Aminopyrine production method

A technology of aminopyrine and production method, which is applied in the direction of organic chemistry, can solve the problems of complex operation of the production method, affecting the yield of aminopyrine, and high energy consumption, so as to save the time of cooling crystallization and centrifugation, and improve the quality of hydrogenation , the effect of guaranteed yield

Inactive Publication Date: 2010-11-24
JIHENG PHARMA HENGSHUI CITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In the existing aminopyrine production technology, after the cooling crystallization and centrifugation process of the 4-aminopyrine oily matter, there is about 15% 4-aminopyrine in the remaining solution after the aminopyrine crude product is crystallized, but th

Method used

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Examples

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Example Embodiment

[0017] Example 1

[0018] The production method of aminopyrine of the present invention includes the following steps: preparation of antipyrine sulfate; nitrosation reaction; first hydrogenation reduction reaction; second hydrogenation reduction reaction; the amino group obtained in the second hydrogenation reduction reaction step The crude bilin is decolorized, crystallized, and dried to obtain the finished amino bilin; a pressure filtration reaction is added between the first hydrogenation reduction reaction step and the second hydrogenation reduction reaction step. The pressure filtration reaction step is: The 4-aminoantipyrine oil obtained in a hydrogenation reduction step is added to the decolorization tank, the mass ratio of the 4-aminoantipyrine oil to the activated carbon is 1:0.022, the temperature is controlled at 80°C, and the mixture is stirred for 30 minutes , Add the weakly alkaline substance sodium carbonate to adjust the pH to 7.2, then pass nitrogen into the deco...

Example Embodiment

[0019] Example 2

[0020] The production method of aminopyrine of the present invention includes the following steps: preparation of antipyrine sulfate; nitrosation reaction; first hydrogenation reduction reaction; second hydrogenation reduction reaction; the amino group obtained in the second hydrogenation reduction reaction step The crude bilin is decolorized, crystallized, and dried to obtain the finished amino bilin; it is characterized in that a pressure filtration reaction is added between the first hydrogenation reduction reaction step and the second hydrogenation reduction reaction step. The pressure filtration reaction step is: Activated carbon and the 4-aminoantipyrine oil obtained from the first hydrogenation reduction step are added to the decolorization tank, the mass ratio of the 4-aminoantipyrine oil to the activated carbon is 1:0.01, and the temperature is controlled at 85°C, Stir for 45 minutes, add the weakly alkaline substance ammonium sulfate to adjust the pH ...

Example Embodiment

[0021] Example 3

[0022] The production method of aminopyrine of the present invention includes the following steps: preparation of antipyrine sulfate; nitrosation reaction; first hydrogenation reduction reaction; second hydrogenation reduction reaction; the amino group obtained in the second hydrogenation reduction reaction step The crude bilin is decolorized, crystallized, and dried to obtain the finished amino bilin; it is characterized in that a pressure filtration reaction is added between the first hydrogenation reduction reaction step and the second hydrogenation reduction reaction step. The pressure filtration reaction step is: Activated carbon and the 4-aminoantipyrine oil obtained in the first hydrogenation reduction step are added to the decolorization tank, the mass ratio of the 4-aminoantipyrine oil to the activated carbon is 1:0.05, and the temperature is controlled at 90°C, Stir for 60 minutes, add weakly alkaline substance ammonia water to adjust the pH to 7.5, t...

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Abstract

The invention relates to an aminopyrine production method, which comprises the following steps of: the preparation of sulfuric acid antipyrine, nitrosation, first hydrogenation reduction reaction, second hydrogenation reduction reaction, and decoloring, crystallization and drying performed on the crude product of the aminopyrine obtained by the second hydrogenation reduction reaction. Filter-pressing reaction is added between the first hydrogenation reduction reaction step and the second hydrogenation reduction reaction step, and comprises the following steps of: adding activated carbon and the oily 4-amino antipyrine obtained in the first hydrogenation reduction reaction step into a decoloring tank, controlling the temperature to be 80 to 90 DEG C, stirring the solution, adjusting a pH value to be 7.0 to 7.5, and then performing the filter-pressing on the solution in the decoloring tank with a three-liner filter to obtain 4-amino antipyrine filter-pressing liquid. The method has the advantages of improving the yield of the aminopyrine at the premise of ensuring the quality of the product, improving the working environment, saving labor, reducing labor intensity, saving energy, reducing emission and reducing the production cost.

Description

technical field [0001] The invention relates to a production method of aminopyrine. Background technique [0002] In the prior art, the production method of aminopyrine comprises the following steps, [0003] The preparation of antipyrine sulfate, antipyrine and sulfuric acid molar ratio is 2: 1 ratio reacts to obtain antipyrine sulfate; Nitrosation reaction, carries out nitrosation with described antipyrine sulfate and sodium nitrite Reaction, obtain nitroso antipyrine, the mass ratio of described antipyrine sulfate and sodium nitrite is 1: 0.35~0.40; The first hydrogenation reduction reaction, described nitroso antipyrine in catalyst Reynolds nickel Under the action of hydrogenation, feed hydrogen to carry out hydrogenation reduction reaction to obtain 4-aminoantipyrine oily substance; crystallization, put the 4-aminoantipyrine oily substance cooling crystallization obtained in the first hydrogenation reduction reaction step into the crystallization tank, open Cool the c...

Claims

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Application Information

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IPC IPC(8): C07D231/48
Inventor 马朝华陈剑芳冯向莉安文德贾树红高振博李海霞马凤霞焦银蕾
Owner JIHENG PHARMA HENGSHUI CITY
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