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Iron catalyst used in butadiene production through n-butylene oxidation dehydrogenation, and preparation method and application thereof

An oxidative dehydrogenation, iron catalyst technology, applied in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical instruments and methods, etc. The problem of obvious effect, etc., achieves the effects of good reaction stability, high butadiene selectivity, and simple preparation process.

Active Publication Date: 2013-04-24
WISON ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The oxidative dehydrogenation of n-butene uses a fluidized bed as the reactor, which requires high catalyst strength and wear resistance. The catalyst powder brought out of the reaction system often blocks the post-treatment system, making it difficult to recover the catalyst. The disadvantage of the fluidized bed also involves operation. Complicated, the amplification effect is obvious
The fluidized bed catalyst disclosed in early Chinese patents CN1184705, CN1072110 and CN1033013 has the advantages of high catalytic activity and good butadiene selectivity, but the mechanical strength and wear resistance of the catalyst are low, and the catalyst is easy to pulverize and lose. Treatment system; Chinese patents CN102580749 and CN102716754 all attempt to prepare microsphere catalysts by spray drying method, on the basis of maintaining good performance of the catalyst, reduce the pulverization and loss of the catalyst in the fluidized state as far as possible, but it is still difficult to avoid catalyst powder Clogging and aftertreatment system clogging

Method used

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  • Iron catalyst used in butadiene production through n-butylene oxidation dehydrogenation, and preparation method and application thereof
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  • Iron catalyst used in butadiene production through n-butylene oxidation dehydrogenation, and preparation method and application thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] After the iron powder and metal zinc are dissolved in nitric acid solution, magnesium nitrate and manganese nitrate are added, and the final configuration is 4.43×10 -3 Mole of magnesium (Mg) / one mole of iron (Fe), 0.247 mole of zinc (Zn) / one mole of iron (Fe) and 0.109 mole of manganese (Mn) / one mole of iron (Fe) concentration, and then mix Add ammonia water dropwise to the metal salt solution, stir well, control the temperature of the precipitation slurry at 60.0°C, control the pH value of the precipitation end point at 7.50, maintain the pH value after the precipitation end point, continue stirring and aging for 60 minutes, filter the precipitation slurry and wash until pH = 7.0-9.0, Then the filter cake is extruded, dried at 200.0°C for 12h, and then activated at 500.0°C for 48h. The prepared catalyst is numbered A, and its mass composition is: iron (Fe) 51.85wt%, magnesium (Mg) 0.01wt%, manganese (Mn) 5.00wt%, zinc (Zn) 15.00wt%, and the rest is oxygen (O). The adi...

Embodiment 2

[0029] The steel is dissolved in a mixed solution of nitric acid and hydrochloric acid, then mixed with ferric nitrate nonahydrate, magnesium nitrate hexahydrate, cobalt nitrate and water and stirred evenly, and finally configured into 0.846 moles of magnesium (Mg) / one mole of iron (Fe), 3.88× 10 -3 Mole of cobalt (Co) / one mole of iron (Fe) concentration mixed metal salt solution, then the mixed metal salt solution is added dropwise in ammonia water, fully stirred, the temperature of the precipitation slurry is controlled at 60.0 ° C, the pH value of the precipitation end point is controlled at 11.0, and then Immediately filter the precipitated slurry and wash it to pH = 7.0-9.0, dry the filter cake at 105.0°C for 12h, then slice it into a granular catalyst, and activate it at 700.0°C for 16h. The prepared catalyst is numbered B, and its mass composition is: iron (Fe) 48.87wt%, magnesium (Mg) 18.00wt%, cobalt (Co) 0.20wt%, and the rest is oxygen (O). The adiabatic fixed bed re...

Embodiment 3

[0031] The steel is dissolved in a mixed solution of nitric acid and hydrochloric acid, then mixed with magnesium nitrate hexahydrate, calcium nitrate, ammonium molybdate, and antimony chloride and stirred evenly. , 1.28×10 -2 One mole of calcium (Ca) / one mole of iron (Fe), 2.32×10 -3 One mole of molybdenum (Mo) / one mole of iron (Fe), 2.96×10 -3 Mixed metal salt solution with molar antimony (Sb) / one molar iron (Fe) concentration, then add ammonia water to the mixed metal salt solution dropwise, stir well, control the temperature of the precipitation slurry at 80.0°C, control the pH value of the precipitation end point at 8.30, and control the precipitation end point Then maintain the pH value, continue to stir and age for 30 minutes, filter the precipitated slurry and wash to pH = 7.0-9.0, dry the filter cake at 200.0°C for 5 hours, and then punch it into a granular catalyst, and activate it at 850.0°C for 4 hours, the prepared catalyst The code is C, and the mass compositio...

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Abstract

The invention relates to an iron catalyst used in butadiene production through n-butylene oxidation dehydrogenation, and a preparation method and an application thereof. The catalyst comprises Fe as a main component, and a co-catalyst comprising Mg, Zn, and other elements. The catalyst is composed of, by mass, 48.80-60.53% of Fe, 0.01-18.00% of Mg, 0-15.00% of Zn, 0-5.00% of other elements, and balance of oxygen element. The catalyst is prepared with a precipitation method. The catalyst is applied in butadiene production through n-butylene oxidation dehydrogenation by using an adiabatic fixed bed. Application conditions comprise: adiabatic fixed bed material inlet temperature is 260.0-445.0 DEG C; molar ratio of inlet oxygen to n-butylene is 0.42-0.90; molar ratio of inlet water to n-butylene is 12.0-25.0; inlet n-butylene volume space velocity is 180-600h<-1>, and an adiabatic fixed bed material outlet temperature is 457.0-650.0 DEG C. Compared with prior arts, the catalyst provided by the invention is suitable for an adiabatic fixed bed, and has the advantages such as high butadiene selectivity, good catalyst reaction stability, and the like.

Description

technical field [0001] The invention relates to a catalyst, in particular to an iron catalyst used for producing butadiene by oxidative dehydrogenation of n-butene in an adiabatic fixed bed, as well as its preparation method and application. Background technique [0002] In recent years, the downstream industries of butadiene such as styrene-butadiene rubber, butadiene rubber, nitrile rubber, ABS resin, SBS thermoplastic elastomer and styrene-butadiene latex have developed rapidly, and the raw materials of butadiene are in short supply. The rise of shale gas chemical industry has caused a decline in the production of butadiene obtained through extraction methods, and the oxidative dehydrogenation of n-butene has become an effective way to obtain butadiene. [0003] The n-butene oxidative dehydrogenation reactor mainly includes fluidized bed and adiabatic fixed bed. [0004] The oxidative dehydrogenation of n-butene uses a fluidized bed as the reactor, which requires high ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/889B01J23/75B01J23/887B01J23/80B01J23/835B01J27/188B01J23/78C07C11/167C07C5/48
Inventor 杨文书吴勇军李延生王彪陈惠梅
Owner WISON ENG
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