CN108716138A - A kind of dye liquor and colouring method of list solute indirect electrochemical indigotin - Google Patents

A kind of dye liquor and colouring method of list solute indirect electrochemical indigotin Download PDF

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Publication number
CN108716138A
CN108716138A CN201810509867.8A CN201810509867A CN108716138A CN 108716138 A CN108716138 A CN 108716138A CN 201810509867 A CN201810509867 A CN 201810509867A CN 108716138 A CN108716138 A CN 108716138A
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China
Prior art keywords
dye liquor
indigotin
dyeing
solute
reduction
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CN201810509867.8A
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Chinese (zh)
Inventor
熊伟
谭晓冬
徐杰
易长海
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Wuhan Textile University
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Wuhan Textile University
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Priority to CN201810509867.8A priority Critical patent/CN108716138A/en
Publication of CN108716138A publication Critical patent/CN108716138A/en
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Classifications

    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General 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
    • D06P1/22General 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 vat dyestuffs including indigo
    • D06P1/228Indigo
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General 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
    • D06P1/44General 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
    • D06P1/64General 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 using compositions containing low-molecular-weight organic compounds without sulfate or sulfonate groups
    • D06P1/651Compounds without nitrogen
    • D06P1/65106Oxygen-containing compounds
    • D06P1/65118Compounds containing hydroxyl groups

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Coloring (AREA)

Abstract

The present invention relates to a kind of dye liquor and colouring method of single solute indirect electrochemical indigotin, its solvent of the dye liquor be water and include following concentration each raw material:The highly basic of 0.01-0.1mol/L, the electronics transfer accelerating agent of 0.001-0.1mol/L, 0.01-0.1mol/L bipseudoindoxyl dyes;The colouring method first restores dye liquor completely in electrolytic cell, it is then transferred in staining bath and to yarn dyeing, it will be restored in dye liquor pumpback to electrolytic cell that a part is aoxidized and again in dyeing course, it is evacuated to again in staining bath to yarn dyeing after reduction, dyeing is lasting to be carried out, the intermittent part pumpback reduction of dye liquor and reuse.It has the beneficial effect that, the use of dihydroxy anthraquinone is electronics transfer accelerating agent, effectively accelerate electrochemical reduction rate, improve current efficiency;It is indigo to be restored in the lye of low concentration after electronics transfer accelerating agent is added, chemical consumption is reduced, production cost is substantially reduced.

Description

A kind of dye liquor and colouring method of list solute indirect electrochemical indigotin
Technical field
The invention belongs to the reduction stain fields of bipseudoindoxyl dye, and in particular to a kind of list solute indirect electrochemical indigotin Dye liquor and colouring method.
Background technology
Indigo is most ancient one of known dye.Due to the prevalence of blue jeans, the consumption of dyestuff be it is huge, Blue jeans indigo dyeing.Indigo and other reducing dyes consumptions reach about 33,000,000 kilograms every year.It is indigo It can be used in dyeing course, but need to be reduced into its water-soluble leuco form.Its reduction form has cellulose fibre very high Affinity, thus be easily absorbed into fiber, when its re-oxidation returns its blue insoluble form, then rest in fiber. Industrial reduction is carried out with sodium dithionite, because the formation of the waste byproducts such as sulphite, sulfate and sulphur is made At environmentally hazardous problem.Therefore, the presence that business Indigo Dyeing substitutes the substitute of sodium dithionite is that have must It wants.
A kind of method reducing waste is the direct or indirect electrochemical reduction using different redox mediators, Indirect Electro Electronation carrys out the electronics between transfer electrode and dye molecule using the complex of redox active iron.But its shortcoming It is the facilitation unobvious of the electronics between its transfer electrode and dye molecule, the efficiency of indirect electrochemical indigotin is not It is high.
Invention content
The present invention provides a kind of dye liquor and colouring method of solute indirect electrochemical indigotin, it is intended to solve the prior art In the indigo dye liquor of electrochemical reduction in it is indigo it is low with the electron transfer efficiency of electrode surface caused by staining efficiency is low, energy consumption The deficiencies of high.
The technical solution that the present invention solves above-mentioned technical problem is as follows:A kind of dye of list solute indirect electrochemical indigotin Liquid, solvent be water and include following concentration each raw material:The highly basic of 0.01-0.1mol/L, the electronics of 0.001-0.1mol/L Shift accelerating agent, 0.01-0.1mol/L bipseudoindoxyl dyes.
Based on the above technical solution, the present invention can also do specific choice further below.
Specifically, the highly basic is sodium hydroxide or potassium hydroxide.
Specifically, the electronics transfer accelerating agent is 1,8- dihydroxy anthraquinones or 2,6- dihydroxy anthraquinones.
The present invention also provides a kind of methods that above-mentioned dye liquor is dyed comprising following steps:Dye liquor is placed in electricity Solve in slot, dye liquor temperature controlled at 40-60 DEG C by heating device, be equipped with cathode and anode in electrolytic cell, anode and cathode with After the positive and negative anodes of DC power supply are connected, control current density is 0.08-2 amperes/square decimeter, after dye liquor completely reduction, is led to It crosses the first pumping press pump dye liquor is evacuated in staining bath to carry out yarn dyeing, 0.25-0.5h is often passed through in dyeing course or monitors to contaminate When the oxidation-reduction potential of liquid is increased to preset value, the dye liquor of partial oxidation is taken out into 1/3 to 1/2 body of press pump pumpback by second Product was in electrolytic cell and connecting DC power supply and restored completely by the dye liquor in pumpback to electrolytic cell, completely after reduction, by the One pumping press pump is evacuated in staining bath again, and so cycle carries out, until dyeing terminates, entire dyeing course continues 1h or more.
Based on the above technical solution, the present invention, which can also be done, further below more preferably selects.
Best, dye liquor temperature is controlled at 45-50 DEG C by heating device.
Best, after connecting DC power supply, current density is controlled in 0.5-1 amperes/square decimeter.
Compared with prior art, the beneficial effects of the invention are as follows:
Using between 1,8- dihydroxy anthraquinones or 2,6- dihydroxy anthraquinones are electronics transfer accelerating agent, indigo in electrochemical reduction During, indigo and electrode surface electronics transfer can be effectively facilitated, electrochemical reduction rate is accelerated, improves electric current effect Rate;It is indigo to be restored in the lye of low concentration after electronics transfer accelerating agent is added, chemical consumption is reduced, is dropped significantly Low production cost;Meanwhile by being monitored to dye liquor oxidation-reduction potential, it can effectively ensure that dyeing quality.
Description of the drawings
Fig. 1 is the schematic diagram of the Electrochemical Dyeing device used with colouring method provided by the invention.
In attached drawing, parts list represented by the reference numerals are as follows:
1. electrolytic cell;2. heating device;3. anode;4. agitating device;5. DC power supply;6. first takes out press pump;7. second Take out press pump;8. cathode;9. staining bath;10. potential measurement instrument.
Specific implementation mode
Principles and features of the present invention are described below in conjunction with drawings and the specific embodiments, example is served only for solving The present invention is released, is not intended to limit the scope of the present invention.
The schematic diagram for the Electrochemical Dyeing device that colouring method provided by the invention uses is as shown in Figure 1 comprising electricity It solves slot 1, heating device 2, anode 3, agitating device 4, DC power supply 5, first and takes out the pumping of press pump 6, second press pump 7, cathode 8, staining bath 9, it both sides that potential measurement instrument 10, anode and cathode are divided into electrolytic cell 1 and amberplex is not used between the two separates, Heating device and agitating device are also set in electrolytic cell 1, potential measurement instrument is set in staining bath, and being additionally provided in staining bath several makes yarn The cord roller contacted with dye liquor.
Embodiment 1
A method of it is dyed using the dye liquor of single solute indirect electrochemical indigotin comprising following steps:
Dye liquor is placed in electrolytic cell, and 0.01mol/L sodium hydroxides, 0.02mol/L1,8- dihydroxy-anthracenes are contained in dye liquor Quinone and 0.01mol/L bipseudoindoxyl dyes, cathode are 20 mesh copper mesh, and anode is 20 mesh stainless (steel) wires, and electroreduction temperature is 60 DEG C, electricity Solution current density is 0.08 ampere/square decimeter, and electrolyte is waited to be reduced into reducing solution completely, and press pump is taken out by reducing solution by first It imports staining bath and carries out yarn dyeing, in dyeing course, every 20min, aoxidized the part of 1/2 volume by the second pumping press pump Dye liquor is drawn back into electrolytic cell, and the reducing solution in a cell being aoxidized the part carries out electrochemical reduction, realize reduction and The cycle of dye liquor between dyeing dyes and continues 1h.After the completion of dyeing, it is 77.5% to measure current efficiency.
Embodiment 2
A method of it is dyed using the dye liquor of single solute indirect electrochemical indigotin comprising following steps:
Dye liquor is placed in electrolytic cell, and 0.1mol/L sodium hydroxides, 0.05mol/L2,6- dihydroxy-anthracenes are contained in dye liquor Quinone, 0.03mol/L bipseudoindoxyl dyes, cathode are 80 mesh stainless (steel) wires, and anode is 80 mesh nickel screens, and electroreduction temperature is 45 DEG C, electricity Solution current density is 0.5 ampere/square decimeter, and electrolyte is waited to be reduced into reducing solution completely, and press pump is taken out by reducing solution by first It imports staining bath and carries out yarn dyeing, in dyeing course, every 20min, aoxidized the part of 1/2 volume by the second pumping press pump Dye liquor is drawn back into electrolytic cell, and the reducing solution in a cell being aoxidized the part carries out electrochemical reduction, realize reduction and The cycle of dye liquor between dyeing dyes and continues 1h.After the completion of dyeing, it is 82.1% to measure current efficiency.
Embodiment 3
A method of it is dyed using the dye liquor of single solute indirect electrochemical indigotin comprising following steps:
Dye liquor is placed in electrolytic cell, and 0.05mol/L sodium hydroxides, 0.002mol/L2,6- dihydroxy-anthracenes are contained in dye liquor Quinone, 0.01mol/L bipseudoindoxyl dyes, cathode are stainless steel substrates, and anode is copper sheet, and electroreduction temperature is 40 DEG C, and Faradaic current is close Degree be 2 amperes/square decimeter, wait electrolyte to be reduced into reducing solution completely, by first take out press pump by reducing solution import staining bath into Row yarn dyeing, in dyeing course, every 20min, by the second pumping press pump by the part of 1/2 volume by oxidation dye liquor draw back to In electrolytic cell, the reducing solution in a cell being aoxidized the part carries out electrochemical reduction, realizes dye liquor between reduction and dyeing Cycle, dye continue 1h.After the completion of dyeing, it is 70.2% to measure current efficiency.
Embodiment 4
A method of it is dyed using the dye liquor of single solute indirect electrochemical indigotin comprising following steps:
Dye liquor is placed in electrolytic cell, in dye liquor contain 0.1mol/L potassium hydroxide, 0.1mol/L1,8- dihydroxy anthraquinones, 0.1mol/L bipseudoindoxyl dyes, cathode are annular nickel screen, and anode is annular copper mesh, and electroreduction temperature is 50 DEG C, and Faradaic current is close Degree be 1 ampere/square decimeter, wait electrolyte to be reduced into reducing solution completely, by first take out press pump by reducing solution import staining bath into Row yarn dyeing, in dyeing course, every 20min, by the second pumping press pump by the part of 1/2 volume by oxidation dye liquor draw back to In electrolytic cell, the reducing solution in a cell being aoxidized the part carries out electrochemical reduction, realizes dye liquor between reduction and dyeing Cycle, dye continue 1h.After the completion of dyeing, it is 85.4% to measure current efficiency.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all the present invention spirit and Within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.

Claims (6)

1. a kind of dye liquor of list solute indirect electrochemical indigotin, which is characterized in that solvent is water and includes following concentration Each raw material:The highly basic of 0.01-0.1mol/L, the electronics transfer accelerating agent of 0.001-0.1mol/L, the indigo dyes of 0.01-0.1mol/L Material.
2. a kind of dye liquor of single solute indirect electrochemical indigotin according to claim 1, which is characterized in that described strong Alkali is sodium hydroxide or potassium hydroxide.
3. a kind of dye liquor of single solute indirect electrochemical indigotin according to claim 1, which is characterized in that the electricity Son transfer accelerating agent is 1,8- dihydroxy anthraquinones or 2,6- dihydroxy anthraquinones.
4. a kind of dyeing side of dye liquor using 3 any one of them list solute indirect electrochemical indigotin of claims 1 to 3 Method, which is characterized in that include the following steps:Dye liquor is placed in electrolytic cell, dye liquor temperature is controlled in 40-60 by heating device DEG C, cathode and anode are equipped in electrolytic cell, after the positive and negative anodes connection of anode and cathode and DC power supply, control current density is 0.08-2 amperes/square decimeter, after dye liquor completely reduction, dye liquor is evacuated to by progress yarn dye in staining bath by the first pumping press pump Color, when often passing through 0.25-0.5h in dyeing course or monitoring that the oxidation-reduction potential of dye liquor is increased to preset value, by part The dye liquor of oxidation is taken out in 1/3 to 1/2 volume to electrolytic cell of press pump pumpback by second and connected DC power supply by pumpback to electricity Dye liquor in Xie Chi restores completely, completely after reduction, is evacuated in staining bath again by the first pumping press pump, so cycle carries out, directly Terminate to dyeing, entire dyeing course continues 1h or more.
5. a kind of colouring method of dye liquor using single solute indirect electrochemical indigotin according to claim 4, It is characterized in that, is controlled dye liquor temperature at 45-50 DEG C by heating device.
6. a kind of colouring method of dye liquor using single solute indirect electrochemical indigotin according to claim 4, It is characterized in that, after connecting DC power supply, current density is controlled in 0.5-1 amperes/square decimeter.
CN201810509867.8A 2018-05-24 2018-05-24 A kind of dye liquor and colouring method of list solute indirect electrochemical indigotin Pending CN108716138A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113416967A (en) * 2021-06-17 2021-09-21 武汉纺织大学 Method for recycling indigo dye in waste jeans and fabric dyeing method
CN113549938A (en) * 2021-06-17 2021-10-26 武汉纺织大学 Method for recycling indigo in waste denim laser waste ash

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1120357A (en) * 1993-03-30 1996-04-10 Basf公司 Method of dyeing cellulose-containing textile material with hydrogenated indigo
WO1999011716A1 (en) * 1997-09-04 1999-03-11 Basf Aktiengesellschaft Process for reducing sulphide dyestuffs
CN1344292A (en) * 1999-04-29 2002-04-10 德意志戴斯达纺织品及染料两合公司 Method for producing aqueous alkaline solutions or reduced indigoid dyes
CN1665983A (en) * 2002-07-31 2005-09-07 德意志戴斯达纺织品及染料两合公司 Method for dyeing with sulphur and sulphur vat dyes

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1120357A (en) * 1993-03-30 1996-04-10 Basf公司 Method of dyeing cellulose-containing textile material with hydrogenated indigo
WO1999011716A1 (en) * 1997-09-04 1999-03-11 Basf Aktiengesellschaft Process for reducing sulphide dyestuffs
CN1344292A (en) * 1999-04-29 2002-04-10 德意志戴斯达纺织品及染料两合公司 Method for producing aqueous alkaline solutions or reduced indigoid dyes
CN1665983A (en) * 2002-07-31 2005-09-07 德意志戴斯达纺织品及染料两合公司 Method for dyeing with sulphur and sulphur vat dyes

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113416967A (en) * 2021-06-17 2021-09-21 武汉纺织大学 Method for recycling indigo dye in waste jeans and fabric dyeing method
CN113549938A (en) * 2021-06-17 2021-10-26 武汉纺织大学 Method for recycling indigo in waste denim laser waste ash
CN113549938B (en) * 2021-06-17 2022-06-21 武汉纺织大学 Method for recycling indigo in waste denim laser waste ash

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Application publication date: 20181030