CN104927396A - Compound active dark-red dye as well as preparation method and application thereof - Google Patents
Compound active dark-red dye as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a compound active dark-red dye as well as a preparation method and application thereof. The dye comprises the following ingredients in parts by weight: 30-80 parts of a compound shown in the formula (1), 10-30 parts of a compound shown in the formula (2) and 10-40 parts of a compound shown in the formula (3), wherein R1 is -H, -OCH3 or -SO3H, and M is an alkali metal ion. The compound active dark-red dye has the properties of good stability, high upgrade rate, solubility and color fixation, and excellent dyeing synchronicity, level dyeing and color reproducibility, particularly has relatively high light fastness, outstanding deep dyeing property and oxygen bleaching resistance property and other favorable properties, and is suitable for printing and dyeing of cellulose fiber materials, particularly cotton, cotton/polyester and the like.
Description
Technical field
The present invention relates to reactive dyestuff field, be specifically related to a kind of composite reactive crimson and its preparation method and application.
Background technology
Reactive dyestuffs chromatogram is wide, lovely luster, excellent performance, suitability are strong, its form and aspect and performance adapt with the requirement of market to fiber and dress material substantially, be one of most important dyestuff of cellulose dyeing and stamp, more originally also gradually adopted reactive dyeing with the textiles that insoluble azo, sulfuration and vat dyes dye.In addition, the application of reactive dyestuffs on protein fibre, synthon and some tencels such as soybean, milk protein fibre etc. also constantly expands.
The unique shortcoming of reactive dyestuffs is hydrolysis problem, and being also affects one of important factor that cotton fibre degree of fixation improves.Usually dyestuff set on cotton in the basic conditions, and this basicity facilitates the reaction of dyestuff and water, causes its inactivation.The dyestuff of inactivation, is also hydrolised dye, can not reacts, thus cause considerable part dyestuff to be depleted with cotton.Hydrolised dye and matrix generation physical adherence, until by eccysis treatment stage of washing, thus cause washing fastness problem.
In addition, after reactive dyestuffs carry out the textile dyeings such as cotton, light fastness and resistance to oxygen bleaching performance also need further raising, and the dark kind that can replace thioxine dyes and vat dyes etc. in reactive dyestuff field is rare especially.
Summary of the invention
The object of this invention is to provide a kind of new composite reactive crimson, this dyestuff high light fastness, good fixation ability and splendid depth, be particularly useful for the multiple cellulose dyeings such as cotton, cotton/wash.
Composite reactive crimson provided by the invention, counts by weight, comprises formula (1) compound of 30 ~ 80 parts, 10 ~ 30 parts of formula (2) compounds and 10 ~ 40 parts of formula (3) compounds:
Wherein, R
1for-H ,-OCH
3or-SO
3h; M is alkalimetal ion.That comparatively commonly uses in alkalimetal ion has sodium ion, potassium ion etc.
There is in above-mentioned three components a chloro-s-triazine base and ethene sulfuryl double active base, they are to avidity, dye uptake, degree of fixation, level-dyeing property, the enhancing rate of fiber, to electrolyte salt, to laking agent bases, to dyeing temperature susceptibility and clean rate all more close, above-mentioned composite go out active deep red dyestuff has good stability, solubleness is high, degree of fixation is high, dyeing synchronism good, good level-dyeing property, color reproducibility are good, especially outstanding higher light fastness and the premium properties such as outstanding pile-on properties and resistance to oxygen bleaching, be applicable to dyeing and printing of cellulosic fibre materials.
Preferably, in above-mentioned composite reactive crimson, M is sodium ion.
The present invention also provides a kind of preparation method of above-mentioned composite reactive crimson Chinese style (1) compound, and step comprises:
1. by H acid making beating, regulating pH=7.0 to dissolving with liquid caustic soda, joining in cyanuric chloride making beating liquid and carrying out primary condensation reaction, regulating pH=3.5 ~ 4.0, react 2 hours;
2. position ester between N-ethyl is joined in said mixture solution, be warming up to T=40 DEG C, maintain pH=3.5 ~ 4.0, react 4 hours to obtain two contracting liquid;
3. ORTHO AMINO PHENOL SULPHONIC and hydrochloric acid mixed solution are added water and ice pull an oar 30 minutes, add the sodium nitrite in aqueous solution that mass percentage concentration is 30%, holding temperature T=0-5 DEG C, react and eliminate unnecessary Sodium Nitrite with thionamic acid after 1 hour; When use starch potassium iodide paper detects aobvious colourless, when showing blue with congo-red test paper detection, terminal arrives simultaneously, obtains diazo liquid;
4. diazo liquid is joined in two contracting liquid, regulate pH=7.0 ~ 7.5, holding temperature T=8 ~ 15 DEG C, react terminal after 6 hours and arrive, obtain coupling solution; Coupling solution is crossed and filters insolubles and carry out spraying dry and namely obtain formula (1) compound.
The present invention also provides a kind of preparation method of above-mentioned composite reactive crimson Chinese style (2) compound, and step comprises:
1. by H acid making beating, regulating pH=7.0 to dissolving with liquid caustic soda, joining in cyanuric chloride making beating liquid and carrying out primary condensation reaction, regulating pH=3.5 ~ 4.0, react 2 hours;
2. position ester between N-ethyl is joined in said mixture solution, be warming up to T=40 DEG C, maintain pH=3.5 ~ 4.0, react 4 hours to obtain two contracting liquid;
3. the mixed solution of para-ester, O-methoxy para-ester or sulfonation para-ester and hydrochloric acid to be added water and ice is pulled an oar 30 minutes, add the sodium nitrite in aqueous solution that mass percentage concentration is 30%, holding temperature T=0 ~ 5 DEG C, react and eliminate unnecessary Sodium Nitrite with thionamic acid after 1 hour; When use starch potassium iodide paper detects aobvious colourless, when showing blue with congo-red test paper detection, terminal arrives simultaneously, obtains diazo liquid;
4. above-mentioned diazo liquid is joined in two contracting liquid, regulate pH=7.0 ~ 7.5, holding temperature T=8 ~ 15 DEG C, react terminal after 6 hours and arrive, obtain coupling solution; Coupling solution is crossed and filters insolubles and carry out spraying dry and namely obtain formula (2) compound.
The present invention also provides a kind of preparation method of above-mentioned composite reactive crimson Chinese style (3) compound, and step comprises:
1. added water by the mixed solution of para-ester and hydrochloric acid and ice is pulled an oar 30 minutes, add the sodium nitrite in aqueous solution that mass percentage concentration is 30%, a holding temperature T=0 ~ 5 DEG C reaction eliminated unnecessary Sodium Nitrite with thionamic acid after 1 hour; When use starch potassium iodide paper detects aobvious colourless, when showing blue with congo-red test paper detection, terminal arrives simultaneously, obtains para-ester diazo liquid;
2. by J acid making beating, regulating pH=7.0 to dissolving with liquid caustic soda, joining in para-ester diazo liquid and carrying out a coupled reaction, regulate pH=2.0 ~ 3.0, maintain reaction 4 hours, a coupling is complete;
3. a conjugates sodium bicarbonate dry powder is regulated pH=7.0 ~ 7.5, holding temperature T=10 ~ 15 DEG C, react terminal after 4 ~ 5 hours and arrive, obtain secondary coupling solution; Secondary coupling solution is crossed and filters insolubles, carry out spraying dry and namely obtain formula (3) compound.
In above-mentioned multiple preparation method, the chemical name of described H acid is 1-amino-8-naphthol-3,6-disulfonic acid, and the chemical name of J acid is 2-amino-5-naphthols-7-sulfonic acid.
The present invention also provides a kind of scarlet dye composite, and comprising any one the present invention above-mentioned also provides a kind of composite reactive crimson.
Preferably, in above-mentioned scarlet dye composite, one or more in dyeing accelerant, laking agent and softening agent are also comprised.
Preferably, in above-mentioned scarlet dye composite, described dyeing accelerant is Na
2sO
4or NaCl, described laking agent is NaOH, Na
2cO
3or NaHCO
3.
Preferably, in above-mentioned scarlet dye composite, fire retardant and/or electrostatic agent is also comprised.
The present invention also provides the application of above arbitrary described scarlet dye composite in cellulosic fibre material printing and dyeing.
Compared with prior art, the present invention has following beneficial effect:
Composite reactive crimson of the present invention, form by meticulously developing composite three kinds of dyestuffs, there is in three components wherein a chloro-s-triazine base and ethene sulfuryl double active base, it has hyperergy, high enhancing rate, high-dissolvability, high colour-fast rate, has good depth especially, high light fastness, the premium propertiess such as resistance to oxygen bleaching, beautiful in colour, dyeing residual liquid is few, belongs to environmental protection and energy saving dyestuff.They are to avidity, dye uptake, degree of fixation, level-dyeing property, the enhancing rate of fiber, to electrolyte salt, to laking agent bases, to dyeing temperature susceptibility and clean rate all more close.This dyestuff has good stability, enhancing rate is good, solubleness is high, degree of fixation is high, dyeing synchronism is good, good level-dyeing property, color reproducibility are good, especially outstanding higher light fastness and the premium properties such as outstanding pile-on properties and resistance to oxygen bleaching, be applicable to dyeing and printing of cellulosic fibre materials, be specially adapted to cotton, cotton/wash.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, can better understand the present invention and can be implemented, but illustrated embodiment is not as a limitation of the invention to make those skilled in the art.
One, compound preparation
Formula (1 ') preparation method is as follows:
1. by H acid making beating, with liquid caustic soda regulate pH=7.0 to dissolve, join cyanuric chloride making beating liquid in carry out primary condensation reaction, regulate pH=3.5 ~ 4.0, react 2 hours stand-by.
2. position ester between N-ethyl is joined in said mixture solution, be warming up to T=40 DEG C, maintain pH=3.5 ~ 4.0, react 4 hours to obtain two contracting liquid.
3. ORTHO AMINO PHENOL SULPHONIC, hydrochloric acid are added water, ice pulls an oar 30 minutes, add 30% (mass percentage concentration) sodium nitrite in aqueous solution, holding temperature T=0 ~ 5 DEG C, react and eliminate unnecessary Sodium Nitrite with thionamic acid after 1 hour.When starch potassium iodide paper shows colourless, congo-red test paper shows blue terminal and arrives, and obtains diazo liquid.
4. above-mentioned diazo liquid is joined in two contracting liquid, regulate pH=7.0 ~ 7.5, holding temperature T=8 ~ 15 DEG C, react terminal after 6 hours and arrive, obtain coupling solution.Coupling solution is crossed and filters insolubles and carry out spraying dry and namely obtain formula (1 ') dyestuff.
Formula (2 ') preparation method is as follows:
1. by H acid making beating, with liquid caustic soda regulate pH=7.0 to dissolve, join cyanuric chloride making beating liquid in carry out primary condensation reaction, regulate pH=3.5 ~ 4.0, react 2 hours stand-by.
2. position ester between N-ethyl is joined in said mixture solution, be warming up to T=40 DEG C, maintain pH=3.5 ~ 4.0, react 4 hours to obtain two contracting liquid.
3. para-ester (O-methoxy para-ester or sulfonation para-ester), hydrochloric acid are added water, ice pulls an oar 30 minutes, add 30% (mass percentage concentration) sodium nitrite in aqueous solution, holding temperature T=0 ~ 5 DEG C, react and eliminate unnecessary Sodium Nitrite with thionamic acid after 1 hour.When starch potassium iodide paper shows colourless, congo-red test paper shows blue terminal and arrives, and obtains diazo liquid.
4. above-mentioned diazo liquid is joined in two contracting liquid, regulate pH=7.0 ~ 7.5, holding temperature T=8 ~ 15 DEG C, react terminal after 6 hours and arrive, obtain coupling solution.Coupling solution is crossed and filters insolubles and carry out spraying dry and namely obtain formula (2 ') dyestuff.
Wherein, step 3. in use para-ester time obtain product (2 '-1), step 3. in use O-methoxy para-ester time obtain product (2 '-2), step 3. in use sulfonation para-ester time obtain product (2 '-3).
Formula (3 ') preparation method is as follows:
1. para-ester, hydrochloric acid added water, ice pulls an oar 30 minutes, add 30% (mass percentage concentration) sodium nitrite in aqueous solution, a holding temperature T=0 ~ 5 DEG C reaction eliminated unnecessary Sodium Nitrite with thionamic acid after 1 hour.When starch potassium iodide paper shows colourless, congo-red test paper shows blue terminal and arrives, and obtains diazo liquid.
2. by J acid making beating, regulating pH=7.0 to dissolving with liquid caustic soda, joining in para-ester diazonium salt and carrying out a coupled reaction, regulate pH=2.0 ~ 3.0, maintain reaction 4 hours, a coupling is complete.
3. a conjugates sodium bicarbonate dry powder is regulated pH=7.0 ~ 7.5, holding temperature T=10 ~ 15 DEG C, react terminal after 4-5 hour and arrive, obtain secondary coupling solution.Secondary coupling solution is crossed and filters insolubles, carry out spraying dry and namely obtain formula (3 ') dyestuff.
Two, composite reactive crimson preparations and applicatio
Embodiment 1:
55g is met formula (1 ') dyestuff, 20g meets formula (2 ') dyestuff (2 '-1) and 25g meets formula (3 ') dyestuff and obtains composite reactive crimson of the present invention through mechanically mixing fully, cellulosic fibre material can be dyeing into that light fastness is high, color is dark, the scarlet of resistance to oxygen bleaching excellent property by this dyestuff.
Embodiment 2:
By the aqueous solution containing 55g formula (1 '), the aqueous solution containing 20g formula (2 ') dyestuff (2 '-1) and containing the drying that stirs after the aqueous solution of 25g formula (3 ') dyestuff, obtain composite reactive crimson of the present invention, cellulosic fibre material can be dyeing into that light fastness is high, color is dark, the scarlet of resistance to oxygen bleaching excellent property by this dyestuff.
Embodiment 3:
70g is met formula (1 ') dyestuff, 15g meets formula (2 ') dyestuff (2 '-2) and 15g meets formula (3 ') dyestuff and obtains composite reactive crimson of the present invention through mechanically mixing fully, cellulosic fibre material can be dyeing into that light fastness is high, color is dark, the scarlet of resistance to oxygen bleaching excellent property by this dyestuff.
Embodiment 4:
80g is met the aqueous solution of formula (1 ') dyestuff, the aqueous solution that the aqueous solution that 10g meets formula (2 ') dyestuff (2 '-2) and 10g meet formula (3 ') dyestuff obtains composite reactive crimson of the present invention through mechanically mixing fully, cellulosic fibre material can be dyeing into that light fastness is high, color is dark, the scarlet of resistance to oxygen bleaching excellent property by this dyestuff.
Embodiment 5:
80g is met formula (1 ') dyestuff, 10g meets formula (2 ') dyestuff (2 '-3) and 10g meets formula (3 ') dyestuff and obtains composite reactive crimson of the present invention through mechanically mixing fully, cellulosic fibre material can be dyeing into that light fastness is high, color is dark, the scarlet of resistance to oxygen bleaching excellent property by this dyestuff.
Embodiment 6:
60g is met formula (1 ') dyestuff, 20g meets formula (2 ') dyestuff (2 '-3) and 20g meets formula (3 ') dyestuff and obtains composite reactive crimson of the present invention through mechanically mixing fully, cellulosic fibre material can be dyeing into that light fastness is high, color is dark, the scarlet of resistance to oxygen bleaching excellent property by this dyestuff.
Following examples are the application of dyestuff of the present invention:
Embodiment 7 dyes:
First make it fully dissolve with appropriate water by the composite reactive crimson that embodiment 1 is obtained 4g, then constant volume is in 500mL volumetric flask.Draw 10mL dye liquor to mix with 50mL water, then 4g cotton is added, 1.8g sodium sulfate, is then raised to 60 DEG C with the heat-up rate of 1 DEG C/min, keeps adding 1g sodium carbonate after 30 minutes, 60 DEG C are kept to dye again 30 minutes, take out by dye cotton subsequently, with non-ionic cleaning agent boiling soap boiling 15 minutes, carry out cold water, hot water intersects after cleaning, and about 70 DEG C oven dry, it obtains, and staining power is high, good level-dyeing property, favorable reproducibility, thick in color and the good scarlet of gorgeous, resistance to oxygen bleaching.
Embodiment 8 dyes:
First make it fully dissolve with appropriate water by the composite reactive crimson that embodiment 2 is obtained 4g, then constant volume is in 500mL volumetric flask.Draw 10mL dye liquor to mix with 50mL water, then 4g cotton is added, 1.8g sodium sulfate, then 60 DEG C are raised to the heat-up rate of 1 DEG C/min, keep adding 1g sodium carbonate after 30 minutes, 60 DEG C are kept to dye again 30 minutes, take out by dye cotton subsequently, with non-ionic cleaning agent boiling soap boiling 15 minutes, after carrying out cold water, the cleaning of hot water intersection, and about 70 DEG C oven dry, it obtains, and staining power is high, good level-dyeing property, favorable reproducibility, dyeing residual liquid are few, thick in color and the good scarlet of gorgeous, resistance to oxygen bleaching.
Embodiment 9 dyes:
First make it fully dissolve with appropriate water by the composite reactive crimson that embodiment 3 is obtained 4g, then constant volume is in 500mL volumetric flask.Draw 10mL dye liquor to mix with 50mL water, then 4g cotton is added, 1.8g sodium sulfate, then 60 DEG C are raised to the heat-up rate of 1 DEG C/min, keep adding 1g sodium carbonate after 30 minutes, 60 DEG C are kept to dye again 30 minutes, take out by dye cotton subsequently, with non-ionic cleaning agent boiling soap boiling 15 minutes, after carrying out cold water, the cleaning of hot water intersection, and about 70 DEG C oven dry, it obtains, and staining power is high, good level-dyeing property, favorable reproducibility, dyeing residual liquid are few, thick in color and the good scarlet of gorgeous, resistance to oxygen bleaching.
Embodiment 10 dyes:
First make it fully dissolve with appropriate water by the composite reactive crimson that embodiment 4 is obtained 4g, then constant volume is in 500mL volumetric flask.Draw 10mL dye liquor to mix with 50mL water, then 4g cotton is added, 1.8g sodium sulfate, then 60 DEG C are raised to the heat-up rate of 1 DEG C/min, keep adding 1g sodium carbonate after 30 minutes, 60 DEG C are kept to dye again 30 minutes, take out by dye cotton subsequently, with non-ionic cleaning agent boiling soap boiling 15 minutes, after carrying out cold water, the cleaning of hot water intersection, and about 70 DEG C oven dry, it obtains, and staining power is high, good level-dyeing property, favorable reproducibility, dyeing residual liquid are few, thick in color and the good scarlet of gorgeous, resistance to oxygen bleaching.
Embodiment 11 dyes:
First make it fully dissolve with appropriate water by the composite reactive crimson that embodiment 5 is obtained 4g, then constant volume is in 500mL volumetric flask.Draw 10mL dye liquor to mix with 50mL water, then 4g cotton is added, 1.8g sodium sulfate, then 60 DEG C are raised to the heat-up rate of 1 DEG C/min, keep adding 1g sodium carbonate after 30 minutes, 60 DEG C are kept to dye again 30 minutes, take out by dye cotton subsequently, with non-ionic cleaning agent boiling soap boiling 15 minutes, after carrying out cold water, the cleaning of hot water intersection, and about 70 DEG C oven dry, it obtains, and staining power is high, good level-dyeing property, favorable reproducibility, dyeing residual liquid are few, thick in color and the good scarlet of gorgeous, resistance to oxygen bleaching.
Embodiment 12 dyes:
First make it fully dissolve with appropriate water by the composite reactive crimson that embodiment 6 is obtained 4g, then constant volume is in 500mL volumetric flask.Draw 10mL dye liquor to mix with 50mL water, then 4g cotton is added, 1.8g sodium sulfate, then 60 DEG C are raised to the heat-up rate of 1 DEG C/min, keep adding 1g sodium carbonate after 30 minutes, 60 DEG C are kept to dye again 30 minutes, take out by dye cotton subsequently, with non-ionic cleaning agent boiling soap boiling 15 minutes, after carrying out cold water, the cleaning of hot water intersection, and about 70 DEG C oven dry, it obtains, and staining power is high, good level-dyeing property, favorable reproducibility, dyeing residual liquid are few, thick in color and the good scarlet of gorgeous, resistance to oxygen bleaching.
Following table is that embodiment 1 ~ 6 scarlet dye composite and reactive red 3BS application indexes detect and contrast:
The above embodiment is only that protection scope of the present invention is not limited thereto in order to absolutely prove the preferred embodiment that the present invention lifts.The equivalent alternative or conversion that those skilled in the art do on basis of the present invention, all within protection scope of the present invention.Protection scope of the present invention is as the criterion with claims.
Claims (10)
1. a composite reactive crimson, is characterized in that, counts by weight, comprises formula (1) compound of 30 ~ 80 parts, 10 ~ 30 parts of formula (2) compounds and 10 ~ 40 parts of formula (3) compounds:
Wherein, R
1for-H ,-OCH
3or-SO
3h; M is alkalimetal ion.
2. composite reactive crimson according to claim 1, is characterized in that, M is sodium ion.
3. a preparation method for composite reactive crimson Chinese style (1) compound as claimed in claim 1, it is characterized in that, step comprises:
1. by H acid making beating, regulating pH=7.0 to dissolving with liquid caustic soda, joining in cyanuric chloride making beating liquid and carrying out primary condensation reaction, regulating pH=3.5 ~ 4.0, react 2 hours;
2. position ester between N-ethyl is joined in said mixture solution, be warming up to T=40 DEG C, maintain pH=3.5 ~ 4.0, react 4 hours to obtain two contracting liquid;
3. ORTHO AMINO PHENOL SULPHONIC and hydrochloric acid mixed solution are added water and ice pull an oar 30 minutes, add the sodium nitrite in aqueous solution that mass percentage concentration is 30%, holding temperature T=0 ~ 5 DEG C, react and eliminate unnecessary Sodium Nitrite with thionamic acid after 1 hour; When use starch potassium iodide paper detects aobvious colourless, when showing blue with congo-red test paper detection, terminal arrives simultaneously, obtains diazo liquid;
4. diazo liquid is joined in two contracting liquid, regulate pH=7.0 ~ 7.5, holding temperature T=8 ~ 15 DEG C, react terminal after 6 hours and arrive, obtain coupling solution; Coupling solution is crossed and filters insolubles and carry out spraying dry and namely obtain formula (1) compound.
4. a preparation method for composite reactive crimson Chinese style (2) compound as claimed in claim 1, it is characterized in that, step comprises:
1. by H acid making beating, regulating pH=7.0 to dissolving with liquid caustic soda, joining in cyanuric chloride making beating liquid and carrying out primary condensation reaction, regulating pH=3.5 ~ 4.0, react 2 hours;
2. position ester between N-ethyl is joined in said mixture solution, be warming up to T=40 DEG C, maintain pH=3.5 ~ 4.0, react 4 hours to obtain two contracting liquid;
3. the mixed solution of para-ester, O-methoxy para-ester or sulfonation para-ester and hydrochloric acid to be added water and ice is pulled an oar 30 minutes, add the sodium nitrite in aqueous solution that mass percentage concentration is 30%, holding temperature T=0 ~ 5 DEG C, react and eliminate unnecessary Sodium Nitrite with thionamic acid after 1 hour; When use starch potassium iodide paper detects aobvious colourless, when showing blue with congo-red test paper detection, terminal arrives simultaneously, obtains diazo liquid;
4. above-mentioned diazo liquid is joined in two contracting liquid, regulate pH=7.0 ~ 7.5, holding temperature T=8 ~ 15 DEG C, react terminal after 6 hours and arrive, obtain coupling solution; Coupling solution is crossed and filters insolubles and carry out spraying dry and namely obtain formula (2) compound.
5. a preparation method for composite reactive crimson Chinese style (3) compound as claimed in claim 1, it is characterized in that, step comprises:
1. added water by the mixed solution of para-ester and hydrochloric acid and ice is pulled an oar 30 minutes, add the sodium nitrite in aqueous solution that mass percentage concentration is 30%, a holding temperature T=0 ~ 5 DEG C reaction eliminated unnecessary Sodium Nitrite with thionamic acid after 1 hour; When use starch potassium iodide paper detects aobvious colourless, when showing blue with congo-red test paper detection, terminal arrives simultaneously, obtains para-ester diazo liquid;
2. by J acid making beating, regulating pH=7.0 to dissolving with liquid caustic soda, joining in para-ester diazo liquid and carrying out a coupled reaction, regulate pH=2.0 ~ 3.0, maintain reaction 4 hours, a coupling is complete;
3. a conjugates sodium bicarbonate dry powder is regulated pH=7.0 ~ 7.5, holding temperature T=10 ~ 15 DEG C, react terminal after 4 ~ 5 hours and arrive, obtain secondary coupling solution; Secondary coupling solution is crossed and filters insolubles, carry out spraying dry and namely obtain formula (3) compound.
6. a scarlet dye composite, is characterized in that, comprises the composite reactive crimson described in claim 1 or 2.
7. scarlet dye composite according to claim 6, is characterized in that, also comprises one or more in dyeing accelerant, laking agent and softening agent.
8. scarlet dye composite according to claim 7, is characterized in that, described dyeing accelerant is Na
2sO
4or NaCl, described laking agent is NaOH, Na
2cO
3or NaHCO
3.
9. the scarlet dye composite according to claim 7 or 8, is characterized in that, also comprises fire retardant and/or electrostatic agent.
10. the application of the arbitrary described scarlet dye composite of claim 6 ~ 9 in cellulosic fibre material printing and dyeing.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108192384A (en) * | 2018-02-12 | 2018-06-22 | 泰兴锦云染料有限公司 | A kind of red reactive dye mixture and its application |
| CN108641408A (en) * | 2018-05-25 | 2018-10-12 | 吴江桃源染料有限公司 | A kind of composite reactive scarlet dye and its application |
| CN111019390A (en) * | 2019-12-26 | 2020-04-17 | 浙江劲光实业股份有限公司 | Preparation method of composite active bright red dye |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1871308A (en) * | 2003-10-20 | 2006-11-29 | 西巴特殊化学品控股有限公司 | Mixtures of reactive dyes and their use |
| CN101250333A (en) * | 2008-04-08 | 2008-08-27 | 赵卫国 | Reactive deep red RGB diazo dyes and preparation method thereof |
| CN101899227A (en) * | 2010-06-08 | 2010-12-01 | 湖北华丽染料工业有限公司 | Composite reactive red dye |
-
2015
- 2015-06-01 CN CN201510294125.4A patent/CN104927396B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1871308A (en) * | 2003-10-20 | 2006-11-29 | 西巴特殊化学品控股有限公司 | Mixtures of reactive dyes and their use |
| CN101250333A (en) * | 2008-04-08 | 2008-08-27 | 赵卫国 | Reactive deep red RGB diazo dyes and preparation method thereof |
| CN101899227A (en) * | 2010-06-08 | 2010-12-01 | 湖北华丽染料工业有限公司 | Composite reactive red dye |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108192384A (en) * | 2018-02-12 | 2018-06-22 | 泰兴锦云染料有限公司 | A kind of red reactive dye mixture and its application |
| CN108192384B (en) * | 2018-02-12 | 2019-05-14 | 泰兴锦云染料有限公司 | A kind of red reactive dye mixture and its application |
| CN108641408A (en) * | 2018-05-25 | 2018-10-12 | 吴江桃源染料有限公司 | A kind of composite reactive scarlet dye and its application |
| CN111019390A (en) * | 2019-12-26 | 2020-04-17 | 浙江劲光实业股份有限公司 | Preparation method of composite active bright red dye |
| CN111019390B (en) * | 2019-12-26 | 2021-02-02 | 浙江劲光实业股份有限公司 | Preparation method of composite active bright red dye |
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