Preparation method for synthesis of methyl isobutyl ketone and methyl isobutyl alcohol

A technology of methyl isobutyl alcohol and methyl isobutyl ketone, which is applied in the field of synthesis of methyl isobutyl ketone and methyl isobutyl alcohol, can solve the problem of short process, poor thermal stability and low energy consumption etc. to achieve the effect of high reaction efficiency, promotion of hydrogenation and high yield

Active Publication Date: 2016-07-06

CENT SOUTH UNIV

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AI-Extracted Technical Summary

Problems solved by technology

The one-pot method has gradually become the mainstream of synthesis due to the advantages of short process flow and low energy consumption. The catalyst used is a palladium catalyst supported by a strong a...

Abstract

The invention discloses a preparation method for synthesis of methyl isobutyl ketone and methyl isobutyl alcohol. The acetone and hydrogen are used as raw materials to synthesize methyl isobutyl ketone and methyl isobutyl alcohol at the reaction temperature of 150-250 DEG C; in the reaction process, Pd/MyOx is used as a catalyst at atmospheric pressure state, the mole ratio of the hydrogen to the acetone is 50:1 to 3: 1, and the volume velocity of the hydrogen is 800-10000h<-1>; the Pd/MyOx is that the amphoteric metal oxide MyOx with baking temperature not higher than 600 DEG C is used as a carrier to load the Pd, x and y in the MyOx are respectively 1, 2 or 3, and M is selected from polyvalent metal in IVB-VIIB family elements, and is in corresponding high valence in the MyOx. The method is applied to the atmospheric pressure gas phase reaction for synthesizing methyl isobutyl ketone and methyl isobutyl alcohol through acetone hydrogenation, the highest conversion rate of the acetone can achieve 62.6%, the highest selectivity of the methyl isobutyl ketone and methyl isobutyl alcohol can achieve 93.2%, and the methyl isobutyl alcohol accounts for 1/3. Compared with the similar catalyst, the catalyst disclosed by the invention is not only simple in preparation method and low in cost, but also obviously improves the selectivity of the methyl isobutyl ketone and methyl isobutyl alcohol.

Application Domain

Oxygen-containing compound preparationOrganic compound preparation +3

Technology Topic

Isobutyl alcoholMethylvinyl ketone +11

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Examples

Experimental program(3)

Example Embodiment

[0018] Example 1

[0019] 1) TiO 2 Powder preparation

[0020] At room temperature, mix 10mL of tetra-n-butyl titanate and 35mL of absolute ethanol in a closed flat-bottomed three-necked flask, stir vigorously for 30 minutes, then take 20mL of glacial acetic acid, 1mL of absolute ethanol, and 0.2mL of distilled water, mix well, and add to the above mixture In the solution, stir vigorously for 1h. At this time, a clear and transparent golden yellow solution was obtained. This solution was evaporated to dryness at about 100°C, and solid powder was precipitated, and then calcined at 500°C for 3h to obtain TiO 2 powder.

[0021] 2)Pd/TiO 2 (Pd loading 0.1wt%) preparation

[0022] 5g1) TiO 2 The powder is immersed in 7.5mL of 0.01mol/L H 2 PdCl 4 In the solution, ultrasonic for 0.5h, after drying at 110°C, roasting at 350°C for 3h, then reducing with potassium borohydride for 0.5h, washing, suction filtration, and finally vacuum drying at 50°C in a vacuum drying oven to obtain Pd/TiO 2 (Pd loading 0.1wt%).

Example Embodiment

[0023] Example 2

[0024] 1)Pd/V 2 O 5 (Pd loading 0.1wt%) preparation

[0025] Dip 5.0g of commercial vanadium pentoxide powder in 7.5mL of 0.01mol/L H 2 PdCl 4 In the solution, ultrasonic for 0.5h, after drying at 110°C, roasting at 350°C for 3h, then reducing with potassium borohydride for 0.5h, washing, suction filtration, and finally vacuum drying at 50°C in a vacuum drying oven to obtain Pd/V 2 O 5 (Pd loading 0.1wt%).

[0026] 2)Pd/V 2 O 5 The catalyst is applied to the hydrogenation of acetone to prepare methyl isobutyl ketone and methyl isobutyl alcohol

[0027] Using hydrogen with a flow rate of 15mL/min to carry acetone at 5°C, add the Pd/V prepared in Example 2 2 O 5 The catalyst reacts in a quartz reaction tube with an inner diameter of 8 mm. The reaction temperature is 200°C. Absorb all reaction products with absolute ethanol at 5°C. After collecting for 2 hours, Shimadzu GC-2010 gas chromatograph was used to analyze the product composition. The conversion of acetone and the selectivity of methyl isobutyl ketone and methyl isobutyl alcohol with different Pd loadings are shown in Table 1.

[0028] Table 1 Pd load vs. Pd/V 2 O 5 Effect of Catalytic Performance of Acetone One-Step Synthesis of MIBK and MIBC

[0029]

[0030] It can be seen from Table 1 that the loading of palladium has a greater impact on the performance of the catalyst. When the loading of palladium is 0.3%, Pd/V 2 O 5 The catalyzed acetone synthesis of MIBK and MIBC has a high conversion rate and selectivity of MIBK and MIBC, of which MIBC accounts for 31%.

Example Embodiment

[0031] Example 3

[0032] Pd/TiO 2 The catalyst is applied to the hydrogenation of acetone to prepare methyl isobutyl ketone and methyl isobutyl alcohol

[0033] Using hydrogen with a flow rate of 15 mL/min to carry acetone at 5°C, add the Pd/TiO prepared in Example 1 2 The catalyst reacts in a quartz reaction tube with an inner diameter of 8 mm. The reaction temperature is 200°C. Absorb all reaction products with absolute ethanol at 5°C. After collecting for 2 hours, Shimadzu GC-2010 gas chromatograph was used to analyze the product composition. Table 2 and Table 3 show the conversion rate of acetone and the selectivity of methyl isobutyl ketone and methyl isobutyl alcohol for different Pd loadings and different catalysts.

[0034] Table 2 Pd loading amount versus Pd/TiO 2 Effect of Catalytic Performance of Acetone One-Step Synthesis of MIBK and MIBC

[0035]

[0036] It can be seen from Table 2 that Pd/TiO 2 The catalyst can convert acetone and hydrogen into methyl isobutyl ketone and methyl isobutyl alcohol under normal pressure conditions, of which methyl isobutyl alcohol accounts for about 1/3. But there is no such report.

[0037] Table 3 The influence of the amount of catalyst on the performance of one-step synthesis of MIBK and MIBC with acetone

[0038]

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Description & Claims & Application Information

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Preparation method for synthesis of methyl isobutyl ketone and methyl isobutyl alcohol

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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