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Method for preparing catalyst of acraldehyde catalyst by selective dehydration of glycerol

A selective and acrolein-based technology, applied in the field of catalysis, can solve the problems of non-compliance with green chemistry, poor utilization of glycerin, selectivity reduction of conversion rate, etc., and achieve the best conversion rate and selectivity, less by-products, and induction period short effect

Inactive Publication Date: 2013-04-17
TSINGHUA UNIV
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Problems solved by technology

[0013] Chinese patent document CN 201010213226.1 proposes a method for preparing acrolein in a miniature fixed-bed reactor by using heteropolyacid supported on alumina, diatomaceous earth, activated carbon, rutile titanium dioxide or kaolin as a catalyst, and the conversion rate of glycerin is 13.5~80.6% , the highest yield of acrolein can reach 49.0~90.5%, but the catalyst is easy to deactivate, the life is short, and the selectivity of the later conversion rate is significantly reduced
[0014] In the patent documents reported above, although an environmentally friendly solid acid catalyst is used to reduce the corrosion of the equipment, there is a disadvantage that the selective conversion rate cannot be stabilized for a long period of time, so the utilization rate of glycerol in the entire reaction process is poor. Does not meet the requirements of green chemistry

Method used

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  • Method for preparing catalyst of acraldehyde catalyst by selective dehydration of glycerol
  • Method for preparing catalyst of acraldehyde catalyst by selective dehydration of glycerol
  • Method for preparing catalyst of acraldehyde catalyst by selective dehydration of glycerol

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preparation example Construction

[0030] The catalyst preparation method for the selective dehydration of glycerin to produce acrolein provided by the present invention specifically comprises the following steps:

[0031] 1) Add Cs 2 CO 3 The molar concentration is 0.1~0.25mol L -1 Aqueous solution (Cs 2 CO 3 The molar concentration is preferably formulated to be 0.15mol L -1 aqueous solution), at room temperature by vacuum impregnation, the carrier Nb 2 o 5 Treat at least 1h at a vacuum of -0.01~-0.1MPa (preferably treat at a vacuum of -0.01MPa for 1h), and then add Cs 2 CO 3 In the aqueous solution, soak at normal pressure for 10~30h, preferably at normal pressure for 24h, so that the load is 5%~60%, preferably 20%; dry at 80°C~120°C for 10~15h; preferably dry The temperature is 100°C, and the drying time is 12 hours;

[0032] 2) Mole ratio Cs 2 CO 3 : Heteropolyacid=0.5:1~1.5:1 Weigh the heteropolyacid, and make the molar concentration of the heteropolyacid is 0.05~0.1mol L -1 The aqueous soluti...

Embodiment 1

[0034] Implementation example 1, 1a and 1b (compared with existing catalysts)

[0035] Will Cs 2 CO 3 Formulated with a molar concentration of 0.1mol L -1 concentration in aqueous solution, the Nb 2 o 5 The carrier is added into the aqueous solution, and after stirring, the vacuum impregnation method is adopted at room temperature, and the carrier Nb 2 o 5 Treat for 1h under vacuum degree -0.1MPa, then add Cs 2 CO 3 The solution was impregnated at normal pressure for 24 hours, so that the loading capacity was 20%, and dried at 100°C for 12 hours for later use; by molar ratio Cs 2 CO 3 : Phosphotungstic acid = 1.25: 1 Weigh phosphotungstic acid and prepare a molar concentration of 0.05mol L -1 concentrated aqueous solution, after stirring, vacuum impregnation method is used at room temperature, and the loaded catalyst carrier obtained in step 1) is treated at a vacuum degree of -0.1MPa for 1 hour, then added with phosphotungstic acid solution and impregnated at normal ...

Embodiment 1b

[0039] For the implementation example 1b, weigh phosphotungstic acid with a molar ratio of Cs2CO3: heteropolyacid = 1.25:1 and prepare an aqueous solution with a molar concentration of 0.05mol L-1. After stirring, filter, wash and dry at room temperature. Calcined at 500°C for 4h, Cs 2.5 h 0.5 PW 12 o 40 Cesium phosphotungstate catalyst, the catalyst is pressed into tablets, pulverized and sieved into 30-50 mesh for later use.

[0040] Reaction condition is the same as implementation example 1

[0041] The results are compared in Table 1 below.

[0042] Table 1

[0043]

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PUM

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Abstract

The invention discloses a method for preparing an acraldehyde catalyst produced by selective dehydration of glycerol. The method comprises the following steps of: loading heteropolyacid cesium salt by using 5-60 percent of loading amount at the room temperature in a vacuum impregnation method by using niobium pentoxide as a carrier; and forging at 400-700 DEG C to prepare the catalyst, wherein the glycerol conversion rate of the catalyst is up to 75-100 percent, and the acraldehyde selectivity is up to 52-90 percent. The catalyst prepared by the invention is short in induction period, high in acraldehyde yield, long in service life and good in renewability, can recover the activity of the reaction by charking at 500 DEG C, and avoids inactivation after reaction for 200 hours.

Description

technical field [0001] The invention relates to a catalyst for preparing acrolein by selective dehydration of glycerin and a preparation method thereof, belonging to the technical field of catalysis. Background technique [0002] Acrolein is an important intermediate in organic synthesis, which plays a bridge role in the conversion and utilization of glycerol—acrolein can be further oxidized to produce acrylic acid and its esters which are widely used, and can also be used as a raw material for polymerization reactions to synthesize polymer materials (such as : The downstream product of acrolein—sodium polyacrylate): [0003] [0004] Acrolein can also be used to synthesize methionine: methionine is an amino acid that organisms cannot synthesize by themselves. It can be used to promote animal growth. The concentration and yield of methionine provided by natural methionine sources (plants, microorganisms) are relatively low, which cannot meet human needs. At present, the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/36C07C47/22C07C45/52
Inventor 王铁峰刘蓉金涌
Owner TSINGHUA UNIV
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