Unlock instant, AI-driven research and patent intelligence for your innovation.

Preparation method of aminoanthraquinone

An aminoanthraquinone and anthraquinone technology, applied in the field of aromatic ammonia organic compound synthesis technology, can solve problems such as hidden dangers of production process safety, and achieve the effects of improving yield, simple and safe technological process

Active Publication Date: 2020-12-11
XUZHOU COLLEGE OF INDAL TECH
View PDF0 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the synthesis method of aminoanthraquinone is mainly in the form of hydrogen reduction after nitration, specifically, the dry anthraquinone is first nitrated by using a mixed acid solution of oleum and nitric acid, thereby preparing nitroanthraquinone. Afterwards, the reduction reaction is carried out by reacting with alkali sulfide or sodium hydrosulfide to obtain the reduced product aminoanthraquinone. This reaction route includes two-step reactions, among which the nitrification reaction is a dangerous process strictly regulated by the state at present. The control requirements are strict, and the production process itself has major safety hazards. In addition, many provinces have ordered the prohibition of the production of products using the nitrification process.

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

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Preparation method of aminoanthraquinone
  • Preparation method of aminoanthraquinone
  • Preparation method of aminoanthraquinone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh 10.4 grams of anthraquinone, 16.4 grams of hydroxylamine sulfate, and 0.18 g of vanadium pentoxide for later use, measure 27 mL of concentrated sulfuric acid into the reactor, then add 10.4 grams of anthraquinone to it, heat up to 60 degrees and stir for 0.5 hours After completely dissolving, put in 16.4 grams of hydroxylamine sulfate, then put 0.18 grams of vanadium pentoxide into the reactor as a catalyst, slowly raise the temperature to 100 degrees, maintain this temperature for 3 hours, then cool to room temperature and add deionized water Dilute, filter with filter paper, wash with water and dry to remove water to obtain the crude product of diaminoanthraquinone.

Embodiment 2

[0029] Take by weighing 10.4g of anthraquinone dry product and add in the reactor that fills the 98% vitriol oil of 48.6ml, stir after being warmed up to 60 degrees and anthraquinone is completely dissolved, then add 16.4g of hydroxylamine sulfate, 0.18g of V 2 o 5 , slowly heating the reactor to an internal temperature of 100 degrees, maintaining this temperature for 3 hours to react, obtaining the reacted material and diluting it with deionized water, then performing suction filtration, washing with water, and drying to obtain the crude product of diaminoanthraquinone.

Embodiment 3

[0031] Change the amount of hydroxylammonium sulfate in the reactant on the basis of embodiment 2, add the hydroxylammonium sulfate of 19.7g, the catalyst V of 0.18g 2 o 5 , with other conditions unchanged, heat preservation and reaction at 100 degrees for 3 hours, then carry out the same post-treatment such as dilution, and obtain the crude product of diaminoanthraquinone after drying.

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 discloses a preparation method of aminoanthraquinone. Anthraquinone, hydroxylamine sulfate or hydroxylamine hydrochloride are used as reactants, and react at 100 DEG C under the action of catalysts such as VO, V2O3, VO2, V2O5, VOSO4 and the like under the medium of concentrated sulfuric acid to prepare a diaminoanthraquinone crude product, and anthraquinone is used as a reactant in the process route, thereby avoiding the traditional nitrification process and avoiding the high-risk reaction process. The safety of the reaction process for preparing aminoanthraquinone can be effectively improved, the content of diamino anthraquinone in the crude product obtained through the process accounts for about 90%, the content is high, and industrial production amplification is facilitated.

Description

technical field [0001] The invention relates to the technical field of synthesis technology of aromatic amino organic compounds, in particular to a preparation method of aminoanthraquinone. Background technique [0002] Anthraquinone organic compounds are important dye intermediates, which belong to advanced dye intermediates in organic synthesis, such as indanthrene vat dyes, acid dyes, and some important raw materials for reactive dyes. Aminoanthraquinone is an important part of anthraquinone dye intermediates, and it has been widely used in the production of important dyes such as vat, disperse, acid and reactive dyes. And among aminoanthraquinones, monoaminoanthraquinone and diaminoanthraquinone are the most widely used and demanded. [0003] At present, the synthesis method of aminoanthraquinone is mainly in the form of hydrogen reduction after nitration, specifically, the dry anthraquinone is first nitrated by using a mixed acid solution of oleum and nitric acid, ther...

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): C07C221/00C07C225/34
CPCC07C221/00C07C2603/24C07C225/34Y02P20/584
Inventor 李想吴祥林李兵窦艳徐宁杜辉陈君孙传益丁宗元王德堂李敢吴羡
Owner XUZHOU COLLEGE OF INDAL TECH