A method for synthesizing 1-aminoanthraquinone
A technology of aminoanthraquinone and nitroanthraquinone, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of high initial reaction cost, complicated method, and low feeding amount, and achieves the difficulty of reaction process. Low, simple raw materials, low energy consumption
Active Publication Date: 2017-06-20
YANCHENG OUHUA CHEM IND +1
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Problems solved by technology
[0003] At present, the conventional methods for synthesizing 1-aminoanthraquinone include: alkali sulfide reduction method, ammonolysis method, and liquid-phase catalytic hydrogenation method. The problems they have are that the method is complicated and the cost is high.
[0005] The inventors found that the above-mentioned selenium catalytic reduction method has the following problems: the price of selenium is relatively high, so that the initial reaction cost is relatively high; at the same time, the amount of feed that can be carried out in the unit reaction vessel is less, which inhibits the improvement of output
Method used
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Effect test
Embodiment 1
[0030] In a 1000ml autoclave equipped with a stirring bar, add 1-nitroanthraquinone (110g), sulfur powder (1g), H 2 O (400ml), NaHCO 3 (20g), the pH value of the reaction system was about 8; carbon monoxide was introduced to 5MPa, then heated to 150°C and stirred for 4 hours, cooled to room temperature, suction filtered, and dried to obtain the target product 1-aminoanthraquinone. The product was analyzed by high performance liquid chromatography and the yield was 98.5%.
Embodiment 2
[0032] Other experimental method and condition are the same as embodiment 1, only change time, record 1-aminoanthraquinone productive rate as follows:
[0033]
Embodiment 3
[0035] Other experimental method and condition are the same as embodiment 1, only change temperature, record 1-aminoanthraquinone productive rate as follows:
[0036]
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The invention relates to a method for synthesizing 1-aminoanthraquinone. The method includes the following steps that 1-aminoanthraquinone is used as a raw material, in the existence of carbon monoxide and water, sulfur is used as a catalyst, inorganic alkali or organic alkali is used as a promoter, a reaction is carried out under the high-temperature and high-pressure condition, and accordingly the 1-aminoanthraquinone is synthesized at one step. Compared with a selenium-catalyzed reduction method, the sulfur-catalyzed reduction method is lower in cost, higher in productive rate and capable of greatly reducing water consumption.
Description
technical field [0001] The invention relates to the synthesis of 1-aminoanthraquinone, in particular to a method for synthesizing 1-aminoanthraquinone by using sulfur and 1-nitroanthraquinone as raw materials in the presence of water and carbon monoxide under high temperature and high pressure. Background technique [0002] 1-Aminoanthraquinone, also known as 1-amino-9,10 anthracenedione, is an important intermediate for the synthesis of anthraquinone dyes. It is widely used and consumes a lot. It is the main raw material for the production of bromic acid and pyrazole anthraquinone . It can be used in the production of disperse, vat, acid, and reactive dyes, as well as in inks, coatings, polymers, and liquid crystal dyes. It occupies an extremely important position in the dye industry. [0003] At present, conventional methods for synthesizing 1-aminoanthraquinone include: alkali sulfide reduction method, ammonolysis method, and liquid-phase catalytic hydrogenation method....
Claims
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IPC IPC(8): C07C221/00C07C225/34
Inventor 刘晓智李超刘云法伊明娟王志伟郭宇卢圣茂
Owner YANCHENG OUHUA CHEM IND
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