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Layered multi-metal molybdenum sulfide catalyst and preparation method

A technology of catalyst and molybdenum sulfide, applied in physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve problems such as environmental pollution, catalyst ratio, pore volume and activity improvement, and achieve simple preparation methods Easy, reproducible, and inexpensive results

Inactive Publication Date: 2017-05-10
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with the single Mo or single W precursor synthesis catalyst, the multimetal catalyst prepared by this method has obvious structural changes; however, ammonia water is used in the synthesis process of this method, which will pollute the environment
[0006] From the work reported now, it is not difficult to find that existing non-supported metal sulfide catalysts also have shortcomings such as: 1) about removing Ni, Co, such as other metals such as Al, Fe, Ce, Mn on the catalyst There is very little work related to the impact; 2) The raw materials used pollute the environment; 3) The specific surface, pore volume and activity of the catalyst still need to be improved

Method used

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  • Layered multi-metal molybdenum sulfide catalyst and preparation method
  • Layered multi-metal molybdenum sulfide catalyst and preparation method
  • Layered multi-metal molybdenum sulfide catalyst and preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Ni 3 Preparation of Fe-Mo-S:

[0035] a)Ni 3 Preparation of Fe-LDHs: Dissolve 0.09mol nickel nitrate and 0.03mol iron nitrate in 250ml deionized water, stir until clear; weigh 9.6g (0.24mol) sodium hydroxide, 6.36g (0.06mol) sodium carbonate (alkali: Precipitant = 4:1) Dissolve in 250mol deionized water, stir until clear; drop the two solutions into 500ml deionized water at the same time, stir in a 40°C water bath, control the titration rate at 1 drop / second, and fine-tune the titration rate according to the pH , to ensure that the pH is between 9-10; after the titration, stop stirring and keep it for 20-120 minutes, then transfer it to an oven, set the temperature at 70°C, and the crystallization time is 12-24 hours. After the crystallization, the precipitate was filtered and washed with deionized water until the pH was neutral, and the obtained precipitate was dried at 70°C for 12 hours to obtain Ni with an atomic ratio of Ni:Fe=3:1. 3 Fe-LDHs. Its hydrotalcite st...

Embodiment 2

[0047] Ni 3 Adjustment of pH in the preparation of Fe-LDHs:

[0048] The preparation process is similar to Example 1, the difference is to adjust the ratio of alkali: alkali precipitant to 10:1, 1:1, so as to control Ni 3 The pH range of the titration during the synthesis of Fe-LDHs to obtain the Ni under different pH conditions 3 Fe-LDHs

Embodiment 3

[0050] Ni 3 Control of LDO decomposition temperature in the preparation of Fe-Mo-S:

[0051] The preparation process is similar to Example 1, the difference is that Ni 3 The decomposition temperature of Fe-LDHs is changed to 350°C, 450°C, 500°C, and the structure will not recover if it is higher than 600°C, and finally different Ni 3 Fe-Mo-S catalyst.

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Abstract

The invention relates to a layered multi-metal molybdenum sulfide catalyst and a preparation method. The catalyst is represented by a formula M1M2-Mo-S, M1 represents <+2>-valence metal of one of Ni, Co, Mg or Mn, and M1 represents <+3>-valence metals of one or two of Fe, Al or Ce. The catalyst uses a M1M2 oxide form as a calculating base, Mo represents a vulcanized state, and the Mo element content is 1%-50%. Soluble salt of the M1 and soluble salt of the M2 are dissolved in ionized water to form a corresponding metal salt solution; then alkali and an alkali precipitant are prepared into a solution, and coprecipitation is performed to obtain a hydrotalcite compound; calcination is performed in a muffle furnace to obtain metallic oxides of corresponding elements; soluble Mo acid radical anion salt is dissolved in water, the metallic oxides are added to obtain the hydrotalcite compound intercalated with Mo acid radical anions, and then the catalyst is obtained through vulcanization. The preparation method is simple, easy to operate and high in repeatability and can be applied to industrial production.

Description

technical field [0001] The invention belongs to the technical field of industrial catalysis and bioenergy conversion, and relates to the preparation of polymetallic sulfide catalysts, in particular to a layered polymetallic molybdenum sulfide catalyst and a preparation method. Background technique [0002] In recent years, unsupported polymetallic sulfide catalysts have attracted more and more attention in the field of hydrogenation catalysis, especially in the deep desulfurization of oil products. Transition metal sulfides are typical two-dimensional layered materials, whose edge sites provide abundant active sites for catalytic processes and have strong catalytic effects. The non-supported polymetallic sulfide catalyst does not need a carrier and has a high content of active components, which has higher hydrogenation activity and can meet the society's requirements for oil cleanliness. [0003] The currently used synthesis methods of non-supported sulfide catalysts includ...

Claims

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Application Information

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IPC IPC(8): B01J27/051C10G45/08
CPCB01J27/0515C10G45/08
Inventor 纪娜刁新勇王琪琪宋静静梁长海刘庆岭宋春风
Owner TIANJIN UNIV