System and method for synthesizing methyl ethyl oxalate based on micro-channel reactor

A microchannel reactor, methyl ethyl oxalate technology, applied in chemical instruments and methods, ester group and hydroxyl reaction preparation, chemical/physics/physicochemical reactors, etc., can solve the problem of long production cycle, complex production process, Affecting problems such as synthesis efficiency, to achieve the effect of reducing human accidents, high yield and high selectivity

Active Publication Date: 2019-09-27
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] Most of these methods are carried out in traditional tank reactors. The preparation cycle is long, the preparation process is complicated, and the unit consumption is high, which greatly affects the synthesis efficiency.

Method used

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  • System and method for synthesizing methyl ethyl oxalate based on micro-channel reactor
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  • System and method for synthesizing methyl ethyl oxalate based on micro-channel reactor

Examples

Experimental program
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Effect test

Embodiment 1

[0053] Continuously pump methanol and diethyl oxalate into the microreactor from a high-pressure infusion pump, and control the reaction at a temperature of 20°C, control the molar ratio of methanol to diethyl oxalate to 3.3:1, and the catalyst concentration to 5mg / mL , by controlling the total flow rate of the liquid to change the residence time of the reaction, the residence time of the two materials in the reactor is 1.38min, 1.73min, 2.3min, 3.45min, 6.9min respectively.

[0054] Collect the output liquids of different flow rates respectively, and all collect the output liquid of 1h, analyze and calculate the transformation rate of diethyl oxalate, the selectivity and productive rate of methyl ethyl oxalate with gas chromatography, the result is as attached figure 2 Shown in, under the microchannel reactor used in this implementation and reaction condition, the flow velocity that improves feed liquid is beneficial to the conversion of diethyl oxalate, but for the selectivi...

Embodiment 2

[0056] The process is the same as in Example 1, with the residence time being 2.3min (total feed flow rate 40μL / min), the molar ratio of methanol to diethyl oxalate being 3.3:1, the catalyst concentration being 5mg / mL, and the reaction temperature being 20°C respectively , 30°C, 40°C, 50°C. The products were analyzed by gas chromatography and the reaction results were shown in the attached image 3 shown. The results are attached image 3 As shown, the change trend of the conversion rate of diethyl oxalate by changing the temperature of the reaction is to decrease first and then remain unchanged slightly, while the conversion rate and selectivity of methyl ethyl oxalate are first increased and then decreased, and are obtained at 40 ° C. The highest, and therefore preferred, reaction temperature is 40°C.

Embodiment 3

[0058] The process is the same as in Example 1, with the residence time being 2.3min, the reaction temperature (total feed flow rate 40μL / min) being 40°C, the catalyst concentration being 5mg / mL, and the molar ratio of methanol to diethyl oxalate being 1.3:1 respectively , 2:1, 3.3:1, 5:1. The product was analyzed by gas chromatography, and the conversion rate of diethyl oxalate, selectivity and yield of methyl ethyl oxalate were calculated. The results are based on the attached Figure 4 It can be known that when the molar ratio is between 1.3:1 and 5:1, the conversion rate of diethyl oxalate has an upward trend first, while the selectivity of methyl ethyl oxalate shows a downward trend, and the yield change trend is first increased and then decreased. When the molar ratio is 2:1, both of them achieve the maximum value, so the better molar ratio is 2:1.

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Abstract

The invention belongs to the field of organic synthesis, and particularly discloses a system and method for synthesizing methyl ethyl oxalate based on a micro-channel reactor. The system comprises a first raw material bottle, a second raw material bottle, the micro-channel reactor and a collecting device. The micro-channel reactor comprises a first inlet micro-channel, a second inlet micro-channel, a micro-channel and a channel outlet. The first inlet micro-channel and the second inlet micro-channel are connected with the first raw material bottle and the second raw material bottle respectively. The other end of the first inlet micro-channel and the other end of the second inlet micro-channel are connected with the micro-channel. The channel outlet is connected with the collecting device. Through the efficient mixing and process strengthening of the micro-reactor, through an ester exchange method, the high methyl ethyl oxalate yield can be realized, and the selectivity is high; compared with a traditional kettle type reactor micro-reactor, continuous feeding can be realized, the production efficiency of the product is greatly improved, the process is safe and controllable, and human error accidents are reduced.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a system and method for synthesizing methylethyl oxalate based on a microchannel reactor. Background technique [0002] Oxalate is an important chemical raw material and pharmaceutical intermediate, such as Diethyl Oxalate (DEO for short) and Dimethyl Oxalate (DMO for short) can be used as intermediates to synthesize the drug Sulfamethoxazole Plastic Accelerator (Transesterification of diethyl oxalate with phenol usingMoO3 / SiO2 catalyst.Applied Catalysis A:General.2005 285,1–2,190-195), dye intermediate; the intermediate process of using syngas to prepare ethylene glycol is to synthesize grass Ester, and then use oxalate hydrogenation to prepare pure ethylene glycol patent (CN106083522A), which is enough to illustrate that oxalate is a kind of important raw material and is also used in coal chemical products. [0003] Therefore, as an intermediate between DEO and DMO, Ethyl Meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/03C07C69/36B01J19/00
CPCC07C67/03B01J19/0093C07C69/36
Inventor 钟秦纪国敬丁杰
Owner NANJING UNIV OF SCI & TECH
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