Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of 1,4-diamido-2,3-dicyano anthraquinone

A technology of dicyanoanthracene and diamino, which is applied in the field of preparation of dye intermediates, can solve problems such as complex operation, not too difficult to imagine, and environmental pollution, and achieve the effects of simple process operation, solving hidden safety hazards, and simple preparation process

Active Publication Date: 2016-04-13
JIANGSU YABANG DYE
View PDF5 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above-mentioned method for preparing 1,4-diamino-2,3-dicyanoanthraquinone mainly has three major disadvantages: 1. use concentrated sulfuric acid, sulfonyl chloride, boric acid and other medicaments for easily corroded equipment; And it needs to consume a large amount of alkali, generate a large amount of salt, the waste water is not easy to treat, and directly discharges the environment; 3. The synthetic route is long and the operation is complicated, so it is difficult to control the quality of key intermediates, and the overall yield is also unsatisfactory
The main reason why cyanide is scary is its high toxicity; another important reason is that cyanide is an important chemical raw material, and its production is not too difficult. too difficult thing
Because chemicals have more or less loopholes in many links such as production, sales, transportation, and use. With the occurrence of the Tianjin Port explosion accident, the production and control of highly toxic substances such as sodium cyanide will become more stringent. Stress and trouble for both cyanide producers and users

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Add N,N-dimethylformamide into a 500mL four-neck flask with sealed stirring, thermometer and reflux device, then start stirring and add 0.1moL 1,4-diamino-2,3-dichloroanthraquinone, 0.6moL Acetic anhydride, 0.4moL anhydrous sodium acetate, 0.03moL benzyltriethylammonium chloride, 0.7moL formamide, after adding, slowly warm up to reflux, keep warm for 12 hours, then cool to room temperature, filter, wash with water until neutral, After drying, 1,4-diamino-2,3-dicyanoanthraquinone can be obtained with a yield of 86% and a purity of 97.2% (determined by high performance liquid chromatography and planimetric method).

Embodiment 2

[0023] The process operation is the same as in Example 1, and the material ratio is 1,4-diamino-2,3-dichloroanthraquinone to acetic anhydride, anhydrous sodium acetate, catalyst benzyltriethylammonium chloride, formamide molar ratio The sequence is 1:8:5:0.6:9, and N,N-dimethylformamide is used as the solvent. 1,4-diamino-2,3-dicyanoanthraquinone was obtained with a yield of 85% and a purity of 96.8% (determined by high performance liquid chromatography and planimetric method).

Embodiment 3

[0025] The process operation is the same as in Example 1, and the material ratio is 1,4-diamino-2,3-dichloroanthraquinone to acetic anhydride, anhydrous sodium acetate, catalyst benzyltriethylammonium chloride, formamide molar ratio The sequence is 1:4:3:0.2:4, and N,N-dimethylformamide is used as the solvent. 1,4-diamino-2,3-dicyanoanthraquinone was obtained with a yield of 86% and a purity of 94.9% (determined by high performance liquid chromatography and planimetric method).

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to a preparation method of 1,4-diamido-2,3-dicyano anthraquinone. The preparation method comprises steps as follows: 1,4-diamido-2,3-dichloroanthraquinone is taken as a raw material and is heated to reflux with a high-boiling-point polar solvent as a reaction medium and formamide as a cyanation reagent in the presence of a phase transfer catalyst, a dehydrating agent and an acid-binding agent, a product is cooled, filtered, washed with water and dried, and 1,4-diamido-2,3-dicyano anthraquinone is prepared. The technical scheme has the characteristics of low environmental toxicity, low environmental protection pressure and simplicity in technological operation; the prepared 1,4-diamido-2,3-dicyano anthraquinone reaches the same level of the prior art when used for preparing disperse turquoise blue S-GL.

Description

technical field [0001] The invention relates to a preparation method of a dye intermediate, in particular to a preparation method of 1,4-diamino-2,3-dicyanoanthraquinone, an intermediate of dispersing Cuilan S-GL. Background technique [0002] 1,4-diamino-2,3-dicyanoanthraquinone is an important intermediate of disperse turquoise blue S-GL, dye index number C.I.Blue60, turquoise blue S-GL has a bright color, green light blue, It is used to spell lake blue, lake green, brilliant green and other bright colors, and has its special purpose in the printing and dyeing industry. [0003] The raw materials required for the synthesis of 1,4-diamino-2,3-dicyanoanthraquinone, the intermediate of disperse turquoise blue S-GL, generally start from 1,4-diaminoanthraquinone leuco, the preparation method in the early patent US2628963A Yes: 1,4-diaminoanthraquinone leuco is chlorinated with sulfuryl chloride in an inert solvent (such as o-dichlorobenzene, nitrobenzene, etc.) to obtain 1,4-d...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Applications(China)
IPC IPC(8): C07C255/58C07C253/06
CPCC07C253/06C07C255/58
Inventor 姚雷吴文燕郑冬松
Owner JIANGSU YABANG DYE
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products