A method for indigo microbial vat dyeing of natural fibers

Abstract

The application relates to the technical field of fiber dyeing, in particular to a natural fiber indigo microbial reduction dyeing method. A yeast decomposition liquid is prepared in a targeted manner, bamboo leaves are used to prepare carbonized powder, a carbonized mixed liquid is formed, a dyeing liquid is obtained by combining the yeast reduction liquid to dip dye natural fibers, a large amount of chemical drugs is avoided, the pollution to the environment is small, yeast bacterial secretion is mainly used to promote the adhesion of indigo, the dyeing stability is improved, the method is beneficial to subsequent popularization, the processing process is simple, and industrialization can be realized.

Description

Technical Field

[0001] This invention relates to the field of fiber dyeing technology, and in particular to a method for indigo microbial reduction dyeing of natural fibers. Background Technology

[0002] Indigo is a classic plant dye in my country, holding an important place in traditional dyeing and weaving culture. Today, with green manufacturing becoming a key trend in the manufacturing industry, re-examining the application of indigo in textile dyeing is significant for achieving harmless and sustainable raw materials in dyeing and printing, and for the production of eco-friendly textiles. However, in current bioreduction dyeing methods, dyeing stability remains a difficult problem to solve, severely impacting the market acceptance of indigo products. Therefore, finding a solution to this problem has become crucial for the industry. Summary of the Invention

[0003] To address the problems existing in the prior art, this invention provides a method for microbial reduction dyeing of indigo on natural fibers. Through targeted process design, it improves the adhesion of indigo to natural fibers and maintains dyeing stability. The specific technical solution is as follows: A method for microbial reduction dyeing of natural fibers with indigo, comprising the following steps, by weight: (1) Take 3-8 sugarcane powder and juice it with a juicer, filter it, mix the filter residue with 10-15 times the amount of pure water, heat it to 50-55℃ and stir for 20-22 minutes, filter it, combine the two filtrates, concentrate it under reduced pressure to 1 / 5 of the original volume, add glucose to the concentrate to obtain nutrient solution A; put the filter residue of the above filtration into a dryer, dry it at 65-70℃, pulverize it with an ultra-micro pulverizer, mix the pulverized material with calcium chloride and ferric sulfate to obtain mixture B; mix 16-18 parts of nutrient solution A with 6-7 parts of beef extract, 3-5 parts of yeast extract powder, 4-6 parts of mixture B, and 110-120 parts of deionized water, stir evenly, dispense and sterilize to obtain culture medium; (2) Cool the culture medium to room temperature, inoculate yeast in the culture medium in a clean environment, and culture for 18-22 h at 35-38℃ and 280-290 r / min to obtain yeast decomposition liquid; (3) Clean the bamboo leaves, drain the water, add 8-10 times the weight of the leaves and soak them at 60-68℃ for 12-15 minutes. Add calcium oxide, cool down to 45-46℃ and continue soaking for 22-26 minutes. Boil the mixture for 5-8 minutes, reduce the pressure, and after the water evaporates, put the mixture into a vacuum roasting. Crush the carbonized material to obtain carbonized powder. (4) Mix 1 part of carbonized powder with 500-550 parts of purified water, add 2-3.2 parts of 75% alcohol and 3 parts of sucrose ester, and homogenize under high pressure to obtain carbonized mixture; (5) Mix the yeast decomposition solution and carbonization mixture at a mass ratio of 11-15:3 to obtain the yeast reduction solution; mix indigo and purified water at a mass ratio of 1:66-75, add ethanol at a mass ratio of 2 times that of indigo and stir for 20 min, add sodium dodecylbenzenesulfonate at a mass ratio of 0.3 times that of indigo, stir evenly, and homogenize by ultrasonication to obtain the dyeing stock solution; mix the dyeing stock solution and yeast reduction solution at a mass ratio of 7-9:3 to obtain the dyeing solution; (6) Prepare a nitric acid solution with a mass fraction of 0.005%, heat it to 38-44℃, immerse the natural fiber in the nitric acid solution for 20-30 seconds, take out the natural fiber and immerse it in the dyeing solution for 8-10 hours, take it out and dry it, put it back into the dyeing solution, and rinse it with water to obtain dyed natural fiber.

[0004] Furthermore, in step (1), the amount of glucose used is 25-33% of the mass of the concentrate.

[0005] Furthermore, in step (1), the mass ratio of the pulverized material to calcium chloride and ferric sulfate is 100-133:1:0.3.

[0006] Furthermore, in step (1), the sterilization conditions are 125°C for 2-3 hours.

[0007] Furthermore, in step (2), the amount of yeast inoculated is 7-8% of the mass of the culture medium.

[0008] Furthermore, in step (3), the amount of calcium oxide added is 3-6% of the weight of the bamboo leaves.

[0009] Furthermore, in step (3), the vacuum calcination conditions are 600-800℃ for 30-50 minutes.

[0010] Compared with the prior art, the technical effects of the present invention are reflected in: The biological reduction staining method of this invention avoids the use of large amounts of chemical reagents, resulting in less environmental pollution. It mainly uses yeast cell secretions to promote indigo adhesion, thereby improving staining stability and facilitating subsequent promotion. The processing is simple and conducive to industrialization. Detailed Implementation

[0011] The technical solution of the present invention will be further defined below with reference to specific embodiments, but the scope of protection is not limited to the description.

[0012] Example 1 A method for microbial reduction staining of natural fibers with indigo, comprising the following steps: (1) Take 3 sugarcane powder and juice it with a juicer, filter it, mix the filter residue with 10 times the amount of pure water, heat it to 50℃ and stir for 20 minutes, filter it, combine the two filtrates, concentrate it under reduced pressure to 1 / 5 of the original volume, add 25% of its mass of glucose to the concentrate to obtain nutrient solution A; put the filter residue of the above-mentioned filter into a dryer, dry it at 65℃, pulverize it with an ultra-micro pulverizer, mix the pulverized material with calcium chloride and ferric sulfate at a mass ratio of 100:1:0.3 to obtain mixture B; mix 16 parts of nutrient solution A with 6 parts of beef extract, 3 parts of yeast extract powder, 4 parts of mixture B and 110 parts of deionized water, stir evenly, divide into portions, and sterilize at 125℃ for 2 hours to obtain culture medium; (2) Cool the culture medium to room temperature, and inoculate yeast in the culture medium in a clean environment. The inoculation amount is 7% of the mass of the culture medium. Culture at 35℃ and 280r / min for 18h to obtain yeast decomposition liquid. (3) Clean the bamboo leaves, drain the water, add 8 times the weight of the water, soak at 60℃ for 12 minutes, add 3% of the weight of the bamboo leaves of calcium oxide, cool down to 45℃ and continue soaking for 22 minutes, boil the mixture for 5 minutes, reduce the pressure, wait for the water to evaporate, put the mixture into 600℃ vacuum roasting for 30 minutes, and crush the carbonized material to obtain carbonized powder. (4) Mix 1 part carbonized powder and 500 parts purified water, add 2 parts 75% alcohol and 3 parts sucrose ester, and homogenize under high pressure to obtain carbonized mixture; (5) Mix the yeast decomposition solution and carbonization mixture at a mass ratio of 11:3 to obtain the yeast reduction solution; mix indigo and purified water at a mass ratio of 1:66, add ethanol at a mass ratio of 2 times that of indigo and stir for 20 min, add sodium dodecylbenzenesulfonate at a mass ratio of 0.3 times that of indigo, stir evenly, and homogenize by ultrasonication to obtain the dyeing stock solution; mix the dyeing stock solution and yeast reduction solution at a mass ratio of 7:3 to obtain the dyeing solution; (6) Prepare a nitric acid solution with a mass fraction of 0.005%, heat it to 38°C, immerse the natural fiber in the nitric acid solution for 20 seconds, take out the natural fiber and immerse it in the dyeing solution for 8 hours, take it out and dry it, put it back into the dyeing solution, and rinse it with water to obtain dyed natural fiber.

[0013] Example 2 A method for microbial reduction staining of natural fibers with indigo, comprising the following steps: (1) Take 8 parts of sugarcane and juice it using a juicer. Filter the juice and mix the residue with 15 times the amount of pure water. Heat the mixture to 55°C and stir for 22 minutes. Filter the mixture and combine the two filtrates. Concentrate the mixture under reduced pressure to 1 / 5 of its original volume. Add 33% of the glucose by mass to the concentrate to obtain nutrient solution A. Place the filtered residue into a dryer and dry it at 65°C. Grind the residue with an ultra-fine pulverizer. Mix the pulverized residue with calcium chloride and ferric sulfate at a mass ratio of 100:1:0.3 to obtain mixture B. Mix 18 parts of nutrient solution A with 7 parts of beef extract, 5 parts of yeast extract, 6 parts of mixture B, and 120 parts of deionized water. Stir the mixture evenly, divide it into portions, and sterilize it at 125°C for 3 hours to obtain the culture medium. (2) Cool the culture medium to room temperature, and in a clean environment, inoculate yeast into the culture medium at an inoculation amount of 8% of the culture medium mass. Incubate at 35℃ and 280r / min for 18h to obtain yeast decomposition liquid. (3) Clean the bamboo leaves, drain the water, add 10 times the weight of the water, soak at 68℃ for 15 minutes, add 6% of the weight of the bamboo leaves of calcium oxide, cool down to 46℃ and continue soaking for 26 minutes, boil the mixture for 8 minutes, reduce the pressure, wait for the water to evaporate, put the mixture into 800℃ vacuum roasting for 50 minutes, and crush the carbonized material to obtain carbonized powder. (4) Mix 1 part carbonized powder and 500 parts purified water, add 2 parts 75% alcohol and 3 parts sucrose ester, and homogenize under high pressure to obtain carbonized mixture; (5) Mix the yeast decomposition solution and carbonization mixture at a mass ratio of 11:3 to obtain the yeast reduction solution; mix indigo and purified water at a mass ratio of 1:66, add ethanol at a mass ratio of 2 times that of indigo and stir for 20 min, add sodium dodecylbenzenesulfonate at a mass ratio of 0.3 times that of indigo, stir evenly, and homogenize by ultrasonication to obtain the dyeing stock solution; mix the dyeing stock solution and yeast reduction solution at a mass ratio of 7:3 to obtain the dyeing solution; (6) Prepare a nitric acid solution with a mass fraction of 0.005%, heat it to 38°C, immerse the natural fiber in the nitric acid solution for 20 seconds, take out the natural fiber and immerse it in the dyeing solution for 8 hours, take it out and dry it, put it back into the dyeing solution, and rinse it with water to obtain dyed natural fiber.

[0014] Example 3 A method for microbial reduction staining of natural fibers with indigo, comprising the following steps: (1) Take 7 parts sugarcane and juice it with a juicer. Filter the juice and mix the residue with 10 times the amount of pure water. Heat the mixture to 53°C and stir for 21 minutes. Filter the mixture and combine the two filtrates. Concentrate the mixture under reduced pressure to 1 / 5 of the original volume. Add 25-33% glucose by mass to the concentrate to obtain nutrient solution A. Place the filtered residue into a dryer and dry it at 65°C. Grind the residue with an ultra-fine pulverizer. Mix the pulverized residue with calcium chloride and ferric sulfate at a mass ratio of 100:1:0.3 to obtain mixture B. Mix 16 parts of nutrient solution A with 7 parts of beef extract, 5 parts of yeast extract, 4 parts of mixture B, and 116 parts of deionized water. Stir the mixture evenly, divide it into portions, and sterilize it at 125°C for 2 hours to obtain the culture medium. (2) Cool the culture medium to room temperature, and in a clean environment, inoculate yeast into the culture medium at an inoculation amount of 8% of the culture medium mass. Incubate at 35℃ and 280r / min for 18h to obtain yeast decomposition liquid. (3) Clean the bamboo leaves, drain the water, add 10 times the weight of water, soak at 60℃ for 15 minutes, add 6% of the weight of calcium oxide of bamboo leaves, cool down to 45℃ and continue soaking for 26 minutes, boil the mixture for 5 minutes, reduce the pressure, wait for the water to evaporate, put the mixture into 800℃ vacuum roasting for 50 minutes, and crush the carbonized material to obtain carbonized powder. (4) Mix 1 part carbonized powder and 500 parts purified water, add 2 parts 75% alcohol and 3 parts sucrose ester, and homogenize under high pressure to obtain carbonized mixture; (5) Mix the yeast decomposition solution and carbonization mixture at a mass ratio of 11:3 to obtain the yeast reduction solution; mix indigo and purified water at a mass ratio of 1:66, add ethanol at a mass ratio of 2 times that of indigo and stir for 20 min, add sodium dodecylbenzenesulfonate at a mass ratio of 0.3 times that of indigo, stir evenly, and homogenize by ultrasonication to obtain the dyeing stock solution; mix the dyeing stock solution and yeast reduction solution at a mass ratio of 7:3 to obtain the dyeing solution; (6) Prepare a nitric acid solution with a mass fraction of 0.005%, heat it to 38°C, immerse the natural fiber in the nitric acid solution for 30 seconds, take out the natural fiber and immerse it in the dyeing solution for 8 hours, take it out and dry it, put it back into the dyeing solution, and rinse it with water to obtain dyed natural fiber.

[0015] Example 4 A method for microbial reduction staining of natural fibers with indigo, comprising the following steps: (1) Take 3 sugarcane powder and juice it with a juicer, filter it, mix the filter residue with 15 times the amount of pure water, heat it to 55℃ and stir for 22 minutes, filter it, combine the two filtrates, concentrate it under reduced pressure to 1 / 5 of the original volume, add 25-33% of its mass of glucose to the concentrate to obtain nutrient solution A; put the filter residue of the above-mentioned filter into a dryer, dry it at 65℃, pulverize it with an ultra-micro pulverizer, mix the pulverized material with calcium chloride and ferric sulfate at a mass ratio of 100:1:0.3 to obtain mixture B; mix 18 parts of nutrient solution A with 7 parts of beef extract, 5 parts of yeast extract powder, 4 parts of mixture B and 110 parts of deionized water, stir evenly, divide into portions, and sterilize at 125℃ for 2 hours to obtain culture medium; (2) Cool the culture medium to room temperature, and inoculate yeast in the culture medium in a clean environment. The inoculation amount is 7% of the mass of the culture medium. Culture at 35℃ and 280r / min for 18h to obtain yeast decomposition liquid. (3) Clean the bamboo leaves, drain the water, add 8 times the weight of the water, soak at 60℃ for 12 minutes, add 3% of the weight of the bamboo leaves of calcium oxide, cool down to 45℃ and continue soaking for 22 minutes, boil the mixture for 8 minutes, reduce the pressure, wait for the water to evaporate, put the mixture into 800℃ vacuum roasting for 50 minutes, and crush the carbonized material to obtain carbonized powder. (4) Mix 1 part carbonized powder and 500 parts purified water, add 2 parts 75% alcohol and 3 parts sucrose ester, and homogenize under high pressure to obtain carbonized mixture; (5) Mix the yeast decomposition solution and carbonization mixture at a mass ratio of 11:3 to obtain the yeast reduction solution; mix indigo and purified water at a mass ratio of 1:66, add ethanol at a mass ratio of 2 times that of indigo and stir for 20 min, add sodium dodecylbenzenesulfonate at a mass ratio of 0.3 times that of indigo, stir evenly, and homogenize by ultrasonication to obtain the dyeing stock solution; mix the dyeing stock solution and yeast reduction solution at a mass ratio of 7:3 to obtain the dyeing solution; (6) Prepare a nitric acid solution with a mass fraction of 0.005%, heat it to 38°C, immerse the natural fiber in the nitric acid solution for 28 seconds, take out the natural fiber and immerse it in the dyeing solution for 8 hours, take it out and dry it, put it back into the dyeing solution, and rinse it with water to obtain dyed natural fiber.

[0016] Example 5 A method for microbial reduction staining of natural fibers with indigo, comprising the following steps: (1) Take 8 parts of sugarcane and juice it using a juicer. Filter the juice and mix the residue with 10 times the amount of pure water. Heat the mixture to 55°C and stir for 20 minutes. Filter the mixture and combine the two filtrates. Concentrate the mixture under reduced pressure to 1 / 5 of its original volume. Add 33% of the glucose by mass to the concentrate to obtain nutrient solution A. Place the filtered residue into a dryer and dry it at 65°C. Grind the residue with an ultra-fine pulverizer. Mix the pulverized residue with calcium chloride and ferric sulfate at a mass ratio of 100:1:0.3 to obtain mixture B. Mix 16 parts of nutrient solution A with 7 parts of beef extract, 5 parts of yeast extract, 4 parts of mixture B, and 110 parts of deionized water. Stir the mixture evenly, divide it into portions, and sterilize it at 125°C for 3 hours to obtain the culture medium. (2) Cool the culture medium to room temperature, and inoculate yeast in the culture medium in a clean environment. The inoculation amount is 7% of the mass of the culture medium. Culture at 35℃ and 280r / min for 18h to obtain yeast decomposition liquid. (3) Clean the bamboo leaves, drain the water, add 8 times the weight of water, soak at 68℃ for 12 minutes, add 6% of the weight of calcium oxide of bamboo leaves, cool down to 46℃ and continue soaking for 22 minutes, boil the mixture for 5 minutes, reduce the pressure, wait for the water to evaporate, put the mixture into 670℃ vacuum roasting for 35 minutes, and crush the carbonized material to obtain carbonized powder. (4) Mix 1 part carbonized powder and 500 parts purified water, add 2 parts 75% alcohol and 3 parts sucrose ester, and homogenize under high pressure to obtain carbonized mixture; (5) Mix the yeast decomposition solution and carbonization mixture at a mass ratio of 11:3 to obtain the yeast reduction solution; mix indigo and purified water at a mass ratio of 1:66, add ethanol at a mass ratio of 2 times that of indigo and stir for 20 min, add sodium dodecylbenzenesulfonate at a mass ratio of 0.3 times that of indigo, stir evenly, and homogenize by ultrasonication to obtain the dyeing stock solution; mix the dyeing stock solution and yeast reduction solution at a mass ratio of 7:3 to obtain the dyeing solution; (6) Prepare a nitric acid solution with a mass fraction of 0.005%, heat it to 38°C, immerse the natural fiber in the nitric acid solution for 25 seconds, take out the natural fiber and immerse it in the dyeing solution for 8 hours, take it out and dry it, put it back into the dyeing solution, and rinse it with water to obtain dyed natural fiber.

Claims

1. A method for microbial reduction staining of indigo on natural fibers, characterized in that, Based on parts by weight, the process includes the following steps: (1) Take 3-8 sugarcane powder and juice it with a juicer, filter it, mix the filter residue with 10-15 times the amount of pure water, heat it to 50-55℃ and stir for 20-22 minutes, filter it, combine the two filtrates, concentrate it under reduced pressure to 1 / 5 of the original volume, add glucose to the concentrate to obtain nutrient solution A; put the filter residue of the above filtration into a dryer, dry it at 65-70℃, pulverize it with an ultra-micro pulverizer, mix the pulverized material with calcium chloride and ferric sulfate to obtain mixture B; mix 16-18 parts of nutrient solution A with 6-7 parts of beef extract, 3-5 parts of yeast extract powder, 4-6 parts of mixture B, and 110-120 parts of deionized water, stir evenly, dispense and sterilize to obtain culture medium; (2) Cool the culture medium to room temperature, inoculate yeast in the culture medium in a clean environment, and culture for 18-22 h at 35-38℃ and 280-290 r / min to obtain yeast decomposition liquid; (3) Clean the bamboo leaves, drain the water, add 8-10 times the weight of the leaves and soak them at 60-68℃ for 12-15 minutes. Add calcium oxide, cool down to 45-46℃ and continue soaking for 22-26 minutes. Boil the mixture for 5-8 minutes, reduce the pressure, and after the water evaporates, put the mixture into a vacuum roasting. Crush the carbonized material to obtain carbonized powder. (4) Mix 1 part of carbonized powder with 500-550 parts of purified water, add 2-3.2 parts of 75% alcohol and 3 parts of sucrose ester, and homogenize under high pressure to obtain carbonized mixture; (5) Mix the yeast decomposition solution and the carbonization mixture at a mass ratio of 11-15:3 to obtain the yeast reduction solution; Mix indigo and purified water at a mass ratio of 1:66-75, add ethanol at a mass ratio of 2 times that of indigo and stir for 20 minutes, add sodium dodecylbenzenesulfonate at a mass ratio of 0.3 times that of indigo and stir evenly, then homogenize by ultrasonication to obtain the dye stock solution; mix the dye stock solution and yeast reducing solution at a mass ratio of 7-9:3 to obtain the dye solution. (6) Prepare a nitric acid solution with a mass fraction of 0.005%, heat it to 38-44℃, immerse the natural fiber in the nitric acid solution for 20-30 seconds, take out the natural fiber and immerse it in the dyeing solution for 8-10 hours, take it out and dry it, put it back into the dyeing solution, and rinse it with water to obtain dyed natural fiber.

2. A method for microbial reduction dyeing of indigo on natural fibers, characterized in that, In step (1), the amount of glucose used is 25-33% of the mass of the concentrate.

3. A method for microbial reduction dyeing of indigo on natural fibers, characterized in that, In step (1), the mass ratio of the pulverized material to calcium chloride and ferric sulfate is 100-133:1:0.

3.

4. A method for microbial reduction dyeing of indigo on natural fibers, characterized in that, In step (1), the sterilization conditions are 125℃ for 2-3 hours.

5. A method for microbial reduction dyeing of indigo on natural fibers, characterized in that, In step (2), the amount of yeast inoculated is 7-8% of the mass of the culture medium.

6. A method for microbial reduction dyeing of indigo on natural fibers, characterized in that, In step (3), the amount of calcium oxide added is 3-6% of the weight of the bamboo leaves.

7. A method for microbial reduction dyeing of indigo on natural fibers, characterized in that, In step (3), the vacuum calcination conditions are 600-800℃ for 30-50 minutes.