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A kind of catalyst and application of acetone hydrogenation liquid-phase method to synthesize methyl isobutyl ketone

A kind of methyl isobutyl ketone, catalyst technology, applied in physical/chemical process catalyst, organic compound preparation, organic chemistry and other directions, can solve the problem that the activity and selectivity cannot meet the requirements of industrialization, etc.

Active Publication Date: 2020-01-07
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Because the activity and selectivity of this kind of catalyst are not up to the requirements of industrialization, there are no reports of practical application.

Method used

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  • A kind of catalyst and application of acetone hydrogenation liquid-phase method to synthesize methyl isobutyl ketone
  • A kind of catalyst and application of acetone hydrogenation liquid-phase method to synthesize methyl isobutyl ketone
  • A kind of catalyst and application of acetone hydrogenation liquid-phase method to synthesize methyl isobutyl ketone

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The surface of the fluorine-modified magnesium oxide support supports titanium dioxide and supported palladium, and the two are physically mixed to obtain a catalyst, which is denoted as TiO 2 / MgO-F&Pd / Cor.

[0036] Step (1): Fluorine-modified magnesium oxide (referred to as MgO-F)

[0037] Weigh 1.85g NH 4 F Add 100ml of distilled water to a polytetrafluoroethylene beaker, stir to make it dissolve in water, and prepare 0.5mol / L NH 4 F solution.

[0038] Weigh 6g of MgO powder in a Teflon beaker, add 100ml of NH 4 F solution (0.5 mol / L or 1 mol / L) was stirred at room temperature for 2 h, then filtered and washed with distilled water until the filtrate was neutral. The resulting filter cake was dried in an oven at 100 °C for 6 h. The dried filter cake was calcined in a muffle furnace at 450°C for 4h to obtain MgO-F.

[0039] Step (2):

[0040] Step (2-a): the surface of fluorine-modified magnesium oxide supports titanium dioxide (denoted as TiO 2 / MgO-F)

[004...

Embodiment 2

[0056] Application of Multifunctional Catalyst in Hydrogenation of Acetone to Prepare MIBK

[0057] 5.5ml of acetone was added to the inner lining of the autoclave, a mixed catalyst of supported titanium dioxide and supported palladium and a magnetic stirrer were added, the inner lining was put into the autoclave and the autoclave was tightly sealed. The high-pressure reactor is placed on the ZNCL-TS intelligent digital display magnetic electric heating jacket, the stirring switch is turned on, and the rotation speed is 600r / min. First, 0.2MPa nitrogen gas is introduced into the high-pressure reactor, and the gas in the reactor is discharged for 3 minutes. N 2 Row twice, pass through hydrogen 0.2MPa for the third time, and discharge the gas after 3 minutes. Close the exhaust valve, and then re-introduce hydrogen at 0.75MPa, close the intake valve and wait for the pressure gauge of the high-pressure reactor to stabilize at 0.75MPa for 5 minutes, then set the temperature of the...

Embodiment 3

[0067] The fluorine-modified magnesia support first supported titanium dioxide and then palladium (denoted as Pd / TiO 2 / MgO-F)

[0068] Step (1): Fluorine-modified magnesium oxide carrier supports titanium dioxide

[0069] First, pour 10ml of tetrabutyl titanate and 35ml of absolute ethanol into a flat-bottomed flask, and stir vigorously on a magnetic stirrer for 30min. Then weigh 5g of MgO-F and add it into a flat-bottomed flask, and continue to stir for 1h. Then pour the obtained liquid into a beaker, let it stand for precipitation, suck up the supernatant with a dropper, and leave a white precipitate, dry the white precipitate, put it into a crucible, and dry it in a muffle furnace at 500°C After burning for 3 hours, a sample was obtained, which was denoted as TiO 2 / MgO-F, grind, sieve, take 200-400 mesh for later use.

[0070] Step (2): TiO 2 / MgO-F supported palladium

[0071] The TiO that 5g step (1) obtains 2 / MgO-F impregnated in 7.5mL of 0.01mol / L H 2 PdCl 4...

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Abstract

The invention discloses a catalyst for liquid phase synthesis of methyl isobutyl ketone (MIBK) through acetone hydrogenation and applications thereof. The catalyst comprises three effective components namely fluorine modified magnesium oxide, titanium dioxide, and palladium and other auxiliary components. The catalyst is applied to high pressure liquid phase reactions of acetone hydrogenation to prepare methyl isobutyl ketone; the acetone conversion rate can reach 70.7%, MIBK selectivity can reach 78.6%, and corresponding MIBK yield can reach 55.6%. In a kettle type reactor, the MIBK yield is 45.6 mol MIBK / g Pd for one unit mass of palladium (primary reactions). Compared with similar catalysts, the catalyst has the characteristics of high MIBK yield, little using amount of palladium, and simple preparation technology.

Description

technical field [0001] The invention relates to a catalyst for synthesizing methyl isobutyl ketone by a high-pressure liquid phase method using acetone and hydrogen as raw materials, and the application of the catalyst. 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 polycondensation (base catalysis), dehydration (acid catalysis) and hydrogenation (metal catalysis) are completed under the action of a multifunctional catalyst to prepare methyl isobutyl ketone (MIBK for short). It is the so-called one-pot process in the literature. MIBK is an exce...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/138C07C45/74C07C49/04
CPCB01J27/138C07C45/74C07C49/04
Inventor 周永华段辉林百宁韦健人赵君叶红齐韩凯
Owner CENT SOUTH UNIV