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Preparation method for magnetic solid acid catalyst and extraction process for saponin

A magnetic solid acid, extraction process technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compound/hydride/coordination complex catalysts, etc. and other problems, to achieve the effect of reducing extremely high COD, reducing environmental pollution and restoring activity

Inactive Publication Date: 2019-05-03
HUBEI DANAO PHARMA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The coexistence problems of the existing production methods are high acidity, large chroma, high salinity, and a large amount of high-concentration organic wastewater with complex composition, which is difficult to treat and seriously pollutes the environment, which has become a bottleneck restricting the industrial production of saponin

Method used

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  • Preparation method for magnetic solid acid catalyst and extraction process for saponin
  • Preparation method for magnetic solid acid catalyst and extraction process for saponin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] The present embodiment provides a kind of preparation method of magnetic solid acid catalyst, it comprises the following steps,

[0044] S1, preparation of magnetic Fe 3 o 4 particles.

[0045] S1-1, take 200mL of 0.12mol / L FeCl 3 solution, stirring to remove oxygen, and heating to 40°C;

[0046] S1-2, add 200mL 0.06mol / L FeSO 4 solution, stir evenly, add 30mL 0.12mol / L NaOH solution, and crystallize for 0.5h;

[0047] S1-3, then add 1.5g trisodium citrate dihydrate, heat up to 80°C, activate Fe 3 o 4 20-40 minutes on the particle surface, cooling after the reaction is completed;

[0048] S1-4, separate the black particles, wash the solution to neutral, vacuum dry and grind to obtain a uniform powder.

[0049] S2, in magnetic Fe 3 o 4 The particle surface is coated with a layer of SiO 2 .

[0050] S2-1, take 2.0g magnetic Fe 3 o 4 Ultrasonic dispersion of particles in a mixture of ethanol and distilled water (V / V=4:1);

[0051] S2-2, add 2mL of 28%wt ammo...

Embodiment 2

[0058] The present embodiment provides a kind of preparation method of magnetic solid acid catalyst, it comprises the following steps,

[0059] S1, preparation of magnetic Fe 3 o 4 particles.

[0060] S1-1, take 200mL of 0.10mol / L FeCl 3 solution, stirring to remove oxygen, and heating to 50°C;

[0061] S1-2, add 200mL 0.04mol / L FeSO 4 solution, stir evenly, add 30mL 0.10mol / L NaOH solution, and crystallize for 1.0h;

[0062] S1-3, add 1.0g trisodium citrate dihydrate, raise the temperature to 90°C, activate Fe 3 o 4 30 minutes on the particle surface, cooling after the reaction is completed;

[0063] S1-4, separate the black particles, wash the solution to neutral, vacuum dry and grind to obtain a uniform powder.

[0064] S2, in magnetic Fe 3 o 4 The particle surface is coated with a layer of SiO 2 .

[0065] S2-1, take 1.8g magnetic Fe 3 o 4 Ultrasonic dispersion of particles in a mixture of ethanol and distilled water (V / V=4:1);

[0066] S2-2, add 2mL of 25%w...

Embodiment 3

[0073] The present embodiment provides a kind of preparation method of magnetic solid acid catalyst, it comprises the following steps,

[0074] S1, preparation of magnetic Fe 3 o 4 particles.

[0075] S1-1, take 200mL 0.15mol / L FeCl 3 solution, stirring to remove oxygen, and heating to 60°C;

[0076] S1-2, add 200mL 0.08mol / L FeSO 4 solution, stir evenly, add 30mL 0.15mol / L NaOH solution, and crystallize for 1.5h;

[0077] S1-3, add 2.0g trisodium citrate dihydrate, raise the temperature to 100°C, activate Fe 3 o 4 40min on the particle surface, cooling after the reaction is completed;

[0078] S1-4, separate the black particles, wash the solution to neutral, vacuum dry and grind to obtain a uniform powder.

[0079] S2, in magnetic Fe 3 o 4 The particle surface is coated with a layer of SiO 2 .

[0080] S2-1, take 2.2g magnetic Fe 3 o 4 Ultrasonic dispersion of particles in a mixture of ethanol and distilled water (V / V=4:1);

[0081] S2-2, add 2mL of 30%wt ammon...

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Abstract

The invention provides a preparation method for a magnetic solid acid catalyst and an extraction process for saponin. According to the invention, magnetic solid acid is utilized as a catalyst for hydrolysis of dioscin, has highly-efficient catalytic performance, can be separated through magnetic adsorption, and is recovered and reutilized, and during hydrolysis of the dioscin, an aqueous solutioncan be recovered and reutilized, so massive discharging with high acidity, high organic matter concentration and complicated components due to hydrolysis of strong acid can be avoided, and environmental pollution caused by massive discharging is greatly reduced; through highly-efficient utilization of Dioscorea Zingiberensis resources, the saponin can be obtained in the whole process, and cellulose and starch are separated from Dioscorea Zingiberensis by adoption of a double separation method at the same time, so the problem of extremely high content of COD in a mother liquor due to hydrolysisof the cellulose and the starch is greatly reduced; meanwhile, the starch can be recovered to be used as a raw material for the alcoholic beverage production industry, and the cellulose can be used as a raw material of a compound fertilizer, so a clean and high-efficiency production process route is provided for extraction of the saponin from the Dioscorea Zingiberensis; and in order to minimizethe discharge of a waste liquid and waste residues, a water circulation process is adopted in the process route, so clean production is realized.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a preparation method of a magnetic solid acid catalyst and a saponin extraction process. Background technique [0002] Saponin is a pharmaceutical intermediate with high medicinal value. It is an irreplaceable raw material for the production of four categories of steroid hormone drugs, including anabolic hormone, adrenocortical hormone, sex hormone and progesterone. It is known as "medicinal gold ". Saponin is mainly obtained by hydrolysis of diosgenin contained in the rhizomes of Dioscoreaceae plants (turmeric, pangolin, etc.). The coexistence problems of the existing production methods are high acidity, high chroma, high salinity, and a large amount of high-concentration organic wastewater with complex composition, which is difficult to treat and seriously pollutes the environment, which has become a bottleneck restricting the industrial production of saponin. It is very imp...

Claims

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Application Information

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IPC IPC(8): B01J31/28C07J71/00C08B30/04D21C5/00
Inventor 崔立新熊丽崔潆文
Owner HUBEI DANAO PHARMA CO LTD