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A coated magnetic nano-fe 3 o 4 Application of supported palladium catalyst in the preparation of lactic acid from glycerol

A magnetic nano, palladium catalyst technology, applied in the direction of organic compound/hydride/coordination complex catalyst, oxidative preparation of carboxylic acid, physical/chemical process catalyst, etc., can solve the problem of long reaction time, low catalyst recycling rate, precious metal High catalyst cost and other problems, to achieve the effect of fast reaction rate, good industrialization prospects, and high selectivity of target products

Active Publication Date: 2020-01-24
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Aiming at the problems of high reaction temperature, high pressure, long reaction time, high cost of noble metal catalysts and low catalyst recycling rate in the prior art, the present invention proposes to use recyclable coated magnetic nano-Fe 3 o 4 Supported palladium catalyst, the noble metal alloy catalyst has high catalytic activity of glycerin to prepare lactic acid, and has good recycling characteristics

Method used

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  • A coated magnetic nano-fe  <sub>3</sub> o  <sub>4</sub> Application of supported palladium catalyst in the preparation of lactic acid from glycerol
  • A coated magnetic nano-fe  <sub>3</sub> o  <sub>4</sub> Application of supported palladium catalyst in the preparation of lactic acid from glycerol
  • A coated magnetic nano-fe  <sub>3</sub> o  <sub>4</sub> Application of supported palladium catalyst in the preparation of lactic acid from glycerol

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Magnetic nano-Fe coated with mesh-like polyaniline with 1% loading 3 o 4 supported palladium catalyst (Fe 3 o 4 @MOPPA-Pd 1 ) Preparation: Carrier Fe 3 o 4 Preparation of @MOPPA: In an air atmosphere, add 0.8g of magnetic nano Fe to the round bottom flask in sequence 3 o 4 , 8.0mmol anhydrous FeCl 3 , 8.0 mmol FDA and 40 mL 1,2-dichloroethane (DCE). Stir for 30min and then slowly add 30mL of a DCE solution of 3mmol aniline dropwise. After the dropwise addition, the reaction was stirred at room temperature for 60 minutes, then the temperature was raised to 50° C. for 6 hours, and the temperature was further raised to 75° C., and then stirred for 24 hours. After the reaction is completed, filter, and the filter cake is washed with deionized water and methanol in turn until the filtrate is colorless, and the pH is measured to be 7-8. It was then washed with acetone for 20 h in a Soxhlet extractor and dried under vacuum at 65 °C to obtain 1.0 g of brown Fe 3 o 4...

Embodiment 2

[0051] Homogeneous and eggshell mesh-like polyaniline-coated magnetic nano-Fe with 3% loading 3 o 4 supported palladium catalyst (Fe 3 o 4 @MOPPA-Pd 3 ) Preparation: Carrier Fe 3 o 4 The preparation conditions and steps of @MOPPA are the same as Fe in Example 1 3 o 4 @MOPPA-Pd 1 The preparation method of the catalyst carrier is the same.

[0052] Homogeneous mesh-like polyaniline-coated magnetic nano-Fe 3 o 4 Loaded palladium catalyst: weigh 52.6mg PdCl 2 Dissolve in 10mL water, then add 7mL 1mol / L HCl. Add 1.0g Fe to the solution at 30°C 3 o 4 @MOPPA stirring for 20h. Weigh 251.8mg Na 2 CO 3 Dissolve in water to form a solution, filter and soak in 10mL Na 2 CO 3 in aqueous solution. Wash about 5 times with 10mL water, and finally get the catalyst Fe containing about 50% water 3 o 4 @MOPPA-Pd 3 .

[0053] Eggshell-shaped grid-like porous polyaniline-coated magnetic nano-Fe 3 o 4 Loaded palladium catalyst: weigh 1.52g Na 2 CO 3Dissolved in water to fo...

Embodiment 3

[0065] Homogeneous and eggshell-type porous network polyaniline-coated magnetic nano-Fe with 5% loading 3 o 4 supported palladium catalyst (Fe 3 o 4 @MOPPA-Pd 5 ) Preparation: Carrier Fe 3 o 4 The preparation conditions and steps of @MOPPA are the same as Fe in Example 1 3 o 4 @MOPPA-Pd 1 The preparation method of the catalyst carrier is the same.

[0066] Homogeneous mesh-like polyaniline-coated magnetic nano-Fe 3 o 4 Supported palladium catalyst: weigh 87.7mg PdCl 2 Dissolve in 10mL water, then add 12mL 1mol / L HCl. Add 1.0g Fe to the solution at 30°C 3 o 4 @MOPPA stirring for 20h. Weigh 419.6mg Na 2 CO 3 Dissolve in water to form a solution, filter and soak in 15mL Na 2 CO 3 in aqueous solution. Wash about 5 times with 10mL water, and finally obtain the catalyst Fe containing about 50% water 3 o 4 @MOPPA-Pd 5 .

[0067] Eggshell-shaped grid-like porous polyaniline-coated magnetic nano-Fe 3 o 4 Loaded palladium catalyst: weigh 2.54g Na 2 CO 3 Dissol...

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Abstract

The invention relates to the technical field of lactic acid preparation, and specifically refers to a coated magnetic nano-Fe 3 O 4 Application of supported palladium catalyst in the preparation of lactic acid from glycerol. The method provided by the invention uses biomass glycerol as raw material, the reaction temperature is 100-200°C, the reaction time is 2-5h, and recyclable coated magnetic nano-Fe 3 O 4 Palladium is used as a catalyst and the reaction is carried out in a high-pressure reactor under alkaline conditions to obtain lactic acid. After the reaction is completed, the coated magnetic nano-Fe is recovered 3 O 4 The palladium catalyst is loaded and recycled, and the catalyst can be reused no less than 10 times. The method of the invention has the advantages of low reaction temperature, high glycerol conversion rate, high target product selectivity, fast reaction rate, high catalyst reusability, simple, safe and environmentally friendly process, and has good industrialization prospects.

Description

technical field [0001] The invention relates to the technical field of lactic acid preparation, in particular to a coated magnetic nano-Fe 3 o 4 Application of supported palladium catalyst in the preparation of lactic acid from glycerol. Background technique [0002] Lactic acid is one of the three major organic acids. It is an important biochemical product, mainly used in industries such as food and medicine. Since lactic acid has no side effects on the human body and is easily absorbed, it can directly participate in internal metabolism, promote digestion and Inhibit the harmful bacteria in the intestinal tract, etc., so it is widely used. Lactic acid and its derivatives are recognized as safe food additives; in the pharmaceutical industry, lactic acid has a strong bactericidal effect, strong polarity and hydrophilicity, and at the same time it can be used as an astringent bactericide, which can also reduce Serum cholesterol, enhance human immunity. In addition, lactic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/28C07C51/16C07C59/08
CPCC07C51/16B01J31/28B01J35/397B01J35/399C07C59/08Y02P20/584
Inventor 周心王东东沈灵沁殷恒波王爱丽
Owner JIANGSU UNIV