Iron catalyst for preparing butadiene through n-butene oxydehydrogenation and preparation method and application of iron catalyst

An oxidative dehydrogenation and iron catalyst technology, which is applied in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problem of easy powder loss and low catalyst wear resistance. and other problems, to achieve the effect of low amplification risk, high butadiene selectivity and yield, and high catalytic activity

Inactive Publication Date: 2014-04-30
WISON ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the oxidative dehydrogenation of n-butene to butadiene mainly adopts iron catalyst, and the reactor adopts fluidized bed or adiabatic fixed bed; Chinese patents CN1184705, CN1072110 and CN1033013 have developed a fluidized reactor with high catalytic activity and good butadiene selectivity. bed catalyst, but the catalyst wear resistance is low, and it is easy to be pulverized and lost. Therefore, Chinese patents CN102580749 and CN102716754 adopt the method of spray drying to prepare microsphere catalysts, which improves the wear resistance of the catalyst and reduces the fluidization of the catalyst. Pulverization running loss in reaction state

Method used

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  • Iron catalyst for preparing butadiene through n-butene oxydehydrogenation and preparation method and application of iron catalyst

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Experimental program
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Effect test

Embodiment 1

[0016] Ferric nitrate, zinc nitrate, aluminum chloride, nitric acid and water are mixed and dissolved in a certain proportion to form a mixed metal salt solution, and then ammonia water and mixed metal salt solution are added dropwise to the precipitation tank at a certain speed, and the slurry in the precipitation tank needs to be fully stirred to precipitate The temperature of the slurry is controlled at 10.0°C, and the pH value of the precipitation slurry is controlled at 5.0. After the precipitation is completed, the pH value is maintained and the stirring and aging is continued for 120 minutes. The catalyst was flaked into granules, and then activated at 650.0°C for 8 hours. The prepared catalyst was numbered A. The mass ratio of iron (Fe) / zinc (Zn) in the catalyst was 5.02:1, and the mass content of aluminum (Al) was 0.001%. is oxygen (O), see Table 1 and Table 2 for the comparison of the adiabatic reaction performance of the catalyst and the comparison catalyst.

Embodiment 2

[0018] Ferric nitrate, zinc nitrate, nickel nitrate, copper nitrate, barium chloride, cobalt nitrate, nitric acid and water are mixed and dissolved in a certain proportion to form a mixed metal salt solution, and then the ammonium bicarbonate solution is added dropwise into the mixed metal salt solution at a certain speed, The precipitation slurry needs to be fully stirred, the temperature of the precipitation slurry is controlled at 100.0°C, and the pH value of the precipitation slurry is controlled at 8.0. After the precipitation is completed, the precipitation slurry is filtered and washed to pH = 6.0-8.0. After the filter cake is dried at 120.0°C for 12 hours, then sliced Particle catalyst, then activated at 800.0°C for 4h, the number of prepared catalyst is B, the mass ratio of iron (Fe) / zinc (Zn) in the catalyst is 6.94:1, the mass content of nickel (Ni) is 0.12%, copper (Cu ) mass content is 0.54%, barium (Ba) mass content is 0.27%, cobalt (Co) mass content is 1.07%, and...

Embodiment 3

[0020] After iron-containing steel, metal zinc and metal copper are dissolved in nitric acid solution, manganese nitrate is added, and a mixed metal salt solution with a certain metal ion ratio is configured as required, and then the ammonia water / urea mixed solution is added dropwise to the mixed metal salt solution at a certain speed, Stir well, control the temperature of the precipitation slurry at 40.0°C, control the pH value of the precipitation end point at 6.50, maintain the pH value after the precipitation end point and continue to stir and age for 60 minutes, filter the precipitation slurry and wash until pH = 6.0-8.0, then dry the filter cake at 120.0°C 24h, then chipped into a granular catalyst, and then activated at 550.0°C for 48h. The prepared catalyst was numbered C. The mass ratio of iron (Fe) / zinc (Zn) in the catalyst was 1.21:1, and the mass content of copper (Cu) was 0.05 %, the mass content of manganese (Mn) is 1.00%, and the rest is oxygen (O). The adiabati...

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Abstract

The invention relates to an iron catalyst for preparing butadiene through n-butene oxydehydrogenation and a preparation method and application of the iron catalyst. The catalyst comprises an iron element, a zinc element, other elements and an oxygen element, wherein the mass ratio of iron (Fe) to zinc (Zn) is (1.21-6.94):1; the total content of other elements is 0.001-2.00wt% of the total content of the catalyst; the other elements are selected from one or more of calcium (Ca), nickel (Ni), copper (Cu), barium (Ba), chromium (Cr), manganese (Mn), phosphorus (P), silicon (Si), vanadium (V), cobalt (Co), aluminum (Al), molybdenum (Mo), stannum (Sn), stibium (Sb), titanium (Ti), zirconium (Zr) and rare earth. The catalyst is prepared by using a precipitation method, and is applicable to a heat insulation fixing bed. Compared with the prior art, the catalyst provided by the invention has the advantages of high activity, high selectivity and the like.

Description

technical field [0001] The invention relates to a catalyst, in particular to an iron catalyst for producing butadiene by oxidative dehydrogenation of n-butene and its use. Background technique [0002] In recent years, ethylene cracking raw materials tend to be lighter, which has led to a slow increase in the production capacity of the by-product butadiene, and even a structural shortage. Chemical application will realize partial replacement of naphtha steam cracking unit, thereby reducing the production capacity of extracting butadiene. With the rapid development of the downstream industry of butadiene worldwide, the demand for butadiene is increasing rapidly, and the development of butadiene oxidative dehydrogenation technology can effectively fill the gap of butadiene. [0003] At present, the oxidative dehydrogenation of n-butene to butadiene mainly adopts iron catalyst, and the reactor adopts fluidized bed or adiabatic fixed bed; Chinese patents CN1184705, CN1072110 an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/80B01J23/889C07C11/167C07C5/48
Inventor 杨文书吴勇军黄孟凯李延生
Owner WISON ENG
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