Biological blue pigment Indigoidine suitable for cellulose fibers and low-temperature printing and dyeing method thereof

Abstract

The invention discloses a biological blue pigment Indigoidine suitable for cellulosic fibers and a low-temperature printing and dyeing method thereof, and the preparation of the Indigoidine comprises the following steps: carrying out transformation expression on plasmids containing BpsA and Sfp genes by using recombinant escherichia coli, carrying out shake culture for 4 hours at 37 DEG C in a fermentation culture medium consisting of glucose, yeast extract, peptone, KH2PO4 and MgSO4. 7H2O, then inoculating to a 5L fermentation tank, and carrying out fermentation for 4 hours at the temperature of 37 DEG C to obtain the Indigoidine. The temperature is controlled to be 30 DEG C, the pH value is 7.0, the ventilation capacity is 1 vvm, the stirring speed is 400 rpm, fermentation is conducted for 48 hours, after fermentation is finished, the pH value is adjusted to 2.5 through 3% hydrochloric acid, pigment is separated out, washing is conducted twice through ethyl alcohol, freeze drying is conducted, Indigoidine powder is obtained, the purity is 82%, and the printing and dyeing method comprises a low-temperature printing and dyeing method. Comprising the following steps: preparing a dye solution, adding an Indigoidine dye into deionized water, adding an environment-friendly additive system, dip-dyeing cellulose fibers for 40 minutes at the temperature of 40 DEG C, washing with water, neutralizing and drying to finish dyeing. The method disclosed by the invention has the advantages of being reasonable, green, environment-friendly and high in printing and dyeing efficiency.

Description

Technical Field

[0001] The invention relates to the technical field of textile printing and dyeing, and in particular to a biological blue pigment Indigoidine suitable for cellulose fibers and a low-temperature printing and dyeing method thereof. Background Art

[0002] Currently, the main blue dye used for cellulose fibers (such as cotton, viscose, and Tencel) is reduced indigo. This dye requires dyeing and fixing at relatively high temperatures (>90°C) in an alkaline environment, resulting in high energy consumption, high pollution, and complex processes, making it difficult to meet the development needs of a green and sustainable textile industry. Indigoidine, a natural blue pigment produced by microbial fermentation, offers advantages such as excellent stability, non-toxicity, and environmental friendliness. However, its dispersibility in aqueous systems and its affinity for fibers still need improvement. To address these issues, the following proposes a solution. Summary of the Invention

[0003] The present invention aims to provide a biological blue pigment Indigoidine suitable for cellulose fibers and a low-temperature printing and dyeing method thereof, which has the advantages of being green, environmentally friendly and having high printing and dyeing efficiency.

[0004] The above technical objectives of the present invention are achieved through the following technical solutions:

[0005] The invention discloses a biological blue pigment, indigoidine, suitable for cellulose fibers. The pigment is indigoidine derived from microbial fermentation. Indigoidine is prepared by transforming recombinant Escherichia coli (E. coli BL21) with a plasmid expressing BpsA and Sfp genes. The pigment is shaken and cultured at 37°C for 4 hours in a fermentation medium consisting of glucose (20 g / L), yeast extract (10 g / L), peptone (20 g / L), KH2PO4 (1.5 g / L), and MgSO4·7H2O (0.5 g / L). The pigment is then inoculated into a 5L fermenter. The fermentation is carried out for 48 hours under the control of temperature at 30°C, pH 7.0, ventilation at 1 vvm, and stirring at 400 rpm. After the fermentation is completed, the pH is adjusted to 2.5 with 3% hydrochloric acid to precipitate the pigment, which is then washed twice with 70% ethanol and freeze-dried to obtain indigoidine powder with a purity of 82%.

[0006] Preferably, the microbially fermented Indigoidine has the following properties: a. good water dispersibility in the pH range of 6.5-8.5; b. good affinity for cellulose fibers and ability to achieve color fixation at low temperatures; c. synergistic use with an environmentally friendly auxiliary system can improve dyeing uniformity and dye adsorption rate.

[0007] Preferably, the preparation of the Indigoidine can also be obtained by expression in Streptomyces or Pseudomonas.

[0008] A low-temperature dyeing method for a biological blue pigment Indigoidine suitable for cellulose fibers is characterized by comprising the following steps:

[0009] Step 1: Prepare a dye solution by adding Indigoidine dye (1 wt%, pH adjusted to 8.0) to deionized water;

[0010] Step 2: Adding an environmentally friendly additive system, including a natural polymer dispersant (such as chitosan, carboxymethyl cellulose), a slow-release chelating agent, and a non-ionic wetting agent;

[0011] Step 3: impregnate the cellulose fibers at a temperature of 40°C for 40 minutes;

[0012] Step 4: Dyeing is completed through washing, neutralization and drying.

[0013] Preferably, the cellulose fiber material is pretreated by using a cationic modifier (such as epoxypropyltrimethylammonium chloride, EPTMAC) or an aminosilane crosslinker, adding the treatment solution at a concentration of 3% (owf), a bath ratio of 1:20, controlling the temperature at 40°C, treating for 20 minutes, adjusting the pH to 6.0, and then washing with water and drying for use.

[0014] Preferably, the cellulose fiber is one of cotton, viscose, Tencel or Modal.

[0015] Preferably, the dye liquor can be recycled at least twice, and the chromaticity of the dyeing wastewater is significantly reduced.

[0016] Preferably, the environmentally friendly auxiliary agent system is one of natural tannic acid 2% (owf), multivalent amine fixing agent 1.5% (owf) or natural tea polyphenols 2% (owf).

[0017] The beneficial effects of the present invention are:

[0018] (1) The dyeing and fixing process is completed below 50°C, which significantly reduces energy consumption.

[0019] (2) The dye solution can be recycled 2-3 times, which has a significant water-saving effect.

[0020] (3) The chromaticity and COD of the wastewater are significantly lower than those of the traditional indigo dyeing process. DETAILED DESCRIPTION

[0021] The following description is only a preferred embodiment of the present invention, and the protection scope is not limited to this embodiment. All technical solutions under the concept of the present invention should fall within the protection scope of the present invention.

[0022] A biological blue pigment, Indigoidine, suitable for cellulose fibers and a low-temperature printing and dyeing method thereof. The pigment is Indigoidine derived from microbial fermentation and has the following properties: a. It exhibits good water dispersibility within the pH range of 6.5-8.5; b. It has good affinity for cellulose fibers and can achieve color fixation under low-temperature conditions; c. It can be used in conjunction with an environmentally friendly auxiliary agent system to improve dyeing uniformity and dye adsorption rate.

[0023] Indigoidine is prepared using recombinant Escherichia coli (E. coli BL21) transformed with a plasmid expressing the BpsA and Sfp genes. Indigoidine can also be produced by expressing in Streptomyces or Pseudomonas. The mixture is shaken and cultured at 37°C for 4 hours in a fermentation medium containing glucose (20 g / L), yeast extract (10 g / L), peptone (20 g / L), KH2PO4 (1.5 g / L), and MgSO4·7H2O (0.5 g / L). The mixture is then inoculated into a 5-L fermentor and fermented for 48 hours under controlled conditions: temperature at 30°C, pH 7.0, aeration at 1 vvm, and agitation at 400 rpm. After fermentation, the pigment is precipitated by adjusting the pH to 2.5 with 3% hydrochloric acid, washed twice with 70% ethanol, and freeze-dried to obtain indigoidine powder with a purity of 82%.

[0024] It includes the following steps:

[0025] Step 1: Prepare dye solution by adding Indigoidine dye (1 wt%, pH adjusted to 8.0) into deionized water.

[0026] Step 2: Add an environmentally friendly additive system, including a natural polymer dispersant (such as chitosan, carboxymethyl cellulose), a slow-release chelating agent and a non-ionic wetting agent.

[0027] Step 3: The cellulose fibers were impregnated at 40°C for 40 minutes.

[0028] Step 4: Dyeing is completed through washing, neutralization and drying.

[0029] The pretreatment of cellulose fiber materials involves using a cationic modifier (such as epoxypropyltrimethylammonium chloride, EPTMAC) or an aminosilane crosslinker, adding the treatment solution at a concentration of 3% (owf), with a bath ratio of 1:20, controlling the temperature at 40°C, treating for 20 minutes, adjusting the pH to 6.0, then washing and drying for later use. The cellulose fiber is selected from cotton, viscose, Tencel, or Modal. The dye solution can be recycled at least twice, and the color of the dyeing wastewater is significantly reduced.

[0030] Example 1

[0031] Indigoidine printing and dyeing method on cotton cloth

[0032] 1. Preparation of Indigoidine: Ferment and extract according to the above method to obtain Indigoidine powder with a purity of 82%;

[0033] 2. Cotton pretreatment: use 3% (owf) EPTMAC, bath ratio 1:20, 40°C for 20 minutes, pH 6.0;

[0034] 3. Staining: Indigoidine 2% (owf), bath ratio 1:25, pH 6.0, temperature 40°C, staining time 45 minutes;

[0035] 4. Fixation treatment: Use 2% natural tannic acid (owf) and treat at 40℃ for 10 minutes.

[0036] 5. Test results: Washing fastness is level 4, rubbing fastness is level 4 / 3-4 in dry / wet conditions respectively, and the color is bright and uniform.

[0037] Example 2

[0038] Printing and dyeing method of Indigoidine on viscose fiber

[0039] 1. Indigoidine preparation: After fermentation, indigoidine with a purity of 80% is obtained;

[0040] 2. Pretreatment of viscose: Use 2% (owf) aminosilane solution, pH 5.8, 35°C for 15 minutes;

[0041] 3. Staining: Indigoidine 1.5% (owf), bath ratio 1:20, pH 6.2, temperature 45°C, time 60 minutes;

[0042] 4. Fixation: 1.5% (owf) of polyvalent amine fixing agent, treatment at 40°C for 12 minutes.

[0043] 5. Test results: Soap fastness is level 4, dry and wet friction fastness is level 3-4, and the distribution is even.

[0044] Example 3

[0045] Printing and dyeing method of Indigoidine on lyocell fiber

[0046] 1. Indigoidine preparation: A pigment powder with a purity of 85% is obtained by fermentation at 30°C;

[0047] 2. Lyocell fabric pretreatment: use 1% (owf) aminosilane modifier, bath ratio 1:20, treatment for 20 minutes;

[0048] 3. Printing and dyeing: Indigoidine 3% (owf), bath ratio 1:30, pH 5.7, temperature 50°C, dyeing for 30 minutes;

[0049] 4. Fixation treatment: natural tea polyphenols 2% (owf), treatment at 40℃ for 10 minutes.

[0050] 5. Color fastness test: Washing fastness is above level 4, dry rubbing fastness is level 4, wet rubbing fastness is level 3, and the dyeing depth is excellent.

[0051] Test method description:

[0052] Color fastness to washing: tested according to GB / T 3921-2008 Textiles—Color fastness to washing—Color fastness to washing, using a Launder-Ometer (SDLAtlas, M238). The test solution is a mixture of 5 g / L nonionic surfactant and 2 g / L sodium carbonate. The clothes are washed at 40°C for 45 minutes and the grey card method is used for scoring.

[0053] Color fastness to rubbing: According to GB / T3920-2008 “Textiles—Tests for Color Fastness—Color Fastness to Rubbing”, use a rubbing color fastness meter (Model Y571) to perform dry and wet rubbing ten times each to assess the fastness of dyed fabrics to rubbing.

[0054] K / S value determination: A Datacolor 650 spectrophotometer was used to measure the reflectance under a D65 light source and a 10° viewing angle. The K / S value was calculated according to the Kubelka-Munk equation and used to evaluate the dyeing depth.

[0055] Color difference ΔE measurement: CIELAB color space model is used to measure the color difference ΔE between the sample and the standard sample using a spectrophotometer. The control standard ΔE<2.5 is qualified.

[0056] Dye uptake determination: The absorbance of the dye solution was measured at the maximum absorption wavelength (λmax=612 nm) using an ultraviolet spectrophotometer (Shimadzu UV-2600). The dye uptake was calculated based on the concentration difference before and after dyeing after preparing a standard curve.

[0057] Residual dye rate: After centrifugation, take the supernatant and measure its A612 absorbance. The residual dye concentration is inferred based on the calibration curve. The residual dye concentration is excellent if it is less than 15%.

[0058] Fabric strength test: According to GB / T3923.1-2013 “Textile fabrics - Determination of breaking strength - Strip method”, an Instron 3365 electronic universal testing machine was used to evaluate the change in breaking strength of the dyed fabric.

[0059] COD and color determination: COD of dyeing wastewater was determined according to HJ / T399-2007 standard, and color was determined by dilution multiple method.

[0060] The specific embodiments described above further illustrate the technical problems, technical solutions and beneficial effects solved by the present invention. It should be understood that the above are only specific embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

Claims

1. A biological blue pigment Indigoidine suitable for cellulose fibers, characterized in that: The pigment is indigoidine derived from microbial fermentation. Indigoidine is prepared by transforming recombinant Escherichia coli (E. coli BL21) with a plasmid expressing the BpsA and Sfp genes. The culture is shaken at 37°C for 4 hours in a fermentation medium consisting of glucose (20 g / L), yeast extract (10 g / L), peptone (20 g / L), KH2PO4 (1.5 g / L), and MgSO4·7H2O (0.5 g / L). The culture is then inoculated into a 5L fermentor tank, and the temperature, pH, and aeration rate are controlled at 30°C, 7.0, 1 vvm, and 400 rpm for 48 hours. After the fermentation is completed, the pH is adjusted to 2.5 with 3% hydrochloric acid to precipitate the pigment, which is then washed twice with 70% ethanol and freeze-dried to obtain indigoidine powder with a purity of 82%.

2. The biological blue pigment Indigoidine suitable for cellulose fibers according to claim 1, characterized in that: Indigoidine fermented by microorganisms has the following properties: a. It exhibits good water dispersibility in the pH range of 6.5-8.5; b. It has good affinity for cellulose fibers and can achieve color fixation under low temperature conditions; c. It can be used in conjunction with an environmentally friendly auxiliary system to improve dyeing uniformity and dye adsorption rate.

3. The biological blue pigment Indigoidine suitable for cellulose fibers according to claim 1, characterized in that: The preparation of the indigoidine can also be obtained by expression in Streptomyces or Pseudomonas.

4. The low-temperature dyeing method for a biological blue pigment Indigoidine suitable for cellulose fibers according to claim 1, characterized in that: The following steps are involved: Step 1: Prepare a dye solution by adding Indigoidine dye (1 wt%, pH adjusted to 8.0) to deionized water; Step 2: Adding an environmentally friendly additive system, including a natural polymer dispersant (such as chitosan, carboxymethyl cellulose), a slow-release chelating agent, and a non-ionic wetting agent; Step 3: impregnate the cellulose fibers at a temperature of 40°C for 40 minutes; Step 4: Dyeing is completed through washing, neutralization and drying.

5. A low-temperature dyeing method for the biological blue pigment Indigoidine suitable for cellulose fibers according to claim 4, characterized in that: Pretreatment of cellulose fiber materials: Use a cationic modifier (such as epoxypropyltrimethylammonium chloride, EPTMAC) or an aminosilane crosslinker, add it to the treatment solution at a concentration of 3% (owf), the bath ratio is 1:20, the temperature is controlled at 40°C, the treatment time is 20 minutes, the pH is adjusted to 6.0, and then washed with water and dried for use.

6. The low-temperature dyeing method for the biological blue pigment Indigoidine suitable for cellulose fibers according to claim 4, characterized in that: The cellulose fiber is one of cotton, viscose, Tencel or Modal.

7. The low-temperature dyeing method for the biological blue pigment Indigoidine suitable for cellulose fibers according to claim 4, characterized in that: The dye liquor can be recycled at least twice, and the chromaticity of the dyeing wastewater is significantly reduced.

8. The biological blue pigment Indigoidine suitable for cellulose fibers and the low-temperature printing and dyeing method thereof according to claim 4, characterized in that: The environmental protection auxiliary agent system is one of natural tannic acid 2% (owf), multivalent amine color fixing agent 1.5% (owf) or natural tea polyphenol 2% (owf).