A kind of preparation method of alumina-coated transesterification catalyst

A catalyst and hydroxide technology, applied in the chemical industry, can solve the problems of difficult separation of homogeneous catalysts, increase the difficulty of promotion, difficult separation and recovery, etc., so as to improve the low temperature reaction activity and thermodynamic stability, and improve the chemical stability and thermodynamics. Stability, the effect of increasing the specific surface area

Active Publication Date: 2022-08-09
SOUTHWEST RES & DESIGN INST OF CHEM IND
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Problems solved by technology

[0003] An important factor affecting the development of transesterification technology to synthesize dimethyl carbonate is the development of high-efficiency catalysts. The homogeneous catalysts with alkali metal hydroxides and alkali metal alkoxides as typical catalysts have fast reaction speeds and high product yields. Attention has been paid to homogeneous catalysts, but the homogeneous catalysts are not easy to separate from the product, the operating cost is high, and the stability is poor, which increases the difficulty of its promotion. Difficulties in separation and recovery, but the target product selectivity and yield of this type of catalyst are low;
[0004] For example, Mobil Corporation (patent US5498743) has successfully developed silica gel as a carrier and loaded alkaline earth metal halide salts as a transesterification catalyst, but the yield and selectivity are low. Patent CN1228358A uses X molecular sieves after potassium ion exchange as a carrier , KOH-KX catalyst is prepared by impregnation method, which can be reused and the product is easy to separate, but the conversion rate of propylene glycol carbonate is only 41%; patent CN 1431053A, also developed a heterogeneous catalyst, with phenolic resin as the main carrier, loaded Alkaline earth metal carbonate, propylene glycol carbonate conversion rate and dimethyl carbonate yield are all better under high temperature, but 80 ℃ propylene glycol carbonate conversion rate is only 68.4%, and reaction time is long; Therefore, the industry of heterogeneous catalyst There are still technical bottlenecks in the promotion, and key breakthroughs are needed

Method used

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  • A kind of preparation method of alumina-coated transesterification catalyst

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preparation example Construction

[0033] one for Al 2 O 3 Coated K 2 O / Na 2 O-WO 3 The preparation method of catalyst comprises the following steps:

[0034] Step A: mix by weighing the soluble alkali metal salt solution or hydroxide solution, soluble tungsten source solution and ethylene glycol in a metered ratio to obtain a mixed solution;

[0035] Step B: carry out a flux thermal reaction at 160-190°C, the reaction time is 12-20h, and then put it into a muffle furnace and calcinate at 450-600°C for 3-8h to obtain nano-K 2 O-WO 3 or Na 2 O-WO 3 particles;

[0036] Step C: The nano-K obtained in step B 2 O / Na 2 O-WO 3 The granules are mixed with 0.2mol / L glucose aqueous solution in a metered ratio, and subjected to a hydrothermal reaction at 160-190°C for 12-20h to obtain K 2 O / Na 2 O-WO 3 @C Granule mother liquor ;

[0037] Step D: Convert the K obtained in Step C to 2 O / Na 2 O-WO 3 @C particle mother liquor is added to the ammonia solution with a pH value of 13, and the addition amount of...

Embodiment 1

[0077] This example A1 2 O 3 Coated K 2 O / Na 2 O-WO 3 The preparation method of the catalyst is as follows:

[0078] Step A:

[0079] First, take the mass as WO 3 Mass 15% potassium nitrate, 3000% ethylene glycol and 100% (in WO 3 meter) of ammonium metatungstate, then add WO 3 Dissolve 5000% deionized water by mass, stir and mix well.

[0080] Step B:

[0081] The above solution was put into a high pressure reactor at 160°C for solvothermal reaction for 20h, and then put into a muffle furnace for calcination at 450°C for 8h to obtain nano-K 2 O-WO 3 particles.

[0082] Step C:

[0083] The resulting nanoK 2 O-WO 3 Granules, mixed with 0.2mol / L glucose aqueous solution in metered ratio, K 2 O-WO 3 The mass ratio of particles to glucose solution was 1:200. After ultrasonic dispersion, it was placed in an autoclave and hydrothermally reacted at 160 °C for 20 h to obtain K. 2 O-WO 3 @C mother liquor.

[0084] Step D:

[0085] The K obtained in step C 2 O-WO ...

Embodiment 2

[0090] This example A1 2 O 3 Coated K 2 O / Na 2 O-WO 3 The preparation method of the catalyst is as follows:

[0091] Step A:

[0092] First, take the mass as WO 3 5% by mass potassium hydroxide, 15% sodium nitrate, 10000% ethylene glycol and 100% (with WO 3 meter) of sodium metatungstate, then add WO 3 Dissolve 5000% deionized water by mass, stir and mix well.

[0093] Step B:

[0094] Put the above solution into a high pressure reactor at 190°C for 12h solvothermal reaction, and then put it into a muffle furnace and calcinate at 600°C for 3h to obtain nano-K 2 O / Na 2 O-WO 3 particles.

[0095] Step C:

[0096] The resulting nanoK 2 O / Na 2 O-WO 3 Granules, mixed with 0.2mol / L glucose aqueous solution in metered ratio, K 2 O / Na 2 O-WO 3 The mass ratio of particles to glucose solution was 1:500. After ultrasonic dispersion, it was placed in an autoclave and hydrothermally reacted at 190 °C for 12 h to obtain K. 2 O / Na 2 O-WO 3 @C mother liquor.

[0097] St...

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Abstract

The invention discloses a preparation method of an alumina-coated transesterification catalyst, in particular an Al 2 O 3 Coated K 2 O / Na 2 O‑WO 3 The preparation method of catalyst, the method starts with K 2 O‑WO 3 or Na 2 O‑WO 3 as the core center, by coating Al 2 O 3 get K 2 O / Na 2 O‑WO 3 @Al 2 O 3 Composite structure catalyst, used in the reaction of propylene glycol carbonate and methanol to dimethyl carbonate, K 2 O / Na 2 O‑WO 3 with Al 2 O 3 Has a synergistic effect, the Al in the composite catalyst 2 O 3 Provide high specific surface area and better pore distribution for adsorption and screening of reactive molecules, K in the catalyst core center 2 O / Na 2 O‑WO 3 The surface reactant undergoes transesterification to generate dimethyl carbonate, which ultimately effectively improves the selectivity of the target product dimethyl carbonate, and the catalyst has better transesterification activity in the low temperature region (60-80°C).

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and relates to a kind of Al 2 O 3 Coated K 2 O / Na 2 O-WO 3 Catalyst, be specifically related to a kind of K that prepares the coating structure of dimethyl carbonate with transesterification 2 O / Na 2 O-WO 3 @Al 2 O 3 The preparation method of type catalyst. Background technique [0002] Dimethyl carbonate is an important green chemical raw material. It has a wide range of uses and can be used as a solvent, gasoline additive, etc. It is also an important raw material for the synthesis of polycarbonate through propylene carbonate. At present, many researchers at home and abroad are actively researching and promoting new carbonic acid. The method for synthesizing dimethyl carbonate, in which methanol is widely sourced and cheap as a raw material, and the process for synthesizing dimethyl carbonate by transesterification method is mild, and can co-produce ethylene glycol or 1,2-pro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/30B01J35/10C07C68/06C07C69/96
CPCB01J23/30B01J23/002B01J35/0013B01J35/1019B01J35/1042C07C68/06B01J2523/00C07C69/96B01J2523/12B01J2523/13B01J2523/31B01J2523/69Y02P20/52
Inventor 程牧曦李博韩伟李勇马磊王雪峰李俊宏龙雨谦肖云山游林杨柳周政宏赵鹏丁亮刘衍沛
Owner SOUTHWEST RES & DESIGN INST OF CHEM IND
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