Preparation method of composite fiber containing Tai Chi stone and fabric thereof
By grafting polyethylene terephthalate with olefin dicarboxyl quaternary ammonium salt monomers and melt-blending it with Tai Chi stone micropowder, a modified PET-Tai Chi stone masterbatch was prepared, which solved the problem of insufficient antibacterial and hydrophilic moisture absorption properties of polyester fibers and fabrics, achieved efficient antibacterial and hydrophilic effects of the fibers, and possessed health care functions.
Patent Information
- Application Number
- CN202411568769.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-05
- Publication Date
- 2025-09-16
- Estimated Expiration
- 2044-11-05
AI Technical Summary
Polyester fibers and fabrics have poor antibacterial and hydrophilic properties.
By grafting polyethylene terephthalate with alkenyl dicarboxyl quaternary ammonium salt monomers, introducing quaternary ammonium salt antibacterial groups and carboxyl hydrophilic groups, and melt-blending and granulating with Taichi stone micropowder, modified PET-Taichi stone masterbatch was prepared, and then melt-blended and spun with polyethylene terephthalate to obtain composite fibers containing Taichi stone.
It significantly improves the antibacterial properties and hydrophilicity of the fiber, enhances the antibacterial rate and moisture absorption rate of the fiber fabric, has far-infrared radiation function, and promotes human blood microcirculation and metabolism.
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Abstract
Description
Technical Field
[0001] The present invention relates to the field of fiber technology, in particular to a preparation method of composite fiber containing Tai Chi stone and a fabric thereof. Background Art
[0002] Tai Chi stone is a natural mineral that contains a variety of trace metal mineral elements and has the function of radiating far infrared rays. It can promote human blood microcirculation, accelerate metabolism and other health benefits, which makes Tai Chi stone have broad application prospects in fiber fabrics and other aspects. Patent CN103726125B discloses an anti-mite and antibacterial polyester staple fiber and its preparation method. Tai Chi stone, boric acid, clay and other raw materials are used to make micron-level heat-storing anti-mite ceramic powder, which is then mixed with silver-loaded nano-titanium dioxide composite antibacterial powder and polyester chips for spinning. The obtained polyester staple fiber has good antibacterial properties. However, this patent does not improve the hydrophilic hygroscopicity of polyester fibers and fabrics, and compared with inorganic degradable agents such as silver and nano-titanium dioxide, organic antibacterial agents have good compatibility with the material matrix and have little effect on the mechanical properties of the material. Among them, quaternary ammonium salt antibacterial agents have the advantages of fast sterilization speed, strong sterilization ability, good broad-spectrum antibacterial properties, etc., and are widely used in fibers, plastics and other aspects. The present invention aims to use a quaternary ammonium salt antibacterial agent to graft-modify polyethylene terephthalate, and then melt-granulate it with Taiji stone micropowder to improve the antibacterial properties and hydrophilic moisture absorption properties of polyester fibers and fabrics. Summary of the Invention
[0003] The invention solves the problem that the polyester fiber and fabric have poor antibacterial performance and poor hydrophilic and moisture absorption performance.
[0004] The technical solution of the present invention is: a method for preparing composite fibers containing Tai Chi stone, comprising:
[0005] (1) Polyethylene terephthalate is pressed into a film, added to an acetone solution containing benzophenone, stirred and evaporated to remove the solvent, and then the polyethylene terephthalate film is added to an aqueous solution containing an alkenyl dicarboxyl quaternary ammonium salt monomer, nitrogen is introduced, and the film is placed under ultraviolet light for grafting reaction, and washed with water, ethanol, and xylene in sequence, and dried to obtain carboxyl quaternary ammonium salt modified PET.
[0006] (2) The Tai Chi stone is ball-milled and sieved to obtain Tai Chi stone powder; the Tai Chi stone powder and carboxyl quaternary ammonium salt modified PET are then added to a high-speed mixer for mixing, and then melt-blended and granulated through a twin-screw extruder to obtain modified PET-Tai Chi stone masterbatch.
[0007] (3) Adding polyethylene terephthalate and modified PET-Tai Chi stone masterbatch into a screw melt spinning machine for spinning, and drawing by a drawing machine to obtain a composite fiber containing Tai Chi stone.
[0008] Preferably, in (1), the mass concentration of benzophenone in the acetone solution is (0.12-0.9) g / L.
[0009] Preferably, in (1), the mass concentration of the aqueous solution of the alkenyl dicarboxyl quaternary ammonium salt monomer is (10-70) g / L.
[0010] Preferably, in (1), the power of the UV lamp is 600-1000W, and the grafting reaction time is 30-90 minutes.
[0011] Preferably, in (2), the mass ratio of Taichi stone powder to carboxyl quaternary ammonium salt modified PET is 8-15%.
[0012] Preferably, in (2), the temperature of zones 1 to 6 of the twin-screw extruder is 180-280° C., and the screw speed is 50-100 r / min.
[0013] Preferably, in (3), the mass ratio of polyethylene terephthalate to modified PET-Taiji stone masterbatch is 100:(5-20).
[0014] Preferably, in (3), the temperature of zones 1 to 4 of the screw melt spinning machine is 275-300°C, the spinning rate is 1500-2000 m / min; the drawing speed is 500-800 m / min, and the drawing ratio is 2-3.
[0015] Preferably, the preparation method of the alkenyl dicarboxyl quaternary ammonium salt monomer comprises:
[0016] (1) Add 1,3-dichloro-2-propanol (CAS registration number 96-23-1) and isocyanoethyl methacrylate (CAS registration number 30674-80-7) in a molar ratio of 1:(0.9-1.2) to tetrahydrofuran, heat to 60-65°C, condense and reflux for 6-10 hours, distill under reduced pressure, and dry to obtain an intermediate.
[0017] (2) Add the intermediate, 1-methyl-1H-imidazole-5-carboxylic acid (CAS registration number 41806-40-0) in a molar ratio of 1:(1.8-2.4) to ethanol, heat to 75-80°C, reflux under condensation for 36-48 hours, distill under reduced pressure, wash with acetone, and recrystallize the product from ethanol to obtain an alkenyl dicarboxyl quaternary ammonium salt monomer. The reaction formula is as follows:
[0018]
[0019] Preferably, the antibacterial and moisture-absorbing Tesla double-sided fabric is made of composite fibers containing Tai Chi stone.
[0020] The technical effect of the present invention is as follows: 1,3-dichloro-2-propanol, isocyanoethyl methacrylate, and 1-methyl-1H-imidazole-5-carboxylic acid are used as reactants to prepare an alkenyl dicarboxyl quaternary ammonium salt monomer containing two quaternary ammonium salt antibacterial groups and two hydrophilic carboxyl groups; then, polyethylene terephthalate is subjected to ultraviolet light irradiation grafting to obtain carboxyl quaternary ammonium salt-modified PET, thereby introducing a large number of quaternary ammonium salt antibacterial groups, as well as carboxyl and carbamate hydrophilic groups, onto the surface of the PET.
[0021] The present invention melt-blends and granulates carboxyl quaternary ammonium salt-modified PET and Tai Chi stone to obtain modified PET-Tai Chi stone masterbatch, which is then melt-blended and spun with polyethylene terephthalate to obtain Tai Chi stone-containing composite fibers. The composite fibers contain a large amount of quaternary ammonium salt antibacterial groups, which significantly improves the antibacterial properties of the fibers. At the same time, the composite fibers contain carboxyl and carbamate hydrophilic groups, which are beneficial to improving the hydrophilicity of the fiber fabric and exhibiting a higher moisture absorption rate.
[0022] The PET-Tai Chi stone masterbatch of the present invention has the function of radiating far infrared rays, which can promote blood microcirculation and accelerate metabolism in the human body. DETAILED DESCRIPTION
[0023] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.
[0024] Example 1
[0025] (1) Add 40 mmol of 1,3-dichloro-2-propanol and 48 mmol of isocyanoethyl methacrylate to 60 mL of tetrahydrofuran, heat to 65°C, reflux under condensation for 6 hours, distill under reduced pressure, and dry to obtain an intermediate.
[0026] (2) Add 30 mmol of the intermediate and 54 mmol of 1-methyl-1H-imidazole-5-carboxylic acid to 30 mL of ethanol, heat to 80°C, reflux under condensation for 36 hours, distill under reduced pressure, wash with acetone, and recrystallize the product from ethanol to obtain an olefin dicarboxyl quaternary ammonium salt monomer.
[0027] (3) Polyethylene terephthalate is pressed into a film and added to an acetone solution of benzophenone with a mass concentration of 0.37 g / L. After stirring, the solvent is evaporated and removed. Then, the polyethylene terephthalate film is added to an aqueous solution of alkenyl dicarboxyl quaternary ammonium salt monomer with a mass concentration of 30 g / L, nitrogen is introduced, and the film is placed under a 600 W ultraviolet lamp for 90 minutes of grafting reaction. The film is washed with water, ethanol, and xylene in sequence and dried to obtain carboxyl quaternary ammonium salt modified PET.
[0028] (4) The Tai Chi stone was ball-milled and sieved to obtain Tai Chi stone powder with an average particle size of 3 μm; then 6.5 g of Tai Chi stone powder and 50 g of carboxyl quaternary ammonium salt modified PET were added to a high-speed mixer for mixing, and then melt-blended through a twin-screw extruder. The temperatures of zones 1 to 6 were 180°C, 210°C, 265°C, 280°C, 280°C, and 275°C, and the screw speed was 100 r / min. Granulation was performed to obtain modified PET-Tai Chi stone masterbatch.
[0029] (5) Add 100g of polyethylene terephthalate and 5g of modified PET-Tai Chi stone masterbatch into a screw melt spinning machine for spinning. The temperatures of zones 1 to 4 are 275°C, 290°C, 300°C, and 295°C, and the spinning rate is 1800m / min. The fibers are stretched by a drawing machine at a speed of 800m / min and a drawing ratio of 3 to obtain a composite fiber containing Tai Chi stone.
[0030] Example 2
[0031] (1) Add 40 mmol of 1,3-dichloro-2-propanol and 36 mmol of isocyanoethyl methacrylate to 80 mL of tetrahydrofuran, heat to 60°C, reflux under condensation for 10 hours, distill under reduced pressure, and dry to obtain an intermediate.
[0032] (2) Add 30 mmol of the intermediate and 72 mmol of 1-methyl-1H-imidazole-5-carboxylic acid to 25 mL of ethanol, heat to 75°C, reflux under condensation for 48 hours, distill under reduced pressure, wash with acetone, and recrystallize the product from ethanol to obtain an olefin dicarboxyl quaternary ammonium salt monomer.
[0033] (3) Polyethylene terephthalate is pressed into a film and added to an acetone solution of benzophenone with a mass concentration of 0.9 g / L. After stirring, the solvent is evaporated and removed. Then, the polyethylene terephthalate film is added to an aqueous solution of alkenyl dicarboxyl quaternary ammonium salt monomer with a mass concentration of 70 g / L, nitrogen is introduced, and the film is placed under an 800 W ultraviolet lamp for 90 minutes of grafting reaction. The film is washed with water, ethanol, and xylene in sequence and dried to obtain carboxyl quaternary ammonium salt modified PET.
[0034] (4) The Tai Chi stone was ball-milled and sieved to obtain Tai Chi stone powder with an average particle size of 3 μm; then 4 g of Tai Chi stone powder and 50 g of carboxyl quaternary ammonium salt modified PET were added to a high-speed mixer for mixing, and then melt-blended through a twin-screw extruder. The temperatures of zones 1 to 6 were 180°C, 210°C, 265°C, 280°C, 280°C, and 275°C, and the screw speed was 100 r / min. Granulation was performed to obtain modified PET-Tai Chi stone masterbatch.
[0035] (5) Add 100g of polyethylene terephthalate and 10g of modified PET-Tai Chi stone masterbatch into a screw melt spinning machine for spinning. The temperatures of zones 1 to 4 are 275°C, 290°C, 300°C, and 295°C, and the spinning rate is 1500m / min. The fibers are stretched by a drawing machine at a speed of 500m / min and a drawing ratio of 3 to obtain a composite fiber containing Tai Chi stone.
[0036] Example 3
[0037] (1) Prepare an alkenyl dicarboxyl quaternary ammonium salt monomer according to the method of Example 1.
[0038] (2) Polyethylene terephthalate is pressed into a film, added to an acetone solution of benzophenone with a mass concentration of 0.12 g / L, stirred and evaporated to remove the solvent, and then the polyethylene terephthalate film is added to an aqueous solution of alkenyl dicarboxyl quaternary ammonium salt monomer with a mass concentration of 10 g / L, nitrogen is introduced, and placed under a 600 W ultraviolet lamp for irradiation to carry out grafting reaction for 30 minutes, and washed with water, ethanol, and xylene in sequence, and dried to obtain carboxyl quaternary ammonium salt modified PET.
[0039] (3) The Tai Chi stone was ball-milled and sieved to obtain Tai Chi stone powder with an average particle size of 3 μm; then 7.5 g of Tai Chi stone powder and 50 g of carboxyl quaternary ammonium salt modified PET were added to a high-speed mixer for mixing, and then melt-blended through a twin-screw extruder. The temperatures of zones 1 to 6 were 180°C, 210°C, 265°C, 280°C, 280°C, and 275°C, and the screw speed was 80 r / min. Granulation was performed to obtain modified PET-Tai Chi stone masterbatch.
[0040] (4) Add 100g of polyethylene terephthalate and 15g of modified PET-Tai Chi stone masterbatch into a screw melt spinning machine for spinning. The temperatures of zones 1 to 4 are 275°C, 290°C, 300°C, and 295°C, and the spinning rate is 1500m / min. The fibers are stretched by a stretching machine at a speed of 600m / min and a stretch ratio of 2 to obtain a composite fiber containing Tai Chi stone.
[0041] Example 4
[0042] (1) Prepare an alkenyl dicarboxyl quaternary ammonium salt monomer according to the method of Example 1.
[0043] (2) Polyethylene terephthalate is pressed into a film, added to an acetone solution of benzophenone with a mass concentration of 0.66 g / L, stirred and evaporated to remove the solvent, and then the polyethylene terephthalate film is added to an aqueous solution of alkenyl dicarboxyl quaternary ammonium salt monomer with a mass concentration of 50 g / L, nitrogen is introduced, and placed under a 1000 W ultraviolet lamp for irradiation to carry out grafting reaction for 60 minutes, and washed with water, ethanol, and xylene in sequence, and dried to obtain carboxyl quaternary ammonium salt modified PET.
[0044] (3) The Tai Chi stone was ball-milled and sieved to obtain Tai Chi stone powder with an average particle size of 3 μm; then 5.2 g of Tai Chi stone powder and 50 g of carboxyl quaternary ammonium salt modified PET were added to a high-speed mixer for mixing, and then melt-blended through a twin-screw extruder. The temperatures of zones 1 to 6 were 180°C, 210°C, 265°C, 280°C, 280°C, and 275°C, and the screw speed was 50 r / min. Granulation was performed to obtain modified PET-Tai Chi stone masterbatch.
[0045] (4) Add 100g of polyethylene terephthalate and 20g of modified PET-Tai Chi stone masterbatch into a screw melt spinning machine for spinning. The temperatures of zones 1 to 4 are 275°C, 290°C, 300°C, and 295°C, and the spinning rate is 2000m / min. The fibers are stretched by a stretching machine at a speed of 800m / min and a stretch ratio of 2.6 to obtain a composite fiber containing Tai Chi stone.
[0046] Comparative Example 1
[0047] (1) 100 g of polyethylene terephthalate was added to a screw melt spinning machine for spinning, with the temperatures of zones 1 to 4 being 275° C., 290° C., 300° C., and 295° C., and the spinning rate being 1800 m / min; the polyester fiber was drawn by a drawing machine at a drawing speed of 800 m / min and a drawing ratio of 3, to obtain polyester fiber.
[0048] Comparative Example 2
[0049] (1) The Tai Chi stone was ball-milled and sieved to obtain Tai Chi stone powder with an average particle size of 3 μm; then 6.5 g of Tai Chi stone powder and 50 g of polyethylene terephthalate were added to a high-speed mixer for mixing, and then melt-blended through a twin-screw extruder. The temperatures of zones 1 to 6 were 180°C, 210°C, 265°C, 280°C, 280°C, and 275°C, and the screw speed was 100 r / min. Granulation was performed to obtain PET-Tai Chi stone masterbatch.
[0050] (2) 100 g of polyethylene terephthalate and 5 g of PET-Tai Chi stone masterbatch were added to a screw melt spinning machine for spinning. The temperatures of zones 1 to 4 were 275°C, 290°C, 300°C, and 295°C, and the spinning rate was 1800 m / min. The fibers were stretched by a drawing machine at a speed of 800 m / min and a drawing ratio of 3 to obtain a composite fiber containing Tai Chi stone.
[0051] Comparative Example 3
[0052] (1) Add 40 mmol of 3-chloro-1-propanol and 48 mmol of isocyanoethyl methacrylate to 60 mL of tetrahydrofuran, heat to 65°C, reflux under condensation for 4 h, distill under reduced pressure, and dry to obtain intermediate 1.
[0053] (2) Add 30 mmol of the intermediate and 30 mmol of 1-methyl-1H-imidazole-5-carboxylic acid to 30 mL of ethanol, heat to 80°C, reflux under condensation for 24 hours, distill under reduced pressure, wash with petroleum ether, and recrystallize the product from ethanol to obtain an alkenyl carboxyl quaternary ammonium salt monomer. The reaction formula is:
[0054]
[0055] (3) Polyethylene terephthalate is pressed into a film and added to an acetone solution of benzophenone with a mass concentration of 0.37 g / L. After stirring, the solvent is evaporated and removed. Then, the polyethylene terephthalate film is added to an aqueous solution of alkenyl carboxyl quaternary ammonium salt monomer with a mass concentration of 30 g / L, nitrogen is introduced, and the film is placed under a 600 W ultraviolet lamp for 90 minutes of grafting reaction. The film is washed with water, ethanol, and xylene in sequence and dried to obtain carboxyl quaternary ammonium salt modified PET.
[0056] (4) The Tai Chi stone was ball-milled and sieved to obtain Tai Chi stone powder with an average particle size of 3 μm; then 6.5 g of Tai Chi stone powder and 50 g of carboxyl quaternary ammonium salt modified PET were added to a high-speed mixer for mixing, and then melt-blended through a twin-screw extruder. The temperatures of zones 1 to 6 were 180°C, 210°C, 265°C, 280°C, 280°C, and 275°C, and the screw speed was 100 r / min. Granulation was performed to obtain modified PET-Tai Chi stone masterbatch.
[0057] (5) Add 100g of polyethylene terephthalate and 5g of modified PET-Tai Chi stone masterbatch into a screw melt spinning machine for spinning. The temperatures of zones 1 to 4 are 275°C, 290°C, 300°C, and 295°C, and the spinning rate is 1800m / min. The fibers are stretched by a drawing machine at a speed of 800m / min and a drawing ratio of 3 to obtain a composite fiber containing Tai Chi stone.
[0058] The fiber was sterilized by ultraviolet light; Escherichia coli or Streptococcus aureus was used as the test bacteria. 5 mL of 10 7 CFU / mL of the test bacterial suspension was added to the shaking bottle, and the blank control fiber and the test antibacterial fiber were added respectively. The suspension was shaken at 25℃ for 0.5-2h, and then 0.5mL of the shaken bacterial suspension was transferred to PBS buffer and diluted 10 times. 0.5mL of the suspension was taken with a concentration of 10 6 A diluted bacterial culture solution with a CFU / mL was spread on the surface of the agar medium and cultured in a constant temperature and humidity incubator at 37°C for 48 hours. After culture, the bacterial count was determined and the inhibition rate W was calculated.
[0059] W = (BC) / B x 100%. B is the bacterial count of the blank control sample, and C is the bacterial count of the test antimicrobial fiber. The polyester fiber of Comparative Example 1 served as the blank control fiber. The composite fibers of Examples 1-4 and Comparative Examples 2-3 served as the test antimicrobial fibers. The test results are shown in Tables 1-2.
[0060] Table 1 Escherichia coli inhibition rate
[0061]
[0062]
[0063] Table 2 Staphylococcus aureus inhibition rate
[0064]
[0065] The fibers were woven into fabrics, and the moisture regain of the fabrics was tested according to GB / T 9995-1997. The test results are shown in Table 3.
[0066] Table 3 Moisture regain of fiber fabrics
[0067] Moisture regain (%) Example 1 0.672 Example 2 0.953 Example 3 1.206 Example 4 1.355 Comparative Example 1 0.426 Comparative Example 2 0.419 Comparative Example 3 0.553
[0068] After testing, compared with Comparative Example 1, modified PET-Tai Chi Stone masterbatch was added to the polyester composite fibers of Examples 1-4. After the modified PET was grafted with olefin dicarboxyl quaternary ammonium salt monomers, a large number of diquaternary ammonium salt antibacterial groups, as well as hydrophilic carboxyl groups and carbamate groups were introduced on the surface. After melt blending and spinning, the antibacterial properties and hydrophilicity of the polyester fibers and their fabrics were significantly improved, showing higher antibacterial rate and moisture absorption rate.
[0069] The PET in the PET-Tai Chi Stone masterbatch of Comparative Example 2 does not contain diquaternary ammonium salt antibacterial groups and hydrophilic carboxyl groups. The antibacterial properties and hydrophilicity of the polyester fiber and its fabric are poor, and the antibacterial rate and moisture absorption rate are low.
[0070] Comparative Example 3 uses 3-chloro-1-propanol, isocyanoethyl methacrylate, and 1-methyl-1H-imidazole-5-carboxylic acid as reactants to prepare an alkenyl carboxyl quaternary ammonium salt monomer, and then graft-modifies polyethylene terephthalate, introducing quaternary ammonium salt antibacterial groups and hydrophilic carboxyl groups on the PET surface to obtain a modified PET-Tai Chi stone masterbatch. After melt blending and spinning, the antibacterial properties and hydrophilicity of the polyester fiber and its fabric are also significantly improved, but the antibacterial rate and moisture absorption rate are lower than those of the embodiments. This is mainly because the alkenyl carboxyl quaternary ammonium salt monomer of Comparative Example 3 contains only one quaternary ammonium salt group and one carboxyl group, and its antibacterial properties and hydrophilicity are lower than those of the alkenyl dicarboxyl quaternary ammonium salt monomer containing two quaternary ammonium salt groups and two carboxyl groups in the embodiment.
[0071] The above description of the disclosed embodiments is intended to enable one skilled in the art to implement or use the present invention. Various modifications to these embodiments will be readily apparent to one skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not limited to the embodiments shown herein but is intended to conform to the widest scope consistent with the principles and novel features disclosed herein.
Claims
1. A method for preparing a composite fiber containing Tai Chi stone, comprising: (1) Polyethylene terephthalate is pressed into a film, added to an acetone solution containing benzophenone, stirred and evaporated to remove the solvent, and then the polyethylene terephthalate film is added to an aqueous solution containing an alkenyl dicarboxyl quaternary ammonium salt monomer, nitrogen is introduced, and the film is placed under ultraviolet light for grafting reaction, and washed with water, ethanol, and xylene in sequence, and dried to obtain carboxyl quaternary ammonium salt modified PET; The chemical structural formula of the alkenyl dicarboxyl quaternary ammonium salt monomer is as follows: ; (2) Ball mill the Tai Chi stone and sieve it to obtain Tai Chi stone powder; then add the Tai Chi stone powder and carboxyl quaternary ammonium salt modified PET into a high-speed mixer for mixing, and then melt blend and granulate through a twin-screw extruder to obtain modified PET-Tai Chi stone masterbatch; the mass ratio of Tai Chi stone powder to carboxyl quaternary ammonium salt modified PET is 8-15%; (3) Adding polyethylene terephthalate and modified PET-Tai Chi stone masterbatch to a screw melt spinning machine for spinning, and drawing by a drawing machine to obtain a composite fiber containing Tai Chi stone; The preparation method of alkenyl dicarboxyl quaternary ammonium salt monomer comprises: (1) Add 1,3-dichloro-2-propanol and isocyanoethyl methacrylate in a molar ratio of 1:(0.9-1.2) to tetrahydrofuran, heat to 60-65°C, condense and reflux for 6-10 hours, distill under reduced pressure, and dry to obtain an intermediate; (2) Add the intermediate, 1-methyl-1H-imidazole-5-carboxylic acid, in a molar ratio of 1:(1.8-2.4) to ethanol, heat to 75-80°C, condense and reflux for 36-48 hours, distill under reduced pressure, wash with acetone, and recrystallize the product from ethanol to obtain an olefin dicarboxyl quaternary ammonium salt monomer.
2. The method for preparing a composite fiber containing Tai Chi stone according to claim 1, characterized in that: In (1), the mass concentration of benzophenone in the acetone solution is (0.12-0.9) g / L.
3. The method for preparing a composite fiber containing Tai Chi stone according to claim 1, characterized in that: In the above (1), the mass concentration of the aqueous solution of the alkenyl dicarboxyl quaternary ammonium salt monomer is (10-70) g / L.
4. The method for preparing a composite fiber containing Tai Chi stone according to claim 1, characterized in that: In the above (1), the power of the UV lamp is 600-1000W, and the grafting reaction time is 30-90min.
5. The method for preparing a composite fiber containing Tai Chi stone according to claim 1, characterized in that: In (2), the temperature of zones 1 to 6 of the twin-screw extruder is 180-280°C, and the screw speed is 50-100 r / min.
6. The method for preparing a composite fiber containing Tai Chi stone according to claim 1, characterized in that: In the above (3), the mass ratio of polyethylene terephthalate to modified PET-Tai Chi stone masterbatch is 100:(5-20).
7. The method for preparing a composite fiber containing Tai Chi stone according to claim 1, characterized in that: In (3), the temperature of zones 1 to 4 of the screw melt spinning machine is 275-300°C, the spinning rate is 1500-2000 m / min; the drawing speed is 500-800 m / min, and the drawing ratio is 2-3.
8. An antibacterial and moisture-absorbing fabric made of composite fibers containing Tai Chi stone obtained by the preparation method according to any one of claims 1 to 7.
Citation Information
Patent Citations
An anti-mite and antibacterial polyester staple fiber and its preparation method
CN103726125B
Manufacturing method of Tai chi stone and polyester fiber composite material
CN109355729A
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CN117966478A