Method for continuous synthesis of dialkyl phosphite in micro-channel reactor

A dialkyl phosphite, microchannel reactor technology, applied in chemical instruments and methods, climate sustainability, sustainable manufacturing/processing, etc., can solve the problem of low yield of target products, achieve temperature and safety Good controllability, high production efficiency, flexible production effect

Inactive Publication Date: 2018-11-20
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, although there are also micro-reactions for the preparation of diethyl phosphite, the yield of the target product is not high. The present invention provides a process for the continuous production of dialkyl phosphite using a tubular reactor with a specific structure. method, realizing the continuous, safe, efficient and stable production of the product

Method used

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  • Method for continuous synthesis of dialkyl phosphite in micro-channel reactor
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  • Method for continuous synthesis of dialkyl phosphite in micro-channel reactor

Examples

Experimental program
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Effect test

Embodiment 1

[0035] (1) Refer to figure 2 Determine the connection mode of the tubular reactor, the pipe type is a straight-line structure and a rhombus structure, the pipe volume and flow rate determine the reaction molar ratio, and the heat exchange medium is heat transfer oil.

[0036] Phosphorus trichloride is regarded as raw material A; Dehydrated alcohol solution is regarded as raw material B, and two streams of materials are injected in the reactor by metering pump with the flow rate of 9ml / min and 29ml / min respectively, now n (trichloride Phosphorus): n (absolute ethanol) = 1:3, using figure 2 In a microchannel reactor, the temperature was controlled at 30° C., and the residence time was 60 s. The reaction solution was collected quantitatively and then distilled under reduced pressure. Finally, it was weighed and calculated to obtain a yield of 99.1% of the product diethyl phosphite. The selectivity of diethyl phosphite was 99.4% by GC analysis.

Embodiment 2

[0038] (1) Refer to figure 2 Determine the connection mode of the tubular reactor, the pipe type is a straight-line structure and a heart-shaped structure, the pipe volume and flow rate determine the reaction molar ratio, and the heat exchange medium is heat transfer oil.

[0039] Phosphorus trichloride is regarded as raw material A; Methanol solution is regarded as raw material B, and two streams of materials are injected in the reactor through metering pumps with the flow velocity of 11ml / min and 35ml / min respectively, at this moment n (phosphorus trichloride) : n (methanol) = 1:4, using figure 2 In a microchannel reactor, the temperature is controlled at 40° C., and the residence time is 300 s. The reaction solution is quantitatively collected, then distilled under reduced pressure, and finally weighed and calculated to obtain a yield of 99.4% of the product dimethyl phosphite. The selectivity of dimethyl phosphite was 99.3% by GC analysis.

Embodiment 3

[0041] (1) Refer to figure 2 Determine the connection mode of the tubular reactor, the pipe type is a straight-line structure and a circular structure, the pipe volume and flow rate determine the reaction molar ratio, and the heat exchange medium is heat transfer oil.

[0042] Phosphorus trichloride is regarded as raw material A; Virahol solution is regarded as raw material B, and two streams of materials are injected in the reactor through metering pumps with the flow rate of 13ml / min and 31ml / min respectively, at this moment n (trichloride Phosphorus): n (isopropanol) = 1:3.8, using figure 2 In a microchannel reactor, the temperature is controlled at 55° C., and the residence time is 60 s. The reaction solution is quantitatively collected and then distilled under reduced pressure. Finally, it is weighed and calculated to obtain a yield of 99.1% of the product diisopropyl phosphite. The selectivity of diisopropyl phosphite was 99.5% by GC analysis.

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Abstract

The invention discloses a method for continuous synthesis of dialkyl phosphite in a micro-channel reactor and belongs to the technical field of organic synthesis technologies. The method is used for generating the dialkyl phosphite through continuous reaction in the micro-channel continuous-flow reactor by using alcohol and phosphorus trichloride as substrates. Phosphorus trichloride is used as the material A, an alcohol solution is used as the material B, and the material A and the material B enter a micro-channel simultaneously through a metering pump for the continuous esterification reaction. According to the technological method, the high mass and heat transfer efficiency of the micro-channel reactor is utilized, the mass transfer rate between the two phase materials is effectively increased, and the safety and the operability of a test are greatly improved.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis technology, and in particular relates to a continuous reaction process for preparing dialkyl phosphite through esterification of alcohol and phosphorus trichloride as raw materials. More specifically, methanol, absolute ethanol, isopropanol and phosphorus trichloride are respectively used as substrates to continuously react in a microchannel continuous flow reactor to generate dimethyl phosphite, diethyl phosphite, and phosphorous acid. Diisopropyl method. Background technique [0002] Dialkyl phosphite is an important phosphorus-containing additive, which has good anti-wear and anti-oxidation properties, and has good composite performance when used in combination with sulfur-based anti-wear agents. At the same time, dialkyl phosphite occupies a very important position in the preparation of pesticide organic phosphorus corrosion inhibitors, plastic additives, dye additives and flame ret...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/142
CPCC07F9/142Y02P20/10
Inventor 严生虎刘倩袁卿凯张跃刘建武沈介发辜顺林马晓明陈代祥
Owner CHANGZHOU UNIV
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