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Catalyst for preparing isosorbide by utilizing celluloses and preparation method of catalyst

A technology for isosorbide and catalyst, which is applied to the preparation of isosorbide, the catalyst for preparing isosorbide from cellulose and the field of preparation thereof, can solve the problems of harsh reaction equipment, complicated separation process, etc. Application prospects, the effect of avoiding equipment corrosion problems

Inactive Publication Date: 2013-09-04
SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existence of liquid acid makes the subsequent separation process complex and requires harsh reaction equipment
To the best of our knowledge, there is no research report on the direct preparation of isosorbide from cellulose using solid acid-supported noble metals as bifunctional catalysts without the aid of inorganic liquid acids.

Method used

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  • Catalyst for preparing isosorbide by utilizing celluloses and preparation method of catalyst
  • Catalyst for preparing isosorbide by utilizing celluloses and preparation method of catalyst
  • Catalyst for preparing isosorbide by utilizing celluloses and preparation method of catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 5g of niobium pentachloride was added to 200mL of water, stirred and hydrolyzed to obtain a white precipitate, washed repeatedly with water until neutral, dried at 80°C to obtain amorphous hydrated niobium oxide (Nb 2 o 5 ·nH 2 o).

[0040] 0.07g RuCl 3 ·nH 2 O (37wt%Ru) was dissolved in 3.5mL water and 0.5g Nb was added 2 o 5 ·nH 2 O, stirred at room temperature for 24h, stirred and dried at 80°C, and the obtained powder was reduced in a hydrogen atmosphere at 265°C for 3h to obtain 5wt% Ru / Nb 2 o 5 ·nH 2 O catalyst.

[0041] Put 0.06g of the above-mentioned catalyst, 0.6g of cellulose and 30mL of water into a 100mL reactor, pass through hydrogen to replace the gas for 6 times, fill with hydrogen to 6MPa, and raise the temperature to 220°C for 1 hour. After the reaction was completed, the temperature was rapidly lowered, and the supernatant liquid after centrifugation was taken for high-performance liquid chromatography analysis. The results are shown in Tabl...

Embodiment 2

[0043] 5g of niobium pentachloride was added to 200mL of water, stirred and hydrolyzed to obtain a white precipitate, washed repeatedly with water until neutral, dried at 80°C to obtain amorphous hydrated niobium oxide (Nb 2 o 5 ·nH 2 o). 1.25g Nb 2 o 5 ·nH 2 O was stirred in 250 mL of 1 mol / L phosphoric acid solution for 48 hours, washed with water until neutral, and dried at 120°C to obtain phosphoric acid-modified niobium oxide. Catalysts are labeled H 3 PO 4 / Nb 2 o 5 .

[0044] 0.07g RuCl 3 ·nH 2 O (37wt%Ru) was dissolved in 3.5 mL of water, and 0.5 g of H 3 PO 4 / Nb 2 o 5 , stirred at room temperature for 24h, stirred and dried at 80°C, and the obtained powder was reduced in a hydrogen atmosphere at 265°C for 3h to obtain 5wt%Ru / H 3 PO 4 / Nb 2 o 5 catalyst.

[0045] Put 0.06g of the above-mentioned catalyst, 0.6g of cellulose and 30mL of water into a 100mL reactor, pass through hydrogen to replace the gas for 6 times, fill with hydrogen to 6MPa, and r...

Embodiment 3

[0047] Dissolve 5g of P123 in 50g of n-propanol, stir to dissolve; add 9.5g of niobium pentachloride, stir to dissolve; add 5mL of 0.05mol / L sodium chloride aqueous solution, and continue to stir for 60min. The obtained colloid was transferred to a hydrothermal synthesis kettle and heated at 40°C for 7 days, and continued at 180°C for 2 days. The obtained colloid was heated in 1500mL of 60°C water for 3h, washed with water and filtered, and this process was repeated 4 times. The filter cake was dried in air at 100°C and calcined in air at 300°C to obtain mesoporous niobium oxide, marked as meso Nb.

[0048] 0.12g RuCl 3 ·nH 2 O (37wt%Ru) was dissolved in 1.8mL water, 0.9g meso Nb was added, stirred at room temperature for 24h, and dried at 110°C. The resulting powder was reduced in a hydrogen atmosphere at 265°C for 3h to obtain a 5wt%Ru / meso Nb catalyst.

[0049] Put 0.06g of the above-mentioned catalyst, 0.6g of cellulose and 30mL of water into a 100mL reactor, pass throu...

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PUM

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Abstract

The invention relates to the technical field of fine chemical engineering and discloses a catalyst for preparing isosorbide by utilizing celluloses and a preparation method of the catalyst. The catalyst is a bifunctional catalyst comprising a solid acid loading metal. The bifunctional catalyst disclosed by the invention can be used for realizing the process of catalyzing the celluloses to obtain the isosorbide under the reaction condition that no inorganic liquid acid is added, and avoiding the corrosion problem of equipment caused by using the inorganic liquid acid, and is easy to recycle; the maximum conversion rate of the celluloses can reach 100%, and the maximum selectivity of the isosorbide can reach 55%; the catalyst has very high stability under the existing reaction condition, still maintains the catalytic performance without loss after being cycled for ten times and has low requirements on equipments; and the catalyst is suitable for the existing common industrial production conditions and has very good application prospect.

Description

technical field [0001] The invention belongs to the technical field of fine chemicals and relates to the preparation of isosorbide, in particular to a catalyst for preparing isosorbide from cellulose and a preparation method thereof. Background technique [0002] The modern industrial system based on petroleum refining is the pillar of national economic development, but due to the excessive dependence on non-renewable fossil resources, the sustainable development of social economy is facing unprecedented challenges of energy resource shortage and ecological environment deterioration. Replacing non-renewable fossil resources with renewable biological resources and realizing a fundamental change in the source of industrial raw materials is a major strategic requirement for changing the economic growth model and ensuring sustainable social and economic development. [0003] Carbohydrates such as cellulose, hemicellulose, and starch are a kind of biomass resources with wide dist...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/648B01J27/195B01J23/652C07D493/04
Inventor 李福伟孙鹏
Owner SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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