CN114921112B - Preparation method and application of pure water system bacterial dye prodigiosin nano suspension dye solution - Google Patents
Preparation method and application of pure water system bacterial dye prodigiosin nano suspension dye solution Download PDFInfo
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- CN114921112B CN114921112B CN202210650916.6A CN202210650916A CN114921112B CN 114921112 B CN114921112 B CN 114921112B CN 202210650916 A CN202210650916 A CN 202210650916A CN 114921112 B CN114921112 B CN 114921112B
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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 125
- 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 125
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000006070 nanosuspension Substances 0.000 title claims abstract description 37
- 230000001580 bacterial effect Effects 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000004744 fabric Substances 0.000 claims abstract description 127
- 229920000742 Cotton Polymers 0.000 claims abstract description 106
- 238000004043 dyeing Methods 0.000 claims abstract description 80
- 238000000034 method Methods 0.000 claims abstract description 58
- 238000000855 fermentation Methods 0.000 claims abstract description 49
- 230000004151 fermentation Effects 0.000 claims abstract description 49
- 230000008569 process Effects 0.000 claims abstract description 45
- 239000002245 particle Substances 0.000 claims abstract description 40
- 239000000693 micelle Substances 0.000 claims abstract description 28
- 241000607715 Serratia marcescens Species 0.000 claims abstract description 12
- 238000012258 culturing Methods 0.000 claims abstract description 10
- 238000011218 seed culture Methods 0.000 claims abstract description 10
- 239000001963 growth medium Substances 0.000 claims abstract description 9
- 241001052560 Thallis Species 0.000 claims abstract description 7
- 230000009471 action Effects 0.000 claims abstract description 6
- 230000003213 activating effect Effects 0.000 claims abstract description 4
- 239000000049 pigment Substances 0.000 claims description 73
- 239000000243 solution Substances 0.000 claims description 58
- 238000010025 steaming Methods 0.000 claims description 38
- 239000000344 soap Substances 0.000 claims description 35
- 238000009835 boiling Methods 0.000 claims description 26
- 239000004094 surface-active agent Substances 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 20
- 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
- 238000005096 rolling process Methods 0.000 claims description 10
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 8
- 230000001105 regulatory effect Effects 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- 238000007667 floating Methods 0.000 claims description 7
- 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
- 239000002105 nanoparticle Substances 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
- 238000005119 centrifugation Methods 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000011248 coating agent Substances 0.000 claims description 4
- 238000000576 coating method Methods 0.000 claims description 4
- 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
- 238000005286 illumination Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 23
- 238000009980 pad dyeing Methods 0.000 abstract description 20
- 239000000725 suspension Substances 0.000 abstract description 9
- 238000005516 engineering process Methods 0.000 abstract description 8
- 239000000975 dye Substances 0.000 description 128
- 239000003960 organic solvent Substances 0.000 description 24
- 239000007788 liquid Substances 0.000 description 15
- 239000004753 textile Substances 0.000 description 13
- 230000000813 microbial effect Effects 0.000 description 11
- 239000000835 fiber Substances 0.000 description 10
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 9
- 230000002378 acidificating effect Effects 0.000 description 8
- 230000003834 intracellular effect Effects 0.000 description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 210000004027 cell Anatomy 0.000 description 6
- 238000011161 development Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000000605 extraction Methods 0.000 description 5
- 230000007246 mechanism Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
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- 230000007935 neutral effect Effects 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000000985 reactive dye Substances 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 239000000979 synthetic dye Substances 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 210000000170 cell membrane Anatomy 0.000 description 2
- 210000002421 cell wall Anatomy 0.000 description 2
- 230000008859 change Effects 0.000 description 2
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- 238000007598 dipping method Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
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- 244000005700 microbiome Species 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000984 vat dye Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 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
- 239000002028 Biomass Substances 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
- 230000001133 acceleration Effects 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000000078 anti-malarial effect Effects 0.000 description 1
- 239000003430 antimalarial agent Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 210000005056 cell body Anatomy 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
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- 238000005520 cutting process Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 210000001723 extracellular space Anatomy 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000978 natural dye Substances 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000000644 propagated effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 125000000168 pyrrolyl group Chemical group 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229930000044 secondary metabolite Natural products 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- 230000009466 transformation Effects 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
- 238000005303 weighing Methods 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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- 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
- 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
- C09B67/0096—Purification; Precipitation; Filtration
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- C12N—MICROORGANISMS OR ENZYMES; COMPOSITIONS THEREOF; PROPAGATING, PRESERVING, OR MAINTAINING MICROORGANISMS; MUTATION OR GENETIC ENGINEERING; CULTURE MEDIA
- 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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- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- 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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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- 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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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- D06B21/00—Successive treatments of textile materials by liquids, gases or vapours
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- 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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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06B—TREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
- 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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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/0004—General aspects of dyeing
- D06P1/0016—Dye baths containing a dyeing agent in a special form such as for instance in melted or solid form, as a floating film or gel, spray or aerosol, or atomised dyes
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/34—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using natural dyestuffs
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
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- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- 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 bacterial dye prodigiosin nanometer suspension dye liquor, comprising the following steps: (1) activating ATCC8100 Serratia marcescens; (2) Culturing Serratia marcescens seed solution in a constant temperature culture shaker; (3) Transferring the seed culture solution into a fermentation culture medium by using a pipetting gun for fermentation culture; (4) Forming a large number of nano-scale prodigiosin micelle particles in the culture solution under the action of a shaking table; (5) Removing thalli in the fermentation liquor to obtain the pure water system prodigiosin nanometer suspension dye liquor. The method also comprises the application of the pure water system bacterial dye prodigiosin nano-suspension dye liquor in cotton fabric padding dyeing process. The invention obviously improves the dye utilization rate, and improves the dye-uptake rate of the prodigiosin to 34.9%. The invention adopts pad dyeing technology to greatly improve production efficiency, is suitable for industrialized mass production and application, and is a great innovation in the field of bacterial dye dyeing technology.
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 pillar industry and the important civil industry in China. Currently, with the acceleration of new and old kinetic energy conversion, as a resource-dependent and environment-sensitive industry, the development of the textile industry is increasingly stressed and constrained. The textile printing and dyeing processing is a key processing link for realizing structure adjustment and transformation upgrading in the textile industry, and the cleanliness of the production process and the ecologization of products become problems for solving the development force of dyeing and finishing processing technology. Along with the increasingly strong pursuit of the ecological environment protection of dyes and the increasing importance of the national importance of renewable resources, biomass dyes are increasingly becoming hot spots for research in the textile dyeing field due to good biodegradability, source sustainability and ecological functionality of dyed products.
Compared with dyes extracted from plants and animals, the microbial dye has the advantages of no limitation of seasons, climate and regions, short production period, easy control of conditions, large yield, rich variety and the like, and has huge potential for development and utilization. The dye/pigment produced by the microorganism can solve the problems of rare raw materials, high cost and the like of the natural dye, and is more beneficial to industrial production.
The application of microbial pigments in the textile dyeing field has been reported at home and abroad, and most of microbial pigments are concentrated on prodigiosin, violacein and fat-soluble monascus pigments. The prodigiosin has bright color, good thermal stability, antibacterial and antimalarial functions, and the like, and can give a textile a high added value when used as a dye, thereby having great development value. Prodigiosin is a natural pigment of a methoxy pyrrole skeleton structure consisting of three pyrrole rings and is a secondary metabolite of Serratia marcescens, aerobacter and some actinomycetes. The bacterial dye prodigiosin is a mauve pigment which is almost insoluble in water and is easy to dissolve in organic solvents, and the bacterial dye prodigiosin has the following structure:
the bacterial dye is insoluble in water, belongs to intracellular pigment, and needs to be extracted by using an organic solvent before being utilized. In addition, organic solvents are required to dissolve the pigments during the dyeing process. The use of organic solvents leads to a significant increase in dyeing costs and contamination problems, which makes it difficult to realize industrial mass production.
At present, the main modes of dyeing cotton fabrics are dip dyeing and pad dyeing, and the 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 means of the substantivity of the dye to the fiber through the circulation of the dye solution and the relative movement of the fabric to be dyed, and the dye is diffused and fixed on the fiber. The method is characterized by being applicable to textiles in various forms; intermittent production has lower labor production efficiency, and is suitable for small-batch and multi-variety production. The main process route of the cotton fabric dip dyeing process is as follows:
alkaline dye liquor, dipping (dyeing), water washing, soaping (fixation), water washing.
The pad dyeing process is to dip the fabric in the dye liquor for a short time (usually several seconds or tens of seconds), then to roll the fabric with a roller, squeeze the dye liquor into the tissues and gaps of the fabric, and simultaneously roll off the redundant dye liquor to uniformly distribute the dye on the fabric. The dye is dyed (or mainly) in the following steaming or baking treatment process. The continuous dyeing process is characterized by continuous dyeing process, high production efficiency and suitability for dyeing of large-batch fabrics.
The two ways are good and bad, and from the viewpoints of saving cost, improving production efficiency and being suitable for industrialized mass production, the padding dyeing process is relatively more advantageous, and the main process route of pad dyeing cotton fabrics by using the two types of dyes at present is as follows:
1. reactive dye: alkaline dye liquor, padding N times (dyeing), steaming (fixation), water washing, soaping (removing floating color), and water washing;
2. vat dye: alkaline dye liquor, padding N times (dyeing), steaming (dyeing), piling (oxidation fixation), water washing, soaping (removing floating color), and water washing;
in summary, in the existing dip dyeing and pad dyeing processes of cotton fabrics, the synthetic dye solution needs to prepare the dye into an aqueous solution in a molecular or ionic state, and the dyeing and fixation are performed in an alkaline environment, and the related dyeing mechanism is the prior art and is not described in detail herein. The synthetic dye dyes cotton fabrics, whether dip or pad dyeing, and the soaping process is to remove flooding. The soaping process of the prodigiosin on cotton fabric dyeing is used for fixation. Then, in the case of the bacterial dye prodigiosin dye liquor of the invention, the prior art discloses the following:
CN111826974a discloses a prodigiosin dyeing method of pure cotton fabric, which comprises the following steps: pretreating pure cotton fabric with hydrogen peroxide; then taking out the pure cotton fabric, and washing and drying the pure cotton fabric; dissolving prodigiosin with ethyl acetate, adding natural dyeing assistant, adding water, and stirring at high speed to obtain dye liquor; putting the dried pure cotton fabric into a dye liquor for dyeing; adding a low-temperature soaping agent into the dye liquor, soaping the dyed pure cotton fabric, taking out, washing, and drying at a low temperature to obtain the dyed pure cotton fabric.
CN102493220B relates to a dyeing method of acrylic fabric using bacterial dye prodigiosin, comprising: (1) Dissolving prodigiosin with ethyl acetate or N, N-dimethylformamide, and then adding the solution into water to prepare a dyeing solution; (2) The dyeing solution is adopted to dye the acrylic fabric, the consumption of the prodigiosin is 0.1-6% of the mass fraction of the acrylic fabric, the dyeing bath ratio is 1:5-20, the pH value of the dyeing solution is regulated to be 4.0-6.0, the dyeing temperature is 80-90 ℃, and the dyeing time is 30-90min.
CN106011195a discloses a preparation method of prodigiosin for silk fabric dyeing, which adjusts the original prodigiosin culture process, so that the effect of the cultured prodigiosin applied to silk fabric is better, especially under the condition of heavy dyeing, the dosage of the added prodigiosin and the time required by dyeing are improved greatly, and no chemical reagent such as mordant is needed to be added in the dyeing process, thereby having low cost, health and environmental protection.
According to the technology of the patent, the dyeing process aiming at bacterial dye adopts a dipping dyeing mode at present, and the prodigiosin dye liquor is required to use an organic solvent for pigment extraction and dissolution of pigment in the dye liquor, so that the dyeing cost is obviously increased, and the pollution problem exists. The defects of saving cost, improving production efficiency and being suitable for industrialized mass production cannot be overcome. However, the padding dyeing method has the problem that the prodigiosin dye liquor is insoluble in water and is prepared by extracting with an organic solvent before use. In addition, organic solvents are required to dissolve the pigments during the dyeing process. Since the existing organic solvent extracts the pigment, the pigment is in a dissolved state in a molecular or ionic form in the organic solvent. In the process of adding water into the dye liquor to prepare the dye liquor, because the pigment is insoluble in water, the pigment added with little water is still in a dissolved state, if the water is added with more 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 inside of the fiber under the water bath environment. Even if the water adding amount is adjusted to the optimal proportion, the dye liquor contains a large amount of organic solvent, even if a dip dyeing mode is adopted, the cost is still huge, and the waste water amount is huge, and then the pad dyeing process is adopted, so that the cost of the organic solvent is higher, the waste water amount is large, a steaming process is needed, the organic solvent is volatilized in a large amount in the steaming process, the environmental pollution is aggravated, the organic solvent cannot be recovered later, the production cost is increased, and the industrial mass production cannot be really realized. Therefore, how to solve the problems of saving cost, improving production efficiency, being suitable for industrialized mass production and the like is a difficult problem which puzzles the technicians in the cotton fabric bacterial dye dyeing field to be solved urgently.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a preparation method and application of a pure water bacterial dye prodigiosin nano-suspension dye solution, which can directly obtain the dye solution without organic solvent extraction, realize the preparation of the dye solution without organic solvent addition under the water-insoluble state of prodigiosin pigment, and effectively improve the dye uptake, the utilization rate of prodigiosin and the fixation effect.
In order to solve the technical problems, the invention adopts the following technical scheme: a preparation method of pure water 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 solution in a constant temperature culture shaker for 12h at 30deg.C with shaking table rotation speed of 160rpm, and naturally illuminating indoor;
(3) Transferring the seed culture solution into a fermentation culture medium by using a pipetting gun for fermentation culture at the temperature of 28 ℃, rotating a shaking table at 200rpm, culturing in a dark place, adjusting the pH value to 6.0, and culturing for 72 hours, wherein 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) Transferring the prodigiosin pigment from cells into a fermentation medium under the action of a shaking table to form a plurality of nano-scale granular pigment particles, and rapidly coating the nano-scale granular pigment particles by a surfactant to form a large number of nano-scale prodigiosin micelle particles in a culture solution;
(5) And after fermentation, removing thalli in the fermentation liquid by using a high-speed refrigerated centrifuge through high-speed low-temperature centrifugation, thus obtaining the pure water-based prodigiosin nano-suspension dye liquor containing a large amount of prodigiosin micelle particles.
The preparation method of the pure water bacterial dye prodigiosin nano-suspension dye solution is characterized by comprising the following steps: in the step (4), the prodigiosin micelle particles are tetrahedral structures similar to triangular pyramid in shape, and the tetrahedral structures have four planes which can be arbitrarily contacted with the surface of cotton fabric.
The preparation method of the pure water bacterial dye prodigiosin nano-suspension dye liquor comprises the step (3), wherein the surfactant is Tween-80.
According to the preparation method of the pure water bacterial dye prodigiosin nano-suspension dye liquor, the particle size distribution range of prodigiosin micelle particles in the pure water system prodigiosin nano-suspension dye liquor obtained in the step (4) is 77-222 nm.
The preparation method of the pure water bacterial dye prodigiosin nano-suspension dye liquor comprises the following steps of (4) setting the rotating speed of a high-speed refrigerated centrifuge to 10000rpm, setting the centrifugal temperature to 20 ℃ and setting the centrifugal time to 10min.
An application of pure water bacterial dye prodigiosin nano-suspension dye liquor in cotton fabric padding dyeing process.
In the application, the padding dyeing process comprises the following steps of:
(1) Preparing a required amount of pure water prodigiosin nano-suspension dye liquor for later use;
(2) And (3) pH blending: 1mol/L hydrochloric acid solution is used for regulating the pH value of the pure water system prodigiosin nano-suspension dye solution to be 2.5-3.5;
(3) Padding cotton fabric: soaking cotton fabric in the dye liquor for 30 seconds, rolling the cotton fabric by using a padder, and removing redundant dye liquor on the cotton fabric, wherein the padding times are one padding to five padding, the pressure of the padder is 0.25bar to 1.0bar, and the padding surplus rate is 75% -85%;
(4) Steaming: steaming the cotton fabric subjected to padding, wherein the steaming time is 1-9 min;
(5) Soap boiling: performing soap boiling fixation on the steamed cotton fabric, wherein the concentration of soap flakes in the soap solution is 2g/L, and the soap boiling time is 5min;
(6) Washing: taking out the cotton fabric after soap boiling, and cleaning with cold water to remove floating color;
(7) And (3) drying: and (5) drying the washed cotton fabric in an oven at a temperature of 70 ℃ for 5min.
In the application, the number of padding in the step (3) is four padding, the pressure of a padder is 0.75bar, and the rolling surplus rate is 80%.
In the application, the steaming time in the step (4) is 5min.
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 bacterial dye prodigiosin nanometer suspension dye solution have the advantages that: from the acquisition mechanism, the prodigiosin pigment is not extracted by an organic solvent, and the extraction of prodigiosin and the preparation of dye liquor do not need any participation of the organic solvent, so that the production cost is effectively saved. The dyeing liquid is prepared without organic solvent from the dyeing mechanism, and aims at the problems that the dyeing liquid is complicated and high in cost because the dyeing liquid is prepared by the organic solvent to dissolve the pigment in the main dip dyeing mode of dyeing cotton fabrics by using the prodigiosin at present. Compared with dip dyeing, the pad dyeing method is used for dyeing cotton fabrics, the dyeing process is shortened from 1-2 hours to 10-15 minutes, and the process is obviously shortened. Meanwhile, the dye utilization rate is obviously improved, and the prodigiosin utilization rate (dye-uptake rate) is improved to 34.9%. The invention adopts pad dyeing technology to greatly improve production efficiency, is suitable for industrialized mass production and application, and is a great innovation in the field of bacterial dye dyeing technology.
Drawings
FIG. 1 is a process flow diagram of the preparation of the prodigiosin nanosuspension dye solution of the present invention;
FIG. 2 is a schematic diagram showing the transfer of prodigiosin pigment from the cell body to the fermentation broth during microbial fermentation;
FIG. 3 is a graph showing the particle size distribution of prodigiosin micelle particles in dye liquor;
FIG. 4 is an electron micrograph of prodigiosin micelle particles in a dye liquor;
FIG. 5 is a flow chart of a pad dyeing process of the dyeing liquor for cotton fabrics.
Detailed Description
The invention will be described in further detail with reference to the accompanying drawings and specific examples.
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 characteristics 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.
Microbial pigments can be divided into two types, namely, intracellular pigments and extracellular pigments, wherein most microbial pigments are enriched in thalli after being produced and are intracellular pigments, and the microbial pigments are usually low in solubility in water and are easily dissolved in organic solvents such as ethanol, ethyl acetate and the like. Prodigiosin is used as an intracellular pigment, most of the pigment exists in bacteria 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 the cells by using an organic solvent, and is prepared into a dye solution after being properly concentrated, and then the textiles are dyed. A large amount of organic solvents are inevitably used in the processes of pigment extraction and dye liquor preparation, which is deviated from the concept of green and environment protection of natural fuel and the development trend of ecological textiles.
1. Preparation of prodigiosin nanosuspension dye liquor by microbial fermentation
As shown in figure 1, the preparation method of the pure water bacterial dye prodigiosin nanosuspension dye solution 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 solution in a constant temperature culture shaker for 12h at 30deg.C with shaking table rotation speed of 160rpm, and naturally illuminating indoor;
(3) Transferring the seed culture solution into a fermentation culture medium by using a pipetting gun for fermentation culture at the temperature of 28 ℃, rotating a shaking table at 200rpm, culturing in a dark place, adjusting the pH value to 6.0, and culturing for 72 hours, wherein 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) Transferring the prodigiosin pigment from cells into a fermentation medium under the action of a shaking table to form a plurality of nano-scale granular pigment particles, and rapidly coating the nano-scale granular pigment particles by a surfactant to form a large number of nano-scale prodigiosin micelle particles in a culture solution;
(5) And after fermentation, removing thalli in the fermentation liquid by using a high-speed refrigerated centrifuge through high-speed low-temperature centrifugation, thus obtaining the pure water-based prodigiosin nano-suspension dye liquor containing a large amount of prodigiosin micelle particles. The rotation speed of the high-speed refrigerated centrifuge is 10000rpm, the centrifugation temperature is 20 ℃, and the centrifugation time is 10min.
As the solubility of the prodigiosin serving as the microbial intracellular pigment in water is extremely low, most of the prodigiosin is accumulated in a common culture medium, only a small part of the pigment is secreted into the culture medium, the pigment content in the bacterial body and the pigment content in the fermentation liquid are in a certain proportion when the components of the fermentation liquid and the fermentation conditions are certain, and the prodigiosin content in the bacterial body and the prodigiosin content in the fermentation liquid are about 59:1. The fermentation preparation mechanism of the prodigiosin nano-suspension dye solution is shown in figure 2, a certain amount of the surfactant Tween-80 is added into the fermentation solution, and the concentration is far higher than the critical micelle concentration, so that Tween-80 molecules can form a large amount of micelles in the fermentation solution, namely Tween-80 micelle 1. During fermentation, prodigiosin 3 is produced in the cell 2 and a small amount of pigment is introduced into the fermentation broth through the cell membrane and the cell wall. The prodigiosin 3 is almost insoluble in water and has strong hydrophobicity, and in the continuous shaking culture dynamic fermentation process 4, prodigiosin particles in the fermentation liquid are coated in Tween-80 micelles to form prodigiosin-Tween-80 micelles 5. Because the free prodigiosin 3 in the fermentation liquor is coated by the surfactant, the balance proportion relation between intracellular and extracellular pigments of the thalli is broken, so that the prodigiosin 3 in the thalli 2 is further transferred to the extracellular. In addition, the nonionic surfactant can increase the permeability of cell membranes and cell walls of the cell 2, and can facilitate extracellular transfer of intracellular prodigiosin 3. Thus, with the progress of the fermentation process 4, the intracellular prodigiosin 3 is continuously generated and transferred to the extracellular space, further more prodigiosin-tween-80 micelles 5 are formed, and after the thallus removing process 6, the pure water prodigiosin nano-suspension dye liquor 7 containing a large amount of prodigiosin micelle particles is obtained.
As shown in figures 2 and 3, in the pure water system prodigiosin nano-suspension dye liquor 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 liquor, the nano-prodigiosin in the dye liquor is dispersed in water in the form of small particles, and the size of the prodigiosin particles is at the nano level. In addition, the nano-prodigiosin obtained by the fermentation method is coated by the surfactant micelle, the hydrophilic end of the surfactant is outwards, the nano-prodigiosin is inside the micelle, and the stability and uniformity of dye liquor can be ensured in two aspects of small pigment size and surfactant coating, so that the uniformity of the color of dyed fabrics is facilitated. Prodigiosin is insoluble in water under neutral conditions and increases in solubility with increasing acidity of the solution. In the pad dyeing process, the pH value of the dye liquor is firstly regulated to be about 3, and the solubility of the prodigiosin small particles is increased in the steaming process of pad dyeing, namely under the condition of acidic high temperature, and the dye liquor has a small size, so that the dye liquor is favorable for dissolving pigment small particles at the nanometer level, and the dyeing effect on fabrics is better as the pigment is more dissolved.
As shown in the electron microscope photograph of fig. 4, in step (4) of this embodiment, the nano-grade prodigiosin micelle particles prepared in this embodiment have a tetrahedral structure similar to a triangular pyramid, also called a triangular pyramid, and have four planes which can be in random contact with the surface of cotton fabric. Compared with spherical particles, each side of the tetrahedral pigment particles is a plane, which is beneficial to being absorbed and fixed on the surface of the fabric, including the fiber surface, fiber gaps and the like, more easily during padding, steaming and soaping in the pad dyeing process. The planar structure makes the contact area between the pigment particles and the surface of the fabric larger, is beneficial to dyeing cotton fabrics by pigment molecules immediately after the pigment particles are dissolved under the hot and acidic conditions, effectively improves the dyeing efficiency and the dyeing rate, and improves the color fixing capability.
In this embodiment, in order to improve the dye-uptake and fixation effect of the prodigiosin pigment in the pad dyeing process, a culture mode of oscillation of an oscillator and rotation of a shaker is adopted in the step (2), so that the strain can be rapidly and massively propagated, more strains are generated, and the yield of the prodigiosin pigment is improved. In the culture process of the step (3), the secondary shaking table is adopted, and the following advantages are shared: 1. in order to enable strains to continuously propagate in a large quantity, 2, the strains can be stimulated to generate a large quantity of prodigiosin pigment, 3, the extraction speed of the pigment can be accelerated under the action of a surfactant, 4, in order to enable the surfactant to rapidly coat prodigiosin nano-particle pigment to form micelles of nano pigment particles, 5, the nano-particle pigment can be prevented from being aggregated into larger pigment particles after being rapidly coated under the action of a shaking table, and stable suspension state cannot be formed after the pigment particles are coated to be more than 400 nanometers or reach the micron level, and pigment molecules are not easy to be dissolved under the hot acidic condition to influence dyeing.
The surfactant in this example is Tween-80. Wherein, the surfactant actually plays a role of an extractant in the fermentation process, and the prodigiosin pigment generated in cells is continuously extracted. After long-time shake culture, a large number of prodigiosin-Tween 80 micelles are formed in the fermentation broth, and the bacteria are removed to obtain the prodigiosin suspension. Later tests show that the prodigiosin particles in the fermentation broth are nano-sized, and the prodigiosin is transferred from the interior of the bacteria body to the fermentation broth and is immediately coated by Tween-80, so that pigment aggregation is prevented, and a stable nano-prodigiosin suspension system is formed. The prodigiosin nanometer suspension dye liquor is directly obtained by utilizing the idea of directly preparing a surfactant fermentation system, the steps of extracting pigment firstly by an organic solvent and preparing the dye liquor by the organic solvent are not needed, the dye liquor which can be used for padding dyeing of cotton fabrics is directly obtained by microorganism fermentation, the process flow of dye liquor preparation is shortened, the cost is saved, and the production efficiency is improved.
2. Application of pure water bacterial dye prodigiosin nano suspension dye liquor in cotton fabric padding dyeing process
Example 1:
as shown in fig. 5, the pad dyeing process of the pure water bacterial dye prodigiosin nanosuspension dye solution for cotton fabric comprises the following steps:
(1) Preparing a required amount of pure water prodigiosin nano-suspension dye liquor for later use;
(2) And (3) pH blending: 1mol/L hydrochloric acid solution is used for adjusting the pH value of the pure water system prodigiosin nano-suspension dye solution to 2.5;
(3) Padding cotton fabric: soaking cotton fabric in the dye liquor for 30 seconds, and rolling the cotton fabric by using a padder to remove redundant dye liquor on the cotton fabric, wherein the padding times are one padding and one padding, the pressure of the padder is 0.25bar, and the padding surplus rate is 75%;
(4) Steaming: steaming the padded cotton fabric for 1min;
(5) Soap boiling: performing soap boiling fixation on the steamed cotton fabric, wherein the concentration of soap flakes in the soap solution is 2g/L, and the soap boiling time is 5min;
(6) Washing: taking out the cotton fabric after soap boiling, and cleaning with cold water to remove floating color;
(7) And (3) drying: and (5) drying the washed cotton fabric in an oven at a temperature of 70 ℃ for 5min.
The cotton fabric to be padded and dyed selected in the embodiment is pure cotton plain weave fabric, warp yarn is 10.6tex, weft yarn is 10.6tex, warp density is 524 pieces/10 cm, weft density is 283 pieces/10 cm, and fabric surface density is 106.6 g/square meter.
In actual industrial production, in order to improve the effect of removing floating color, after steaming in the step (4), a cold water cleaning process can be performed once, or warm water and cold water can be cleaned once respectively, after soap boiling, a mode of cleaning warm water and cold water once respectively can be adopted, and the actual situation can be selected according to the production requirement or the requirement of product quality.
Prodigiosin has a special property of being insoluble in water under neutral conditions and increasing in solubility in water under acidic conditions. By utilizing this property, the pH of the dye liquor is adjusted to be acidic, and the prodigiosin is partially dissolved under the high-temperature condition of dyeing, and the prodigiosin is nano-scale, which is also helpful for dissolving under the hot acidic condition. In the pad dyeing steaming process, dissolved pigment molecules enter the cotton fiber, after dyeing is finished, the acid-base environment on the cotton fiber becomes neutral through washing and soaping, and prodigiosin is changed from a dissolved state into an insoluble state, so that the pigment molecules are deposited in the fiber, dyeing is realized, and better fastness is obtained. The pH value is regulated, and the difference between the pH value and the prior art is that the dye liquor is acidic, and more importantly, the thermal acidity degree needs to be controlled, namely, the pH value is precisely matched with the steaming temperature, so that pigment particles in the prodigiosin-Tween-80 micelle 5 can be dissolved into pigment in molecular and ionic forms to the greatest extent, and the structure of cotton fabric fibers cannot be damaged, and the method is a core technical means.
The most important technical means of the invention comprises two, the first is to adjust the pH value of dyeing to about 3, and the main purposes are discussed above. The second important step is steaming, which is more conducive to prodigiosin dissolution by the high temperature conditions of steaming. The second effect of steaming is to transfer the dye molecules into the fiber as in conventional pad dyeing. After steaming, washing cotton fabric with water and soaping, and the process is the same as that of traditional pad dyeing, but the present invention skillfully uses water system and soaping to change the internal environment of fiber from acidity to alkalinity and change prodigiosin from dissolved state to insoluble state, thereby realizing fixation of pigment in the fiber and obtaining good dyeing fastness.
Example 2:
the same parts as those of embodiment 1 are not repeated, and the difference is that:
(2) And (3) pH blending: 1mol/L hydrochloric acid solution is used for adjusting the pH value of the pure water system prodigiosin nano-suspension dye solution to 3;
(3) Padding cotton fabric: soaking cotton fabric in the dye liquor for 30 seconds, and rolling the cotton fabric by using a padder to remove redundant dye liquor on the cotton fabric, wherein the padding times are three padding and three padding, the pressure of the padder is 0.75bar, and the padding surplus rate is 80%;
(4) Steaming: steaming the padded cotton fabric for 5min;
example 3:
the same parts of the present embodiment as those of embodiments 1 and 2 are not repeated, and the difference is that:
(2) And (3) pH blending: 1mol/L hydrochloric acid solution is used for adjusting the pH value of the pure water system prodigiosin nano-suspension dye solution to 3.5;
(3) Padding cotton fabric: soaking cotton fabric in the dye liquor for 30 seconds, and rolling the cotton fabric by using a padder, wherein the padding times are five padding and five padding, the pressure of the padder is 1.0bar, and the padding residual rate is 85%;
(4) Steaming: steaming the padded cotton fabric for 9min;
example 4:
(1) Regulating the pH value of the prodigiosin nano-suspension dye solution to 3 by using a 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, removing redundant dye liquor on the cotton fabric by padding, wherein the pressure of the padder is 0.75bar, and repeating four times (namely four padding and four padding);
(3) Steaming the cotton fabric in a steaming box for 5min by using saturated steam;
after steaming, washing the cotton fabric with cold water;
(4) And then soap boiling is carried out, wherein 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 5min;
(5) Washing cotton fabric with cold water after soap boiling is finished;
(6) And drying the cotton fabric by using an oven at the drying temperature of 70 ℃ for 5min.
Example 5:
(1) Regulating the pH value of the prodigiosin nano-suspension dye solution to 3.5 by using a 1mol/L hydrochloric acid solution;
soaking the cotton fabric in the dye liquor for 30 seconds, rolling the cotton fabric by using a padder, removing redundant dye liquor on the cotton fabric by padding, wherein the pressure of the padder is 0.5bar, and repeating four times (namely four padding and four padding);
(2) Steaming the cotton fabric in a steaming box for 5min by using saturated steam;
(3) After steaming, washing the cotton fabric with cold water;
(4) And then soap boiling is carried out, wherein 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 5min;
(5) Washing cotton fabric with cold water after soap boiling is finished;
(6) And drying the cotton fabric by using an oven at the drying temperature of 70 ℃ for 5min.
Example 6:
(1) Regulating the pH value of the prodigiosin nano-suspension dye solution to 3 by using a 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, removing redundant dye liquor on the cotton fabric by padding, wherein the pressure of the padder is 0.75bar, and repeating four times (namely four padding and four padding);
(3) Steaming cotton fabric in a steaming box for 10min by using saturated steam;
after steaming, washing the cotton fabric with cold water;
(4) And then soap boiling is carried out, wherein 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 5min;
(5) Washing cotton fabric with cold water after soap boiling is finished;
(6) And drying the cotton fabric by using an oven at the drying temperature of 70 ℃ for 5min.
3. Performance test of dyed fabrics:
after dyeing is completed, the K/S value of the dyed fabric (this value is used to characterize the color depth of the fabric) is determined using a Datacolor colorimeter.
The rubbing color fastness was determined according to GB/T3920-2008 "rubbing color fastness for textile color fastness test".
Soaping-resistant color fastness according to GB/T3921-2008 textile color fastness test soaping-resistant color fastness: test 1.
The dye utilization rate determination method comprises the following steps:
(1) Accurately weighing 0.04g of dyed cotton fabric subjected to soap boiling to remove floating color, cutting the dyed cotton fabric, putting the cut cotton fabric into a 5mL centrifuge tube, then adding 4mL of 90% acidic ethanol water solution (pH 3.0), and standing for 24h to enable prodigiosin in cotton fibers to be fully dissolved in the ethanol solution. The mixture was centrifuged at 8000rpm for 5 minutes, and the supernatant was collected and absorbance at 535nm was measured. And calculating the quality (quality 1) of the prodigiosin on the dyed cotton fabric according to a standard curve of the corresponding relation between the concentration and absorbance of the prodigiosin standard substance solution and the weight of the used fabric and the dosage of the ethanol solution.
(2) And (3) directly drying the fabric after padding the dyeing liquid in the dyeing process, and performing no steaming and subsequent procedures, wherein the dried fabric adopts the method in (1) to obtain the quality (quality 2) of prodigiosin on the cotton fabric after padding the dyeing liquid. The mass 1 is divided by the mass 2, and the fixation rate (namely the dye utilization rate) of the prodigiosin on pad dyeing of cotton fabric is calculated.
The performance test result of the prodigiosin nano suspension pad-dyed cotton fabric 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％ |
| Fastness to dry rubbing | 5 | 5 | 5 |
| Wet rub color fastness | 5 | 5 | 5 |
| Fastness to washing to discoloration | 4 | 4 | 4 |
| Color fastness of soaping-resistant cotton | 5 | 5 | 5 |
| Fastness to staining of soaping hair | 5 | 5 | 5 |
The pad dyeing method for cotton fabric by using the prodigiosin nanometer suspension dye liquor directly prepared by the surfactant fermentation system, which is developed by the invention, solves the problem that the water-insoluble pigment dye liquor prepared by the microbial fermentation technology cannot be directly used for dyeing cotton fabric. The dye-uptake mechanism is directly prepared by microbial fermentation without complex processes of pigment extraction, concentration and purification and dye liquor preparation, and complex preparation process of common dispersion liquid is not needed, so that the requirement on equipment is low, time is saved, raw materials are saved, the dye-uptake rate is improved to more than 34%, and the utilization rate of prodigiosin is remarkably improved. Energy saving and environment protection, simple operation, industrialized production conditions and promotion of development of cotton fabric bacterial dye dyeing technology.
It should be understood that the above description is not intended to limit the invention to the particular embodiments disclosed, but to limit the invention to the particular embodiments disclosed, and that various changes, modifications, additions and substitutions can be made by those skilled in the art without departing from the spirit and scope of the invention.
Claims (4)
1. The application of the pure water system bacterial dye prodigiosin nano-suspension dye liquor in cotton fabric padding dyeing process is characterized in that the preparation method of the 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 solution in a constant temperature culture shaker at 30deg.C at 160rpm under natural indoor illumination;
(3) Transferring the seed culture solution into a fermentation culture medium by using a pipetting gun for fermentation culture at the temperature of 28 ℃, rotating a shaking table at 200rpm, culturing in a dark place, adjusting the pH value to 6.0, and culturing for 72 hours, wherein the fermentation culture medium consists of the following components in percentage by mass: 15g/L of peptone, g g/L of sodium chloride, 2g/L of potassium chloride, 2g/L of magnesium sulfate, 4g/L of glycerol and 18g/L of surfactant, wherein the surfactant is Tween-80;
(4) Transferring the prodigiosin pigment from cells into a fermentation medium under the action of a shaking table to form a plurality of nano-sized granular pigment particles, rapidly coating the nano-sized granular pigment particles by a surfactant, and forming a large number of nano-sized prodigiosin micelle particles in a culture solution, wherein the particle size distribution range of the prodigiosin micelle particles is 77-222 nm; the prodigiosin micelle particles are tetrahedral structures similar to triangular pyramid in shape, and have four planes which can be in random contact with the surface of cotton fabric;
(5) Removing thalli in the fermentation liquor by using a high-speed refrigerated centrifuge through high-speed low-temperature centrifugation after fermentation is finished, and obtaining the pure water system prodigiosin nano-suspension dye liquor containing a large amount of prodigiosin micelle particles;
the padding dyeing process comprises the following steps:
(1) Preparing a required amount of pure water prodigiosin nano-suspension dye liquor for later use;
(2) And (3) pH blending: 1mol/L hydrochloric acid solution is used for regulating the pH value of the pure water system prodigiosin nano-suspension dye solution to be 2.5-3.5;
(3) Padding cotton fabric: soaking cotton fabric in the dye liquor for 30 seconds, rolling the cotton fabric by using a padder, and removing redundant dye liquor on the cotton fabric, wherein the padding times are one padding to five padding, the pressure of the padder is 0.25bar to 1.0bar, and the padding surplus rate is 75% -85%;
(4) Steaming: steaming the cotton fabric subjected to padding, wherein the steaming time is 1-9 min;
(5) Soap boiling: performing soap boiling fixation on the steamed cotton fabric, wherein the concentration of soap flakes in the soap solution is 2g/L, and the soap boiling time is 5min;
(6) Washing: taking out the cotton fabric after soap boiling, and cleaning with cold water to remove floating color;
(7) And (3) drying: and (5) drying the washed cotton fabric in an oven at a temperature of 70 ℃ for 5min.
2. The use according to claim 1, characterized in that: the padding times in the step (3) are four padding, the pressure of a padder is 0.75bar, and the rolling surplus rate is 80%.
3. The use according to claim 1, characterized in that: and (3) steaming for 5min in the step (4).
4. The use according to claim 1, characterized in that: the cotton fabric is pure cotton plain weave fabric, warp yarn is 10.6tex, weft yarn is 10.6tex, warp density is 524 pieces/10 cm, weft density is 283 pieces/10 cm, and fabric surface density is 106.6 g/square meter.
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