Synthesis method for aromatic hydrazine sulfate

A synthetic method and sulfate technology, applied in the preparation of hydrazine, organic chemistry, etc., can solve the problems of high infrastructure cost and operating cost, high acidity, complicated operation, etc., and achieve high recycling value, high yield and purity, and application good effect
CN106565534AActive Publication Date: 2017-04-19ZHEJIANG QICAI ECO TECH CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
ZHEJIANG QICAI ECO TECH CO LTD
Publication Date
2017-04-19

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Abstract

The invention discloses a synthesis method for aromatic hydrazine sulfate. The synthesis method includes the steps that firstly, aromatic amine is added in sulfuric acid with the mass fraction ranging from 15% to 65%, the temperature is lowered to -5-15 DEG C, a diazotization reagent is dropwise added in the reaction liquid, and diazonium salt is obtained after reaction; secondly, a reducing agent is prepared into a solution, a reducing solution is obtained, the diazonium salt obtained in the first step is dropwise added in the reducing solution, heating reduction is conducted after drop-by-drop addition is completed, and reducing material liquid is obtained through filtration; and thirdly, the reducing material liquid obtained in the second step is heated, dilute sulphuric acid is dropwise added in the reducing material liquid to conduct the acidolysis reaction, the temperature is lowered after the reaction is finished, the aromatic hydrazine sulfate is separated out, a filter cake and filtrate are obtained through filtration, the filter cake is washed with dilute sulphuric acid, and an aromatic hydrazine sulfate product is obtained, and sodium sulfate salt is recycled after the filtrate is preprocessed. Compared with a traditional process, the obtained aromatic hydrazine sulfate is high in yield and purity, the purity reaches 97% or above, the yield is higher than 91%, salt in the wastewater obtained through the reaction is the simplex sodium sulfate salt, and the recycling value is high.
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Description

technical field

[0001] The invention relates to the field of organic compound synthesis, in particular to a method for synthesizing aromatic hydrazine sulfate, a commonly used pharmaceutical intermediate. Background technique

[0002] As an important chemical raw material and intermediate, aromatic hydrazine plays a very important role in the fields of organic synthesis and fine chemicals such as medicine, pesticides and dyes, especially in recent years with the in-depth research and continuous expansion of heterocyclic compounds , the role of aromatic hydrazines in the fields of fine chemicals and organic synthesis is becoming more and more obvious.

[0003] At present, the synthesis method of aromatic hydrazine is mainly to carry out diazotization reaction under hydrochloric acid condition with aromatic amine as raw material, the obtained diazonium salt is reduced with sodium sulfite or sodium bisulfite, after the reduction solution is acidolysis with dilute hydrochloric a...

Claims

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