CN101205415A - Synthetic process of vat blue RSN - Google Patents
Synthetic process of vat blue RSN Download PDFInfo
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- CN101205415A CN101205415A CNA2007101912334A CN200710191233A CN101205415A CN 101205415 A CN101205415 A CN 101205415A CN A2007101912334 A CNA2007101912334 A CN A2007101912334A CN 200710191233 A CN200710191233 A CN 200710191233A CN 101205415 A CN101205415 A CN 101205415A
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- aminoanthraquinone
- vat blue
- blue rsn
- dmi
- synthetic process
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Abstract
The invention belongs to the dye processing technology field, in particular to a new synthesis technology for a vat blue RSN dye. The invention utilizes a new solvent for condensation reaction, realizes one step reaction without the prior processes of refinement and oxidation, and obtains high purity vat blue RSN raw dye with high yield; the yield of the prior technology only reaches 70 percent, while the yield of the new technology with one step condensation reaction can reach over 90 percent, which not only greatly reduces production cost and improves product quality, but also tremendously reduces pollution and emission of three wastes.
Description
Technical field
The invention belongs to the dyestuff processing technique field, particularly a kind of Vat Blue RSN dyestuff new synthetic process.
Background technology
At present in the dyestuff processing industry, its traditional processing technology is: condensation reaction: the 1-aminoanthraquinone, dimethyl sulfoxide (DMSO) is in the condensation still, through dissolving, heat up, the hydro-oxidation potassium solution, condensation reaction is carried out in insulation and atmospheric oxidation, dilution then, oxidation, filter-press water-washing obtains the former dyestuff of crude product Vat Blue RSN, refining reaction: the former dyestuff of crude product Vat Blue RSN is through making beating, add alkali, add vat powder, refining reaction is carried out in insulation, press filtration then, washing obtains refining former dyestuff, oxidation, acid is boiled: refining former dyestuff is through making beating, oxidation, acidification reaction, press filtration then, washing, blowing obtains the former dyestuff filter cake of Vat Blue RSN.The problem that traditional technology exists: 1, dimethyl sulfoxide (DMSO) is as the condensation solvent, and the reaction mass condensation is incomplete, and the former dye strength of generation is low, yield is low, production cost is high; 2, the condensation reaction still is little, and batch charging coefficient is low, and efficient is low, single batch amount is few; 3, the assorted dyestuff of refining step generation is many, and three-waste pollution is big; 4, reaction time long, facility investment is many, the running cost height; 5, the solvent dimethyl sulfoxide (DMSO) rate of recovery is low.
Summary of the invention
It is low to the objective of the invention is to overcome the former dyestuff yield of traditional technology, reaction time is long, the weak point that production cost is high, a kind of Vat Blue RSN dyestuff new synthetic process is provided, with the 1-aminoanthraquinone is raw material, and in a kind of synthetic solvent, alkaline condition exists down, with quaternary ammonium salt series is that phase-transfer catalyst carries out condensation, dilution, filtration and obtains the former dyestuff filter cake of Vat Blue RSN, then former dyestuff drying after additive compound, sand milling, stdn is made commercial dye.
The present invention realizes with following technical scheme: a kind of synthetic process of vat blue RSN, with the 1-aminoanthraquinone is raw material, at a kind of synthetic solvent (1,3-dimethyl-2-imidazolone 1,3-Dimethyl-2-imidazolidinone, DMI) in, alkaline condition exists down, with quaternary ammonium salt series is that phase-transfer catalyst carries out condensation, dilution, filtration and obtains the former dyestuff filter cake of Vat Blue RSN, it is characterized in that: described condensation reaction is the application in synthetic solvent DMI, is that raw material carries out condensation reaction in solvent DMI with the 1-aminoanthraquinone;
(1) described proportioning raw materials weight part: DMI usage quantity (in 1-aminoanthraquinone weight), be generally 0.5-5 part, the best is 1-3 part;
(2) alkaline condensing agent used in the present invention, potassium hydroxide or sodium hydroxide, wherein potassium hydroxide is more suitable, can be the solid or the aqueous solution, consumption (in 1-aminoanthraquinone weight): be 0.2-5 part, the best is 0.5-2 part;
(3) catalyzer used in the present invention is quaternary ammonium salt series phase-transfer catalyst, and consumption is (in a 1-aminoanthraquinone weight): the best is 0.1%-0.5%;
(4) 1-aminoanthraquinone used in the present invention is a powdery, and content is more than 〉=90%, also available wet cake.
Described synthetic process of vat blue RSN, setting-up point are 70-160 ℃.
Described synthetic process of vat blue RSN, former dyestuff drying after additive compound, sand milling, stdn makes commercial dye.
Advantage of the present invention is: the present invention utilizes novel dissolvent to carry out condensation reaction, the energy single step reaction is refining without traditional technology, the process of oxidation, obtain the former dyestuff of highly purified Vat Blue RSN with high yield, the yield of traditional technology can only reach 70%, this technology one step condensation reaction yield can reach more than 90%, not only greatly reduce former dyestuff production cost, improved quality product, and greatly reduced the pollution and the discharging of the three wastes.
Embodiment
The invention will be further described below in conjunction with embodiment:
Embodiment 1.
In the 100 gram 1-aminoanthraquinone adding 200ml solvents, Hybrid Heating is warming up to 115 ℃, drips water 15ml, is warming up to 120 ℃ of insulations 30 minutes, evenly drips the potassium hydroxide solution 100ml. for preparing then at 3 hours and is incubated 30 minutes.Be warming up to 120 ℃ of insulations 5 hours, add water isolation and filter, obtain 92 and restrain the dyestuff of giving money as a gift.(by used 1-aminoanthraquinone, yield is 92%)
Embodiment 2.
100 gram 1-aminoanthraquinone add in the 250ml solvent, and Hybrid Heating is warming up to 115 ℃, drips water 15ml, is warming up to 120 ℃ of insulations 30 minutes.Evenly drip the potassium hydroxide solution 100m1. for preparing then at 3 hours and be incubated 30 minutes.Be warming up to 130 ℃ of insulations 5 hours, add water isolation and filter, obtain 95 and restrain the dyestuff of giving money as a gift.(by used 1-aminoanthraquinone, yield is 95%)
Embodiment 3.
100 gram 1-aminoanthraquinone add in the 250ml solvent, Hybrid Heating is warming up to 120 ℃, drip water 15ml, be warming up to 120 ℃ of insulations 30 minutes, evenly dripped the potassium hydroxide solution 100ml for preparing then at 3.5 hours and be incubated 30 minutes, be warming up to 130 ℃ of insulations 5 hours, 135 ℃ of insulations 2 hours continue to heat up, add water isolation and filter, obtain 99 and restrain the dyestuff of giving money as a gift.(is 99% by used 1-aminoanthraquinone yield)
Embodiment 4.
Material with embodiment 3 carries out sand milling, commercialization processing, and 10 gram embodiment, 3 material add 25 gram auxiliary agents, and water 100ml sand milling 6 hours gets commercial dye 30 grams, and coloured light and intensity can reach the requirement of commodity processing.
The Vat Blue RSN exterior of commodity is mazarine powder or particle, former dyestuff is blue paste, water insoluble, acetic acid, pyridine, toluene, dimethylbenzene, acetone and ethanol, be slightly soluble in hot chloroform and ortho chloro phenol and the quinoline, being blue in alkaline vat powder reduced liquid, is the ruddiness blueness in acid liquid.Be brown in the vitriol oil, be blue precipitation after the dilution, its toxicity, pungency are very weak, are mainly used in the dyeing of cellulosic fibre, and yarn dyed fabric is mainly used in and dyes cotton yarn, also can be used for the direct printing of cotton, also can dye fabrics such as polyamide fibre, polyvinyl.Can use separately, also can also can be used for making pigment for printing ink in colorant match.
Claims (3)
1. synthetic process of vat blue RSN, with the 1-aminoanthraquinone is raw material, at a kind of synthetic solvent (1,3-dimethyl-2-imidazolone 1,3-Dimethyl-2-imidazolidinone, DMI) in, alkaline condition exists down, with quaternary ammonium salt series is that phase-transfer catalyst carries out condensation, dilution, filtration and obtains the former dyestuff filter cake of Vat Blue RSN, and it is characterized in that: described condensation reaction is the application in synthetic solvent DMI, is that raw material carries out condensation reaction in solvent DMI with the 1-aminoanthraquinone;
(1) described proportioning raw materials: DMI usage quantity (in 1-aminoanthraquinone weight): be generally 0.5-5 part, the best is 1-3 part;
(2) alkaline condensing agent used in the present invention, potassium hydroxide or sodium hydroxide, wherein potassium hydroxide is more suitable, can be the solid or the aqueous solution, consumption (in 1-aminoanthraquinone weight): be generally 0.2-5 part, the best is 0.5-2 part;
(3) catalyzer used in the present invention is quaternary ammonium salt series phase-transfer catalyst, and common consumption is (in a 1-aminoanthraquinone weight): the best is 0.1%-0.5%;
(4) 1-aminoanthraquinone used in the present invention is a powdery, content is generally 〉=and more than 90%, also available wet cake.
2. described synthetic process of vat blue RSN of claim 1, it is characterized in that: setting-up point is 70-160 ℃.
3. the described synthetic process of vat blue RSN of root a tree name claim 1, it is characterized in that: former dyestuff drying after additive compound, sand milling, stdn makes commercial dye.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710191233A CN100590150C (en) | 2007-12-07 | 2007-12-07 | Synthetic process of vat blue RSN |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710191233A CN100590150C (en) | 2007-12-07 | 2007-12-07 | Synthetic process of vat blue RSN |
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| Publication Number | Publication Date |
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| CN101205415A true CN101205415A (en) | 2008-06-25 |
| CN100590150C CN100590150C (en) | 2010-02-17 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN200710191233A Active CN100590150C (en) | 2007-12-07 | 2007-12-07 | Synthetic process of vat blue RSN |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101987300A (en) * | 2010-08-16 | 2011-03-23 | 天津德凯化工股份有限公司 | Phase transfer catalyst composition and preparation method thereof |
| CN102206425A (en) * | 2010-04-26 | 2011-10-05 | 安徽亚邦化工有限公司 | Preparation method of vat blue dye |
| CN104371347A (en) * | 2014-11-29 | 2015-02-25 | 萧县凯奇化工科技有限公司 | Method for preparing vat blue RSN |
| CN105778553A (en) * | 2016-04-08 | 2016-07-20 | 南通恒盛精细化工有限公司 | Improvement method for preparing C.I.vat blue 4 |
-
2007
- 2007-12-07 CN CN200710191233A patent/CN100590150C/en active Active
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102206425A (en) * | 2010-04-26 | 2011-10-05 | 安徽亚邦化工有限公司 | Preparation method of vat blue dye |
| CN102206425B (en) * | 2010-04-26 | 2012-07-04 | 安徽亚邦化工有限公司 | Preparation method of vat blue dye |
| CN101987300A (en) * | 2010-08-16 | 2011-03-23 | 天津德凯化工股份有限公司 | Phase transfer catalyst composition and preparation method thereof |
| CN101987300B (en) * | 2010-08-16 | 2013-06-19 | 天津德凯化工股份有限公司 | Phase transfer catalyst composition and preparation method thereof |
| CN104371347A (en) * | 2014-11-29 | 2015-02-25 | 萧县凯奇化工科技有限公司 | Method for preparing vat blue RSN |
| CN105778553A (en) * | 2016-04-08 | 2016-07-20 | 南通恒盛精细化工有限公司 | Improvement method for preparing C.I.vat blue 4 |
| CN105778553B (en) * | 2016-04-08 | 2017-05-24 | 南通恒盛精细化工有限公司 | Improvement method for preparing C.I.vat blue 4 |
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| Publication number | Publication date |
|---|---|
| CN100590150C (en) | 2010-02-17 |
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Application publication date: 20080625 Assignee: Jiangsu Jiali Fine Chemical Co. Ltd. Assignor: Xuzhou Kaida Fine Chemicals Co., Ltd. Contract record no.: 2013320000782 Denomination of invention: Synthetic process of vat blue RSN Granted publication date: 20100217 License type: Exclusive License Record date: 20131120 |
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Effective date of registration: 20210226 Address after: 221000 west head of Jiali Road, Xuzhou Industrial Park, Xuzhou City, Jiangsu Province Patentee after: Jiangsu Jiali Fine Chemical Co.,Ltd. Address before: 221000 south suburb water dam of Jiangsu City, Xuzhou Province Patentee before: XUZHOU KAIDA FINE CHEMICAL Co.,Ltd. |
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