A process of preparing dimethyl carbonate by oxidative carbonylation of methanol

A technology for the oxidation of dimethyl carbonate and methanol, which is applied in the purification/separation of carbonate/haloformate, the preparation of organic compounds, the preparation of carbonate/haloformate, etc., and can solve the reaction and separation process Complexity and other problems, to achieve the effect of simplifying the reaction and separation process, improving the service life and small investment

Active Publication Date: 2015-09-09
TAIYUAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the reaction and separation process is relatively complicated, and the DMC content in the crude product separated after the system is stable is only 19.2%.

Method used

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  • A process of preparing dimethyl carbonate by oxidative carbonylation of methanol
  • A process of preparing dimethyl carbonate by oxidative carbonylation of methanol
  • A process of preparing dimethyl carbonate by oxidative carbonylation of methanol

Examples

Experimental program
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Effect test

Embodiment 1

[0023] The inner diameter of the catalytic distillation tower is 80mm. The upper part of the catalytic distillation tower is the rectification section, the middle part is the reaction section, and the lower part is the stripping section. The bottom of the stripping section is equipped with a reboiler, and the top of the rectification section is equipped with a condenser and a buffer tank. . The reaction section is randomly packed with CuY catalyst formed into Raschig rings, with a height of 2800mm. The rectification section and stripping section are packed with ordinary separation packing stainless steel θ rings, the heights are respectively 200mm and 1000mm. After the catalytic distillation tower device is ready for purging and solid gas replacement, liquid methanol is fed from the top of the reaction section of the catalytic distillation tower at a space velocity of 0.2h -1 , CO and nitrogen are fed from the bottom of the stripping section, O 2 It is divided into 4 feeds in th...

Embodiment 2-10

[0024] Example 2-10: On the basis of the operation of Example 1, the filling height of each section of the catalytic distillation tower, the inner diameter of the tower, the type of packing, the type of catalyst, composition and molding, and the reaction operating conditions were changed. The specific catalytic distillation column parameters are shown in Table 1, the specific catalyst composition and preparation method are shown in Table 2, and the specific process conditions and reaction results are shown in Table 3.

[0025] Table 1

[0026]

[0027] Table 2

[0028]

[0029] table 3

[0030]

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Abstract

A process of preparing dimethyl carbonate by oxidative carbonylation of methanol adopts a catalytic rectification column as the main reacting device. The upper part of the catalytic rectification column is adopted as a rectification section, the middle part of the catalytic rectification column is adopted as a reacting section and the lower part of the catalytic rectification column is adopted as a distillation section. A reboiler is disposed at the bottom of the distillation section. A condensation reflux device is disposed at the top of the rectification section. Liquid methanol is fed from the top of the reacting section of the catalytic rectification column. Pressurized CO and nitrogen are fed from the bottom of the distillation section. O2 is divided into 1-5 parts and fed from the reacting section in a staged manner. Descending methanol and ascending CO / O2 in the reacting section are subjected to countercurrent contact, and react continuously to produce the dimethyl carbonate product in a catalyst filler bed layer in the reacting section. The rectification section mainly separates unreacted methanol from byproducts with low boiling points. A crude dimethyl carbonate product is obtained by rectification in the upper part of the distillation section. The process is advantageous in that the synthetic process is simple, the methanol conversion rate is high and purity of the dimethyl carbonate product is high.

Description

Technical field [0001] The invention belongs to a process for synthesizing dimethyl carbonate, and specifically relates to a process for synthesizing dimethyl carbonate by a methanol liquid phase oxidative carbonylation method. technical background [0002] Dimethyl carbonate (DMC) is an important organic synthesis intermediate because it contains methyl, methoxy, carbonyl, ester and other functional groups in its molecule, which can replace phosgene and dimethyl sulfate. A variety of highly toxic chemicals are widely used in the preparation of high-performance resins, dye intermediates, drugs, food preservatives, lubricating additives and other fields. Because of the high oxygen content in the molecule, it can increase the octane number and be used as a gasoline additive. DMC has good solvent properties and low vapor pressure, and can be used as a solvent for lithium battery liquid components and special coatings. The preparation methods include phosgene method, transesterific...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/96C07C68/00
CPCC07C68/00C07C68/08C07C69/96Y02P20/10
Inventor 李忠王霞郑华艳付廷俊
Owner TAIYUAN UNIV OF TECH
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