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Dimethyl carbonate synthesis method by using methanol and carbon dioxide

A technology of dicyclohexylcarbodiimide and methanol, which is applied to the preparation of carbon dioxide or inorganic carbonate, chemical instruments and methods, nickel organic compounds, etc. It can solve the problems of difficult activation, reaction thermodynamic limitations, and low reaction conversion rate. , to achieve the effects of less dosage, chemical transformation and simple preparation

Active Publication Date: 2013-04-17
陕西高安绿能生物化工有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Due to the presence of CO in this reaction 2 Difficult activation and thermodynamic limitations of the reaction lead to low reaction conversion, which has become a bottleneck for the industrial application of methanol and carbon dioxide to synthesize dimethyl carbonate.

Method used

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  • Dimethyl carbonate synthesis method by using methanol and carbon dioxide
  • Dimethyl carbonate synthesis method by using methanol and carbon dioxide
  • Dimethyl carbonate synthesis method by using methanol and carbon dioxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1: Preparation and characterization of catalyst

[0022] Catalyst of the present invention is benzimidazole derivative ligand and Ni(OAc) 2 . 4H 2 The complex generated by the O reaction, wherein the benzimidazole derivative ligand is synthesized according to the method reported in the literature, that is, it is prepared by condensation of o-phenylenediamine and the corresponding benzoic acid derivative, and the preparation route of the catalyst is as follows figure 1 shown.

[0023] Preparation of Catalyst I

[0024] Ligand 1 Synthesis

[0025] Add 10.80 g of o-phenylenediamine and 16.6 g of phthalic acid into a 250 ml round bottom flask, then add an appropriate amount of PPA (polyphosphoric acid), slowly raise the temperature, stir and heat, and start timing when the temperature rises to 150 °C. After 4 h, the reaction solution was emerald green. After the reaction was over, it was poured into a 500 ml beaker filled with cold water, stirred thorou...

Embodiment 2

[0038] Embodiment 2: Methanol and carbon dioxide synthesis dimethyl carbonate catalyst screening

[0039] In 250 ml autoclave, add corresponding catalyst (catalyst 1~ Ⅲ ) 1 mmol, 2.06 g DCC and 32 g methanol, the CO 2 After replacing the reactor three times, control the pressure to 1.0 MPa, stir and heat, and start timing when the temperature rises to 70 °C. After reacting for 6 hours, cool the reactor to room temperature, distill the reaction liquid, and use GCMS to collect the liquid Detect the content of dimethyl carbonate (using n-butanol as internal standard), and calculate the reaction yield (in DCC). The results are shown in Table 1, the catalyst Ⅰ The catalytic effect is the best.

[0040]

Embodiment 3

[0041] Embodiment 3: take DCC as coupling agent, catalyst Ⅰ is the catalyst, methanol and carbon dioxide synthesis of dimethyl carbonate reaction temperature screening

[0042] Similar to Example 2, the difference is: methanol and carbon dioxide synthesize dimethyl carbonate, with DCC as coupling agent, catalyst Ⅰ As a catalyst, the reaction temperature is from 50-100°C. The results are shown in Table 2, the optimum reaction temperature is 80°C.

[0043]

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PUM

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Abstract

The invention discloses a chemical compound as shown in a structural formula (1) and an application thereof in dimethyl carbonate synthesis. According to the invention, methanol and carbon dioxide serve as raw materials, DCC serves as a coupling agent, and dimethyl carbonate with satisfactory production rate is obtained under the condition of the existence of Ni coordination compound catalyst and relatively mild condition. The condition of the dimethyl carbonate synthesis in the catalyst system of the invention is relatively mild, and the requirement of equipment strength of high pressure is avoid; the catalyst is easy to prepare and the cost is low; and the usage amount of catalyst is small, the reaction time is short, the recycling after separation is easy, and the industrialized production is facilitated.

Description

technical field [0001] The invention relates to a method for synthesizing dimethyl carbonate from methanol and carbon dioxide, belonging to the technical field of organic chemistry. Background technique [0002] Dimethyl carbonate (DMC) is an environmentally friendly green chemical product that has been widely concerned at home and abroad in recent years, and is known as the "new building block" of organic synthesis in the 21st century. It can replace toxic reagents such as phosgene, dimethyl sulfate, and methyl chloride, and can perform reactions such as methylation, carbonylation, and methoxylation, and is used to synthesize a variety of important fine chemicals. Dimethyl carbonate is a good solvent that can be used as an electrode solution for lithium batteries. In addition, the oxygen content of dimethyl carbonate molecules is as high as 53%, which can replace methyl tert-butyl ether (MTBE) as an environmentally friendly petroleum additive. [0003] At present, the meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/04B01J31/22C07C69/96C07C68/04
CPCY02P20/141
Inventor 师艳宁金洗郎李剑利史真白俊明常学军
Owner 陕西高安绿能生物化工有限公司
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