Catalyst for preparation of 1,3-propanediol from glycerin through hydrogenation as well as preparation method and application of catalyst

A technology for the preparation of catalysts and hydrogen, applied in metal/metal oxide/metal hydroxide catalysts, heterogeneous catalyst chemical elements, physical/chemical process catalysts, etc., can solve complex process, complicated reaction process, propylene glycol selectivity Low and other problems, to achieve the effect of low reaction temperature, low preparation cost and high selectivity

Inactive Publication Date: 2017-04-26
南京大学扬州化学化工研究院 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

These methods have complex processes and serious environmental pollution problems.
[0003] The literature (Angew Chem, Int Ed, 2001, 40:3887) uses Rh, Pd, Ru and other noble metals to form metal complexes similar to Rh(CO)2 as catalysts to perform the selective hydrogenation of glycerol to generate 1,3-propanediol. The reaction process is cumbersome and the product separation is difficult
[0004] Literature (Catalysis Communications, 2008, 9: 1360-1363.) with Pt/WO 3 /ZrO2 as catalyst, 1,3-dimethyl-2-imidazolidinone (DMI) as solvent, H at 170°C and 8MPa pressure 2 Reaction in an autoclave under reaction conditions, but the catalyst catalyzed glycerol hydrogenation reaction conversion rate is l

Method used

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  • Catalyst for preparation of 1,3-propanediol from glycerin through hydrogenation as well as preparation method and application of catalyst

Examples

Experimental program
Comparison scheme
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Example Embodiment

[0019] Example 1

[0020] Solid ZrO 2 The carrier is placed in a muffle furnace, raised to 650°C at a rate of 2°C / min, kept at a constant temperature for 2h, and cooled to room temperature to obtain ZrO 2 Forming carrier; weighing and measuring the formed ZrO 2 The carrier is immersed in the content of ammonium tungstate solution, vacuum shaken at 80°C, and dried in air at 110°C for 2h. The resulting sample is placed in a tube furnace, heated to 500°C at a rate of 2°C / min, kept at a constant temperature for 2h, and cooled to room temperature. Get WO 3 / ZrO 2 ; Weigh the WO prepared above 3 / ZrO 2 , Immerse in a certain content of ammonium niobium oxalate solution, vacuum and shake at 80°C to dry, and air dry at 110°C for 2h. Place the resulting sample in a tube furnace, heat up to 500°C at a rate of 2°C / min, keep the temperature for 2h, and cool to room temperature , Get a series of Nb 2 O 5 / WO 3 / ZrO 2 Sample; accurately measure a certain concentration of H with a pipette 2 PtCl...

Example Embodiment

[0022] Example 2

[0023] Pt-Nb was prepared by a step-wise impregnation method similar to that in Example 1. 2 O 5 / WO 3 / ZrO 2 Catalyst (including Pt content 2.0%wt, Nb 2 O 5 Content 0.8%wt, WO 3 Content 4.5%wt). 6g Pt-Nb 2 O 5 / WO 3 / ZrO 2 The catalyst is placed in a fixed bed reactor, a 10wt% glycerin aqueous solution is passed through, the hydrogen flow rate is controlled to be 50ml / min, the reaction temperature is 135°C, and the reaction pressure is 2.5MPa. During the reaction, samples were taken every 2h for analysis in a gas chromatograph. (Results are shown in Table 1)

Example Embodiment

[0024] Example 3

[0025] Pt-Nb was prepared by a step-wise impregnation method similar to that in Example 1. 2 O 5 / WO 3 / ZrO 2 Catalyst (including Pt content 2.0%wt, Nb 2 O 5 Content 1.0%wt, WO 3 Content 4.5%wt). 6g Pt-Nb 2 O 5 / WO 3 / ZrO 2 The catalyst is placed in a fixed bed reactor, a 10wt% glycerin aqueous solution is passed through, the hydrogen flow rate is controlled to be 50ml / min, the reaction temperature is 135°C, and the reaction pressure is 2.5MPa. During the reaction, samples were taken every 2h for analysis in a gas chromatograph. (Results are shown in Table 1)

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Abstract

The invention discloses a catalyst for preparation of 1,3-propanediol from glycerin through hydrogenation. ZrO2 is taken as a carrier, W, Nb and Pt salt solutions are carried by ZrO2 sequentially with an impregnation method and exist in forms of WO3, Nb2O5 and Pt in the catalyst, and the Pt-Nb2O5/Wo3/ZrO2 catalyst contains 2.5%-4.5% of WO3, 0.3%-2% of No2O5, 0.5%-2% of Pt and the balance of ZrO2. The catalyst has the advantages that a preparation method is simple, the stability is high, the catalyst is easy to separate and recover after a reaction and the like. The catalyst is used for catalyzing the reaction for preparing 1,3-propanedioll from glycerin through hydrogenation, the conversion rate and the selectivity are higher, and the preparation cost of the catalyst is lower. The invention further discloses the preparation method of the catalyst.

Description

technical field [0001] The invention relates to a catalyst for the selective hydrogenation of glycerin to prepare 1,3-propanediol and a use method thereof. Background technique [0002] 1,3-propanediol (1,3-PDO) is a very important chemical raw material, which is mainly used to produce new polytrimethylene terephthalate (PTT), and can also be used to synthesize various drugs, plasticizers, detergents, Emulsifier and other fine chemical products. At present, the preparation methods of 1,3-PDO mainly include acrolein hydration hydrogenation method, ethylene oxide carbonylation hydrogenation method, biological fermentation method, and glycerol as raw material by catalytic hydrogenation synthesis. These methods are complicated in technology, and the problem of environmental pollution is also relatively serious. [0003] The literature (Angew Chem, Int Ed, 2001, 40:3887) uses Rh, Pd, Ru and other noble metals to form metal complexes similar to Rh(CO)2 as catalysts to perform th...

Claims

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Application Information

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IPC IPC(8): C07C29/60B01J23/652C07C31/20
CPCB01J23/002B01J23/6527B01J2523/00C07C29/60B01J2523/69B01J2523/56B01J2523/48C07C31/205
Inventor 范以宁宗安忆许波连仝庆周军
Owner 南京大学扬州化学化工研究院
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