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Refining method of aminopyrine crude product

A technology of aminopyrine and refining method, which is applied in the field of chemical synthesis and pharmaceuticals, can solve the problems of material quality decline, aminopyrine cost increase, and ethanol content increase, and achieve the effects of reducing ethanol consumption, saving ethanol, and improving quality

Inactive Publication Date: 2020-01-21
SHANDONG XINHUA PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when the output of Analgin is higher than the equilibrium value, it will inevitably cause the accumulation of aminopyrine crude product, and this part of aminopyrine crude product has a small amount of extractant in the material. If the aminopyrine production line excessively digests the material, it will affect normal The ethanol content in the raffinate of the aminopyrine ethanol recovery system increases sharply, resulting in an increase in the cost of aminopyrine
In addition, the forced digestion of crude aminopyrine will also lead to a general decline in the quality of various materials in the aminopyrine mother liquor recovery system

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 1000kg of aminopyrine crude product, 1200kg of water, and 13kg of activated carbon to the aminopyrine refining tank in turn, (the weight ratio is 1:1.2:0.013, open the refining tank to heat up the interlayer steam to 98°C, steam out 200-300L of water, and keep warm for 98 -100°C, after the water is evaporated, continue to reflux for 2-3 hours to decolorize; after the decolorization is completed, turn on the nitrogen in the refining tank, filter the activated carbon while it is hot, and then press the filtrate into the crystallization tank to cool down to 65-70°C for crystallization, and then Cool down to below 10°C and centrifuge to obtain the refined crude material; put the obtained refined crude material into the refining tank, add 1000kg of ethanol and 30kg of activated carbon (the weight ratio is 1:1.0:0.03), open the refining tank and heat the interlayer steam to 78 ℃, keep warm at 78-92℃, decolorize for 2-3 hours; after decolorization, turn on the nitrogen gas ...

Embodiment 2

[0017] Add 1000kg of aminopyrine crude product, 1300kg of water, and 18kg of activated carbon to the aminopyrine refining tank in turn (weight ratio is 1:1.3:0.018), open the refining tank and heat up the interlayer steam to 98°C, distill 200-300L of water, and keep warm during the period 98-100°C, after the water is evaporated, continue to reflux for 2-3 hours to decolorize; after the decolorization is completed, turn on the nitrogen in the refining tank, filter the activated carbon while it is hot, and then press the filtrate into the crystallization tank to cool down to 65-70°C for crystallization. Then lower the temperature to below 10°C for centrifugation to obtain refined crude material; put the resulting refined crude material into the refining tank, add 1100 kg of ethanol and 40 kg of activated carbon (weight ratio is 1:1.1:0.04), open the refining tank interlayer steam to heat up to 78°C, keep warm at 78-92°C, decolorize for 2-3 hours; after decolorization, turn on the...

Embodiment 3

[0019] Add 1000kg of aminopyrine crude product, 1500kg of water, and 20kg of activated carbon to the aminopyrine refining tank in turn (weight ratio is 1:1.5:0.02), open the refining tank and heat up the interlayer steam to 98°C, steam out 200-300L of water, and keep warm during the period 98-100°C, after the water is evaporated, continue to reflux for 2-3 hours to decolorize; after the decolorization is completed, turn on the nitrogen in the refining tank, filter the activated carbon while it is hot, and then press the filtrate into the crystallization tank to cool down to 65-70°C for crystallization. Then lower the temperature to below 10°C for centrifugation to obtain refined crude material; put the resulting refined crude material into the refining tank, add 1200 kg of ethanol and 50 kg of activated carbon (weight ratio is 1:1.2:0.05), open the refining tank interlayer steam and heat up to 78°C, keep warm at 78-92°C, decolorize for 2-3 hours; after decolorization, turn on t...

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PUM

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Abstract

The invention provides a refining method of an aminopyrine crude product, which is characterized by comprising the following steps: (1) proportionally heating and refluxing the aminopyrine crude product, water and activated carbon, and then performing filtration, cooling, crystallizing and centrifugation to obtain a refined crude product material; (2) heating and refluxing the refined crude product material, ethanol and activated carbon in a proportion, and then performing filtration, cooling, crystallizing and centrifugation to obtain a refined material. According to the method, the problem that an aminopyrine crude product material is difficult to digest due to a relatively high analgin yield can be solved; meanwhile, the method does not influence an aminopyrine ethanol recovery system,and can save ethanol than the previous production mode.

Description

technical field [0001] The invention belongs to the field of chemical synthesis and pharmaceuticals, and relates to a method for refining crude aminopyrine. Background technique [0002] Aminophenazone chemical name is 1-phenyl-2,3-dimethyl-4-dimethylaminopyrazolone, white or almost white crystalline powder; odorless, slightly bitter taste; Deterioration; aqueous solution shows alkaline reaction. This product is soluble in ethanol or chloroform, soluble in water or ether. The molecular formula is C13H17N3O, and the molecular weight is 231.29. Aminopyrine is a pyrazolone antipyretic, analgesic and anti-inflammatory drug, which can inhibit the synthesis and release of prostaglandin E1 in the neurons of the anterior hypothalamus, restore the normal reactivity of sensory neurons in the temperature regulation center and play an antipyretic effect; Aminopyrine can also inhibit the synthesis and release of prostaglandins in local tissues of inflammation, stabilize lysosome membr...

Claims

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Application Information

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IPC IPC(8): C07D231/48
CPCC07D231/48
Inventor 王龙闯曲荣昌郭超林龙龙宋忠文张建强赵林桐韩冠英蔡金萍
Owner SHANDONG XINHUA PHARMA CO LTD
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