Recovery process of analginum finished product centrifugal mother liquid

A technology of centrifugal mother liquor and analgin, which is applied in the field of medicine and chemical industry, can solve the problems of potential safety hazards and non-compliance with environmental protection requirements, and achieve the effect of easy industrial production, compliance with environmental protection and audit requirements, and high crystallization rate

Active Publication Date: 2012-07-18
SHANDONG XINHUA PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ethanol and other gases emitted from materials exposed to the open not only pose safety hazards but also do not meet current environmental protection requirements

Method used

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  • Recovery process of analginum finished product centrifugal mother liquid
  • Recovery process of analginum finished product centrifugal mother liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Measure 4000ml of analgin finished centrifuged mother liquor, first use the recovery tower to concentrate to a density of 1.21g / ml, and then use a concentrator to concentrate, control the concentration temperature to 70±10°C, vacuum degree to -0.05MP, and concentrate to a density of 1.30 g / ml, its loss on drying is 18.0%; add anhydrous methanol (methanol purity ≥ 99%) to dissolve; after the material is completely dissolved, open the interlayer circulating water to cool down, cool down to 67°C after 1.5 hours, use salt water to cool down, and Cool down to 35°C in 3.5 hours, turn off the brine and prepare for centrifugation; adjust the speed of the centrifuge to 1200 rpm, feed and centrifuge, after centrifuging for 40 minutes, stop the centrifuge, wash with 230g of anhydrous methanol, centrifuge for 40 minutes, and discharge . The content of the crude product of Analgin in the primary recycled material of Analgin is 77.28%, and the crystallization rate of the finished cen...

Embodiment 2

[0026] Measure 4000ml of analgin finished centrifuged mother liquor, concentrate it with a concentrator, control the concentration temperature at 81.5±10.5°C, vacuum degree at -0.07MP, concentrate to a density of 1.40g / ml; add 90kg of anhydrous isopropanol, and continue to concentrate When the weight loss on drying is 14.5%, add isopropanol (isopropanol purity ≥ 99%) to dissolve; after all the materials are dissolved, open the interlayer circulating water to cool down, and cool down to 60°C after 2.0 hours, then use salt water to cool down, after 4.5 hours Cool down to 25°C, turn off the brine and prepare for centrifugation; adjust the speed of the centrifuge to 1200 rpm, feed the material for centrifugation, and after centrifugation for 40 minutes, stop the centrifuge, wash with 230g of anhydrous isopropanol and then centrifuge for 40 minutes, discharge the material . The content of the crude product of Analgin in the primary recycled material of Analgin is 78.33%, and the cr...

Embodiment 3

[0028] Measure 4000ml of analgin finished centrifuged mother liquor, first use the recovery tower to concentrate to a density of 1.225g / ml, and then use a concentrator to concentrate, control the concentration temperature to 89±2°C, vacuum degree to -0.08MP, and concentrate to a density of 1.45 g / ml, add dehydrated ethanol (ethanol purity ≥ 99%) 89kg, continue to concentrate until the loss on drying is 12.5%, then add dehydrated ethanol to dissolve, after the materials are all dissolved, open the interlayer circulating water to cool down, after 1.5 hours, cool down to 68°C, switch to brine to cool down, cool down to 25°C after 5.5 hours, turn off the brine and prepare for centrifugation; adjust the speed of the centrifuge to 1200 rpm, feed the material for centrifugation, and after centrifugation for 40 minutes, stop the centrifuge and use 230g of absolute ethanol After washing, centrifuge for 40 minutes and discharge. The content of the crude product of Analgin in the primary...

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Abstract

The invention belongs to the field of medicine chemical and particularly relates to a recovery process of analginum finished product centrifugal mother liquid. Firstly, the analginum finished product centrifugal mother liquid is concentrated, then, organic solvents are added into concretes for dissolution, and analginum primary recovery materials and secondary recovery mother liquid are prepared through temperature reduction, crystallization and centrifugation. The recovery process provided by the invention has the advantages that the process is simple, the content in the analginum primary recovery materials can reach 77 to 80 percent, and the crystallization rate of the finished product centrifugation mother liquid reaches 84 to 92 percent. The centrifugation rate is improved, the analginum content in the secondary recovery mother liquid only accounts for 3 to 5 percent of the total theoretical quantity of the analginum, and the secondary recovery mother liquid can be directly delivered to aminopyrine waste mother liquid methylation posts. The recovery temperature reduction problem of secondary recovery mother liquid to quartic recovery mother liquid is avoided. An open type stainless steel groove can be directly removed, the in-site environment is obviously improved, and the recovery process more perfectly conforms to the environment-protection and audit requirement. The analginum recovery purity is high, the crystallization rate is high, the pollution is avoided, and the industrial production is easily realized.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, in particular to a recovery process of analgin finished centrifuged mother liquor. Background technique [0002] The crystallization rate of Analgin finished product is about 73%, and about 27% of Analgin enters the centrifuged mother liquor. The existing mother liquor recovery process is: concentrate the finished centrifuged mother liquor, cool down, crystallize, and centrifuge to recover Analgin once. material and the secondary recovery mother liquor, the secondary recovery mother liquor is concentrated, cooled, crystallized, and centrifuged to obtain the secondary recovery material of analgin and the mother liquor of the third recovery of analgin, the content of the secondary recovery material of analgin is about 75%, and the crystallization rate It is about 35%, and so on, until recycling to analgin four recycling materials. The content of the third recycling material and the fo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D231/48
Inventor 王凯广万士元未雅楠
Owner SHANDONG XINHUA PHARMA CO LTD
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