Methods for preparing piperazine and catalyst by gas-solid-phase catalytic synthesis of ethylene glycol
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A kind of ethylene glycol, gas-solid phase technology
Inactive Publication Date: 2017-05-31
SHAANXI YANCHANG PETROLEUM GRP
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[0010] The problem of above-mentioned synthetic piperazine method is to use ethanolamine, ethylenediamine or hydroxyethylethylenediamine as reaction raw material, at first will set out to prepare the raw material of synthetic piperazine from ethylene or ethylene oxide or ethylene glycol, and its raw material price is relatively high. high, the overall process is complex, and the cost of synthesizing piperazine is relatively high; secondly, the raw materials often need to be diluted with a large amount of diluent, resulting in high preheating energy consumption and separation costs, and a decrease in product yield; in addition, the required reaction temperature or pressure is relatively high. High, the reaction conditions are relatively harsh
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Embodiment 1
[0032] Catalyst preparation
[0033] Weigh 9.9102 grams of nickel nitrate hexahydrate, 7.6034 grams of copper nitrate trihydrate, add 16 milliliters of deionized water, stir and dissolve to prepare an aqueous nitrate solution, weigh 20 grams of mordenite carrier and add it to the aqueous nitrate solution for immersion, and soak for 24 hours at normal temperature. Thereafter, it was dried at 110° C. for 6 hours, and then calcined at 450° C. for 4 hours to prepare composite metal oxide catalyst A.
[0034] Catalyst evaluation conditions: reaction temperature 230°C, pressure 10MPa, ammonia to ethylene glycol molar ratio 30:1, hydrogen to ethylene glycol molar ratio 1:1, raw material ethylene glycol liquid space velocity 0.2h -1 .
Embodiment 2
[0036] Catalyst A prepared in Example 1 was used for testing.
[0037] Catalyst evaluation conditions: reaction temperature 227°C, pressure 13MPa, ammonia to ethylene glycol molar ratio 30:1, hydrogen to ethylene glycol molar ratio 1:1, raw material ethylene glycol liquid space velocity 0.2h -1 .
Embodiment 3
[0039] Catalyst preparation
[0040] Weigh 9.9102 gram of nickel nitrate hexahydrate, 6.0827 gram of copper nitrate trihydrate, 0.9061 gram of zinc acetate, add 16 milliliters of deionized water, stirring and dissolving is mixed with nitrate aqueous solution, takes by weighing 20 gram of mordenite carrier and adds in the nitrate aqueous solution to impregnate, Immerse at a constant temperature of 50°C for 20 hours, then dry at 110°C for 6 hours, and then bake at 480°C for 4 hours to prepare composite metal oxide catalyst B.
[0041] Catalyst evaluation conditions: reaction temperature 232°C, pressure 9MPa, ammonia to ethylene glycol molar ratio 30:1, hydrogen to ethylene glycol molar ratio 1:1, raw material ethylene glycol liquid space velocity 0.2h -1 .
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Abstract
The invention provides methods for preparing piperazine and a catalyst by gas-solid-phase catalytic synthesis of ethylene glycol. The raw material (ethylene glycol) is mixed with certain quantities of ammonia and nitrogen to react via an amination catalyst to produce piperazine and derivatives of piperazine; and nickel, iron, copper, zinc, cobalt and the like serve as active components or additives in the amination process, mordenite serves as a carrier, and the mixed metal oxide amination catalyst is prepared by the impregnation method. The conversion rate of ethylene glycol can reach 42%, and the selectivity of piperazine reaches 75%.
Description
technical field [0001] The invention belongs to the technical field of ethylene glycol catalytic application, and in particular relates to a method for preparing piperazine through catalytic amination of ethylene glycol and a preparation method for a corresponding supported composite metal oxide catalyst. Background technique [0002] Piperazine is mainly used in the pharmaceutical industry to make insect repellent, anti-tuberculosis, antihypertensive, and antibacterial drugs. It can be used to make dyes and prevent fading of printed and dyed fabrics. It can also be used as rubber vulcanization accelerators, antioxidants, Stabilizers, surfactants, polyurethane production aids, etc., are widely used due to their low toxicity and high economic value. [0003] The homogeneous synthesis process has been gradually eliminated due to serious environmental pollution and equipment corrosion. At present, the research at home and abroad mainly focuses on heterogeneous catalytic synthes...
Claims
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