A kind of method for directly preparing dimethylamine from synthesis gas
A synthesis gas and dimethylamine technology, which is applied in the preparation of amino compounds, chemical instruments and methods, and the preparation of hydroxyl compounds, can solve the problems of high proportion of trimethylamine and low selectivity of dimethylamine, and achieve low catalyst cost , Improve the selectivity of dimethylamine, the effect of simple synthesis
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[0044] And, the preparation method of described methanol catalyst, comprises the following steps:
[0045] (1) The copper salt, zinc salt and aluminum salt are adjusted according to CuO: 30-60%, ZnO: 30-60%, Al 2 O 3 : 5-10% metal molar ratio is configured into mixed salt solution, and copper salt solution and zinc salt solution are one or more of hydrochloride solution, nitrate solution and acetate solution;
[0046] (2) The mixed salt solution and the precipitating agent are reacted, the pH value of the solution is 8-10, the precipitation temperature is 40-80 °C, and the precipitating agent is Na 2 CO 3 , NaHCO 3 One or more of , NaOH and urea;
[0047] (3) After the precipitate is separated from the mother liquor, the precipitate is repeatedly washed with deionized water, the temperature of the deionized water is 40-60 ° C, and then dried and roasted in the air, the drying temperature is 90-120 ° C, and the drying time is 12- 24h, the calcination temperature is 300-500...
Embodiment 1
[0058] Methanol catalyst CuZnAl synthesis: Weigh 10.87g of copper nitrate trihydrate, 13.38g of zinc nitrate hexahydrate and 3.75g of aluminum nitrate nonahydrate, put them into a beaker containing 200mL, keep at 60°C, and take this solution as solution A. Dissolve 9.54 g of sodium carbonate solution in 100 mL of deionized water, and use this solution as solution B. The solution B was slowly added dropwise to the solution A, while vigorously stirring, the temperature was maintained at 60°C, and the pH in the system was controlled at about 8.6 by the rate of addition of the sodium carbonate solution. After the precipitation was completed, it was aged at room temperature overnight, filtered, washed with deionized water at 60 °C for 5 times until the filtrate was neutral, and finally dried at 120 °C for 6 hours, and calcined at 350 °C for 5 hours in a muffle furnace to obtain CuZnAl methanol catalyst, CuZnAl The molar ratio is 45:45:10, and the XRD pattern of the CuZnAl sample is...
Embodiment 2
[0060] Synthesis of HZSM-5 catalyst: Weigh 4.87g of silica, 0.48g of boehmite, 0.28g of sodium hydroxide, and 0.25g of tetrapropylammonium bromide, add them to an agate mortar, grind for 5-10min, and then add them to In a hydrothermal kettle, crystallize at 200°C for 16h. After crystallization, cool to room temperature in an ice-water bath, repeatedly wash with deionized water until neutral, and dry at 120°C overnight to obtain NaZSM-5 molecular sieve. The NaZSM-5 powder was added to a 1M ammonium nitrate aqueous solution with a solid-liquid mass ratio of 1:10, vigorously stirred, and ion exchanged at 80 °C. This process was repeated three times. After filtration, the powder was dried at 120 °C for 6 hours. Finally, it was calcined in air at 500 °C for 5 h to obtain HZSM-5 molecular sieve. The XRD pattern of the ZSM-5 sample is as follows image 3 shown.
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