solution; the dosage of the aziridine crosslinking agent accounts for 0.5 wt% of the mass of the hydrophobic antibacterial finishing solution.

[0076] The parameters of the ultrasonic treatment in step X4 of this embodiment are: the ultrasonic frequency is 35 kHz, the ultrasonic power is 150 W, and the ultrasonic time is 6 min; the citric acid buffer solution is a 0.15 mol / L citric acid buffer solution; the pH is 6.

[0077] In step three of this embodiment, the impregnation bath ratio of base material B to the hydrophobic nano-ceramic antibacterial slurry is 1:2.5, the impregnation temperature is 45 °C, and the impregnation time is 25 min; the stirring speed is 25 rpm; the temperature and curing time for low-temperature curing are 85 °C and 35 min, respectively.

[0078] The preparation method of the hydrophobic nano-antibacterial slurry in step three of this embodiment includes the following steps:

[0079] Step Y1: Mix 2.5 parts by weight of titanium dioxide with an average particle size of 20 nm, 0.05 parts by weight of sodium polyacrylate, 0.025 parts by weight of polyvinylpyrrolidone, and 13 parts by weight of deionized water, stir at a speed of 550 rpm for 15 min, then add 2.8 parts by weight of waterborne polyurethane, and continue to stir at the same speed for 25 min to obtain the slurry.

[0080] The regenerated antibacterial polyester of this embodiment is short fiber.

[0081] Comparative Example 1

[0082] Based on Example 3, the plasma treatment in step one is removed, and other conditions are the same as those in Example 3.

[0083] Comparative Example 2

[0084] Based on Example 3, the plasma treatment time in step one is extended to 5 min, and other conditions are the same as those in Example 3.

[0085] Comparative Example 3

[0086] Based on Example 3, while keeping other conditions the same, the process for preparing the regenerated antibacterial polyester using waste polyester materials is changed to the following steps:

[0087] Step one: Wash the waste polyester bottle chips with 60 °C water, dry them at 60 °C until the water content is less than 0.5 wt%, melt-spin them, cool them, and perform plasma treatment to obtain base material A;

[0088] Step two: Immerse base material A in the hydrophobic nano-antibacterial slurry, stir and process it, take it out and drain it, and perform low-temperature curing to obtain the product.

[0089] Comparative Example 4

[0090] Based on Example 3, the modified silicone emulsion in the hydrophobic antibacterial finishing liquid is removed and replaced with an equal weight of microemulsified paraffin emulsion, and other conditions are the same as those in Example 3.

[0091] Comparative Example 5

[0092] Based on Example 3, the microemulsified paraffin emulsion in the hydrophobic antibacterial finishing solution was removed and replaced with an equal weight of modified silicone emulsion, and other conditions were kept the same as those in Example 3.

[0093] Comparative Example 6

[0094] Based on Example 3, while keeping other conditions the same, the process for preparing regenerated antibacterial polyester using waste polyester materials was changed to the following steps:

[0095] Step 1: After cleaning the waste polyester bottle chips with 60°C water, drying them at 60°C until the water content is lower than 0.5 wt%, melt-spinning, cooling, and performing plasma treatment to obtain base material A;

[0096] Step 2: Immerse base material A in the hydrophobic antibacterial finishing solution, control the temperature and stir, take it out and drain, and dry it at a low temperature to obtain the product.

[0097] Comparative Example 7

[0098] Based on Example 3, the aqueous polyurethane in Step Y1 was removed and replaced with an equal weight of deionized water, and other conditions were kept the same as those in Example 3.

[0099] Taking the regenerated antibacterial polyester prepared in Examples 1 - 3 and Comparative Examples 1 - 7 as samples, testing was carried out in accordance with GB / T31713 - 2015 "Hygiene Requirements for the Safety of Antibacterial Textiles" and GB / T20944.3 - 2008 "Evaluation of Antibacterial Properties of Textiles - Part 3: Oscillation Method". Using Staphylococcus aureus numbered ATCC29213, the antibacterial properties were detected before washing and after 50 washes, and the test results are recorded in Table 1 below.

[0100] Table 1

[0101]

[0102] As can be seen from Table 1, the regenerated polyester prepared from waste polyester materials in Examples 1 - 3 of the present invention has good antibacterial effects.

[0103] The above are only the preferred embodiments of the present invention, and do not impose any form of limitation on the present invention. Although the present invention has been disclosed above with preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some changes or modifications to the above-disclosed technical content to form equivalent embodiments with equivalent changes, but as long as they do not depart from the technical content of the present invention, any indirect modifications, equivalent changes, and modifications made to the above embodiments based on the technical essence of the present invention still fall within the scope of the technical solution of the present invention.

Claims

1. A process for preparing regenerated antibacterial polyester using waste polyester materials, characterized in that: The process comprises the following steps: Step 1: After washing the waste polyester bottle flakes with 60°C water, drying at 60°C until the moisture content is less than 0.5wt%, melt spinning, cooling, and plasma treatment to obtain base material A; Step 2: immersing base material A in a hydrophobic antibacterial finishing liquid, stirring under controlled temperature, taking out, draining, and drying at low temperature to obtain base material B; Step 3: immerse the base material B in the hydrophobic nano antibacterial slurry, stir it, take it out and drain it, and cure it at low temperature to obtain the product.

2. The process for preparing regenerated antibacterial polyester using waste polyester materials according to claim 1, characterized in that: The melting temperature in step 1 is 260-280°C; the operation of the plasma treatment is to set the treatment power to 100-200W, the gas flow rate to 20-30sccm, and the treatment time to 2-3min under argon conditions.

3. The process for preparing regenerated antibacterial polyester using waste polyester materials according to claim 1, characterized in that: Step 2: The immersion bath ratio of the base material A to the hydrophobic antibacterial finishing liquid is 1:3-5, the immersion temperature is 30-40°C, and the immersion time is 30-50min; the temperature-controlled stirring is stirring at 35-40°C and 100-140rpm; the low-temperature drying temperature is 60-70°C.

4. The process for preparing regenerated antibacterial polyester from waste polyester materials according to claim 1, characterized in that: The preparation method of the hydrophobic antibacterial finishing liquid in step 2 comprises the following steps: Step X1, controlling the stirring speed to 300-500 rpm, dissolving chitosan in deionized water to prepare a chitosan solution with a mass concentration of 2-3 wt%, stirring evenly, adding 8-12 wt % of sodium lignin sulfonate based on the mass of chitosan, stirring evenly, adding 7.5-8.5 wt % of hexadecyltrimethylammonium chloride based on the mass of chitosan, and continuing to stir evenly to obtain a basic solution; Step X2, 4-5 parts by weight of octamethylcyclotetrasiloxane, 0.5-0.6 parts by weight of vinyltriethoxysilane, 0.2-0.3 parts by weight of octylphenol polyoxyethylene ether and 8-12 parts by weight of deionized water are mixed, stirred at a speed of 200-400 rpm, and then 0.03-0.05 parts by weight of potassium persulfate are added, the temperature is raised to 75-85° C. for 4-6 hours, the stirring speed is 150-250 rpm, and the mixture is cooled to room temperature to obtain a modified silicone emulsion; Step X3, after heating and melting 2.8-3.2 parts by weight of paraffin wax, add 0.2-0.3 parts by weight of Span 80 and 0.3-0.4 parts by weight of Tween 80, stir evenly at 300-400 rpm, add 10-12 parts by weight of deionized water and 0.01-0.02 parts by weight of sodium hydroxide, stir at 60-70° C. for 1-2 hours, and cool to room temperature to obtain a microemulsified paraffin wax emulsion; Step X4, control the stirring speed to 100-200 rpm, add modified silicone emulsion, microemulsified paraffin emulsion, γ-aminopropyltriethoxysilane and aziridine crosslinker to the base solution, ultrasonically treat, add citric acid buffer dropwise to adjust the pH, and continue stirring for 2-3 hours to obtain.

5. The process for preparing regenerated antibacterial polyester using waste polyester materials according to claim 4, characterized in that: The amount of the modified silicone emulsion in step X4 is 11-13wt% of the mass of the base solution; the amount of the microemulsified paraffin emulsion is 5-7wt% of the mass of the base solution; the amount of the γ-aminopropyltriethoxysilane is 1.5-2.5wt% of the mass of the base solution; the amount of the aziridine crosslinker is 0.4-0.6wt% of the mass of the hydrophobic antibacterial finishing liquid.

6. The process for preparing regenerated antibacterial polyester from waste polyester materials according to claim 4, characterized in that: The parameters of the ultrasonic treatment in step X4 are: ultrasonic frequency is 30-40kHz, ultrasonic power is 100-200W, and ultrasonic time is 5-7min; the citric acid buffer is 0.1-0.2mol / L citric acid buffer; and the pH is 5.5-6.

5.

7. The process for preparing regenerated antibacterial polyester from waste polyester materials according to claim 1, characterized in that: Step 3: The immersion bath ratio of the base material B to the hydrophobic nano-ceramic antibacterial slurry is 1:2-3, the immersion temperature is 40-50°C, and the immersion time is 20-30min; the stirring speed is 20-30rpm; the low-temperature curing temperature and curing time are 80-90°C and 30-40min respectively.

8. The process for preparing regenerated antibacterial polyester from waste polyester materials according to claim 1, characterized in that: Step 3: The method for preparing the hydrophobic nano antibacterial slurry comprises the following steps: Step Y1, mix 2-3 parts by weight of titanium dioxide with an average particle size of 20 nm, 0.04-0.06 parts by weight of sodium polyacrylate, 0.02-0.03 parts by weight of polyvinyl pyrrolidone and 10-16 parts by weight of deionized water, stir at a speed of 500-600 rpm for 10-20 min, then add 2.6-3 parts by weight of aqueous polyurethane, keep the speed unchanged and continue stirring for 20-30 min to obtain.

9. A process for preparing regenerated antibacterial polyester using waste polyester materials according to any one of claims 1 to 8, characterized in that: The regenerated antibacterial polyester is short fiber.

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