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Method for preparing propanediol by direct hydrogenation of glycerol

A technology of glycerol and propylene glycol, which is applied in the preparation of hydroxyl groups and organic chemistry, etc., can solve the problems of harsh reaction conditions, complex catalyst preparation process, low conversion rate and target product selectivity, and achieve mild reaction conditions and promotion effect Obvious, simple process effect

Inactive Publication Date: 2008-09-03
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] Although the above-mentioned prior art can convert glycerol to produce propylene glycol, either the conversion rate and the selectivity of the target product are not high, or the reaction conditions are relatively harsh or the catalyst preparation process is complex

Method used

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Effect test

preparation example Construction

[0034] The step of preparing propylene glycol of the present invention is:

[0035] (1) In a 100ml autoclave, add a certain amount of ruthenium catalyst, rhenium compound and raw material glycerol aqueous solution;

[0036](2) After the reaction kettle is sealed, replace the air in the reaction kettle with hydrogen, and place the reaction kettle in a heating furnace to heat to the reaction temperature (120-180° C.);

[0037] (3) At a given reaction temperature (120-180° C.), fill the reactor with hydrogen to a reaction pressure (4-10 MPa). Under reaction temperature and reaction pressure, react under stirring for 1 to 8 hours;

[0038] (4) After the reaction finishes, the reactor is taken out from the heating furnace, and after being cooled to room temperature, the pressure in the reactor is released to normal pressure, the lid of the reactor is opened, the reaction solution containing the product is taken out, and a certain amount of internal standard (2 Glycol dimethyl eth...

Embodiment 1

[0048] (1), ZrO 2 preparation of

[0049] The ammonia solution (2.5%) of 60ml is dripped into 60ml of ZrO(NO 3 ) 2 Aqueous solution (0.1mol / L), the resulting precipitate was filtered, washed with deionized water to neutrality, and then washed with ethanol, and the filter cake obtained by filtration was dried at 110°C for 12 hours and roasted at 550°C for 5 hours to obtain ZrO 2 .

[0050] (2), 5wt% Ru / ZrO 2 preparation of

[0051] 5ml RuCl 3 Aqueous solution (0.1mol / L) impregnated ZrO prepared above 2 , the loading amount of Ru metal is 5% (weight percentage). After soaking for 7 hours, evaporate the solvent to dryness, dry at 110°C for 12 hours, bake at 350°C for 5 hours, and then dry at 450°C 2 Reduction for 4 hours to get Ru / ZrO 2 .

[0052] (3), reaction

[0053] In a stainless steel autoclave with an internal volume of 100ml, add the catalyst Ru / ZrO prepared above 2 0.15g, additive Re 2 (CO) 10 0.0242g, glycerin aqueous solution (40wt%) 10ml. After sealing ...

Embodiment 2

[0055] Except using commercial reagent 5wt%Ru / Al 2 o 3 0.15g instead of 5wt% Ru / ZrO 2 Except, other operation is the same as embodiment 1. The reaction results are listed in Table 1.

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Abstract

The invention relates to a method for preparing propylene glycol by direct hydrogenation from glycyl alcohol under an exist of ruthenium catalyst and rhenium auxiliary. The invention is characterized in that the glycyl alcohol is directly converted to be propylene glycol by using supported ruthenium as a catalytic agent, using rhenium carbonyl as an auxiliary and using glycyl alcohol solution and hydrogen as raw materials, under a reaction temperature of 120-180 degree C, in a mild condition that the pressure of hydrogen is 4-10MPa. The method provided in the invention has a simple process, a mid reaction condition, and a sufficient promote effect for Ru catalytic agent by using rhenium carbonyl as the auxiliary.

Description

technical field [0001] The invention relates to a method for directly hydrogenating propylene glycol from glycerol in the presence of a ruthenium catalyst and a rhenium additive, belonging to the field of fine chemicals. Background technique [0002] As a new energy source that is environmentally friendly and derived from renewable biological resources, biodiesel is being popularized and applied at home and abroad. When biodiesel is produced by transesterification of oil and alcohol, glycerol is also produced by-product. With the mass production of biodiesel, the amount of by-product glycerol will also increase greatly (about 1 kilogram of glycerol is produced for every 9 kilograms of biodiesel produced). [0003] The traditional use of glycerol is mainly used in skin care products industry (moisturizers, etc.), food industry (sweet additives, etc.), daily necessities industry (leather processing, antifreeze), pharmaceutical industry (nitroglycerin expansion of coronary art...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/20C07C29/60
Inventor 贺德华马兰
Owner TSINGHUA UNIV
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