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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  • Abstract
  • Description
  • Claims
  • Application Information

AI 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 acidic resin, which has the disadvantage of poor thermal stability. Therefore, the current relevant alternative catalysts (such as metal oxides are Supported palladium catalyst) is still under investigation

Method used

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

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Experimental program
Comparison scheme
Effect test

Embodiment 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-neck flask, stir vigorously for 30min, then take 20mL of glacial acetic acid, 1mL of absolute ethanol, and 0.2mL of distilled water to mix evenly, and add to the above mixture solution, stirred vigorously for 1 h. At this time, a clear and transparent golden yellow solution was obtained, and the solution was evaporated to dryness at about 100°C to precipitate solid powder, and then calcined at 500°C for 3 hours to obtain TiO 2 powder.

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

[0022] With 5g1) the prepared TiO 2 Powder impregnated in 7.5mL of 0.01mol / L H 2 PdCl 4 solution, ultrasonication for 0.5h, drying at 110°C, roasting at 350°C for 3h, reduction with potassium borohydride for 0.5h, washing, suction filtration, and finally vacuum drying at 50°C in a vacuum oven to obtain Pd / TiO 2 (Pd loading 0....

Embodiment 2

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

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

[0026] 2) Pd / V 2 o 5 Application of Catalyst in Hydrogenation of Acetone to Prepare Methyl Isobutyl Ketone and Methyl Isobutyl Alcohol

[0027] Acetone at 5°C is carried by hydrogen with a flow rate of 15mL / min, and the Pd / V prepared in Example 2 is added 2 o 5 The catalyst was reacted in a quartz reaction tube with an inner diameter of 8 mm. The reaction temperature was 200°C. Absorb all reaction products with absolute ethanol at 5°C. After 2 hours of collection, the composition of the product was analyzed using a Shimadzu GC-2010 gas chromatograph. Table 1 shows the ...

Embodiment 3

[0032] Pd / TiO 2 Application of Catalyst in Hydrogenation of Acetone to Prepare Methyl Isobutyl Ketone and Methyl Isobutyl Alcohol

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

[0034] Table 2 Pd loading vs. Pd / TiO 2 Catalytic Acetone One-step Synthesis of MIBK and Effect of MIBC Properties

[0035]

[0036] As can be seen from Table 2, Pd / TiO 2 The catalyst can convert acetone and hydrogen into methyl isobutyl ketone and...

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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.

Description

technical field [0001] The invention relates to a preparation method for synthesizing methyl isobutyl ketone and methyl isobutyl alcohol. Background technique [0002] Acetone is a by-product of the phenol production industry as well as the propylene oxide production industry and is currently in surplus worldwide. At the same time, acetone is also an important platform compound for the production of chemical raw materials from biomass. How to convert acetone into chemical products with high added value has important economic value. [0003] At present, acetone and hydrogen are mainly mixed at home and abroad, and the polycondensation, dehydration and hydrogenation processes are completed under the action of a multifunctional catalyst to prepare methyl isobutyl ketone (abbreviated as MIBK), which is the so-called one-pot process in the literature. Methyl isobutyl ketone is an excellent medium-boiling organic solvent with stable chemical properties and is widely used in the ...

Claims

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Application Information

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IPC IPC(8): C07C27/00C07C45/73C07C49/04C07C29/145C07C31/125B01J23/44B01J23/648B01J23/652B01J23/656
CPCB01J23/44B01J23/648B01J23/652B01J23/656C07C29/145C07C45/73C07C49/04C07C31/125
Inventor 周永华杨乐群钟宏叶红齐王晖
Owner CENT SOUTH UNIV
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