CN101481536B - Preparation of brilliant blue KN-R - Google Patents
Preparation of brilliant blue KN-R Download PDFInfo
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- CN101481536B CN101481536B CN 200810154131 CN200810154131A CN101481536B CN 101481536 B CN101481536 B CN 101481536B CN 200810154131 CN200810154131 CN 200810154131 CN 200810154131 A CN200810154131 A CN 200810154131A CN 101481536 B CN101481536 B CN 101481536B
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- filter cake
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- esterification
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Abstract
The invention relates to a method for preparing a reactive dye KN-R used for fur. The method comprises condensation, refining, esterification and dilution of bromamine acid and metaposition oil; wherein dilution in the invention is improved and is carried out below 0 DEG C while the pH value is adjusted to 8.0-9.0, so that filtration efficiency and yield are 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
The distinguishing features such as reactive dyestuffs have lovely luster, application performance is excellent, easy to use, and suitability is strong.Enter 21 century, because the economic factors of environmental ecology restriction, more and more higher to the requirement of manufacture, 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 blue KN-R.The reactive blue KN-R dyestuff all adopts bromamine acid and position oil condensation under catalyst action in the industry in preparation process at present, refining through twice again, remove purple insolubles, then color base is dried, use 98% sulphating, dilute with ice at 15 ℃ after esterification is complete, filter, the filter cake making beating is used in the yellow soda ash and PH=6.0, the finished product of spraying to get.The main filtration temperature of present preparation method is too high, filters the problem of stopping up filtering net that easily produces, and method of the present invention has overcome above-mentioned technical problem.Improve the efficient of filtering, and improved the yield rate of product.
Summary of the invention
Solve the problems of the technologies described above, the invention provides a kind of improved reactive blue KN-R preparation of dyestuff method, the dilution step among this preparation method below 0 ℃, regulate under the condition of pH=8.0-9.0 and carry out.
Particularly, the invention provides the preparation method of the blue KN-R of a kind of wool reactive-dye brilliant, the method comprises the condensation of bromamine acid and a position oil, refining, esterification, dilution step, it is characterized in that dilution step below 0 ℃, regulate under the condition of pH=8.0-9.0 and carry out.
In the aforesaid method, dilution step is regulated the pH value and is used sodium bicarbonate to regulate.
Particularly, dilution step is: esterification reaction product is diluted with ice, and temperature is controlled at below 0 ℃, fast filtering, get the filter cake making beating, be cooled to 15 ℃ with ice, add 10% sodium-chlor, see and ooze the qualified rear filtration of circle, the filter cake making beating is transferred PH=6.2 with sodium bicarbonate after filtering, and filters, and gets product.
The preparation method of above-mentioned reactive blue KN-R dyestuff of the present invention has excellent effect, and dilution step is to dilute, transfer PH=8.0-9.0 with sodium bicarbonate with ice under 0 ℃, can once pull an oar like this, prevents the sulfate group hydrolysis, crosses the rate speed.
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, preparation of dyestuff technique 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 control 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, then divides itself and 0.4g electrolytic copper powder 4 times and add in the above-mentioned mixed solution, and every minor tick 30 minutes, adds complete after, temperature is controlled 70-75 ℃, stirring reaction 6 hours gets 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 reapplication in reaction next time;
(c) refining: that the filter cake that (b) step obtains is pulled an oar, in the time of 25 ℃, transfer PH=1.3-2.0 with hydrochloric acid, stirred 30 minutes, filter to get filter cake, this filter cake is pulled an oar again, be warming up to 70-75 ℃ and transfer PH=1.3-2.0 with hydrochloric acid, stirred 30 minutes, filter to such an extent that filter cake is dried, removed purple secondary dyestuff;
(d) esterification: filter cake is pulverized, slowly joined in 100% sulfuric acid of 800g, 25-30 ℃ of insulation reaction 2 hours, get esterification reaction product after adding;
(e) dilution; Esterification reaction product is diluted to below 0 degree with ice, and fast filtering is pulled an oar filter cake again, is cooled to 15 ℃ with ice, adds 10% sodium-chlor, sees to ooze the qualified rear filtration of circle, with the filter cake making beating, transfers PH=6.2 with sodium bicarbonate after the filtration; Filter and collect filtrate;
(f) adjust coloured light and intensity: the filtrate of (f) step is dry with the small spraying tower, and the adjustment of coloured light and intensity is carried out in dyeing again according to coloration result;
(g) carry out spraying drying;
Above-described embodiment 1 preparation hair is as follows with the performance perameter of reactive blue KN-R in dyeing:
We can find out from upper table, and the dyestuff of the method preparation of embodiment 1 has good performance, especially excellent performance aspect solubleness, colour fastness.
Dyestuff of the present invention and preparation of dyestuff method are described by specific embodiment; Those skilled in the art can use for reference the 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 deemed to be included within the scope of the present invention.
Claims (3)
1. the preparation method of the blue KN-R of a wool reactive-dye brilliant, the method comprise the condensation of bromamine acid and a position oil, refining, esterification, dilution step, it is characterized in that dilution step below 0 ℃, regulate under the condition of pH=8.0-9.0 and carry out.
2. according to claim 1 method is characterized in that regulating the pH value and uses sodium bicarbonate to regulate.
3. according to claim 1 and 2 method, it is characterized in that dilution step is: esterification reaction product is diluted with ice, and temperature is controlled at below 0 ℃, fast filtering, get the filter cake making beating, be cooled to 15 ℃ with ice, add 10% sodium-chlor, see and ooze the qualified rear filtration of circle, filter cake making beating after filtering, transferring pH with sodium bicarbonate is 6.2, filters, and gets product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810154131 CN101481536B (en) | 2008-12-12 | 2008-12-12 | Preparation of brilliant blue KN-R |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200810154131 CN101481536B (en) | 2008-12-12 | 2008-12-12 | Preparation of brilliant blue KN-R |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101481536A CN101481536A (en) | 2009-07-15 |
| CN101481536B true CN101481536B (en) | 2013-01-16 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200810154131 Expired - Fee Related CN101481536B (en) | 2008-12-12 | 2008-12-12 | Preparation of brilliant blue KN-R |
Country Status (1)
| Country | Link |
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| CN (1) | CN101481536B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1034012A (en) * | 1987-12-30 | 1989-07-19 | 大连工学院 | A kind of synthesis method of reactive blue dye |
| US5112971A (en) * | 1988-08-10 | 1992-05-12 | Sumitomo Chemical Company, Limited | Anthraquinone dye compounds having fibers reactive group |
| CN1127277A (en) * | 1994-06-24 | 1996-07-24 | 赫彻斯特股份公司 | Preparation of C.I. active blue 19 |
-
2008
- 2008-12-12 CN CN 200810154131 patent/CN101481536B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1034012A (en) * | 1987-12-30 | 1989-07-19 | 大连工学院 | A kind of synthesis method of reactive blue dye |
| US5112971A (en) * | 1988-08-10 | 1992-05-12 | Sumitomo Chemical Company, Limited | Anthraquinone dye compounds having fibers reactive group |
| CN1127277A (en) * | 1994-06-24 | 1996-07-24 | 赫彻斯特股份公司 | Preparation of C.I. active blue 19 |
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| Publication number | Publication date |
|---|---|
| CN101481536A (en) | 2009-07-15 |
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