CN104877368A - Chrysophenine G production process - Google Patents
Chrysophenine G production process Download PDFInfo
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- CN104877368A CN104877368A CN201510245721.3A CN201510245721A CN104877368A CN 104877368 A CN104877368 A CN 104877368A CN 201510245721 A CN201510245721 A CN 201510245721A CN 104877368 A CN104877368 A CN 104877368A
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- sodium
- chrysophene
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- chrysophenine
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Abstract
The invention aims at providing a chrysophenine G production process with high yield and low pollution in order to mainly overcome defects in the existing chrysophenine G production technology, and provides a favorable solution for solving problems of high cost, high energy consumption and high pollution caused in the chrysophenine G production process. Chrysophenine G is a direct dye, is orange powder seen from the appearance and belongs to the technical field of organic dyes. The production process comprises the steps of diazotizing DSD acid, and then, coupling the diazotized DSD acid and dimolecular phenol; and next, converting hydroxyl on the phenyl into ethyoxyl by using chloroethane. The process mainly aims at solving the technical problem of serious equipment corrosion caused by sodium chloride in the prior art through salting out realized by using anhydrous sodium sulfate; after the old process in which sodium chloride is used is changed into the process in which the anhydrous sodium sulfate is used, the yield is greatly increased, and the environment pollution is reduced to a great extent. The process meets the national requirement for mainly protecting the environment and conforms to the decisions of firmly supporting the great decision of the state for protecting the environment, reducing pollution and putting into more investment for improving new processes.
Description
Specification sheets
Technical field
The present invention relates to a kind of production technique of chrysophene G, belong to organic dye technical field.
Background technology
Chrysophene G is a kind of substantive dyestuff, outward appearance is safran powder, and soluble in water is golden yellow to yellow solution, and the aqueous solution freezes the precipitation of shape throw out lower than having when 15 DEG C, therefore claims to freeze Huang.Its dyeing power is strong, and sun-proof, is a kind of valuable yellow dyes in textile industry, is widely used in the dyeing of cotton, hair, silk, cloth, artificial cotton, artificial silk, tynex, leather, paper, biology etc., also can be used for manufacturing color lake, pigment.
At present widely way be by DSD acid after diazotization with dimolecular phenol coupling, then make the conversion of hydroxyl on phenol be that oxyethyl group forms through monochloroethane.
Concrete building-up reactions formula is:
(1) diazotization:
(2) coupling:
(3) ethylize
But adopt aforesaid method to have following shortcoming, the productive rate using sodium-chlor to carry out saltouing is often not high, 65-66%, and through production after a while, the corrosion condition of equipment is serious, the waste water produced is extremely difficult, has had a strong impact on the raising of ecotope and production efficiency.CN102040855B discloses a kind of anhydrous preparation method of chrysophene G, water in production process is replaced with ethanol by it, although the method does not produce waste water, no matter but from raw material production cost or the energy consumption reclaiming a large amount of ethanol, its cost, energy consumption are too high, are unfavorable for large-scale permanent production.
Therefore, a kind of cost, less energy consumption are provided, the production technique of pollution is little, productive rate is high chrysophene G has very high using value.
Summary of the invention
Object of the present invention is mainly to avoid the deficiency in existing chrysophene G production technology, there is provided one to have high yield, oligosaprobic chrysophene G production technology, provide a good solution to problems such as the cost in chrysophene G production process, energy consumption, pollution are high.
The production technique of chrysophene G of the present invention is realized by following steps:
Step 1:DSD acid making beating and diazotization
Diazonium tank is rinsed well, put into deionized water, sodium carbonate is dropped into after heating, the paste of DSD acid is slowly dropped in whipping process, continue after feeding intake to be warming up to 60 DEG C, pH value is 7-8, obtain dark brown clarified liq, then under whipped state, Temperature fall, to 45 DEG C, slowly adds dilute hydrochloric acid and carries out acidifying, acidificatoin time is 2-2.5h, then continue to stir 4h, be cooled to less than 30 DEG C, add sodium nitrite solution in 1h and carry out diazotization, then put into coupling tank and continue stirring reaction 3h, obtain diazo solution;
Step 2: the preparation of sodium phenylate
In phenol storage, add deionized water, be warming up to 30 DEG C after dropping into sodium carbonate, then add phenol, after stirring, obtain sodium phenylate;
Step 3: coupling
Sodium sulfate is added in the diazo solution obtained in step 1, then the sodium phenylate solution obtained in step 2 is injected in diazo liquid fast and carries out coupling, then stir 4h, when the pH value of reactant is 9, direct steam heating to 50 DEG C is saltoutd, stir 0.5h, then slowly add dilute sulphuric acid and the pH value of reactant is adjusted to 6.5-7, after filtration, obtain filter cake, in brightness Huang making beating tank, add ethanol, sodium hydroxide, then drop into filter cake, stir 0.5h and obtain brightness Huang;
Step 4: brightness Huang ethylizes
Brightness Huang step 3 obtained is pressed in ethylization cylinder, and drop into sodium hydroxide, be then heated to 102 DEG C, in 10-12h, then input monochloroethane ethylize, the pressure during ethylization is 4kg/cm
2, temperature is 102-108 DEG C;
Step 5: refining
Stir distillation in reaction product press-in retort step 4 made, to reclaim ethanol, after recovery, metabisulfite solution is pressed into retort and saltouts, then filter at 80 DEG C, obtained chrysophene G after drying, mixture.
In step 1, the mol ratio of DSD acid and sodium carbonate, Sodium Nitrite is 1:(2-3): (5-7).
In step 3, the mol ratio of diazo solution and sodium phenylate is 1:4-6.
In step 4, the ethylating reaction times is 18-20h.
Drying tower is used to carry out drying in step 5.
The present invention adopts anhydrous sodium sulphate to saltout, solve the technical problem that existing sodium-chlor is serious to equipment corrosion, further, applicant surprisingly finds, after using anhydrous sodium sulphate, the productive rate of chrysophene G has brought up to 95-99% by original 65-66%, greatly improve output, decrease the content of the dyestuff in waste water, reduce the pollution of waste water to environment, and anhydrous sodium sulphate reclaims easily, reduce further the content of Pollutants in Wastewater; In addition, the application adopts drying tower to carry out the drying of chrysophene G, solves the shortcoming that existing drying plant dust is serious, energy consumption is high, improves production efficiency, saved the energy.Compare traditional technology, production technique of the present invention can reduce the production cost of chrysophene G, reduce environmental pollution, and the chrysophene G produced has good guarantor's colourity and stamina, has good economic benefit.
Embodiment
Embodiment 1:
Step 1:DSD acid making beating and diazotization
Diazonium tank is rinsed well, put into deionized water, sodium carbonate is dropped into after heating, the paste of DSD acid is slowly dropped in whipping process, continue after feeding intake to be warming up to 60 DEG C, pH value is 7-8, obtain dark brown clarified liq, then under whipped state, Temperature fall, to 45 DEG C, slowly adds dilute hydrochloric acid and carries out acidifying, acidificatoin time is 2-2.5h, then continue to stir 4h, be cooled to less than 30 DEG C, add sodium nitrite solution in 1h and carry out diazotization, then put into coupling tank and continue stirring reaction 3h, obtain diazo solution;
Step 2: the preparation of sodium phenylate
In phenol storage, add deionized water, be warming up to 30 DEG C after dropping into sodium carbonate, then add phenol, after stirring, obtain sodium phenylate;
Step 3: coupling
Sodium sulfate is added in the diazo solution obtained in step 1, then the sodium phenylate solution obtained in step 2 is injected in diazo liquid fast and carries out coupling, then stir 4h, when the pH value of reactant is 9, direct steam heating to 50 DEG C is saltoutd, stir 0.5h, then slowly add dilute sulphuric acid and the pH value of reactant is adjusted to 6.5-7, after filtration, obtain filter cake, in brightness Huang making beating tank, add ethanol, sodium hydroxide, then drop into filter cake, stir 0.5h and obtain brightness Huang;
Step 4: brightness Huang ethylizes
Brightness Huang step 3 obtained is pressed in ethylization cylinder, and drop into sodium hydroxide, be then heated to 102 DEG C, in 10-12h, then input monochloroethane ethylize, the pressure during ethylization is 4kg/cm
2, temperature is 102-108 DEG C;
Step 5: refining
Stir distillation in reaction product press-in retort step 4 made, to reclaim ethanol, after recovery, metabisulfite solution is pressed into retort and saltouts, then filter at 80 DEG C, obtained chrysophene G after the drying of drying tower, mixture.
In step 1, the mol ratio of DSD acid and sodium carbonate, Sodium Nitrite is 1:2:5, and in step 3, the mol ratio of diazo solution and sodium phenylate is 1:4, and in step 4, the ethylating reaction times is 18h.
Embodiment 2:
Basic preparation technology is adopted with embodiment 1, difference is: in step 1, the mol ratio of DSD acid and sodium carbonate, Sodium Nitrite is 1:3:7, in step 3, the mol ratio of diazo solution and sodium phenylate is 1:6, and in step 4, the ethylating reaction times is 20h.
Embodiment 3:
Basic preparation technology is adopted with embodiment 1, difference is: in step 1, the mol ratio of DSD acid and sodium carbonate, Sodium Nitrite is 1:2.5:6, in step 3, the mol ratio of diazo solution and sodium phenylate is 1:5, and in step 4, the ethylating reaction times is 19h.
Comparative example
Adopt basic preparation technology with embodiment 1, difference is: use sodium-chlor to saltout.
The test result (all according to the test of this area traditional test methods) of chrysophene G in table 1 embodiment 1-3, comparative example
Claims (5)
1. a production technique for chrysophene G, is characterized in that, comprises following steps:
Step 1:DSD acid making beating and diazotization
Diazonium tank is rinsed well, put into deionized water, sodium carbonate is dropped into after heating, the paste of DSD acid is slowly dropped in whipping process, continue after feeding intake to be warming up to 60 DEG C, pH value is 7-8, obtain dark brown clarified liq, then under whipped state, Temperature fall, to 45 DEG C, slowly adds dilute hydrochloric acid and carries out acidifying, acidificatoin time is 2-2.5h, then continue to stir 4h, be cooled to less than 30 DEG C, add sodium nitrite solution in 1h and carry out diazotization, then put into coupling tank and continue stirring reaction 3h, obtain diazo solution;
Step 2: the preparation of sodium phenylate
In phenol storage, add deionized water, be warming up to 30 DEG C after dropping into sodium carbonate, then add phenol, after stirring, obtain sodium phenylate;
Step 3: coupling
Sodium sulfate is added in the diazo solution obtained in step 1, then the sodium phenylate solution obtained in step 2 is injected in diazo liquid fast and carries out coupling, then stir 4h, when the pH value of reactant is 9, direct steam heating to 50 DEG C is saltoutd, stir 0.5h, then slowly add dilute sulphuric acid and the pH value of reactant is adjusted to 6.5-7, after filtration, obtain filter cake, in brightness Huang making beating tank, add ethanol, sodium hydroxide, then drop into filter cake, stir 0.5h and obtain brightness Huang;
Step 4: brightness Huang ethylizes
Brightness Huang step 3 obtained is pressed in ethylization cylinder, and drop into sodium hydroxide, be then heated to 102 DEG C, in 10-12h, then input monochloroethane ethylize, the pressure during ethylization is 4kg/cm
2, temperature is 102-108 DEG C;
Step 5: refining
Stir distillation in reaction product press-in retort step 4 made, to reclaim ethanol, after recovery, metabisulfite solution is pressed into retort and saltouts, then filter at 80 DEG C, obtained chrysophene G after drying, mixture.
2. the production technique of chrysophene G according to claim 1, is characterized in that: in step 1, the mol ratio of DSD acid and sodium carbonate, Sodium Nitrite is 1:(2-3): (5-7).
3. the production technique of chrysophene G according to claim 1 and 2, is characterized in that: in step 3, the mol ratio of diazo solution and sodium phenylate is 1:4-6.
4. the production technique of the chrysophene G according to claim 1 or 2 or 3, is characterized in that: in step 4, the ethylating reaction times is 18-20h.
5. the production technique of the chrysophene G according to claim 1 or 2 or 3 or 4, is characterized in that:
Drying tower is used to carry out drying in step 5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510245721.3A CN104877368A (en) | 2015-05-14 | 2015-05-14 | Chrysophenine G production process |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510245721.3A CN104877368A (en) | 2015-05-14 | 2015-05-14 | Chrysophenine G production process |
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| CN104877368A true CN104877368A (en) | 2015-09-02 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110358323A (en) * | 2019-07-30 | 2019-10-22 | 于克兢 | A kind of chrysophene G production technology of non-wastewater discharge |
| CN110903680B (en) * | 2019-12-23 | 2021-09-03 | 上海染料研究所有限公司 | Low-salt purification method of edible colorant |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05171054A (en) * | 1991-12-25 | 1993-07-09 | Tokyo Gas Co Ltd | Synthesis of organic coloring agent |
| CN1569788A (en) * | 2003-07-11 | 2005-01-26 | 上海欣晨新技术公司 | Process for continuous hydrolysis synthesis of guaiacol |
| CN102040855A (en) * | 2010-12-01 | 2011-05-04 | 平顶山市凯斯特染料有限公司 | Method for preparing direct yellow G |
-
2015
- 2015-05-14 CN CN201510245721.3A patent/CN104877368A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH05171054A (en) * | 1991-12-25 | 1993-07-09 | Tokyo Gas Co Ltd | Synthesis of organic coloring agent |
| CN1569788A (en) * | 2003-07-11 | 2005-01-26 | 上海欣晨新技术公司 | Process for continuous hydrolysis synthesis of guaiacol |
| CN102040855A (en) * | 2010-12-01 | 2011-05-04 | 平顶山市凯斯特染料有限公司 | Method for preparing direct yellow G |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110358323A (en) * | 2019-07-30 | 2019-10-22 | 于克兢 | A kind of chrysophene G production technology of non-wastewater discharge |
| CN110358323B (en) * | 2019-07-30 | 2020-10-27 | 于克兢 | Direct frozen yellow G production process without wastewater discharge |
| CN110903680B (en) * | 2019-12-23 | 2021-09-03 | 上海染料研究所有限公司 | Low-salt purification method of edible colorant |
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Application publication date: 20150902 |