Method for recovering molybdenum and method for preparing catalyst
A recovery method and a technology for manufacturing methods, which are applied in catalyst activation/preparation, organic compound preparation, catalyst regeneration/reactivation, etc., can solve problems such as limitations, and achieve the effect of less restrictions
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[0067]Hereinafter, the present invention will be described by way of examples. "Parts" in the examples are parts by mass. In addition, quantitative analysis of contained elements (or molecules) is performed by ICP emission spectrometry and atomic absorption spectrometry. Analysis of raw material gases and products in the process of producing methacrylic acid was performed by gas chromatography.
[0068] The recovery rate of each element, the conversion rate of methacrolein as a raw material, the selectivity rate and yield rate of produced methacrylic acid are defined as follows.
[0069] (a) Recovery rate of each element
[0070] Recovery rate (mass %)=(W r / W s )×100
[0071] Here, W r is the mass of the element contained in the obtained composition, W s is the mass of the element contained in the composition for recovery.
[0072] (b) The conversion rate of methacrolein as a raw material, the selectivity rate of produced methacrylic acid, and the per-pass yield rate....
reference example 1
[0078] (Manufacture of catalyst A for the production of methacrylic acid)
[0079] 100 parts of ammonium paramolybdate, 4.4 parts of ammonium metavanadate and 9.2 parts of cesium nitrate were dissolved in 300 parts of pure water at 70°C. Then add 8.7 parts of 85% by mass phosphoric acid dissolved in 10 parts of pure water, then add 5.5 parts of antimony trioxide, heat up to 95°C while stirring, then add 1.1 parts of nitric acid dissolved in 10 parts of pure water solution of copper. Furthermore, after stirring this liquid mixture at 95 degreeC for 15 minutes, it evaporated to dryness thoroughly, heating and stirring. The dried product obtained by drying the obtained solid at 130°C for 16 hours was press-molded, crushed, and sieved to obtain particles that passed through a sieve with a mesh size of 1.70 mm and remained on a sieve with a mesh size of 0.85 mm. Under air circulation, heat treatment was carried out at 380° C. for 5 hours to obtain catalyst A (composition except o...
Embodiment 1
[0083] (recovery of molybdenum1)
[0084] Use the catalyst (composition other than oxygen atoms: P 1.6 Mo 12 Cs 1 ) After performing the methacrylic acid production test A for 2000 hours, the catalyst was recovered. 56.3 parts of molybdenum, 2.4 parts of phosphorus, and 6.5 parts of cesium were contained in 100 parts of the recovered catalyst. 100 parts of this used catalyst was dispersed in 400 parts of pure water. 130 parts of 45 mass % sodium hydroxide aqueous solution was added there, and it stirred at 60 degreeC for 3 hours. The pH is 12.3. After neutralizing the solution to pH 7 with 36 mass % hydrochloric acid, a solution of 20.5 parts of magnesium chloride hexahydrate dissolved in 50 parts of pure water and 4.5 parts of 29 mass % ammonia water were added, and then 29 mass % ammonia water was added to adjust the pH to 9 Thereafter, the mixture was kept at 30° C. for 3 hours while stirring, and the resulting precipitate and solution were separated by filtration (re...
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