CN114921112A - Preparation method and application of pure water system bacterial dye prodigiosin nano suspension dye liquor - Google Patents
Preparation method and application of pure water system bacterial dye prodigiosin nano suspension dye liquor Download PDFInfo
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- HCOLPNRPCMFHOH-UHFFFAOYSA-N Prodigiosin Natural products CCCCCC1C=C(C=C/2N=C(C=C2OC)c3ccc[nH]3)N=C1C HCOLPNRPCMFHOH-UHFFFAOYSA-N 0.000 title claims abstract description 140
- TWFGRJUTAULJPZ-USZBIXTISA-N prodigiosin Chemical compound N1=C(C)C(CCCCC)=C\C1=C/C1=NC(C=2[N]C=CC=2)=C[C]1OC TWFGRJUTAULJPZ-USZBIXTISA-N 0.000 title claims abstract description 140
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 82
- 239000006070 nanosuspension Substances 0.000 title claims abstract description 36
- 230000001580 bacterial effect Effects 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000004744 fabric Substances 0.000 claims abstract description 129
- 229920000742 Cotton Polymers 0.000 claims abstract description 107
- 238000004043 dyeing Methods 0.000 claims abstract description 74
- 238000000034 method Methods 0.000 claims abstract description 63
- 238000000855 fermentation Methods 0.000 claims abstract description 51
- 230000004151 fermentation Effects 0.000 claims abstract description 51
- 230000008569 process Effects 0.000 claims abstract description 50
- 239000002245 particle Substances 0.000 claims abstract description 43
- 239000000693 micelle Substances 0.000 claims abstract description 29
- 238000009980 pad dyeing Methods 0.000 claims abstract description 18
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 241001052560 Thallis Species 0.000 claims abstract description 15
- 241000607715 Serratia marcescens Species 0.000 claims abstract description 12
- 238000011218 seed culture Methods 0.000 claims abstract description 10
- 239000001963 growth medium Substances 0.000 claims abstract description 9
- 238000012258 culturing Methods 0.000 claims abstract description 6
- 238000012546 transfer Methods 0.000 claims abstract description 6
- 230000009471 action Effects 0.000 claims abstract description 5
- 230000003213 activating effect Effects 0.000 claims abstract description 4
- 239000000049 pigment Substances 0.000 claims description 79
- 239000000243 solution Substances 0.000 claims description 65
- 239000000344 soap Substances 0.000 claims description 35
- 238000010025 steaming Methods 0.000 claims description 35
- 238000009835 boiling Methods 0.000 claims description 26
- 238000005406 washing Methods 0.000 claims description 22
- 239000004094 surface-active agent Substances 0.000 claims description 21
- 238000005096 rolling process Methods 0.000 claims description 20
- 239000000725 suspension Substances 0.000 claims description 18
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 15
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- 229920000053 polysorbate 80 Polymers 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 12
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- 238000005119 centrifugation Methods 0.000 claims description 9
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 8
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 claims description 6
- 239000001888 Peptone Substances 0.000 claims description 6
- 108010080698 Peptones Proteins 0.000 claims description 6
- 239000011248 coating agent Substances 0.000 claims description 6
- 238000000576 coating method Methods 0.000 claims description 6
- 235000019319 peptone Nutrition 0.000 claims description 6
- 239000001103 potassium chloride Substances 0.000 claims description 6
- 235000011164 potassium chloride Nutrition 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000009826 distribution Methods 0.000 claims description 4
- 240000004808 Saccharomyces cerevisiae Species 0.000 claims description 3
- 229910052943 magnesium sulfate Inorganic materials 0.000 claims description 3
- 235000019341 magnesium sulphate Nutrition 0.000 claims description 3
- 239000002609 medium Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 claims description 3
- 239000008149 soap solution Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 20
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- 239000000975 dye Substances 0.000 description 133
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- 239000004753 textile Substances 0.000 description 13
- 239000000835 fiber Substances 0.000 description 11
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 9
- 230000003834 intracellular effect Effects 0.000 description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 8
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- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
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- 229920006395 saturated elastomer Polymers 0.000 description 3
- 239000000979 synthetic dye Substances 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 2
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- FYXXJXKLTCPPHW-UHFFFAOYSA-N 2-methoxy-1h-pyrrole Chemical group COC1=CC=CN1 FYXXJXKLTCPPHW-UHFFFAOYSA-N 0.000 description 1
- 241000186361 Actinobacteria <class> Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 101001018064 Homo sapiens Lysosomal-trafficking regulator Proteins 0.000 description 1
- 102100033472 Lysosomal-trafficking regulator Human genes 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 244000038561 Modiola caroliniana Species 0.000 description 1
- 235000010703 Modiola caroliniana Nutrition 0.000 description 1
- 241000228347 Monascus <ascomycete fungus> Species 0.000 description 1
- 229930182559 Natural dye Natural products 0.000 description 1
- 241000607598 Vibrio Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
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- 201000004792 malaria Diseases 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
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- 239000000978 natural dye Substances 0.000 description 1
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- 230000001590 oxidative effect Effects 0.000 description 1
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- 230000009466 transformation Effects 0.000 description 1
- 239000000984 vat dye Substances 0.000 description 1
- XAPNKXIRQFHCHN-QGOAFFKASA-N violacein Chemical compound O=C\1NC2=CC=CC=C2C/1=C(C(=O)N1)/C=C1C1=CNC2=CC=C(O)C=C21 XAPNKXIRQFHCHN-QGOAFFKASA-N 0.000 description 1
- LEJQUNAZZRYZKJ-UHFFFAOYSA-N violacein Natural products Oc1ccc2NCC(C3=CC(=C4/C(=O)Nc5ccccc45)C(=O)N3)c2c1 LEJQUNAZZRYZKJ-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
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- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
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- C12N1/00—Microorganisms, e.g. protozoa; Compositions thereof; Processes of propagating, maintaining or preserving microorganisms or compositions thereof; Processes of preparing or isolating a composition containing a microorganism; Culture media therefor
- C12N1/20—Bacteria; Culture media therefor
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- C12P17/00—Preparation of heterocyclic carbon compounds with only O, N, S, Se or Te as ring hetero atoms
- C12P17/16—Preparation of heterocyclic carbon compounds with only O, N, S, Se or Te as ring hetero atoms containing two or more hetero rings
- C12P17/165—Heterorings having nitrogen atoms as the only ring heteroatoms
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- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B19/00—Treatment of textile materials by liquids, gases or vapours, not provided for in groups D06B1/00 - D06B17/00
- D06B19/0005—Fixing of chemicals, e.g. dyestuffs, on textile materials
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- D06B23/00—Component parts, details, or accessories of apparatus or machines, specially adapted for the treating of textile materials, not restricted to a particular kind of apparatus, provided for in groups D06B1/00 - D06B21/00
- D06B23/20—Arrangements of apparatus for treating processing-liquids, -gases or -vapours, e.g. purification, filtration or distillation
- D06B23/22—Arrangements of apparatus for treating processing-liquids, -gases or -vapours, e.g. purification, filtration or distillation for heating
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- D06B3/00—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating
- D06B3/10—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fabrics
- D06B3/18—Passing of textile materials through liquids, gases or vapours to effect treatment, e.g. washing, dyeing, bleaching, sizing, impregnating of fabrics combined with squeezing, e.g. in padding machines
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- D06P1/0004—General aspects of dyeing
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- C12R—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES C12C - C12Q, RELATING TO MICROORGANISMS
- C12R2001/00—Microorganisms ; Processes using microorganisms
- C12R2001/01—Bacteria or Actinomycetales ; using bacteria or Actinomycetales
- C12R2001/425—Serratia
- C12R2001/43—Serratia marcescens
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Abstract
The invention discloses a preparation method and application of pure water system bacterial dye prodigiosin nano suspension dye liquor, which comprises the following steps: (1) activating ATCC8100 Serratia marcescens; (2) culturing the serratia marcescens seed liquid in a constant-temperature culture oscillator; (3) transferring the seed culture solution into a fermentation culture medium by using a liquid transfer gun for fermentation culture; (4) under the action of a shaking table, a large number of nano-scale prodigiosin micelle particles are formed in a culture solution; (5) and removing thalli in the fermentation liquor to obtain the pure water system prodigiosin nano suspension dye liquor. Also comprises the application of the pure water system bacterial dye prodigiosin nano suspension dye liquor in the padding dyeing process of cotton fabrics. The invention obviously improves the utilization rate of the dye, and the dye uptake of prodigiosin is improved to 34.9%. The pad dyeing process adopted by the invention greatly improves the production efficiency, is suitable for industrial batch production and application, and is a great innovation in the field of bacterial dye dyeing processes.
Description
Technical Field
The invention relates to the technical field of cotton fabric dyeing, in particular to a preparation method and application of pure water bacterial dye prodigiosin nano suspension dye liquor.
Background
The textile industry is the traditional strut industry and the important civil industry in China. Currently, as the advance of accelerating the conversion of new and old kinetic energy is accelerated, the development of the textile industry is increasingly stressed and restrained as a resource-dependent and environment-sensitive industry. Textile printing and dyeing processing is a key processing link for realizing structure adjustment and transformation upgrading in the textile industry, and the cleanness of the production process and the ecology of products become the problems which are energetically solved in the development of dyeing and finishing processing technology. With the increasingly strong pursuit of the ecological environment protection of the dye by people and the improvement of the attention degree of the state to renewable resources, the biomass dye with good biodegradability, source sustainability and ecological functionality of the dyeing product increasingly becomes a hot point of research in the field of textile dyeing.
In biomass dyes, compared with dyes extracted from plants and animals, the production of microbial dyes has the advantages of no limitation of seasons, climates and regions, short production period, easy control of conditions, high yield, rich varieties and the like, and has huge potential for development and utilization. The method for producing the dye/pigment by using the microorganism can solve the problems of rare raw materials, high cost and the like of natural dyes and is more beneficial to industrial production.
The application of microbial pigments in the field of textile dyeing has been reported at home and abroad, and most of the microbial pigments are concentrated on prodigiosin, violacein and fat-soluble monascus pigments. The prodigiosin has bright color and good thermal stability, has the functions of antibiosis, malaria resistance and the like, can endow textiles with higher added value when being used as dye, and has great development value. Prodigiosin is a natural pigment with a methoxy pyrrole skeleton structure consisting of three pyrrole rings, and is a secondary metabolite of serratia marcescens, vibrio aeroginicus and a plurality of actinomycetes. The bacterial dye prodigiosin is a mauve pigment, is almost insoluble in water and easily soluble in an organic solvent, and has the following structure:
the bacterial dye is insoluble in water, belongs to intracellular pigments, and needs to be extracted by using an organic solvent before utilization. In addition, an organic solvent is required to dissolve the pigment during the dyeing process. The use of organic solvents obviously increases dyeing cost, has pollution problems and is difficult to realize industrialized mass production.
At present, the main modes for dyeing cotton fabrics are dip dyeing and pad dyeing, and synthetic dyes for dyeing cotton fabrics comprise two types of reactive dyes and vat dyes, wherein the reactive dyes are mainly used. The dip dyeing process is a dyeing method in which a fabric to be dyed is immersed in a dye solution, and the dye is dyed by the substantivity of the dye to the fiber by the circulation of the dye solution and the relative movement of the fabric to the fabric, and is diffused and fixed on the fiber. It is characterized in that the fabric is suitable for textiles with various shapes; intermittent production, low labor production efficiency and suitability for small-batch and multi-variety production. The main process route of the cotton fabric dip dyeing process is as follows:
alkaline dye liquor → impregnation (dyeing) → washing with water → soaping (fixing) → washing with water.
The pad dyeing process is that the fabric is dipped in the dye liquor for a short time (generally for several seconds or dozens of seconds), then is rolled by a roller, the dye liquor is extruded into the tissues and gaps of the fabric, and simultaneously, the redundant dye liquor is rolled off, so that the dye is uniformly distributed on the fabric. The dye is dyed (or mainly dyed) in the subsequent steaming or baking treatment process. The method has the characteristics of continuous dyeing processing, high production efficiency and suitability for dyeing of large-batch fabrics.
The two modes are good and bad, the padding dyeing process is relatively more advantageous from the aspects of saving cost, improving production efficiency and being suitable for industrialized mass production, and the current two types of dyes have the following main process routes for padding cotton fabrics:
1. reactive dyes: alkaline dye liquor → padding for N times (dyeing) → steaming (fixing) → washing with water → soaping (removing floating color) → washing with water;
2. reducing a dye: alkaline dye liquor → padding for N times (dyeing) → steaming (dyeing) → piling (oxidative fixation) → washing with water → soaping (removing floating color) → washing with water;
in summary, in the existing dip dyeing and pad dyeing processes for cotton fabrics, the synthetic dye solution is required to be prepared into molecular or ionic aqueous solution for dyeing and fixing color in alkaline environment, and the related dyeing mechanism is the prior art and is not described in detail herein. Synthetic dyes are used for dyeing cotton fabrics, and both dip dyeing and pad dyeing and soaping procedures are used for removing loose colors. The soaping process of the prodigiosin for dyeing cotton fabrics is used for fixing colors. Then, as for the bacterial dye prodigiosin dye liquor of the present invention, the prior art discloses the following:
CN111826974A discloses a prodigiosin dyeing method of pure cotton fabric, which comprises the following steps: pretreating the pure cotton fabric by using hydrogen peroxide; then taking out the pure cotton fabric, and washing and drying the pure cotton fabric; dissolving prodigiosin with ethyl acetate, adding a natural dyeing assistant, adding water, and uniformly stirring at a high speed to prepare a dye solution; putting the dried pure cotton fabric into a dye solution for dyeing; and adding a low-temperature soaping agent into the dye liquor, soaping the dyed pure cotton fabric, taking out, washing, and drying at low temperature to obtain the dyed pure cotton fabric.
CN102493220B relates to a method for dyeing acrylic fabric by using bacterial dye prodigiosin, which comprises the following steps: (1) dissolving prodigiosin in ethyl acetate or N, N-dimethylformamide, and then adding the dissolved prodigiosin into water to prepare a dyeing solution; (2) the dyeing solution is adopted to dye the acrylic fabric, the mass fraction of the prodigiosin is 0.1-6%, the dyeing bath ratio is 1: 5-20, the pH value of the dye solution is adjusted to 4.0-6.0, the dyeing temperature is 80-90 ℃, and the dyeing time is 30-90 min.
CN106011195A discloses a preparation method of prodigiosin for silk fabric dyeing, which adjusts the original culture process of prodigiosin to make the effect of the cultured prodigiosin applied to silk fabric better, especially under the condition of heavier dyeing, the dosage of the added prodigiosin and the time required by dyeing are greatly improved, chemical reagents such as mordants and the like are not required to be added in the dyeing process, the cost is low, and the method is healthy and environment-friendly.
According to the patent technology, at present, in the dyeing process aiming at bacterial dyes, a dip dyeing mode is adopted, and the prodigiosin dye solution needs to use an organic solvent to extract pigments and dissolve the pigments in the dye solution, so that the dyeing cost is obviously increased, and the pollution problem exists. The defects of cost saving, production efficiency improvement and suitability for industrialized mass production cannot be overcome. The padding dyeing mode is adopted, and the problem is that the prodigiosin dye solution is insoluble in water due to intracellular pigments, and the organic solvent is required to be used for extraction before utilization to prepare the dye solution. In addition, an organic solvent is required to dissolve the pigment during the dyeing process. After the pigment is extracted by the conventional organic solvent, the pigment is in a molecular or ionic dissolved state in the organic solvent. In the process of adding water to prepare the dye solution, because the pigment is insoluble in water, a small amount of the pigment added into water is still in a dissolved state, if a large amount of the pigment is added into water, the pigment can be separated out from the solution, but the separated granular pigment can not dye cotton fabrics, because only the pigment in a molecular or ionic state can be deposited on the surface and the inside of the fibers in a water bath environment. Even through adjusting the water adding amount to the optimal proportion, the dye liquor contains a large amount of organic solvents, the cost is still huge even if a dip dyeing mode is adopted, the amount of wastewater is huge, the pad dyeing process is adopted, the cost of the organic solvents is high, the amount of wastewater is large, a steaming process is needed, the organic solvents can volatilize in a large amount in the steaming process, the environmental pollution is aggravated, the organic solvents cannot be subsequently recovered, the production cost can be increased, and the industrial batch production cannot be really realized. Therefore, how to solve the problems of saving cost, improving production efficiency, being suitable for industrialized batch production and the like is an urgent problem which puzzles the technical personnel in the field of cotton fabric bacterial dye dyeing.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to solve the technical problem of providing a preparation method and application of pure water-based bacterial dye prodigiosin nano suspension dye liquor, which can directly obtain the dye liquor without organic solvent extraction, realize the preparation of the dye liquor without organic solvent addition under the condition that prodigiosin pigment is insoluble in water, and effectively improve the dye-uptake rate, the utilization rate of prodigiosin and the color fixing effect.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a preparation method of a pure water system bacterial dye prodigiosin nanometer suspension dye liquor comprises the following steps:
(1) activating ATCC8100 serratia marcescens, and inoculating the serratia marcescens colony with the largest colony and the deepest color in the third generation strain into a seed culture solution, wherein the seed culture solution comprises the following components in percentage by mass: 5g/L of yeast powder, 10g/L of peptone, 3g/L of sodium chloride and 2g/L of potassium chloride;
(2) culturing the serratia marcescens seed liquid in a constant-temperature culture oscillator for 12 hours at the temperature of 30 ℃, the rotating speed of a shaking table is 160rpm, and naturally illuminating indoors;
(3) the seed culture solution is transferred into a fermentation culture medium by using a liquid transfer gun for fermentation culture at the temperature of 28 ℃, the rotating speed of a shaking table is 200rpm, the light-shielding culture is carried out, the pH is adjusted to 6.0, the culture time is 72 hours, and the fermentation culture medium consists of the following components in percentage by mass: 15g/L of peptone, 3g/L of sodium chloride, 2g/L of potassium chloride, 2g/L of magnesium sulfate, 4g/L of glycerol and 18g/L of surfactant;
(4) under the action of a shaking table, transferring the prodigiosin pigment from the cells to a fermentation medium to form a plurality of nano-scale granular pigment particles, quickly coating the nano-scale granular pigment particles by a surfactant, and forming a large number of nano-scale prodigiosin micelle particles in a culture solution;
(5) and after the fermentation is finished, removing thalli in the fermentation liquor by using a high-speed refrigerated centrifuge through high-speed low-temperature centrifugation to obtain the pure water-based prodigiosin nano-suspension dye liquor containing a large number of prodigiosin micelle particles.
The preparation method of the pure water system bacterial dye prodigiosin nano suspension dye liquor is characterized by comprising the following steps: in the step (4), the prodigiosin micelle particle is of a tetrahedral structure similar to a triangular pyramid shape and is provided with four planes which can be in random contact with the surface of the cotton fabric.
In the preparation method of the pure water system bacterial dye prodigiosin nano suspension dye liquor, the surfactant in the step (3) is tween-80.
According to the preparation method of the pure water system bacterial dye prodigiosin nanometer suspension dye solution, the particle size distribution range of the prodigiosin micelle particles in the pure water system prodigiosin nanometer suspension dye solution obtained in the step (4) is 77-222 nm.
The preparation method of the pure water system bacterial dye prodigiosin nanometer suspension dye liquor comprises the step (4) of rotating the high-speed refrigerated centrifuge at 10000rpm, the centrifugation temperature at 20 ℃ and the centrifugation time for 10 min.
An application of pure water system bacterial dye prodigiosin nanometer suspension dye liquor in a cotton fabric padding dyeing process.
In the above application, the padding dyeing process comprises the following steps:
(1) preparing pure water prodigiosin nano suspension dye liquor with required quantity for later use;
(2) and pH blending: adjusting the pH value of the pure water system prodigiosin nanometer suspension dye liquor to 2.5-3.5 by using 1mol/L hydrochloric acid solution;
(3) and padding cotton fabrics: soaking the cotton fabric in the dye liquor for 30 seconds, rolling the cotton fabric by using a padder, and removing the redundant dye liquor on the cotton fabric, wherein the padding times are one-padding to five-padding, the pressure of the padder is 0.25 bar-1.0 bar, and the rolling allowance rate is 75-85%;
(4) and steaming: steaming the padded cotton fabric for 1-9 min;
(5) soap boiling: performing soap boiling color fixation on the steamed cotton fabric, wherein the concentration of soap flakes in soap solution is 2g/L, and the soap boiling time is 5 min;
(6) and (3) washing: taking out the cotton fabric after soap boiling, and washing the cotton fabric with cold water to remove loose color;
(7) and drying: and (4) drying the cleaned cotton fabric in an oven at the drying temperature of 70 ℃ for 5 min.
In the application, the padding times in the step (3) are four-padding and four-rolling, the pressure of a padder is 0.75bar, and the rolling residual rate is 80%.
In the above application, the steaming time in the step (4) is 5 min.
In the application, the cotton fabric is a pure cotton plain weave fabric, the warp yarn is 10.6tex, the weft yarn is 10.6tex, the warp density is 524 pieces/10 cm, the weft density is 283 pieces/10 cm, and the fabric surface density is 106.6 g/square meter.
The preparation method and the application of the pure water system bacterial dye prodigiosin nano suspension dye liquor have the advantages that: based on the acquisition mechanism, the prodigiosin pigment is not extracted by an organic solvent, and the extraction of prodigiosin and the preparation of a dye solution do not need any organic solvent, so that the production cost is effectively saved. The pure water system prodigiosin nanometer suspension dye liquor directly obtained by microbial fermentation is adopted, the dye liquor is in a nanometer-level prodigiosin micelle suspension state, the prodigiosin pigment exists in a nanometer-level particle suspension state in the dye liquor, the prodigiosin pigment does not need to be dissolved in the dye liquor, the solid is dissolved into a molecular state for releasing under the thermal acid environment of the prodigiosin in the steaming process, the diffusion and adsorption are carried out on the surface and the inside of the fiber, the dyeing is carried out, and the color fixation is realized in the soaping process. The cotton fabric is dyed by adopting a pad dyeing method, compared with dip dyeing, the dyeing process is shortened from 1-2 hours to 10-15 minutes, and the process flow is obviously shortened. Meanwhile, the utilization rate of the dye is obviously improved, and the utilization rate (dye uptake) of prodigiosin is improved to 34.9%. The pad dyeing process adopted by the invention greatly improves the production efficiency, is suitable for industrial batch production and application, and is a great innovation in the field of bacterial dye dyeing process.
Drawings
FIG. 1 is a process flow diagram for preparing a prodigiosin nano-suspension dye liquor of the present invention;
FIG. 2 is a schematic diagram of the transfer of prodigiosin pigment from the interior of thalli to the fermentation broth during the microbial fermentation process;
FIG. 3 is a graph of the distribution of the particle size of the prodigiosin micelle particles in the dye liquor;
FIG. 4 is an electron micrograph of prodigiosin micelle particles in a dye solution;
FIG. 5 is a flow chart of a padding dyeing process for cotton fabric by using the dye liquor of the invention.
Detailed Description
The invention is further described in detail below with reference to the drawings and specific embodiments.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
The microbial pigments can be divided into intracellular pigments and extracellular pigments, wherein most of the microbial pigments are enriched in thalli after being produced and are intracellular pigments, and the microbial pigments are generally low in water solubility and easy to dissolve in organic solvents such as ethanol and ethyl acetate. Prodigiosin is used as an intracellular pigment, most of the pigment exists in a bacterial body in a common fermentation culture solution, and when the prodigiosin is used as a dye for dyeing textiles at present, the prodigiosin is generally extracted from cells by using an organic solvent, and is prepared into a dye solution after being appropriately concentrated, and then the textiles are dyed. A large amount of organic solvent is inevitably used in the processes of extracting the pigment and preparing the dye liquor, which deviates from the concept of green and environment-friendly natural fuel and the development trend of ecological textiles.
Preparation of prodigiosin nano suspension dye liquor by microbial fermentation
As shown in figure 1, a preparation method of a pure water system bacterial dye prodigiosin nano suspension dye liquor comprises the following steps:
(1) activating ATCC8100 serratia marcescens, and inoculating the serratia marcescens colony with the largest colony and the deepest color in the third generation strain into a seed culture solution, wherein the seed culture solution comprises the following components in percentage by mass: 5g/L of yeast powder, 10g/L of peptone, 3g/L of sodium chloride and 2g/L of potassium chloride;
(2) culturing serratia marcescens seed liquid in a constant-temperature culture oscillator for 12h at 30 ℃, wherein the rotating speed of a shaking table is 160rpm, and naturally illuminating indoors;
(3) transferring the seed culture solution to a fermentation culture medium by using a liquid transfer gun for fermentation culture at the temperature of 28 ℃, with the rotating speed of a shaking table of 200rpm, performing light-shielding culture, adjusting the pH value to 6.0, and culturing for 72 hours, wherein the fermentation culture medium comprises the following components in percentage by mass: 15g/L of peptone, 3g/L of sodium chloride, 2g/L of potassium chloride, 2g/L of magnesium sulfate, 4g/L of glycerol and 18g/L of surfactant;
(4) under the action of a shaking table, transferring the prodigiosin pigment into a fermentation medium from the interior of cells to form a plurality of nano-scale granular pigment particles, quickly coating the nano-scale granular pigment particles by using a surfactant, and forming a large number of nano-scale prodigiosin micelle particles in a culture solution;
(5) and after the fermentation is finished, removing thalli in the fermentation liquor by using a high-speed refrigerated centrifuge through high-speed low-temperature centrifugation to obtain the pure water-based prodigiosin nano-suspension dye liquor containing a large number of prodigiosin micelle particles. The rotation speed of the high-speed freezing centrifuge is 10000rpm, the centrifugation temperature is 20 ℃, and the centrifugation time is 10 min.
The prodigiosin serving as a microbial intracellular pigment has extremely low solubility in water, so that in a common culture medium, most of the prodigiosin gathers in thalli, only a small part of pigment is secreted into the culture medium, when the components of a fermentation liquid and the fermentation conditions are fixed, the pigment content in the thalli and the pigment content in the fermentation liquid are in a certain proportion, and the content of the prodigiosin in the thalli and the content of the prodigiosin free in the fermentation liquid in the common fermentation liquid are about 59: 1. The fermentation preparation mechanism of the prodigiosin nanometer suspension dye liquor is shown in figure 2, a certain amount of surfactant Tween-80 is added into fermentation liquor, and because the concentration is far higher than the critical micelle concentration, Tween-80 molecules can form a large amount of micelles in the fermentation liquor, namely Tween 80 micelle 1. During the fermentation process, prodigiosin 3 is generated inside the thalli 2, and a small amount of pigment enters the fermentation liquor through cell membranes and cell walls. The prodigiosin 3 is almost insoluble in water and has strong hydrophobicity, and the prodigiosin particles in the fermentation liquor are coated in the Tween-80 micelles to form the prodigiosin-Tween-80 micelles 5 in the continuous shaking culture dynamic fermentation process 4. Because the free prodigiosin 3 in the fermentation liquor is coated by the surfactant, the balance proportion relation between intracellular pigments and extracellular pigments of thalli is broken, and the prodigiosin 3 in the thalli 2 is further transferred to the outside of the thalli. In addition, the nonionic surfactant can increase the permeability of cell membrane and cell wall of the thallus 2, and is helpful for transferring intracellular prodigiosin 3 to the outside. Thus, as the fermentation process 4 is carried out, the intracellular prodigiosin 3 is continuously generated and transferred to the outside of the cell, so that more prodigiosin-Tween-80 micelles 5 are formed, and after the thallus removing process 6, the pure water-based prodigiosin nano suspension dye solution 7 containing a large number of prodigiosin micelle particles is obtained.
As shown in figures 2 and 3, in the pure water-based prodigiosin nano-suspension dye solution obtained by adopting a surfactant fermentation system, the particle size distribution range of prodigiosin micelle particles is 77-222 nm. The prodigiosin micelle particles are in a stable and uniform suspension state in the dye solution, the nano prodigiosin in the dye solution is dispersed in water in the form of small particles, and the size of the prodigiosin particles is in a nano level. In addition, the nano-prodigiosin obtained by the fermentation method is coated by the surfactant micelle, the hydrophilic end of the surfactant faces outwards, the nano-prodigiosin is in the micelle, the pigment size is small, and the surfactant coating can ensure the stability and uniformity of the dye solution, thereby being beneficial to the color uniformity of dyed fabrics. Prodigiosin is insoluble in water under neutral conditions, and the solubility is increased along with the increase of the acidity of the solution. In the pad dyeing process, the pH value of the dye liquor is adjusted to about 3, the solubility of the small particles of the prodigiosin is increased in the steaming process of pad dyeing, namely under the acidic high-temperature condition, and the small particles of the prodigiosin are dissolved in the nano level due to small size, so that the dissolving of the small particles of the pigment is facilitated, and the more the pigment is dissolved, the better the dyeing effect on the fabric is.
As shown in the electron microscope photograph of fig. 4, in the step (4) of this embodiment, the prepared nano-grade prodigiosin micelle particle has a tetrahedral structure similar to a triangular pyramid, also called a triangular pyramid, and has four planes capable of contacting with the surface of the cotton fabric at will. Compared with spherical particles, each surface of the pigment particles with the tetrahedral structure is a plane, so that the pigment particles can be more easily adsorbed and fixed on the surface of a fabric, including the positions of fiber surfaces, fiber gaps and the like, during padding, steaming and soaping in a pad dyeing process. The planar structure enables the contact area between the pigment particles and the surface of the fabric to be larger, so that the pigment molecules can be used for dyeing cotton fabrics immediately after the pigment particles are dissolved under the hot acidic condition, the dyeing efficiency and the dyeing rate are effectively improved, and the color fixing capability is improved.
In this embodiment, in order to improve the dye uptake and color fixing effect of the prodigiosin pigment in the pad dyeing process, a culture mode of shaking by an oscillator and rotation by a shaking table is adopted in the step (2), so as to enable strains to be rapidly propagated in a large quantity, generate more strains and improve the yield of the prodigiosin pigment. In the culture process of the step (3), the secondary shaking table function is adopted, and the following advantages are shared: 1. 2, stimulating the strain to generate a large amount of prodigiosin pigment, 3, accelerating the extraction speed of the pigment under the action of a surfactant, 4, quickly coating the prodigiosin nanoparticle pigment by the surfactant to form a micelle of the nanoparticle pigment, 5, quickly coating the nanoparticle pigment by the surfactant to prevent the pigment particles transferred from the cells from agglomerating into larger pigment particles, wherein the pigment particles can not form a stable suspension state after being coated and can not be easily dissolved to form pigment molecules under the condition of thermal acidity and influence the dyeing.
In this example, the surfactant was tween-80. Wherein, the surfactant actually plays a role of an extracting agent in the fermentation process, and the prodigiosin pigment generated in cells is continuously extracted. After long-time shake culture, a large amount of prodigiosin-Tween 80 micelles are formed in the fermentation liquor, and the thalli are removed to obtain the prodigiosin suspension. Later tests show that the prodigiosin particles in the fermentation liquor are in a nanometer level, and the prodigiosin is transferred from the interior of thalli to the fermentation liquor and immediately coated by Tween-80, so that pigment agglomeration is prevented, and a stable nanometer prodigiosin suspension system is formed. The prodigiosin nanometer suspension dye liquor is directly obtained by utilizing the idea of direct preparation of a surfactant fermentation system, the steps of firstly extracting pigment by using an organic solvent and then preparing the dye liquor by using the organic solvent are not needed, the dye liquor which can be used for padding and dyeing cotton fabrics is directly obtained after microbial fermentation is completed, the process flow of dye liquor preparation is shortened, the cost is saved, and the production efficiency is improved.
Second, relates to application of pure water system bacterial dye prodigiosin nanometer suspension dye liquor in padding dyeing process of cotton fabrics
Example 1:
as shown in figure 5, the padding dyeing process of the pure water system bacterial dye prodigiosin nanometer suspension dye for cotton fabrics comprises the following steps:
(1) preparing pure water prodigiosin nano suspension dye liquor with required amount for later use;
(2) and pH blending: adjusting the pH value of the pure water system prodigiosin nano suspension dye solution to 2.5 by using 1mol/L hydrochloric acid solution;
(3) and padding cotton fabrics: soaking the cotton fabric in a dye solution for 30 seconds, rolling the cotton fabric by using a padder, and removing the redundant dye solution on the cotton fabric, wherein the padding times are one padding and one rolling, the padder pressure is 0.25bar, and the percent of padding is 75%;
(4) and steaming: steaming the padded cotton fabric for 1 min;
(5) soap boiling: performing soap boiling color fixation on the steamed cotton fabric, wherein the concentration of soap flakes in soap solution is 2g/L, and the soap boiling time is 5 min;
(6) and washing with water: taking out the cotton fabric after soap boiling, and washing the cotton fabric with cold water to remove loose color;
(7) and drying: and (4) drying the cleaned cotton fabric in an oven at the drying temperature of 70 ℃ for 5 min.
The cotton fabric to be padded and dyed selected in the embodiment is a pure cotton plain weave fabric, the warp yarn is 10.6tex, the weft yarn is 10.6tex, the warp density is 524 pieces/10 cm, the weft density is 283 pieces/10 cm, and the fabric surface density is 106.6 g/square meter.
In actual industrial production, in order to improve the loose color removing effect, after the steaming in the step (4) is finished, a cold water cleaning process can be carried out, or warm water and cold water are respectively cleaned once, and after soap boiling, a mode that warm water and cold water are respectively cleaned once can be adopted, so that the practical situation can be selected for use according to production requirements or product quality requirements.
Prodigiosin has a special property that it is insoluble in water under neutral conditions and increases in solubility in water under acidic conditions. By utilizing the property of the prodigiosin, the pH of a dye solution is adjusted to be acidic, and the prodigiosin is partially dissolved under the high-temperature condition of dyeing, and the prodigiosin is nano-grade, so that the dissolution of the prodigiosin under the thermal acidic condition is also facilitated. In the pad dyeing and steaming process, dissolved pigment molecules enter the interior of cotton fibers, the acid-base environment on the cotton fibers is changed into neutral by washing and soaping after dyeing is finished, and the prodigiosin is changed into an insoluble state from a dissolved state, so that the prodigiosin is deposited in the fibers, the dyeing is realized, and better fastness is obtained. Compared with the prior art, the pH value adjustment method is different from the prior art in that the dye solution is acidic, more importantly, the thermal acidity degree needs to be controlled, namely, the pH value and the steaming temperature are accurately matched, so that pigment particles in the prodigiosin-Tween-80 micelle 5 can be dissolved into pigments in molecular and ionic forms to the maximum extent, and the structure of cotton fabric fibers cannot be damaged, which is a core technical means of the invention.
The most important technical means of the present invention include two, the first is to adjust the pH of the dyeing to about 3, the main purpose of which is discussed above. The second important step is steaming, which is more favorable for dissolving prodigiosin through the high-temperature condition of steaming. The second effect of steaming is to transfer the pigment molecules to the interior of the fiber, which is the same as steaming in a conventional pad dyeing process. After steaming is finished, the cotton fabric is subjected to water washing and soaping, the process is the same as the traditional pad dyeing, but a water system and the soaping are ingeniously utilized, so that the internal environment of the fiber is changed from acidity to alkalinity, and the prodigiosin is changed from a dissolved state to an insoluble state, so that the pigment is fixed in the fiber, and good dyeing fastness is obtained.
Example 2:
the same parts of this embodiment as those of embodiment 1 are not described again, but the differences are as follows:
(2) and pH blending: adjusting the pH value of the pure water system prodigiosin nano suspension dye solution to 3 by using 1mol/L hydrochloric acid solution;
(3) and padding cotton fabrics: soaking the cotton fabric in the dye liquor for 30 seconds, rolling the cotton fabric by using a padder, and removing the redundant dye liquor on the cotton fabric, wherein the padding times are three-soaking and three-rolling, the padder pressure is 0.75bar, and the percent of afterrolling is 80%;
(4) and steaming: steaming the padded cotton fabric for 5 min;
example 3:
the same parts of this embodiment as those of embodiments 1 and 2 are not described again, but the differences are as follows:
(2) and pH blending: adjusting the pH value of the pure water system prodigiosin nano suspension dye solution to 3.5 by using 1mol/L hydrochloric acid solution;
(3) and padding cotton fabrics: soaking the cotton fabric in a dye solution for 30 seconds, rolling the cotton fabric by using a padder, and removing the redundant dye solution on the cotton fabric, wherein the padding times are five-padding and five-padding, the padder pressure is 1.0bar, and the percent mangle is 85%;
(4) and steaming: steaming the padded cotton fabric for 9 min;
example 4:
(1) adjusting the pH value of the prodigiosin nano suspension dye liquor to 3 by using 1mol/L hydrochloric acid solution;
(2) soaking the cotton fabric in the dye liquor for 30 seconds, rolling the cotton fabric by using a padder, rolling off the redundant dye liquor on the cotton fabric, wherein the pressure of the padder is 0.75bar, and repeating for four times (namely four-soaking and four-rolling);
(3) placing the cotton fabric into a steaming box to be steamed by using saturated steam for 5 min;
after steaming, washing the cotton fabric with cold water;
(4) then soap boiling is carried out, the concentration of soap flakes in soap liquid used for soap boiling is 2g/L, the soap boiling temperature is 100 ℃, and the time is 5 min;
(5) washing the cotton fabric with cold water after finishing soap boiling;
(6) and drying the cotton fabric in an oven at 70 ℃ for 5 min.
Example 5:
(1) adjusting the pH value of the prodigiosin nano suspension dye liquor to 3.5 by using 1mol/L hydrochloric acid solution;
soaking the cotton fabric in the dye liquor for 30 seconds, rolling the cotton fabric by using a padder, rolling off the redundant dye liquor on the cotton fabric, wherein the pressure of the padder is 0.5bar, and repeating for four times (namely four-soaking and four-rolling);
(2) placing the cotton fabric into a steaming box to be steamed by using saturated steam for 5 min;
(3) after steaming, washing the cotton fabric with cold water;
(4) then soap boiling is carried out, the concentration of soap flakes in soap liquid used for soap boiling is 2g/L, the soap boiling temperature is 100 ℃, and the time is 5 min;
(5) washing the cotton fabric with cold water after finishing soap boiling;
(6) and drying the cotton fabric in an oven at 70 ℃ for 5 min.
Example 6:
(1) adjusting the pH value of the prodigiosin nano suspension dye liquor to 3 by using 1mol/L hydrochloric acid solution;
(2) soaking the cotton fabric in the dye solution for 30 seconds, rolling the cotton fabric by using a padder, removing the redundant dye solution on the cotton fabric, wherein the pressure of the padder is 0.75bar, and repeating for four times (namely four-soaking and four-rolling);
(3) placing the cotton fabric into a steaming box to be steamed by using saturated steam for 10 min;
after steaming, washing the cotton fabric with cold water;
(4) then soap boiling is carried out, the concentration of soap flakes in soap liquid used for soap boiling is 2g/L, the soap boiling temperature is 100 ℃, and the time is 5 min;
(5) washing the cotton fabric with cold water after finishing soap boiling;
(6) and drying the cotton fabric in an oven at 70 ℃ for 5 min.
Thirdly, testing the performance of the dyed fabric:
after the dyeing is finished, the K/S value of the dyed fabric is measured using a Datacolor colorimeter (this value is used to characterize the color depth of the fabric).
The color fastness to rubbing is determined according to GB/T3920-2008 "color fastness to rubbing" of textile color fastness test ".
Soaping color fastness is determined according to GB/T3921-2008 textile color fastness test soaping color fastness: test 1.
The method for measuring the dye utilization rate comprises the following steps:
(1) 0.04g of dyed cotton fabric with the flooding removed by soap boiling is accurately weighed, cut into pieces and put into a 5mL centrifuge tube, then 4mL of 90% acidic ethanol aqueous solution (pH 3.0) is added, and the mixture is kept stand for 24 hours, so that the prodigiosin in the cotton fiber is fully dissolved in the ethanol solution. The mixture was centrifuged at 8000rpm for 5 minutes using a centrifuge, and the supernatant was collected to determine the absorbance at 535 nm. And calculating the mass (mass 1) of the prodigiosin on the dyed cotton fabric according to a standard curve of the corresponding relation between the concentration and the absorbance of the prodigiosin standard substance solution, the weight of the used fabric and the using amount of the ethanol solution.
(2) And (3) directly drying the fabric after padding the fabric with dye liquor in the dyeing process without steaming and subsequent processes, wherein the quality (quality 2) of the prodigiosin on the cotton fabric after padding the dye liquor is obtained by adopting the method in the step (1) for the dried fabric. And dividing the mass 1 by the mass 2 to calculate the fixation rate (namely the dye utilization rate) of the prodigiosin to the pad dyeing of the cotton fabric.
The performance test result of cotton fabric pad-dyed by the prodigiosin nano-suspension liquid is as follows:
| example 4 | Example 5 | Example 6 | |
| K/S value | 0.52 | 0.45 | 0.51 |
| Dye uptake | 34.9％ | 29.5％ | 34.8％ |
| Colour fastness to dry rubbing | 5 | 5 | 5 |
| Color fastness to wet rubbing | 5 | 5 | 5 |
| Color fastness to soaping | 4 | 4 | 4 |
| Color fastness to soaping |
5 | 5 | 5 |
| Color fastness to soaping hair staining | 5 | 5 | 5 |
The pad dyeing method for cotton fabrics by utilizing the prodigiosin nano-suspension dye liquor directly prepared by a surfactant fermentation system developed by the invention breakthroughs the problem that the water-insoluble pigment dye liquor prepared by a microbial fermentation technology cannot be directly used for dyeing cotton fabrics. The dye-uptake mechanism of the invention is directly prepared by microbial fermentation, complex processes of pigment extraction, concentration, purification and dye liquor preparation are not needed, complex preparation processes of common dispersion liquid are not needed, the requirement on equipment is low, time and raw materials are saved, the dye-uptake rate is improved to more than 34%, and the utilization rate of prodigiosin is obviously improved. The method is energy-saving and environment-friendly, is simple to operate, has industrial production conditions, and promotes the development of cotton fabric bacterial dye dyeing technology.
It is to be understood that the above description is not intended to limit the present invention, and the present invention is not limited to the above examples, and those skilled in the art should understand that they can make various changes, modifications, additions and substitutions within the spirit and scope of the present invention.
Claims (10)
1. A preparation method of a pure water system bacterial dye prodigiosin nanometer suspension dye liquor is characterized by comprising the following steps:
(1) activating ATCC8100 serratia marcescens, and inoculating the serratia marcescens colony with the largest colony and the deepest color in the third generation strain into a seed culture solution, wherein the seed culture solution comprises the following components in percentage by mass: 5g/L of yeast powder, 10g/L of peptone, 3g/L of sodium chloride and 2g/L of potassium chloride;
(2) culturing serratia marcescens seed liquid in a constant-temperature culture oscillator for 12h at 30 ℃, wherein the rotating speed of a shaking table is 160rpm, and naturally illuminating indoors;
(3) transferring the seed culture solution to a fermentation culture medium by using a liquid transfer gun for fermentation culture at the temperature of 28 ℃, with the rotating speed of a shaking table of 200rpm, performing light-shielding culture, adjusting the pH value to 6.0, and culturing for 72 hours, wherein the fermentation culture medium comprises the following components in percentage by mass: 15g/L of peptone, 3g/L of sodium chloride, 2g/L of potassium chloride, 2g/L of magnesium sulfate, 4g/L of glycerol and 18g/L of surfactant;
(4) under the action of a shaking table, transferring the prodigiosin pigment into a fermentation medium from the interior of cells to form a plurality of nano-scale granular pigment particles, quickly coating the nano-scale granular pigment particles by using a surfactant, and forming a large number of nano-scale prodigiosin micelle particles in a culture solution;
(5) and after the fermentation is finished, removing thalli in the fermentation liquor by using a high-speed refrigerated centrifuge through high-speed low-temperature centrifugation to obtain the pure water-based prodigiosin nano-suspension dye liquor containing a large number of prodigiosin micelle particles.
2. The preparation method of pure water-based bacterial dye prodigiosin nano suspension dye liquor according to claim 1, which is characterized in that: in the step (4), the prodigiosin micelle particle is of a tetrahedral structure similar to a triangular pyramid shape and is provided with four planes which can be in random contact with the surface of the cotton fabric.
3. The preparation method of pure water-based bacterial dye prodigiosin nano suspension dye liquor according to claim 1, which is characterized in that: and (4) in the step (3), the surfactant is tween-80.
4. The preparation method of the pure water-based bacterial dye prodigiosin nano-suspension dye solution according to claim 1, which is characterized in that: the particle size distribution range of the prodigiosin micelle particles in the pure water system prodigiosin nano suspension dye solution obtained in the step (4) is 77-222 nm.
5. The preparation method of the pure water-based bacterial dye prodigiosin nano-suspension dye solution according to claim 1, which is characterized in that: and (4) enabling the rotation speed of the high-speed refrigerated centrifuge in the step (4) to be 10000rpm, the centrifugation temperature to be 20 ℃ and the centrifugation time to be 10 min.
6. The application of the pure water system bacterial dye prodigiosin nano suspension dye liquor obtained by the preparation method of any one of claims 1-5 in the padding dyeing process of cotton fabrics.
7. Use according to claim 6, characterized in that the pad dyeing process comprises the following steps:
(1) preparing pure water prodigiosin nano suspension dye liquor with required amount for later use;
(2) and pH blending: adjusting the pH value of the pure water system prodigiosin nano suspension dye solution to 2.5-3.5 by using 1mol/L hydrochloric acid solution;
(3) and padding cotton fabrics: soaking the cotton fabric in the dye liquor for 30 seconds, rolling the cotton fabric by using a padder, and removing the redundant dye liquor on the cotton fabric, wherein the padding times are one-padding to five-padding, the pressure of the padder is 0.25 bar-1.0 bar, and the rolling allowance rate is 75-85%;
(4) and steaming: steaming the padded cotton fabric for 1-9 min;
(5) soap boiling: performing soap boiling color fixation on the steamed cotton fabric, wherein the concentration of soap flakes in soap solution is 2g/L, and the soap boiling time is 5 min;
(6) and washing with water: taking out the cotton fabric after soap boiling, and washing the cotton fabric with cold water to remove loose color;
(7) and drying: and (3) drying the cotton fabric after cleaning in an oven at the drying temperature of 70 ℃ for 5 min.
8. Use according to claim 7, characterized in that: in the step (3), the padding frequency is four-padding and four-padding, the padder pressure is 0.75bar, and the rolling residual rate is 80%.
9. Use according to claim 7, characterized in that: and the steaming time in the step (4) is 5 min.
10. Use according to claim 7, characterized in that: the cotton fabric is a pure cotton plain weave fabric, the warp yarn is 10.6tex, the weft yarn is 10.6tex, the warp density is 524 pieces/10 cm, the weft density is 283 pieces/10 cm, and the fabric surface density is 106.6 g/square meter.
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