CN104594072A - Non-aqueous medium dyeing method for reactive dyes - Google Patents
Non-aqueous medium dyeing method for reactive dyes Download PDFInfo
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Abstract
The invention provides a non-aqueous medium dyeing method for reactive dyes. The method comprises the following steps: (1) pretreating an alkaline solution, namely fully swelling a to-be-dyed material in the alkaline solution, controlling the liquid carrying rate and drying; and (2) performing non-aqueous medium dyeing of the reactive dyes, namely performing non-aqueous medium dyeing of reactive dyes on the dried to-be-dyed material, thereby obtaining the finished dyeing product. According to the method, a small amount of good solvents of reactive dyes and carbon dioxide are taken as dyeing media, so that the reactive dyes can be prevented from being hydrolyzed during dyeing, the toxicity of the dyeing media can be greatly reduced, the good solvents of the reactive dyes and the carbon dioxide are depressurized and are spontaneously separated after the dyeing operation is ended, the dyes can be recycled, and environment-friendly dyeing of the reactive dyes can be really realized.
Description
Technical field
The present invention relates to a kind of non-aqueous media colouring method of REACTIVE DYES, belong to textile dyeing and finishing technical field.
Background technology
The dyeing of current reactive fibre adopts REACTIVE DYES mostly, because active group is hydrolyzed in aqueous medium in dyeing course, not only cause the waste of a large amount of REACTIVE DYES, and need consume a large amount of water and discharge a large amount of reluctant high chroma sewage in dyeing course, this is also REACTIVE DYES Problems existing all the time.
In order to avoid the hydrolysis of REACTIVE DYES, improve the utilization rate of REACTIVE DYES, scientists is being noted very early and have studied the dyeing of REACTIVE DYES in non-aqueous media.Adopt the advantage of non-aqueous media dyeing to be that REACTIVE DYES can not be hydrolyzed in dyeing course, be expected to the extent of reaction that can improve REACTIVE DYES and fiber.But simultaneously, adopt non-aqueous media dyeing also to there is more problem always, mainly comprise the dissolubility of REACTIVE DYES in non-aqueous media, the Swelling Capacity of fiber in non-aqueous media, the fixation alkaline agent solubility in non-aqueous media and the level-dyeing property, through-dyeing etc. of dyeing.Although REACTIVE DYES dyes and there is many difficult points in non-aqueous media, present stage use water cost raise gradually, and people more and more pay attention to environmental protection, and the dyeing of REACTIVE DYES non-aqueous media also more and more receives publicity with its good application prospect.
The eighties in last century, textile technology research institute of India adopts dimethyl formamide lytic activity dyestuff C.I. active red 12, and add trichloro-ethylene in batches and be incubated 1h being warming up in the process of 80 DEG C, dyestuff is completely upper dye almost, and degree of fixation is 84%.Although the method provides a good solvent dyeing thinking, dyeing terminates rear method separation and recovery two kinds of solvents needing to adopt distillation, and energy consumption is high, and the solvent recovery cycle is long.Meanwhile, the chlorinated solvents toxicity of use is higher, and this is also one of key factor always limiting the method development.
Supercritical carbon dioxide enjoys people to pay close attention to its environmental protection cheapness, supercritical carbon-dioxicle dyeing method also enjoys people to pay close attention to always, but up to the present, supercritical carbon dioxide is suitable only for the dyeing of polyster fibre, and is in bottleneck stage to the dyeing of natural fabric always.Sight is concentrated on the exploitation of new reactive dyes by research workers, improves in the preliminary treatment of the solubility of REACTIVE DYES in supercritical carbon dioxide and natural fabric.
In existing supercritical carbon-dioxicle dyeing method, without exception be all by supercritical carbon dioxide go dissolve or dispersed activity dyestuff, again dyestuff is transferred on fiber, but mostly there is intrinsic drawback in these methods, do not reach the Color of expection.Such as, in order to realize solving the low problem of traditional activated dyestuff solubility in supercritical carbon dioxide, designers develop the dispersed activity dyestuff without water soluble group, can to a certain degree solve dyestuff problem insoluble in supercritical carbon dioxide, but low without the affinity of dispersed activity dyestuff to natural fabric of water soluble group, be difficult to dye dark color and permeability level-dyeing property is poor; In order to solve low polar dies (as DISPERSE DYES, dispersed activity dyestuff) problem low to fiber affinity, designers attempt hydrophobic modification fiber, improve the affinity of dyestuff and fiber, but the method result in the change of fibre composition and feel, and complex process, be difficult to the sense comfortable and easy to wear keeping natural fabric.In a word, supercritical carbon-dioxicle dyeing method at present to the dyeing of natural fabric also exist always dye dark, contaminate irregular, that dye is not saturating technical bottleneck.
Summary of the invention
For solving the problems of the technologies described above, the invention provides a kind of non-aqueous media colouring method of REACTIVE DYES, the series of advantages such as the method has low toxicity, cheapness, Color is excellent, dye utilization rate is high, solvent load is little, solvent recovery is easy.
For achieving the above object, the invention provides a kind of non-aqueous media colouring method of REACTIVE DYES, it comprises the following steps:
(1) alkaline solution preliminary treatment: thing to be dyed is carried out in alkaline solution fully swelling after, control liquid carrying rate and also dry;
(2) the non-aqueous media dyeing of REACTIVE DYES: the non-aqueous media dyeing thing to be dyed of above-mentioned oven dry being carried out REACTIVE DYES, obtains dyeing product.
In the above-mentioned methods, preferably, in step (1), thing to be dyed is carried out fully swelling comprising in alkaline solution: thing to be dyed is placed in the alkaline solution that concentration is 1-100g/L, at 10-40 DEG C, soaks 1-30min; More preferably, the concentration of described alkaline solution is 5-50g/L.
In the above-mentioned methods, preferably, in step (1), described alkaline solution comprises the combination of one or more in sodium carbonate liquor, sodium bicarbonate solution, sodium hydroxide solution, lithium hydroxide solution, potassium hydroxide solution.
In the above-mentioned methods, preferably, in step (1), described liquid carrying rate controls as 30-200%; More preferably, the method controlling liquid carrying rate comprises centrifugal dehydration or roll pressure rolling.
In the above-mentioned methods, preferably, described step (2) comprising: be placed in reaction vessel by the thing to be dyed after step (1) process, add the good solvent of REACTIVE DYES and REACTIVE DYES wherein, then pass into CO wherein
2gas, the pressure in adjustment reaction vessel and temperature are to CO
2in supercriticality, isothermal reaction is to the fully upper dye of REACTIVE DYES at such a temperature, obtains dyeing product.
In the above-mentioned methods, preferably, in step (2), the mass ratio of the good solvent of described thing to be dyed and REACTIVE DYES is 1:2-50, is preferably 1:3-10; Described CO
2the mass ratio of the good solvent of gas and REACTIVE DYES is 3-50:1; The consumption of described REACTIVE DYES is not particularly limited, can according to the consumption of the requirement determination dyestuff of actual dye level.
In the above-mentioned methods, preferably, in step (2), the good solvent of described REACTIVE DYES can lytic activity dyestuff, but not with REACTIVE DYES generation chemical reaction; More preferably, the good solvent of described REACTIVE DYES is polar solvent, and it comprises the combination of one or more in DMF, DMA, dimethyl sulfoxide (DMSO), ionic liquid, alcohol ether solvents.
When dyeing, the good solvent of REACTIVE DYES and supercritical carbon dioxide act synergistically, by slowly reducing the solubility of REACTIVE DYES in the good solvent of REACTIVE DYES, REACTIVE DYES is shifted on fiber, the good solvent of this REACTIVE DYES can be miscible mutually with supercritical carbon dioxide simultaneously, and reducing energy and carbon dioxide separation under temperature and pressure.
In the above-mentioned methods, preferably, the material of described thing to be dyed comprises cellulose fibre, protein fibre, the combination of one or more had in the synthetic fiber of reactive group, wherein, the reactive group had described in the synthetic fiber of reactive group comprises the combination of one or more in amide groups, amino, hydroxyl; More preferably, described cellulose fibre comprises the combination of one or more in cotton fiber, flax fibre, viscose acetal fibre; Protein fibre comprises one or both the combination in wool, silk; The synthetic fiber with reactive group comprise nylon; The form of described thing to be dyed comprises fiber, yarn, fabric or ready-made clothes.
In the above-mentioned methods, preferably, the method is also included in step (2) and terminates rear recovery CO
2the step of the good solvent of gas and REACTIVE DYES.
In the above-mentioned methods, preferably, described recovery CO
2the step of the good solvent of gas and REACTIVE DYES comprises: after dyeing terminates, by the Pressure Drop in autoclave to below 100bar, to the CO discharged
2the good solvent of gas and REACTIVE DYES reclaims.
Beneficial effect of the present invention:
The present invention looks for another way, first the good solvent of dyestuff by REACTIVE DYES is dissolved and uniform wet thing to be dyed, reduce dyestuff solubility in a solvent by the compatibility of the good solvent of supercritical carbon dioxide and REACTIVE DYES again, reach the object that dye efficient contaminates.This Staining Protocol can farthest avoid supercritical carbon dioxide to be applied to REACTIVE DYES to the drawback existed during stock-dye, makes the state that the effect of dyestuff reaches best.
The non-aqueous media colouring method of REACTIVE DYES provided by the invention uses good solvent and the CO of a small amount of REACTIVE DYES
2gas, as dyeing medium, not only can avoid the hydrolysis of REACTIVE DYES, significantly can reduce the toxicity of dyeing medium simultaneously, and dyeing terminate after the good solvent of REACTIVE DYES and CO
2gas is spontaneous separation after step-down, can be recycled, and really achieves the environmental protection dyeing of REACTIVE DYES.The method effectively combines supercritical CO
2the advantage of good solvent dyeing medium in REACTIVE DYES application of dyeing medium and REACTIVE DYES, the series of advantages such as have low toxicity, cheapness, Color is excellent, dye utilization rate is high, solvent load is little, solvent recovery is easy, for the non-aqueous media dyeing of REACTIVE DYES opens up a new way.
Detailed description of the invention
In order to there be understanding clearly to technical characteristic of the present invention, object and beneficial effect, existing following detailed description is carried out to technical scheme of the present invention, but can not be interpreted as to of the present invention can the restriction of practical range.
Embodiment 1
Present embodiments provide a kind of REACTIVE DYES non-aqueous media colouring method, the method comprises the following steps:
2g pure cotton knitting is arranged in soaking at room temperature 10min in the sodium hydrate aqueous solution of 10g/L, a leaching one is rolled, and controlled by liquid carrying rate, 100%, then to dry, bake out temperature is 60 DEG C, and drying time is 10min.
Be arranged in autoclave by pretreated pure cotton knitting, add 0.06g (3%o.w.f) E BR Red 3BS, 15g dimethyl sulfoxide (DMSO), passes into 100g CO
2, the pressure in autoclave is risen to 230bar, and temperature rises to 100 DEG C, now CO
2gas is supercriticality, at 100 DEG C, be incubated 2h.
By the Pressure Drop in autoclave to 50bar, CO
2automatically be separated with the good solvent of REACTIVE DYES, by the CO reclaimed
2store after compression, can be used for dyeing cycle; The dimethyl sulfoxide (DMSO) raffinate of separating out is almost colourless, directly can continue on for dyeing, the dye-uptake nearly 100% of dyestuff.
After being washed by the cloth specimen of taking-up, dyeing cloth specimen is peony, and its K/S=15.3, dyefastness and traditional water bath dye quite.
Embodiment 2
Present embodiments provide a kind of REACTIVE DYES non-aqueous media colouring method, the method comprises the following steps:
2g purified cotton yarns is placed in the sodium hydrate aqueous solution soaking at room temperature 10min of 10g/L, centrifugal dehydration, is controlled by liquid carrying rate, 30%, then to dry, bake out temperature is 60 DEG C, and drying time is 10min.
Be placed in autoclave by pretreated purified cotton yarns, add 0.06g (3%o.w.f) Avitera orange SE, 15g DMA, passes into 60g CO
2, the pressure in autoclave is risen to 230bar, and temperature rises to 100 DEG C, now CO
2gas is supercriticality, at 100 DEG C, be incubated 2h.
By the Pressure Drop in autoclave to 50bar, CO
2automatically be separated with the good solvent of REACTIVE DYES, by the CO reclaimed
2store after compression, can be used for dyeing cycle; The DMA raffinate of separating out is almost colourless, directly can continue on for dyeing, the dye-uptake nearly 100% of dyestuff.
Be orange after the yarn of taking-up being carried out washing, its K/S=20.9, dyefastness and traditional water bath dye quite.
Embodiment 3
Present embodiments provide a kind of REACTIVE DYES non-aqueous media colouring method, the method comprises the following steps:
Be arranged in soaking at room temperature 10min in the sodium carbonate liquor of 20g/L by blended knitted for cotton for 2g/fiber crops (60% cotton+40% fiber crops), a leaching one is rolled, and controlled by liquid carrying rate, 100%, then to dry, bake out temperature is 60 DEG C, drying time 10min.
Cotton/hemp blended knittedly be arranged in autoclave by pretreated, add 0.1g (5%o.w.f) Avitera blueSE, 15g dipropylene glycol methyl ether, passes into 60g CO
2, the pressure in autoclave is risen to 230bar, and temperature rises to 100 DEG C, now CO
2gas is supercriticality, at 100 DEG C, be incubated 2h.
By the Pressure Drop in autoclave to 50bar, CO
2automatically be separated with the good solvent of REACTIVE DYES, by the CO reclaimed
2store after compression, can be used for dyeing cycle; The dipropylene glycol methyl ether raffinate of separating out is almost colourless, directly can continue on for dyeing, dyestuff dye-uptake nearly 100%.
After being washed by the cloth specimen of taking-up, dyeing cloth specimen is in blue, and its K/S=22.9, dyefastness and traditional water bath dye quite.
Embodiment 4
Present embodiments provide a kind of REACTIVE DYES non-aqueous media colouring method, the method comprises the following steps:
Be arranged in soaking at room temperature 10min in the sodium carbonate liquor of 20g/L by blended knitted for 2g cotton/nylon (70% cotton+30% nylon), a leaching one is rolled, and controlled by liquid carrying rate, 100%, then to dry, bake out temperature is 60 DEG C, and drying time is 10min.
Be placed in autoclave by pretreated cotton/nylon blend knitted cloth, add 0.06g (3%o.w.f) AviteraRed SE, 15g dimethyl sulfoxide (DMSO), passes into 70g CO
2, the pressure in autoclave is risen to 230bar, and temperature rises to 100 DEG C, now CO
2gas is supercriticality, at 100 DEG C, be incubated 2h.
By the Pressure Drop in autoclave to 50bar, CO
2automatically be separated with the good solvent of REACTIVE DYES, by the CO reclaimed
2store after compression, can be used for dyeing cycle; The dimethyl sulfoxide (DMSO) raffinate of separating out is almost colourless, directly can continue on for dyeing, dyestuff dye-uptake nearly 100%.
After being washed by the cloth specimen of taking-up, dyeing cloth specimen takes on a red color, and its K/S=18.9, dyefastness and traditional water bath dye quite.
Embodiment 5
Present embodiments provide a kind of REACTIVE DYES non-aqueous media colouring method, the method comprises the following steps:
Cotton for 2g bulk fibre is placed in the sodium carbonate liquor soaking at room temperature 10min of 20g/L, centrifugal dehydration, controlled by liquid carrying rate, 30%, then to dry, bake out temperature is 60 DEG C, and drying time is 10min.
Be placed in autoclave by pretreated cotton bulk fibre, add 0.06g (3%o.w.f) Avitera Red SE, 15g dimethyl sulfoxide (DMSO), passes into 70g CO
2, the pressure in autoclave is risen to 230bar, and temperature rises to 100 DEG C, now CO
2gas is supercriticality, at 100 DEG C, be incubated 2h.
By the Pressure Drop in autoclave to 50bar, CO
2automatically be separated with the good solvent of REACTIVE DYES, by the CO reclaimed
2store after compression, can be used for dyeing cycle; The dimethyl sulfoxide (DMSO) raffinate of separating out is almost colourless, directly can continue on for dyeing, dyestuff dye-uptake nearly 100%.
After being washed by the cotton bulk fibre taken out, dyeing processes is peony, and dyefastness and traditional water bath dye quite.
Claims (10)
1. a non-aqueous media colouring method for REACTIVE DYES, it comprises the following steps:
(1) alkaline solution preliminary treatment: thing to be dyed is carried out in alkaline solution fully swelling after, control liquid carrying rate and also dry;
(2) the non-aqueous media dyeing of REACTIVE DYES: the non-aqueous media dyeing thing to be dyed of above-mentioned oven dry being carried out REACTIVE DYES, obtains dyeing product.
2. method according to claim 1, wherein: described thing to be dyed is carried out fully swelling comprising in alkaline solution:
Thing to be dyed is placed in the alkaline solution that concentration is 1-100g/L, at 10-40 DEG C, soaks 1-30min;
Preferably, the concentration of described alkaline solution is 5-50g/L.
3. method according to claim 1 and 2, wherein: described alkaline solution comprises the combination of one or more in sodium carbonate liquor, sodium bicarbonate solution, sodium hydroxide solution, lithium hydroxide solution, potassium hydroxide solution.
4. method according to claim 1, wherein: described liquid carrying rate controls as 30-200%;
Preferably, the method controlling liquid carrying rate comprises centrifugal dehydration or roll pressure rolling.
5. method according to claim 1, wherein, described step (2) comprising:
Thing to be dyed after step (1) process is placed in reaction vessel, adds the good solvent of REACTIVE DYES and REACTIVE DYES wherein, then pass into CO wherein
2gas, the pressure in adjustment reaction vessel and temperature are to CO
2in supercriticality, isothermal reaction is to the fully upper dye of REACTIVE DYES at such a temperature, obtains dyeing product.
6. method according to claim 5, wherein: the mass ratio of the good solvent of described thing to be dyed and REACTIVE DYES is 1:2-50, is preferably 1:3-10; Described CO
2the mass ratio of the good solvent of gas and REACTIVE DYES is 3-50:1.
7. the method according to claim 5 or 6, wherein: the good solvent of described REACTIVE DYES can lytic activity dyestuff, but not with REACTIVE DYES generation chemical reaction;
Preferably, the good solvent of described REACTIVE DYES is polar solvent;
More preferably, the good solvent of described REACTIVE DYES comprises the combination of one or more in DMF, DMA, dimethyl sulfoxide (DMSO), ionic liquid, alcohol ether solvents.
8. the method according to any one of claim 1-7, wherein: the material of described thing to be dyed comprises cellulose fibre, protein fibre, the combination of one or more had in the synthetic fiber of reactive group; The form of described thing to be dyed comprises fiber, yarn, fabric or ready-made clothes;
Preferably, the reactive group had described in the synthetic fiber of reactive group comprises the combination of one or more in amide groups, amino, hydroxyl.
9. method according to claim 1, wherein: the method is also included in step (2) and terminates rear recovery CO
2the step of the good solvent of gas and REACTIVE DYES.
10. method according to claim 9, wherein, described recovery CO
2the step of the good solvent of gas and REACTIVE DYES comprises:
After dyeing terminates, by the Pressure Drop in autoclave to below 100bar, to the CO discharged
2the good solvent of gas and REACTIVE DYES reclaims.
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| CN105002753A (en) * | 2015-06-29 | 2015-10-28 | 西南大学 | Reactive dye micro-extraction dyeing method |
| CN105064078A (en) * | 2015-08-05 | 2015-11-18 | 广东溢达纺织有限公司 | Reactive dye non-aqueous medium dyeing and soaping method |
| CN105239294A (en) * | 2015-10-20 | 2016-01-13 | 东华大学 | Waterless dyeing device and dyeing method thereof by utilizing activated dye for cotton cone yarns |
| CN105332301A (en) * | 2015-12-11 | 2016-02-17 | 广东溢达纺织有限公司 | Dye fixing method for washing-free reactive dye non-aqueous agent |
| CN105696378A (en) * | 2016-03-25 | 2016-06-22 | 广东溢达纺织有限公司 | Non-aqueous-medium dyeing and washing-free color fixation method for reactive dye |
| CN105862471A (en) * | 2016-05-18 | 2016-08-17 | 派得羽绒家纺南通有限公司 | Waterless dyeing method for textiles |
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| CN105002753B (en) * | 2015-06-29 | 2017-03-08 | 西南大学 | The micro-extraction colouring method of reactive dye |
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| WO2017028306A1 (en) * | 2015-08-18 | 2017-02-23 | 香港纺织及成衣研发中心有限公司 | Cotton fiber dye for supercritical co2 fluid dyeing, and dyeing method thereof |
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| CN105862471A (en) * | 2016-05-18 | 2016-08-17 | 派得羽绒家纺南通有限公司 | Waterless dyeing method for textiles |
| CN107653707A (en) * | 2016-07-26 | 2018-02-02 | 海宁绿宇纺织科技有限公司 | A kind of non-aqueous media color-fixing method suitable for reactive dye |
| CN107090728A (en) * | 2017-06-23 | 2017-08-25 | 东华大学 | A kind of reactive dye pickering emulsion colouring method using methyl phenyl ethers anisole as medium |
| CN107090728B (en) * | 2017-06-23 | 2019-05-03 | 东华大学 | It is a kind of using methyl phenyl ethers anisole as the reactive dye pickering emulsion colouring method of medium |
| CN109355929A (en) * | 2018-10-16 | 2019-02-19 | 苏州大学 | It is a kind of using supercritical carbon dioxide fluid as the anhydrous fine dyeing method of medium |
| CN109355928A (en) * | 2018-10-16 | 2019-02-19 | 苏州大学 | A kind of anhydrous fine dyeing method of fluid-mixing medium |
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| WO2020077702A1 (en) * | 2018-10-16 | 2020-04-23 | 苏州大学 | Water-free fiber dyeing method using supercritical carbon dioxide fluid as medium |
| WO2020077701A1 (en) * | 2018-10-16 | 2020-04-23 | 苏州大学 | Anhydrous fiber dyeing method for cotton |
| JP2021503561A (en) * | 2018-10-16 | 2021-02-12 | 蘇州大学 | Anhydrous fiber dyeing method for cotton |
| CN109355928B (en) * | 2018-10-16 | 2022-01-18 | 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 |
| US11608592B2 (en) | 2018-10-16 | 2023-03-21 | Soochow University | Fiber dyeing method using supercritical carbon dioxide fluid as medium |
| CN110080019A (en) * | 2019-04-30 | 2019-08-02 | 苏州经贸职业技术学院 | A kind of dacron thread zero-emission dyeing |
| CN111926593A (en) * | 2020-08-04 | 2020-11-13 | 大连工业大学 | Double-medium circulating dyeing method with high dye-uptake and color fastness |
| CN111926593B (en) * | 2020-08-04 | 2022-08-19 | 大连工业大学 | Double-medium circulating dyeing method with high dye-uptake and color fastness |
| CN115045127A (en) * | 2022-07-28 | 2022-09-13 | 河南水工智造科技有限公司 | Energy-saving environment-friendly polyamide fiber superfluid dyeing process |
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