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Monitoring method for liquid holdup in process of preparing high-purity elemene

A technology of elemene and liquid holding capacity, which is applied in the field of separation and rectification of natural medicines to achieve the effects of stabilizing product quality, stabilizing column efficiency and improving purity

Active Publication Date: 2019-07-16
JINGANG PHARMA DALIAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, there is no method for monitoring and controlling liquid holdup to control product quality in the existing rectification technology

Method used

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  • Monitoring method for liquid holdup in process of preparing high-purity elemene
  • Monitoring method for liquid holdup in process of preparing high-purity elemene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] A method for monitoring liquid holdup in the process of preparing high-purity elemene:

[0029] A. Put 3000 grams of turmeric oil into the tower kettle of the vacuum precision fractionation equipment. The tower kettle starts to set the heating temperature to 300°C, adjust the valve on the vacuum pipeline to control the vacuum degree below 500Pa, until there is reflux, adjust the tower kettle Set the temperature at 260°C for 30 minutes of full reflux and begin to receive Fraction 1. The liquid holdup of Fraction 1 is controlled at 4mL / min, and the reflux ratio is controlled at 4:1;

[0030] B. Until crystallization occurs, begin to receive fraction 2 until the crystallization disappears;

[0031] C. Full reflux for 60 minutes;

[0032] D. Start to receive fraction three after step C, the liquid hold-up is controlled at 2mL / min, and the reflux ratio is controlled at 5:1 until the fractions received are clearly stratified;

[0033] E. Start receiving fraction 4 after ste...

Embodiment 2

[0035] A method for monitoring liquid holdup in the process of preparing high-purity elemene:

[0036] A. Put 3000 grams of turmeric oil into the tower kettle of the vacuum precision fractionation equipment. The tower kettle starts to set the heating temperature to 300°C, adjust the valve on the vacuum pipeline to control the vacuum degree below 500Pa, until there is reflux, adjust the tower kettle Set the temperature at 260°C for 30 minutes of total reflux and begin to receive Fraction 1. The liquid holdup of Fraction 1 is controlled at 7mL / min, and the reflux ratio is controlled at 4:1;

[0037] B. Until crystallization occurs, begin to receive fraction 2 until the crystallization disappears;

[0038] C. Full reflux for 60 minutes;

[0039] D. Start to receive fraction three after step C, the liquid hold-up is controlled at 5mL / min, and the reflux ratio is controlled at 5:1 until the fractions received are clearly stratified;

[0040] E. Start to receive fraction 4 after s...

Embodiment 3

[0042] A method for monitoring liquid holdup in the process of preparing high-purity elemene:

[0043] A. Put 3000 grams of turmeric oil into the tower kettle of the vacuum precision fractionation equipment. The tower kettle starts to set the heating temperature to 300°C, adjust the valve on the vacuum pipeline to control the vacuum degree below 500Pa, until there is reflux, adjust the tower kettle Set the temperature at 260°C for 30 minutes of full reflux and begin to receive Fraction 1. The liquid holdup of Fraction 1 is controlled at 11mL / min, and the reflux ratio is controlled at 4:1;

[0044] B. Until crystallization occurs, begin to receive fraction 2 until the crystallization disappears;

[0045] C. Full reflux for 60 minutes;

[0046] D. Start to receive fraction three after step C, the liquid hold-up is controlled at 7mL / min, and the reflux ratio is controlled at 5:1 until the fractions received are clearly stratified;

[0047]E. Start to receive fraction 4 after st...

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Abstract

The invention belongs to the technical fields of natural medicine separation and rectification, and discloses a monitoring method for a liquid holdup in the process of preparing high-purity elemene. Under a certain heating temperature and vacuum degree of a tower kettle, more gas-liquid conversion times in a rectification column, less gas that rises to a condenser part per unit time, an amount ofliquid condensed by the condenser, that is, the liquid holdup is monitored, so that the fractional distillation effect in the rectification column can be judged. The method provided by the invention can obtain a liquid holdup range of the stably-produced high-quality product, determine the control range of liquid holdup, monitor the liquid holdup in the production process, and timely adjust the liquid holdup to achieve the purpose of stably producing the high-quality product.

Description

technical field [0001] The invention belongs to the technical field of separation and rectification of natural medicines, and relates to a method for monitoring liquid holdup in the process of preparing high-purity elemene. Background technique [0002] In the 1970s, it was found that the zedoary oil extracted from the curcuma had antiviral and anti-tumor effects; in the 1990s, elemene was isolated from the turmeric oil. After research, it was believed that elemene is an effective anti-tumor ingredient. The mechanism is that elemene has a strong affinity with tumor cells. By destroying the tumor cell membrane, it changes the permeability of the tumor cell membrane, leading to the leakage of the tumor cell interstitium and inducing tumor cell apoptosis. Elemene can play a better role in direct contact with tumor cells. its antitumor efficacy. Therefore, it is of great significance to realize the industrialization of the production of elemene and to obtain high-purity elemene...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C7/04C07C13/19
CPCC07C7/04C07C2601/14C07C13/19
Inventor 张立华刘登禹王琼
Owner JINGANG PHARMA DALIAN
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