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Sinomenine hydrochloride and preparation method thereof

A technology of sinomenine hydrochloride and centrifugal extractor, which is applied in the direction of organic chemistry, can solve the problems of serious extraction emulsification, difficulty in two-phase separation, and low extraction production efficiency

Inactive Publication Date: 2018-08-03
HUNAN ZHENGQING PHARM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] It was found in production that the above-mentioned extraction process has the following problems: the extraction emulsification is serious, and the two-phase separation is difficult after the liquid medicine and the extraction agent chloroform are mixed, so that the waiting time for separation is very long (one tank needs 2 to 3 days), and some The emulsification is seriously unable to separate (about 20%) and discarded, resulting in low extraction production efficiency and low production yield

Method used

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  • Sinomenine hydrochloride and preparation method thereof
  • Sinomenine hydrochloride and preparation method thereof
  • Sinomenine hydrochloride and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

experiment example 1

[0024] 1. Description of the original extraction process (mixed and clarified)

[0025] Process method

[0026] Pump the liquid to be extracted (volume V) into the extraction tank, extract twice with chloroform as follows, and combine the extracts.

[0027] The first extraction: pump 1 / 2 times the amount of chloroform into the extraction tank, and start the extraction tank stirrer to stir for 30 minutes. After 30 minutes, stop stirring, let the layers stand for more than 1 hour, and slowly put the lower chloroform layer into the extract storage tank. After putting the layered chloroform, stir it 3 times, then let the layers stand for more than 1 hour, and then slowly put the lower layer of chloroform into the extract storage tank. Repeat the above inching stirring, standing and layering methods, so that the extraction yield meets the requirements (extraction yield = the amount of the extracted extract / the amount of chloroform fed, the requirement is ≥ 80.0%).

[0028] The s...

experiment example 2

[0085] Experimental Example 2: Experimental Research Data

[0086] 1. Purpose of the experiment

[0087] In order to solve the problems of emulsification, difficult stratification and small processing capacity in the current mixing and clarification extraction process, after preliminary experiments, the centrifugal extraction machine can use centrifugal method to quickly and effectively break the emulsion and separate, solve the problem, and realize continuous production. In order to confirm the feasibility of the centrifugal extraction process and determine the extraction and separation conditions of the centrifugal extraction machine, an extraction experiment was carried out.

[0088] 2. Experimental method

[0089] (1) Process design

[0090] Basic process: take Qingfengteng percolation alkalization solution (take Qingfengteng, use 0.3mol / L hydrochloric acid solution as solvent, wet, impregnate, percolate, add calcium hydroxide to the percolation liquid to adjust the pH v...

Embodiment 1

[0149] Embodiment 1: Single-stage extraction prepares sinomenine hydrochloride

[0150] Extract with a single centrifugal extractor, turn on the drum motor of the centrifugal extractor, and extract the liquid medicine at a rate of 10,000 liters / hour; connect two extraction centrifuges, turn on the drum motor of the centrifugal extractor, and extract the liquid medicine at a rate of 10,000 liters / hour The speed is pumped in from the light phase inlet of the first-stage centrifugal extractor, and then flows through the second-stage centrifugal extractor; the extraction agent chloroform is pumped in from the heavy-phase inlet of the second-stage centrifugal extractor at a speed of 7500 liters / hour, and then flows through the first-stage centrifugal extractor. Centrifugal extractor to collect the extract.

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Abstract

The invention discloses sinomenine hydrochloride and a preparation method thereof. According to the technical scheme, sinomenine hydrochloride is prepared with a single-stage extraction or multi-stageextraction method. The single-stage extraction is based on a single centrifugal extractor for extraction, a centrifugal extractor drum motor is started, a liquid medicine is pumped into the centrifugal extractor from a light phase inlet at a speed of 10000 L / h, an extraction agent chloroform is pumped into the centrifugal extractor from a heavy phase inlet at a speed of 7500 L / h, and extract liquor is collected; the multi-stage extraction is based on two or more centrifugal extractors for extraction in a series-connection manner.

Description

technical field [0001] The invention relates to a preparation method of medicine, in particular to a sinomenine hydrochloride and a preparation method thereof. Background technique [0002] The production of sinomenine hydrochloride is carried out according to the patented process (application number ZL201110361882.0 or 201410366210.2), including crude and refined production. The crude product production process is as follows: take Qingfengteng, carry out heavy percolation with dilute hydrochloric acid, alkalinize the percolation liquid, centrifuge, then extract twice with chloroform, concentrate and crystallize. Among them, the realization of the extraction process is the traditional mixed clarification type - the extraction tank type, that is, the liquid medicine and the extraction agent chloroform are placed in the extraction tank together, stirred and mixed, left to clarify and separate, and the lower layer of the extract is released. Extract twice and combine the extra...

Claims

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Application Information

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IPC IPC(8): C07D221/28
CPCC07D221/28
Inventor 彭祖仁刘翘翘杨远香龙宪军王鹏滕健仇萍吴飞驰
Owner HUNAN ZHENGQING PHARM GRP CO LTD
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