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Catalyst and method used for preparing 1,3-butadiene by oxidative dehydrogenation of n-butene

A technology for oxidative dehydrogenation and catalysts, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxides/metal hydroxide catalysts, etc., can solve the problem of poor catalytic activity and selectivity, and the inability to obtain effective C4 fractions Utilization and other issues to achieve high activity, selectivity, and efficient utilization

Active Publication Date: 2012-12-19
SHAANXI COAL & CHEM TECH INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

For these C4 fractions, after the isobutene is removed by the domestic mature methyl tert-butyl ether method, the n-butene content can reach more than 90%, which can be used as the raw material for oxidative dehydrogenation to prepare butadiene, but compared with petrochemical by-product C4 fractions , the C4 fraction of coal-to-olefins contains a high content of low-reactivity trans-2-butene, and contains active oxygen-containing compounds and other impurities. The above-mentioned cobalt-molybdenum catalyst used by Mitsubishi Chemical Corporation or the traditional single zinc ferrite catalyst is used , the catalytic activity and selectivity are poor, and the conversion rate of n-butene is less than 50%, so a complicated raw material purification process must be carried out, otherwise the C4 fraction cannot be effectively utilized

Method used

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  • Catalyst and method used for preparing 1,3-butadiene by oxidative dehydrogenation of n-butene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Catalyst preparation process

[0031] In a 500mL beaker, add 21.78gFe(NO 3 ) 3 9H 2 O, 8.02gZn(NO 3 ) 2 ·6H 2 O, 1.17gCo(NO 3 ) 3 ·6H 2 O, 0.21gMg(NO 3 ) 2 ·6H 2 O and 200mL deionized water, wherein the molar ratio of iron to zinc is 2:1, the molar ratio of cobalt to zinc is 0.15:1, and the molar ratio of magnesium to zinc is 0.03:1, stir to dissolve it, and add the mass fraction It is 25% ammonia solution, adjust the pH value of the solution to 9, after the dropwise addition, heat to 60°C and stir for 1h, cool to 20°C, filter with a Buchner funnel, wash the filter cake with deionized water until neutral, the obtained solid is in After drying at 120°C for 10 hours, place it in a muffle furnace and bake at 600°C for 8 hours, cool, grind, and sieve to obtain a 20-60 mesh cobalt and magnesium-modified zinc ferrite catalyst, which is sealed and stored.

[0032] Oxidative Dehydrogenation Process

[0033] Fill 2mL of the above catalyst into a stainless steel reac...

Embodiment 2

[0036] Catalyst preparation process

[0037] In a 500mL beaker, add 21.78gFe(NO 3 ) 3 9H 2 O, 8.02gZn(NO 3 ) 2 ·6H 2 O, 0.39gCo(NO 3 ) 3 ·6H 2 O, 0.21gMg(NO 3 ) 2 ·6H 2 O and 200mL deionized water, wherein the molar ratio of iron to zinc is 2:1, the molar ratio of cobalt to zinc is 0.05:1, and the molar ratio of magnesium to zinc is 0.03:1, stir to dissolve it, and add the mass fraction It is 25% ammonia solution, adjust the pH value of the solution to 10, after the dropwise addition, heat to 50°C and stir for 2h, cool to 20°C, filter with Buchner funnel, wash the filter cake with deionized water until neutral, the obtained solid is in After drying at 100°C for 12 hours, place it in a muffle furnace and bake at 500°C for 10 hours, cool, grind, and sieve to obtain a 20-60 mesh cobalt and magnesium-modified zinc ferrite catalyst, which is sealed and stored.

[0038] Oxidative Dehydrogenation Process

[0039] Fill 2mL of the above catalyst into a stainless steel reac...

Embodiment 3

[0042] Catalyst preparation process

[0043] In a 500mL beaker, add 21.78gFe(NO 3 ) 3 9H 2 O, 8.02gZn(NO 3 ) 2 ·6H 2 O, 1.17gCo(NO 3 ) 3 ·6H 2 O, 0.07gMg(NO 3 ) 2 ·6H 2 O and 200mL deionized water, wherein the molar ratio of iron to zinc is 2:1, the molar ratio of cobalt to zinc is 0.15:1, and the molar ratio of magnesium to zinc is 0.01:1, stir to dissolve it, and add the mass fraction It is 25% ammonia solution, adjust the pH value of the solution to 9, after the dropwise addition, heat to 70°C and stir for 0.5h, cool to 20°C, filter with a Buchner funnel, wash the filter cake with deionized water until neutral, the obtained solid After drying at 140°C for 8 hours, place it in a muffle furnace and bake at 700°C for 6 hours, cool, grind, and sieve to obtain a 20-60 mesh cobalt and magnesium-modified zinc ferrite catalyst, which is sealed and stored.

[0044] Oxidative Dehydrogenation Process

[0045] Fill 2mL of the above catalyst into a stainless steel reactor w...

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Abstract

The invention discloses a catalyst and a method used for preparing 1,3-butadiene by oxidative dehydrogenation of n-butene. The catalyst is a cobalt and magnesium modified zinc ferrite catalyst which is obtained by proportioning a ferric salt, a zinc salt, a cobalt salt, a magnesium salt and a deionized water in a mole ratio, regulating pH value with ammonia water, concentrating, filtering, drying, roasting, cooling, grinding and screening. The method for preparing 1,3-butadiene by utilizing the catalyst comprises the following steps of: with C4 fraction produced by MTO (methanol to olefin) as a raw material, carrying out catalytic oxidative dehydrogenation reaction on a reaction mixture which is formed by the C4 fraction, air and vapour under the action of the cobalt and magnesium modified zinc ferrite catalyst so as to efficiently prepare1,3-butadiene, wherein the main ingredient of the C4 fraction is n-butene. The method disclosed by the invention has the advantage that the C4 fraction is not required to be refined to remove impurities such as oxygenated chemicals, thus the method disclosed by the invention is a simple and efficient method for preparing a high-additional-value product by utilizing C4 resource of the MTO.

Description

technical field [0001] The invention relates to a catalyst for 1,3-butadiene, and a method for preparing 1,3-butadiene using the catalyst, in particular to a zinc ferrite catalyst modified with cobalt and magnesium elements, and the catalyst The method is applied to the method for preparing 1,3-butadiene by oxidative dehydrogenation of C4 fraction produced from coal-to-olefins. Background technique [0002] 1,3-butadiene is an important monomer for synthetic rubber and resin, and its position in petrochemical olefin raw materials is second only to ethylene and propylene. In the 1960s and 1970s, the Petro-Tex Corporation of the United States first successfully developed the process of preparing 1,3-butadiene by oxidative dehydrogenation of n-butene, and realized industrialization. After that, my country also carried out research and development, and realized the industrial production of butadiene by oxidative dehydrogenation of n-butene. This method requires that the conten...

Claims

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Application Information

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IPC IPC(8): B01J23/80C07C11/167C07C5/48
Inventor 杨永忠唐应吉闵小建张生军张志刚
Owner SHAANXI COAL & CHEM TECH INST
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