CN102311663A - Nylon yellow reactive dye and preparation method thereof - Google Patents
Nylon yellow reactive dye and preparation method thereof Download PDFInfo
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- CN102311663A CN102311663A CN201110189862A CN201110189862A CN102311663A CN 102311663 A CN102311663 A CN 102311663A CN 201110189862 A CN201110189862 A CN 201110189862A CN 201110189862 A CN201110189862 A CN 201110189862A CN 102311663 A CN102311663 A CN 102311663A
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- 0 *c(c(*=*c(ccc1cc(N)ccc11)c1N=O)c1)cc(*)c1N=O Chemical compound *c(c(*=*c(ccc1cc(N)ccc11)c1N=O)c1)cc(*)c1N=O 0.000 description 1
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Abstract
The invention relates to a nylon yellow reactive dye of the following molecular structure and a preparation method thereof. The nylon yellow reactive dye has the advantages of bright-colored and beautiful colored light, excellent wet fastnesses, extremely high inhalation rate and lifting rate, and simple operation.
Description
Technical field
The present invention relates to a kind of reactive dyestuffs and preparation method thereof, yellow reactive dyestuffs of especially a kind of nylon and preparation method thereof.
Background technology
Generally dye the used dyestuff of nylon now and be matching stain and weak acid dye.Because not good enough with the wet fastness of nylon each item that matching stain dyed, coloured light is not very gorgeous, clean absorption rate is low, and the dyeing liquid waste concentration is high, pollutes to environment.Get into 21 century, because the restriction of environmental ecology, for dye uptake, requiring of degree of fixation and dyeing waste liquid is increasingly high, and matching stain can not satisfy the dyeing nylon demand.The present invention provides one type of nonmetal complexdyes, and is better to dyeing nylon.
Summary of the invention
Technical problem to be solved by this invention provides one can reduce environmental pollution; The desired raw material cost is low, and beautiful in colour, each item fastness (wet rub, soap, alkali sweat, sour sweat, washing) excellent performance that wets; Easy to use, yellow reactive dyestuffs of nylon that suitability is strong and preparation method thereof.
In order to solve the problems of the technologies described above, the technical scheme that the present invention adopts is: the yellow reactive dyestuffs of a kind of nylon, the molecular structure of these reactive dyestuffs are suc as formula (I): shown in
R in the formula
1Be following structural formula (R
1-1) to structural formula (R
1-4) any substituting group:
Preferably, these reactive dyestuffs possess following structural formula:
The present invention also provides a kind of preparation method of above-mentioned Yellow active dye, comprises the steps:
A, 2,4-diamino benzene sulfonic acid sodium acetylize: in retort, add water, add 2 then; 4-diamino benzene sulfonic acid sodium stirs, and transfers pH=9 with yellow soda ash; Temperature is controlled at 35 ℃, and (below the liquid level) adds acetic anhydride under the liquid, and acetic anhydride dropwises; React after 30 minutes, get 2,4-diamino benzene sulfonic acid sodium acetylate reaction solution.Subsequent use;
B, diazotization reaction: in retort, add water, add 2-naphthylamines-6-beta-hydroxyethyl sulfonyl sulfuric ester-1-sulfonic acid then, stir, add trash ice; Temperature is controlled at 0 ℃, adds 30% hydrochloric acid, adds 30% sodium nitrite solution again, at temperature 6-8 ℃; Reacted 2 hours, it is blue that reaction process is guaranteed to be after congo-red test paper soaks all the time, is little blueness after the KI test paper soaks; Reaction finishes and removes the residue Sodium Nitrite with thionamic acid, gets doazo reaction liquid, and is subsequent use;
C, coupled reaction: the doazo reaction liquid with the b step obtains, be added drop-wise to 2 of step a, in the 4-diamino benzene sulfonic acid sodium acetylate reaction solution, stir.Transfer pH=8 with yellow soda ash simultaneously, be warming up to 15 ℃, reacted 3 hours, reaction finishes.Filter, get coupled reaction liquid, be i.e. the yellow reactive dyestuffs of nylon.
Preferably, method of the present invention can also comprise steps d:
D is refining:
With adding sodium-chlor in the yellow reactive dyestuffs feed liquid of c step gained nylon, make dyestuff separate out, again precipitate is joined in the solid-liquid separator, separate, collect filter cake, weigh, analyze content, subsequent use;
Preferably, method of the present invention can also comprise step e:
E is dry: with d step filter cake, dry, pulverize;
Preferably, method of the present invention can also comprise step f:
F adjustment coloured light and intensity:
With the dyeing of e step material, carry out coloured light, intensity adjustment according to coloration result again;
Preferably, method of the present invention can also comprise step g:
G finished product packing: the article of f step gained are packed.
Among the above-mentioned preparation method, the structural formula of 2-naphthylamines-6-beta-hydroxyethyl sulfonyl sulfuric ester-1-sulfonic acid is:
The beneficial effect that the present invention had:
The yellow reactive dyestuffs of nylon of the present invention have bright-coloured beautiful coloured light, and each item wet fastness properties is very superior, very high inspiration rate and lifting rate, and also easy and simple to handle.
Yellow active dye of the present invention in dyeing nylon, is compared with matching stain, no matter is each item fastness, all is excellent to the environment protection aspect still.
Embodiment
For specifying technical scheme of the present invention, enumerate embodiment below and specify technical scheme of the present invention, this embodiment does not form any restriction of the present invention.
Embodiment 1
A kind of Yellow active dye has following structural formula:
The preparation method of above-mentioned Yellow active dye comprises the steps:
A, 2,4-diamino benzene sulfonic acid sodium acetylize: in retort, add 1100 liters in water, add 2 then; 4-diamino benzene sulfonic acid sodium 300kg stirs, and transfers pH=9 with yellow soda ash; Temperature is controlled at 35 ℃, and (below the liquid level) adds acetic anhydride 90Kg under the liquid, and acetic anhydride dropwises; React after 30 minutes, get 2,4-diamino benzene sulfonic acid sodium acetylate reaction solution.Subsequent use;
B, 2-naphthylamines-6-beta-hydroxyethyl sulfonyl sulfuric ester-1-sulfonic acid diazotization reaction: in retort, add 1500 liters in water, add 2-naphthylamines-6-beta-hydroxyethyl sulfonyl sulfuric ester-1-sulfonic acid of 240kg then, stir, add trash ice, temperature is controlled at 0 ℃.The hydrochloric acid 267kg of adding 30% adds 30% sodium nitrite solution 240kg, again at temperature 6-8 ℃; Reacted 2 hours; It is blue that reaction process is guaranteed to be after congo-red test paper soaks all the time, is little blueness after the KI test paper soaks, and reaction finishes and removes the residue Sodium Nitrite with thionamic acid; Get doazo reaction liquid, subsequent use;
C, coupled reaction: the doazo reaction liquid with the b step obtains, be added drop-wise to 2 of step a, in the 4-diamino benzene sulfonic acid sodium acetylate reaction solution, stir.Transfer pH=8 with yellow soda ash simultaneously, be warming up to 15 ℃, reacted 3 hours, reaction finishes.Filter, get coupled reaction liquid, i.e. Yellow active dye.
D is refining:
With adding sodium-chlor in the c step gained Yellow reactive dyes feed liquid, make dyestuff separate out, again precipitate is joined in the solid-liquid separator, separate, collect filter cake, weigh, analyze content, subsequent use;
E is dry: with d step filter cake, dry, pulverize;
F adjustment coloured light and intensity:
With the dyeing of e step material, carry out coloured light, intensity adjustment according to coloration result again;
G finished product packing: the article of f step gained are packed.
Preparing method of the present invention, the yellow reactive dyestuffs of prepared nylon have bright-coloured beautiful coloured light, and each item wet fastness properties is very superior, very high inspiration rate and lifting rate, and also easy and simple to handle.
The dyeing behavior data of the yellow reactive dyestuffs of nylon of the method preparation of embodiment 1 are following:
Table one: Yellow active dye performance, quality index
Table two: performance index contrast
Dyestuff of the present invention and dyestuff preparation method are described through concrete 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 the present invention; 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 all to be regarded as and are included within the scope of the present invention.
Claims (3)
1. yellow reactive dyestuffs of a nylon is characterized in that: the molecular structure of these reactive dyestuffs is suc as formula (I): shown in
R in the formula
1Be following structural formula (R
1-1) to structural formula (R
1-4) any substituting group:
2. a kind of Yellow active dye according to claim 1 is characterized in that: the molecular structural formula of these reactive dyestuffs is:
3. the preparation method of claim 1 or 2 described Yellow active dyes is characterized in that: comprise the steps:
A, 2,4-diamino benzene sulfonic acid sodium acetylize: in retort, add water, add 2 then, 4-diamino benzene sulfonic acid sodium; Stir, transfer pH=9 with yellow soda ash, temperature is controlled at 35 ℃; Liquid adds acetic anhydride down, and acetic anhydride dropwises, and reacts after 30 minutes; Get 2,4-diamino benzene sulfonic acid sodium acetylate reaction solution, subsequent use;
B, diazotization reaction: in retort, add water, add 2-naphthylamines-6-beta-hydroxyethyl sulfonyl sulfuric ester-1-sulfonic acid then, stir, add trash ice; Temperature is controlled at 0 ℃, adds 30% hydrochloric acid, adds 30% sodium nitrite solution again, at temperature 6-8 ℃; Reacted 2 hours, it is blue that reaction process is guaranteed to be after congo-red test paper soaks all the time, is little blueness after the KI test paper soaks; Reaction finishes and removes the residue Sodium Nitrite with thionamic acid, gets doazo reaction liquid, and is subsequent use;
C, coupled reaction: the doazo reaction liquid with the b step obtains, be added drop-wise to 2 of step a, in the 4-diamino benzene sulfonic acid sodium acetylate reaction solution, stir.Transfer pH=8 with yellow soda ash simultaneously, be warming up to 15 ℃, reacted 3 hours, reaction finishes, and filters, and gets coupled reaction liquid, i.e. the yellow reactive dyestuffs of nylon;
Preferably, method of the present invention can also comprise steps d:
D is refining:
With adding sodium-chlor in the yellow reactive dyestuffs feed liquid of c step gained nylon, make dyestuff separate out, again precipitate is joined the solid-liquid branch
In device, separate, collect filter cake, weigh, analyze content, subsequent use;
Preferably, method of the present invention can also comprise step e:
E is dry: with d step filter cake, dry, pulverize;
Preferably, method of the present invention can also comprise step f:
F adjustment coloured light and intensity:
With the dyeing of e step material, carry out coloured light, intensity adjustment according to coloration result again;
Preferably, method of the present invention can also comprise step g:
G finished product packing: the article of f step gained are packed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110189862A CN102311663A (en) | 2011-07-07 | 2011-07-07 | Nylon yellow reactive dye and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110189862A CN102311663A (en) | 2011-07-07 | 2011-07-07 | Nylon yellow reactive dye and preparation method thereof |
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| CN102311663A true CN102311663A (en) | 2012-01-11 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201110189862A Pending CN102311663A (en) | 2011-07-07 | 2011-07-07 | Nylon yellow reactive dye and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4703112A (en) * | 1981-08-31 | 1987-10-27 | Hoechst Aktiengesellschaft | Water-soluble benzothiazole-azo- and phenyl-azo-compounds containing a 2-sulfo-5-acylamino-aniline coupling component, suitable as fibre-reactive dyestuffs |
| CN1861695A (en) * | 2006-06-19 | 2006-11-15 | 湖北华丽染料工业有限公司 | Yellow ozo dye mixture and its use |
| CN101481527A (en) * | 2008-12-12 | 2009-07-15 | 天津市德凯化工有限公司 | Red reactive dye for fur and preparation thereof |
| CN101633796A (en) * | 2009-08-17 | 2010-01-27 | 浙江劲光化工有限公司 | Composite active black dye |
-
2011
- 2011-07-07 CN CN201110189862A patent/CN102311663A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4703112A (en) * | 1981-08-31 | 1987-10-27 | Hoechst Aktiengesellschaft | Water-soluble benzothiazole-azo- and phenyl-azo-compounds containing a 2-sulfo-5-acylamino-aniline coupling component, suitable as fibre-reactive dyestuffs |
| CN1861695A (en) * | 2006-06-19 | 2006-11-15 | 湖北华丽染料工业有限公司 | Yellow ozo dye mixture and its use |
| CN101481527A (en) * | 2008-12-12 | 2009-07-15 | 天津市德凯化工有限公司 | Red reactive dye for fur and preparation thereof |
| CN101633796A (en) * | 2009-08-17 | 2010-01-27 | 浙江劲光化工有限公司 | Composite active black dye |
Non-Patent Citations (2)
| Title |
|---|
| 张兴华 等: ""浅谈活性染料结构与性能的关系"", 《染料与染色》 * |
| 杨振梅: ""黄色活性染料结构与性能的关系及其拼混增效的探讨"", 《染料与染色》 * |
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Application publication date: 20120111 |
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