A kind of catalyst for preparing unsaturated acid or unsaturated ester
A catalyst and compound technology, applied in molecular sieve catalysts, physical/chemical process catalysts, preparation of carboxylate esters, etc., can solve problems such as inability to meet large-scale production, easy loss of active ingredients, and complex influencing factors, and achieve good industrial application prospects , low cost, simple effect of industrial preparation
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Embodiment 1
[0058] Example 1 Preparation of catalyst
[0059] Na-molecular sieve with FER configuration
[0060] Na-FER molecular sieve was purchased from Shanghai Zhuoyue Chemical Technology Co., Ltd.
[0061] Table 1 Three Na-FER molecular sieves with different average particle size
[0062] Na-FER Si / Al Grain size (μm)D 50 (μm)
Sample A2 / 6.50.1-0.51.6 Sample B30 / 70.5-1.53.0 Sample C50 / 6.51.5-3.54.8
[0063] Preparation of H-FER
[0064] Na-FER catalyst was purchased from Shanghai Zhuoyue Chemical Technology Co., Ltd. Exchange 10 grams of calcined Na-molecular sieve with FER configuration three times with 0.5mol / L ammonium nitrate for 2 hours each time, wash with deionized water, dry, calcined at 550°C for 4 hours, and prepare 20 by extrusion ~40 mesh H-FER catalyst, samples A, B, and C were prepared into catalyst samples 1#, 2#, and 3# respectively.
[0065] Preparation of supported M-FER (M stands for supported metal)
[0066] The M-FER catalyst was prepared by the equal volume impregna...
Embodiment 2
[0091] Example 2 Reaction of methylal DMM with methyl acetate MAc
[0092] 10g of the above-mentioned catalyst samples 1# to 10# and catalyst samples D0# to D10# were respectively put into a fixed bed reactor with a tube inner diameter of 28 mm, and the temperature was raised to 550°C at 5°C / min under a nitrogen atmosphere and kept for 4 hours. Then, the reaction temperature was lowered to 350° C. in a nitrogen atmosphere, and the pressure of the reaction system was increased to a reaction pressure of 3 Mpa with nitrogen. The reaction raw materials (where the molar ratio of methylal and methyl acetate is 2:1) from top to bottom with a total feed space velocity of 0.3h -1 Through the catalyst bed, the catalyst evaluation results are shown in Table 3. Sampling and analysis after 30h reaction time, the results are shown in Table 3.
[0093] Table 3 Evaluation results of catalysts for reaction between methylal DMM and methyl acetate MAc
[0094]
Embodiment 3
[0095] Example 3 Different reaction conditions
[0096] Put 10g of the above-mentioned 10# catalyst into a 28 mm fixed-bed reactor respectively in a tube and heat up to 550°C at 5°C / min under a nitrogen atmosphere and keep it for 4 hours. Then, in a nitrogen atmosphere, the reaction temperature is lowered to 200°C to 400°C, the DMM / MAc molar ratio is 2 / 1, and the pressure of the reaction system is increased to a reaction pressure of 0.2Mpa to 15.0Mpa with nitrogen. The reaction raw materials from top to bottom with the total feed space velocity of 0.05h -1 To 10.0h -1 Through the catalyst bed. The specific reaction conditions are shown in Table 4. Sampling and analysis after 30h reaction time, the results are shown in Table 4.
[0097] Table 4 Catalyst pretreatment and reaction conditions
[0098]
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