Magnetic solid acid catalyst and application thereof to extracting saponin

A magnetic solid acid and catalyst technology, applied in physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, organic chemistry, etc., can solve problems such as biomass hydrolysis research, and achieve practicability and applicability wide range, mild reaction conditions, and environmental friendliness

Active Publication Date: 2019-02-22
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, great progress has been made in the theoretical and applied research of solid acids at home and abroad, but there are still some problems to be solved, such as the theoretical research on the hydrolysis of solid acids needs to be strengthened, and its industrial application research needs to be further deepened, especially There are few researches on the hydrolysis of biomass for special purposes

Method used

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  • Magnetic solid acid catalyst and application thereof to extracting saponin
  • Magnetic solid acid catalyst and application thereof to extracting saponin
  • Magnetic solid acid catalyst and application thereof to extracting saponin

Examples

Experimental program
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Effect test

Embodiment 1

[0045] A kind of magnetic solid acid catalyst, its preparation method comprises the steps:

[0046] 1) Fe 3 o 4 Granules and tetraethoxysilane as the main raw materials were prepared by sol-gel method to Fe 3 o 4 @SiO 2 Particles; specifically comprise the steps of: weighing Fe 3 o 4 Particles (1.0g) were dispersed in a mixed solution of 60mL of absolute ethanol and 15mL of distilled water by ultrasound for 10min, mechanically stirred at room temperature for 20min, and then 1mL of ammonia water was added (one-time addition); after stirring evenly, 1mL of TEOS+10mL of Water ethanol solution (30min drop); stir at room temperature for 16h after dropwise addition; use magnet to separate Fe 3 o 4 @SiO 2 Particles were washed three times with distilled water and ethanol, and dried under vacuum at 60°C;

[0047] 2) Weigh 1g Fe 3 o 4 @SiO 2 Particles, ultrasonically dispersed in a mixed solution of 60mL ethanol and 15mL distilled water, mechanically stirred for 20min at ro...

Embodiment 2

[0054] Step 1 described in embodiment 2) adopts sol-gel method to prepare Fe 3 o 4 @SiO 2 Particle, and step 3) sulfonation reaction is identical with embodiment 1, difference is: step 2) Fe 3 o 4 @SiO 2 @NH-(CH 2 ) 2 -NH 2 The preparation conditions of the particles are different. Its preparation method is as follows:

[0055] Weigh 1g Fe 3 o 4 @SiO 2 Particles were ultrasonically dispersed in a mixed solution formed by 25mL of anhydrous toluene, mechanically stirred at 110°C for 2h under the protection of argon, and after stirring evenly, 2mL of N-[3-(trimethoxysilyl)propane was added dropwise with a constant pressure funnel. Base] ethylenediamine solution, continue to mechanically stir for 18h; use a magnet to separate Fe 3 o 4 @SiO 2 @NH-(CH 2 ) 2 -NH 2 , washed three times with distilled water and ethanol, and dried under vacuum at 60°C.

Embodiment 3

[0057] Step 1 described in embodiment 3) adopts sol-gel method to prepare Fe 3 o 4 @SiO 2 Particle, and step 3) sulfonation reaction is identical with embodiment 1, difference is: step 2) Fe 3 o 4 @SiO 2 @NH-(CH 2 ) 2 -NH 2 The preparation conditions of the particles are different. Its preparation method is as follows:

[0058] Weigh 0.5g Fe 3 o 4 @SiO 2Particles, ultrasonically dispersed in the mixed solution formed by 50mL cyclohexane, add 1.5g Span-80, mechanically stir at room temperature for 20min, then add 1mL of ammonia water (one-time addition), after stirring evenly, add 1mL dropwise with a constant pressure funnel N-[3-(trimethoxysilyl)propyl]ethylenediamine solution, continue to stir at room temperature for 16h; use a magnet to separate Fe 3 o 4 @SiO 2 @NH-(CH 2 ) 2 -NH 2 , washed three times with distilled water and ethanol, and dried under vacuum at 60°C.

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Abstract

The invention discloses a magnetic solid acid catalyst which uses Fe3O4 as a magnetic core. Tetraethoxysilane and N-[3-(trimethoxysilyl)propyl]ethylenediamine are subjected to sol-to-gel reaction in water and ethanol solution separately, the surface of the magnetic core is coated with amino silica, and a sulfonic acid group is modified by the sulfonation reaction of chlorosulfonic acid, so that magnetic solid acid is obtained. The invention proposes that the magnetic solid acid catalyst is applied to the hydrolysis of dioscorea nipponica and the like to extract saponin for the first time, theobtained magnetic solid acid has high catalytic activity and environmental friendliness, the yield of saponin is effectively improved, and remarkable environmental and economic benefits are achieved.

Description

technical field [0001] The invention belongs to the technical field of magnetic nano catalysts, in particular to a magnetic solid acid catalyst and its application for extracting saponin. 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 traditional methods all use inorganic strong acid hydrolysis. The coexistence problems are high acidity, high chroma, high salinity, and complex composition of high-concentration organic wastewater, which is difficult to treat and causes great environmental pollution. Become the bottleneck restricting the industrial production of saponin. It is v...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/28C07J71/00
CPCC07J71/00B01J31/28B01J35/0033
Inventor 周红张发蓉潘志权程清蓉
Owner WUHAN INSTITUTE OF TECHNOLOGY
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