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A kind of high-purity decolorization filter press technology of cycle-effective sulfonamide

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 problems of not specifically disclosing the refined processing and purification method of crude sulfonamide, impossibility of direct application, high impurity content, etc.

Active Publication Date: 2022-04-01
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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  • A kind of high-purity decolorization filter press technology of cycle-effective sulfonamide
  • A kind of high-purity decolorization filter press technology of cycle-effective sulfonamide
  • A kind of high-purity decolorization filter press technology of cycle-effective sulfonamide

Examples

Experimental program
Comparison scheme
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 decolorization and filter-pressing process for cycle-effect sulfonamide. The activated carbon decolorization process includes adding activated carbon to a solution of the cycle-effect sulfonamide crude product for adsorbing impurities, and after cooling, the material is fed into a filter press for filtration, wherein , the filter press includes a filter press cavity with a periodic sulfonamide filtrate outlet at the bottom and a feeding port on the upper part. The pressure device is connected to inject pressure into the filter press chamber. The first filter press mechanism and the second filter press mechanism are fixedly arranged around the filter press chamber and are distributed at an upper and lower interval. The first filter press mechanism is close to the feeding port, and its mesh size is The range is 60-80 meshes, and the second filter press mechanism is close to the outlet of the periodic sulfonamide filtrate, and its mesh number is in the range of 100-120 meshes; the present invention, through the structural design of the filter press device, can ensure that the decolorizing agent in the decolorization process can be removed. And impurities are removed at a high content to further ensure the purity of the finished products of Zhouxiao sulfonamide.

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 Patents(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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