CN101817989A - Method for preparing disperse blue 60 and homologues thereof - Google Patents
Method for preparing disperse blue 60 and homologues thereof Download PDFInfo
- Publication number
- CN101817989A CN101817989A CN201010142513A CN201010142513A CN101817989A CN 101817989 A CN101817989 A CN 101817989A CN 201010142513 A CN201010142513 A CN 201010142513A CN 201010142513 A CN201010142513 A CN 201010142513A CN 101817989 A CN101817989 A CN 101817989A
- Authority
- CN
- China
- Prior art keywords
- diamino
- condensation reaction
- reaction
- anthraquinone
- disperse blue
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
Abstract
The invention discloses a method for preparing disperse blue 60 and homologues thereof. The method comprises the following steps of: adding a 1,4-diamino-2,3-dicarboximide wet product into water, adding gamma-alkoxy propylamine into the mixture, performing condensation reaction under the conditions that the temperature is between 95 and 105 DEG C and the reaction pressure is between 0.07 and 0.18 MPa for 4 to 6 hours, and after the condensation reaction, filtering, washing and drying to obtain the disperse blue 60 and the homologues thereof; and after completing the condensation reaction, re-using the filtered mother solution in the next condensation reaction. In the method for preparing the disperse blue 60 and the homologues thereof, water is used as a solvent, so that the method realizes pollution-free production and circular economy, and has extremely obvious economic and environmental benefits.
Description
Technical field
The invention belongs to the dyestuff preparation field, relate in particular to the preparation method of a kind of Disperse Blue-60 and homologue thereof.
Background technology
The existing production method of Disperse Blue-60 mainly is with 1, and 4-diamino-anthraquinone leuco compound is a raw material, makes 1 with the chlorsulfonic acid reaction in the orthodichlorobenzene medium, 4-diamino-2,3-disulfonic acid anthraquinone transfers to about pH to 8 with liquid caustic soda then, utilize steam distillation to steam orthodichlorobenzene, after the filtration, join the cyaniding pot, carry out cyanogenation, drip dilute sulphuric acid control pH value, the cyanogenation temperature is 98 ℃～100 ℃, after cyaniding is finished, adds Sulfothiorine and removes poison; Send the pressure filter filtration washing again to neutrality, oven dry.In oxidation pot, add the vitriol oil, be no more than under 65 ℃ of conditions, add dry good 1,4-diamino-2,3-dicyan anthraquinone, 60 ℃～90 ℃ insulation reaction, and then add water hydrolysis closed loop and generate 1,4-diamino-2,3-dicarboximide, after filtering, washing, add aqueous sodium hydroxide solution then, generate suitable sodium salt and water-soluble entirely, add activated carbon adsorption and remove out impurity, acidifying becomes 1 again, 4-diamino-2, the 3-dicarboximide, oven dry obtains exsiccant 1,4-diamino-2, the 3-dicarboximide; To dry then 1,4-diamino-2,3-dicarboximide and γ-methoxy propanamine are in anhydrous ethanol medium, under reflux temperature, carry out condensation reaction, after-filtration is finished in reaction, obtain the Disperse Blue-60 filter cake, the mother liquor after the filtration steams ethanol and γ-methoxy propanamine by distillation again, and the ethanol that steams and γ-methoxy propanamine be the condensation reaction of reuse next batch again.But the condensation product Disperse Blue-60 contains certain solubleness in ethanol and γ-methoxy propanamine causes the Disperse Blue-60 yield low; Contain a certain amount of ethanol and γ-methoxy propanamine in the Disperse Blue-60 filter cake after the filtration, it is high to cause ethanol and γ-methoxy propanamine to consume; Used 1,4-diamino-2, the 3-dicarboximide must be dried, and drying course also needs to consume a certain amount of steam; Using dehydrated alcohol is inflammable explosive article, exists certain potential safety hazard in condensation reaction and still-process.
Dye processing plant, Suzhou Wu family health etc. (are improved one key operation that disperses bright blue S-GL coloured light, Wu Jiakang, Shanghai dyestuff, 1998,26 (5): 27) propose to improve the bright blue coloured light method of dispersion, one key operation wherein is after oxide compound is transferred basic hydrolysis, before Acid precipitation, solution be filtered to remove insoluble impurities, the coloured light of obtaining, this mainly is 1,4-diamino-2,3-dicarboximide intermediate method of purification.
Patent documentation CN101130640 mentions a kind of Disperse Blue-60 and the homologue synthetic method craft improves, hydrolysis is obtained 1,4-diamino-anthraquinone-2, the 3-dicarboximide is with also water-soluble entirely with sodium hydroxide reaction generation corresponding sodium salts, add activated carbon again and remove impurity, filtered while hot, acidifying closed loop again obtains 1,4-diamino-anthraquinone-2,3-dicarboxylic anhydride, this acid anhydrides promptly obtained Disperse Blue-60 product and homologue thereof in 40-50 ℃ of insulation reaction 2-3 hour in pure γ-methoxy propanamine (or γ-ethoxy propylamine) medium.Since 1,4-diamino-anthraquinone-2, the solubleness of 3-dicarboximide in water is relatively poor, and also not having bibliographical information to adopt with water at present is the preparation method of solvent.
Summary of the invention
The invention provides that a kind of production cost is low, technology is simple and the eco-friendly method for preparing Disperse Blue-60 and homologue thereof.
The preparation method of a kind of Disperse Blue-60 and homologue thereof, step comprises:
(1) in the sulfonation reaction still, add orthodichlorobenzene, the dehydration that heats up, the cooling of dehydration back drops into 1, and the 4-diamino-anthraquinone drips chlorsulfonic acid and carries out sulfonation reaction; With about liquid adjusting PH with base to 8, reaction distillation was with distillate suction cyaniding pot after sulfonation was finished; Add sodium cyanide solution, add reserve salt again and carry out cyaniding, drip dilute sulphuric acid control pH value, the cyanogenation temperature is 98 ℃; Cyaniding is finished, and adds sodium thiosulfate and remove poison in the cyaniding product, filters, and filter cake washing is dried to neutrality; Add the vitriol oil at oxidation pot, add exsiccant 1 under 65 ℃ being no more than, 4-diamino-2, the 3-dicyan anthraquinone, 60～75 ℃ of insulation reaction, reaction is finished, suction dilution pot, dilute with water, filtration, filter cake washing join filter cake in the aqueous sodium hydroxide solution then, regulating the pH value is alkalescence, add activated carbon adsorption and remove out impurity, be acidified to the pH value, filter the mother liquor that obtains and be collected in mother liquor tank for acid, filter cake washing is to pH neutrality, promptly get 1,4-diamino-2,3-dicarboximide anthraquinone;
(2) with 1,4-diamino-2,3-dicarboximide anthraquinone is put in the water, adds γ-alkoxy propyl amine, carries out condensation reaction, and filtration is finished in condensation, washing, oven dry obtains Disperse Blue-60 and homologue thereof;
Adopt water as reaction solvent in the condensation reaction, the adding of γ-alkoxy propyl amine makes 1, and 4-diamino-2, the 3-dicarboximide anthraquinone solubleness in the aqueous solution increases, and preferred, the mass ratio of water and γ-alkoxy propyl amine is 8: 1～2;
In order to improve raw material 1,4-diamino-2, the transformation efficiency of 3-dicarboximide anthraquinone, and mother liquor can be used by recovery set after considering condensation, so in the condensation reaction 1,4-diamino-2, the mol ratio of 3-dicarboximide anthraquinone and γ-alkoxy propyl amine is 1: 2～5;
Wherein, γ-alkoxy propyl amine is preferably γ-methoxy propanamine or γ-ethoxy propylamine.
Wherein, the condition of condensation reaction is: temperature: 95～105 ℃, and pressure: 0.07～0.18MPa, the reaction times is: 4～6h.Selection is controlled at certain temperature, carries out the reaction of certain hour under the pressure, the raising of the complete and quality product that helps reacting.
Condensation reaction finish mother liquor that after-filtration obtains can direct reuse in the next batch condensation reaction, the a spot of Disperse Blue-60 of dissolved or its homologue in the mother liquor so both can have been reclaimed, improve the productive rate and the rate of recovery of overall product, can avoid again that solvent and reagent reclaim environmental pollution and the energy expenditure of bringing in the mother liquor; In addition, also can improve the utilization ratio of γ-methoxy propanamine or γ-ethoxy propylamine; Apply mechanically in the process of mother liquor,, can reclaim γ-alkoxy propyl amine, use again as raw material by the distillatory method if unnecessary mother liquor is arranged.
Shown in the following chemical equation of the preparation process of Disperse Blue-60 of the present invention and homologue thereof:
Wherein R is methyl or ethyl.
The used raw material reagent of the present invention is and is fit to the commercially available industrial goods that the dye well intermediate uses, used 1,4-diamino-2,3-dicarboximide anthraquinone are all pressed existing with 1, and 4-diamino-anthraquinone leuco compound is a raw material, obtain 1 through chlorosulphonation, distillation, cyaniding, oxidation, hydrolysis, make with extra care etc., 4-diamino-2,3-dicarboximide anthraquinone, filtration, washing obtain filter cake, drying-free can be directly used in the condensation reaction.
The beneficial effect that the present invention obtains is:
(1) in condensation reaction water consumption substitution be reaction solvent with the dehydrated alcohol, solved environmental protection, safety problem and the alcoholic acid consumption problem of using dehydrated alcohol to bring;
(2) the present invention adopts wet product 1,4-diamino-2,3-dicarboximide anthraquinone replaces 1 of dry product, 4-diamino-2,3-dicarboximide anthraquinone, solved the oven dry problem, give money as a gift 1,4-diamino-2,3-dicarboximide anthraquinone meter by 500kg for every batch, every batch can be reduced 1.2 tons of moisture evaporation, and reducing steam consumption is about 1.2 tons;
(3) in the mother liquor reuse next batch condensation reaction that obtains by the condensation reaction after-filtration, dissolved Disperse Blue-60 etc. is back to the next batch condensation reaction in the mother liquor that the condensation reaction after-filtration is obtained, can on the basis of original technology, improve 5～10% yield, solved the waste of distillation γ-alkoxy propyl amine steam consumption and γ-alkoxy propyl amine, reduced the distillation energy consumption and the pollution of environment;
(4) condensation reaction is adopted and is carried out under certain pressure and temperature, has guaranteed the quality of the complete and the finished product of condensation reaction;
(5) adopt method products obtained therefrom Disperse Blue-60 of the present invention and homologue quality thereof good and very stable, the product yield height, γ-alkoxy propyl amine consumes low.
Embodiment
Embodiment 1
1,4-diamino-2,3-dicarboximide anthraquinone is to adopt method synthetic well known in the art, and concrete steps are: add the 2000kg orthodichlorobenzene in the sulfonation still, be warming up to 120 ℃ of dehydrations, be cooled to 50 ℃ and drop into 250kg 1, the 4-diamino-anthraquinone drips the 480kg chlorsulfonic acid at 50～55 ℃ and carries out sulfonation reaction, finishes, slowly be warming up to 140 ℃, 140～145 ℃ of insulation reaction 7 hours; After sulfonation is finished, be cooled to 70 ℃, with adding water 3000L, the sulfonation material that suction has been got ready is used about liquid adjusting PH with base to 8 again in still kettle, reaction distillation, and distillation is finished, and filters; Filtrate changes in the cyaniding pot, adds 30% sodium cyanide solution 500kg, adds reserve salt again and carries out cyaniding, and dripping dilute sulphuric acid control pH value is 9.0-9.5, and the cyanogenation temperature is 98 ℃; Cyaniding is finished, and adds sodium thiosulfate and remove poison in the cyaniding product, and filtration washing is dried to neutrality; Add vitriol oil 500L, add exsiccant 1,4-diamino-2 under 65 ℃ being no more than, 3-dicyan anthraquinone 150kg, 60～75 ℃ of insulation reaction, reaction is finished, pot is diluted in suction then, being diluted with water to acidity is 20-23%, filters, after the washing, adds the suitable sodium salt of the generation of 50-70kg sodium hydroxide and water-soluble entirely then, add activated carbon adsorption and remove out impurity, acidifying becomes 1 again, 4-diamino-2,3-dicarboximide; Filtration washing promptly gets 1 to pH neutrality, 4-diamino-2, the 3-dicarboximide anthraquinone product that wet, this 1,4-diamino-2, the wet product of 3-dicarboximide anthraquinone can be directly used in the following condensation reaction.
Put into 2000kg water at the enamel still of 5000L, open and stir, add the wet product of having got ready 1,4-diamino-2,3-dicarboximide anthraquinone (450kg gives money as a gift) is thrown and is finished, add and got γ-methoxy propanamine 400kg ready, build kettle cover, stir half an hour, be warming up to 100 ℃, the still internal pressure is 0.12MPa, is incubated 6 hours, be cooled to 60 ℃ then, filter, filter the mother liquor that obtains and be collected in mother liquor tank, filter cake is washed to neutrality, obtains Disperse Blue-60.
Embodiment 2:
Put into embodiment 1 condensation reaction at the enamel still of 5000L and finish after-filtration and obtain mother liquor 2000kg, open and stir, add the wet product of having got ready 1,4-diamino-2,3-dicarboximide anthraquinone (450kg gives money as a gift) is thrown and is finished, add and got γ-methoxy propanamine 150kg ready, build kettle cover, stir half an hour, be warming up to 102 ℃, reaction pressure is 0.13MPa, is incubated 6 hours, be cooled to 60 ℃ then, filter, filter the mother liquor that obtains and be collected in mother liquor tank, filter cake is washed to neutrality, obtains Disperse Blue-60.
Embodiment 3:
Putting into embodiment 2 condensation reactions at the enamel still of 5000L finishes after-filtration and obtains mother liquor 1500kg, water 500kg, open and stir, add the wet product of having got ready 1,4-diamino-2,3-dicarboximide anthraquinone (450kg gives money as a gift), throw and finish, add and got γ-methoxy propanamine 160kg ready, build pot cover, stir half an hour, be warming up to 95 ℃, reaction pressure is 0.11MPa, is incubated 6 hours, is cooled to 60 ℃ then, filter, the mother liquor that filtration obtains is collected in mother liquor tank, and filter cake is washed to neutrality, obtains Disperse Blue-60.
Embodiment 4:
Put into embodiment 3 condensation reactions at the enamel still of 5000L and finish after-filtration and obtain mother liquor 2500kg, open and stir, add the wet product of having got ready 1,4-diamino-2,3-dicarboximide anthraquinone (450kg gives money as a gift) is thrown and is finished, add and got γ-methoxy propanamine 130kg ready, build pot cover, stir half an hour, be warming up to 95 ℃, reaction pressure is 0.09MPa, is incubated 6 hours, be cooled to 60 ℃ then, filter, filter the mother liquor that obtains and be collected in mother liquor tank, filter cake is washed to neutrality, obtains Disperse Blue-60.
Embodiment 5:
Put into embodiment 4 condensation reactions at the enamel still of 5000L and finish after-filtration and obtain mother liquor 2000kg, open and stir, add the wet product of having got ready 1,4-diamino-2,3-dicarboximide anthraquinone (450kg gives money as a gift) is thrown and is finished, add and got γ-methoxy propanamine 145kg ready, build pot cover, stir half an hour, be warming up to 95 ℃, reaction pressure is 0.14MPa, is incubated 6 hours, be cooled to 60 ℃ then, filter, filter the mother liquor that obtains and be collected in mother liquor tank, filter cake is washed to neutrality, obtains Disperse Blue-60.
Comparative Examples 1:
Put into γ-methoxy propanamine 400kg at the enamel still of 5000L, dehydrated alcohol 1200L opens and stirs, add the wet product of having got ready 1,4-diamino-2,3-dicarboximide anthraquinone (450kg gives money as a gift), throw and finish, first-class pot cover is opened reflux exchanger into and out of water valve, be warming up to 75 ℃, back flow reaction 6 hours is cooled to 60 ℃ then, filter, filtration obtains mother liquor and reclaims ethanol and γ-methoxy propanamine by distillation again, and filter cake is washed to neutrality, prepares Disperse Blue-60.
Embodiment 6:
Put into 2000kg water at the enamel still of 5000L, open and stir, add the wet product of having got ready 1,4-diamino-2,3-dicarboximide anthraquinone (450kg gives money as a gift) is thrown and is finished, add and got γ-ethoxy propylamine 460kg ready, build pot cover, stir half an hour, be warming up to 100 ℃, pot inner pressure is 0.12MPa, is incubated 6 hours, be cooled to 60 ℃ then, filter, filter the mother liquor that obtains and be collected in mother liquor tank, filter cake is washed to neutrality, prepares the homologue of Disperse Blue-60.
Embodiment 7:
Putting into embodiment 6 condensation reactions at the enamel still of 5000L finishes after-filtration and obtains mother liquor 2000kg, open and stir, add the wet product of having got ready 1,4-diamino-2,3-dicarboximide anthraquinone (450kg gives money as a gift) is thrown and is finished, and adds and has got γ-ethoxy propylamine 160kg ready, build pot cover, stir half an hour, be warming up to 103 ℃, reaction pressure is 0.15MPa, be incubated 5.5 hours, be cooled to 60 ℃ then, filter, filter the mother liquor that obtains and be collected in mother liquor tank, filter cake is washed to neutrality, prepares the homologue of Disperse Blue-60.
Embodiment 8:
Putting into embodiment 7 condensation reactions at the enamel still of 5000L finishes after-filtration and obtains mother liquor 2500kg, open and stir, add the wet product of having got ready 1,4-diamino-2,3-dicarboximide anthraquinone (450kg gives money as a gift) is thrown and is finished, and adds and has got γ-ethoxy propylamine 140kg ready, build pot cover, stir half an hour, be warming up to 95 ℃, reaction pressure is 0.08MPa, be incubated 6 hours, be cooled to 60 ℃ then, filter, filter the mother liquor that obtains and be collected in mother liquor tank, filter cake is washed to neutrality, prepares the homologue of Disperse Blue-60.
Embodiment 9:
Putting into embodiment 8 condensation reactions at the enamel still of 5000L finishes after-filtration and obtains mother liquor 2000kg, open and stir, add the wet product of having got ready 1,4-diamino-2,3-dicarboximide anthraquinone (450kg gives money as a gift) is thrown and is finished, and adds and has got γ-ethoxy propylamine 150kg ready, build pot cover, stir half an hour, be warming up to 105 ℃, reaction pressure is 0.15MPa, be incubated 6 hours, be cooled to 60 ℃ then, filter, filter the mother liquor that obtains and be collected in mother liquor tank, filter cake is washed to neutrality, prepares the homologue of Disperse Blue-60.
Embodiment 10:
Putting into embodiment 9 condensation reactions at the enamel still of 5000L finishes after-filtration and obtains mother liquor 1800kg, open and stir, add the wet product of having got ready 1,4-diamino-2,3-dicarboximide anthraquinone (450kg gives money as a gift) is thrown and is finished, and adds and has got γ-ethoxy propylamine 170kg ready, build pot cover, stir half an hour, be warming up to 100 ℃, reaction pressure is 0.11MPa, be incubated 6 hours, be cooled to 60 ℃ then, filter, filter the mother liquor that obtains and be collected in mother liquor tank, filter cake is washed to neutrality, prepares the homologue of Disperse Blue-60.
Disperse Blue-60 and homologue thereof that embodiment 1～10 and Comparative Examples 1 are prepared carry out analytical results such as table 1.Reacted mother liquor is satisfying under the condition of follow-up condensation reaction, and remaining mother liquor can reclaim γ-alkoxy propyl amine through the distillation back, and as the raw material use of follow-up condensation reaction, mother liquor described herein is and needs the distillatory mother liquor in the table 1.
Table 1
Above-mentioned staining power is to be the staining power that standard substance are surveyed with respect to 200% commercialization EX-SF DISPERSE BLUE EX-SF 300, and concrete measuring method is GB/T2394-200.
Can draw from above embodiment and Comparative Examples, by the process modification of the present invention to Disperse Blue-60, guaranteeing that the product staining power is greater than 472, coloured light is under approximate-little red situation, can improve the yield (the product filter cake is given money as a gift greater than 470kg) of product on the one hand, ((γ-methoxy propanamine of being thrown in the Comparative Examples is 400kg to the consumption of every batch of γ-methoxy propanamine less than 200kg under the condition of mother liquor reuse to reduce raw material consumption reduction raw material consumption, can steam 200kg by distillation, actual every batch of consumption γ-methoxy propanamine is 190kg).Can reduce the energy expenditure that must drop on the other hand, realize energy-saving and emission-reduction owing to distill mother liquor, the purpose of cleaner production, recycling economy, economic benefit and environmental benefit are remarkable.
Claims (7)
1. the preparation method of Disperse Blue-60 and homologue thereof, comprise: with 1, the 4-diamino-anthraquinone is successively through carrying out sulfonation reaction with chlorsulfonic acid in the orthodichlorobenzene medium, in sodium cyanide solution, carry out cyanogenation, in the vitriol oil and water, carry out oxidizing reaction and ring-closure reaction filtration and obtain 1,4-diamino-2,3-dicarboximide anthraquinone is characterized in that: with 1, and 4-diamino-2,3-dicarboximide anthraquinone is put in the water, add γ-alkoxy propyl amine again, carry out condensation reaction, after-filtration is finished in condensation, washing, oven dry obtains Disperse Blue-60 and homologue thereof.
2. preparation method according to claim 1 is characterized in that: after described condensation reaction is finished, filter the mother liquor that obtains and be back to use in the next batch condensation reaction.
3. preparation method according to claim 1 and 2 is characterized in that: described γ-alkoxy propyl amine is γ-methoxy propanamine or γ-ethoxy propylamine.
4. preparation method according to claim 1 is characterized in that: the mass ratio of water and γ-alkoxy propyl amine is 8: 1～2 in the described condensation reaction.
5. preparation method according to claim 1 is characterized in that: in the described condensation reaction 1, and 4-diamino-2, the mol ratio of 3-dicarboximide anthraquinone and γ-alkoxy propyl amine is 1: 2～5.
6. preparation method according to claim 1 is characterized in that: the condition of described condensation reaction is: temperature: 95～105 ℃, and pressure: 0.07～0.18MPa.
7. preparation method according to claim 1 is characterized in that: the reaction times of described condensation reaction is: 4～6 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010142513.8A CN101817989B (en) | 2010-04-08 | 2010-04-08 | Method for preparing disperse blue 60 and homologues thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010142513.8A CN101817989B (en) | 2010-04-08 | 2010-04-08 | Method for preparing disperse blue 60 and homologues thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101817989A true CN101817989A (en) | 2010-09-01 |
| CN101817989B CN101817989B (en) | 2014-04-02 |
Family
ID=42653272
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010142513.8A Active CN101817989B (en) | 2010-04-08 | 2010-04-08 | Method for preparing disperse blue 60 and homologues thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101817989B (en) |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102199364A (en) * | 2011-03-11 | 2011-09-28 | 河南洛染股份有限公司 | Blue temporary water-soluble disperse dye, preparation method thereof and application thereof |
| CN102212029A (en) * | 2011-04-20 | 2011-10-12 | 江苏亚邦染料股份有限公司 | Synthesis method of disperse blue 60 intermediate |
| CN103242208A (en) * | 2013-05-03 | 2013-08-14 | 盐城市瓯华化学工业有限公司 | Process for preparing 1, 4-diamino-anthraquinone-2, 3-disulfonic acid by nicotinic acid method |
| CN103497142A (en) * | 2013-10-09 | 2014-01-08 | 江苏和利瑞科技发展有限公司 | Preparation method of disperse blue 60 and/or homolog thereof |
| CN109096789A (en) * | 2018-07-20 | 2018-12-28 | 江苏华尔化工有限公司 | A kind of No. 60 blue synthesis in water technique |
| CN111574484A (en) * | 2020-06-10 | 2020-08-25 | 浙江博澳新材料股份有限公司 | Water-saving and environment-friendly anhydride preparation method |
| CN112500718A (en) * | 2020-09-21 | 2021-03-16 | 浙江恩盛染料化工有限公司 | Resource utilization method of C.I. disperse blue 60 condensation reclaimed material |
| CN112795207A (en) * | 2020-12-19 | 2021-05-14 | 浙江恩盛染料化工有限公司 | Post-treatment method of disperse blue 60 |
| CN113930085A (en) * | 2021-11-08 | 2022-01-14 | 浙江理工大学 | Sun-proof anthraquinone disperse dye and preparation method thereof |
| CN116855099A (en) * | 2023-06-30 | 2023-10-10 | 浙江闰土股份有限公司 | Process for preparing disperse blue 60 and its derivative |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4491666A (en) * | 1981-03-14 | 1985-01-01 | Basf Aktiengesellschaft | Preparation of anthraquinoid disperse dyes |
| CN1995012A (en) * | 2006-12-28 | 2007-07-11 | 江苏亚邦染料股份有限公司 | Process for preparing 1,4-diamino-2,3-dicyan anthraquinone |
| CN101130640A (en) * | 2007-08-13 | 2008-02-27 | 江苏亚邦染料股份有限公司 | Improved technique for synthesizing dispersion blue 60 |
-
2010
- 2010-04-08 CN CN201010142513.8A patent/CN101817989B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4491666A (en) * | 1981-03-14 | 1985-01-01 | Basf Aktiengesellschaft | Preparation of anthraquinoid disperse dyes |
| CN1995012A (en) * | 2006-12-28 | 2007-07-11 | 江苏亚邦染料股份有限公司 | Process for preparing 1,4-diamino-2,3-dicyan anthraquinone |
| CN101130640A (en) * | 2007-08-13 | 2008-02-27 | 江苏亚邦染料股份有限公司 | Improved technique for synthesizing dispersion blue 60 |
Non-Patent Citations (2)
| Title |
|---|
| 季军安等: "C.I.分散蓝60的合成工艺对色光的影响", 《染料工业》 * |
| 李少文: "双氰合成新工艺", 《安徽化工》 * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102199364A (en) * | 2011-03-11 | 2011-09-28 | 河南洛染股份有限公司 | Blue temporary water-soluble disperse dye, preparation method thereof and application thereof |
| CN102199364B (en) * | 2011-03-11 | 2014-04-09 | 河南洛染股份有限公司 | Blue temporary water-soluble disperse dye, preparation method thereof and application thereof |
| CN102212029A (en) * | 2011-04-20 | 2011-10-12 | 江苏亚邦染料股份有限公司 | Synthesis method of disperse blue 60 intermediate |
| CN103242208A (en) * | 2013-05-03 | 2013-08-14 | 盐城市瓯华化学工业有限公司 | Process for preparing 1, 4-diamino-anthraquinone-2, 3-disulfonic acid by nicotinic acid method |
| CN103497142A (en) * | 2013-10-09 | 2014-01-08 | 江苏和利瑞科技发展有限公司 | Preparation method of disperse blue 60 and/or homolog thereof |
| CN109096789A (en) * | 2018-07-20 | 2018-12-28 | 江苏华尔化工有限公司 | A kind of No. 60 blue synthesis in water technique |
| CN111574484A (en) * | 2020-06-10 | 2020-08-25 | 浙江博澳新材料股份有限公司 | Water-saving and environment-friendly anhydride preparation method |
| CN111574484B (en) * | 2020-06-10 | 2021-11-09 | 浙江博澳新材料股份有限公司 | Water-saving and environment-friendly anhydride preparation method |
| CN112500718A (en) * | 2020-09-21 | 2021-03-16 | 浙江恩盛染料化工有限公司 | Resource utilization method of C.I. disperse blue 60 condensation reclaimed material |
| CN112795207A (en) * | 2020-12-19 | 2021-05-14 | 浙江恩盛染料化工有限公司 | Post-treatment method of disperse blue 60 |
| CN113930085A (en) * | 2021-11-08 | 2022-01-14 | 浙江理工大学 | Sun-proof anthraquinone disperse dye and preparation method thereof |
| CN113930085B (en) * | 2021-11-08 | 2023-08-08 | 浙江万丰化工股份有限公司 | Sun-proof anthraquinone disperse dye and preparation method thereof |
| CN116855099A (en) * | 2023-06-30 | 2023-10-10 | 浙江闰土股份有限公司 | Process for preparing disperse blue 60 and its derivative |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101817989B (en) | 2014-04-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101817989B (en) | Method for preparing disperse blue 60 and homologues thereof | |
| CN100543012C (en) | Preparation 1,4-diamino-2, the method for 3-dicyan anthraquinone | |
| CN102617412B (en) | Preparation method of bromoamine acid | |
| CN104725251A (en) | Method for preparing solvent blue 78 | |
| CN112724700B (en) | Process for synthesizing permanent violet RL by one-pot method | |
| CN101130640A (en) | Improved technique for synthesizing dispersion blue 60 | |
| CN109928945B (en) | 1-bromodibenzofuran and synthetic method thereof | |
| CN101108816A (en) | Method of synthesizing sulfonation paratope ester | |
| CN102703070A (en) | Preparation method of stable fluorescent carbon | |
| CN102212029B (en) | Synthesis method of disperse blue 60 intermediate | |
| CN101633631A (en) | Method for synthesizing sulfonated para-ester | |
| CN100413928C (en) | Preparation technique of solvent red 179 | |
| CN104926636A (en) | Method for preparing 1,4-dihydroxy anthraquinone | |
| CN111087832A (en) | Environment-friendly preparation method of disperse red 60 | |
| CN101863781A (en) | Preparation method of 1, 2-di (o-amino phenoxyl) ethane | |
| CN100590150C (en) | Synthetic process of vat blue RSN | |
| CN108864730A (en) | A kind of new process of pigment yellow PY138 production | |
| CN106675081B (en) | A kind of environment-friendly preparation method of 04 dyestuff of solvent blue 19 | |
| CN102627551B (en) | Method for isomerizing rosin resin acid promoted by solid super acid | |
| CN102139893B (en) | Method for preparing potassium carbonate | |
| CN102040855B (en) | Method for preparing direct yellow G | |
| CN101717401B (en) | Preparing method of phthalocyaninatoaluminium chloride | |
| CN112707807A (en) | Preparation method of 4, 5-difluorophthalic acid | |
| CN103897424B (en) | A kind of preparation method of Vat Olive Green B dyestuff | |
| CN103172506B (en) | A kind of take nano cupric oxide as the method for catalyst preparing croconic acid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |