Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of silica-supported carbon-nitrogen-coated cobalt-ruthenium catalyst and method for catalytic transfer hydrogenation of unsaturated compound through silica-supported carbon-nitrogen-coated cobalt-ruthenium catalyst

A silicon dioxide and ruthenium catalyst technology, which is applied in the preparation of organic compounds, physical/chemical process catalysts, hydrogenation preparation, etc., can solve the problems of long reaction time, inconvenient storage and transportation, flammability and explosion, etc., and achieves a simple preparation method, Good persistence of activity, not easy to lose effect

Inactive Publication Date: 2018-01-19
HUBEI UNIV
View PDF7 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the process of catalytic quinoline hydrogenation mainly uses relatively expensive hydrogen as a raw material. For example, the Chinese patent application number 201310619958.4 discloses "a method for preparing hydrogenated quinoline", using quinoline and Raney nickel catalysts, in order to obtain Higher activity and selectivity, higher reaction temperature 180-240°C, H 2 The pressure needs to reach 2-9MPa, and the final product is mainly 1,2,3,4-tetrahydroquinoline, and also contains a very small amount of decahydroquinoline and 5,6,7,8-tetrahydroquinoline; application The Chinese patent No. 201610844274.8 discloses a "preparation method of substituted 1,2,3,4-tetrahydroquinoline", using quinoline and its derivatives, nanoporous palladium catalyst, the reaction temperature is -50 ~ 150 ℃, the reaction time is 12~36h, the pressure of hydrogen is 0.1~20.0Mpa, the final selective hydrogenation produces 1,2,3,4-tetrahydroquinoline, the temperature or / and pressure required for the reaction of the two High, some reaction time is too long, in addition, because the current industrial hydrogen is still mainly obtained from fossil resources, and the use of high-pressure hydrogen has safety problems such as inconvenient storage and transportation, flammability and explosion, so from the perspective of economy, environmental protection and practicality From a perspective, it is necessary to develop a new catalytic hydrogenation system that does not rely on traditional fossil resources to generate hydrogen

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
  • Preparation method of silica-supported carbon-nitrogen-coated cobalt-ruthenium catalyst and method for catalytic transfer hydrogenation of unsaturated compound through silica-supported carbon-nitrogen-coated cobalt-ruthenium catalyst
  • Preparation method of silica-supported carbon-nitrogen-coated cobalt-ruthenium catalyst and method for catalytic transfer hydrogenation of unsaturated compound through silica-supported carbon-nitrogen-coated cobalt-ruthenium catalyst
  • Preparation method of silica-supported carbon-nitrogen-coated cobalt-ruthenium catalyst and method for catalytic transfer hydrogenation of unsaturated compound through silica-supported carbon-nitrogen-coated cobalt-ruthenium catalyst

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0030] The preparation method of silicon dioxide supported carbon nitrogen coated cobalt ruthenium catalyst comprises the following steps:

[0031]1) Mix ruthenium salt, cobalt salt, organic ligand, and solvent at a mass ratio of 5.89-35.34:47.5-570:198.2-1189:19.725 and heat for a certain period of time to form A solution; wherein the ruthenium salt is ruthenium chloride, The cobalt salt is cobalt chloride hexahydrate, the organic ligand is o-phenanthroline, and the solvent is absolute ethanol; heating is carried out in a water bath, and the temperature of the water bath heating is 60°C for 1 to 3 hours; preferably, ruthenium salt, cobalt The mass ratio of salt, organic ligand and solvent is 5.89~11.78:95~190:198.2~396.4:19.725; the mass ratio of cobalt to ruthenium is 4:1;

[0032] 2) Add nano silicon dioxide to A solution and mix to form B solution; the mass ratio of nano silicon dioxide to ruthenium salt is 589:5.89~35.34, and the particle diameter of nano silicon dioxide ...

Embodiment 1

[0037] Add 2945mg of ruthenium chloride aqueous solution (mass fraction is 1%) into the round bottom flask and dry the water therein with a rotary evaporator, add 107mg of cobalt chloride hexahydrate, 198.2mg of phenanthroline, and 25mL of absolute ethanol into the dry round flask In the bottom flask, add magnetons, stir in a water bath at 60°C for 1 hour to obtain solution A; add 589 mg of nano-silica to solution A, and mix with ultrasound for 20 minutes, and the power of ultrasound is 100W to obtain solution B; use a rotary evaporator Evaporate the solvent in solution B to dryness, put it in a vacuum oven and keep it for 4 hours, the drying temperature is 60°C, scrape off the solid on the wall of the flask, grind it finely in an agate mortar, transfer it to a crucible, put the crucible in a vacuum tube In a type furnace, the temperature was raised at a rate of 5°C / min, under N 2 Calcined in the atmosphere for 2h, the temperature was kept at 700°C, and a silica-supported carb...

Embodiment 2

[0040] Add 589mg of ruthenium chloride aqueous solution (mass fraction is 1%) into the round bottom flask and dry the water therein with a rotary evaporator, add 95mg of cobalt chloride hexahydrate, 198.2mg of phenanthroline, and 25mL of absolute ethanol into the dry round flask In the bottom flask, add magnetons, stir in a water bath at 60°C for 1 hour to obtain solution A; add 589 mg of nano-silica to solution A, and mix with ultrasound for 20 minutes, and the power of ultrasound is 100W to obtain solution B; use a rotary evaporator Evaporate the solvent in solution B to dryness, put it in a vacuum oven and keep it for 4 hours, the drying temperature is 60°C, scrape off the solid on the wall of the flask, grind it finely in an agate mortar, transfer it to a crucible, put the crucible in a vacuum tube In a type furnace, the temperature was raised at a rate of 5°C / min, under N 2 Calcined in the atmosphere for 2h, the temperature was kept at 700°C, and a silica-supported carbon...

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

PropertyMeasurementUnit
Particle sizeaaaaaaaaaa
Login to View More

Abstract

The invention discloses a preparation method of a silica-supported carbon-nitrogen-coated cobalt-ruthenium catalyst. The preparation method comprises uniformly mixing a ruthenium salt, a cobalt salt,an organic ligand and a solvent in a mass ratio of 2.945 to 3.354: 47.5 to 570: 198.2: 19.725, heating the mixture for some time to obtain a solution A, adding nano-silica into the solution A, carrying out uniform mixing to obtain a solution B, removing the solvent in the solution B, carrying out drying to obtain solids, calcining the solids and cooling the solids to obtain the silica-supported carbon-nitrogen-coated cobalt-ruthenium catalyst. The invention also discloses a method for catalytic transfer hydrogenation of an unsaturated compound through the catalyst. The method has simple processes, utilizes easily available raw materials and is suitable for promotion and application. The bimetallic cobalt and ruthenium are respectively chelated with o-phenanthroline and the chelate is supported on nano-silica particles so that carbon-nitrogen-coated metal is formed. The catalyst reduces a metal loss, resists acid corrosion and toxicity of CO obtained by decomposition of formic acid, isfree of high-pressure hydrogen and is economic and environmentally friendly.

Description

technical field [0001] The invention belongs to the technical field of composite material catalysts, in particular to a preparation method of a silica-supported carbon-nitrogen-coated cobalt-ruthenium catalyst and a method for catalytic transfer hydrogenation of unsaturated compounds. Background technique [0002] 1,2,3,4-Tetrahydroquinoline (THQ1) is the structural unit of many quinoline alkaloids, which are widely used as drug intermediates and have anti-vasodilation, anti-arrhythmic and anti-tumor activities. In addition, when THQ1 is used in asphalt pretreatment, it can improve the quality of pitch carbon fiber and produce pitch carbon fiber with high strength and high modulus. At present, the methods for industrially synthesizing THQ1 and its derivatives mainly include chemical synthesis and quinoline catalytic hydrogenation, and quinoline catalytic hydrogenation is used to produce THQ1 with fewer reaction steps and low raw material costs. [0003] At present, the proc...

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
IPC IPC(8): B01J27/24C07C29/143C07C35/08C07D215/06C07D295/027C07B31/00C07C29/17C07C33/20C07C209/36C07C211/46
Inventor 聂仁峰杨环环喻小龙夏清华
Owner HUBEI UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com