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Method of preparing alkyl carbonate and cycloalkyl alcohol synchronously

A kind of technology of dialkyl carbonate and cycloalkyl glycol is applied in the field of simultaneous preparation of dialkyl carbonate and cycloalkyl glycol, which can solve the problem of simultaneous preparation of dialkyl carbonate and cycloalkyl glycol. Glycol etc.

Inactive Publication Date: 2007-10-24
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In summary, there is no report on the simultaneous preparation of dialkyl carbonate and cycloalkyl glycols so far.

Method used

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  • Method of preparing alkyl carbonate and cycloalkyl alcohol synchronously
  • Method of preparing alkyl carbonate and cycloalkyl alcohol synchronously
  • Method of preparing alkyl carbonate and cycloalkyl alcohol synchronously

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] CO control 2 The mol ratio of cyclohexane / epoxide is 1.1: 1, enters synthesis reactor, the amount of tetraethylamine bromide (catalyst 1) is 1% of cyclohexane weight, 180 ℃ of temperature of reaction, raw material 7MPa, reaction time 1 hour. The intermediate rectification tower is a packed tower with 30 plates, a vacuum of 0.09Mpa, a reflux ratio of 1.0, an intermediate purity of 99.3%, and a total yield of 99.0% (in terms of epoxycyclohexane).

[0045] Regulate the mol ratio of methyl alcohol / intermediate 10: 1, enter transesterification rectifying column, sodium methylate is catalyst 2, the consumption of sodium methylate is 0.5% of intermediate and methyl alcohol gross weight, and reaction temperature remains on 60~70 ℃, Under normal pressure, react for 1.5 hours, the intermediate conversion rate is 99.5%, and the selectivity of 1,2-cyclohexanediol is 100%. The transesterification distillation column is a plate column with 60 plates and a reflux ratio of 1.5.

[0...

Embodiment 2

[0049] CO control 2 The 1.1:1 mol ratio of epoxy cyclohexane enters the synthetic reactor, and the amount of KI / PEG400 compound (catalyst 1) is 1% of epoxy cyclohexane weight, 150 ℃ of reaction temperature, raw material 4MPa, reaction time 1 hour. The intermediate rectification tower is a packed tower with 30 plates, a vacuum of 0.09Mpa, a reflux ratio of 1.0, an intermediate purity of 99.5%, and a total yield of 99.2% (in terms of epoxycyclohexane).

[0050] Regulate the mol ratio of methyl alcohol / intermediate 9.5: 1, enter transesterification rectifying column, potassium hydroxide is catalyzer (catalyst 2), and the consumption of potassium hydroxide is 0.8% of intermediate and methyl alcohol gross weight, and temperature of reaction remains at 60-70°C, normal pressure, reaction for 1.5 hours, the conversion rate of intermediates is 99.6%, and the selectivity of 1,2-cyclohexanediol is 100%. The transesterification distillation column is a packed column with 70 trays and th...

Embodiment 3

[0054] CO 2 The 1.1:1 mol ratio of epoxy cyclohexane enters the synthetic reactor, and catalyst 1 is nickel chloride, triphenylphosphine, zinc powder and tetrabutylammonium bromide (TBAB) system, and the consumption of catalyst 1 is ring 2% by weight of oxycyclohexane, reaction temperature 150° C., raw material 3 MPa, reaction time 1 hour. The intermediate rectifying tower is a packed tower with 30 trays, a vacuum of 0.09Mpa, and a reflux ratio of 1.0. The resulting intermediate has a purity of 99.6% and a total yield of 99.6% (in terms of epoxycyclohexane).

[0055] Regulate the mol ratio of methyl alcohol / intermediate 10.5: 1, enter transesterification reaction rectification column, strong basic anion exchange resin is catalyst 2, and its consumption is 5% of intermediate and methanol gross weight, and reaction temperature remains on 60~ 70°C, normal pressure, reaction for 1.5 hours, the conversion rate of intermediates is 99.7%, and the selectivity of 1,2-cyclohexanediol i...

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Abstract

The invention discloses a preparing method of carbonic dialkyl ester and cycloalkyl dihydroxy alcohol, which comprises the following steps: (1) reacting cycloalkyl epoxy compounds and carbon dioxide to produce intermediate acted by catalyst; (2) reacting intermediate in the step (1) and R1OH to obtain the object. The invention improves quality of carbonic dialkyl ester and cycloalkyl dihydroxy alcohol, which supplements the blank of present technique.

Description

technical field [0001] The present invention relates to a method for simultaneously preparing alkyl carbonate and cycloalkyl alcohol, in particular to a method for simultaneously preparing dialkyl carbonate and cycloalkyl glycol. Background technique [0002] Dialkyl carbonate is a "green" alkylating agent, carbonylating agent and oil additive, and its representative compound is dimethyl carbonate (DMC). Similarly, cycloalkyl diols are also an extremely important organic chemical raw material. For example, 1,2-cyclohexanediol is a key intermediate for the preparation of polyamides, polyesters and pharmaceuticals, and so far, 1,2-cyclohexanediol has not been produced in a large scale. [0003] There have been many reports on the preparation of dialkyl carbonate and cycloalkyl glycol respectively. As far as the preparation of dialkyl carbonate is concerned, there are mainly three types. One is: "ester exchange method" (U.S.Pat.No.6,365,767, U.S.Pat.No.6,207,850 and U.S.Pat....

Claims

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Application Information

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IPC IPC(8): C07C69/96C07C68/06C07C35/14C07C27/02
Inventor 方云进刘百萍
Owner EAST CHINA UNIV OF SCI & TECH
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