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Method for continuously synthesizing diethyl phosphite in microchannel reactor

A technology of diethyl phosphite and microchannel reactor, which is applied in chemical instruments and methods, chemical/physical/physicochemical reactors, climate sustainability, etc., can solve the problem of diethyl phosphite yield decline, difficult Guarantee product quality, difficult to control reaction temperature and other issues, to achieve the effect of improving production efficiency, good temperature and safety controllability, and short reaction time

Inactive Publication Date: 2018-12-28
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, if the by-product separation process is not properly operated, it is easy to bring diethyl phosphite into the by-product, resulting in a decrease in the yield of diethyl phosphite
[0007] In the production process of the above method, the reaction temperature is difficult to control. If there is a risk of decomposition and explosion if the temperature is overheated, and the reaction temperature is high, it is difficult to guarantee the quality of the product.
In addition, the reaction conditions are too harsh to be implemented industrially

Method used

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  • Method for continuously synthesizing diethyl phosphite in microchannel reactor
  • Method for continuously synthesizing diethyl phosphite in microchannel reactor
  • Method for continuously synthesizing diethyl phosphite in microchannel reactor

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Experimental program
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Effect test

Embodiment 1

[0030] (1) Reference figure 2 Determine the connection method of the tubular reactor. The pipeline type is a straight structure and a diamond structure. The volume and flow rate of the pipeline determine the reaction molar ratio, and the heat exchange medium is heat transfer oil.

[0031] Phosphorus trichloride and chloroform are mixed uniformly in a volume ratio of 1:2, which is regarded as raw material A; anhydrous ethanol solution is regarded as raw material B, and the two materials are passed at a flow rate of 48ml / min and 19ml / min respectively The metering pump is injected into the reactor. At this time, n (anhydrous ethanol): n (phosphorus trichloride) = 1:3.5, adopt figure 2 In the microchannel reactor, the temperature is controlled at 30°C, the residence time is 60s, the reaction liquid is quantitatively collected, washed, then distilled under reduced pressure, and finally weighed and calculated to obtain a yield of 99.2% of the product diethyl phosphite. The selectivity...

Embodiment 2

[0033] (1) Reference figure 2 Determine the connection method of the tubular reactor. The pipeline type is a straight-through structure and a heart-shaped structure. The volume and flow rate of the pipeline determine the reaction molar ratio, and the heat exchange medium is heat transfer oil.

[0034] Phosphorus trichloride and chloroform are mixed uniformly at a volume ratio of 1:4, which is regarded as raw material A; anhydrous ethanol solution is regarded as raw material B, and the two materials are passed at a flow rate of 50ml / min and 22ml / min respectively The metering pump is injected into the reactor. At this time, n (anhydrous ethanol): n (phosphorus trichloride) = 1:4, adopt figure 2 In the microchannel reactor, the temperature is controlled at 55°C, the residence time is 300s, the reaction solution is quantitatively collected, washed with water, then distilled under reduced pressure, and finally weighed and calculated to obtain a yield of 99.4% of the product diethyl ph...

Embodiment 3

[0036] (1) Reference figure 2 Determine the connection method of the tubular reactor. The pipeline type is a straight structure and a circular structure. The volume and flow rate of the pipeline determine the reaction molar ratio, and the heat exchange medium is heat transfer oil.

[0037] Phosphorus trichloride and chloroform are mixed uniformly at a volume ratio of 1:5, which is regarded as raw material A; anhydrous ethanol solution is regarded as raw material B, and the two materials are passed at a flow rate of 58ml / min and 25ml / min respectively The metering pump is injected into the reactor. At this time, n (anhydrous ethanol): n (phosphorus trichloride) = 1:4, adopt figure 2 In the microchannel reactor, the temperature was controlled at 55°C, the residence time was 60s, the reaction liquid was quantitatively collected, washed with water, then distilled under reduced pressure, and finally weighed and calculated to obtain a yield of 99.1% of the product diethyl phosphite. Th...

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Abstract

The invention discloses a method for continuously synthesizing diethyl phosphite in a microchannel reactor, and belongs to the technical field of organic synthesis processes. More specifically, the method is a method for generating diethyl phosphite by a continuous reaction in a microchannel continuous flow reactor using anhydrous ethanol and phosphorus trichloride as a substrate and chloroform asa solvent, wherein the mixed solution of the chloroform and the phosphorus trichloride is a material A, the anhydrous ethanol solution is a material B, and the material A and the material B simultaneously enter a microchannel through a metering pump. According to the method, the efficient mass transfer and heat transfer efficiency of the microchannel reactor are utilized to effectively strengthenthe mass transfer rate between two-phase materials, and the safety and operability of an experiment are greatly improved.

Description

Technical field [0001] The invention belongs to the technical field of organic synthesis processes, and specifically relates to a continuous reaction process for preparing diethyl phosphite by esterification with anhydrous ethanol and phosphorus trichloride as raw materials. More specifically, it is a method in which absolute ethanol and phosphorus trichloride are used as substrates, and chloroform is used as a solvent to continuously react to produce diethyl phosphite in a microchannel continuous flow reactor. Background technique [0002] Diethyl phosphite, also known as diethyl phosphite, is an organic chemical raw material. It is an intermediate for the preparation of organophosphorus compounds. It is also used as an extractant and phosphate intermediate. It is used in fine chemicals. Has a very important position. It is also used in the synthesis of pesticides rice fenjing and aluminum triethylphosphonate. It can also be used to synthesize plasticizers, flame retardants, e...

Claims

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Application Information

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IPC IPC(8): C07F9/142B01J19/00
CPCB01J19/0093C07F9/142Y02P20/10
Inventor 严生虎刘倩张跃刘建武沈介发辜顺林马晓明陈代祥
Owner CHANGZHOU UNIV
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