CN103788705A - Black reactive dye composition - Google Patents
Black reactive dye composition Download PDFInfo
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- CN103788705A CN103788705A CN201210420381.XA CN201210420381A CN103788705A CN 103788705 A CN103788705 A CN 103788705A CN 201210420381 A CN201210420381 A CN 201210420381A CN 103788705 A CN103788705 A CN 103788705A
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Abstract
The invention discloses a black reactive dye composition which is prepared as follows: step 1, synthesizing C.1.reactive black 5; step two, synthesizing an orange mixture component; step three, directly mixing 150g of the reactive black 5, 45g of the orange mixture and 20 g of anhydrous sodium sulphate with dry mixing equipment to obtain a black dye mixture by full and even mixing, or, by measurement of the liquid dye solid content, taking a liquid dye amounting to the 150g of the reactive black 5 and a liquid dye amounting to the 45g of the reactive orange mixture to fully and evenly mix in liquid mixing equipment, and then obtaining the black dye composition by spray drying; step four, according to the weight ratio of C.1. reactive black 5 to reactive orange mixture of (25-75): (75-25), choosing different ratios to process black dye compositions with different color-light levels; and step five, preparing the mixed product in the step 3 into 100ml of a 10g / L dye liquid, continuously pad dyeing a 10cm * 10m long-strip shaped fabric under the same conditions, and after processing of the pad-dyed fabric, using a color photometer for color measurement in every 0.5m.
Description
Technical field
the present invention relates to a kind of black and active dye composition.
Background technology
Particularly reactive black 5 C.1. of black and active dye, that Present Global application is wider, the kind that output is larger, C.1. the λ max of reactive black 5 is between 590-600mm, and reality is also a navy dyestuff, pitch black degree is inadequate, so reach aterrimus, all adopt both at home and abroad at present take reactive black 5 C.1. as basis, utilize compounded technology to obtain, not only cost is high, and making processes more complicated.
Summary of the invention
The invention provides one
black and active dye composition,its dye uptake is high, solubility property is good, and application performance excellence has not only reached the requirement of pad dyeing stamp, and has overcome the problems such as the head and the tail aberration in dyeing process.
The present invention has adopted following technical scheme:
a kind of black and active dye composition, it comprises the following steps:step 1, C.1. reactive black 5 is synthetic: in beaker, put mixture of ice and water 150g, take 100% para-ester 56.2g, para-ester is put into mixture of ice and water pulled an oar after 1 hour, add 30% hydrochloric acid 24ml, then at the 5-10 ℃ of aqueous solution that adds 100% Sodium Nitrite 13.8g, maintain 5-10 ℃, with reaction solution to the micro-blue colour response of starch potassium iodide paper 2 hours, after eliminating with thionamic acid, add folding hundred H acid 33.1g, control 15-18 ℃ of reaction of temperature 4 hours, with sodium bicarbonate adjusting pH value 5-5.5 reaction 3 hours, add a certain amount of stablizer, can be drying to obtain the black finished product of KN-B by Direct spraying, step 2, mix the synthetic of orange component: in beaker, put into mixture of ice and water, take 100% para-ester 28.1g and 100% sulfonation para-ester 36.1g, pull an oar 2 hours, add 30% hydrochloric acid 15ml, then 5-10 ℃ adds the aqueous solution of 100% Sodium Nitrite 13.8g, maintaining 5-10 ℃ reacts 2 hours the micro-blueness of starch potassium iodide examination with reaction solution, eliminate with thionamic acid, add the J acid 11.96g of folding hundred, and folding hundred between two 10.5g, stir 4 hours, with sodium bicarbonate adjusting pH value, 5.5-6.5 reacts 3 hours to terminal, add quantitative stablizer, can be dried the mixture that gets final product orangely by Direct spraying, step 3, the mixture of the reactive black 5 of 150g and 45g orange and 20g Sodium sulfate anhydrous.min(99) are passed through to the dry direct mixture of blending equipment, fully mix, can arrive the mixture of black dyes, or by the solid content of metering liquid dyestuff, get after being equivalent to stir in liquid blending still containing the liquid dye of the reactive black 5 of 150g and the liquid dye of mixture of reactive orange that are equivalent to 45g and obtain black dye composition by spraying after dry, step 4, by by weight reactive black 5 C.1.: the active orange=(25-75) of mixing: (75-25), select the proportioning of different ratios, can be processed into the black dye composition of the rank of different color light, step 5, is made into the blending product of above-mentioned step 3 the dye liquor 100ml of 10g/l, and the long strip shape of fabric 10cm × 10 m, with condition continuous knot dyeing on cotton fibre.Fabric after pad dyeing after treatment, carries out colour examining every 0.5m with color measurement instrument.
The present invention
step 4black dye composition is solid preparation or liquid preparation, when dye composite is while using solid preparation, in the gross weight of dyestuff pulvis or granule, can comprise the ionogen of 10-30% weight or comprise 5-30% weight the buffer substance with shock absorption; In the time that dye composite exists with liquid preparation form, dyestuff total amount is less than or equal to 40% of aqueous dye solutions weight, and the amount that comprises buffer substance in the aqueous solution is less than or equal to 5% of aqueous solution weight.
The present invention has following beneficial effect: the composition good water solubility of reactive dyestuffs of the present invention, 25 ℃ time, be greater than 200g/l, and dye liquor is even, has solved the problem of head and the tail aberration in dyeing process.Especially the commercialization of liquid preparation is used, and has saved a large amount of energy consumptions, has reduced environmental pollution.
Embodiment
The invention provides
a kind of black and active dye composition, it comprises the following steps:step 1, C.1. reactive black 5 is synthetic: in beaker, put mixture of ice and water 150g, take 100% para-ester 56.2g, para-ester is put into mixture of ice and water pulled an oar after 1 hour, add 30% hydrochloric acid 24ml, then at the 5-10 ℃ of aqueous solution that adds 100% Sodium Nitrite 13.8g, maintain 5-10 ℃, with reaction solution to the micro-blue colour response of starch potassium iodide paper 2 hours, after eliminating with thionamic acid, add folding hundred H acid 33.1g, control 15-18 ℃ of reaction of temperature 4 hours, with sodium bicarbonate adjusting pH value 5-5.5 reaction 3 hours, add a certain amount of stablizer, can be drying to obtain the black finished product of KN-B by Direct spraying, chemical formula is:
Step 2, mix the synthetic of orange component: in beaker, put into mixture of ice and water, take 100% para-ester 28.1g and 100% sulfonation para-ester 36.1g, pull an oar 2 hours, add 30% hydrochloric acid 15ml, then 5-10 ℃ adds the aqueous solution of 100% Sodium Nitrite 13.8g, maintaining 5-10 ℃ reacts 2 hours the micro-blueness of starch potassium iodide examination with reaction solution, eliminate with thionamic acid, add the J acid 11.96g of folding hundred, and folding hundred between two 10.5g, stir 4 hours, with sodium bicarbonate adjusting pH value, 5.5-6.5 reacts 3 hours to terminal, add quantitative stablizer, can be dried the mixture that gets final product orangely by Direct spraying,
Step 3, the mixture of the reactive black 5 of 150g and 45g orange and 20g Sodium sulfate anhydrous.min(99) are passed through to the dry direct mixture of blending equipment, fully mix, can arrive the mixture of black dyes, or by the solid content of metering liquid dyestuff, get after being equivalent to stir in liquid blending still containing the liquid dye of the reactive black 5 of 150g and the liquid dye of mixture of reactive orange that are equivalent to 45g and obtain black dye composition by spraying after dry;
Step 4, by by weight reactive black 5 C.1.: the active orange=(25-75) of mixing: (75-25), select the proportioning of different ratios, can be processed into the black dye composition of the rank of different color light, black dye composition is solid preparation or liquid preparation, when dye composite is while using solid preparation, in the gross weight of dyestuff pulvis or granule, can comprise the ionogen of 10-30% weight or comprise 5-30% weight the buffer substance with shock absorption; In the time that dye composite exists with liquid preparation form, dyestuff total amount is less than or equal to 40% of aqueous dye solutions weight, and the amount that comprises buffer substance in the aqueous solution is less than or equal to 5% of aqueous solution weight;
Step 5, is made into the blending product of above-mentioned step 3 the dye liquor 100ml of 10g/l, and the long strip shape of fabric 10cm × 10 m, with condition continuous knot dyeing on cotton fibre.Fabric after pad dyeing after treatment, carries out colour examining every 0.5m with color measurement instrument, and examination chromatic number is according in table 1
The colour examining data of table 1 DYED FABRICS
Sequence number | △L | △a | △b | △E | Apparent |
1 | -0.01 | 0.004 | -0.21 | 0.3 | 99.99 |
2 | -0.023 | 0.12 | -0.22 | 0.25 | 99.93 |
3 | 0.03 | -0.015 | -0.32 | 0.36 | 100.2 |
4 | 0.18 | 0.12 | -0.126 | 0.29 | 100.52 |
5 | 0.22 | 0.21 | -0.09 | 0.32 | 101.21 |
6 | 0.17 | 0.031 | -0.05 | 0.35 | 100.82 |
7 | 0.07 | -0.06 | -0.12 | 0.28 | 99.95 |
8 | 0.12 | -0.08 | -0.26 | 0.34 | 100.20 |
As can be seen from Table 1, the colour examining data of DYED FABRICS do not have obvious gap, and head and the tail aberration is very little.
Claims (2)
1. a black and active dye composition, it comprises the following steps:
Step 1, C.1. reactive black 5 is synthetic: in beaker, put mixture of ice and water 150g, take 100% para-ester 56.2g, para-ester is put into mixture of ice and water pulled an oar after 1 hour, add 30% hydrochloric acid 24ml, then at the 5-10 ℃ of aqueous solution that adds 100% Sodium Nitrite 13.8g, maintain 5-10 ℃, with reaction solution to the micro-blue colour response of starch potassium iodide paper 2 hours, after eliminating with thionamic acid, add folding hundred H acid 33.1g, control 15-18 ℃ of reaction of temperature 4 hours, with sodium bicarbonate adjusting pH value 5-5.5 reaction 3 hours, add a certain amount of stablizer, can be drying to obtain the black finished product of KN-B by Direct spraying,
Step 2, mix the synthetic of orange component: in beaker, put into mixture of ice and water, take 100% para-ester 28.1g and 100% sulfonation para-ester 36.1g, pull an oar 2 hours, add 30% hydrochloric acid 15ml, then 5-10 ℃ adds the aqueous solution of 100% Sodium Nitrite 13.8g, maintaining 5-10 ℃ reacts 2 hours the micro-blueness of starch potassium iodide examination with reaction solution, eliminate with thionamic acid, add the J acid 11.96g of folding hundred, and folding hundred between two 10.5g, stir 4 hours, with sodium bicarbonate adjusting pH value, 5.5-6.5 reacts 3 hours to terminal, add quantitative stablizer, can be dried the mixture that gets final product orangely by Direct spraying,
Step 3, the mixture of the reactive black 5 of 150g and 45g orange and 20g Sodium sulfate anhydrous.min(99) are passed through to the dry direct mixture of blending equipment, fully mix, can arrive the mixture of black dyes, or by the solid content of metering liquid dyestuff, get after being equivalent to stir in liquid blending still containing the liquid dye of the reactive black 5 of 150g and the liquid dye of mixture of reactive orange that are equivalent to 45g and obtain black dye composition by spraying after dry;
Step 4, by by weight reactive black 5 C.1.: the active orange=(25-75) of mixing: (75-25), select the proportioning of different ratios, can be processed into the black dye composition of the rank of different color light;
Step 5, is made into the blending product of above-mentioned step 3 the dye liquor 100ml of 10g/l, the long strip shape of fabric 10cm × 10 m, and with condition continuous knot dyeing on cotton fibre, the fabric after pad dyeing after treatment, carries out colour examining every 0.5m with color measurement instrument.
2. black and active dye composition according to claim 1, the black dye composition that it is characterized in that described step 4 is solid preparation or liquid preparation, when dye composite is while using solid preparation, in the gross weight of dyestuff pulvis or granule, can comprise the ionogen of 10-30% weight or comprise 5-30% weight the buffer substance with shock absorption; In the time that dye composite exists with liquid preparation form, dyestuff total amount is less than or equal to 40% of aqueous dye solutions weight, and the amount that comprises buffer substance in the aqueous solution is less than or equal to 5% of aqueous solution weight.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104559310A (en) * | 2014-12-19 | 2015-04-29 | 浙江劲光化工有限公司 | Synthetic method of active black dye |
CN106634042A (en) * | 2016-12-08 | 2017-05-10 | 浙江劲光实业股份有限公司 | One-step synthesis method of active black dye |
WO2018203746A1 (en) * | 2017-05-02 | 2018-11-08 | Spgprints B.V. | One-pot synthesis of reactive deep black |
CN112708285A (en) * | 2020-12-29 | 2021-04-27 | 杭州吉华江东化工有限公司 | Production method for improving color matching and efficiency of active black W |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101125966A (en) * | 2007-07-31 | 2008-02-20 | 朱海根 | Composite reactive black dye used for cellulose fibre coloring |
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Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101125966A (en) * | 2007-07-31 | 2008-02-20 | 朱海根 | Composite reactive black dye used for cellulose fibre coloring |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104559310A (en) * | 2014-12-19 | 2015-04-29 | 浙江劲光化工有限公司 | Synthetic method of active black dye |
CN106634042A (en) * | 2016-12-08 | 2017-05-10 | 浙江劲光实业股份有限公司 | One-step synthesis method of active black dye |
WO2018203746A1 (en) * | 2017-05-02 | 2018-11-08 | Spgprints B.V. | One-pot synthesis of reactive deep black |
NL2018826B1 (en) * | 2017-05-02 | 2018-11-09 | Spgprints B V | One-pot synthesis of reactive deep black |
US10669425B2 (en) | 2017-05-02 | 2020-06-02 | Spgprints B.V. | One-pot synthesis of reactive deep black |
JP2020530036A (en) * | 2017-05-02 | 2020-10-15 | エスピージープリンツ・ベー・フェー | Reactive dark black one-pot synthesis |
JP7062014B2 (en) | 2017-05-02 | 2022-05-02 | エスピージープリンツ・ベー・フェー | Reactive dark black one-pot synthesis |
CN112708285A (en) * | 2020-12-29 | 2021-04-27 | 杭州吉华江东化工有限公司 | Production method for improving color matching and efficiency of active black W |
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Application publication date: 20140514 |