Unlock instant, AI-driven research and patent intelligence for your innovation.

A kind of nitrogen-sulfur co-doped catalyst and its preparation method and application

A nitrogen-sulfur co-doping and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic chemistry, etc., can solve the problems of increasing industrial application costs, low hydrogenation selectivity, and inability to recycle, etc., to achieve The effect of increasing the number of applications, increasing the hydrogenation selectivity, and increasing the reactivity

Active Publication Date: 2022-04-19
XIAMEN UNIV
View PDF7 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The common palladium-carbon catalyst currently used has a low hydrogenation selectivity to the preparation of the target biotin intermediate after completing a reaction, and the catalyst is deactivated due to the loss and poisoning of metal palladium, which cannot be recycled, greatly increasing the The cost of industrial applications, resulting in waste of catalyst

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A kind of nitrogen-sulfur co-doped catalyst and its preparation method and application
  • A kind of nitrogen-sulfur co-doped catalyst and its preparation method and application
  • A kind of nitrogen-sulfur co-doped catalyst and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0035] The invention provides a method for preparing a nitrogen-sulfur co-doped catalyst, comprising the following steps:

[0036] 1) Preparation of nitrogen-sulfur co-doped carbon carrier: Mix carbon material, urea, and thiourea, grind evenly, calcinate in air atmosphere, wash, filter, and dry to obtain nitrogen-sulfur co-doped carbon carrier CxNySz.

[0037] 2) Prepare a nitrogen-containing compound-modified noble metal precursor solution: add urea aqueous solution dropwise into the noble metal precursor solution, stir, and disperse evenly to obtain a nitrogen-containing compound-modified noble metal precursor solution.

[0038] 3) Preparation of nitrogen-sulfur co-doped catalyst: Add the precursor solution prepared in 2) dropwise into the CxNySz aqueous solution prepared in 1), stir for 6-15 hours, add alkali solution to adjust the pH to 8~9, and filter with suction , washed, dried, and reduced under hydrogen to obtain a nitrogen-sulfur co-doped catalyst. figure 1 It is a ...

Embodiment 1

[0049] 1-1 Preparation of nitrogen-sulfur co-doped carbon support

[0050] Mix and grind 1g of activated carbon, 5.5g of urea and 0.5g of thiourea evenly, put it into a crucible and seal it with aluminum foil, place it in a muffle furnace for calcination at 550°C for 4 hours in an air atmosphere, and the heating rate is 5°C / min. After washing with pure water for 3 times, suction filtration and drying were carried out to obtain a nitrogen-sulfur co-doped carbon carrier for future use.

[0051] 1-2 Configure the precursor solution of palladium modified by nitrogen-containing compounds

[0052] Dilute 2.5mL of 20g / 1000mL aqueous solution of chloropalladium acid to 100mL with deionized water, then add urea so that the molar ratio of urea to Pd is (2~4):1, stir at room temperature for 1 hour, and disperse evenly to obtain The precursor solution of palladium modified by the nitrogen-containing compound is ready for use.

[0053] 1-3 Preparation of nitrogen-sulfur co-doped catalyst...

Embodiment 2

[0062] 1-1 Preparation of nitrogen-sulfur co-doped carbon support

[0063] Mix and grind different amounts of activated carbon, urea and thiourea evenly to form test groups 1-4, put them into crucibles and seal them with aluminum foil paper, and place them in a muffle furnace for calcination at 550°C for 4 hours in an air atmosphere with a heating rate of 5 ℃ / min, washed 3 times with ultrapure water, then filtered and dried to obtain nitrogen-sulfur co-doped carbon carrier for future use.

[0064] 1-2 Configure the precursor solution of palladium modified by nitrogen-containing compounds

[0065] Dilute 2.5mL of 20g / 1000mL chloropalladium acid aqueous solution to 100mL with deionized water, then add 0.0846g of urea so that the molar ratio of urea to Pd is 3:1, stir at room temperature for 1 hour, and disperse evenly to obtain nitrogen-containing The precursor solution of compound-modified palladium is ready for use.

[0066] 1-3 Preparation of nitrogen-sulfur co-doped cataly...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention provides a nitrogen-sulfur co-doped catalyst as well as a preparation method and application thereof. In the present invention, the carrier prepared by doping and wrapping carbon materials with nitrogen and sulfur species is used to load the catalyst prepared by the noble metal coordinated with nitrogen species, which effectively improves the catalytic hydrogenation reaction activity and has higher hydrogenation effect on biotin intermediates. It is selective and recyclable; moreover, the present invention introduces a small amount of alkaline additives such as sodium hydroxide and potassium hydroxide into the hydrogenation reaction system for preparing biotin intermediates, which can effectively improve the reaction activity and reduce the esterification selectivity.

Description

technical field [0001] The invention relates to the technical field of catalysts, in particular to a nitrogen-sulfur co-doped catalyst and its preparation method and application. Background technique [0002] Biotin, also known as vitamin B7, vitamin H, and coenzyme R, is an essential substance for the synthesis of vitamin C and an essential nutrient for maintaining normal growth, development, and health of the body. In recent years, biotin has become one of the most concerned water-soluble vitamins, and it has a wide range of uses in the current feed industry, pharmaceutical industry, and food industry. [0003] The molecular formula of biotin is C 10 h 16 o 3 N 2 S, composed of an imidazole ring and a tetrahydrothiophene ring, and a n-valeric acid side chain connected to the thiophene ring, is the most complex variety of vitamins. Its synthesis requires multi-step reactions. The earliest industrial synthesis method is the lactone-thiolactone synthesis method developed...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24C07D495/04
CPCB01J27/24C07D495/04Y02P20/584
Inventor 郑南峰严升祥刘圣杰陈洁
Owner XIAMEN UNIV