CN1569969A - Active yellow SHE, synthetic method and its composite active yellow dye - Google Patents
Active yellow SHE, synthetic method and its composite active yellow dye Download PDFInfo
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- CN1569969A CN1569969A CN 200410014846 CN200410014846A CN1569969A CN 1569969 A CN1569969 A CN 1569969A CN 200410014846 CN200410014846 CN 200410014846 CN 200410014846 A CN200410014846 A CN 200410014846A CN 1569969 A CN1569969 A CN 1569969A
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- aniline
- reactive yellow
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Abstract
Disclosed is a yellow SBE monomer which is prepared by coupling 3,6,8-trisulfonic acid -2- naphthylamine diazonium with meta-amino-benzeneamine acetylized hydrochlorate, primary condensation with cyanuric chloride, then carrying out second condensation to p(beta-sulfate ethyl sulfone)aniline diazonium salt and 2,4-disulfonic phenylamine coupling liquid, and drying.
Description
Technical field
The present invention relates to dye field, be meant a kind of new reactive yellow monomer and synthetic this reactive yellow monomer methods, the composite reactive yellow dye that to provide with this reactive yellow monomer simultaneously be major ingredient.
Technical background
At present, the yellow kind of warm type mainly was a reactive yellow M-3RE product during dyeing was employed, and its molar extinction coefficient is than little, maximum absorption wavelength is about 440nm, under 10g/l concentration, it mangles and detects the k/s value between 3～4, is 0.6～0.7 than transplanting Rf.Its synthesis technique mainly is to utilize 3; 6; the diazonium thing of 8-trisulfonic acid-2-naphthylamines and the coupling of m-aminophenyl amine acetylize hydrochloride; the coupling terminal point to after carry out 20～30% sodium-chlor and saltout, press filtration, filter cake dissolves then; analyze with the oxidation-reduction method; calculated yield, again and the material about 0 ℃, pulverized of the cyanuric chloride of calculated amount carry out primary condensation then and a position ester carry out the secondary condensation, spray is done.The technology shortcoming is the unit cost height, and secondary condensation proportioning reaches 1.2～1.3, and material waste is serious, and a position ester number lattice is about 2 times of para-ester, the generation sewage of saltouing, and dyestuff can not dye dark color.
Summary of the invention
The invention provides a kind of new reactive yellow monomer, have lovely luster, get color depth, solubleness height, advantages such as substantivity is low, compatibleness good, favorable reproducibility, excellent levelling property, enhancing rate height, degree of fixation height, easily washing property is good, colour fastness is good.The monomeric structural formula of this reactive yellow SHE is:
Synthetic this reactive yellow SHE monomer methods is with 3; 6; the diazonium thing of 8-trisulfonic acid-2-naphthylamines and the coupling of m-aminophenyl amine acetylize hydrochloride; again with the cyanuric chloride primary condensation of calculated amount; carry out the secondary condensation with coupling solution to (beta-sulfuric ester ethyl sulfonyl) diazonium salt of aniline and 2,4-disulfonic acid aniline then, spray is done.
The present invention adopts the coupling material of para-ester diazonium salt and 2,4-disulfonic acid aniline to replace simple para-ester to carry out two to contract, the effect that two " N==N-" groups reach increases chromophoric group is arranged in the monomer structure; With position ester between the para-ester replacement, reduced the technology of saltouing, reduce secondary condensation proportioning, when promptly using coupling solution to (beta-sulfuric ester ethyl sulfonyl) diazonium salt of aniline and 2,4-disulfonic acid aniline to carry out the secondary condensation, the proportioning of (beta-sulfuric ester ethyl sulfonyl) aniline has been controlled to be 0.8-1.0; A whole set of system that adopts nanometer film, spraying drying to combine in addition on the technology has reduced the generation of pollution section, reaches to clean the production purpose.
Composite reactive yellow dye, it is a major ingredient with above-mentioned reactive yellow SHE monomer, weight consists of: reactive yellow SHE monomer 70～95%, dust-proofing agent 1～5%, Sodium sulfate anhydrous.min(99) 5～30%.
Reactive yellow SHE of the present invention reaches about 150% through this explained hereafter power part, and solubleness reaches 200 grams per liters, and light fastness reaches 6 grades, soaping fastness 4-5 level, crock fastness 4-5 level, ironing fastness 4-5 level, than transplanting Rf is 0.85～0.95, shows as substantivity and is better than yellow M-3RE; (2) production process does not directly produce sewage, and what vent gas treatment adopted is the immersion method dedusting, has stopped dye granule and has brought into hot blast and cause environmental pollution in the atmosphere; (3) production cost reduces, and product gets color depth, has reduced the printing and dyeing cost.
Embodiment
Embodiment 1
Diazonium: with 100 part 3,6,8-trisulfonic acid-2-naphthylamines dry product is pulled an oar with ice, adds the hydrochloric acid of proportioning 1-1.5 then, adds inferior sodium solution and carries out diazonium, and temperature is controlled to be 0-10 ℃.
Coupling: 100 parts of m-aminophenyl amine acetylize hydrochlorides are joined in the above-mentioned diazonium thing carry out coupling, pH value 4-7, temperature 5-10 ℃.
Primary condensation: 105 parts of cyanuric chlorides are iced mill about-2-2 ℃, add above-mentioned coupling material then and carry out primary condensation, controlled temperature 5-15 ℃, pH value 5-7.
The para-ester diazo coupling: 85 parts are pulled an oar under the condition that ice exists to (beta-sulfuric ester ethyl sulfonyl) aniline dry product, add the hydrochloric acid that proportioning is 1-1.5 then, receive solution with the Asia and carry out diazonium, diazonium finishes to add 2,4-disulfonic acid aniline carries out coupling.
The secondary condensation: the primary condensation material is added in the above-mentioned coupling material, carries out the secondary condensation, controlled temperature 40-60 ℃, pH value 6-8, be reacted to pH value basicly stable after, filter caudacoria with pressure filter and handle, the back stdn is done in spray.
Embodiment 2, when reference example 1, two contracts, the coupling solution of 95 parts of para-ester diazonium salts and 2,4-disulfonic acid aniline carried out the secondary condensation, control PH=7-9, and temperature 40-60 ℃, reaction finishes the back spray and does stdn.
Embodiment 3, and composite reactive yellow is made up of 90 parts of reactive yellow SHE monomers, 1 part of dust-proofing agent, 9 parts of Sodium sulfate anhydrous.min(99).
Embodiment 4, and composite reactive yellow is made up of 80 parts of reactive yellow SHE monomers, 2 parts of dust-proofing agents, 18 parts of Sodium sulfate anhydrous.min(99).
Embodiment 5, and composite reactive yellow is made up of 75 parts of reactive yellow SHE monomers, 5 parts of dust-proofing agents, 20 parts of Sodium sulfate anhydrous.min(99).
Claims (6)
1. reactive yellow SHE monomer is characterized in that structural formula is:
2. the monomeric synthetic method of reactive yellow SHE; it is characterized in that with 3; 6; the diazonium thing of 8-trisulfonic acid-2-naphthylamines and the coupling of m-aminophenyl amine acetylize hydrochloride; again with the cyanuric chloride primary condensation; carry out the secondary condensation with coupling solution to (beta-sulfuric ester ethyl sulfonyl) diazonium salt of aniline and 2,4-disulfonic acid aniline then, spray is done.
3. synthetic method according to claim 2 when it is characterized in that using coupling solution to (beta-sulfuric ester ethyl sulfonyl) diazonium salt of aniline and 2,4-disulfonic acid aniline to carry out the secondary condensation, is 0.8-1.0 to the proportioning of (beta-sulfuric ester ethyl sulfonyl) aniline.
4. according to claim 2 or 3 described synthetic methods, it is characterized in that the parameter of control is when contracting with two: PH=6-9, temperature 40-60 ℃.
5. synthetic method according to claim 4, it is characterized in that two after contracting solution by film handle the back directly spray do and promptly get monomer reactivity Huang SHE finished product.
6. composite reactive yellow dye is characterized in that weight consists of: reactive yellow SHE monomer 70～95%, dust-proofing agent 1～5%, Sodium sulfate anhydrous.min(99) 5～30%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410014846 CN1569969A (en) | 2004-04-30 | 2004-04-30 | Active yellow SHE, synthetic method and its composite active yellow dye |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410014846 CN1569969A (en) | 2004-04-30 | 2004-04-30 | Active yellow SHE, synthetic method and its composite active yellow dye |
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| Publication Number | Publication Date |
|---|---|
| CN1569969A true CN1569969A (en) | 2005-01-26 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CN 200410014846 Pending CN1569969A (en) | 2004-04-30 | 2004-04-30 | Active yellow SHE, synthetic method and its composite active yellow dye |
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| CN (1) | CN1569969A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1321159C (en) * | 2005-07-26 | 2007-06-13 | 江苏申新染料化工股份有限公司 | Active yellow dye and its built brown active dye |
| CN102876078A (en) * | 2012-10-29 | 2013-01-16 | 上海雅运纺织化工股份有限公司 | Yellow reactive dye compound and applications thereof to synthesis and dyeing |
-
2004
- 2004-04-30 CN CN 200410014846 patent/CN1569969A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1321159C (en) * | 2005-07-26 | 2007-06-13 | 江苏申新染料化工股份有限公司 | Active yellow dye and its built brown active dye |
| CN102876078A (en) * | 2012-10-29 | 2013-01-16 | 上海雅运纺织化工股份有限公司 | Yellow reactive dye compound and applications thereof to synthesis and dyeing |
| CN102876078B (en) * | 2012-10-29 | 2016-10-05 | 苏州科法曼化学有限公司 | Reactive yellow compound and synthesis thereof and tint applications |
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