Process for synthesizing 3,3-dimethyl-2-butanone

A technology of dimethyl and butanone, applied in the direction of condensation to prepare carbonyl compounds, organic chemistry, etc., to achieve the effects of simple refining operation, lower reaction temperature, and simple operation

Active Publication Date: 2008-10-22
BC P INC CHINA NAT PETROLEUM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Domestic literature provides a kind of process method that takes tert-amyl alcohol as the starting material to synthesize pinaconone; also reports several methods for preparing pinacol, i.e., the isoamyl alcohol method, the tert-amyl alcohol method, and the pinacol method. Alcohol rearrangement method, alkene oxidation method, valeric acid-acetone method, hydrazone electrochemical oxidation method, no patent application for this technical route in China

Method used

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  • Process for synthesizing 3,3-dimethyl-2-butanone

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Experimental program
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Effect test

Embodiment 1

[0024] Add 114 g of lanthanum nitrate into the dipping kettle, add 100 g of deionized water to prepare a lanthanum nitrate solution for later use. Weigh the specific surface as 150m 2 / g, φ1.5mm strip Al with a pore volume of 0.9ml / g 2 o 3 After drying at 120°C for 4 hours and calcining at 700°C for 4 hours, 80 g of the treated carrier was added to the impregnation kettle, immersed at room temperature for 24 hours, and the remaining liquid was filtered off, dried at 120°C and calcined at 550°C for 4 hours to prepare catalyst A. Add 320g of the mixed solution prepared in a certain proportion to the thin jar, and use a metering pump to enter a fixed-bed reactor equipped with 100g of catalyst A under normal pressure for catalytic decarboxylation reaction. The reaction temperature is 400°C and the space velocity For 0.8h-, the gas phase product obtained by the reaction was condensed, the crude product was collected from the bottom of the condensing device, and a sample was taken...

Embodiment 2-5

[0026] Adopt neodymium nitrate, cerium nitrate, lanthanum nitrate-neodymium nitrate and lanthanum nitrate-cerium nitrate to prepare respectively catalyst B, C, D, E according to the catalyst preparation method of embodiment 1;

[0027] Table 1

[0028] Reality

Embodiment 6

[0030] The test process is the same as in Example 1, adopting a catalyst A 100g fixed-bed reactor to carry out the catalytic decarboxylation reaction, the temperature of reaction is 380°C, and the space velocity is 0.8h-, pivalic acid: acetic acid: water=1: 1.4: 3 , the gas phase product obtained by the reaction is condensed, the crude product is collected from the bottom of the condensing device, and the sample is analyzed. The test results are shown in Table 1.

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Abstract

The invention relates to a synthesis method of 3, 3-dimethyl-2-butanone by using pivalic acid and glacial acetic acid as raw materials which are catalyzed to react by gas phase under the conditions of normal pressure. The pivalic acid and the glacial acetic acid and water are uniformly mixed up under the normal temperature according to the molar ratio of 1:1:3 to 1:1.4:3; after vaporization, the pivalic acid and the glacial acetic acid and the water are catalyzed to have a decarboxylation reaction and then pinacolone is produced under the normal pressure with the temperature of 380 to 400 DEG C in a fixed bed reactor; the carrier of the catalyst is A12O3; active components are one or two compounds of rare earth metals Ce, Nd, La or oxides thereof; the active component content which is calculated according to the weight of metal oxides takes up 20-30 percent of the weight of the carrier A12O3; the bulk density of the catalyst is 0.47 to 0.5; after analysis, the selectivity of the pinacolone is above 95 percent and then the 3, 3-dimethyl-2-butanone product with the purity of 99 percent can be obtained after the pinacolone is purified by rectification under the normal pressure.

Description

technical field [0001] The invention relates to a method for synthesizing 3,3-dimethyl-2-butanone under normal pressure by adopting gas-phase catalytic reaction and using pivalic acid and glacial acetic acid as raw materials. Background technique [0002] Pinatone appears as a colorless liquid. It has mint flavor, easily soluble in alcohol ether, insoluble in water. It is an important raw material for the production of pesticides, and it is used for the production of dozens of fungicides and plants such as triadimefon (triadimefon), paclobutrazol, triadimenol, benzyl chloride triaconazole, specific effect azoles, diniconazole, tebuconazole, mecitrione, etc. Intermediates of growth regulators and pesticides. In the existing technology for preparing pinacolone, there are many problems such as many reaction steps, long flow process, complicated process, and low production efficiency, or the harsh reaction conditions, high equipment requirements, high investment and high cost,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/04C07C45/48
Inventor 赵英翠刘长清田振生王硕侯淑兰王芳盛光郑翔
Owner BC P INC CHINA NAT PETROLEUM CORP
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