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Technological process for synthesizing methyl isobutyl ketone and diisobutyl ketone with acetone

A technology of methyl isobutyl ketone and diisobutyl ketone, which is applied in the field of one-step synthesis of methyl isobutyl ketone and diisobutyl ketone from acetone, can solve the problem of high reaction temperature, low conversion rate, methyl isobutyl ketone Eliminate the problems of poor ketone selectivity, etc., and achieve the effect of high activity and simple production process

Inactive Publication Date: 2005-09-14
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] According to reports, palladium / resin type catalyst (US3,953,517) is widely used in the method for synthesizing methyl isobutyl ketone by acetone one-step method at present, but this type of catalyst has poor thermal stability, catalyst regeneration is difficult, and the control requirements of operating conditions are harsh
The method for synthesizing methyl isobutyl ketone with palladium-loaded activated alumina as a catalyst introduced in Japanese Patent No. 63-119436 has problems such as high reaction temperature, low conversion rate, and poor selectivity of methyl isobutyl ketone.
And the traditional method of synthesizing methyl isobutyl ketone from acetone is carried out under high pressure

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] Weigh 26.15gZrOCl 2 ·8H 2 O, dissolved in deionized water, prepared as a 0.20mol / l aqueous solution. Another 44.63ml of ammonia water (28%) was taken and diluted to a 0.2mol / l aqueous solution. ZrOCl 2 ·8H 2 The aqueous solution of O is added dropwise to the precipitant ammonia solution, and the pH value of the solution is kept at about 10. After the dropwise addition, aging in the mother liquor at normal temperature for 24 hours, Zr(OH) 4 Hydrosol. Zr(OH) 4 The hydrosol was thoroughly washed with deionized water to be free of Cl -1 Exist, filter, and dry the filter cake in 383K air atmosphere for 10h, and then roast in 823K air for 3h, the particle size of zirconia is 18.09nm. The obtained product is compressed into tablets and crushed into 30-50 mesh particles.

[0012] According to the Pd content of 0.5wt%, take 0.0094g / ml of H 2 PdCl 4 solution, adjust the pH value to 3, impregnate the above-mentioned carrier with an equal volume, dry, roast, and then red...

Embodiment 2

[0015] The preparation of zirconia hydrosol is the same as in Example 1. After the dropwise addition, the reaction liquid was heated and boiled at 373K to reflux for 3 hours, and then fully washed with deionized water until there was no Cl -1 exist. After filtering, the filter cake was dried in 383K air atmosphere for 10h, and then calcined in 823K air for 3h, and the particle size of zirconia was 14.00nm. The obtained product is compressed into tablets and crushed into 30-50 mesh particles.

[0016] According to the Pd content of 0.5wt%, take 0.0094g / ml of H 2 PdCl 4 solution, adjust the pH value to 3, impregnate the above-mentioned carrier with an equal volume, dry, roast, and then reduce by passing hydrogen at 573K for 3 hours. The desired catalyst can be obtained.

[0017] Get 3g of above-mentioned catalysts and pack in the reactor, and reaction condition is the same as embodiment 1, and the results are shown in attached table.

Embodiment 3

[0019] Zr(OH) 4 The preparation of the hydrosol is the same as in Example 1. Zr(OH) 4 The hydrosol was added to the NaOH solution to keep the pH value at around 11, and heated and cooked under reflux for 3 hours at 373K. Then fully wash with deionized water until the ionic conductivity is less than 15μΩ -1 , dried in 373K air for 10h, and roasted in 823K air for 3h, the particle size of zirconia was 12.16nm. The obtained product is compressed into tablets and crushed into 30-50 mesh particles.

[0020] According to the Pd content of 0.5wt%, take 0.0094g / ml of H 2 PdCl 4 solution, adjust the pH value to 3, impregnate the above-mentioned carrier with an equal volume, dry, roast, and then reduce by passing hydrogen at 573K for 3h. The desired catalyst can be obtained.

[0021] Get 3g of above-mentioned catalysts and pack in the reactor, and reaction condition is the same as embodiment 1, and the results are shown in attached table.

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Abstract

The invention discloses a one-step process of acetone and a process for forming methyl isobutyl ketone and diisobutyl ketone. The method uses Pd / ZrO2 as a catalyst, the Pd content is 0.5wt%, and at normal pressure, the reaction temperature is 423K, the space velocity is 2h-1, and the hydroketone molar ratio is 2. Under the operating conditions, in a fixed bed reactor, acetone The highest conversion rate is 62%, and the highest selectivity of methyl isobutyl ketone and diisobutyl ketone is 100%.

Description

technical field [0001] The invention relates to a process method for synthesizing methyl isobutyl ketone and diisobutyl ketone in one step by catalyzing acetone. Background technique [0002] Methyl isobutyl ketone (MIBK) is an important organic solvent, which has excellent solubility and can dissolve most paint resins. It can also be used as a solvent for the production of tetracycline and penicillin. Wax agent can save cooling capacity, reduce solvent consumption, improve device processing capacity, reduce production cost, increase yield, and can also be used to produce refined paraffin and microcrystalline paraffin. [0003] Diisobutyl ketone (DIBK) has a high boiling point and a fast evaporation rate. It can be used as a solvent for nitro spray paint, vinyl resin paint and other synthetic resin paints to improve its moisture resistance. It can also be used as a dispersant for the manufacture of organic aerosols, an intermediate for food refinement and certain drugs and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C45/61C07C49/04
Inventor 徐贤伦刘晓红刘淑文汤爱华
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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