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Method for synthesizing methyl isopropyl ketone by one-step method

A technology of methyl isopropyl ketone and step method, which is applied in the field of chemical synthesis, can solve the problems of low yield of methyl isopropyl ketone, many wastes, complex procedures, etc., achieve simple and easy control of the process, and reduce the amount of waste water and waste gas , the effect of increasing the reaction yield

Active Publication Date: 2021-01-12
山东智永化工产业技术研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] CN102861577A reacts methyl ethyl ketone (butanone) with methanol and water to synthesize methyl isopropyl ketone; however, the reaction temperature is high, reaching 320-440°C, and the yield of methyl isopropyl ketone is low. The highest yield recorded is only 18.36% (Example 12)
[0005] The method has cumbersome steps and complex procedures, three reactions and multiple separations, many wastes, difficult odor control, low yield, multiple rectification separations, high energy consumption and high cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Embodiment 1 one-step method synthetic method for methyl isopropyl ketone

[0025] Include the following steps:

[0026] (1) Feeding

[0027] Put 380 grams of methyl ethyl ketone and 1.2 grams of palladium carbon (3% palladium content) into the autoclave. At the same time, add 9.8 grams of condensation catalyst and 385 grams of formaldehyde (37%). After the feeding is completed, nitrogen and hydrogen replace the system three times respectively.

[0028] The condensation catalyst is a macroporous strongly basic anion exchange resin.

[0029] (2) The first stage insulation reaction

[0030] After the replacement, keep the hydrogen pressure at 1.2 MPa, start stirring, adjust the rotation speed to 450 rpm, and raise the temperature to 45°C, and keep it at 45°C for 40 minutes.

[0031] (3) The second stage insulation reaction

[0032] After the 45°C heat preservation is completed, the reaction pressure is maintained, and the temperature is raised to 120°C for the heat pr...

Embodiment 2

[0035] Embodiment 2 one-step method synthesizes the method for methyl isopropyl ketone

[0036] Include the following steps:

[0037] (1) Feeding

[0038] Put 380 grams of butanone and 1.5 grams of platinum carbon (platinum content is 3%) into the autoclave, add 9.8 grams of condensation catalyst and 300 grams of formaldehyde solution (37%) at the same time, and replace the system with nitrogen and hydrogen respectively three times after feeding is completed.

[0039] The condensation catalyst is a macroporous strongly basic anion exchange resin.

[0040] (2) The first stage insulation reaction

[0041] After the replacement is completed, keep the hydrogen pressure at 0.7MPa, start stirring, adjust the rotation speed to 300 rpm, and raise the temperature to 65°C, and keep it warm for 120 minutes.

[0042] (3) The second stage insulation reaction

[0043] After the heat preservation at 65°C, the reaction pressure was maintained, and the temperature was raised to 100°C for t...

Embodiment 3

[0046] Embodiment 3 one-step method synthesizes the method for methyl isopropyl ketone

[0047] Include the following steps:

[0048] (1) Feeding

[0049] Put 380 grams of methyl ethyl ketone and 1.0 grams of Raney nickel into the autoclave, and at the same time add 9.8 grams of condensation catalyst and 300 grams of formaldehyde solution (37%), and replace the system with nitrogen and hydrogen respectively three times after feeding is completed.

[0050] The condensation catalyst is a macroporous strongly acidic cation exchange resin.

[0051] (2) The first stage insulation reaction

[0052] After the replacement, keep the hydrogen pressure at 2.0MPa, start the stirring, adjust the rotation speed to 700 rpm, raise the temperature to 80°C, and keep this temperature for 90 minutes.

[0053] (3) The second stage insulation reaction

[0054] After the heat preservation at 80°C, the reaction pressure was maintained, and the temperature was raised to 130°C for the heat preserva...

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Abstract

The invention provides a method for synthesizing methyl isopropyl ketone through a one-step method. The method comprises the steps of feeding, a first-stage heat preservation reaction process and a second-stage heat preservation reaction process. According to the synthesis method, the reaction yield and the production efficiency are improved, the yield is 70-80% (metered by formaldehyde), operations such as material turnover and separation are reduced, the amount of waste water and waste gas is obviously reduced, and the method is safe and easy to control. Compared with the traditional synthesis method, the method significantly reduces the use amount of equipment and the like, greatly shortens the reaction time and has simple and easily-controlled processes. Various expenses of material consumption, equipment investment, three-waste treatment, personnel and the like are reduced, and the cost advantage is obviously improved. According to the synthesis method disclosed by the invention,the yield of the methyl isopropyl ketone can be 80-85% (metered by formaldehyde) and the purity of the methyl isopropyl ketone is 99.5% or above by virtue of a preferable technical scheme.

Description

technical field [0001] The invention relates to a method for synthesizing methyl isopropyl ketone in one step, and belongs to the technical field of chemical synthesis. Background technique [0002] The methods for synthesizing methyl isopropyl ketone in the prior art include butanone methanol method, butanone formaldehyde method and the like. [0003] CN102861577A reacts methyl ethyl ketone (butanone) with methanol and water to synthesize methyl isopropyl ketone; however, the reaction temperature is high, reaching 320-440°C, and the yield of methyl isopropyl ketone is low. The highest yield recorded was only 18.36% (Example 12). [0004] The existing butanone-formaldehyde synthesis of methyl isopropyl ketone is generally carried out according to a three-step method. In the first step, formaldehyde is added dropwise to butanone under alkaline catalysis, and condensation reaction is carried out to obtain alcohol ketone, which is separated by rectification. Excess butanone; ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/75C07C49/04
CPCC07C45/75C07C49/04
Inventor 侯永生吴国军朱素娟马华青邹敏侯龙张建波张立滨柳伟杰
Owner 山东智永化工产业技术研究院有限公司
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