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Mixed solvent low-pressure fluid critical extract method

A technology of mixed solvents and extraction methods, applied in the direction of solid solvent extraction, etc., can solve the problems of large direct impact, large environmental pollution, high production cost, etc., and achieve the effects of reducing the loss of volatile substances, improving product purity, and improving extraction efficiency

Inactive Publication Date: 2009-07-08
符文飙
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantages of the traditional method are complex process, time-consuming, large environmental pollution, low product purity and easy residue of harmful substances
The carbon dioxide supercritical extraction method that has emerged in recent years can produce high-purity products with specific properties, but the operating pressure is high (10-60Mpa) and the equipment manufacturing cost is expensive, making it difficult to achieve large-scale production
Chinese patent application number 200610070495.0 discloses "a low-pressure supercritical extraction process and its equipment", which uses 1,1,1,2-tetrafluoroethane tetrafluoroethane (chemical code HFC-134a) as the critical extraction Solvent, although its operating pressure is lower than the carbon dioxide supercritical extraction method, but because 1,1,1,2-tetrafluoroethane is a greenhouse gas, it can block infrared radiation from returning to the sky, and has a direct impact on global warming. Its global warming potential value GWP is as high as 1300, so its emission (emission), use, and production are subject to strict international controls; moreover, the unit price of industrial-grade 1,1,1,2-tetrafluoroethane is higher than food-grade carbon dioxide More than 50 times, used as an extractant, the production cost is high, which is also unacceptable for enterprises in industrial production

Method used

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  • Mixed solvent low-pressure fluid critical extract method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Embodiment 1: extract lavender oil from lavender

[0024] ①Preparation

[0025] Clean the equipment and pipelines, confirm that the water, electricity, gas and other equipment are in a normal state of operation, and confirm that the valves are in the correct position;

[0026] ②Extraction

[0027] (A) material lavender is placed in the extraction tank with jacket, then airtight, extraction tank, separation tower and pipeline are evacuated to<-0.08Mpa and keep airtight;

[0028] (B) 95% by weight of 1,1,1,2-tetrafluoroethane and 5% by weight of n-butane are mixed uniformly as a mixed solvent, which is pressurized and pumped into the extraction tank, and simultaneously Heat hot water in the jacket, control the temperature of the extraction tank to 35°C, and the pressure to 2.5Mpa. The mixed solvent is in liquid state and contacts with the material to dissolve the active ingredients of the material. After maintaining this temperature and pressure for 10 minutes, the extr...

Embodiment 2

[0036] Embodiment 2: extract essential oil (star anise oil) from star anise

[0037] Step 1. and 4. are identical with embodiment 1, difference is:

[0038] ②Extraction

[0039] (A) place the material star anise in the extraction tank with jacket, then airtight, vacuumize the extraction tank, separation tower and pipeline to <-0.08Mpa and keep airtight;

[0040] (B) 92% by weight of 1,1,1,2-tetrafluoroethane and 8% by weight of n-butane are mixed uniformly as a mixed solvent, which is pressurized and pumped into the extraction tank, and simultaneously Heating with hot water in the jacket, control the temperature of the extraction tank at 40°C, and the pressure at 1.0-3.0Mpa. The mixed solvent is in liquid state and contacts with the material to dissolve the active ingredients of the material. After maintaining this temperature and pressure for 10 minutes, the extraction tank begins to emit The liquid of the active ingredient is sent to the heat exchanger to be heated while m...

Embodiment 3

[0043] Embodiment 3: extract alkane base oil from waste sludge oil

[0044] Step 1. and 4. are identical with embodiment 1, difference is:

[0045] ②Extraction

[0046] (A) Put the material waste sludge oil in an extraction tank with a jacket, and its filling capacity is 75-85% of the volume of the extraction tank, then seal it, and vacuumize the extraction tank, separation tower and pipeline to <-0.08 Mpa and keep airtight;

[0047] (B) 85% by weight of 1,1,1,2-tetrafluoroethane and 15% by weight of n-butane are mixed uniformly as a mixed solvent, and it is pressurized and pumped into the extraction tank, and the stirring is started Mix the mixed solvent and waste sludge oil evenly, and heat the jacket with hot water at the same time. Control the temperature of the extraction tank at 75°C and the pressure at 1.0-3.5Mpa. The mixed solvent is in a liquid state and contacts with the material to dissolve the active ingredients of the material. Keep this After 10 minutes of tempe...

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Abstract

The invention relates to a method for critically extracting component solvent low pressure fluid, which comprises extraction, separation and solvent recovery. The method is characterized in that 75-95 wt% of 1, 1, 1, 2-tetrafluoroethane and 5-25 wt% of normal butane are taken as component solvent; in the extracting process, the component solvent is controlled to be in a liquid to be contacted with materials to lead the active ingredients of the materials to be dissolved in the liquid component solvent; in the separating process, the component solvent is controlled to be in a gas state and separated from the extracted liquid active ingredients; the separated component solvent is compressed and cooled to become liquid in a mixed state, and then is recovered for cyclic utilization; and the steps of extraction, separation and solvent recovery are carried out in a sealing state at the same time. The operating pressure and the manufacturing cost of the equipment are both lower than those of a carbon dioxide supercritical extraction method; the GWP of the component solvent is lower than that of the 1, 1, 1, 2-tetrafluoroethane, so that the method of the invention is in accordance with environmental requirements, is low in price and has high extraction efficiency.

Description

technical field [0001] The invention relates to a mixed solvent low-pressure fluid critical extraction method. It is especially suitable for the extraction of active ingredients contained in natural plants and Chinese herbal medicines. Background technique [0002] Traditional methods for extracting active ingredients from natural plants and Chinese herbal medicines include steam distillation, vacuum distillation, and solvent extraction. The disadvantages of the traditional method are complex process, time-consuming, great environmental pollution, low product purity and easy residue of harmful substances. Although the carbon dioxide supercritical extraction method that has emerged in recent years can produce high-purity products with specific properties, it is difficult to achieve large-scale production due to high operating pressure (10-60Mpa) and expensive equipment manufacturing costs. Chinese patent application number 200610070495.0 discloses "a low-pressure supercriti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D11/02
Inventor 符文飙
Owner 符文飙
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