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A tungsten-based hydrotalcite hydrodesulfurization catalyst free of presulfurization and its preparation method

A pre-sulfurized water, hydrodesulfurization technology, applied in physical/chemical process catalysts, chemical instruments and methods, petroleum industry, etc., can solve the problems of complex preparation of pre-sulfur-free catalysts, complicated pre-sulfurization process, etc., and shorten the processing cycle. , the preparation method is simple, the effect of high hydrodesulfurization activity

Active Publication Date: 2022-02-01
SOUTHWEST PETROLEUM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] An object of the present invention is to provide a tungsten-based non-presulfurized hydrotalcite for oil hydrodesulfurization in view of the existing oxidized state catalysts that require a complex presulfurization process and the existing presulfurization-free catalysts. Catalyst

Method used

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  • A tungsten-based hydrotalcite hydrodesulfurization catalyst free of presulfurization and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Weigh Ni(NO 3 ) 2 ·6H 2 O and Al(NO 3 ) 3 9H 2 O and dissolved in boiled deionized water, set the volume to 100mL, and prepared a mixed salt solution with the total concentration of two metal salts being 1mol / L; weigh 8.0g NaOH and dissolve it in boiled deionized water, set the volume to 100mL, Prepare a 2mol / L alkali solution as a precipitant; pour the mixed salt solution into a 250mL flask, and stir magnetically; then add the alkali solution dropwise, when the pH of the solution is 8, stop adding the alkali solution and continue stirring for 0.5h; then The resulting mixed solution was poured into a hydrothermal reaction kettle and reacted at 100°C for 12 hours; the obtained precipitate was washed several times with deionized water until the washing solution was neutral; then the filtrate was vacuum-dried at 80°C for 6 hours; the obtained sample was Nitrate-type nickel aluminum hydrotalcite (Ni 2 Al-NO 3 -LDH).

Embodiment 2

[0032] Weigh Ni(NO 3 ) 2 ·6H 2 O and Al(NO 3 ) 3 9H 2 O, and dissolved in boiled deionized water, set the volume to 100mL to prepare a mixed salt solution with the total concentration of the two metal salts being 1mol / L; weigh 8.0g NaOH and dissolve it in boiled deionized water, set the volume to 100mL, configure A 2mol / L alkali solution was used as a precipitant; the mixed salt solution was poured into a 250mL flask, and magnetically stirred; then the alkali solution was added dropwise, and when the pH of the solution was 9, the dropwise addition of the alkali solution was stopped and stirring continued for 0.5h; then the The resulting mixed solution was poured into a hydrothermal reaction kettle and reacted at 120°C for 8 hours; the obtained precipitate was washed several times with deionized water until the washing liquid was neutral; then the filtrate was vacuum-dried at 80°C for 6 hours; the obtained sample was nitric acid Root-type nickel aluminum hydrotalcite (Ni ...

Embodiment 3

[0034] Weigh Ni(NO 3 ) 2 ·6H 2 O and Al(NO 3 ) 3 9H 2 O, and dissolved in boiled deionized water, set the volume to 100mL, and prepared a mixed salt solution with the total concentration of the two metal salts being 1mol / L; weigh 4.0g NaOH and dissolve it in boiled deionized water, set the volume to 100mL , prepared into a 1mol / L alkali solution as a precipitant; pour the mixed salt solution into a 250mL flask, and magnetically stir; then add the alkali solution dropwise, when the pH of the solution is 7, stop adding the alkali solution and continue stirring for 0.5h; The resulting mixed solution was then poured into a hydrothermal reactor and reacted at 110°C for 15 hours; the obtained precipitate was washed several times with deionized water until the washing solution was neutral; then the filtrate was vacuum-dried at 80°C for 6 hours; the obtained sample Nitrate-type nickel-aluminum hydrotalcite (NiAl-NO 3 -LDH).

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Abstract

The invention discloses a tungsten-based presulfurization-free hydrotalcite hydrodesulfurization catalyst and a preparation method thereof. The catalyst is nickel-aluminum hydrotalcite containing tetrathiotungstate intercalation layer activated by nitrogen gas at high temperature. Preparation method: S1, preparing nickel-aluminum hydrotalcite; S2, dissolving ammonium tetrathiotungstate in boiled deionized water to prepare ammonium tetrathiotungstate solution; S3, mixing nickel-aluminum hydrotalcite with tetrathiotungsten Mix the ammonium acid solution, adjust the pH value to 7-9, conduct ion exchange reaction at 50-70°C for 12-28 hours, filter, wash and dry the obtained exchange product to obtain tetrathiotungstate-intercalated nickel-aluminum hydrotalcite ; S4. Calcining tetrathiotungstate-intercalated nickel-aluminum hydrotalcite at 300-600° C. for 2-4 hours under a nitrogen atmosphere to obtain a tungsten-based hydrodesulfurization-free hydrotalcite catalyst. The catalyst of the invention realizes high dispersion and high loading of active metal components, and the catalyst exhibits high hydrodesulfurization activity in the hydrodesulfurization reaction of oil products.

Description

technical field [0001] The invention relates to the technical field of catalytic hydrodesulfurization, in particular to a tungsten-based presulfidation-free hydrotalcite catalyst and a preparation method thereof. Background technique [0002] In recent years, with the increasingly stringent environmental protection requirements, the pace of upgrading clean oil products has gradually accelerated. Hydrodesulfurization is the main means of producing clean oil, and the development of highly active catalysts is the key to improving the depth of hydrodesulfurization. The main active component of the hydrodesulfurization catalyst is the VIB group metal Mo or W as the main agent, and the VIII group metal Co or Ni as the auxiliary agent. According to whether the carrier is used, the hydrodesulfurization catalyst can be divided into supported catalyst and non-supported catalyst. supported catalyst. [0003] Supported catalysts mainly use alumina or molecular sieves as carriers, and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/25B01J27/02C10G45/08
CPCB01J27/25B01J27/02C10G45/08C10G2300/202C10G2400/04C10G2300/1055C10G2300/1048C10G2300/70
Inventor 王豪杨振东杨帆杨晗吴雁
Owner SOUTHWEST PETROLEUM UNIV