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A kind of preparation method of synthesizing methyl isobutyl ketone and methyl isobutyl alcohol

A technology for methyl isobutyl alcohol and methyl isobutyl ketone is applied in the field of synthesizing methyl isobutyl ketone and methyl isobutyl alcohol, and can solve the problems of poor thermal stability, short process and low energy consumption and other problems, to achieve the effect of promoting hydrogenation, high reaction efficiency and high yield

Active Publication Date: 2018-05-25
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • A kind of preparation method of synthesizing methyl isobutyl ketone and methyl isobutyl alcohol
  • A kind of preparation method of synthesizing methyl isobutyl ketone and methyl isobutyl alcohol
  • A kind of preparation method of synthesizing methyl isobutyl ketone and methyl isobutyl alcohol

Examples

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-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] Add 5g of the TiO obtained in 1) 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 / T...

Embodiment 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 selectivi...

Embodiment 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 isobu...

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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 method for preparing synthetic methyl isobutyl ketone and methyl isobutyl alcohol. Background technique [0002] Acetone is a by-product of the phenol production industry and the propylene oxide production industry, and it is currently in excess 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 to complete the polycondensation, dehydration and hydrogenation processes under the action of a multifunctional catalyst to prepare methyl isobutyl ketone (MIBK for short), which is called the one-pot process in the literature. Methyl isobutyl ketone is an excellent medium boiling point organic solvent with stable chemical properties and is widely used in the chemical industry. The o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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