CN101481534A - Preparation of reactive dye brilliant blue KN-R - Google Patents
Preparation of reactive dye brilliant blue KN-R Download PDFInfo
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- CN101481534A CN101481534A CNA2008101540872A CN200810154087A CN101481534A CN 101481534 A CN101481534 A CN 101481534A CN A2008101540872 A CNA2008101540872 A CN A2008101540872A CN 200810154087 A CN200810154087 A CN 200810154087A CN 101481534 A CN101481534 A CN 101481534A
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- cuprous chloride
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Abstract
The invention relates to a method for preparing reactive dye brilliant blue KN-R applicable to dyeing of pure cotton. In the method, bromamine acid, metaposition oil, calcined soda, sodium bicarbonate, hydrochloric acid and concentrated sulfuric acid are taken as main raw materials. The reactive dye of the invention is prepared by condensation, esterification, improvement of dye strength, chromatic light adjustment, intensity adjustment, drying and packing with catalysts cuprous chloride and electrolytic copper powder applied. In the preparation method, the reaction between the bromamine acid and the metaposition oil is condensation under the dual effect of the catalyst and the addition agent, the reaction time is short and the reaction efficiency is improved.
Description
Technical field
The present invention relates to a kind of preparation method of reactive dyestuffs, particularly relate to a kind of improved preparation method who is applicable to the blue KN-R of reactive-dye brilliant of pure cotton dyeing.
Background technology
Distinguishing features such as reactive dyestuffs have lovely luster, application performance excellence, easy to use, and suitability is strong.Enter 21 century, because it is the economic factors of environmental ecology restriction, more and more higher to the requirement of production preparation, dye uptake, degree of fixation and the dyeing waste-water of reactive dyestuffs.Existing a kind of gorgeous blue reactive dyestuffs, its structural formula is shown in (I):
Dye industry is referred to as reactive brilliant blue KN-R.Reactive brilliant blue KN-R dyestuff all adopts bromamine acid and position oil condensation under catalyst action in the industry in preparation process at present, and is refining through twice again, removes purple insolubles, and color base is dried then.The yield of present preparation method's principal reaction thing bromamine acid is 70%, and present novel process makes the yield of bromamine acid bring up to 86%.Catalyst consumption has also been lacked many than before, and production cost reduces.
Summary of the invention
Solve the problems of the technologies described above, the invention provides a kind of improved reactive brilliant blue KN-R dyestuff preparation method, this preparation method has adopted the catalyst condensation reaction that is dissolved in auxiliary agent, and the reaction times shortens, and reaction efficiency improves.
For solving the problems of the technologies described above, the invention provides the preparation method of the gorgeous blue KN-R of a kind of reactive dye for wool, this method comprises the condensation of a bromamine acid and a position oil, refining, esterification, dilution step, it is characterized in that adopting in the condensation reaction catalyzer cuprous chloride and electrolytic copper powder, and the catalyzer cuprous chloride is dissolved in the auxiliary agent, under catalyzer and auxiliary agent dual function, carry out condensation reaction.
In the aforesaid method, auxiliary agent is DMF.
In the aforesaid method, catalyzer and auxiliary agent are mixed, and mixture divided join in the reaction solution each 20-40 minute at interval for 4 times.
Particularly, the invention provides the method for preparing the blue KN-R of reactive-dye brilliant that comprises following step of condensation:
The step of condensation reaction is:
In water, add bromamine acid, a position oil, stir the adding sodium bicarbonate, make the PH=8-10 of this solution, controlled temperature 95-98 ℃, be incubated 10 minutes, be cooled to 75-80 ℃, get mixed solution, cuprous chloride is added among the auxiliary agent DMF, make the cuprous chloride dissolving, then itself and electrolytic copper powder being divided together joins for 4 times in the above-mentioned mixed solution, and each 20-40 minute at interval, after adding finishes, 74-75 ℃ of temperature control, stirring reaction 6 hours gets condensated liquid;
The preparation method of above-mentioned reactive brilliant blue KN-R dyestuff of the present invention has excellent effect, the reaction of a bromamine acid and a position oil is condensation under catalyzer and auxiliary agent dual function in the preparation process, reaction times shortens, improve reaction efficiency, by the dyestuff dye uptake of method preparation of the present invention, degree of fixation and solubleness better effects if, the quality of dyestuff has obtained further raising, and this method reduced the use of catalyzer, reduces the pollution to environment.
Embodiment
Embodiment 1
1, allocation sheet:
| Material name | Molecular weight | Molecular ratio | Roll over hundred consumptions (Kg) | Charging capacity (mole) |
| Bromamine acid | 404 | 1.0 | 80.8 | 0.2 |
| Between position oil | 201 | 1.2 | 48.2 | 0.24 |
| Sodium bicarbonate | 84 | 4.0 | 67.2 | 0.8 |
| Cuprous chloride | 199 | 0.05 | 1.99 | 0.01 |
| Electrolytic copper powder | 64 | 0.15 | 0.4 | 0.0063 |
| Sulfuric acid | 98 | 40.8 | 800 | 8.16 |
| DMF (dimethyl formamide) | 1.2 |
2, dyestuff preparation technology of the present invention operates as follows:
(a) condensation: the dissolving of bromamine acid, a position oil: add end water 200ml in four-hole bottle, add the bromamine acid of 80.8g, position oil heats up between 48.2g, 95 ℃ of controlled temperature, and material all dissolves, and is incubated 10 minutes, is cooled to 80 ℃, gets mixed solution; 1.99g Red copper oxide is dissolved in the DMF of 1.2g, divides itself and 0.4g electrolytic copper powder 4 times then and add in the above-mentioned mixed solution, and each 30 minutes at interval, add finish after, 70-75 ℃ of temperature control, stirring reaction 6 hours, condensated liquid;
(b) extract bromamine acid under the hot conditions: condensated liquid is warming up to 90 ℃, is incubated 10 minutes, heat filtering gets filter cake and filtrate, and bromamine acid just is dissolved in the filtrate, and filtrate is used in reaction next time once more;
(c) refining: as with the filter cake making beating that (b) step obtains, in the time of 25 ℃, to transfer PH=1.3-2.0, stirred 30 minutes with hydrochloric acid, filter filter cake, this filter cake is pulled an oar once more, be warming up to 70-75 ℃ and transfer PH=1.3-2.0 with hydrochloric acid, stirred 30 minutes, and filtered to such an extent that filter cake is dried, removed purple secondary dyestuff;
(d) esterification: filter cake is pulverized, is slowly joined in 100% sulfuric acid of 800g, add the back 25-30 ℃ of insulation reaction 2 hours, esterification reaction product;
(e) dilution; Esterification reaction product is diluted to below 0 degree with ice, filters fast, filter cake is pulled an oar again, be cooled to 15 ℃, add 10% sodium-chlor, see and ooze the qualified after-filtration of circle, with the filter cake making beating, transfer PH=6.2 after the filtration with sodium bicarbonate with ice; Filter and collect filtrate;
(f) adjust coloured light and intensity: filtrate that will (f) step is dyeed with small-sized spray tower drying, carries out the adjustment of coloured light and intensity again according to coloration result;
(g) carry out spraying drying;
The foregoing description 1 preparation hair is as follows with the performance perameter of reactive brilliant blue KN-R in dyeing:
From last table we as can be seen, the dyestuff of the method for embodiment 1 preparation has good performance, especially excellent performance aspect solubleness, colour fastness.
Dyestuff of the present invention is not only excellent on performance, and effect is also relatively good aspect environmental protection, and the reaction efficiency of bromamine acid improves on the one hand, has reduced the content of bromamine acid in the waste liquid, and the content that is exactly copper in the waste liquid in addition reduces, and has reduced the heavy metal contamination to environment.
The norm quota of consumption table of material among the embodiment 1 preparation reactive brilliant blue KN-R
| Material name | Consume, (Kg) |
| Bromamine acid | 80.8 |
| Between position oil | 48.2 |
| Sodium bicarbonate | 67.2 |
| Cuprous chloride | 1.99 |
| Electrolytic copper powder | 0.4 |
| Sulfuric acid | 800 |
| DMF | 1.2 |
Under situation about obtaining with the product of the same amount of the foregoing description 1, it is as follows to use the supplies consumption table that old technology (do not answer used additives and do not extract the preparation method of bromamine acid) produces:
| Material name | Consume (Kg) |
| Bromamine acid | 80.8 |
| Between position oil | 52.2 |
| Sodium bicarbonate | 67.2 |
| Cuprous chloride | 4 |
| Electrolytic copper powder | 1.5 |
| Sulfuric acid | 800 |
Dyestuff of the present invention and dyestuff preparation method are described by specific embodiment; Those skilled in the art can use for reference links such as content appropriate change raw material of the present invention, processing condition and realize corresponding other purpose, its relevant change does not all break away from content of the present invention, all similar replacements and change will become apparent to those skilled in the art that and all be regarded as comprising within the scope of the present invention.
Claims (4)
1, the preparation method of the gorgeous blue KN-R of a kind of reactive dye for wool, this method comprises the condensation of a bromamine acid and a position oil, refining, esterification, dilution step, it is characterized in that adopting in the condensation reaction catalyzer cuprous chloride and electrolytic copper powder, and the catalyzer cuprous chloride is dissolved in the auxiliary agent, under catalyzer and auxiliary agent dual function, carry out condensation reaction.
2,, it is characterized in that auxiliary agent is DMF according to the method for claim 1.
3,, it is characterized in that catalyzer and auxiliary agent are mixed, and mixture divided join in the reaction solution each about 20-40 minute at interval for 4 times according to the method for claim 1 or 2.
4,, it is characterized in that step of condensation is according to the method for claim 3:
In water, add bromamine acid, a position oil, stir the adding sodium bicarbonate, make the PH=8-10 of this solution, the about 95-98 of controlled temperature ℃, be incubated 10 minutes, be cooled to 75-80 ℃, get mixed solution, cuprous chloride is added among the auxiliary agent DMF, make the cuprous chloride dissolving, then itself and electrolytic copper powder being divided together joins for 4 times in the above-mentioned mixed solution, and each 20-40 minute at interval, after adding finishes, about 74-75 ℃ of temperature control, stirring reaction 6 hours gets condensated liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810154087 CN101481534B (en) | 2008-12-12 | 2008-12-12 | Preparation of reactive dye brilliant blue KN-R |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810154087 CN101481534B (en) | 2008-12-12 | 2008-12-12 | Preparation of reactive dye brilliant blue KN-R |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101481534A true CN101481534A (en) | 2009-07-15 |
| CN101481534B CN101481534B (en) | 2013-03-20 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 200810154087 Expired - Fee Related CN101481534B (en) | 2008-12-12 | 2008-12-12 | Preparation of reactive dye brilliant blue KN-R |
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Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1032177A (en) * | 1988-09-15 | 1989-04-05 | 上海染料化工八厂 | One-step method for preparing kn-series activated black dyes |
| CN1108348C (en) * | 2000-10-24 | 2003-05-14 | 泰兴市锦鸡染料有限公司 | Reactive azo orange dye and its preparing process |
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Granted publication date: 20130320 Termination date: 20161212 |