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Pd-Re catalyst for propylene glycol preparation by glycerol hydrogenolysis and preparation method thereof

A technology of catalyst and glycerol, which is applied in the direction of catalyst activation/preparation, metal/metal oxide/metal hydroxide catalyst, chemical instruments and methods, etc., can solve complex process, inability to convert glycerin, and the amount of metal palladium Large and other problems, to achieve the effect of high activity and simple preparation process

Inactive Publication Date: 2015-01-14
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But no 1,3-propanediol is produced
Literature (Green Chem., 2009, 11, 1511-1513) reported that Pd / Fe 2 o 3 As a catalyst, 2-propanol as a solvent and hydrogen source, at 180 ° C, 5 bar inert gas pressure, using the hydrogen generated by the dehydrogenation of 2-propanol to react with glycerol to obtain high conversion of glycerol rate and selectivity of 1,2-propanediol, but this method uses 2-propanol as a solvent, and the amount of metal palladium is relatively large, and no 1,3-propanediol is generated
Another document (Journal of Catalysis, 2012,296, 1) discloses that Cu 0.4 / Zn 5.6-x Mg x Al 2 o 8.6 As a catalyst for the hydrogenolysis of glycerol, at 200°C, high conversion of glycerol and selectivity to 1,2-propanediol are obtained, but no formation of 1,3-propanediol
Literature (Green Chem., 2011, 13, 2004) reported the use of Pt / SO4 2- / ZrO 2 As a catalyst, DMI (1,3-dimethyl-2-imidazolidinone) is used as a method for solvent hydrogenolysis of glycerol, which can obtain higher conversion rate of glycerol and 1,3-propanediol yield, However, the DMI solvent used in this method is expensive and toxic. In addition, DMI itself will undergo a hydrogenolysis reaction with glycerol.
Although the existing technologies can hydrogenolyze glycerol into 1,2-propanediol under certain conditions, some technologies have complex processes for catalyst preparation, some technologies use expensive and toxic reagents, and some technologies use The catalyst is not yet able to convert glycerol to 1,3-propanediol

Method used

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  • Pd-Re catalyst for propylene glycol preparation by glycerol hydrogenolysis and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Preparation of 5%Pd-5%Re / SBA-15 precursor

[0019] With 4.00g block copolymer P123 (commodity reagent: (polyethylene oxide) 20 (polypropylene oxide) 70 (polyethylene oxide) 20 ) was dissolved in 122mL of 2mol / L hydrochloric acid solution, and after stirring and dissolving at 35°C, 9.5mL of tetraethyl orthosilicate (commercial reagent) with a mass fraction of 28% was added, and after stirring for 20 hours at 35°C, the temperature was raised to 80°C and aged at 80°C for 24 hours, the obtained gel was washed with deionized water repeatedly until the filtrate was neutral, and the final gel was dried at 40°C for 48 hours, and then calcined at 500°C for 6 Hours, the carrier solid powder mesoporous silica (SBA-15) was obtained.

[0020] 0.1mol / L of PdCl 2 (Commercial reagent) 5.2 mL of hydrochloric acid solution and 0.1 mol / L of HReO 4 (Commercial reagent) Mix 3.0mL of aqueous solution, stir evenly, then add 1.00g of the above-mentioned SBA-15 carrier into the mixed s...

Embodiment 2

[0026] (1), preparation of 5%Pd-10%Re / SBA-15 precursor

[0027] Except for 0.1mol / L HReO 4 Except that the amount of the aqueous solution used is 6.3 mL, other steps are the same as the step (1) of Example 1.

[0028] (2), activation treatment of 5%Pd-10%Re / SBA-15 precursor

[0029] Except for using the precursor of 5%Pd-10%Re / SBA-15, other steps are the same as step (2) of Example 1. A 5%Pd-10%Re / SBA-15 catalyst was obtained, labeled 5Pd-10Re / SBA-15.

[0030] (3), Hydrogenolysis reaction of glycerol over 5Pd-10Re / SBA-15 catalyst and product analysis

[0031] Except using 5Pd-10Re / SBA-15 catalyst, other steps are the same as step (3) of Example 1, and the reaction results are listed in Table 1.

Embodiment 3

[0033] (1), 5%Pd-5%Re / A1 2 o 3 Precursor preparation

[0034] In addition to using vector A1 2 o 3 (Commercial reagent) replace SBA-15, other steps are the same as step (1) of embodiment 1.

[0035](2), 5%Pd-5%Re / Al 2 o 3 Activation of precursors

[0036] Except using 5%Pd-5%Re / Al 2 o 3 In addition to the precursor, other steps are the same as step (2) of Example 1. Get 5%Pd-5%Re / Al 2 o 3 Catalyst, labeled 5Pd-5Re / Al 2 o 3 .

[0037] (3), 5Pd-5Re / Al 2 o 3 Hydrogenolysis of glycerol over catalyst and product analysis

[0038] In addition to using 5Pd-5Re / Al 2 o 3 Except catalyzer, other steps are with the step (3) of embodiment 1, and reaction result is listed in table 1.

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Abstract

The invention relates to a Pd-Re catalyst for propylene glycol preparation by glycerol hydrogenolysis and a preparation method thereof and belongs to the technical field of comprehensive utilization of resources and fine chemical engineering. The invention is characterized in that Pd is used as a main catalyst component, Re is used as a co-catalyst component and an inorganic oxide or carbon nanotube is used as a carrier; a supported Pd-Re catalyst precursor is prepared by an immersion method; and without roasting, hydrogen is directly used for reduction, so as to obtain the supported Pd-Re catalyst. The supported Pd-Re catalyst prepared by the method is used in a glycerol hydrogenolysis reaction so as to directly convert glycerol to propylene glycol, and has high activity and sensitivity.

Description

technical field [0001] The invention relates to a Pd-Re catalyst prepared by using a method of reducing a precursor without roasting, and a method for directly hydrogenating glycerol to prepare propylene glycol in the presence of the catalyst, which belongs to the field of fine chemical industry. Background technique [0002] As a new type of energy, biodiesel has been vigorously developed at home and abroad due to its environmental friendliness, renewable and other advantages. Using vegetable or animal fats, transesterification with methanol or ethanol can produce biodiesel, but the by-product glycerol is also produced at the same time. On average, for every 9Kg of biodiesel produced, 1Kg of glycerol is by-produced. In traditional application fields, glycerol can be used in the defense industry (such as the production of glyceryl trinitrate, etc.), the pharmaceutical field (such as the production of nitroglycerin), the skin care industry (such as used in moisturizers, etc....

Claims

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Application Information

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IPC IPC(8): B01J23/656C07C31/20C07C29/60B01J37/18
Inventor 贺德华李宇明刘会敏张娟
Owner TSINGHUA UNIV