CN105133396A - Supercritical CO<2> dyeing and printing process - Google Patents

Supercritical CO<2> dyeing and printing process Download PDF

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Publication number
CN105133396A
CN105133396A CN201510529652.9A CN201510529652A CN105133396A CN 105133396 A CN105133396 A CN 105133396A CN 201510529652 A CN201510529652 A CN 201510529652A CN 105133396 A CN105133396 A CN 105133396A
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China
Prior art keywords
dyeing
supercritical
fabric
pump
printing process
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CN201510529652.9A
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Chinese (zh)
Inventor
郭峻山
王威强
刘燕
曲延鹏
崔书水
王明禄
刘虎廷
陈银
王胜德
于丽杰
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BEIJING GUOBANG SCIENCE AND TECHNOLOGY DEVELOPMENT Co Ltd
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BEIJING GUOBANG SCIENCE AND TECHNOLOGY DEVELOPMENT Co Ltd
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Priority to CN201510529652.9A priority Critical patent/CN105133396A/en
Publication of CN105133396A publication Critical patent/CN105133396A/en
Pending legal-status Critical Current

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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06BTREATING TEXTILE MATERIALS USING LIQUIDS, GASES OR VAPOURS
    • D06B19/00Treatment of textile materials by liquids, gases or vapours, not provided for in groups D06B1/00 - D06B17/00

Abstract

The invention belongs to the field of dyeing process, and especially relates to a supercritical CO<2> fluid solubilizing dyeing method. A dye is dissolved in a CO<2> supercritical fluid, a solubilizer being added when needed, for dyeing a fabric. The method comprises device initialization, fabric pretreatment, dyeing, and after-treatment of fabric. The method comprises more concretely: placing a dye in a dye kettle, placing the solubilizer in the solvent tank, winding a fabric around a dyeing shaft and placing the wound fabric in a dyeing device, inputting liquid CO<2> via a booster pump, and enabling the supercritical CO<2> fluid in which the dye is dissolved to circulate in the dyeing kettle and the dye kettle via a circulating pump. In the invention, the dye is dissolved in the supercritical CO<2> fluid, and the solubilizer is added when needed, for dyeing the fabric; the supercritical CO<2> dyeing and printing process saves a large amount of water resource; furthermore, dyeing process conditions such as the pressure, temperature and time are optimized to promote the solubility and dyeing deepness of the dispersed dye in the supercritical CO<2> fluid so that the dyeing is suitable for all kinds of plant fiber fabrics and synthetic fiber fabrics.

Description

A kind of supercritical CO 2dyeing and printing process
Technical field
The invention belongs to field of dyeing process, particularly relate to a kind of supercritical CO 2 fluid colouring method.
Background technology
Along with textile industry develops rapidly, the environmental pollution that process of textile production causes receives publicity day by day.Country has worked out a series of strict environmental legislation in succession, supervises the sewage disposal of industrial quarters and discharge etc.According to statistics, the fabric weight of textile printing and dyeing processing and the ratio of water consumption are up to 1:100 ~ 1:150, and national dyeing and printing process water consumption estimates annual 1600000000 tons.At present, the Treated sewage reusing ratio of the sector production process is very low, and sewage disposal and discharge account for production cost ratio increases gradually.
Traditional dyeing course, using water as medium, plays dispersion and dissolving dye and auxiliary agent, soaks and the important function such as swollen fiber, seem do not have water just cannot dye.But nature freshwater resources start shortage, water pollutions is very serious.Now, in order to reduce water consumption and the dyeing waste of Colour Difference, people carry out large quantity research, are devoted to exploitation water saving and anhydrous staining technique.
Adopt supercritical CO 2 fluid technique, utilizes reusable CO 2 , at supercritical conditions with CO 2 fluid is that medium carries out Colour Difference, the integrated costs such as its energy resource consumption are lower than conventional dyeing process, achieve non-aqueous dyeing, energy-saving and emission-reduction, therefore, supercritical CO2 fluid dyeing technology have anhydrous, reduce discharging, energy-conservation technical advantage, be a suitability for industrialized production new technology with development prospect.
Supercritical CO 2 fluid refers to CO 2 in the density fluid state higher than the non-condensed property under critical-temperature (Tc=31 DEG C) and critical force (Pc=7.2MPa) condition, namely at more than Tc by CO 2 gas compression is to higher than more than Pc, CO 2 density can carry out consecutive variations significantly in the scope from gas to liquid.Supercritical CO 2 the character of fluid system, as gas, specifically has the high density as liquid and the low viscosity as liquid.By changing these two performance variables of temperature and pressure of system, the density of fluid, viscosity (intermolecular distance) can be regulated, make it have specific physical property.
Supercritical CO 2 the feature of fluid is as follows: 1, only slightly change pressure, its density is just more big changes, and due to its low viscosity and high diffusibility, is conducive to the movement of material; 2, because the temperature difference moves greatly, higher translational speed can be obtained.At present, supercritical CO is utilized 2 the advantage of fluid, it is used for extraction and is separated with chromatographic and refined substance etc., such as extracting hop, natural product extraction etc., have a wide range of applications future in light industry, food, chemical industry, medicine and other fields.
As everyone knows, Colour Difference water consumption is many, electric energy and consumption of heat energy large, the chemicals used is many, dyestuff containing non-set in the waste water of discharging after dyeing and auxiliary agent, reclaim difficulty, waste water treatmentntrol difficult, needs constantly to increase cost of water treatment to reach the sewage drainage standard improved gradually.Obviously, conventional colouring method more and more will be difficult to adapt to national energy-saving and reduce discharging industrial development strategy.
Summary of the invention
The object of the invention is to: a kind of supercritical CO is provided 2 the fluid side of dyeing technique, is intended to solve the problem that existing water dyeing causes shortage of water resources and pollution.
Below concrete technical scheme:
A kind of supercritical CO 2dyeing and printing process, passes through supercritical CO 2fluid dissolving dye, then solubilizer is increased as solubilizer need be added according to fabric types, fabric is dyeed, comprise device initialization, fabric pretreatment, dyeing, fabric post processing, be specially: dyestuff is loaded dyestuff still, solvent put into when solvent tank fabric does not need and then do not add, fabric is wound on dyeing axle and puts into dyeing apparatus, input liquid carbon dioxide by booster pump, will the supercritical CO of DISPERSE DYES be dissolved with by circulating pump 2dyeing fluid circulates between dyeing caldron and dyestuff still.
Wherein said device initialization step comprises:
Open by hydraulic control device device of dying cloth, carry out treating that dye thing is loaded, after filling, close device of dying cloth;
Open dyestuff dissolvers after closedown, add dyestuff according to activity coefficient, then close dyestuff dissolvers.
Described fabric pretreatment step comprises:
Open valve and control valve and open vavuum pump, carrying out vacuumizing of dyeing apparatus, when vacuum characterization device low vacuum is in 0.003MPa, closes vavuum pump and close the valve be connected with vavuum pump, closedown control valve;
Open again and CO 2the valve that storage tank is connected, passes through CO 2gas, keeps in storage tank and CO 2source of the gas is connected.
Described fabric pretreatment step comprises:
In heat exchanger, pass into industrial steam, control steam flow rate and make temperature at about 80 DEG C;
Open cold-producing medium, make CO 2before flowing through booster pump, whole condensation, passes through CO 2booster pump makes liquid CO 2obtain preheating after supercharging, enter dyeing cycle unit through heat exchanger.
By heating, control temperature is at about 120 DEG C, and pressure about 20MPa, carries out fabric cleaning by the power circulating device of stainer, and under keeping plant to be in tensile force effect in cleaning process, cleaning process completes one-period.
Described staining procedure comprises:
After having cleaned, be held open heat exchanger, CO 2force (forcing) pump, preheater, solvent pump, make CO 2post liquefaction fully mixes in flow mixing device with auxiliary agent;
Carry out dyeing cycle unit afterwards, make amount of carbon dioxide in dyeing cycle unit reach capacity after 1 hour, ON cycle heater, circulating pump afterwards, then open device drive motors of dying cloth, carry out supercritical CO 2fluid dyestuff carries out the upper dye of fabric.
Described lock out operation comprises the following steps:
Heater, keeps separator pressure in about 4MPa, temperature at about 70 DEG C, the CO after separation after filtering 2condensation after heat exchanger, condenser heat exchange, reclaims into storage tank.
Described fabric cleaning comprises the following steps:
After lock out operation terminates, when circulating pump pressure is 1MPa, ON cycle pump, passes into pure CO 2carry out loose colour cleaning.
Described one-period comprise roller of dying cloth complete one twine cloth, put cloth circulation.
CO is carried out after described fabric cleaning terminates 2separation and recovery, its separation and recovery step comprise lock out operation institute in steps.
Described CO 2separation and recovery terminate after, new round dying operation again, closes indivedual valve and opens some valves, device of dying cloth enter dyeing cycle loop carry out fabric pretreatment institute in steps.
Beneficial effect: the present invention passes through supercritical CO 2fluid dissolving dye, and add solubilizer when needed, fabric is dyeed, save a large amount of water resources, simultaneously, by optimizing the dyeing such as pressure, temperature and time condition, improving the solubility of DISPERSE DYES in supercritical fluid CO 2, dye level etc., being applicable to the dyeing of various vegetable fibre fabric, synthetic fabrics etc.
Accompanying drawing explanation
Fig. 1 is technological process application drawing of the present invention.
Detailed description of the invention
Below in conjunction with Figure of description, the invention will be further described.
A kind of supercritical CO 2dyeing and printing process, passes through supercritical CO 2fluid dissolves DISPERSE DYES, and increase solubilizer when needed, fabric is dyeed, comprise device initialization, fabric pretreatment, dyeing, fabric post processing, be specially: dyestuff is put into dyeing caldron, as needed solubilizer that solubilizer is put into solvent tank, fabric be wound on dyeing axle and put into dyeing apparatus, inputting liquid carbon dioxide by booster pump, is the supercritical CO being dissolved with dyestuff by circulating pump 2dyeing fluid circulates between dyeing caldron and dyestuff still.
Wherein said device initialization step comprises:
Open by control device device of dying cloth, carry out treating that dye thing is loaded, after filling, close device of dying cloth;
Open dyestuff dissolvers after closedown, add DISPERSE DYES according to activity coefficient, then close dyestuff dissolvers.
Described fabric pretreatment step comprises:
Open valve and control valve and open vavuum pump, carrying out vacuumizing of dyeing apparatus, when vacuum characterization device low vacuum is in 0.003MPa, closes vavuum pump and close the valve be connected with vavuum pump, closedown control valve;
Open again and CO 2the valve that storage tank is connected, passes through CO 2gas, keeps storage tank to be connected with CO2 source of the gas.
Described fabric pretreatment step comprises:
In heat exchanger, pass into industrial steam, control steam flow rate and make temperature at about 80 DEG C;
Open cold-producing medium, make CO 2before flowing through booster pump, whole condensation, passes through CO 2booster pump makes liquid CO 2obtain preheating after supercharging, enter dyeing cycle unit through heat exchanger.
By heating, control temperature is at about 120 DEG C, and pressure about 20MPa, carries out fabric cleaning by the power circulating device of stainer, and under keeping plant to be in tensile force effect in cleaning process, cleaning process completes one-period.
Described staining procedure comprises:
After having cleaned, be held open heat exchanger, CO 2force (forcing) pump, preheater, solvent pump, make CO 2post liquefaction fully mixes in flow mixing device with auxiliary agent;
Carry out dyeing cycle unit afterwards, make amount of carbon dioxide in dyeing cycle unit reach capacity after 1 hour, ON cycle heater, circulating pump afterwards, then open device drive motors of dying cloth, carry out supercritical CO 2fluid dyestuff carries out the upper dye of fabric.
Described lock out operation comprises the following steps:
Heater, keeps separator pressure in about 4MPa, temperature at about 70 DEG C, the CO after separation after filtering 2condensation after heat exchanger, condenser heat exchange, reclaims into storage tank.
Described fabric cleaning comprises the following steps:
After lock out operation terminates, when circulating pump pressure is 1MPa, ON cycle pump, passes into pure CO 2carry out loose colour cleaning.
Described one-period comprise roller of dying cloth complete one twine cloth, put cloth circulation.
CO is carried out after described fabric cleaning terminates 2separation and recovery, its separation and recovery step comprise lock out operation institute in steps.
Described CO 2separation and recovery terminate after, new round dying operation again, closes indivedual valve and opens some valves, device of dying cloth enter dyeing cycle loop carry out fabric pretreatment institute in steps.
Embodiment 1
Below that combined process flow operations figure does further optimization to the present invention.
1, device initializes:
Ensure that all valves are all in closed condition before driving;
First open by hydraulic control device device D401 and the D402 that dyes cloth, carry out the filling waiting to contaminate thing, after filling, close device of dying cloth;
Open dyestuff dissolvers Et401, according to activity coefficient, about 1/3 adds DISPERSE DYES, closes dyestuff dissolvers Et401 afterwards; Solvent tank needs to determine whether add corresponding dyeing assistant according to technique.
2, device air purge:
Open valve V108, V204, V205, V401, V405, V406, V408, V411, V412, V414, FV501(all-pass state successively), FV502(all-pass state);
Open valve V109, open vavuum pump P101, carry out vacuumizing of dyeing apparatus, after about ten minutes, when namely vacuum meter PI101 characterizes whole equipment vacuum degree lower than 0.003MPa, valve-off V109, closes vavuum pump P101, closes control valve FV501;
Open valve V104, whole circuit passes into a certain amount of CO 2gas, maintenance C101 communicates with source of the gas.
3. fabric pretreatment:
Pass into industrial steam in heat exchanger E202, after hot water temperature reaches 80 DEG C, control steam flow maintain this temperature.Open valve V104, opening refrigeration machine Re201, is CO 2after flowing through heat exchanger E201, whole condensation, opens CO 2booster pump P201, liquid CO 2obtain preheating after flowing through accumulator E202, enter dyeing cycle unit through heat exchanger E203, now V402, V404 are in closed condition, CO 2constantly enter dyeing cycle unit, add the CO of appropriate amount 2after, valve-off V104, V205, close heat exchanger E201, E202, closes force (forcing) pump P201.Continuous increasing temperature and pressure under heat exchanger E401 heats, control temperature about 120 DEG C, pressure is at about 20MPa, open the power circulating device of stainer, carry out the cleaning of fabric, under keeping fabric to be in suitable tensile force effect in cleaning process, cleaning process complete one-period (roller of dying cloth complete one twine cloth, put cloth circulation).
After cleaning terminates, open control valve FV501, regulate FV502, heater E501, under 4MPa, the process conditions of 60 DEG C, carry out lock out operation, make dissolved matter and the CO of cleaning process 2be separated in S501, open valve V107, V106 and V104 successively, open pump P201, through the condensed CO of E202, E201 after being separated 2pump in storage tank C101.
Reclaim CO 2terminate, close pump P201, heat exchanger E201, valve-off V104, V106, V107, FV501, FV502.
4. dying operation:
Open valve V104, V106, V204, V205, CO 2enter dyeing cycle unit, treat line pressure and CO 2when storage tank V101 reaches balance (PI401 registration is basicly stable), valve-off V106, opens valve V108 and opens heat exchanger E201, CO 2force (forcing) pump P201, preheater E203, open V302, V306 and solvent pump P301, at this moment CO simultaneously 2post liquefaction fully mixes in flow mixing device X201 with auxiliary agent, enters dyeing cycle unit afterwards, and in about 1h Posterior circle dye unit, amount of carbon dioxide reaches capacity, and at this moment PIC201 can control CO 2pump quits work, valve-off V104, V108, V204, V205; Close V302, solvent pump P301, V306 simultaneously.
Open valve V402, V404, valve-off V401; ON cycle heater E401, circulating pump P401, open device D401 drive motors of dying cloth after temperature, pressure all reach coloration requirements in loop to be recycled, supercritical CO 2fluid carry-over dyestuff carries out the upper dye of fabric.
After having dyeed, close device D401 driving motor of dying cloth, dyestuff dissolvers Et401 heater, circulating pump P401, heat exchanger E401; Open valve V401, valve-off V402, V404.Open valve V407, V409, make after in D401 and D402, pressure reaches balance, closes V407, V409,
5. lock out operation
Valve-off V411, Open valve FV501, FV502, heater E501, controls pressure in separator S501 and remains on about 4MPa, temperature 70 DEG C about, Open valve V107, condenser E201 simultaneously, separation CO after metre filter 2condensation after heat exchanger E202, condenser E203 heat exchange, at this moment opens CO 2pump P201, valve V104, V106, by liquid CO 2pump in storage tank C101; Valve-off FV501, FV502, V107, condenser E201, CO after whole separation process terminates 2pump P201, V104 and V106.
6. fabric cleaning
After lock out operation terminates, if clean textile loose colour, Open valve V104, V106, V204, V205 and V412, after PI401 pressure reaches 1MPa, valve-off V104, V106, V204 and V205; Then ON cycle pump P401, passes into pure CO 2carry out loose colour cleaning, after cleaning, close circulating pump P401, valve-off V412, carries out CO 2separation and recovery, operation is with 5.
After lock out operation completes, new round dying operation again, at this moment valve-off V413, V415, Open valve V407, V409, the device D402 that dyes cloth enters dyeing cycle loop, and other operation is with step 3.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.

Claims (10)

1. a supercritical CO 2dyeing and printing process, is characterized in that, described technique is for passing through supercritical CO 2fluid dissolving dye, and at taken increase solubilizer, fabric is dyeed, comprise device initialization, fabric pretreatment, dyeing, fabric post processing, be specially: dyestuff is put into dyestuff still, solvent tank put into by solubilizer, fabric be wound on dyeing axle and put into dyeing apparatus, input liquid carbon dioxide by booster pump, make by circulating pump the supercritical CO being dissolved with DISPERSE DYES 2dyeing fluid circulates between dyeing caldron and dyestuff still.
2. a kind of supercritical CO according to claim 1 2dyeing and printing process, is characterized in that, described device initialization step comprises:
Open by control device device of dying cloth, carry out treating that dye thing is loaded, after filling, close device of dying cloth;
Open dyestuff dissolvers after closedown, add dyestuff according to activity coefficient, then close dyestuff dissolvers.
3. a kind of supercritical CO according to claim 1 2dyeing and printing process, is characterized in that, described fabric pretreatment step comprises:
Open valve and control valve and open vavuum pump, carrying out vacuumizing of dyeing apparatus, when vacuum characterization device low vacuum is in 0.003MPa, closes vavuum pump and close the valve be connected with vavuum pump, closedown control valve;
Open again and CO 2the valve that storage tank is connected, passes through CO 2gas, keeps in storage tank and CO 2source of the gas is connected.
4. a kind of supercritical CO according to claim 1 2dyeing and printing process, is characterized in that, described fabric pretreatment step comprises:
In heat exchanger, pass into industrial steam, control steam flow rate and make temperature at about 80 DEG C;
Open cold-producing medium, make CO 2before flowing through booster pump, whole condensation, passes through CO 2booster pump makes liquid CO 2obtain preheating after supercharging, enter dyeing cycle unit through heat exchanger;
By heating, control temperature is at about 120 DEG C, and pressure about 20MPa, carries out fabric cleaning by the power circulating device of stainer, and under keeping plant to be in tensile force effect in cleaning process, cleaning process completes one-period.
5. a kind of supercritical CO according to claim 1 2dyeing and printing process, is characterized in that, it is characterized in that, described staining procedure comprises:
After having cleaned, open heat exchanger, CO 2force (forcing) pump, preheater, solvent pump, make CO 2post liquefaction fully mixes in flow mixing device with auxiliary agent;
Carry out dyeing cycle unit afterwards, make amount of carbon dioxide in dyeing cycle unit reach capacity after 1 hour, ON cycle heater, circulating pump afterwards, then open device drive motors of dying cloth, carry out supercritical CO 2fluid dyestuff carries out the upper dye of plant.
6. a kind of supercritical CO according to claim 1 2dyeing and printing process, is characterized in that, described lock out operation comprises the following steps:
Heater, keeps separator pressure in about 4MPa, temperature at about 70 DEG C, the CO after separation after filtering 2condensation after heat exchanger, condenser heat exchange, reclaims into storage tank.
7. a kind of supercritical CO according to claim 1 2dyeing and printing process, is characterized in that, described fabric cleaning comprises the following steps:
After lock out operation terminates, when circulating pump pressure is 1MPa, ON cycle pump, passes into pure CO 2carry out loose colour cleaning.
8. a kind of supercritical CO according to claim 4 2dyeing and printing process, is characterized in that, described one-period comprise roller of dying cloth complete one twine cloth, put cloth circulation.
9. a kind of supercritical CO according to claim 7 2dyeing and printing process, is characterized in that, carries out CO after described fabric cleaning terminates 2separation and recovery, its separation and recovery step comprise according to claim 6 in steps.
10. a kind of supercritical CO according to claim 9 2dyeing and printing process, is characterized in that, described CO 2separation and recovery terminate after, new round dying operation again, closes indivedual valve and opens some valves, device of dying cloth enter dyeing cycle loop carry out according to claim 4 in steps.
CN201510529652.9A 2015-08-26 2015-08-26 Supercritical CO<2> dyeing and printing process Pending CN105133396A (en)

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CN106087310A (en) * 2016-08-26 2016-11-09 广州绿和缘生物科技有限公司 A kind of omnidistance anhydrous dyeing and finishing system and dyeing and finishing method thereof
CN106835556A (en) * 2016-12-23 2017-06-13 青岛国邦工业科技发展有限公司 A kind of continuous jig dyeing device of supercritical fluid and dyeing
CN106835758A (en) * 2016-11-21 2017-06-13 大连工业大学 A kind of crudefiber crop rove supercritical carbon dioxide biology enzyme boils bleaching and dyeing method
CN107034691A (en) * 2016-12-02 2017-08-11 江苏新瑞贝科技股份有限公司 A kind of anhydrous gaseous state dyeing process of synthetic fibers
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WO2021068277A1 (en) * 2019-10-11 2021-04-15 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
CN112981804A (en) * 2021-02-18 2021-06-18 刘州豪 Anhydrous printing and dyeing process
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WO2017206195A1 (en) * 2016-05-30 2017-12-07 南通纺织丝绸产业技术研究院 Multi-pipe quantitative medium refill system of supercritical fluid anhydrous dyeing machine
TWI649478B (en) * 2016-05-30 2019-02-01 南通紡織絲綢產業技術研究院 Supercharging system of supercritical fluid anhydrous dyeing machine
TWI649473B (en) * 2016-05-30 2019-02-01 南通紡織絲綢產業技術研究院 Multi-channel quantitative medium tank filling system for supercritical fluid waterless dyeing machine
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CN106087310A (en) * 2016-08-26 2016-11-09 广州绿和缘生物科技有限公司 A kind of omnidistance anhydrous dyeing and finishing system and dyeing and finishing method thereof
CN106835758B (en) * 2016-11-21 2019-10-22 大连工业大学 A kind of crudefiber crop rove supercritical carbon dioxide biological enzyme boils bleaching and dyeing method
CN106835758A (en) * 2016-11-21 2017-06-13 大连工业大学 A kind of crudefiber crop rove supercritical carbon dioxide biology enzyme boils bleaching and dyeing method
CN107034691A (en) * 2016-12-02 2017-08-11 江苏新瑞贝科技股份有限公司 A kind of anhydrous gaseous state dyeing process of synthetic fibers
CN106835556B (en) * 2016-12-23 2019-05-24 青岛国邦工业科技发展有限公司 A kind of continuous jig dyeing device of supercritical fluid and dyeing
CN106835556A (en) * 2016-12-23 2017-06-13 青岛国邦工业科技发展有限公司 A kind of continuous jig dyeing device of supercritical fluid and dyeing
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
CN113795599A (en) * 2019-04-29 2021-12-14 伊科斯克有限公司 Device for leather processing
WO2021068277A1 (en) * 2019-10-11 2021-04-15 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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CN112981804A (en) * 2021-02-18 2021-06-18 刘州豪 Anhydrous printing and dyeing process

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