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A kind of catalyst for preparing dimethyl carbonate and its preparation method and application

A technology of dimethyl carbonate and catalyst, which is applied to the catalyst and preparation field for the preparation of dimethyl carbonate, can solve the problems of equipment corrosion, the catalytic activity cannot be further improved, the catalyst life is short, etc., and achieves the improvement of the reaction activity, the elimination of pollution, the promotion of the effect of diffusion

Active Publication Date: 2020-09-22
SHANXI LUAN MINING GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In addition, in the traditional method for the preparation of copper-based supported catalysts for methanol oxidative carbonylation, compared with the impregnation method (IWIM) and solution ion exchange method (LSIE), the solid-state ion exchange method (SSIE) can prepare the catalyst with a high content of Cu. + The catalyst of the active center, and this method has simple steps and will not be affected by the solvent, but the commonly used CuCl copper source will cause problems such as equipment corrosion and short catalyst life
Wang Yuchun from Taiyuan University of Technology and others (Wang Yuchun, Chemical Journal of Chinese Universities, 2015(12): 2540-2549) prepared a copper-based molecular sieve catalyst using copper acetylacetonate as a copper source, which avoided the pollution of the catalyst by chloride ions and improved the catalytic performance of the catalyst. Activity and stability, but due to the limitation of the support structure, the catalytic activity cannot be further improved

Method used

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  • A kind of catalyst for preparing dimethyl carbonate and its preparation method and application
  • A kind of catalyst for preparing dimethyl carbonate and its preparation method and application
  • A kind of catalyst for preparing dimethyl carbonate and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] (1) Weigh 5g Al-KIT-6 molecular sieve (the specific surface area is 798.2m 2 / g, the pore diameter is 9.17nm, and the pore volume is 2.69cm 3 / g, Si / Al=40) and 2.05g copper acetylacetonate were uniformly mixed in an agate mortar, and steam impregnated in a muffle furnace at 250°C for 4h to obtain a catalyst precursor.

[0044] (2) Weigh 2g of the catalyst precursor, and perform a temperature-programmed activation under a protective gas with a nitrogen-to-oxygen volume ratio of 10:1. ℃, constant temperature 10h. After cooling to room temperature, a Cu-Al-KIT-6(S) catalyst was obtained, and the copper species loading amount in the catalyst was 10wt% in terms of metal. The specific surface area of ​​the catalyst is 499.3m 2 / g, the pore volume is 1.62cm 3 / g, the mesopore diameter is 7.02nm.

[0045] The activity of the catalyst in the gas-phase oxidative carbonylation of methanol is listed in Table 1, and the specific evaluation process is as follows:

[0046] Take ...

Embodiment 2

[0048] (1) Weigh 5g Al-KIT-6 molecular sieve (the specific surface area is 910.3m 2 / g, the pore diameter is 8.99nm, and the pore volume is 2.56cm 3 / g, Si / Al=60) and 3.07g copper acetylacetonate were uniformly mixed in an agate mortar, and steam impregnated in a muffle furnace at 250°C for 4h to obtain a catalyst precursor.

[0049] (2) Weigh 2g of the catalyst precursor, and perform a temperature-programmed activation under a protective gas with a nitrogen-to-oxygen volume ratio of 10:1. ℃, constant temperature 10h. After cooling to room temperature, a Cu-Al-KIT-6(S) catalyst was obtained, and the copper species loading amount in the catalyst was 15wt% in terms of metal. The specific surface area of ​​the catalyst is 530.6m 2 / g, the pore volume is 1.78cm 3 / g, the mesopore diameter is 7.54nm.

[0050] (3) Raise the temperature of the catalyst bed to 160° C. for catalyst evaluation. Other parameters and test methods are as in Example 1. The activities of the catalysts ...

Embodiment 3

[0052] (1) Weigh 5g Al-KIT-6 molecular sieve (specific surface area is 772.9m 2 / g, the pore diameter is 7.39nm, and the pore volume is 2.17cm 3 / g, Si / Al=10) and 3.07g copper acetylacetonate were evenly mixed in an agate mortar, and steam impregnated in a muffle furnace at 300°C for 10h to prepare a catalyst precursor.

[0053] (2) Weigh 2g of the catalyst precursor, and perform a temperature-programmed activation under a protective gas with a nitrogen-to-oxygen volume ratio of 10:2. ℃, constant temperature 5h. After cooling to room temperature, a Cu-Al-KIT-6(S) catalyst was obtained, and the copper species loading amount in the catalyst was 15wt% in terms of metal. The specific surface area of ​​the catalyst is 470.8m 2 / g, the pore volume is 1.25cm 3 / g, the mesopore diameter is 6.78nm.

[0054] (3) The proportion of raw materials for reaction sampling is: CO:O 2 :CH 3 OH=9:1:5, the volume space velocity is 5000h -1 , the catalyst bed temperature is 160° C., and oth...

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Abstract

A catalyst for preparing dimethyl carbonate is composed of an active component Cu and an Al-KIT-6 dielectric pore molecular sieve, wherein the Cu accounts for 10-30wt%, and the balance is the Al-KIT-6dielectric molecular sieve. The catalyst provided by the invention has the advantages of high catalytic activity.

Description

technical field [0001] The invention relates to the field of catalysts, in particular to a catalyst for preparing dimethyl carbonate, a preparation method and an application. Background technique [0002] Dimethyl carbonate is a low-toxic, environmentally friendly intermediate in organic synthesis, which is widely used. The Y-type molecular sieve commonly used in the gas-phase oxidative carbonylation reaction of methanol to prepare dimethyl carbonate is limited by the window aperture (0.23nm) of the small cage, so that a part of the copper species exchanged in the small cage cannot play the role of its catalytic active center (Huang Shouying, Industrial&Engineering Chemistry Research, 2013,52(19):6349-6356.), reduces the utilization rate of active species; in addition, similar microporous materials cause the adsorption of macromolecular reactants and the diffusion of products due to the limitation of pore size. certain influence. [0003] In this regard, the current resear...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/03B01J35/10B01J37/02B01J37/08B01J37/30C07C68/01C07C69/96
CPCB01J29/0333B01J35/1019B01J35/1023B01J35/1047B01J35/1061B01J37/0203B01J37/086B01J37/30B01J2229/18C07C68/00C07C69/96
Inventor 李忠阎立飞张国强尹娇郑华艳
Owner SHANXI LUAN MINING GRP