CN103554989B - A kind of low temperature modification composite active black dye and application thereof - Google Patents

A kind of low temperature modification composite active black dye and application thereof Download PDF

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CN103554989B
CN103554989B CN201310508741.6A CN201310508741A CN103554989B CN 103554989 B CN103554989 B CN 103554989B CN 201310508741 A CN201310508741 A CN 201310508741A CN 103554989 B CN103554989 B CN 103554989B
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formula
reactive dyestuffs
low temperature
composite active
active black
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CN103554989A (en
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孟胜锋
栾金鑫
秦杰锋
潘克存
康定
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Zhejiang Yide New Material Co., Ltd
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ZHEJIANG YIDE CHEMICAL CO Ltd
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Abstract

The invention belongs to the exhaust dyeing technical field of textiles, be specifically related to a kind of low temperature modification composite active black dye and application thereof, this low temperature modification composite active black dye, by the reactive dyestuffs A shown in formula (1), reactive dyestuffs B shown in formula (2), reactive dyestuffs C shown in formula (3), reactive dyestuffs D shown in formula (4), reactive dyestuffs E shown in formula (5) and auxiliary agent are composited, described reactive dyestuffs A, B, C, the massfraction of D and E is followed successively by: 50-70%, 10-25%, 0-10%, 0-10%, 0-10%, surplus is auxiliary agent, between each reactive dye compound that low temperature composite active black dye of the present invention is chosen, there is splendid compatibleness, look flower and color dot is not easily produced when using low temperature composite active black dye of the present invention to dye, in addition, can low temperature fixation during low temperature composite active black dye of the present invention dyeing, add that technique adopts low alkali and repeatedly adds alkali operation, the percent hydrolysis of dyestuff is reduced greatly, thus the absolute degree of fixation of dyestuff is improved greatly.<!-- 2 -->

Description

A kind of low temperature modification composite active black dye and application thereof
Technical field
The invention belongs to the exhaust dyeing technical field of textiles, relate to a kind of low temperature modification composite active black dye and the application thereof of the fabric dyeing of applicable cellulosic fibre or cellulose.
Background technology
Dyeing is always the industry of highly energy-consuming, high water consumption, high pollution, particularly in recent years, the problem such as the energy, environmental protection more and more causes showing great attention to of country and the whole society, larger pressure is brought to dyeing, in the urgent need to the appearance of reactive monoazo dyestuffs, new auxiliary, novel process, solve or alleviate this many pressure.Current, there is power consumption for the reactive dyestuffs of cellulose dyeing in a large number higher, dyestuff dye uptake is low to be caused producing large amount of sewage, needs to add a large amount of inorganic salt and alkali fixation causes the problems, particularly dark series such as wastewater treatment difficulty, as active black.Active black consumption generally accounts for more than 60% of all colour system dye dosages, and active black ordinary stain depth requirements reaches more than 6%, active black dye consumption so all can be caused large, and waste is also large, effective rate of utilization is low, causes huge social resources waste.
For these problems, many dye manufactures commercial cities are being studied, but be mostly at increase active group, improve dyestuff substantivity to wait to improve dyestuff dye uptake, we are at the new dye structure of exploitation, improve on the basis of dyestuff dye uptake and degree of fixation, according to the Structure and Properties of dyestuff, experimental study is matched dyeing with it, make the utilization ratio of dyestuff reach optimum value, accomplished existing commercially reactive dyestuffs and technique dye less than the degree of depth.By the combination of dyestuff and technique, bring out the best in each other, reach reduction energy consumption, improve dye utilization rate, reduce sewage, the object reduced costs.
Different activities dyestuff has different effects, and in actual production at present, substantially similar to the operation of reactive dyestuffs, and in a lot of actual production, do not pay attention to the operation of different activities dyestuff, a lot of factory still unified a set of technique contaminates nearly all reactive dyestuffs of the same type.The reactive dyestuffs that there be limited evidence currently of people studies different components targetedly need the best staining technique matched with it.This group dye structure of our company, is equipped with the innovative point that the technique be applicable to it is dyestuff development & application technology.
Summary of the invention
The object of the invention is to solve the deficiencies in the prior art, a kind of low temperature modification composite active black dye is provided.
Another object of the present invention is to provide a kind of application of low temperature modification composite active black dye, i.e. its dyeing for dyeing.
The technical scheme that the present invention solves the employing of its technical problem is as follows:
A kind of low temperature modification composite active black dye, be composited by reactive dyestuffs D, the reactive dyestuffs E shown in formula (5) and the auxiliary agent shown in the reactive dyestuffs B shown in the reactive dyestuffs A shown in formula (1), formula (2), the reactive dyestuffs C shown in formula (3), formula (4), the massfraction of described reactive dyestuffs A, B, C, D and E is followed successively by: 50-70%, 10-25%, 0-10%, 0-10%, 0-10%, surplus is auxiliary agent:
In formula (1), R 1, R 2, R 3, R 4respective independence is-SO 3m ,-CH 3,-OCH 3or-H; Wherein M is hydrogen or basic metal;
In formula (2), R 5, R 6, R 7, R 8respective independence is-SO 3m ,-CH 3,-OCH 3or-H; Wherein M is hydrogen or basic metal;
In formula (3), R 9, R 10, R 11, R 12respective independence is-SO 3m ,-CH 3,-OCH 3or-H; Wherein M is hydrogen or basic metal;
In formula (4), R 13, R 14, R 15, R 16respective independence is-SO 3m ,-CH 3,-OCH 3or-H; Wherein M is hydrogen or basic metal;
In formula (5), R 17, R 18, R 19, R 20respective independence is-SO 3m ,-CH 3,-OCH 3or-H; Wherein M is hydrogen or basic metal.
As preferably ,-SO in formula (1) to formula (5) 2cH=CH 2by-SO 2cH 2cH 2oSO 3na adds soda ash degreasing and forms.
A kind of application of low temperature modification composite active black dye, for the dyeing of fibre-bearing fabric, concrete staining procedure is as follows: bath raio 1:3 ~ 30, dyestuff and the auxiliary agent of fabric weight 1 ~ 10% is added under normal temperature, the consumption of auxiliary agent is 80 ~ 100g/L, run 5 ~ 8min, be warming up to 30-50 DEG C by the temperature rise rate of 1-3 DEG C/min, insulation 10 ~ 12min, then adds dyeing alkaline agent, its consumption is 2.0 ~ 7.4g/L, run, 30min, is then incubated 40 ~ 60min, then carry out aftertreatment, postprocessing working procedures be followed successively by just wash, soap, after washing and oven dry.
As preferably, described dyeing auxiliary is the mixture of one or more in Sodium sulfate anhydrous.min(99), Sodium hexametaphosphate 99, condensation compound of methyl naphthalene sulfonic acid and formaldehyde and naphthalene sulfonic acidformaldehyde condensation product.
As preferably, described dyeing alkaline agent is soda ash and caustic soda, soda ash consumption is 1-5g/L, caustic soda divides three times and adds, amount of caustic soda is followed successively by 0.1-0.3g/L, 0.3-0.6g/L, 0.6-1.5g/L, soda ash adds rear operation 10min and adds caustic soda again, runs 10min respectively after first time and second time add caustic soda.
As preferably, in aftertreatment, just washing water temperature is 20-25 DEG C, and first washing time is 5-15min; Soap and adopt common soap flakes, temperature of soaping is 95-100 DEG C, and the time of soaping is 5-15min; After washing temperature is 20-25 DEG C, and the after washing time is 5-15min; Bake out temperature is 60-80 DEG C, and drying time is 30-60min.
Beneficial effect of the present invention is as follows:
(1) between each reactive dye compound that low temperature composite active black dye of the present invention is chosen, there is splendid compatibleness, when using low temperature composite active black dye of the present invention to dye, not easily produce look flower and color dot;
(2) can low temperature fixation during low temperature composite active black dye of the present invention dyeing, add that technique adopts low alkali and repeatedly adds alkali operation, the percent hydrolysis of dyestuff is reduced greatly, thus the absolute degree of fixation of dyestuff is improved greatly;
(3) use the dye level of low temperature composite active black dye of the present invention than same structure and not do the active black of skimming treatment and conventional dyeing process high by more than 30%, thus make the usage quantity of dyestuff save more than 30%, COD and saline and alkalinely also greatly to reduce in the waste water of printing and dyeing mill, low temperature dyeing can also make printing and dyeing mill save the energy consumption of more than 20% than traditional technology.
Four, specific implementation method
Below by specific embodiment, explanation is further explained to technology of the present invention.
A kind of low temperature modification composite active black dye of the present invention, as its component formula (1) shown in reactive dyestuffs A, the reactive dyestuffs B shown in formula (2), the reactive dyestuffs C shown in formula (3), the reactive dyestuffs E shown in the reactive dyestuffs D shown in formula (4) and formula (5) be all conventional dye composition, there is document to record, commercially can to obtain.
Embodiment 1
A kind of low temperature modification composite active black dye, be composited by reactive dyestuffs D, the reactive dyestuffs E shown in formula (5) and the auxiliary agent shown in the reactive dyestuffs B shown in the reactive dyestuffs A shown in formula (1), formula (2), the reactive dyestuffs C shown in formula (3), formula (4), in every 100g low temperature modification composite active black dye, the content of reactive dyestuffs A, B, C, D, E and auxiliary agent is in table 1.
To-SO in formula (5) in formula (1) 2cH=CH 2by-SO 2cH 2cH 2oSO 3na adds soda ash degreasing and forms, and substituent composition is in table 2.
In compound active black dye composition of the present invention, the fitting method of each reactive dyestuffs is not particularly limited, and can adopt: manufacture each reactive dyestuffs respectively, carries out the method coordinated afterwards; The reaction solution containing each reactive dyestuffs generated when manufacturing is mixed, carries out drying afterwards and obtain the method for composition; And each reactive dyestuffs are dissolved in dye bath, in dye bath, obtain the composing method etc. identical with each composition.Now, in composite active black dye, the blending ratio of each dye component suitably can coordinate according to required tone, in addition, according to demand, also can contain known additive in composition of the present invention, such as, and concentration regulator, dispersion agent, reductive agent etc.
Composite reactive dye composition of the present invention is for cellulosic fibre and the fiber useful (as: cotton, fiber crops, artificial silk, wool) containing cellulosic fibre.
A kind of application of low temperature modification composite active black dye, for contaminating textile black, concrete staining procedure is as follows: bath raio 1:3, dyestuff and the Sodium sulfate anhydrous.min(99) of fabric weight 1% is added under normal temperature, the consumption of Sodium sulfate anhydrous.min(99) is 80g/L, run 5min, 30 DEG C are warming up to by the temperature rise rate of 1 DEG C/min, insulation 10min, then dyeing alkaline agent is added, described dyeing alkaline agent is soda ash and caustic soda, soda ash consumption is 1g/L, 10min is run after adding soda ash, then divide three times and add caustic soda, three times amount of caustic soda is followed successively by 0.1g/L, 0.6g/L, 0.6g/L, 10min is run respectively after first time and second time add caustic soda, last caustic soda adds rear insulation 40min, then aftertreatment is carried out, in aftertreatment, just washing water temperature is 20 DEG C, first washing time is 15min, soap and adopt common soap flakes, temperature of soaping is 95 DEG C, and the time of soaping is 15min, after washing temperature is 25 DEG C, and the after washing time is 5min, bake out temperature is 80 DEG C, and drying time is 30min.
Embodiment 2
A kind of low temperature modification composite active black dye, be composited by reactive dyestuffs D, the reactive dyestuffs E shown in formula (5) and the auxiliary agent shown in the reactive dyestuffs B shown in the reactive dyestuffs A shown in formula (1), formula (2), the reactive dyestuffs C shown in formula (3), formula (4), in every 100g low temperature modification composite active black dye, the content of reactive dyestuffs A, B, C, D, E and auxiliary agent is in table 1, to-SO in formula (5) in formula (1) 2cH=CH 2by-SO 2cH 2cH 2oSO 3na adds soda ash degreasing and forms, and substituent composition is in table 2.
A kind of application of low temperature modification composite active black dye, for contaminating textile black, concrete staining procedure is as follows: bath raio 1:30, dyestuff and the Sodium hexametaphosphate 99 of fabric weight 10% is added under normal temperature, the consumption of Sodium hexametaphosphate 99 is 100g/L, run 8min, 50 DEG C are warming up to by the temperature rise rate of 3 DEG C/min, insulation 12min, then dyeing alkaline agent is added, described dyeing alkaline agent is soda ash and caustic soda, soda ash consumption is 5g/L, 10min is run after adding soda ash, then divide three times and add caustic soda, three times amount of caustic soda is followed successively by 0.3g/L, 0.3g/L, 1.5g/L, 10min is run respectively after first time and second time add caustic soda, last caustic soda adds rear insulation 60min, then aftertreatment is carried out, in aftertreatment, just washing water temperature is 25 DEG C, first washing time is 5min, soap and adopt common soap flakes, temperature of soaping is 100 DEG C, and the time of soaping is 5min, after washing temperature is 20 DEG C, and the after washing time is 15min, bake out temperature is 60 DEG C, and drying time is 60min.
Embodiment 3 ~ 5
The composition of the low temperature modification composite active black dye of embodiment 3 to 5 in table 1, in formula (1) to substituent composition in formula (5) in table 2.
Table 1: each component ratio of low temperature modification composite active black dye of embodiment 1 ~ 5
Table 2: the substituent composition in embodiment 1 ~ 5
Embodiment 1 Embodiment 2 Embodiment 3 Embodiment 4 Embodiment 5
R 1 -SO 3M -CH 3 -OCH 3 -H -OCH 3
R 2 -CH 3 -OCH 3 -H -CH 3 -H
R 3 -OCH 3 -H -CH 3 -SO 3M -SO 3M
R 4 -H -SO 3M -SO 3M -OCH 3 -CH 3
R 5 -SO 3M -CH 3 -OCH 3 -H -OCH 3
R 6 -CH 3 -OCH 3 -H -CH 3 -H
R 7 -OCH 3 -H -CH 3 -SO 3M -SO 3M
R 8 -H -SO 3M -SO 3M -OCH 3 -CH 3
R 9 -SO 3M -OCH 3 -OCH 3 -H -OCH 3
R 10 -CH 3 -H -H -CH 3 -H
R 11 -OCH 3 -SO 3M -CH 3 -SO 3M -SO 3M
R 12 -H -CH 3 -SO 3M -OCH 3 -CH 3
R 13 -SO 3M -OCH 3 -OCH 3 -H -OCH 3 7 -->
R 14 -CH 3 -H -H -CH 3 -H
R 15 -OCH 3 -SO 3M -CH 3 -SO 3M -SO 3M
R 16 -H -CH 3 -SO 3M -OCH 3 -CH 3
R 17 -SO 3M -OCH 3 -H -H -OCH 3
R 18 -CH 3 -H -CH 3 -CH 3 -H
R 19 -OCH 3 -SO 3M -OCH 3 -SO 3M -SO 3M
R 20 -H -CH 3 -SO 3M -OCH 3 -CH 3
M H Na K Na K
The low temperature modification composite active black dye of embodiment 1-5 carries out Performance Detection for the sample cloth obtained after dyeing, observe sample cloth coloured light, adopt GB/T3921, GB/T3920, GB/T5718 tests its washing fastness, fastness to perspiration and fastness to rubbing etc. respectively, and concrete test result is in table 3.
Table 3 sample cloth the performance test results
Shown by table 3, low temperature modification composite active black dye of the present invention is resistance to for the sample cloth that obtains after dyeing
The grade of washing fastness, fastness to perspiration and fastness to rubbing is all excellent.

Claims (1)

1. a low temperature modification composite active black dye, it is characterized in that, by the reactive dyestuffs A shown in formula (1), reactive dyestuffs B shown in formula (2), reactive dyestuffs C shown in formula (3), reactive dyestuffs D shown in formula (4), reactive dyestuffs E shown in formula (5) and auxiliary agent are composited, the massfraction of described reactive dyestuffs A is 50-65%, the massfraction of reactive dyestuffs B is 10-25%, the massfraction of reactive dyestuffs C is greater than 0 and is less than or equal to 10%, the massfraction of reactive dyestuffs D is 5-10%, the massfraction of reactive dyestuffs E is greater than 0 and is less than or equal to 10%, surplus is auxiliary agent:
In formula (1), R 1, R 2, R 3, R 4respective independence is-SO 3m ,-CH 3,-OCH 3or-H; Wherein M is hydrogen or basic metal;
In formula (2), R 5, R 6, R 7, R 8respective independence is-SO 3m ,-CH 3,-OCH 3or-H; Wherein M is hydrogen or basic metal;
In formula (3), R 9, R 10, R 11, R 12respective independence is-SO 3m ,-CH 3,-OCH 3or-H; Wherein M is hydrogen or basic metal;
In formula (4), R 13, R 14, R 15, R 16respective independence is-SO 3m ,-CH 3,-OCH 3or-H; Wherein M is hydrogen or basic metal;
In formula (5), R 17, R 18, R 19, R 20respective independence is-SO 3m ,-CH 3,-OCH 3or-H, wherein M is hydrogen or basic metal ,-SO in formula (1) to formula (5) 2cH=CH 2by-SO 2cH 2cH 2oSO 3na adds soda ash degreasing and forms, this low temperature composite active black dye is used for the dyeing of fibre-bearing fabric, concrete staining procedure is as follows: bath raio 1:3 ~ 30, dyestuff and the auxiliary agent of fabric weight 1 ~ 10% is added under normal temperature, the consumption of auxiliary agent is 80 ~ 100g/L, run 5 ~ 8min, 30-50 DEG C is warming up to by the temperature rise rate of 1-3 DEG C/min, insulation 10 ~ 12min, then dyeing alkaline agent is added, its consumption is 2.0 ~ 7.4g/L, run 30min, then be incubated 40 ~ 60min, then aftertreatment is carried out, postprocessing working procedures is followed successively by just washing, soap, after washing and oven dry, described dyeing auxiliary is the mixture of one or more in Sodium sulfate anhydrous.min(99), Sodium hexametaphosphate 99, condensation compound of methyl naphthalene sulfonic acid and formaldehyde and naphthalene sulfonic acidformaldehyde condensation product, described dyeing alkaline agent is soda ash and caustic soda, soda ash consumption is 1-5g/L, and caustic soda divides three times and adds, and amount of caustic soda is followed successively by 0.1-0.3g/L, 0.3-0.6g/L, 0.6-1.5g/L, soda ash adds rear operation 10min and adds caustic soda again, runs 10min respectively after first time and second time add caustic soda, in aftertreatment, just washing water temperature is 20-25 DEG C, and first washing time is 5-15min, soap and adopt common soap flakes, temperature of soaping is 95-100 DEG C, and the time of soaping is 5-15min, after washing temperature is 20-25 DEG C, and the after washing time is 5-15min, bake out temperature is 60-80 DEG C, and drying time is 30-60min.
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CN104073024B (en) * 2014-07-10 2016-07-06 浙江瑞华化工有限公司 A kind of Black reactive dye composition and its purposes
CN104404797B (en) * 2014-11-17 2016-08-24 浙江恒生印染有限公司 A kind of reactive dye low-alkali dyeing method of black regenerated celulose fibre cheese
CN104530755B (en) * 2014-12-19 2017-02-08 浙江亿得化工有限公司 Composite active black dye
CN105385191B (en) * 2015-12-24 2017-08-18 上海雅运纺织化工股份有限公司 Water-soluble dye composition and its tint applications
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CN108530946A (en) * 2017-03-01 2018-09-14 湖北丽源科技股份有限公司 A kind of black reactive dye mixture and its application
CN108102423B (en) * 2017-12-18 2020-06-26 浙江瑞华化工有限公司 Black reactive dye composition and preparation method and application thereof
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CN1730566A (en) * 2005-08-30 2006-02-08 大连理工大学 Alkali resistant black active dye suitable for batch cold process
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