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Preparation method of catalyst used in reaction of preparing methylacrolein by selective oxidation of isobutene/tertiary butanol

A technology of methacrolein and selective oxidation, which is applied in the preparation of oxygenated compounds by hydrocarbon oxidation, the preparation of organic compounds, the preparation of carbon-based compounds, etc. The problem of high reaction hot spot temperature of the catalyst can achieve the effect of prolonging the service life, reducing the reaction hot spot temperature and good selectivity.

Inactive Publication Date: 2011-06-15
SHANGHAI HUAYI ACRYLIC-ACID CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] In order to overcome the high temperature of catalyst reaction hot spots in the above patents and the inability to have both high conversion rate, high selectivity and high stability of the catalyst, the present invention

Method used

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  • Preparation method of catalyst used in reaction of preparing methylacrolein by selective oxidation of isobutene/tertiary butanol
  • Preparation method of catalyst used in reaction of preparing methylacrolein by selective oxidation of isobutene/tertiary butanol
  • Preparation method of catalyst used in reaction of preparing methylacrolein by selective oxidation of isobutene/tertiary butanol

Examples

Experimental program
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Effect test

Embodiment 1

[0020] Dissolve 1000 grams of ammonium paramolybdate tetrahydrate in 1 liter of distilled water, then add 494.5 grams of cobalt nitrate hexahydrate, 346.8 grams of ferric nitrate nonahydrate, 329.7 grams of bismuth nitrate pentahydrate, and 11.4 grams of potassium nitrate, and stir to dissolve into a mixed aqueous solution , then add 336.5 grams of silicon micropowder with a particle size of 1000-1500 nm to the above solution, continue to stir and mix at 60°C for 50 minutes, then transfer the above mixed slurry to an oven for 12 hours at 120°C, and take 300 grams of dry slurry Tablets are formed into hollow columnar particles with an outer diameter of 5mm, an inner diameter of 2mm, and a length of 5mm. The obtained catalyst particles are calcined at 550°C in air for 7 hours to obtain a composition of Mo 10 Bi 1.2 Fe 1.5 co 3 K 0.2 Si 10 catalyst.

[0021] Get 50 grams of catalyzer and pack in the fixed-bed tubular reactor, pass into the raw material isobutylene after preh...

Embodiment 2

[0023] The catalyst preparation method is the same as in Example 1, except that 336.5 grams of silicon micropowder with a particle diameter of 1000 to 1500 nm is changed to 3365 grams of white carbon black with a particle diameter of 30 to 50 nm in the catalyst preparation process, and the roasting temperature is changed from 550 ° C to 630 ° C. ℃, the catalyst composition is Mo 10 Bi 1.2 Fe 1.5 co 3 K 0.2 Si 100 . Catalyst activity evaluation conditions are also the same as in Example 1, and the results are shown in Table 1.

Embodiment 3

[0025] 577.0 grams of cobalt nitrate hexahydrate, 462.3 grams of ferric nitrate nonahydrate, 549.5 grams of bismuth nitrate pentahydrate, and 2018.7 grams of white carbon black with a particle size of 100 to 200 nm were prepared as a mixed slurry, which was recorded as A; 1000 grams of paramolybdic acid tetrahydrate Dissolve ammonium and 17.1 grams of potassium nitrate in 1 liter of distilled water, and record it as B; add B to A under stirring, and continue to stir at 75°C for 2 hours, then transfer the above mixed slurry to an oven for 10°C and dry at 120°C hour, take 500 grams of dry slurry and mold it into hollow columnar particles with an outer diameter of 5 mm, an inner diameter of 2 mm, and a length of 5 mm; 10 Bi 2 Fe 2 co 3.5 K 0.3 Si 60 catalyst. Catalyst evaluation conditions are the same as in Example 1, and the results after 100 hours of reaction are listed in Table 1.

[0026] Oxidation reaction result in table 1 embodiment 1~3

[0027]

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Abstract

The invention provides a preparation method of a catalyst used in reaction of preparing methylacrolein by selective oxidation of isobutene / tertiary butanol, wherein the catalyst is a composite oxide containing Mo, Bi, Fe, Co, K and Si. The preparation method comprises the steps of: stirring and mixing one or two of precursor compound silicon micro powder of Si and white carbon black with precursor compounds of other active components except for the Si to obtain mixed slurry, and then drying, forming and roasting the mixed slurry to obtain the catalyst. The catalyst has high activity and lower required reaction temperature when used in the reaction of preparing unsaturated aldehyde through selective oxidation of isobutene / tertiary butanol; better methylacrolein can be obtained, and the selectivity is high; and the reaction hot point is lower and the stability of the catalyst is good.

Description

technical field [0001] The invention relates to a catalyst with high activity and high selectivity suitable for selective oxidation of isobutene / tert-butanol to prepare methacrolein and a preparation method of the catalyst. Background technique [0002] Methacrylic acid is an important organic chemical product. At present, isobutene or tert-butanol is often used as raw material, and methacrolein is first selectively oxidized, and then methacrylic acid is further oxidized. [0003] For the selective oxidation of isobutene / tert-butanol to prepare methacrolein, a composite oxide catalyst containing Mo, Bi, Fe, and Co as the main active components is often used at present, and some trace elements are further added to the above components as additives , to further enhance the activity and selectivity of the catalyst. [0004] The selective oxidation of isobutene / tert-butanol to methacrolein is a strong exothermic reaction, and the heat generated is accumulated in the catalyst be...

Claims

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Application Information

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IPC IPC(8): B01J23/887C07C27/14C07C47/22C07C45/35C07C45/37C07C57/05C07C51/25C07C51/23
Inventor 罗鸽温新赵小岐庄岩马建学褚小东邵敬铭
Owner SHANGHAI HUAYI ACRYLIC-ACID CO LTD
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