Catalyst for preparing methylacrolein in fixed bed, preparation method and application

A technology of methacrolein and methylenebisacrylamide, which is applied in catalyst activation/preparation, chemical instruments and methods, preparation of organic compounds, etc., can solve problems such as poor repeatability, poor sintering activity, and poor uniformity. , to achieve the effect of small particle size, reduced powder agglomeration, and easy control of uniformity.

Pending Publication Date: 2022-05-03

CHINA PETROLEUM & CHEM CORP +1

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AI-Extracted Technical Summary

Problems solved by technology

The existing catalysts including the previous comparison are all prepared by coprecipitation method, the powder agglomeration phenomenon is more serious, the uniformity is poor, ...

Abstract

The invention discloses a catalyst for preparing methylacrolein in a fixed bed, a preparation method and application. The composition of the catalyst is Mo Bi Fe < c > Co < d > Cu < e > Mg < f > C < sg > O < x >, a is equal to 12, 0lt; blt; 3.5, 0 lt; clt; ct; 3, 0lt; dlt; 8, 0lt; lt, lt; 3, 0lt; flt; 3, 0lt; glt; 2; and x is the number of oxygen atoms required for forming the composite oxide. In the preparation process of the catalyst, salts or oxides containing Mo, Bi, Fe, Co, Cu, Mg and Cs are added to form a dispersion system, and meanwhile, a complexing agent, a polymer monomer and a cross-linking agent are added into the dispersion system step by step or directly, so that the purposes of controlling the morphology, granularity and uniformity of the catalyst and further improving the activity and selectivity of the catalyst are achieved.

Application Domain

Organic compound preparationHeterogenous catalyst chemical elements +3

Technology Topic

ChemistryComposite oxide +5

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Examples

Experimental program(8)
Comparison scheme(8)

Example Embodiment

[0077] Example 1

[0078] At 50 °C, 12.6 g bismuth pentahydrate, 16.9 g iron hexahydrate, 12.2 g cobalt nitrate hexahydrate, 12.4 g copper hexahydrate, 5.38 g magnesium hexahydrate, 2.72 g cesium nitrate dissolved in 100 mL 5% nitric acid solution, after the solution is clarified and transparent, add 25 g tartaric acid, after the tartaric acid is completely dissolved, add 10 g glucose, the concentration of sugar in the system after addition is 0.1 g / mL, Then a 350mL solution containing 278g of acrylamide and 62g of methylenebis acrylamide was added. Each of the above steps is accompanied by agitation to allow the additives to dissolve sufficiently. To mix the solution evenly, after clarification, add 150mL of the solution containing 50g of ammonium heptamolybdate tetrahydrate. Finally, the resulting mixed solution was heated to 80 °C to produce a polymerization reaction. Wait for the solution to slowly transform into gels. Place the obtained gel in a thermostatic drying chamber to dry to form a dry gel. The dry gel was ground into a fine powder and calcined at 500 °C for 6 hours to obtain a catalyst sample Mo 12 Bi 1.1 Fe 1.8 Co 1.8 Cu 1.8 Mg 0.9 Cs 0.6 O x 。

[0079] After the catalyst is pressed into a fixed bed reactor, it is loaded into a fixed bed reactor at 350 ° C according to isobutene / tert-butanol: oxygen: nitrogen: water = 1: 2: 9: 4 feeding, air velocity 1200h-1 , analyzed with online chromatography. The results are shown in Table 1.

Example Embodiment

[0080] Example 2

[0081] At 50 °C, 12.6 g bismuth nitrate, 16.9 g iron nitrate, 12.2 g cobalt nitrate, 6.2 g copper nitrate, 5.38 g magnesium nitrate, 2.72 g cesium nitrate were dissolved in 100 mL of 5% nitric acid solution, after the solution was clear and transparent, 25 g tartaric acid was added. After tartaric acid is completely dissolved, 10g of glucose is added, the concentration of sugar in the system is 0.1g/mL, and then 350mL of solution containing 278g of acrylamide and 62g of methylenebisacrylamide is added. Each of the above steps is accompanied by agitation to allow the additives to dissolve sufficiently. After the solution is mixed evenly, 150mL of solution containing 50g of ammonium heptamolybdate is added after clarification. Finally, the resulting mixed solution was heated to 80 °C to produce a polymerization reaction. Wait for the solution to slowly transform into gels. Place the obtained gel in a thermostatic drying chamber to dry to form a dry gel. The dry gel was ground into a fine powder and calcined at 500 °C for 6 hours to obtain a catalyst sample Mo 12 Bi 1.1 Fe 1.8 Co 1.8 Cu 0.9 Mg 0.9 Cs 0.6 O x 。

[0082] After the catalyst was pressed and molded into a fixed bed reactor, at 360 ° C according to isobutene / tert-butanol: oxygen: nitrogen: water = 1: 2: 9: 4 feeding, air velocity 1000h -1 , analyzed with online chromatography. The results are shown in Table 1.

Example Embodiment

[0083] Example 3

[0084] At 50 °C, 12.6 g of bismuth nitrate, 16.9 g of iron nitrate, 12.2 g of cobalt nitrate, 12.4 g of copper nitrate, 10.75 g of magnesium nitrate, 2.72 g of cesium nitrate were dissolved in 100 mL of 5% nitric acid solution, and after the solution was clarified and transparent, 25 g of tartaric acid was added. After tartaric acid was completely dissolved, 10g of glucose was added, the concentration of sugar in the system was 0.1g/mL, and then a 350mL solution containing 278g of acrylamide and 124g of methylenebisacrylamide was added. Each of the above steps is accompanied by agitation to allow the additives to dissolve sufficiently. After the solution is mixed evenly, 150mL of solution containing 50g of ammonium heptamolybdate is added after clarification. Finally, the resulting mixed solution was heated to 80 °C to produce a polymerization reaction. Wait for the solution to slowly transform into gels. Place the obtained gel in a thermostatic drying chamber to dry to form a dry gel. The dry gel was ground into a fine powder and calcined at 500 °C for 6 hours to obtain a catalyst sample Mo12 Bi 1.1 Fe 1.8 Co 1.8 Cu 1.8 Mg 1.8 Cs 0.6 O x 。

[0085] After the catalyst is pressed into a fixed bed reactor, it is loaded into a fixed bed reactor at 350 ° C according to isobutene / tert-butanol: oxygen: nitrogen: water = 1: 2: 9: 4 feeding, air velocity 1200h -1 , analyzed with online chromatography. The results are shown in Table 1.

PUM

Property	Measurement	Unit
Concentration	0.1	g/ml

Description & Claims & Application Information

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Classification and recommendation of technical efficacy words

reduce clumping

Catalyst for preparing methylacrolein in fixed bed, preparation method and application

AI-Extracted Technical Summary

Problems solved by technology

Abstract

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Examples

Example Embodiment

Example Embodiment

Example Embodiment

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Description & Claims & Application Information

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