CN106835758A - A kind of crudefiber crop rove supercritical carbon dioxide biology enzyme boils bleaching and dyeing method - Google Patents
A kind of crudefiber crop rove supercritical carbon dioxide biology enzyme boils bleaching and dyeing method Download PDFInfo
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- CN106835758A CN106835758A CN201611039624.XA CN201611039624A CN106835758A CN 106835758 A CN106835758 A CN 106835758A CN 201611039624 A CN201611039624 A CN 201611039624A CN 106835758 A CN106835758 A CN 106835758A
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- carbon dioxide
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 372
- 238000004043 dyeing Methods 0.000 title claims abstract description 195
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 181
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 181
- 238000004061 bleaching Methods 0.000 title claims abstract description 107
- 108090000790 Enzymes Proteins 0.000 title claims abstract description 87
- 102000004190 Enzymes Human genes 0.000 title claims abstract description 87
- 238000000034 method Methods 0.000 title claims abstract description 63
- 238000009835 boiling Methods 0.000 claims abstract description 95
- 229940088598 enzyme Drugs 0.000 claims abstract description 86
- 239000000835 fiber Substances 0.000 claims abstract description 45
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 25
- 108010015776 Glucose oxidase Proteins 0.000 claims abstract description 18
- 239000004366 Glucose oxidase Substances 0.000 claims abstract description 18
- 229940116332 glucose oxidase Drugs 0.000 claims abstract description 18
- 235000019420 glucose oxidase Nutrition 0.000 claims abstract description 18
- 238000005516 engineering process Methods 0.000 claims abstract description 13
- 239000002671 adjuvant Substances 0.000 claims abstract description 4
- 229960004424 carbon dioxide Drugs 0.000 claims description 187
- 239000000975 dye Substances 0.000 claims description 144
- 239000012530 fluid Substances 0.000 claims description 108
- 239000006184 cosolvent Substances 0.000 claims description 53
- 239000000243 solution Substances 0.000 claims description 44
- 238000002156 mixing Methods 0.000 claims description 42
- 230000000694 effects Effects 0.000 claims description 24
- 238000003860 storage Methods 0.000 claims description 23
- 230000010354 integration Effects 0.000 claims description 22
- 239000000463 material Substances 0.000 claims description 22
- 238000000926 separation method Methods 0.000 claims description 22
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000000889 atomisation Methods 0.000 claims description 16
- 235000004431 Linum usitatissimum Nutrition 0.000 claims description 12
- 238000002347 injection Methods 0.000 claims description 11
- 239000007924 injection Substances 0.000 claims description 11
- 238000012545 processing Methods 0.000 claims description 11
- 229910002090 carbon oxide Inorganic materials 0.000 claims description 10
- 240000008564 Boehmeria nivea Species 0.000 claims description 9
- 229920002488 Hemicellulose Polymers 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 244000025254 Cannabis sativa Species 0.000 claims description 6
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 claims description 6
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 claims description 6
- 235000009120 camo Nutrition 0.000 claims description 6
- 235000005607 chanvre indien Nutrition 0.000 claims description 6
- 239000000986 disperse dye Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 239000011487 hemp Substances 0.000 claims description 5
- 239000000985 reactive dye Substances 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 2
- 240000006240 Linum usitatissimum Species 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 abstract description 13
- 229940059442 hemicellulase Drugs 0.000 abstract description 12
- 108010002430 hemicellulase Proteins 0.000 abstract description 12
- 238000009987 spinning Methods 0.000 abstract description 6
- 239000004753 textile Substances 0.000 abstract description 4
- 238000011161 development Methods 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 106
- 239000007788 liquid Substances 0.000 description 16
- 241000273930 Brevoortia tyrannus Species 0.000 description 14
- 238000005057 refrigeration Methods 0.000 description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 11
- 241000208202 Linaceae Species 0.000 description 11
- 239000012752 auxiliary agent Substances 0.000 description 11
- 238000007789 sealing Methods 0.000 description 9
- 241000790917 Dioxys <bee> Species 0.000 description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 238000004090 dissolution Methods 0.000 description 7
- 238000009826 distribution Methods 0.000 description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 6
- 230000002779 inactivation Effects 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 230000004580 weight loss Effects 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- -1 pectase Proteins 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000012546 transfer Methods 0.000 description 5
- 241000722949 Apocynum Species 0.000 description 4
- 238000004891 communication Methods 0.000 description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 229920005610 lignin Polymers 0.000 description 3
- 238000012544 monitoring process Methods 0.000 description 3
- 239000001814 pectin Substances 0.000 description 3
- 229920001277 pectin Polymers 0.000 description 3
- 235000010987 pectin Nutrition 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000000982 direct dye Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000002609 medium Substances 0.000 description 2
- 239000003595 mist Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 235000009754 Vitis X bourquina Nutrition 0.000 description 1
- 235000012333 Vitis X labruscana Nutrition 0.000 description 1
- 240000006365 Vitis vinifera Species 0.000 description 1
- 235000014787 Vitis vinifera Nutrition 0.000 description 1
- GCNLQHANGFOQKY-UHFFFAOYSA-N [C+4].[O-2].[O-2].[Ti+4] Chemical compound [C+4].[O-2].[O-2].[Ti+4] GCNLQHANGFOQKY-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 229910001632 barium fluoride Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910001919 chlorite Inorganic materials 0.000 description 1
- 229910052619 chlorite group Inorganic materials 0.000 description 1
- QBWCMBCROVPCKQ-UHFFFAOYSA-N chlorous acid Chemical compound OCl=O QBWCMBCROVPCKQ-UHFFFAOYSA-N 0.000 description 1
- 230000009514 concussion Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000002657 fibrous material Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 125000003051 glycosyloxy group Chemical group 0.000 description 1
- 238000009897 hydrogen peroxide bleaching Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000003116 impacting effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 235000017550 sodium carbonate Nutrition 0.000 description 1
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 description 1
- 229960002218 sodium chlorite Drugs 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 238000002166 wet spinning Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- D06P1/94—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 dyes dissolved in solvents which are in the supercritical state
-
- 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
- D06B23/205—Arrangements of apparatus for treating processing-liquids, -gases or -vapours, e.g. purification, filtration or distillation for adding or mixing constituents of the treating material
-
- 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
- D06B9/00—Solvent-treatment of textile materials
- D06B9/02—Solvent-treatment of textile materials solvent-dyeing
-
- 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
- D06B9/00—Solvent-treatment of textile materials
- D06B9/06—Solvent-treatment of textile materials with recovery of the solvent
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
- D06M16/003—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic with enzymes or microorganisms
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/06—Processes in which the treating agent is dispersed in a gas, e.g. aerosols
-
- 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
- D06P1/44—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 insoluble pigments or auxiliary substances, e.g. binders
- D06P1/445—Use of auxiliary substances before, during or after dyeing or printing
-
- 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
- D06P3/6033—Natural or regenerated cellulose using dispersed dyes
-
- 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
- D06P3/62—Natural or regenerated cellulose using direct dyes
-
- 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
- D06P3/66—Natural or regenerated cellulose using reactive dyes
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- Microbiology (AREA)
- Dispersion Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Treatment Of Fiber Materials (AREA)
Abstract
Bleaching and dyeing method is boiled the present invention relates to a kind of crudefiber crop rove supercritical carbon dioxide biology enzyme, belongs to field of textiles.A kind of crudefiber crop rove supercritical carbon dioxide biology enzyme boils bleaching and dyeing method, it is adjuvant used for biology enzyme boils drift agent in boiling drift and boiling drift separating technology, the biology enzyme boils drift agent with the percentages of crudefiber crop roving yarn quality (o.w.f.), is made up of following components：Hemicellulase 0.2~3%, pectase 0.2~5%, glucose oxidase 0.2~3%.Rove supercritical carbon dioxide biology enzyme of the present invention is boiled bleachinges and dyeing that integral method overall process is pollution-free, zero-emission, meets the demand for development of low-carbon economy, embodies fashion bast fibre spinning, the modern life theory of green bast fibre spinning.
Description
Technical field
Bleaching and dyeing method is boiled the present invention relates to a kind of crudefiber crop rove supercritical carbon dioxide biology enzyme, belongs to field of textiles.
Background technology
Flaxen fiber is the quality plant fiber that the mankind use earliest, its chemical composition mainly include cellulose, hemicellulose,
Pectin, lignin, wax and nitrogen substance etc., wherein hemicellulose, lignin, pectin are difficult to remove, and flaxen fiber molecule
Crystallinity and the degree of orientation are higher, it is easy to which ductility, elasticity, convergence, flexibility and crimpiness on fiber produce influence, to fiber crops
Fiber spinning weaving process brings inconvenience.Therefore, crudefiber crop roving boiling and bleaching dye is always the problem of bast industry concern.It is many
Since year, solution this problem is all based oneself upon in many research work, and until later stage the 1950's, people's rove that just begins one's study is boiled
Bleaching and dyeing process, wet spinning is carried out after roving boiling and bleaching is contaminated, and makes accompaniment fully swelling, so as to remove partial impurities, increasing fiber can
The property spun.
It is main with water as medium in traditional crudefiber crop roving boiling and bleaching dye process, sequentially pass through soda boiling, chlorite bleaching,
Washing, hydrogen peroxide bleaching, water Xian, sour Xian, water Xian's operation, hemicellulose, lignin and pectin in removal fiber are final to meet
To the requirement of numb roving fibers intensity and whiteness in spinning process.After boiling and bleachinging and dyeing treatment, eliminate between part adhesive fiber
Material, reduce the contact between fiber, improve the fiber thinness of flaxen fiber, increased the spinnability of flaxen fiber.However, passing
The numb roving boiling and bleaching of system and dyeing dyer's sequence have that water consumption big energy-consuming, technological process be long, financial cost is high.Meanwhile, boil drift and dye
After production, containing auxiliary agents such as substantial amounts of sodium chlorite, soda ash, hydrogen peroxide in the sewage of discharge, intractability is big, is brought to environment
Serious pollution.
When material under normality temperature and pressure be higher than its critical-temperature and critical pressure when, the material be transform into it is super
Critical fluids.In the supercritical state, the minor alteration of pressure and temperature, can cause the significant difference of fluid density, and table
It is now the change of fluid solubility, so that supercritical fluid has application value.Is held from West Germany Essen in 1978
One " supercritical fluid extraction " international conference rises, and over more than 30 years, supercritical liquid extraction technique is widely used to medicine, changes
The fields such as work, food and environmental protection.Supercritical liquid extraction technique is under conditions of chemical composition is not changed, using shooting flow
The solvability of body and the relation of its density, supercritical fluid is contacted with separate substance, makes it selectively that polarity is big
The composition of small, boiling point height and molecular size range is extracted successively, and supercritical fluid is dissolved using temperature and pressure then
The influence of ability and realize extract and separate purpose.In conventional material, carbon dioxide is so that its is nontoxic, harmless, non-ignitable, with change
The quadrupole moment structure of inertia and uniqueness is learned, the features such as critical-temperature (31.1 DEG C) and relatively low critical pressure (7.37MPa), as answering
Use most commonly used supercritical fluid.
The content of the invention
For the high pollution for solving bast-fibre roving boiling and bleaching and dyeing process, highly water intensive problem, the invention provides fiber crops
Class rove supercritical carbon dioxide biology enzyme is boiled bleachinges and dyeing integral method, and the method is realized using carbon dioxide instead of aqueous medium
The cleaning to boil of flax roving bleachinges and dyeing production；Meanwhile, in the supercritical state, completion flaxen fiber is boiled, floated, a step of dyer's sequence connects
Continuousization is completed, and both can significantly shorten the time used for boiling drift and dyeing process, and the energy consumption of whole operation can be reduced again, is solved
High pollution, the problem of high energy consumption of crudefiber crop roving boiling and bleaching dyer's sequence.
A kind of crudefiber crop rove supercritical carbon dioxide biology enzyme boils bleaching and dyeing method, and the bleaching and dyeing method that boils includes overcritical boiling
The processing step of drift-separation and dyeing is floated, boils, it is described overcritical to boil drift, boil drift-separation and dyeing with overcritical titanium dioxide
Carbon is carrier, crudefiber crop rove is carried out boiling drift, drift-separation is boiled and is dyeed,
It is wherein, adjuvant used for biology enzyme boils drift agent in boiling drift and boiling drift-separating technology,
The biology enzyme boils drift agent with the percentages of flax roving quality (o.w.f.), is made up of following components：
The biology enzyme boils drift agent with the percentages of crudefiber crop roving yarn quality (o.w.f.), is made up of following components：Half is fine
The plain enzyme 0.2~3% of dimension, pectase 0.2~5%, glucose oxidase 0.2~3%,
Further, the biology enzyme boils drift agent and is formulated as the biology enzyme that mass concentration is 1~5% when in use and boils drift agent
Solution.
Further, methods described includes following processing steps：
1. overcritical boiling and bleaching process：Temperature is 25-70 DEG C, and pressure is 8-30MPa, boils the drift time for 10-60min；
2. it is overcritical to boil drift-separating technology：Temperature is 25-70 DEG C, and pressure is 8-30MPa, and it is 10- to boil drift disengaging time
30min；
3. supercritical dyeing technique：Temperature is 80-120 DEG C, and pressure is 18-30MPa, and dyeing time is 10-60min.
Further, described crudefiber crop rove is flax roving, ramie rove, bluish dogbane rove, hemp rove；Described
Dyestuff be disperse dyes, reactive dye, direct dyes, reactive disperse dyes or biochrome, it is commercially available.
The preferably crudefiber crop rove supercritical carbon dioxide biology enzyme of the invention boils bleaching and dyeing method in supercritical carbon dioxide
Liquid waterless is boiled to be bleachinged and dyeing integration apparatus and carries out, and the supercritical carbon dioxide fluid is anhydrous to be boiled and bleaching and dyeing under integration apparatus include
State unit：
Carbon dioxide storage system for storing and/or producing carbon dioxide；
Cosolvent tank for storing cosolvent；
Ultrasonic mist for receiving the cosolvent of carbon dioxide and common solution storage tank from carbon dioxide storage system
Change device, cosolvent forms fluid-mixing after being atomized in the ultrasonic atomizer with carbon dioxide mix；
Booster pump and heater, the booster pump and heater are used for the fluid-mixing received from ultrasonic atomizer or connect
Receive the carbon dioxide from carbon dioxide storage system；Carbon dioxide is pressurized and heater with cosolvent fluid-mixing through booster pump
Fluid-mixing is set to be changed into being dissolved with the supercritical carbon dioxide fluid of cosolvent after heating；Carbon dioxide is pressurized and adds through booster pump
It is changed into supercritical carbon dioxide fluid after hot device heating；
Receive the dyestuff kettle of the supercritical carbon dioxide fluid from heater；
Receive the supercritical carbon dioxide fluid for being dissolved with cosolvent from heater or being dissolved with from dyestuff kettle
Kettle is bleachinged and dyeing in boiling for the supercritical carbon dioxide fluid of dyestuff；
Receive from the piece-rate system for boiling the material for bleachinging and dyeing kettle, piece-rate system can make the material carry out gas solid separation.
Further, the technique is as follows：
1. overcritical boiling and bleaching process：Crudefiber crop rove, dyestuff and biology enzyme are boiled into drift agent solution it is sequentially placed into described boiling and bleachinges and dyeing
In kettle, dyestuff kettle and cosolvent tank；Carbon dioxide storage system is opened, to carbon dioxide is passed through in ultrasonic atomizer, makes dioxy
It is 1-5m to change carbon flow speed3/h；Biology enzyme in cosolvent tank is boiled in drift agent solution injection ultrasonic atomizer, through supersonic generator
Effect be atomized；The fluid-mixing that carbon dioxide and the biology enzyme of atomization boil drift agent solution mixes in ultrasonic atomizer；
Uniform dissolution has the carbon dioxide that biology enzyme boils drift agent to enter supercriticality in the presence of heater, and in the work of booster pump
It is injected into boil under and bleachinges and dyeing inside kettle, interior circulation is carried out to bast-fibre rove in the presence of magnetic force circulating pump and/or is followed outward
Ring boils drift, and overcritical boiling and bleaching process condition is：Temperature is 25-70 DEG C, and pressure is 8-30MPa, boils the drift time for 10-60min；
2. it is overcritical to boil drift-separating technology：Magnetic force circulating pump is closed, carries out boiling drift-separation work in the presence of booster pump
Sequence, boiling drift-separation process conditions is：Temperature is 25-70 DEG C, and pressure is 8-30MPa, and it is 10-30min to boil drift disengaging time；
3. supercritical dyeing technique：Boil after the completion of drift-separating technology, close cosolvent tank, and utilize heater by dyestuff
Kettle and boil and bleaching and dyeing kettle and be warming up to 80-120 DEG C；During dyeing process, access dyestuff kettle in the system of bleachinging and dyeing, carbon dioxide storage are being boiled first
Carbon dioxide outflow in deposit system, enters supercriticality, and injected in the presence of booster pump in the presence of heater
Dyestuff kettle；Supercritical carbon dioxide fluid flows into the dyestuff that dyestuff kettle is dissolved in it first, subsequently enters to boil and bleachinges and dyeing in kettle, to it
In bast-fibre rove dyeed, and bast-fibre rove carried out in the presence of magnetic force circulating pump interior dye and outer dye plus
Work；After dyeing terminates, the supercritical carbon dioxide fluid for being dissolved with dyestuff is separated in piece-rate system, realizes dyestuff and gaseous state
Carbon dioxide is sufficiently separated.
Further, the drift-separating technology that boils is：Opening booster pump boils fresh supercritical carbon dioxide entrance
Kettle is bleachinged and dyeing, carries out boiling drift using fresh supercritical carbon dioxide, the material that will be boiled while boiling drift in drift kettle is sent into point successively
Separated in system.
Anhydrous the boiling of supercritical carbon dioxide fluid of the present invention bleachinges and dyeing the equipment with identical function in integration apparatus
Unit can such as may include some cosolvent tanks, some ultrasonic atomizers, some booster pumps and heater, some comprising multiple
If dyestuff kettle, dry cook bleaching and dyeing kettle etc..Those skilled in the art can be according to being configured the need for treating capacity.
Supercritical carbon dioxide fluid of the present invention is anhydrous to be boiled and bleachinges and dyeing integration apparatus and further include infrared online prison
Examining system, the infrared on-line monitoring system is by infrared spectrum detector, high-resolution pick-up device and BaF2Form is constituted.It is red
Outer on-line monitoring system with boil the system of bleachinging and dyeing and piece-rate system is connected, can be changed by pipe-line, timely monitor boils drift
Dye effect and separation and recovery effect.The system of bleachinging and dyeing of boiling is bleachinged and dyeing kettle, dyestuff kettle and magnetic force circulating pump and is constituted by boiling.
Supercritical carbon dioxide fluid of the present invention is anhydrous to be boiled and bleachinges and dyeing integration apparatus and further include to set for connecting
The pipeline and assembling pipe joint of standby unit.The pipeline is the connecting pipe road known to those skilled in the art, such as steel
Pipe etc.；The assembling pipe joint refers to mechanical fasteners part, such as flange, bolt.
Supercritical carbon dioxide fluid of the present invention is anhydrous to be boiled and bleachinges and dyeing integration apparatus and further include fluid conveying dress
Put and flow display device, the fluid delivery system refers to the pump for fluid known to those skilled in the art；Flow
Display device refers to for showing by the device of pipeline fluid flow, such as meter, flow indicator.
Supercritical carbon dioxide fluid of the present invention is anhydrous boil bleaching and dyeing integration apparatus further include pressure detecting and
Display device, the pressure detecting and display refer to known to those skilled in the art for detecting fluid or gas pressure
Pressure gauge etc..
Supercritical carbon dioxide fluid of the present invention is anhydrous boil bleaching and dyeing integration apparatus further include temperature detection and
Display device, the temperature detection and display refer to known to those skilled in the art for detecting fluid or gas temperature
Thermometer etc..
Supercritical carbon dioxide fluid of the present invention is anhydrous to be boiled and bleachinges and dyeing integration apparatus and further include that Flow-rate adjustment is filled
Put, for the flow in control pipeline, such as valve.
Supercritical carbon dioxide fluid of the present invention is anhydrous to be boiled and bleachinges and dyeing integration apparatus and further include heating system, institute
State heating system thermal source needed for for being provided for unit.
Further, the heating system is heat-conducting oil system, and it includes being stored for the conduction oil for storing conduction oil
Tank, heat-conducting oil heating tank and oil pump.The heat-conducting oil system can be equipment in separating still, dyestuff kettle, boil bleaching and dyeing kettle etc. offer
Thermal source.
Supercritical carbon dioxide fluid of the present invention is anhydrous to be boiled and bleachinges and dyeing integration apparatus and further include circularly cooling system
System, the cycle refrigeration system is used for the low-temperature receiver for needed for unit is provided.
Further, the cycle refrigeration system is made up of compressor, cooling tower, eg pump, clarified water pump.It is described to follow
Ring refrigeration system is used for the low-temperature receiver for needed for condenser is provided.
The preferably supercritical carbon dioxide fluid of the invention is anhydrous to be boiled and bleachinges and dyeing integration apparatus and include magnetic force circulating pump, institute
Magnetic force circulating pump is stated to be circulated for making to boil the material bleachinged and dyeing in kettle.It is that fiber is carried out effectively sufficiently to boil to bleaching and dyeing step,
Of the present invention boiling bleachinges and dyeing kettle equipped with circulating pump, and the circulating pump can will be flowed through and boil the supercritical carbon dioxide fluid for bleachinging and dyeing kettle again
Injection is boiled and bleachinges and dyeing kettle, carries out boiling and bleaching and dyeing repeatedly.Described circulating pump one end is connected by pipeline and boils the fluid intake for bleachinging and dyeing kettle, separately
One end is connected by pipeline and boils the fluid issuing for bleachinging and dyeing kettle.
Preferably anhydrous the boiling of the supercritical carbon dioxide fluid of the invention bleachinges and dyeing carbon dioxide storage described in integration apparatus
System includes gas reservoir, and carbon dioxide source connects gas reservoir by gas transfer pump, and the gas reservoir is by pipe
Road connects ultrasonic atomizer.Can be realized using gas transfer pump and its subsidiary pipeline straight with gas tank on carbon dioxide haulage vehicle
Connect in succession, and complete liquid carbon dioxide filling to gas reservoir, with energy-conservation, quickly fill the characteristics of.
In above-mentioned technical proposal, the carbon dioxide source can be carbon dioxide generating device or carbon dioxide tank
Car.
The preferably supercritical carbon dioxide fluid of the invention is anhydrous to be boiled and bleachinges and dyeing piece-rate system described in integration apparatus and include
Receive from the cooler for boiling the material for bleachinging and dyeing kettle, cooler downstream connects separating still by pipeline, and material enters in separating still
Row is separated；Separating still downstream connection adsorbs kettle, the absorption kettle be used to adsorbing remain in supercritical carbon dioxide fluid boil drift
Product and color additive.
Separate bed is provided with the separating still, separate bed is multilayer gradient mesh structure, and grid hole footpath is from bottom to top
5mm-0.05mm gradual changes.Meanwhile, changed by pipeline, it is possible to achieve carbon dioxide blowback, so as to solve separate bed
Cleaning problem.
The preferably supercritical carbon dioxide fluid of the invention is anhydrous to be boiled and bleachinges and dyeing integration apparatus and include condenser, described cold
Condenser receives the carbon dioxide from absorption kettle, and it is cooled down；The condensator outlet end connects gas reservoir.
The preferably ultrasonic atomizer of the invention includes supersonic generator, porous liquid-gas distributor and atomization pond, gas
Entrance, gas passage and gas vent composition, wherein, the cosolvent pipeline communication is atomized pond, and atomization pond is located at ultrasonic atomizatio
The bottom of device, supersonic generator is located in atomization pond；Atomization pond top is provided with porous liquid-gas distributor, the porous liquid qi leel
Cloth device top is provided with gas passage, is provided with gas access in gas passage side, the gas access and carbon dioxide storage tank
By pipeline communication.
Porous liquid-gas distributor of the present invention is by 3~10 porous central tubes, many porous circular cylinders, antipriming pipe distribution grids
Ith, antipriming pipe distribution grid II is constituted.Wherein, porous central tube is bottom opening, top closure structure, inner diameter of centerpipe is 10~
20mm；Through hole is provided with the tube wall of porous central tube, aperture is 0.5~2mm；Porous circular cylinder is bottom lock, top end opening
Structure, cylinder internal diameter is 1~10mm；Through hole is provided with the post jamb of porous circular cylinder, aperture is 0.5~2mm；Porous circular cylinder around
Around porous central tube.The porous liquid-gas distributor side is provided with fluid-mixing outlet, and fluid-mixing outlet is by pipe
Road connects booster pump.
It is of the present invention boil to bleaching and dyeing be mounted with kettle boil drift unit, described boiling bleachinges and dyeing unit, mainly by bottom distributor, many
Hole central tube and external connection cylinder are constituted.Boil drift unit bottom distributor and bleaching and dyeing kettle fluid intake and be connected with boiling, external connection
Bleaching and dyeing kettle fluid issuing and be connected with boiling in cylinder gas access.Wherein, porous central tube is 1-50, and porous central tube is a diameter of
35mm, porous central tube aperture is 1mm-5mm.
Dyestuff kettle of the present invention includes dyestuff cylinder, and its bottom and top are respectively equipped with CO 2 fluid entrance and charging
Mouthful, the CO 2 fluid entrance is connected with the fluid intake of dyestuff cylinder；Valve III, batch mixing are sequentially provided with from outlet upwards
Storehouse II, valve II, blending bunker I, valve I and feeding chamber.
The dyestuff cylinder cylinder body bottom is provided with gas access, cylinder and is provided with central tube connecting plate, porous point from the bottom to top
Fabric swatch and top multihole distributor, above-mentioned central tube connecting plate, multihole distributor and top multihole distributor with cylinder inner circle
Phase is fixed；Cavity between the cylinder bottom and central tube connecting plate constitutes bottom gas passage；Set on central tube connecting plate
There is the antipriming pipe communicated with bottom gas passage, the antipriming pipe is bottom opening, top closure structure, in the tube wall of antipriming pipe
It is provided with through hole；The multihole distributor is provided with through hole；Region is used for for sealing structure centered on the top multihole distributor
The top of sealing porous pipe, periphery is porous cyclic structure；Gas vent, top and the top of cylinder are provided with the top of the cylinder
The cavity that portion's multihole distributor is formed is top gas hybrid channel.
Further, the feeding chamber includes valve I, blending bunker I, valve II, blending bunker II and valve III.It is capable of achieving to boil
The in good time addition of dyestuff, auxiliary agent during bleachinging and dyeing.
Beneficial effects of the present invention are：A kind of crudefiber crop rove supercritical carbon dioxide biology enzyme boils bleaching and dyeing method, is boiling drift
Adjuvant used for biology enzyme boils drift agent in drift-separating technology with boiling, the biology enzyme boils drift agent with crudefiber crop roving yarn quality
(o.w.f.) percentages, are made up of following components：Hemicellulase 0.2~3%, pectase 0.2~5%, grape glycosyloxy
Change enzyme 0.2~3%.Boil after the completion of bleachinging and dyeing, the K/S values of rove can reach more than 5, and colour fastness to rubbing is more than 4 grades, water-fastness
Color fastness is more than 4 grades；Meanwhile, flaxen fiber rove rate of weight loss 6-12%, residual gum content 7-15%, broken filament intensity 6-
13cN/dtex, elongation at break 4.5-8.5%.Rove supercritical carbon dioxide biology enzyme of the present invention is boiled bleachinges and dyeing integral method
Overall process is pollution-free, zero-emission, meets the demand for development of low-carbon economy, embodies fashion bast fibre spinning, the modern life of green bast fibre spinning
Theory.
Brief description of the drawings
Fig. 1 bleachinges and dyeing integration apparatus schematic diagram for a kind of anhydrous the boiling of supercritical carbon dioxide fluid, and reference is as follows：1
Carbon dioxide tank car, 2 gas transfer pumps, 3 glycol head tanks, 4 cooling towers, 5 clarified water pumps, 6 compressors, 7 eg pumps,
8 condensers, 9 gas reservoirs, 10 cosolvent tanks, 11 liquid delivery pumps, 12 ultrasonic atomizers, 13 booster pumps, 14 heaters, 15 dyes
Material kettle 16,17 is boiled bleachinges and dyeing kettle, 18 magnetic force circulating pumps, 19 on-line monitoring systems, 20 coolers, 21 separating stills, 22 absorption kettles, 23
Conduction oil head tank, 24 heat-conducting oil systems, 25 reclaim compressor；
Fig. 2 be a kind of supercritical carbon dioxide fluid it is anhydrous boil in drift equipment boil bleaching and dyeing kettle in ultrasonic atomizer illustrate
Figure, reference is as follows：
201 supersonic generators, 202 atomization ponds, 203 antipriming pipe distribution grids I, 204 porous circular cylinders, 205 porous central tubes,
206 antipriming pipe distribution grids II, 207 gas accesses, 208 gas passages, 209 gas vents, 210 cosolvent entrances；
Fig. 3 be a kind of supercritical carbon dioxide fluid it is anhydrous boil to bleaching and dyeing boiling in integration apparatus and bleaching and dyeing kettle load that to boil drift single
First schematic diagram, reference is as follows：
301 boil and bleaching and dyeing kettle, 302 gas accesses, 303 top gas passages, 304 porous central tube end sealings, 305 outer layers
Sleeve, 306 internal layer porous sleeves, 307 porous central tubes, 308 bottom distributors, 309 flaxen fiber flyer bobbins, 310 boil and bleaching and dyeing
Bottom portion fluid intake；
Fig. 4 is that a kind of anhydrous dyestuff cylinder boiled in the dyestuff kettle bleachinged and dyeing in integration apparatus of supercritical carbon dioxide fluid shows
It is intended to, reference is as follows：
401 gas accesses, 402 bottom gas passages, 403 central tube connecting plates, 404 antipriming pipes, 405 multihole distributors,
406 top multihole distributors, 407 top gas hybrid channels, 408 gas vents；
Fig. 5 is that a kind of anhydrous dyestuff kettle bleachinged and dyeing in integration apparatus that boils of supercritical carbon dioxide fluid loads schematic diagram,
Reference is as follows：
501 fast Kaifeng lids, 502 CO 2 fluid entrances, the outlet of 503 CO 2 fluids, 504 heat-conducting medium entrances,
505 heat-conducting mediums are exported, 506 feeding chambers, 507 valve Is, 508 blending bunkers I, 509 valves II, 510 blending bunkers II, 511 valves
Ⅲ。
Specific embodiment
Following non-limiting examples can make one of ordinary skill in the art be more fully understood the present invention, but not with
Any mode limits the present invention.
Test method described in following embodiments, unless otherwise specified, is conventional method；The reagent and material, such as
Without specified otherwise, commercially obtain.
A kind of anhydrous the boiling of supercritical carbon dioxide fluid bleachinges and dyeing integration apparatus, including following units：
Carbon dioxide storage system, the carbon dioxide storage system includes gas reservoir 9, carbon dioxide tank car 1
Gas reservoir 9 is connected by gas transfer pump 2, the gas reservoir 9 connects ultrasonic atomizer 12 by pipeline.
Cosolvent tank 10 for storing cosolvent；
Ultrasound for receiving the cosolvent of carbon dioxide and common solution storage tank 10 from carbon dioxide storage system
Atomizer 12, cosolvent forms fluid-mixing after being atomized in the ultrasonic atomizer 12 with carbon dioxide mix；
Booster pump 13 and heater 14, the booster pump and heater are used to receive the titanium dioxide from ultrasonic atomizer 12
Carbon and cosolvent fluid-mixing or carbon dioxide receive the carbon dioxide from carbon dioxide storage system；Fluid-mixing is through increasing
Fluid-mixing is set to be changed into being dissolved with the supercritical carbon dioxide fluid of cosolvent after press pump 13 is pressurized and heater 14 is heated；Dioxy
Change carbon gas makes carbon dioxide be changed into supercritical carbon dioxide fluid after booster pump 13 is pressurized and heater 14 is heated；
Receive the dyestuff kettle 15 of the supercritical carbon dioxide fluid from heater 14；
Receive the supercritical carbon dioxide fluid for being dissolved with cosolvent from heater 14 or from the molten of dyestuff kettle 15
Solution has boiling for the supercritical carbon dioxide fluid of dyestuff to bleaching and dyeing kettle 16 and boil and bleaching and dyeing kettle 17；
Receive from the piece-rate system for boiling the material for bleachinging and dyeing kettle, piece-rate system can make the material carry out gas solid separation.Described point
Include receiving from the cooler 20 for boiling the material for bleachinging and dyeing kettle from system, the downstream of cooler 20 connects separating still 21 by pipeline,
Material is separated in separating still 21；The downstream connection of separating still 21 adsorbs kettle 22, and absorption kettle 22 is used to adsorb overcritical dioxy
Boiling for residual floats product and color additive in changing carbon flow body.
Magnetic force circulating pump 18, the magnetic force circulating pump 18 is used to make to boil the material bleachinged and dyeing in kettle to be circulated.
Condenser 8, the condenser 8 receives the supercritical carbon dioxide fluid from absorption kettle, and it is cooled down；
The port of export of the condenser 8 connects gas reservoir 9.
Heating system, the heating system is used for the thermal source for needed for unit is provided, and the heating system is conduction oil
System, it includes the conduction oil head tank 23 and heat-conducting oil system 24 for storing conduction oil.The heat-conducting oil system includes using
In the storage conduction oil storage tank of conduction oil, heat-conducting oil heating tank and oil pump, can be separating still 21 in equipment, dyestuff kettle 15,
Boil and the offer thermal source such as kettle 16,17 is provided.
Cycle refrigeration system, the cycle refrigeration system is used for the low-temperature receiver for needed for unit is provided.The circularly cooling
System is made up of compressor 6, cooling tower 4, eg pump 7, clarified water pump 5.The cycle refrigeration system is used to be provided for condenser 8
Required low-temperature receiver.
The ultrasonic atomizer includes supersonic generator 201, porous liquid-gas distributor and atomization pond 202, gas access
207th, gas passage 208 and gas vent 209 are constituted, wherein, the cosolvent pipeline communication is atomized pond 202, is atomized 202, pond
In the bottom of ultrasonic atomizer, supersonic generator 201 is located in atomization pond 202；The top of atomization pond 202 is provided with porous liquid qi leel
Cloth device, the porous liquid-gas distributor top is provided with gas passage 208, and gas access 207 is provided with the side of gas passage 208,
The gas access 207 passes through pipeline communication with carbon dioxide storage tank 9.Its operation principle is：On the one hand, cosolvent is in liquid
Injected in ultrasonic atomizer by cosolvent entrance 210 in the presence of delivery pump, and made under the concussion of supersonic generator 201
Use lower atomization.The cosolvent of spray pattern initially enters the porous central tube 205 being connected with antipriming pipe distribution grid I 203, it is possible to
Flowed out along the aperture on porous central tube 205.On the other hand, carbon dioxide enters gas passage 208 by gas access 207,
Then enter coupled porous circular cylinder 204 by antipriming pipe distribution grid II 206, it is possible to along small on porous circular cylinder 204
Flow out in hole.The cosolvent and carbon dioxide of spray pattern are mutually mixed, so as to realize gas-liquid two-phase in liquid-gas distributor
Be sufficiently mixed.Then, gas-liquid mixture fluid is by the fluid of gas vent 209, into boiling the system of bleachinging and dyeing.
Used boiling is bleachinged and dyeing kettle and refers to super facing in the Chinese patent that publication No. is CN102787459A in following embodiments
Boundary's carbon dioxide bobbin dyeing yarn kettle, dyeing caldron such as described in embodiment 1.Described boiling is bleachinged and dyeing kettle by kettle and is loaded in kettle
The drift unit that boils in body is constituted.The autoclave body bottom is provided with to boil bleachinges and dyeing kettle fluid intake, and top is provided with to boil bleachinges and dyeing kettle fluid issuing.
Described boiling bleachinges and dyeing unit, is mainly made up of bottom distributor 308, porous central tube 307 and external connection cylinder.The outside connects
Cylinder is connect by gas access 302, top gas passage 303, porous central tube end sealing 304, outer layer sleeve 305, internal layer is more
Borehole jack cylinder 306 is constituted.The internal layer porous sleeve 306 is set in outer layer sleeve 305, is provided with the top of outer layer sleeve 305
Gas access 302, has cavity between gas access 302 and internal layer porous sleeve 306, and the cavity is top gas passage 303；
Some porous central tubes 307 are provided with internal layer porous sleeve 306, the top of porous central tube 307 passes through porous central tube top
Sealing 304 is sealed；The lower end of porous central tube 307 communicates with bottom distributor 308.Boil drift unit bottom distributor 308 and boil drift
Kettle is bleachinged and dyeing with kiering dye kettle 16,17 boiling for kettle top is located in dye kettle fluid intake connection, external connection cylinder gas access 302
Fluid issuing is connected.Wherein, porous central tube 307 is 6, a diameter of 35mm of porous central tube 307, the hole of porous central tube 307
Footpath is 1mm.Its operation principle is：Boil when bleachinging and dyeing production, CO 2 fluid is flowed by gas access 302 (external connection cylinder)
Enter, be made up of with internal layer porous sleeve 306 into outer layer sleeve 305 afterwards top gas passage 303 (external connection cylinder)
Gas passage, flow through the pore of internal layer porous sleeve 306, it is possible to achieve fluid is high-strength to the orientation of cylinder yarn to be penetrated, and is solved first
The unordered sinuous flow state of gas determined in conventional supercritical fluid outer loop process, has been effectively ensured to boil and has bleachinged and dyeing effect.It is overcritical
CO 2 fluid by porous central tube 307, by bottom distributor 308, then by flowing out, boil and bleaching and dyeing outer circulation by completion.
In addition, external connection cylinder is directly connected to the top of porous central tube 307, changes each porous central tube and be both needed to individually sealing
Mode, realize the integral sealing to it, so as to avoid fluid short phenomenon, further enhance fluid mass-transfer effect.
When the fluid intake that CO 2 fluid bleachinges and dyeing bottom portion by boiling is flowed into, bottom distributor 308 is initially entered, and flow into porous
Central tube 307, to flaxen fiber thereon boil and bleachinges and dyeing production.After CO 2 fluid penetrates flaxen fiber bobbin, by internal layer
The gas passage that porous sleeve 306 is constituted into outer layer sleeve 305 and inner layer sleeve 306.Subsequently enter top gas passage
303, and flowed out by gas access 302 (external connection cylinder), completion is boiled and bleachinges and dyeing outer circulation.
The dyestuff kettle includes dyestuff cylinder, and its bottom and top are respectively equipped with CO 2 fluid entrance 502 and charge door,
The CO 2 fluid entrance 502 is connected with the carbon dioxide entrance 401 of dyestuff cylinder；It is sequentially provided with upwards from charge door
Valve III511, blending bunker II510, valve II509, blending bunker I508, valve I507 and feeding chamber 506.
The dyestuff cylinder cylinder body bottom is provided with gas access 401, cylinder and is provided with central tube connecting plate 403 from the bottom to top,
Multihole distributor 405 and top multihole distributor 406, above-mentioned central tube connecting plate 403, multihole distributor 405 and top are porous
Distribution grid 406 is fixed with cylinder inner circle phase；Cavity between the cylinder bottom and central tube connecting plate 403 constitutes bottom gas
Body passage 402；Central tube connecting plate 403 is provided with the antipriming pipe 404 communicated with bottom gas passage 402, the antipriming pipe 404
It is bottom opening, top closure structure is provided with through hole on the tube wall of antipriming pipe 404；The multihole distributor 405 is provided with logical
Hole；The central area of the top multihole distributor 406 is sealing structure, and for the top of sealing porous pipe 404, periphery is many
Hole cyclic structure；Gas vent 408, top and the formation of top multihole distributor 406 of cylinder are provided with the top of the cylinder
Cavity is top gas hybrid channel 407.Its operation principle is：Boil before bleachinging and dyeing, dyestuff is added in antipriming pipe 404, then will dye
Barrel is placed in inside dyestuff kettle, and dyestuff cylinder gas access 401 is connected with dyestuff bottom portion CO 2 fluid entrance 502.Boil drift
Dye production when, supercritical carbon dioxide first by gas access 401 enter dyestuff cylinder bottom gas passage 402, and then flow into
In the connected antipriming pipe 404 of central tube connecting plate 403；The CO 2 fluid for being dissolved with dyestuff or auxiliary agent passes through antipriming pipe 404
The pore on surface enters the gas passage between central tube connecting plate 403, multihole distributor 405, top multihole distributor 406；Together
When, 405 CO 2 fluid can be flowed through on multihole distributor 405 positioned between central tube connecting plate 403 and multihole distributor
Pore enter gas passage between multihole distributor 405, top multihole distributor 406.The outer of top multihole distributor 406 is
Annular porous structure, core is that closed structure is sealed with being formed with the top of antipriming pipe 404, so as to avoid process fluid flow
In short circuit phenomenon.The CO 2 fluid of dyestuff or auxiliary agent is dissolved with by the porous outer of top multihole distributor 406, is entered
Enter top gas hybrid channel 407, and flowed out via gas vent, kettle is bleachinged and dyeing into boiling, carry out flaxen fiber flyer bobbin 309
Boil and bleaching and dyeing.Antipriming pipe 404, multihole distributor 405 and top gas hybrid channel 407 in dyestuff cylinder can divide to greatest extent
The dyestuff in it is dissipated, it is high-quality beneficial to flaxen fiber rove, uniform to increase the solubility of CO 2 fluid in unit volume
Property dyeing process.
The operation principle of the dyestuff kettle is：CO 2 fluid flows into dyestuff kettle by CO 2 fluid entrance 502,
And enter dyestuff or auxiliary agent that dyestuff cylinder is dissolved in it.The supercritical carbon dioxide fluid for being dissolved with dyestuff or auxiliary agent passes through dioxy
Change carbon fluid issuing 503 to flow out, into the pipeline that kettle is connected is bleachinged and dyeing with boiling, production and application is bleachinged and dyeing for boiling.Boil the process of bleachinging and dyeing
In, certain mass color blending dye or other auxiliary agents are added in feeding chamber, valve I 507 is first turned on, dyestuff or auxiliary agent are injected
In blending bunker I 508, when dyestuff or auxiliary agent fully enter blending bunker I 508, valve I 507 is closed.It is slow to open valve II 509,
So that dyestuff or auxiliary agent the injection blending bunker II 510 in blending bunker I 508, are then turned off valve II 509.It is slow to open valve III
511 so that CO 2 fluid flows slowly into blending bunker II 510, with dissolving dye.Treat the pressure and dye in blending bunker II 510
After material kettle balance, standard-sized sheet valve III 511 realizes connecting for blending bunker II 510 and dyestuff kettle, so as to complete dyestuff or auxiliary agent to dye
Expect the addition of kettle.
The process route for carrying out kiering dye using the said equipment is as follows：
Carbon dioxide is stored in gas reservoir 9, and biology enzyme boils drift agent and is placed in cosolvent tank 10, and dyestuff is placed in dyestuff kettle
In 15, flaxen fiber flyer bobbin 309 is placed on to boil and bleachinges and dyeing on unit, is placed in boiling and bleachinges and dyeing inside kettle.Carbon dioxide is first in gas
Outflow in body storage tank 9, flows into ultrasonic atomizer 12.Biology enzyme boils drift agent and is atomized in the presence of ultrasonic atomizer 12, with
The carbon dioxide of inflow is sufficiently mixed in porous gas-liquid distributor.Uniform dissolution has the carbon dioxide that biology enzyme boils drift agent adding
Enter supercriticality in the presence of hot device 14, and dyestuff kettle 15 is injected in the presence of booster pump 13 or is boiled and bleaching and dyeing kettle 16,17
(dyestuff kettle 15 or boil hereafter is bleachinged and dyeing into kettle 16,17 to be referred to as supercritical non-aqueous boiling bleaching equipment), and.It is dispersed to there is biology enzyme to boil
The supercritical carbon dioxide fluid of drift agent flows into boil to be bleachinged and dyeing in kettle 16,17, first to numb fine in the presence of magnetic force circulating pump 18
Dimension rove carries out interior circulation and drift is boiled in outer circulation.Then, magnetic force circulating pump 18 is closed, unlatching booster pump 13 makes in gas reservoir 9
Carbon dioxide enter to boil and bleaching and dyeing kettle 16,17 and carry out boiling drift-separation circuit, travel further into separating still 21 carry out separation circuit with
Further increase and boil drift effect, and drift product is boiled in separation, to avoid impacting dyeing process.
After the completion of boiling drift and separating, cosolvent tank 10 is closed, make the carbon dioxide from the outflow of gas reservoir 9 through ultrasonic atomizatio
Enter dyestuff kettle 15 through booster pump 13 and heater 14 after device 12, and using heating system dyestuff kettle 15 and boiling is bleachinged and dyeing kettle 16,
17 heat up, and improve kettle temperature to meet dyeing needs, and cause the biology enzyme inactivation in kettle, it is to avoid it causes shadow to dyeing
Ring.During dyeing process, access dyestuff kettle 15 in the system of bleachinging and dyeing is being boiled first, the carbon dioxide outflow in gas reservoir 9, in supercharging
Be injected into the presence of pump 13 it is supercritical non-aqueous boil inside bleaching equipment, and in the presence of heater 14 enter supercritical state
State.Supercritical carbon dioxide fluid flows into the dyestuff that dyestuff kettle 15 is dissolved in it first, subsequently enters to boil and bleachinges and dyeing in kettle 16,17,
Flaxen fiber rove therein is dyeed, and carries out interior dye and outer dye to flaxen fiber rove in the presence of magnetic force circulating pump 18
Processing.After dyeing terminates, the supercritical carbon dioxide fluid for being dissolved with dyestuff and boiling drift object drops in cooler 20 first
Temperature, is separated subsequently into separating still 21, and realizes dividing completely for the component of gas-solid two in the presence of the separate bed of separating still 21
From, dyestuff or boil the solids fractions such as drift object and be deposited in the bottom of separating still 21.Meanwhile, in order to realize the solid matters such as dyestuff
It is completely separated, carbon dioxide is adsorbed again in absorption kettle 22.Subsequent gaseous carbon dioxide is via cycle refrigeration system
Reclaim and enter gas reservoir 9, in case using next time.
Method of testing is as follows in following implementations：Rove color fastness of the present invention is according to GB/T 3920-1997《Textile color jail
Degree experiment colour fastness to rubbing》、GB/T 3921-2008《Textile color stability tests fastness to soaping》；Residual gum content according to
GB/T 5889-86《Ramie chemical composition quantitative analysis method》Tested；Broken filament intensity, elongation at break according to
GB/T 5886-86《Ramie broken filament intensity experiment method》Tested.
Embodiment 1
Hemicellulase, pectase and glucose oxidase are purchased from Jiangsu Ruiyang Biological Technology Co., Ltd., hemicellulose
Enzyme：Vigor >=20000U/g, is applicable pH value 4.0-5.5, optimal pH 4.5-5,30-60 DEG C of Applicable temperature, optimum temperature 45-50
℃；Pectase：Vigor >=10000U/g, is applicable pH value 3.5-6.5, optimal pH 5.5-6,45-65 DEG C of Applicable temperature, optimal temperature
50-55 DEG C of degree；Glucose oxidase：Vigor >=300U/g, is applicable pH value 4.0-5.5, optimal pH 3.5-6.5, Applicable temperature
20-70 DEG C, 50-55 DEG C of optimum temperature.It is proportionally 1 by hemicellulase, pectase, glucose oxidase：1：1 is configured to
The complex biological enzyme solutions of concentration 1%, stir stand-by.
10kg flax rovings, disperse dyes 1% (o.w.f.) and the complex biological enzyme solutions of concentration 1% are inserted into super facing successively
Boundary's carbon dioxide is boiled in bleachinging and dyeing kettle 16,17, dyestuff kettle 15 and cosolvent tank 10；Gas reservoir 9 is opened, in ultrasonic atomizer 12
Carbon dioxide is passed through, makes carbon dioxide flow rate be 4m3/h；Complex biological enzyme solutions in cosolvent tank 10 are in liquid delivery pump 11
In the presence of with the speed of 50g/min injection ultrasonic atomizer 12 in, be atomized through the effect of supersonic generator 201；Two
The mixing in ultrasonic atomizer 12 of the fluid-mixing of carbonoxide and the complex biological enzyme solutions of atomization；Uniform dissolution has complex biological
The carbon dioxide of enzyme solutions is heated to 35 DEG C in the presence of heater 14 and enters supercriticality, and is being pressurized the work of 13 pumps
10MPa is pressurized under it is injected into boil and bleachinges and dyeing inside kettle 16,17.The dispersed overcritical titanium dioxide for having a complex biological enzyme solutions
Carbon flow body flows into and boils and bleaching and dyeing in kettle 16,17, carries out interior circulation and outer to flax roving first in the presence of magnetic force circulating pump 18
Drift 20min is boiled in circulation.Magnetic force circulating pump 18 is closed, temperature and pressure is held in 35 DEG C, under conditions of 10MPa, in booster pump
Carry out boiling drift-separation 20min in the presence of 13, isolate and boil drift product, further increase and boil drift effect, to avoid to dyer
Sequence is impacted.
Boil after the completion of drift, close cosolvent tank 10, and make dyestuff kettle 15 and boil using heating system to bleaching and dyeing the intensification of kettle 16,17
To 100 DEG C, kettle temperature is improved to meet dyeing needs, and cause the biology enzyme inactivation in kettle, it is to avoid it is caused to dyeing
Influence.During dyeing process, access dyestuff kettle 15 in the system of bleachinging and dyeing is being boiled first, the carbon dioxide outflow in gas reservoir 9 is adding
Enter supercriticality in the presence of hot device 14, and the effect of booster pump 13 is pressurized to 20MPa injection dyestuffs kettle 15；Overcritical two
Carbon oxide fluid flows into the dyestuff that dyestuff kettle 15 is dissolved in it first, subsequently enters to boil and bleachinges and dyeing in kettle 16,17, to flax therein
Fiber roving is dyeed, and carries out interior dye and outer dye processing 60min to flaxen fiber rove in the presence of magnetic force circulating pump 18；
After dyeing terminates, the supercritical carbon dioxide fluid for being dissolved with dyestuff is separated in separating still 21, realizes dyestuff and gaseous state two
Carbonoxide is sufficiently separated.Gaseous carbon dioxide is reclaimed via cycle refrigeration system and enters gas reservoir 9, in case using next time.
After supercritical carbon dioxide biology enzyme is boiled and bleachinged and dyeing, the K/S values of flax roving can reach 8.5, rub resistance color jail
4.5 grades of degree, 4 grades of washing color fastness, fast light and colour fastness to weathering can reach 3-4 grades；Rate of weight loss 9.5%, cull
Rate 9.2%, broken filament intensity 9.8cN/dtex, elongation at break 6.3%.
Embodiment 2
Hemicellulase, pectase and glucose oxidase are purchased from Jiangsu Ruiyang Biological Technology Co., Ltd., hemicellulose
Enzyme：Vigor >=20000U/g, is applicable pH value 4.0-5.5, optimal pH 4.5-5,30-60 DEG C of Applicable temperature, optimum temperature 45-50
℃；Pectase：Vigor >=10000U/g, is applicable pH value 3.5-6.5, optimal pH 5.5-6,45-65 DEG C of Applicable temperature, optimal temperature
50-55 DEG C of degree；Glucose oxidase：Vigor >=300U/g, is applicable pH value 4.0-5.5, optimal pH 3.5-6.5, Applicable temperature
20-70 DEG C, 50-55 DEG C of optimum temperature.It is proportionally 1 by hemicellulase, pectase, glucose oxidase：1：3 are configured to
The complex biological enzyme solutions of concentration 4%, stir stand-by.
15kg ramies rove, reactive disperse dyes 2% (o.w.f.) and the complex biological enzyme solutions of concentration 4% are inserted successively
Supercritical carbon dioxide is boiled in bleachinging and dyeing kettle 16,17, dyestuff kettle 15 and cosolvent tank 10；Gas reservoir 9 is opened, to ultrasonic atomizer
Carbon dioxide is passed through in 12, makes carbon dioxide flow rate be 3m3/h；Complex biological enzyme solutions in cosolvent tank 10 are conveyed in liquid
Injected in ultrasonic atomizer 12 with the speed of 30g/min in the presence of pump 11, the effect through supersonic generator 201 occurs mist
Change；The mixing in ultrasonic atomizer 12 of the fluid-mixing of carbon dioxide and the complex biological enzyme solutions of atomization；Uniform dissolution has multiple
Carbon dioxide with biological enzyme solutions is heated to 45 DEG C in the presence of heater 14 and enters supercriticality, and in supercharging 13
15MPa is pressurized in the presence of pump it is injected into boil and bleachinges and dyeing inside kettle 16,17.It is dispersed to have the overcritical of complex biological enzyme solutions
CO 2 fluid is flowed into boil and bleachinged and dyeing in kettle 16,17, carries out interior following to ramie rove first in the presence of magnetic force circulating pump 18
Drift 10min is boiled in ring and outer circulation.Close magnetic force circulating pump 18, temperature and pressure is held in 45 DEG C, under conditions of 15MPa,
Carry out boiling drift-separation 10min in the presence of booster pump 13, isolate and boil drift product, further increase and boil drift effect, it is right to avoid
Dyeing process is impacted.
Boil after the completion of drift, close cosolvent tank 10, and make dyestuff kettle 15 and boil using heating system to bleaching and dyeing the intensification of kettle 16,17
To 90 DEG C, kettle temperature is improved to meet dyeing needs, and cause the biology enzyme inactivation in kettle, it is to avoid it causes shadow to dyeing
Ring.During dyeing process, access dyestuff kettle 15 in the system of bleachinging and dyeing is being boiled first, the carbon dioxide outflow in gas reservoir 9, in heating
Supercriticality is incorporated in the presence of device 14, and the effect of booster pump 13 is pressurized to the 25MPa injection kettles of dyestuff 15；Overcritical dioxy
Change carbon flow body and flow into the dyestuff that dyestuff kettle 15 is dissolved in it first, subsequently enter to boil and bleaching and dyeing in kettle 16,17, it is fine to ramie therein
Dimension rove is dyeed, and carries out interior dye and outer dye processing 40min to flaxen fiber rove in the presence of magnetic force circulating pump 18；Dye
After color terminates, the supercritical carbon dioxide fluid for being dissolved with dyestuff is separated in separating still 21, realizes dyestuff and gaseous state dioxy
Change being sufficiently separated for carbon.Gaseous carbon dioxide is reclaimed via cycle refrigeration system and enters gas reservoir 9, in case using next time.
After supercritical carbon dioxide biology enzyme is boiled and bleachinged and dyeing, the K/S values of ramie rove can reach 7.2, and ramie rove is resistance to
4 grades of colorfastness to rubbing, 3.5 grades of washing color fastness, fast light and colour fastness to weathering can reach 4 grades；Rate of weight loss
8.8%, residual gum content 10.5%, broken filament intensity 10.2cN/dtex, elongation at break 5.6%.
Embodiment 3
Hemicellulase, pectase and glucose oxidase are purchased from Jiangsu Ruiyang Biological Technology Co., Ltd., hemicellulose
Enzyme：Vigor >=20000U/g, is applicable pH value 4.0-5.5, optimal pH 4.5-5,30-60 DEG C of Applicable temperature, optimum temperature 45-50
℃；Pectase：Vigor >=10000U/g, is applicable pH value 3.5-6.5, optimal pH 5.5-6,45-65 DEG C of Applicable temperature, optimal temperature
50-55 DEG C of degree；Glucose oxidase：Vigor >=300U/g, is applicable pH value 4.0-5.5, optimal pH 3.5-6.5, Applicable temperature
20-70 DEG C, 50-55 DEG C of optimum temperature.It is proportionally 1 by hemicellulase, pectase, glucose oxidase：2：3 are configured to
The complex biological enzyme solutions of concentration 3%, stir stand-by.
20kg hemps rove, reactive dye 1.5% (o.w.f.) and the complex biological enzyme solutions of concentration 3% are inserted successively super
Critical carbon dioxide is boiled in bleachinging and dyeing kettle 16,17, dyestuff kettle 15 and cosolvent tank 10；Gas reservoir 9 is opened, to ultrasonic atomizer 12
In be passed through carbon dioxide, make carbon dioxide flow rate be 4m3/h；Complex biological enzyme solutions in cosolvent tank 10 are in liquid delivery pump
Injected in ultrasonic atomizer 12 with the speed of 20g/min in the presence of 11, be atomized through the effect of supersonic generator 201；
The mixing in ultrasonic atomizer 12 of the fluid-mixing of carbon dioxide and the complex biological enzyme solutions of atomization；Uniform dissolution has compounding to give birth to
The carbon dioxide of thing enzyme solutions is heated to 65 DEG C in the presence of heater 14 and enters supercriticality, and is being pressurized 13 pumps
28MPa is pressurized under effect it is injected into boil and bleachinges and dyeing inside kettle 16,17.The dispersed overcritical dioxy for having a complex biological enzyme solutions
Change carbon flow body and flow into boil and bleachinges and dyeing in kettle 16,17, hemp rove is carried out first in the presence of magnetic force circulating pump 18 interior circulation and
Drift 45min is boiled in outer circulation.Magnetic force circulating pump 18 is closed, temperature and pressure is held in 65 DEG C, under conditions of 20MPa, in supercharging
Carry out boiling drift-separation 15min in the presence of pump 13, isolate and boil drift product, further increase and boil drift effect, to avoid to dyeing
Operation is impacted.
Boil after the completion of drift, close cosolvent tank 10, and make dyestuff kettle 15 and boil using heating system to bleaching and dyeing the intensification of kettle 16,17
To 120 DEG C, kettle temperature is improved to meet dyeing needs, and cause the biology enzyme inactivation in kettle, it is to avoid it is caused to dyeing
Influence.During dyeing process, access dyestuff kettle 15 in the system of bleachinging and dyeing is being boiled first, the carbon dioxide outflow in gas reservoir 9 is adding
Enter supercriticality in the presence of hot device 14, and the effect of booster pump 13 is pressurized to 28MPa injection dyestuffs kettle 15；Overcritical two
Carbon oxide fluid flows into the dyestuff that dyestuff kettle 15 is dissolved in it first, subsequently enters to boil and bleachinges and dyeing in kettle 16,17, to hemp therein
Fiber roving is dyeed, and carries out interior dye and outer dye processing 45min to flaxen fiber rove in the presence of magnetic force circulating pump 18；
After dyeing terminates, the supercritical carbon dioxide fluid for being dissolved with dyestuff is separated in separating still 21, realizes dyestuff and gaseous state two
Carbonoxide is sufficiently separated.Gaseous carbon dioxide is reclaimed via cycle refrigeration system and enters gas reservoir 9, in case using next time.
After supercritical carbon dioxide biology enzyme is boiled and bleachinged and dyeing, the K/S values of hemp rove can reach 8.9, rub resistance color jail
4 grades of degree, 3.5 grades of washing color fastness, fast light and colour fastness to weathering can reach 4 grades；Rate of weight loss 9.7%, residual gum content
10.9%, broken filament intensity 9.5cN/dtex, elongation at break 6.8%.
Embodiment 4
Hemicellulase, pectase and glucose oxidase are purchased from Jiangsu Ruiyang Biological Technology Co., Ltd., hemicellulose
Enzyme：Vigor >=20000U/g, is applicable pH value 4.0-5.5, optimal pH 4.5-5,30-60 DEG C of Applicable temperature, optimum temperature 45-50
DEG C, pectase：Vigor >=10000U/g, is applicable pH value 3.5-6.5, optimal pH 5.5-6,45-65 DEG C of Applicable temperature, optimal temperature
50-55 DEG C of degree；Glucose oxidase：Vigor >=300U/g, is applicable pH value 4.0-5.5, optimal pH 3.5-6.5, Applicable temperature
20-70 DEG C, 50-55 DEG C of optimum temperature.It is proportionally 1 by hemicellulase, pectase, glucose oxidase：2：1 is configured to
The complex biological enzyme solutions of concentration 2%, stir stand-by.
25kg bluish dogbanes rove, direct dyes 2% (o.w.f.) and the complex biological enzyme solutions of concentration 2% are inserted successively super
Critical carbon dioxide is boiled in bleachinging and dyeing kettle 16,17, dyestuff kettle 15 and cosolvent tank 10；Gas reservoir 9 is opened, to ultrasonic atomizer 12
In be passed through carbon dioxide, make carbon dioxide flow rate be 2m3/h；Complex biological enzyme solutions in cosolvent tank 10 are in liquid delivery pump
Injected in ultrasonic atomizer 12 with the speed of 60g/min in the presence of 11, be atomized through the effect of supersonic generator 201；
The mixing in ultrasonic atomizer 12 of the fluid-mixing of carbon dioxide and the complex biological enzyme solutions of atomization；Uniform dissolution has compounding to give birth to
The carbon dioxide of thing enzyme solutions is heated to 55 DEG C in the presence of heater 14 and enters supercriticality, and is being pressurized 13 pumps
25MPa is pressurized under effect it is injected into boil and bleachinges and dyeing inside kettle 16,17.The dispersed overcritical dioxy for having a complex biological enzyme solutions
Change carbon flow body flows into boil to be bleachinged and dyeing in kettle 16,17, and interior circulation is carried out to bluish dogbane rove first in the presence of magnetic force circulating pump 18
Drift 30min is boiled with outer circulation.Close magnetic force circulating pump 18, temperature and pressure is held in 55 DEG C, under conditions of 25MPa, is increasing
Carry out boiling drift-separation 30min in the presence of press pump 13, isolate and boil drift product, further increase and boil drift effect, to avoid to dye
Color operation is impacted.
Boil after the completion of drift, close cosolvent tank 10, and make dyestuff kettle 15 and boil using heating system to bleaching and dyeing the intensification of kettle 16,17
To 110 DEG C, kettle temperature is improved to meet dyeing needs, and cause the biology enzyme inactivation in kettle, it is to avoid it is caused to dyeing
Influence.During dyeing process, access dyestuff kettle 15 in the system of bleachinging and dyeing is being boiled first, the carbon dioxide outflow in gas reservoir 9 is adding
Enter supercriticality in the presence of hot device 14, and the effect of booster pump 13 is pressurized to 30MPa injection dyestuffs kettle 15；Overcritical two
Carbon oxide fluid flows into the dyestuff that dyestuff kettle 15 is dissolved in it first, subsequently enters to boil and bleachinges and dyeing in kettle 16,17, is spreaded out to therein
Flaxen fiber rove is dyeed, and carries out interior dye and outer dye processing to flaxen fiber rove in the presence of magnetic force circulating pump 18
30min；Dyeing terminate after, the supercritical carbon dioxide fluid for being dissolved with dyestuff is separated in separating still 21, realize dyestuff and
Gaseous carbon dioxide is sufficiently separated.Gaseous carbon dioxide is reclaimed via cycle refrigeration system and enters gas reservoir 9, in case next
Use.
After supercritical carbon dioxide biology enzyme is boiled and bleachinged and dyeing, the K/S values of bluish dogbane rove can reach 9.5, rub resistance color
4 grades of fastness, 3.5 grades of washing color fastness, fast light and colour fastness to weathering can reach 4 grades；Rate of weight loss 9.7%, cull
Rate 9.8%, broken filament intensity 9.5cN/dtex, elongation at break 6.8%.
Embodiment 5
Hemicellulase, pectase and glucose oxidase are purchased from Jiangsu Ruiyang Biological Technology Co., Ltd., hemicellulose
Enzyme：Vigor >=20000U/g, is applicable pH value 4.0-5.5, optimal pH 4.5-5,30-60 DEG C of Applicable temperature, optimum temperature 45-50
DEG C, pectase：Vigor >=10000U/g, is applicable pH value 3.5-6.5, optimal pH 5.5-6,45-65 DEG C of Applicable temperature, optimal temperature
50-55 DEG C of degree；Glucose oxidase：Vigor >=300U/g, is applicable pH value 4.0-5.5, optimal pH 3.5-6.5, Applicable temperature
20-70 DEG C, 50-55 DEG C of optimum temperature.It is proportionally 1 by hemicellulase, pectase, glucose oxidase：3：3 are configured to
The complex biological enzyme solutions of concentration 3%, stir stand-by.
10kg flax rovings, biochrome 3% (o.w.f.) and the complex biological enzyme solutions of concentration 3% are inserted into super facing successively
Boundary's carbon dioxide is boiled in bleachinging and dyeing kettle 16,17, dyestuff kettle 15 and cosolvent tank 10；Gas reservoir 9 is opened, in ultrasonic atomizer 12
Carbon dioxide is passed through, makes carbon dioxide flow rate be 3m3/h；Complex biological enzyme solutions in cosolvent tank 10 are in liquid delivery pump 11
In the presence of with the speed of 10g/min injection ultrasonic atomizer 12 in, be atomized through the effect of supersonic generator 201；Two
The mixing in ultrasonic atomizer 12 of the fluid-mixing of carbonoxide and the complex biological enzyme solutions of atomization；Uniform dissolution has complex biological
The carbon dioxide of enzyme solutions is heated to 50 DEG C in the presence of heater 14 and enters supercriticality, and is being pressurized the work of 13 pumps
22MPa is pressurized under it is injected into boil and bleachinges and dyeing inside kettle 16,17.The dispersed overcritical titanium dioxide for having a complex biological enzyme solutions
Carbon flow body flows into and boils and bleaching and dyeing in kettle 16,17, carries out interior circulation and outer to flax roving first in the presence of magnetic force circulating pump 18
Drift 60min is boiled in circulation.Magnetic force circulating pump 18 is closed, temperature and pressure is held in 50 DEG C, under conditions of 22MPa, in booster pump
Carry out boiling drift-separation 20min in the presence of 13, isolate and boil drift product, further increase and boil drift effect, to avoid to dyer
Sequence is impacted.
Boil after the completion of drift, close cosolvent tank 10, and make dyestuff kettle 15 and boil using heating system to bleaching and dyeing the intensification of kettle 16,17
To 100 DEG C, kettle temperature is improved to meet dyeing needs, and cause the biology enzyme inactivation in kettle, it is to avoid it is caused to dyeing
Influence.During dyeing process, access dyestuff kettle 15 in the system of bleachinging and dyeing is being boiled first, the carbon dioxide outflow in gas reservoir 9 is adding
Enter supercriticality in the presence of hot device 14, and the effect of booster pump 13 is pressurized to 25MPa injection dyestuffs kettle 15；Overcritical two
Carbon oxide fluid flows into the dyestuff that dyestuff kettle 15 is dissolved in it first, subsequently enters to boil and bleachinges and dyeing in kettle 16,17, to flax therein
Fiber roving is dyeed, and carries out interior dye and outer dye processing 60min to flaxen fiber rove in the presence of magnetic force circulating pump 18；
After dyeing terminates, the supercritical carbon dioxide fluid for being dissolved with dyestuff is separated in separating still 21, realizes dyestuff and gaseous state two
Carbonoxide is sufficiently separated.Gaseous carbon dioxide is reclaimed via cycle refrigeration system and enters gas reservoir 9, in case using next time.
After supercritical carbon dioxide biology enzyme is boiled and bleachinged and dyeing, the K/S values of flax roving can reach 8.4, rub resistance color jail
3-4 grades of degree, washing color fastness 3-4 grades, fast light and colour fastness to weathering can reach 3-4 grades；Rate of weight loss 9.2%, it is residual
Glue rate 10.4%, broken filament intensity 8.3cN/dtex, elongation at break 7.2%.
Claims (8)
1. a kind of crudefiber crop rove supercritical carbon dioxide biology enzyme boils bleaching and dyeing method, it is characterised in that：It is described to boil bleaching and dyeing method bag
Include it is overcritical boil drift, boil drift-separation and dyeing processing step, it is described it is overcritical boil drift, boil drift-separation and dyeing with surpass
Critical carbon dioxide is carrier, crudefiber crop rove is carried out boiling drift, drift-separation is boiled and is dyeed,
It is wherein, adjuvant used for biology enzyme boils drift agent in boiling drift and boiling drift-separating technology,
The biology enzyme boils drift agent with the percentages of crudefiber crop roving yarn quality (o.w.f.), is made up of following components：Hemicellulose
Enzyme 0.2~3%, pectase 0.2~5%, glucose oxidase 0.2~3%.
2. method according to claim 1, it is characterised in that：The biology enzyme boils drift agent, and to be formulated as quality when in use dense
The biology enzyme spent for 1~5% boils drift agent solution.
3. method according to claim 1, it is characterised in that：Methods described includes following processing steps：
1. overcritical boiling and bleaching process：Temperature is 25-70 DEG C, and pressure is 8-30MPa, boils the drift time for 10-60min；
2. it is overcritical to boil drift-separating technology：Temperature is 25-70 DEG C, and pressure is 8-30MPa, and it is 10-30min to boil drift disengaging time；
3. supercritical dyeing technique：Temperature is 80-120 DEG C, and pressure is 18-30MPa, and dyeing time is 10-60min.
4. method according to claim 1, it is characterised in that：The crudefiber crop rove is flax roving, ramie rove, spreads out
Numb rove, hemp rove.
5. method according to claim 1, it is characterised in that：The dyestuff is disperse dyes, reactive dye, directly contaminates
Material, reactive disperse dyes or biochrome.
6. method according to claim 1, it is characterised in that：The crudefiber crop rove supercritical carbon dioxide biology enzyme boils drift
Dyeing method is bleachinged and dyeing integration apparatus and is carried out in anhydrous the boiling of supercritical carbon dioxide fluid, and the supercritical carbon dioxide fluid is anhydrous
Boil and bleaching and dyeing integration apparatus including following units：
Carbon dioxide storage system for storing and/or producing carbon dioxide；
Cosolvent tank for storing cosolvent；
Ultrasonic atomizer for receiving the cosolvent of carbon dioxide and common solution storage tank from carbon dioxide storage system,
Cosolvent forms fluid-mixing after being atomized in the ultrasonic atomizer with carbon dioxide mix；
Booster pump and heater, the booster pump and heater are used to receive the fluid-mixing from ultrasonic atomizer or receive
From the carbon dioxide of carbon dioxide storage system；Carbon dioxide is pressurized with cosolvent fluid-mixing through booster pump and heater is heated
Fluid-mixing is set to be changed into being dissolved with the supercritical carbon dioxide fluid of cosolvent afterwards；Carbon dioxide is pressurized and heater through booster pump
It is changed into supercritical carbon dioxide fluid after heating；
Receive the dyestuff kettle of the supercritical carbon dioxide fluid from heater；
Receive the supercritical carbon dioxide fluid for being dissolved with cosolvent from heater or be dissolved with dyestuff from dyestuff kettle
Boiling for supercritical carbon dioxide fluid bleaching and dyeing kettle；
Receive from the piece-rate system for boiling the material for bleachinging and dyeing kettle, piece-rate system can make the material carry out gas solid separation.
7. method according to claim 6, it is characterised in that：
1. overcritical boiling and bleaching process：Crudefiber crop rove, dyestuff and biology enzyme are boiled into drift agent solution it is sequentially placed into described boiling and bleachinges and dyeing kettle, dye
In material kettle and cosolvent tank；Carbon dioxide storage system is opened, to carbon dioxide is passed through in ultrasonic atomizer, makes carbon dioxide stream
Speed is 1-5m3/h；Biology enzyme in cosolvent tank is boiled in drift agent solution injection ultrasonic atomizer, through the effect of supersonic generator
It is atomized；The fluid-mixing that carbon dioxide and the biology enzyme of atomization boil drift agent solution mixes in ultrasonic atomizer；It is uniform molten
Solution has the carbon dioxide that biology enzyme boils drift agent to enter supercriticality in the presence of heater, and is noted in the presence of booster pump
Enter to boiling and bleaching and dyeing inside kettle, interior circulation is carried out to bast-fibre rove in the presence of magnetic force circulating pump and/or drift is boiled in outer circulation,
Overcritical boiling and bleaching process condition is：Temperature is 25-70 DEG C, and pressure is 8-30MPa, boils the drift time for 10-60min；
2. it is overcritical to boil drift-separating technology：Magnetic force circulating pump is closed, carries out boiling drift-separation circuit in the presence of booster pump, boiled
Drift-separation process conditions are：Temperature is 25-70 DEG C, and pressure is 8-30MPa, and it is 10-30min to boil drift disengaging time；
3. supercritical dyeing technique：After the completion of boiling drift-separating technology, close cosolvent tank, and using heater by dyestuff kettle and
Boil and bleaching and dyeing kettle and be warming up to 80-120 DEG C；During dyeing process, access dyestuff kettle, carbon dioxide storage system in the system of bleachinging and dyeing are being boiled first
Carbon dioxide outflow in system, enters supercriticality, and dyestuff is injected in the presence of booster pump in the presence of heater
Kettle；Supercritical carbon dioxide fluid flows into the dyestuff that dyestuff kettle is dissolved in it first, subsequently enters to boil and bleachinges and dyeing in kettle, to therein
Bast-fibre rove is dyeed, and carries out interior dye and outer dye processing to bast-fibre rove in the presence of magnetic force circulating pump；
After dyeing terminates, the supercritical carbon dioxide fluid for being dissolved with dyestuff is separated in piece-rate system, realizes dyestuff and gaseous state two
Carbonoxide is sufficiently separated.
8. method according to claim 7, it is characterised in that：Drift-the separating technology that boils is：Unlatching booster pump makes fresh
Supercritical carbon dioxide enter and boil and bleaching and dyeing kettle, carry out boiling drift using fresh supercritical carbon dioxide, will be boiled while boiling drift
Material in drift kettle is separated in sending into piece-rate system successively.
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| WO2020077665A1 (en) * | 2018-10-16 | 2020-04-23 | 苏州大学 | Anhydrous fiber dyeing method for mixed fluid medium |
| US11560669B2 (en) | 2018-10-16 | 2023-01-24 | Soochow University | Fiber dyeing method using mixed fluid medium |
| CN110528089A (en) * | 2019-09-12 | 2019-12-03 | 大连工业大学 | Super (Asia) the critical CO of one kind2Scouring of wool method |
| CN110528089B (en) * | 2019-09-12 | 2022-02-18 | 大连工业大学 | Super (sub) critical CO2 wool scouring method |
| CN110565415A (en) * | 2019-10-11 | 2019-12-13 | 上海复璐帝流体技术有限公司 | Supercritical carbon dioxide printing and dyeing process and printing and dyeing system thereof |
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