Method for synthesizing cyclic carbonate ester in micro reactor system

A technology of cyclic carbonates and microreactors, applied in chemical instruments and methods, organic chemistry methods, formation/introduction of functional groups, etc., can solve the problem of low catalyst system activity, poor heat and mass transfer performance, and difficult process control and other issues, to achieve the effect of improving energy utilization, operating flexibility, and shortening response time

Active Publication Date: 2012-05-23
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0004] All of the above catalytic reaction systems mostly adopt batch stirred tank reactor technology, which has disadvantages such as poor heat and mass transfer performance, low space-time yield, discontinuous process, and low safety.
The synthesis of cyclic carbonates from carbon dioxide and epoxy compounds is a strong exothermic and fast gas-liquid reaction (≈-96 kJ / mol), which is controlled by gas-liquid mass transfer. Therefore, the existing reaction process in the kettle is generally below 120 °C. It is operated for a long time (several hours or even more than ten hours), and the pressure in the kettle changes greatly during the reaction process, which makes process control difficult. In addition, the activity of the existing catalyst system is not high, so that the overall efficiency of the process is low.

Method used

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  • Method for synthesizing cyclic carbonate ester in micro reactor system
  • Method for synthesizing cyclic carbonate ester in micro reactor system

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Experimental program
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Embodiment 1

[0018] For the reaction process, see figure 1 . The microreactor system consists of a preheater 11 , a micromixer 4 , a microchannel reactor 5 and a microheat exchanger 10 . The inner channel of the micro-mixer 4 adopts the interdigitated T-shaped mixing method, and the channel is a square channel of 300 μm×300 μm, that is, the equivalent diameter is 300 μm; the length of the channel in the micro-channel reactor 5 is 300 mm, and the equivalent diameter is 300 μm.

[0019] The microreactor system specifically includes a storage tank 1 containing carbon dioxide gas, a storage tank 2 for the reaction raw material liquid, a high-pressure metering pump 3; a micromixer 4, a microchannel reactor 5, a gas-liquid separation tank 6, a first-stage flash Steam tank 7, second stage flash tank 8, vacuum distillation tower 9, microchannel heat exchanger 10, preheater 11;

[0020] The storage tank 1 of carbon dioxide gas is connected to one inlet of the micro-mixer 4 through a preheater 11 ...

Embodiment 2～8

[0024] The reaction process is described with reference to Example 1. Change the concentration of key reaction materials in the process, that is, change the molar ratio of carbon dioxide to propylene oxide (denoted as, CO 2 / PO), and the mass ratio of propylene oxide and 1-ethanol-3-methylimidazolium bromide (recorded as PO / Cat.), at the same reaction temperature, reaction pressure and material residence time conditions as in Example 1 Next, in the microreactor system, carry out the ring closure synthesis reaction, the selectivity of the obtained target product propylene carbonate ( Selectivity ) and yield ( Yield ) are listed in the table below:

[0025]

Embodiment 9

[0027] The reaction process is described with reference to Example 1. The concentration of the key reactant material in the fixed process, i.e. the molar ratio of carbon dioxide to propylene oxide (CO 2 / PO) is 1.4, and the mass ratio of propylene oxide to 1-ethanol-3-methylimidazolium bromide (PO / Cat.) is 9, and the residence time of the reaction materials in the micro-mixer and microchannel reactor is 60 seconds, reaction pressure 3.5MPa, synthesis of propylene carbonate under the conditions of reaction temperature 100°C, 140°C, 160°C, 220°C, the one-pass yield of the target product propylene carbonate under the corresponding conditions were 35.62%, 53.84%, 79.58% %, 68.74%, the selectivity is greater than 99.7%.

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Abstract

The invention relates to a method for synthesizing cyclic carbonate ester in a micro reactor system, which comprises the following steps of: firstly mixing a liquid material containing an epoxy compound and a catalyst with a gas material containing carbon dioxide in a micro mixer, and then synthesizing cyclic carbonate ester in a micro channel reactor through a cyclization reaction. For the method, the reaction temperature is 100-220 DEG C, the pressure is 1.0-7.0 MPa, the molar ratio of carbon dioxide to epoxy compound in the gas-liquid two-phase material is 1.0-5:1, the mass ratio of the epoxy compound to the catalyst is 1.0-1000:1, and the retention time of the gas-liquid two-phase material in the micro channel reactor is 1.0-300 s. The reaction system has quick mass transfer and heat transfer rates, continuous process, easiness in control, high process safety and high energy utilization ratio, and the space-time yield and the selectivity of the target product can be greatly increased.

Description

technical field [0001] The present invention relates to a method for synthesizing cyclic carbonate, in particular to a method for synthesizing cyclic carbonate in a microreactor system. Background technique [0002] Carbon dioxide is an important greenhouse gas. As countries around the world pay more and more attention to it, its capture, storage and recycling technology has become the focus of world attention. People have been looking for solutions for the recycling of carbon dioxide, and the synthesis of cyclic carbonate compounds from carbon dioxide and epoxy compounds is one of the main ways to recycle carbon dioxide. Cyclic carbonate compounds are high-boiling-point and high-polarity organic solvents with excellent performance, and have been widely used in organic synthesis (synthesis of dimethyl carbonate, etc.), gas absorption, battery electrolyte and metal extraction and other fields. [0003] At present, most of the public reports on the synthesis of cyclic carbona...

Claims

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Application Information

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IPC IPC(8): C07B41/00C07D317/36C07D317/38B01J19/00
CPCY02P20/10
Inventor 陈光文赵玉潮
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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