CN104594078B - The nonaqueous solvents composition with temperature control separating property for reactive dye - Google Patents

The nonaqueous solvents composition with temperature control separating property for reactive dye Download PDF

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CN104594078B
CN104594078B CN201510053260.XA CN201510053260A CN104594078B CN 104594078 B CN104594078 B CN 104594078B CN 201510053260 A CN201510053260 A CN 201510053260A CN 104594078 B CN104594078 B CN 104594078B
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reactive dye
solvent
fiber
dyeing
reactive
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CN104594078A (en
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张玉高
邓勇
邱孝群
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Guangdong Esquel Textiles Co Ltd
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Guangdong Esquel Textiles Co Ltd
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Abstract

The invention provides a kind of nonaqueous solvents composition with temperature control separating property for reactive dye.Said composition includes:The good solvent of reactive dye and the poor solvent of reactive dye, the volume ratio of the two are 1:3‑20;Wherein, the good solvent of the reactive dye is that can dissolve reactive dye but the nonaqueous solvents not chemically reacted with reactive dye;The poor solvent of the reactive dye is that can not dissolve reactive dye and the nonaqueous solvents not chemically reacted with reactive dye.The advantages of dicyandiamide solution, is:After one dyeing cycle terminates, only need by the temperature for reducing solvent can reach solvent separate purpose, the spontaneous separation after cooling of two kinds of solvents, it can be recycled, without separating the mixture of solvent using distillation process during consumption energy consumption, greatly save and recycle the time, saved energy consumption, significantly reduced dyeing cost.

Description

The nonaqueous solvents composition with temperature control separating property for reactive dye
Technical field
The present invention relates to a kind of nonaqueous solvents group with temperature control separating property for reactive dye solvent dyeing Compound, belong to textile dyeing and finishing technical field.
Background technology
The dyeing of reactive fibre at present uses reactive dye mostly, because active group is in aqueous medium in dyeing course Hydrolysis, do not only result in the waste of a large amount of reactive dye, and need in dyeing course to consume substantial amounts of water and discharge is big Reluctant high chroma sewage is measured, this is also all the time existing bottleneck for being difficult to overcome of reactive dye.
In order to be avoided that the hydrolysis of reactive dye, the utilization rate of reactive dye is improved, scientists are very early Through paying attention to and have studied dyeing of the reactive dye in non-aqueous media.The advantage dyed using non-aqueous media is that reactive dye exist It will not be hydrolyzed in dyeing course, be expected to improve the extent of reaction of reactive dye and fiber.But meanwhile contaminated using non-aqueous media Color also be there are problems that more always, and main dissolubility including reactive dye in non-aqueous media, fiber are in non-aqueous media Solubility in non-aqueous media of Swelling Capacity, fixation alkaline agent and the level-dyeing property of dyeing, through-dyeing etc..Although activity dye Material is dyed there is many difficult points in non-aqueous media, but is gradually risen at this stage with water cost, and people are more next to environmental protection More pay attention to, the dyeing of reactive dye non-aqueous media is also increasingly attracted attention with its good application prospect.
Therefore it provides a kind of non-aqueous solvent dyeing method of reactive dye turns into this area technical problem urgently to be resolved hurrily.
The content of the invention
In order to solve the above technical problems, it is an object of the invention to provide a kind of having for reactive dye solvent dyeing The nonaqueous solvents composition of temperature control separating property, reactive dyeing is carried out using the nonaqueous solvents composition, had molten The advantages of agent separation is fast, energy consumption is low.
To reach above-mentioned purpose, there is the non-of temperature control separating property for reactive dye the invention provides a kind of Water solvent combinations thing, it includes:
The good solvent of reactive dye and the poor solvent of reactive dye, the volume ratio of the two are 1:3-20;
Wherein, the good solvent of the reactive dye can dissolve reactive dye but not chemically reacted with reactive dye Nonaqueous solvents;The poor solvent of the reactive dye can not dissolve reactive dye and not chemically reacted with reactive dye Nonaqueous solvents.
In above-mentioned nonaqueous solvents composition, it is preferable that the good solvent of the reactive dye is polar solvent.
In above-mentioned nonaqueous solvents composition, it is preferable that the good solvent of the reactive dye includes N, N- dimethyl formyls One or more of combinations in amine, DMAC N,N' dimethyl acetamide, dimethyl sulfoxide (DMSO), ionic liquid, alcohol ether solvents.
In above-mentioned nonaqueous solvents composition, it is preferable that the poor solvent of the reactive dye includes alkane, chloride alkane One or more of combinations in hydrocarbon, alkene, aromatic hydrocarbons, ketones solvent, silanes solvent, esters solvent and ether solvent;It is more excellent Selection of land, the poor solvent of the reactive dye include C6-C8N-alkane, C6-C8Isoparaffin, perchloroethylene and decamethyl ring One or more of combinations in five siloxanes.
In above-mentioned nonaqueous solvents composition, it is preferable that the good solvent of the reactive dye and the reactive dye are not Good solvent can be miscible at a temperature of more than 40 DEG C, can be layered at a temperature of less than 40 DEG C.
Present invention also offers a kind of reactive dye non-aqueous solvent dyeing method, and it is used for reactive dye using above-mentioned What the nonaqueous solvents composition with temperature control separating property was carried out, this method comprises the following steps:
A, fiber (or yarn, fabric or ready-made clothes made of fiber) is placed in the aqueous solution of alkaline matter and is swelling to band Liquid rate is 30%-200%, drying;
B, by the fiber (or yarn, fabric or ready-made clothes made of fiber) after drying and reactive dye, reactive dye Good solvent mixing, add the poor solvent of reactive dye, be warming up to dyeing temperature and dyed, be incubated 1-2h, take out fiber (or yarn, fabric or ready-made clothes made of fiber), washing, complete dyeing;
C, by after dyeing solvent separate, be cooled to less than 40 DEG C (preferably room temperatures), make its layering, respectively take out upper strata with The solvent of lower floor, is recycled;
The poor solvent of the reactive dye is added or added in temperature-rise period before heating;
In the above-mentioned methods, it can be made of staple in bulk or fiber to add in the aqueous solution of alkaline matter Yarn, fabric or ready-made clothes.
In the above-mentioned methods, it is preferable that the fiber of use includes cellulose fibre, protein fibre and has reactive group Synthetic fibers in one or more of combinations;
It is highly preferred that the reactive group used includes amino, hydroxyl, sulfydryl;
It is highly preferred that the cellulose fibre used includes one or more of groups in cotton fiber, fiber crops and viscose rayon etc. Close, the protein fibre of use includes wool and/or silk etc., and the synthetic fibers with reactive group of use include nylon Deng.
In the above-mentioned methods, it is preferable that the volume of the good solvent of reactive dye and yarn, face made of fiber or fiber The ratio of the quality of material or ready-made clothes is 2-50:1, more preferably 3-10:1, wherein, the volume unit of good solvent is mL, fiber (or Yarn, fabric or ready-made clothes made of fiber) mass unit be g.
In the above-mentioned methods, it is preferable that used alkaline matter includes sodium carbonate, sodium acid carbonate, sodium hydroxide, hydrogen-oxygen Change one or more of combinations in lithium and potassium hydroxide.
In the above-mentioned methods, it is preferable that the concentration of the aqueous solution of alkaline matter is 1g/L-100g/L, more preferably 5g/L- 50g/L。
Nonaqueous solvents composition provided by the invention is a kind of non-aqueous solvent dyeing of new reactive dye solvent dyeing System, its used solvent are unmixing at room temperature, are miscible under dyeing temperature.The advantages of dicyandiamide solution, exists In:After one dyeing cycle terminates, it is only necessary to which the temperature by reducing solvent can reach the purpose of solvent separation, two kinds of solvents Spontaneous separation, can be recycled after cooling, without separating the mixture of solvent using distillation process during consumption energy consumption, greatly The recycling time has been saved greatly, energy consumption has been saved, has significantly reduced dyeing cost.
Embodiment
In order to which technical characteristic, purpose and the beneficial effect of the present invention is more clearly understood, now to the skill of the present invention Art scheme carry out it is described further below, but it is not intended that to the present invention can practical range restriction.
Embodiment 1
The present embodiment provides a kind of nonaqueous solvents composition with temperature control separating property for reactive dye, its Including dimethyl sulfoxide (DMSO) and tetrachloro-ethylene, wherein, the volume ratio of the two is 15:60.
The present embodiment additionally provides a kind of colouring method of reactive dye, and it comprises the following steps:
Pure cotton knitting cloth is mixed with the aqueous sodium carbonate that concentration is 20g/L and is swelled, is by liquid carrying rate control 100%, drying;
2g is put into dyeing cup by pretreated pure cotton knitting cloth, adds 0.06g (3%o.m.f) Avitera RedSE and 15mL dimethyl sulfoxide (DMSO), 60 DEG C enter dye, and regulation heating rate is that 1 DEG C/min is warming up to 90 DEG C, in temperature-rise period Add 60mL tetrachloro-ethylenes altogether in three batches;
1h is incubated at 90 DEG C, cloth specimen is wrung out into solvent, room temperature washing, completes dyeing.
Solvent is poured out, is cooled to 30 DEG C, takes out upper strata dimethyl sulfoxide (DMSO) and lower floor's tetrachloro-ethylene respectively, carries out next follow Ring dyes;Dyeing cycle 6 times altogether, the degree of fixation of resulting dyeing looped fabric are as shown in table 1.
Table 1
Cycle-index Degree of fixation %
1 97.1
2 97.6
3 98.1
4 96.0
5 96.3
6 95.6
Embodiment 2
The present embodiment provides a kind of nonaqueous solvents composition with temperature control separating property for reactive dye, its Including DMA and n-hexane, wherein, the volume ratio of the two is 15:75.
The present embodiment additionally provides a kind of colouring method of reactive dye, and it comprises the following steps:
Pure cotton knitting cloth is mixed with the aqueous sodium carbonate that concentration is 20g/L and is swelled, is by liquid carrying rate control 100%, drying;
2g is put into dyeing cup by pretreated pure cotton knitting cloth, adds 0.06g (3%o.m.f) Avitera Orange SE and 15mL DMA, 60 DEG C enter dye, and regulation heating rate is that 1 DEG C/min is warming up to 90 DEG C, Add 75mL n-hexanes in temperature-rise period altogether in three batches;
1h is incubated at 90 DEG C, cloth specimen is wrung out into solvent, room temperature washing, completes dyeing.
Solvent is poured out, is cooled to 30 DEG C, upper strata n-hexane and lower floor's DMA is taken out respectively, carries out down One dyeing cycle;Dyeing cycle 6 times altogether, the degree of fixation of resulting dyeing looped fabric are as shown in table 2.
Table 2
Cycle-index Degree of fixation %
1 98.1
2 98.6
3 97.8
4 97.3
5 96.9
6 97.0
Embodiment 3
The present embodiment provides a kind of nonaqueous solvents composition with temperature control separating property for reactive dye, its Including DMF and decamethylcyclopentaandoxane, wherein, the volume ratio of the two is 15:75.
The present embodiment additionally provides a kind of colouring method of reactive dye, and it comprises the following steps:
Pure cotton knitting cloth is mixed with the sodium hydrate aqueous solution that concentration is 10g/L and is swelled, is by liquid carrying rate control 100%, drying;
2g is put into dyeing cup by pretreated pure cotton knitting cloth, adds 0.06g (3%o.m.f) Novacron Super Black G and 15mL DMF, 60 DEG C enter dye, and regulation heating rate is that 1 DEG C/min is warming up to 95 DEG C, add 75mL n-hexanes in temperature-rise period altogether in three batches;
1h is incubated at 95 DEG C, cloth specimen is wrung out into solvent, washing, completes dyeing.
Solvent is poured out, is cooled to 30 DEG C, takes out upper strata DMF and the silicon of lower floor's decamethyl ring five respectively Oxygen alkane, carry out subsequent cycle dyeing;Dyeing cycle 6 times altogether, the degree of fixation of resulting dyeing looped fabric are as shown in table 3.
Table 3
Cycle-index Degree of fixation %
1 94.6
2 95.0
3 94.1
4 93.6
5 93.1
6 93.7
Embodiment 4
The present embodiment provides a kind of nonaqueous solvents composition with temperature control separating property for reactive dye, its Including DMA and isohexane, wherein, the volume ratio of the two is 15:75.
The present embodiment additionally provides a kind of colouring method of reactive dye, and it comprises the following steps:
Cotton/fiber crops (fiber crops of 60% cotton+40%) blended knitted cloth is mixed into progress with the sodium hydrate aqueous solution that concentration is 10g/L Swelling, it is 100% by liquid carrying rate control;
2g is put into dyeing cup by pretreated blended knitted cloth, adds 0.06g (3%o.m.f) Avitera Blue SE and 15mL DMA, 60 DEG C enter dye, and regulation heating rate is that 1 DEG C/min is warming up to 90 DEG C, is risen Add 75mL isohexanes during temperature altogether in three batches;
1h is incubated at 90 DEG C, cloth specimen is wrung out into solvent, room temperature washing, completes dyeing.
Solvent is poured out, is cooled to 30 DEG C, upper strata DMA and lower floor's isohexane is taken out respectively, carries out down One dyeing cycle;Dyeing cycle 6 times altogether, the degree of fixation of resulting dyeing looped fabric are as shown in table 4.
Table 4
Cycle-index Degree of fixation %
1 97.6
2 97.3
3 97.9
4 96.8
5 96.1
6 96.4
Embodiment 5
The present embodiment provides a kind of nonaqueous solvents composition with temperature control separating property for reactive dye, its Including DMA and isoheptane, wherein, the volume ratio of the two is 15:75.
The present embodiment additionally provides a kind of colouring method of reactive dye, and it comprises the following steps:
Cotton/nylon (nylon of 70% cotton+30%) blended knitted cloth is mixed with the sodium bicarbonate aqueous solution that concentration is 40g/L It is swelled, is 100% by liquid carrying rate control;
2g is put into dyeing cup by pretreated blended knitted cloth, adds 0.06g (3%o.m.f) Avitera Blue SE, 15mL DMA and 75mL isoheptane, in 60 DEG C enter dye, regulation heating rate be 1 DEG C/ Min is warming up to 90 DEG C;
1h is incubated at 90 DEG C, cloth specimen is wrung out into solvent, room temperature washing, completes dyeing.
Solvent is poured out, is cooled to 30 DEG C, upper strata DMA and lower floor's isoheptane is taken out respectively, carries out down One dyeing cycle;Dyeing cycle 6 times altogether, the degree of fixation of resulting dyeing looped fabric are as shown in table 5.
Table 5
Cycle-index Degree of fixation %
1 96.6
2 96.3
3 96.9
4 95.8
5 95.1
6 94.4
Embodiment 6
The present embodiment provides a kind of nonaqueous solvents composition with temperature control separating property for reactive dye, its Including dimethyl sulfoxide (DMSO) and tetrachloro-ethylene, wherein, the volume ratio of the two is 15:60.
The present embodiment additionally provides a kind of colouring method of reactive dye, and it comprises the following steps:
Purified cotton yarns are mixed with the aqueous sodium carbonate that concentration is 20g/L and are swelled, are by liquid carrying rate control 100%, drying.
2g is put into dyeing cup by pretreated purified cotton yarns, adds 0.06g (3%o.m.f) Avitera Red SE and 15mL dimethyl sulfoxide (DMSO), 60 DEG C enter dye, and regulation heating rate is that 1 DEG C/min is warming up to 90 DEG C, is divided in temperature-rise period Three batches add 60mL tetrachloro-ethylenes altogether;
1h is incubated at 90 DEG C, yarn is wrung out into solvent, room temperature washing, completes dyeing.
Solvent is poured out, is cooled to 30 DEG C, takes out upper strata dimethyl sulfoxide (DMSO) and lower floor's tetrachloro-ethylene respectively, carries out next follow Ring dyes;Dyeing cycle 6 times altogether, the degree of fixation of resulting dyed yarn is as shown in table 6.
Table 6
Cycle-index Degree of fixation %
1 96.8
2 96.6
3 97.1
4 95.8
5 94.9
6 95.1
Embodiment 7
The present embodiment provides a kind of nonaqueous solvents composition with temperature control separating property for reactive dye, its Including dimethyl sulfoxide (DMSO) and tetrachloro-ethylene, wherein, the volume ratio of the two is 15:60.
The present embodiment additionally provides a kind of colouring method of reactive dye, and it comprises the following steps:
Pure cotton staple in bulk is mixed with the aqueous sodium carbonate that concentration is 20g/L and is swelled, centrifugal dehydration to liquid carrying rate For 30%, drying.
2g is put into dyeing cup by pretreated pure cotton staple in bulk, adds 0.06g (3%o.m.f) Avitera Deep Blue SE, 15mL dipropylene glycol methyl ether and 60mL tetrachloro-ethylenes, 60 DEG C enter dye, regulation heating rate be 1 DEG C/ Min is warming up to 90 DEG C;
1h is incubated at 90 DEG C, staple in bulk is taken out, solvent is pressed dry, washing, completes dyeing.
Solvent is poured out, is cooled to 30 DEG C, takes out upper strata dimethyl sulfoxide (DMSO) and lower floor's tetrachloro-ethylene respectively, carries out next follow Ring dyes;Dyeing cycle 6 times altogether, the degree of fixation of resulting dyed yarn is as shown in table 7.
Table 7
Cycle-index Degree of fixation %
1 96.3
2 95.9
3 96.4
4 94.8
5 94.9
6 95.4
As can be seen from the above embodiments, the dye of reactive dye is carried out using nonaqueous solvents composition provided by the invention Color, the recovery of solvent and recycles very convenient, and energy consumption is low, and the cycle is short, and circulation carries out dyeing resulting finished product still With very high degree of fixation.

Claims (10)

1. a kind of nonaqueous solvents composition with temperature control separating property for reactive dye, it includes:
The good solvent of reactive dye and the poor solvent of reactive dye, the volume ratio of the two are 1:3-20;
Wherein, the good solvent of the reactive dye is that can dissolve reactive dye but not chemically reacted with reactive dye non-aqueous Solvent;The poor solvent of the reactive dye is that can not dissolve reactive dye and not chemically reacted with reactive dye non-aqueous Solvent;
The poor solvent of the good solvent of the reactive dye and the reactive dye can at a temperature of more than 40 DEG C miscible, energy It is enough to be layered at a temperature of less than 40 DEG C, also, the good solvent of the reactive dye includes DMF, N, N- bis- One or more of combinations in methylacetamide, dimethyl sulfoxide (DMSO), ionic liquid and alcohol ether solvents;The reactive dye are not Good solvent includes C6-C8N-alkane, C6-C8One or more in isoparaffin, perchloroethylene and decamethylcyclopentaandoxane Combination.
2. a kind of reactive dye non-aqueous solvent dyeing method, it is to be used for having for reactive dye using described in claim 1 What the nonaqueous solvents composition of temperature control separating property was carried out, this method comprises the following steps:
Yarn, fabric or ready-made clothes made of fiber or fiber are placed in and is swelling to liquid carrying rate in the aqueous solution of alkaline matter and is 30%-200%, drying;
By yarn, fabric or ready-made clothes made of the fiber or fiber after drying and reactive dye, the good solvent of reactive dye Mixing, adds the poor solvent of reactive dye, is warming up under dyeing temperature and is incubated, take out yarn made of fiber or fiber, Fabric or ready-made clothes, washing, complete dyeing;
Solvent after dyeing is separated, cooling, makes its layering, the solvent of the upper and lower is taken out respectively, recycles;
The poor solvent of the reactive dye is added or added in temperature-rise period before heating.
3. non-aqueous solvent dyeing method according to claim 2, wherein, the fiber includes cellulose fibre, protein Fiber and with reactive group synthetic fibers in one or more of combinations.
4. non-aqueous solvent dyeing method according to claim 3, wherein, the reactive group includes amino, hydroxyl, mercapto Base.
5. the non-aqueous solvent dyeing method according to claim 3 or 4, wherein, the cellulose fibre includes cotton fiber, fiber crops With one or more of combinations in viscose rayon, the protein fibre includes wool and/or silk, described to have reactive group The synthetic fibers of group include nylon.
6. non-aqueous solvent dyeing method according to claim 2, wherein, the volume of the good solvent of the reactive dye and institute The ratio for stating the quality of yarn, fabric or ready-made clothes made of fiber or fiber is 2-50:1, wherein, the volume unit of good solvent is The mass unit of yarn, fabric or ready-made clothes made of mL, fiber or fiber is g.
7. non-aqueous solvent dyeing method according to claim 6, wherein, the volume of the good solvent of the reactive dye and institute The ratio for stating the quality of yarn, fabric or ready-made clothes made of fiber or fiber is 3-10:1.
8. non-aqueous solvent dyeing method according to claim 2, wherein, the alkaline matter includes sodium carbonate, bicarbonate One or more of combinations in sodium, sodium hydroxide, lithium hydroxide and potassium hydroxide.
9. the non-aqueous solvent dyeing method according to claim 2 or 8, wherein, the concentration of the aqueous solution of the alkaline matter For 1g/L-100g/L.
10. non-aqueous solvent dyeing method according to claim 9, wherein, the concentration of the aqueous solution of the alkaline matter is 5g/L-50g/L。
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