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Supported heteropoly compound catalyst, preparation method and application thereof
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A heteropoly compound and catalyst technology, which is applied in the preparation of organic compounds, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc., can solve the problems of less active sites, large amount of catalysts, and high production costs. problems to achieve high selectivity
Active Publication Date: 2018-07-17
QUFU NORMAL UNIV
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Abstract
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Problems solved by technology
Catalysts based on phosphomolybdovanadium heteropolyacids and their salts still have the disadvantages of low mechanical strength and poor thermal stability. Some patents improve this. For example, in patent JP55079340, metalsulfate is added to the catalyst to improve the mechanical strength. It has a certain effect, but the catalyst does not show good catalytic activity. The patent JP59183832 adds ceramicwhiskers such as siliconcarbide to the catalyst to improve the mechanical strength, but it is difficult to industrialize the application due to the high price of ceramicwhiskers.
[0003] Heteropolyacid catalysts generally have a low specific surface area, and the selective oxidation reaction of methacrolein on heteropolyacid catalysts is a typical surface-type reaction, and the low specific surface area leads to fewer active sites per unit mass of catalyst, so It brings problems such as low production efficiency, large amount of catalyst, and high production cost
If the heteropolyacid catalyst is highly dispersed on the porous carrier, the problem of low specific surface area can be completely solved. Common loading methods include impregnation method, grafting method, sol-gel method, etc. The carrier includes siliconoxide, titaniumoxide, activated carbon, etc., but There are few reports on the selective oxidation of methacrolein over supported heteropoly compound catalysts
Method used
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[0022] (2) Prepare a cesium carbonateaqueous solution with a concentration of 0.1mol / L, take 27mL of impregnated carrier after pretreatment in the previous step, shake at a constant temperature of 50°C for 12 hours, then dry at 105°C, and then calcinate at 600°C for 3 hours;
[0023] (3) Weigh 3.6g of γ-aminopropyltriethoxysilane, dissolve it in 165mL of toluene, immerse the carrier treated in the previous step, modify it at 50°C for 12 hours, and then filter it. Wash the filter cake with ethanol, and dry to obtain the modified carrier;
[0028] The preparation step of catalyst is consistent with embodiment 1, and concrete preparation condition has following differences:
[0029] In (2) step, the concentration of cesium carbonateaqueous solution is 0.15mol / L, and the gained catalyst composition is marked as: (P 1 Mo 11 V 1 Cs 1.5 Cu 0.5 Fe 0.2 ) / SiO 2 .
[0030] The gas-phase oxidation of methacrolein to methacrylic acid was carried out under the same conditions as in Example 1, and the catalytic effects are shown in Table 1.
Embodiment 3
[0032] The preparation step of catalyst is consistent with embodiment 1, and concrete preparation condition has following differences:
[0033] In (2) step, the concentration of cesium carbonateaqueous solution is 0.2mol / L, and the gained catalyst composition mark is: (P 1 Mo 11 V 1 Cs 2 Cu 0.5 Fe 0.2 ) / SiO 2 .
[0034] The gas-phase oxidation of methacrolein to methacrylic acid was carried out under the same conditions as in Example 1, and the catalytic effects are shown in Table 1.
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Abstract
The invention discloses a supported type heteropoly compound catalyst as well as a preparation method and an application thereof and belongs to the field of preparation of catalysts. Porous silica is taken as a supporter and is subjected to acid treatment, caesium exchange and aminated modification, the heteropoly compound containing transition metal counter ions is introduced, so that composite heteropolyacid salt taking caesium and transition metal as counter ions is supported on the supporter surface through high dispersion, and the supported type catalyst is obtained. The catalyst prepared with the method is used for catalyzing methylacrolein to be oxidized for preparation of methacrylic acid. According to the supported type heteropoly compound catalyst as well as the preparation method and the application thereof, the catalyst prepared with the method has high activity and high selectivity for reaction in preparation of methacrylic acid through gas phase oxidation of methylacrolein.
Description
technical field [0001] The invention belongs to the field of catalyst preparation, and in particular relates to a supported heteropoly compound catalyst, a preparation method and an application thereof. Background technique [0002] Heteropolyacid catalysts can effectively catalyze the selective oxidation of organic compounds, among which the oxidation of methacrolein to methacrylic acid is an important industrial application. This reaction uses isobutylene as raw material to produce methyl methacrylate. The key step in the process, since the 1970s, it has been found that the catalyst based on phosphomolybdenum heteropolyacid has high activity and selectivity for the selective oxidation of methacrolein, but the catalyst has poor stability. The lifespan is short, and many companies have published patents afterwards, mainly to improve the performance of the catalyst from two aspects of optimizing the catalyst composition and improving the preparation process. U.S. Patent No. ...
Claims
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Application Information
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