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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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

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

Examples

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Example Embodiment

[0017] Example 1

[0018] Reaction process see figure 1 . The micro-reactor system consists of a preheater 11, a micro-mixer 4, a micro-channel reactor 5 and a micro heat exchanger 10. The internal channel of the micromixer 4 adopts an interdigital T-type mixing method, and the channel is a 300μm×300μm square channel, that is, an equivalent diameter of 300μm; the internal channel of the microchannel reactor 5 is 300mm long and has an equivalent diameter of 300μm.

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

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

Example

[0023] Examples 2-8

[0024] Refer to Example 1 for the reaction process. 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 to 1-ethanol-3-methylimidazolium bromide (denoted as PO / Cat.), at the same reaction temperature, reaction pressure and material residence time conditions as in Example 1 Next, the cyclization synthesis reaction is carried out in the microreactor system, and the selectivity of the target product propylene carbonate ( Selectivity ) And yield ( Yield ) Listed in the following table:

[0025]

Example Embodiment

[0026] Example 9

[0027] Refer to Example 1 for the reaction process. The concentration of the key reaction materials in the fixed process, that is, the molar ratio of fixed 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, the residence time of the reaction materials in the micromixer and microchannel reactor is For 60 seconds, the reaction pressure is 3.5MPa, and propylene carbonate is synthesized at the reaction temperature of 100°C, 140°C, 160°C, and 220°C. Under the corresponding conditions, the single-pass yield of the target product propylene carbonate is 35.62%, 53.84%, and 79.58, respectively. %, 68.74%, 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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