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Method for preparing high-activity carbonyl hydrogenation ruthenium-carbon catalyst

A ruthenium carbon catalyst and ruthenium catalyst technology, applied in the field of catalysis, can solve problems such as difficult regeneration, low catalyst activity, and harsh reaction conditions

Active Publication Date: 2011-02-09
CHENZHOU GAOXIN MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

my country started late in the sorbitol synthesis industry, and most industrial production still uses the traditional Raney Ni catalyst, which has low activity, harsh reaction conditions, complex product refining, many industrial wastes, difficult regeneration, and easy loss of active source

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Accurately weigh 270.3gRuCl 3 ·nH 2 O was dissolved in a 5000mL large beaker by adding 0.05-4mol / L hydrochloric acid, filtered, and placed in a 100L kettle, started stirring, and added NaOH, Na 2 CO 3 , KOH, NaHCO 3 Adjust the pH value to 0.1-5, and dilute the ruthenium solution with 4% gum arabic aqueous solution to obtain a ruthenium precursor with a concentration of 5-20 g / L. Quickly add the prepared ruthenium precursor into 1900g of activated carbon and inhale it into the reaction kettle, raise the temperature to 30-60°C, stir for 0.5-1h, stand still for 0.5-1h, and the intermittent stirring adsorption time is 2-20h. Under the condition of 10-30°C, slowly add the alkali metal salt solution with a mass fraction of 5-10% dropwise, control the pH at 8-11, stir and balance for 1-3 hours after adding the precipitant. Adding mass fraction is 0.5~10% ethanol, n-propanol, formaldehyde, isopropanol, hydrazine hydrate, sodium borohydride in one or two kinds of mixture red...

Embodiment 2

[0022] Accurately weigh 258.39g K 2 RuO 4 ·H 2 O is placed in a 5000mL large beaker, and 0.05-4mol / L hydrochloric acid is added to dissolve potassium ruthenate. The pH of the ruthenium solution is adjusted to 0.1-5, which is the amount of hydrochloric acid. The gum solution is used to dilute the ruthenium solution to obtain a ruthenium precursor with a concentration of 5-20 g / L. Quickly add the prepared ruthenium precursor into 1900g of activated carbon and inhale it into the reaction kettle, raise the temperature to 30-60°C, stir for 0.5-1h, stand still for 0.5-1h, and the intermittent stirring adsorption time is 2-20h. Under the condition of 10-30°C, slowly drop the mixed solution of alkali metal salt and methanol with a mass fraction of 5-10%, control the pH at 8-11, and stir for 1-3 hours to balance after adding the precipitant. Adding mass fraction is 0.5~10% ethanol, n-propanol, formaldehyde, isopropanol, hydrazine hydrate, sodium borohydride in one or two kinds of mi...

Embodiment 3

[0025] Accurately weigh 1351.4g RuCl 3 ·nH 2 O was dissolved in a 5000mL large beaker by adding 0.05-4mol / L hydrochloric acid solution, filtered, and placed in a 100L kettle, started stirring, and added NaOH, Na 2 CO 3 , KOH, NaHCO 3 Adjust the pH value to 0.1-5, and dilute the ruthenium solution with 4% gum arabic aqueous solution to obtain a ruthenium precursor with a concentration of 5-20 g / L. Quickly add the prepared ruthenium precursor to 9500g of activated carbon and inhale it into the reaction kettle, raise the temperature to 30-60°C, stir for 0.5-1h, stand still for 0.5-1h, and the intermittent stirring adsorption time is 2-20h. Under the condition of 10-30°C, slowly add the alkali metal salt solution with a mass fraction of 5-10% dropwise, control the pH at 8-11, stir and balance for 1-3 hours after adding the precipitant. Adding mass fraction is 0.5~10% ethanol, n-propanol, formaldehyde, isopropanol, hydrazine hydrate, sodium borohydride in one or two kinds of mi...

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PUM

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Abstract

The invention provides a method for preparing a high-activity carbonyl hydrogenation ruthenium-carbon catalyst. The method comprises the steps of preparing a ruthenium precursor, intermittently stirring and adsorbing the ruthenium precursor, neutralizing and precipitating, reducing ruthenium, filtering, washing, pulping and drying. The technology and the product of the invention are applied to hydrogenation of glucose; and the conversion rate of the glucose is 99.95 percent under more mild reaction conditions. The method breaks through the technology that alkali metals, such as potassium, barium, cobalt, cesium, iron and the like, or alkali metal salts serving as an accelerant are necessarily added during the preparation of the ruthenium-carrying catalyst in the conventional process, and solves the problems that catalytic activity is low and reaction conditions are rigorous because the accelerant is not added, and the hydrogenation product is contaminated by components of the accelerant. The ruthenium-carbon catalyst prepared by the method of the invention has the characteristics of high catalytic activity, high selectivity, mild reaction conditions, high product purity, a few industrial three wastes (waste water, waste gas and industrial residues), long service life for carbonyl hydrogenation, and is easy to regenerate and the like.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and in particular relates to a preparation method of a highly active carbonyl hydrogenation ruthenium carbon catalyst. Background technique [0002] Ruthenium is a hard and brittle polyvalent noble metal element with a light gray color. The chemical symbol is Ru and the atomic number is 44. Its d-electron orbital is not filled, and the surface is easy to adsorb reactants. The surface atoms are the endpoints of the periodic arrangement. There is at least one unsaturated coordination, and the coordination unsaturation of surface atoms is high, which makes ruthenium have a strong ability to activate reactant molecules. It is an excellent catalyst and is often used in hydrogenation, oxidation, isomerization, and carbonyl addition. Hydrogen and reforming reactions. Especially in the reaction of glucose hydrogenation to sorbitol, it shows more excellent catalytic performance. [0003] Sorbitol is a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C29/141C07C31/26B01J23/46
Inventor 雷涤尘杨拥军邓春玲叶咏祥舒涛杨静
Owner CHENZHOU GAOXIN MATERIAL