CN1297001A - Disperse blud dye and its synthetic process and application - Google Patents
Disperse blud dye and its synthetic process and application Download PDFInfo
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- CN1297001A CN1297001A CN 00131205 CN00131205A CN1297001A CN 1297001 A CN1297001 A CN 1297001A CN 00131205 CN00131205 CN 00131205 CN 00131205 A CN00131205 A CN 00131205A CN 1297001 A CN1297001 A CN 1297001A
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Abstract
A disperse blue dye is prepared through dissolving the 3-amino-5-nitro-2,1-benzoisothiazole in concentrated sulfuric acid, adding it dropwise to the solution of soldium nitrite in concentrated sulfuric acid for diazotization, coupling with the solution of m-diethylamino phenol in acetic acid to separate out crystal, negative-pressure filtering, and water washing to pH=6-7. Its advantages are high yield (higher than 92%), high purity (higher than 97%), gay colour, good dispersity and low cost.
Description
The present invention relates to blue dyestuff of a kind of dispersion and synthetic method thereof, purposes, the blue dyestuff of dispersion of the present invention belongs to field of fine chemical, and it is applicable to the dyeing and the stamp of terylene and blending thereof, also is applicable to the dyeing of cellulose acetate, polyamide fibre and acrylic fibers.
The early 1990s in this century, the government of some developed countries of west has issued that forbidding can decomposite the decree of the azoic dyestuff of aromatic amine under special conditions, and this brings certain negative impact to the azoic dyestuff of China and the outlet of intermediate.3-amino-5-nitro-2,1 benzisothiazole (BIT) [Wang Jiaru, Li Muji, Yang Lingxiao etc., " dyestuffs industries " 1986 (4) 80] the azo dispersion dyes nontoxicity, and coloured light is gorgeous, good dispersity, every fastness such as sun-proof, washable, perspiration resistance are good, easy to use, both be fit to pad-dry-cure dyeing, also be fit to high-temperature pressure dyeing, cost is low, has good application prospects.Both at home and abroad the structure of this dyestuff, synthetic, performance, use all there is not report.
The objective of the invention is to: in order to adapt to the ban that bans use of the azoic dyestuff that contains aromatic amine, seek a kind of avirulent azo dispersion dyes, and provide a kind of coloured light gorgeous, good dispersity, every fastness such as sun-proof, washable, perspiration resistance are good, and cost is low, both are fit to pad-dry-cure dyeing, be fit to the blue dyestuff of dispersion of the SE type of high-temperature pressure dyeing again, and a kind of synthetic method easy, that productive rate content is high of synthesizing is provided.
The present invention realizes by following step: the synthetic of this dyestuff is a certain amount of 3-amino-5-nitro-2,1 benzisothiazole (BIT) is dissolved in the vitriol oil, be added drop-wise to then in the sulphuric acid soln of Sodium Nitrite and carry out diazotization, again with the acetum coupling of m-diethylaminophenol.After separating out crystallization, negative pressure filtration, washing product are to PH=6-7, and productive rate＞92% is analyzed purity 〉=97% through HPLC.
The molecular structural formula of the blue dyestuff of dispersion of the present invention:
A certain amount of BIT is joined in 98% vitriol oil of 3.8～4.8 times of weight, heating in water bath, stirring and dissolving: in another container, add 98% vitriol oil of 5.5-6.5 times of weight of Sodium Nitrite amount, slowly add and the equimolar Sodium Nitrite of BIT then, after the dissolving, the ice bath cooling, when temperature be chilled to＜5 ℃, the concentrated sulfuric acid solution of BIT is slowly added, after adding, stir 2.0-2.5h down at 5-10 ℃, diazotization is finished.
Take by weighing with the equimolar m-diethylaminophenol of BIT and be dissolved in 25% acetic acid of 5-6 times of weight, add the water of 8-10 times of weight again, the cooling of reactor ice bath, when temperature＜5 ℃, drip the BIT diazotization liquid that has prepared, in the dropping process, temperature＜10 ℃, stir 2.0-2.5h down at 0-5 ℃ after a while, place 10h under the room temperature, crystallization is separated out, negative pressure filtration, the washing product is to PH=6-7, get blue black coccoid product, productive rate＞92%, purity 〉=97%.
Advantage of the present invention:
The invention provides a kind of blue dyestuff of dispersion of every excellent property, product detects through Tianjin dyestuff institute, and the result is as follows: soap 5 grades 204 ℃ of 90.5% 5 grades of 5 grades of 4-5 levels of 5 grades of A/5 levels of water logging friction distillation optimum hot melting temperature of the dispersed dye uptake of diffustivity
Their examining report is pointed out: " this dyestuff lovely luster; dynamics height; cost lower (can reach the substandard of existing market raw materials cost); fastness is good; belong to megathermal dispersed dye, and in the dyeing of High Temperature High Pressure, can obtain power branch preferably simultaneously, so this dyestuff both had been fit to High Temperature High Pressure; be fit to pad-dry-cure dyeing again, meet the SE type and disperse.This dyestuff is rising, and its advantage is bright in colour, the dynamics height, and cost is low, and fastness is good.It is rare to be that current dispersed dye have both above effect simultaneously." performance of this dyestuff is better than the blue dyestuff H-GL of commercially available dispersion.
The present invention both provided and had disperseed blue dyestuff new variety, also provided this dyestuff simple and practical synthetic method simultaneously, and productive rate is up to 92%, purity 〉=96%.It is applicable to the dyeing and the stamp of terylene and blending thereof, also is applicable to the dyeing of cellulose acetate, polyamide fibre and acrylic fibers.
Embodiment:
A certain amount of BIT is joined in 98% the sulfuric acid of 4 times of amounts, heating in water bath, stirring and dissolving, 6 times 98% sulfuric acid of adding Sodium Nitrite amount slowly adds and the equimolar Sodium Nitrite of BIT then in another container, after the dissolving, ice bath cooling when temperature＜5 ℃, adds the sulphuric acid soln of BIT, stir 2.0h down at 5-10 ℃, diazotization is finished.Take by weighing with the equimolar m-diethylaminophenol of BIT and be dissolved in 25% acetic acid of 5.5 times of amounts, add the water of 9 times of amounts again, the ice bath cooling reactor, when temperature＜5 ℃, drip diazonium liquid, in the dropping process, temperature≤10 ℃ then, are stirred 2h down at 0-5 ℃, place 10h under the room temperature, crystallization is separated out, negative pressure filtration, and the washing product gets blue black coccoid product to PH=6-7, productive rate 92%, purity 〉=97%.
Claims (3)
1. one kind is disperseed blue dyestuff, and it is characterized in that: this disperses the molecular structural formula of blue dyestuff to be
2. the synthetic method of the blue dyestuff of the described dispersion of claim 1, it is characterized in that: with a certain amount of 3-amino-5-nitro-2,1 benzisothiazole is that BIT joins in 98% vitriol oil of 3.8～4.8 times of weight heating in water bath, stirring and dissolving; 98% vitriol oil that in another container, adds 5.5-6.5 times of weight of Sodium Nitrite amount, slowly add and the equimolar Sodium Nitrite of BIT then, after the dissolving, the ice bath cooling, when temperature be chilled to＜5 ℃, the concentrated sulfuric acid solution of BIT is slowly added, after adding, stir 2.0-2.5h down at 5-10 ℃, diazotization is finished; Then take by weighing with the equimolar m-diethylaminophenol of BIT and be dissolved in 25% acetic acid of 5-6 times of weight, the water that adds 8-10 times of weight again, reactor ice bath cooling is when temperature＜5 ℃, drip the BIT diazotization liquid that has prepared, in the dropping process, temperature＜10 ℃ are stirred 2.0-2.5h down at 0-5 ℃ after a while, place 10h under the room temperature, crystallization is separated out, negative pressure filtration, and the washing product gets blue black coccoid product to PH=6-7.
3. the purposes of claim 1 or the blue dyestuff of 2 described dispersions, it is characterized in that: the range of application of dyestuff of the present invention is that it is applicable to the dyeing and the stamp of terylene, blending, also is applicable to the dyeing of cellulose acetate, polyamide fibre and acrylic fibers.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00131205A CN1108346C (en) | 2000-12-04 | 2000-12-04 | Disperse blud dye and its synthetic process and application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN00131205A CN1108346C (en) | 2000-12-04 | 2000-12-04 | Disperse blud dye and its synthetic process and application |
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| Publication Number | Publication Date |
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| CN1297001A true CN1297001A (en) | 2001-05-30 |
| CN1108346C CN1108346C (en) | 2003-05-14 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN00131205A Expired - Fee Related CN1108346C (en) | 2000-12-04 | 2000-12-04 | Disperse blud dye and its synthetic process and application |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101054477B (en) * | 2007-05-18 | 2010-05-26 | 浙江龙盛染料化工有限公司 | Dispersion dyes composition |
| CN101067050B (en) * | 2007-06-01 | 2010-08-18 | 浙江龙盛染料化工有限公司 | Disperse black dye composition |
| CN101081838B (en) * | 2006-12-21 | 2010-12-15 | 浙江龙盛集团股份有限公司 | Benzo isothiazole compound, preparation and application and disperse dyes composition |
| CN102070552A (en) * | 2010-12-23 | 2011-05-25 | 浙江吉华集团有限公司 | Method for preparing 3-amino-5-nitro-2,1-benzisothiazole and diazonium salt thereof |
| CN102161839A (en) * | 2011-02-24 | 2011-08-24 | 浙江万丰化工有限公司 | Composition of disperse dyes |
| CN102924960A (en) * | 2012-11-29 | 2013-02-13 | 南京大学 | Benzo isothiazole azo pyrazolone disperse dye as well as preparation method and use thereof |
| CN103073918A (en) * | 2013-01-21 | 2013-05-01 | 江苏亚邦染料股份有限公司 | Medium temperature type three-primary-color disperse dyes |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19523924A1 (en) * | 1995-06-30 | 1997-01-02 | Hoechst Ag | Nitrobenzisothiazole azo dye |
-
2000
- 2000-12-04 CN CN00131205A patent/CN1108346C/en not_active Expired - Fee Related
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101081838B (en) * | 2006-12-21 | 2010-12-15 | 浙江龙盛集团股份有限公司 | Benzo isothiazole compound, preparation and application and disperse dyes composition |
| CN101054477B (en) * | 2007-05-18 | 2010-05-26 | 浙江龙盛染料化工有限公司 | Dispersion dyes composition |
| CN101067050B (en) * | 2007-06-01 | 2010-08-18 | 浙江龙盛染料化工有限公司 | Disperse black dye composition |
| CN102070552A (en) * | 2010-12-23 | 2011-05-25 | 浙江吉华集团有限公司 | Method for preparing 3-amino-5-nitro-2,1-benzisothiazole and diazonium salt thereof |
| CN102070552B (en) * | 2010-12-23 | 2012-11-28 | 浙江吉华集团股份有限公司 | Method for preparing 3-amino-5-nitro-2,1-benzisothiazole and diazonium salt thereof |
| CN102161839A (en) * | 2011-02-24 | 2011-08-24 | 浙江万丰化工有限公司 | Composition of disperse dyes |
| CN102161839B (en) * | 2011-02-24 | 2013-05-29 | 浙江万丰化工有限公司 | Composition of disperse dyes |
| CN102924960A (en) * | 2012-11-29 | 2013-02-13 | 南京大学 | Benzo isothiazole azo pyrazolone disperse dye as well as preparation method and use thereof |
| CN103073918A (en) * | 2013-01-21 | 2013-05-01 | 江苏亚邦染料股份有限公司 | Medium temperature type three-primary-color disperse dyes |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1108346C (en) | 2003-05-14 |
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