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Method for synthesizing methyl isobutyl ketone from acetone by two-step process

A technology of methyl isobutyl ketone and acetone, applied in chemical instruments and methods, preparation of organic compounds, separation/purification of carbonyl compounds, etc., can solve the problems of difficulty in purification and separation of MIBK, increase in production cost, and high product cost, Achieve the effect of being conducive to smooth operation, improving the economic benefits of the enterprise, and long service life

Active Publication Date: 2015-02-18
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0013] The above reaction formulas (1) and (2) are controlled by thermodynamic equilibrium, and the conversion rate is relatively low. Among them, the conversion rate of formula (1) is about 15% at 10° C., and the selectivity is 90% to 95%.
The three-step method can only be carried out in different reactors due to the different mechanism of each step, and the reaction conditions and catalysts are different. The production process is long, the process is complicated, the production efficiency is low, and the product cost is high.
Due to the limitations of the one-step method, the presence of by-products such as 2-methylpentane, IPA, MO, and DIBK in the product affects the purity of the target product, resulting in difficulties in the purification and separation of MIBK, which increases production costs

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～3

[0052] Preparation of acetone condensation solid catalyst: mix pseudo-boehmite (produced by Shandong Aluminum Factory), extrusion aid and adhesive evenly, add water, knead and extrude to make a cylindrical shape. Dry the extrudate at 130°C, and then bake it at 500°C for 3 hours to obtain γ-Al 2 o 3 carrier. 500ml γ-Al 2 o 3 The carrier was immersed in 500ml of 7.5% calcium nitrate aqueous solution for 4 hours, then dried at 120°C for 4 hours, and calcined at 400°C for 4 hours to obtain the catalyst BTM-I. The physical properties of the catalyst are listed in Table 1.

[0053] Table 1

[0054] Example

[0055] Preparation of MO selective hydrogenation catalyst: Mix pseudo-boehmite (produced by Shandong Aluminum Factory), extrusion aid and adhesive evenly, add water, knead and extrude to make a cylindrical shape. Dry the extrudate at 130°C, and then bake it at 650°C for 3 hours to obtain γ-Al 2 o 3 carrier. 500ml γ-Al 2 o 3 The carrier is immersed in 500ml0....

Embodiment 4

[0066] Preparation of acetone condensation solid catalyst: mix pseudo-boehmite (produced by Shandong Aluminum Factory), extrusion aid and adhesive evenly, add water, knead and extrude to make a cylindrical shape. Dry the extrudate at 130°C, and then bake it at 500°C for 3 hours to obtain γ-Al 2 o 3 carrier. 500ml γ-Al 2 o 3 The carrier was immersed in 500ml of 5.3% barium nitrate aqueous solution for 4 hours, then dried at 120°C for 4 hours, and calcined at 400°C for 4 hours to obtain the catalyst BTM-II. The physical properties of the catalyst are listed in Table 1.

[0067] Preparation of MO selective hydrogenation catalyst: Mix pseudo-boehmite (produced by Shandong Aluminum Factory), extrusion aid and adhesive evenly, add water, knead and extrude to form a cylindrical shape. Dry the extrudate at 130°C, and then bake it at 650°C for 3 hours to obtain γ-Al 2 o 3 carrier. 500ml γ-Al 2 o 3 The carrier is immersed in 500ml0.12% Pd solution (take PdCl 2 It is Pd metal ...

Embodiment 5

[0072] Preparation of acetone condensation solid catalyst: mix pseudo-boehmite (produced by Shandong Aluminum Factory), extrusion aid and adhesive evenly, add water, knead and extrude to make a cylindrical shape. Dry the extrudate at 130°C, and then bake it at 500°C for 3 hours to obtain γ-Al 2 o 3 carrier. 500ml γ-Al 2 o 3 The carrier was immersed in 500ml of 12.3% calcium nitrate aqueous solution for 4 hours, then dried at 120°C for 4 hours, and calcined at 400°C for 4 hours to obtain the catalyst BTM-II. The physical properties of the catalyst are listed in Table 1.

[0073] The bimolecular acetone condensation reactions were carried out in trickle bed reactors, and the loading amount of catalyst BTM-I in each reactor was 100ml. The reaction conditions are shown in Table 4. The acetone raw material passes through the catalyst bed of the first reactor from top to bottom, and the output product enters the molecular sieve adsorption and dehydration tank. The molecular siev...

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Abstract

The invention relates to a method for synthesizing methyl isobutyl ketone from acetone by a two-step process. The method comprises the following steps: a fixed bed catalytic condensation reactor is filled with a solid catalyst, and acetone used as a reaction raw material is subjected to condensation-dehydration reaction on the catalytic condensation reaction bed to generate mesityl oxide and water; the product from the reactor enters a molecular sieve adsorption dehydration tank; the organic oil phase after dehydration enters a second fixed bed catalytic condensation reactor, and the acetone is further subjected to condensation-dehydration reaction to generate mesityl oxide and water; and the product enters a fixed bed catalytic hydrogenation reactor, the mesityl oxide is subjected to selective hydrogenation reaction on a Pd / Al2O3 catalyst to generate methyl isobutyl ketone, and the hydrogenation product is sent into a subsequent rectification separation system and subjected to separation to obtain the methyl isobutyl ketone product with the purity of greater than 99%. The invention provides a method for producing methyl isobutyl ketone from dimolecular acetone by a condensation-hydrogenation two-step process; and the acetone conversion rate is greater than or equal to 30.0%, and the methyl isobutyl ketone selectivity is greater than or equal to 99.0%.

Description

technical field [0001] The invention relates to a method for synthesizing methyl isobutyl ketone by a two-step method from acetone. Background technique [0002] Methyl isobutyl ketone (abbreviated as MIBK) is an important organic solvent used for dewaxing waxy oil in paints, and is also one of the raw materials for the production of rubber antioxidants, resin coatings, and can also be used as a solvent for the production of tetracycline and penicillin. In oil refining, it is widely used as a petroleum dewaxing agent for the production of refined paraffin. [0003] The traditional production method of MIBK is a three-step method: [0004] The first step: Two molecules of acetone (abbreviated as AC) are condensed under the action of a basic catalyst to generate one molecule of diacetone alcohol, referred to as DAA. [0005] 2CH 3 COCH 3 →(CH 3 ) 2 COHCH 2 COCH 3 (1) [0006] AC DAA [0007] Second step: diacetone alcohol is dehydrated under the action of an acid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/04C07C45/62C07C49/203C07C45/74
CPCC07C45/74C07C45/79C07C45/82C07C49/203C07C49/04
Inventor 南军于海斌张景成张玉婷耿姗曲晓龙臧甲忠刘艳姜雪丹张雪梅
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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