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Method for synthesizing methyl isobutyl ketone from acetone through one-step method

A technology of methyl isobutyl ketone and acetone, applied in chemical instruments and methods, preparation of organic compounds, preparation of carbon-based compounds, etc., can solve the problem of low acetone conversion rate and MIBK selectivity, high reaction temperature and low conversion rate And other issues

Active Publication Date: 2012-07-11
PETROCHINA CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Japanese Patent No. 63-19436 uses alumina as a catalyst carrier to synthesize methyl isobutyl ketone, but there are problems such as high reaction temperature, low conversion rate, and poor selectivity of product methyl isobutyl ketone.
Patent CN1069674A uses Pd / molecular sieve catalyst in the synthesis of MIBK from acetone. The disadvantage of this catalyst is that the production process route is long and the method is cumbersome, resulting in high production cost of MIBK
[0005] Patent CN1255404A uses modified γ-Al 2 o 3 and calcium carbonate as a composite carrier to support metal palladium. The catalyst produced has the advantages of no resin, wide temperature range, good stability, strong resistance to palladium loss, and long service life, but the conversion rate of acetone and the selectivity of MIBK are low. The problem

Method used

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  • Method for synthesizing methyl isobutyl ketone from acetone through one-step method

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Effect test

Embodiment 1

[0017] Take a certain amount of γ-Al 2 o 3 Baking at 500°C for 4 hours. Take 100g of roasted γ-Al 2 o 3 , immerse in 100ml of 0.0005g / mL lanthanum nitrate solution, let stand at a constant temperature of 30°C for 12 hours, dry at a constant temperature of 120°C for 12 hours, and bake at a constant temperature of 400°C for 4 hours. After cooling to room temperature, impregnate an equal volume of palladium chloride solution at 30°C for 2.0 hours, filter, dry at 120°C for 6 hours, bake at 400°C for 4 hours, and impregnate 0.05% Pd. The catalyst is designated as PL-1.

[0018] The catalytic reaction is carried out in a trickle bed reactor, the catalyst is filled with 80ml, the pressure is 3.0MPa, the temperature is 130°C, and the liquid space velocity is 1.0h -1 , the ratio of hydrogen to ketone is 2, acetone and hydrogen pass through the catalyst bed from top to bottom, the product is collected after being cooled by a cold trap, and the product is analyzed by capillary gas c...

Embodiment 2

[0020] Get the Al after roasting among the embodiment 1 2 o 3 100g, soak in 100ml 0.0008g / mL lanthanum nitrate solution, let stand at 30°C for 12 hours, dry at 120°C for 12 hours, and bake at 450°C for 4 hours. After cooling to room temperature, an equal volume of PdCl was impregnated 2 , immersion temperature 40°C, immersion time 2.0 hours, filter, 120°C constant temperature drying for 6 hours, 400°C calcination, constant temperature 4hr, Pd impregnation amount 0.05%. The catalyst is designated as PL-2. The reaction results are shown in Table 1

Embodiment 3

[0022] Get the Al after roasting among the embodiment 1 2 o 3 100g, immerse in 100ml 0.001g / Ml lanthanum nitrate solution, let stand at 40°C for 12 hours, dry at 120°C for 6 hours, and bake at 450°C for 4 hours. After cooling to room temperature, an equal volume of PdCl was impregnated 2 , immersion temperature 40°C, immersion time 3.0 hours, filter, 120°C constant temperature drying for 6 hours, 400°C calcination, constant temperature 4 hours, Pd impregnation amount 0.08%. The catalyst is designated as PL-3. The reaction results are shown in Table 1

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Abstract

The invention relates to a method for synthesizing methyl isobutyl ketone from acetone through a one-step method. Acetone and hydrogen gas are taken as raw materials; a three-phase trickle bed reactor is adopted; the reaction conditions are that: the temperature is 120-160 DEG C, and the pressure is 2.5-4.0 MPa; the liquid air speed is 0.8-2.0 h<-1>; in a catalyst, gamma-Al2O3 is taken as a carrier after being modified by using a lanthanum salt for carrying metal palladium; the mass percentage content of lanthanum is 0.5-3.0 percent; and the mass percentage content of Pd is 0.03-0.10 percent. The preparation method comprises the following specific steps of: soaking a lanthanum component in an isometric way for gamma-Al2O3 to obtain modified gamma-Al2O3; and soaking metal palladium in an isometric way to obtain a catalyst, wherein the content of palladium serving as a catalyst is very low; the content of mesityl oxide serving as a byproduct is less than or equal to 0.07 percent; stability is kept for a long time; the acetone transformation rate is more than or equal to 30.0 percent; and the selectivity of methyl isobutyl ketone is more than or equal to 93.0 percent.

Description

technical field [0001] The invention relates to a method for synthesizing methyl isobutyl ketone in one step with acetone and hydrogen. Background technique [0002] Methyl isobutyl ketone is an important organic solvent, which is used for dewaxing waxy oil in paints. It is also one of the raw materials for the production of rubber antioxidants and resin coatings. It can also be used as a solvent for the production of tetracycline and penicillin. In oil refining, As a petroleum dewaxing agent, it is widely used in the production of refined paraffin. [0003] At present, the main method of producing methyl isobutyl ketone is to use acetone and hydrogen as raw materials to synthesize methyl isobutyl ketone in one step. There are many types of catalysts used in this technology. According to reports, the one-step synthesis of methyl isobutyl ketone from acetone is widely used as a Pd / resin catalyst, such as patent US3,953,517. The advantage of this type of catalyst is that the ...

Claims

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Application Information

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IPC IPC(8): C07C49/04C07C45/73B01J23/63
Inventor 马中义田艳明周玮李正赵胤侯立波董立杰庞玉林
Owner PETROCHINA CO LTD
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