CN102516796A - Preparation method for vulcanized reactive dye - Google Patents
Preparation method for vulcanized reactive dye Download PDFInfo
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- CN102516796A CN102516796A CN2011103704120A CN201110370412A CN102516796A CN 102516796 A CN102516796 A CN 102516796A CN 2011103704120 A CN2011103704120 A CN 2011103704120A CN 201110370412 A CN201110370412 A CN 201110370412A CN 102516796 A CN102516796 A CN 102516796A
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Abstract
The invention discloses a preparation method for vulcanized reactive dye, which comprises the following steps: under the condition that 2,4-dinitrochlorobenzene and sodium hydroxide solution are near boiling, hydrolyzing to prepare the dinitrophenol sodium solution; then, heating and boiling the dinitrophenol sodium solution with sodium polysulfide aqueous solution at a certain molecular ratio; under the condition of pressurization or non pressurization, reducing and carrying out sulphureting reaction to prepare; after sulphureting reaction is finished, drying directly by a roller drier to obtain raw dye; and splicing and mixing to obtain commodity dye. The preparation method for the vulcanized reactive dye has the beneficial effect that sodium sulfide or sodium hydrosulfite is used for reducing into a water-soluble leuco body when the vulcanized dye is used, and the water-soluble leuco body is adsorbed by a dyed object to be changed into the original insoluble colored object by the oxidation or other actions to fix the dye on the dyed object.
Description
Technical field
The present invention relates to garment industry, specially refer to a kind of preparation method of sulphur vat dye.
Background technology
Thioxine dyes is to be mainly used in cotton fiber dyeing with Sodium Sulphide dissolved dyestuff, also can be used for cotton/dimension BLENDED FABRIC.With low cost, dying article generally still can washable sun-proof, but color and luster is bright-coloured inadequately.Kind commonly used has SULPHUR BLACK CRUDE, SULPHUR BLUE BRN 150 etc.Now existing soluble fulfur dye comes out.By amine, phenols or the nitro thing of aromatic hydrocarbons and sulphur or sodium polysulphide through the dyestuff that vulcanization reaction generates, be the french chemist clusianone high with mine-laying Tong Niai synthetic at first.
Application number is that 96110039 patent application document discloses a kind of new thioxine dyes, in its preparation, comprises the thioxine dyes midbody of at least a formula I; Wherein R ↓ ［ 1 ］ and R are nitro, nitroso-group or amino independently, and this dyestuff can be selected from the aldehyde by (A) through in its preparation, adding; (B) urea; (C) benzoquinones or naphthoquinones; (D) at least a properties-correcting agent of the group of monoethanolamine composition is produced, or produces through handling the thioxine dyes (in its preparation, containing this type of midbody) that has made with at least a aldehyde (A), benzaldehyde or naphthoquinones (C) or monoethanolamine (D).
Summary of the invention
The technical problem that the present invention mainly solves provides a kind of preparation method of sulphur vat dye, can solve some problems that exist in the traditional dress dyestuff.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: a kind of preparation method of sulphur vat dye is provided, and said preparation method is with 2; 4-DNCB and sodium hydroxide solution are under nearly ebullient situation; The dinitrophenol(DNP) sodium solution is processed in hydrolysis, subsequently with aqueous sodium polysulfide by certain molecular ratio heated and boiled, in pressurization or do not add to depress to reduce and add reaction of Salmon-Saxl and produce; After adding the reaction of Salmon-Saxl completion; Directly dry with roller letter moisture eliminator, obtain former dyestuff, be commercial dye through piecing together to blend together again.
In one embodiment of the invention, said sulphur vat dye is processed by all the components uniform mixing.
In one embodiment of the invention, the color of said sulphur vat dye is a black, and is red or yellow.
Beneficial effect of the present invention is: will be absorbed after oxidation or other effects become original insoluble colored substance again, so that dyestuff is bonded on the pollutant by pollutant with sodium sulphite or vat powder reduction becoming water-soluble leuco body when thioxine dyes uses again.
Embodiment
The preparation method of a kind of sulphur vat dye of the present invention; It is with 2; 4-DNCB and sodium hydroxide solution are under nearly ebullient situation; The dinitrophenol(DNP) sodium solution is processed in hydrolysis, subsequently with aqueous sodium polysulfide by certain molecular ratio heated and boiled, in pressurization or do not add to depress to reduce and add reaction of Salmon-Saxl and produce.After adding the reaction of Salmon-Saxl completion, directly use roller letter moisture eliminator dry, obtain former dyestuff.Be commercial dye through piecing together to blend together again.During sulfuration, phenol sodium and the molecular ratio of sodium polysulphide, the x (being the sulphur index) among the sodium polysulphide Na2Sx and temperature of reaction is different make the coloured light of SULPHUR BLACK CRUDE finished product that the difference of blue or green light, blue or green ruddiness and ruddiness arranged.The maximum shortcoming of black sulfide dye is that crisp cloth phenomenon is arranged.This is because contain many sulphur catenate active sulphur in the SULPHUR BLACK CRUDE molecule.The sulphur of this composition is unstable, when with the dyestuff heating or when being positioned in the damp and hot air, just is prone to oxidation and generates sulfuric acid, causes tendering to cotton.Through improving the production technique of SULPHUR BLACK CRUDE, after processing, common SULPHUR BLACK CRUDE is cooled to about 100 ℃, add formaldehyde and monochloroacetic acid, make that unsettled sulphur settles out in the dyestuff, process a kind of brittle resistance sulphur black dyestuff.
Beneficial effect of the present invention is: will be absorbed after oxidation or other effects become original insoluble colored substance again, so that dyestuff is bonded on the pollutant by pollutant with sodium sulphite or vat powder reduction becoming water-soluble leuco body when thioxine dyes uses again.
The above is merely embodiments of the invention; Be not so limit claim of the present invention; Every equivalent structure or equivalent flow process conversion that utilizes description of the present invention to do; Or directly or indirectly be used in other relevant technical fields, all in like manner be included in the scope of patent protection of the present invention.
Claims (3)
1. the preparation method of a sulphur vat dye is characterized in that, said preparation method is with 2; 4-DNCB and sodium hydroxide solution are under nearly ebullient situation, and the dinitrophenol(DNP) sodium solution is processed in hydrolysis, press certain molecular ratio heated and boiled with aqueous sodium polysulfide subsequently; In pressurization or do not add to depress to reduce and add reaction of Salmon-Saxl and produce, after adding reaction of Salmon-Saxl and accomplishing, directly use roller letter moisture eliminator dry; Obtain former dyestuff, be commercial dye through piecing together to blend together again.
2. the preparation method of a kind of sulphur vat dye according to claim 1 is characterized in that, said sulphur vat dye is processed by all the components uniform mixing.
3. the preparation method of a kind of sulphur vat dye according to claim 1 is characterized in that, the color of said sulphur vat dye is a black, and is red or yellow.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103704120A CN102516796A (en) | 2011-11-21 | 2011-11-21 | Preparation method for vulcanized reactive dye |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103704120A CN102516796A (en) | 2011-11-21 | 2011-11-21 | Preparation method for vulcanized reactive dye |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102516796A true CN102516796A (en) | 2012-06-27 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011103704120A Pending CN102516796A (en) | 2011-11-21 | 2011-11-21 | Preparation method for vulcanized reactive dye |
Country Status (1)
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| CN (1) | CN102516796A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106221277A (en) * | 2016-07-26 | 2016-12-14 | 萧县凯奇化工科技有限公司 | A kind of black vat dye and preparation method thereof |
| CN111100475B (en) * | 2020-01-08 | 2022-02-18 | 山西临汾染化(集团)有限责任公司 | Preparation method of sulfur dye |
| CN115011140A (en) * | 2022-06-28 | 2022-09-06 | 石家庄腾辉化工有限公司 | High-yield vulcanized black processing technology |
-
2011
- 2011-11-21 CN CN2011103704120A patent/CN102516796A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106221277A (en) * | 2016-07-26 | 2016-12-14 | 萧县凯奇化工科技有限公司 | A kind of black vat dye and preparation method thereof |
| CN111100475B (en) * | 2020-01-08 | 2022-02-18 | 山西临汾染化(集团)有限责任公司 | Preparation method of sulfur dye |
| CN115011140A (en) * | 2022-06-28 | 2022-09-06 | 石家庄腾辉化工有限公司 | High-yield vulcanized black processing technology |
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| PB01 | Publication | ||
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20120627 |