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Method for preparing 1,3-propylene glycol by utilizing glycerol one-step hydrogenolysis method

A technology of propylene glycol and glycerol, which is applied in the preparation of hydroxyl groups, chemical instruments and methods, molecular sieve catalysts, etc., can solve the problems of high reaction temperature and reaction pressure, low catalyst activity and selectivity, etc., and achieves improved dispersion and obvious industrial application. Prospects, the effect of improving the conversion rate of glycerol

Inactive Publication Date: 2012-02-08
SOUTHEAST UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are relatively few studies on the direct production of 1,3-propanediol by catalytic hydrogenolysis reaction using glycerol as raw material, and there are generally problems such as high reaction temperature and reaction pressure, low activity and selectivity of the catalyst, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0022] Another object of the present invention is to provide a catalyst preparation method capable of preparing 1,3-propanediol with high selectivity under mild conditions, comprising the following steps:

[0023] (1) Dissolve the heteropoly acid in water to make a solution of 0.005-1.0 mol / L, add the catalyst carrier under rapid stirring, stir for 1-36 hours, mix well, and dry at 80-150 ℃ for 1-24 hours , calcination at 200-400°C for 2-10 hours to prepare a molecular sieve-supported heteropolyacid precursor. The concentration of the prepared solution is preferably 0.005-0.5 mol / L, the stirring time is preferably 10-24 hours, preferably dried at 80-120°C for 5-10 hours, and calcined at 200-300°C for 2-5 hours.

[0024] (2) Dissolve the soluble metal additive salt in deionized water to make a solution with a concentration of 0.01-1.0 mol / L, stir, add molecular sieve-loaded heteropolyacid precursor, and add a certain amount of chloroplatinic acid or palladium chloride at the sam...

example 1

[0028] Take 5 g of modified USY zeolite (DUSY), add 1 g of phosphotungstic acid, dissolve in 50 mL of deionized water, stir for 24 hours, dry at 100 °C for 6 hours, and roast at 300 °C for 3 hours to prepare DUSY loaded phosphotungstic acid precursor. Weigh 0.46 g Cu(NO 3 ) 2 ·3H 2 O was dissolved in 50 mL deionized water, added the prepared DUSY loaded phosphomolybdic acid precursor and 6.75 mL chloroplatinic acid solution (0.019 mol / L), stirred at room temperature for 24 hours, dried at 110 °C for 8 hours, and calcined at 300 °C for 3 hours, the catalyst CuPt / PW / DUSY was prepared.

[0029] Add 15 g glycerol and 60 g deionized water in a 0.1 L autoclave, mix well, get 0.5 g of the catalyst prepared by the above-mentioned method, seal the kettle, and use N 2 Replace the air in the kettle, and then use H 2 After replacing the nitrogen in the kettle, fill it with 2 MPa of H 2 , start stirring at 300 rpm, and heat to 160 °C for 20 hours. The obtained feed liquid was filter...

example 2

[0031] In the autoclave of 0.1 L, add 10 g glycerol and 80 g sulfolane, mix, get the catalyst prepared in 0.5 g example one, seal the still, use N 2 The air in the kettle will be replaced, and then H 2 After replacing the nitrogen in the kettle, fill it with 5 MPa of H 2 , start stirring at 300 rpm, and heat to 180 °C for 24 hours. The obtained feed liquid was filtered to remove the catalyst, and the composition of the product was analyzed by gas chromatography. The conversion rate of glycerol was 53%, the selectivity of 1,3-propanediol was 33%, and the selectivity of 1,2-propanediol was 16%.

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Abstract

The invention relates to a method for preparing 1,3-propylene glycol by utilizing a glycerol one-step hydrogenolysis method, in particular to preparation of a loaded solid acid bifunctional catalyst and a method for preparing 1,3-propylene glycol by virtue of glycerol selective hydrogenolysis by utilizing the catalyst. The method provided by the invention comprises the step of introducing hydrogen and reacting for 6-48 hours under the conditions that glycerol is taken as raw material, solvent and catalyst exist, reaction temperature is 100-230 DEG C and reaction pressure is absolute pressure of 0.2-10.0MPa. In the bimetal modified loaded strong acid catalyst prepared by adopting the method provided by the invention, a second non-precious metal is doped into the catalyst, dispersion degree of previous metal is further improved, thus the catalyst has stronger acidity, larger specific area and good stability; in the catalyst containing trace previous metal, cheap non-previous metal is introduced; glycol conversion rate is improved under lower reaction pressure while selectivity of 1,3-propylene glycol is obviously improved; meanwhile, effective utilization rate of the previous metal is improved, and cost of the catalyst is reduced.

Description

technical field [0001] The invention relates to a preparation method of 1,3-propanediol, in particular to the preparation of a supported solid acid bifunctional catalyst and the method for using the catalyst in selective hydrogenolysis of glycerin to prepare 1,3-propanediol. Background technique [0002] Glycerin can be used as a raw material to synthesize important chemical intermediates such as propylene glycol, epichlorohydrin, glyceryl carboxylate, and pyruvic acid. Among them, 1,3-propanediol, one of the two isomers of propylene glycol, is not only a good solvent, Antifreeze and protective agent, it can also be used in synthetic fibers, plasticizers, detergents, preservatives or emulsifiers, etc. In particular, polytrimethylene terephthalate (PTT), which is synthesized with 1,3-propanediol as a monomer, not only has the excellent properties of polyethylene terephthalate (PET), but also has the same good resilience as nylon It is widely used in the fields of carpets, en...

Claims

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Application Information

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IPC IPC(8): C07C31/20C07C29/60B01J29/16B01J29/78B01J29/48B01J27/188
Inventor 魏瑞平肖国民牛磊李想
Owner SOUTHEAST UNIV
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