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High-purity decoloration filter pressing process of sulfadoxine

A high-purity technology of sulfonamide, which is applied in the fields of filtration and separation, membrane filter, fixed filter element filter, etc., can solve the problem of not specifically disclosing the method of fine processing and purification of crude sulfonamide, high impurity content, and inability to be directly applied, etc. question

Active Publication Date: 2020-01-17
CHANGSHU JINSHEN MEDICAL PROD CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method does not specifically disclose the specific finishing and purification method for the crude product of sulfonamide, and the impurity content is relatively high, so it cannot be directly applied.

Method used

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  • High-purity decoloration filter pressing process of sulfadoxine
  • High-purity decoloration filter pressing process of sulfadoxine
  • High-purity decoloration filter pressing process of sulfadoxine

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Embodiment 1: add 4500kg water in dissolving pot, add under heating and stirring 285kg of the sulfonamide crude product that is made by CN102391190A embodiment 1, add 67.5kg calcium hydroxide and adjust pH value to 12, after fully dissolving, add 22.5kg respectively Activated carbon and 22.5kg acidic preactivated pore-enlarging activated carbon are used for decolorization, and the temperature is at 90° C., and it is incubated for 70 minutes; The temperature is set at 10°C, and all the comparative examples and examples below are the same as the implementation conditions), centrifuged and dehydrated; the filter cake is washed with water until the liquid outlet is clarified, and the centrifuged and dried discharge is dried by a double-cone rotary vacuum drier to obtain Zhou The finished product of sulfonamide has a purity of about 99.99%.

Embodiment 2

[0038] Embodiment 2: add 4500kg water in dissolving pot, add under heating and stirring 285kg of the sulfonamide crude product that is made by CN102391190A embodiment 1, add 67.5kg calcium hydroxide and adjust pH value to 12, after fully dissolving, add 45kg activated carbon decolorization , the temperature is at 90°C, and it is incubated for 70 minutes; after cooling, the pressure filter 10 provided by the present embodiment is filtered and then sent to the fine crystallization pot for cooling and recrystallization. Glacial acetic acid solution, until the pH value is 5.5, after retesting unchanged, centrifugal dehydration; wash the filter cake with water until the liquid outlet is clarified, centrifugally dry and discharge the material and use a double-cone rotary vacuum dryer to dry to obtain the finished product of sulfonamide, which has a purity of It is about 99.8%.

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Abstract

The invention discloses a high-purity decoloration filter pressing process of sulfadoxine. According to the process, an active carbon decolorization process comprises: adding active carbon into a crude sulfadoxine dissolving solution to adsorb impurities, cooling, feeding into a filter press, and filtering; the filter press comprises a filter pressing cavity, wherein the bottom of the filter pressing cavity is provided with a sulfanilamide filtrate outlet, and the upper portion of the filter pressing cavity is provided with a feeding port; a filter pressing cavity cover plate is cooperativelymounted at the feeding port; the filter pressing cavity is connected to an external pressure device through the filter pressing cavity cover plate, and is used for injecting pressure into the filter pressing cavity; a first filter pressing mechanism and a second filter pressing mechanism are vertically distributed at intervals and are fixedly arranged on the inner periphery of the filter pressingcavity; the first filter pressing mechanism is close to the feeding port, and has a mesh number of 60-80; and the second filter pressing mechanism is close to the sulfanilamide filtrate outlet, and has a mesh number of 100-120. According to the invention, through the structural design of the filter pressing device, the removal of the high-content decolorizing agent and the high-content impuritiesin the decoloration process can be ensured, and the purity of the sulfadoxine finished product is further ensured.

Description

technical field [0001] The invention belongs to the technical field of preparation of sulfonamide antibacterial drugs, and in particular relates to a high-purity decolorization and pressure filtration process of sulfonamide. Background technique [0002] Zhouxiao sulfonamide, also known as Zhouxiao sulfonamide, sulfa-o-dimethoxine or 4-sulfa-5,6-dimethoxypyrimidine, is a white or off-white crystalline powder with a slightly bitter taste, odorless, and gradually changes color when exposed to light. Slightly soluble in water, methanol and ethanol, insoluble in ether, soluble in sodium hydroxide and dilute inorganic acids, belonging to sulfonamide antibacterial drugs. Sulfonamide has the characteristics of long curative effect and low toxicity. It can treat common inflammations, such as upper respiratory tract infection pancreatitis, bacillary dysentery enteritis and skin infection, and it has a certain curative effect on the treatment of pulmonary tuberculosis and lymphatic tu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D29/01B01D29/58C07D239/69
CPCB01D29/01B01D29/58C07D239/69B01D2201/202
Inventor 李涛徐盛杰
Owner CHANGSHU JINSHEN MEDICAL PROD CO LTD
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