Preparation method of catalyst for partial oxidization of isobutene to prepare methylacrolein

A methacrolein and catalyst technology, which is applied in the preparation of organic compounds, metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, etc., can solve problems such as waste catalyst pollution, and achieve a reasonable process structure. , the method is simple, the effect of low energy consumption

Active Publication Date: 2014-05-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method not only utilizes Mo, Co, and Ni in the spent hydrotreating catalyst, but also makes full use of the Fe, Ni, and V deposited on the spent h

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Preparation of the catalyst, the steps are as follows:

[0035] Selection of waste hydrodesulfurization HDS MoCo / Al in fixed bed residual oil hydrogenation industrial unit 2 o 3 Catalyst, after extracting to remove the oil on the surface of the catalyst, drying and roasting to obtain the treated waste HDS catalyst (containing Mo: 12.7 wt%, Co: 2.2 wt%, V: 2.4 wt%, Ni: 1.7 wt%, Fe : 0.15 wt%, Al 2 o 3 : 71.6 wt%), grind the catalyst to 200 mesh (referring to passing through a 200 mesh sieve), weigh 100 g of powder, add 250 mL of 98 wt% concentrated sulfuric acid, stir at 50 °C until the solid is almost completely dissolved, filter Collect the filtrate, add 10.7 g bismuth nitrate, 19.5 g cobalt nitrate, 1.5 g ammonium metavanadate, 4.1 g nickel nitrate, 4.2 g ferric nitrate to the filtrate, stir and dissolve, add ammonia water to adjust the pH value to 8.0, and stir for 15 min , adding 40 wt% sodium hydroxide solution to adjust the pH value of the solution to 12.0...

Embodiment 2

[0039] Grind the catalyst used in Example 1 to 200 mesh (referring to passing through a 200 mesh sieve), weigh 100 grams of powder, add 300 mL of a mixed solution of 98 wt% concentrated sulfuric acid and 65 wt% nitric acid, and the volume ratio is 2:1 , stirred at a constant temperature at 50°C until the solids were almost completely dissolved, and the filtrate was collected by filtration, 10.7 g of bismuth nitrate, 20.7 g of cobalt nitrate, 1.3 g of ammonium metavanadate, 4.1 g of nickel nitrate, and 4.6 g of iron nitrate were added to the filtrate, and stirred After dissolving, add ammonia water to adjust the pH value to 9.0. After stirring for 15 min, add 40 wt% sodium hydroxide solution to adjust the pH value of the solution to 13.0. After aging for 4 h, filter the precipitate and wash it three times with deionized water. , the filter cake was dried at 110 °C for 8 h, calcined at 600 °C for 4 h, and pressed into pellets to obtain the final catalyst Mo 9 Bi 1.5 co 7.5 V ...

Embodiment 3

[0042] Waste Hydrodesulfurization HDS MoCoNi / Al in Fixed Bed Residue Hydrogenation Industrial Unit 2 o 3 Catalyst (containing Mo: 15.6 wt%, Co: 1.6 wt%, V: 1.7 wt%, Ni: 2.3 wt%, Fe: 0.21 wt%, Al 2 o 3 : 68.5 wt%), the catalyst was ground to 200 mesh (referring to passing through a 200 mesh sieve), weighed 100 grams of powder, added 350 mL of a mixed solution of 98 wt% concentrated sulfuric acid and 65 wt% concentrated nitric acid, and the volume ratio was 1:1 , stirred at a constant temperature at 50°C until the solids were almost completely dissolved, collected the filtrate by filtration, added 8.7 g of bismuth nitrate, 18 g of cobalt nitrate, 0.35 g of ammonium metavanadate, and 2.1 g of ferric nitrate to the filtrate, stirred and dissolved, then added ammonia water Adjust the pH value to 10.0. After stirring for 15 min, add 40 wt% sodium hydroxide solution to adjust the pH value of the solution to 14.0. After aging for 4 h, filter the precipitate and wash it three times w...

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PUM

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Abstract

The invention discloses a preparation method of a catalyst for partial oxidation of isobutene to prepare methylacrolein. The preparation method comprises the following steps: grinding waste hydro-treatment catalysts into powder, dissolving the powder in a strong inorganic acid, filtering, then adding a precursor of Bi, adding an alkaline solution to adjust the pH value to a range of 7.0 to 10.0, then adding a strong alkaline solution to adjust the pH value to a range of 12.0 to 14.0, heating and stirring at the same time, filtering so as to obtain the precipitant, washing, drying, and burning the precipitant, and finally forming so as to obtain the catalyst. The preparation method recycles the active metals in waste hydro-treatment catalysts, and at the same time fully utilizes the Fe, Ni and V which are deposited on the waste catalysts to prepare the catalyst, which has the advantages of large specific surface area and high activity and is used to catalyze partial oxidation of isobutene to prepare methylacrolein; wherein the byproduct of the preparation method is meta-aluminate. The preparation method has the advantages of simpleness and easy operation, and is capable of fully utilizing the carriers and metals in waste hydro-treatment catalysts.

Description

technical field [0001] The invention relates to a method for preparing a catalyst for preparing methacrolein by partial oxidation of isobutene from a waste catalyst, in particular a method for preparing a catalyst for preparing a catalyst for preparing methacrolein by partial oxidation of isobutene from a waste hydrogenation treatment catalyst. Background technique [0002] Every year, a large amount of spent catalysts that cannot be regenerated are produced all over the world, and hydrogenation catalysts account for a considerable proportion. Enterprises generally discard these spent catalysts or use them as fillers in construction and other industries, but there is a big problem: hydrogenation catalysts generally contain molybdenum, tungsten, cobalt, nickel, etc. Valuable metal oxides, such treatment will cause waste of resources; and the loss of metals will cause certain pollution to the environment, especially the pollution of water resources is more serious. Recently, ...

Claims

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Application Information

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IPC IPC(8): B01J23/887C07C47/22C07C45/35
CPCY02P20/584
Inventor 金浩孙素华朱慧红刘杰杨光
Owner CHINA PETROLEUM & CHEM CORP
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