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Method for performing alkoxylation reaction in microreactor

A micro-reactor and alkoxylation technology, applied in chemical instruments and methods, preparation of organic compounds, preparation of aminohydroxy compounds, etc., can solve the problems of reducing the production efficiency of the reaction device, affecting the appearance of products, and prolonging the production cycle, etc. Achieve the effect of low epoxy compound content, saving washing water and reducing energy consumption

Inactive Publication Date: 2015-06-24
LIAONING OXIRANCHEM INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This not only consumes a lot of energy, but also prolongs the production cycle, reduces the production efficiency of the reaction device, and easily leads to yellowing of the product, affecting the appearance of the product

Method used

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  • Method for performing alkoxylation reaction in microreactor
  • Method for performing alkoxylation reaction in microreactor
  • Method for performing alkoxylation reaction in microreactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0087] In the microreactor (including two inlets) in series of four microreactor units, the active hydrogen compound and the catalyst mixture are used as fluid A, and the epoxy compound is used as fluid B, so that the two are mixed in the microreactor reaction. The microreactor is placed in a bath at a certain temperature, and the temperature is regulated through the outer wall of the microreactor unit. The microreactors of Examples 1.1 to 1.11 include a reaction zone of 20 ml, and the minimum equivalent diameter of the cross section is 0.05 mm. The flow rate adopted by fluid A is 15 g / min, and fluid B is put into the first microreactor unit in a certain molar ratio. Table 1 shows the selectivity of mono-addition products collected after the reaction of different active hydrogen compounds and epoxy compounds in Examples 1.1 to 1.11 and the residual amount of epoxy compounds.

[0088] Table 1

[0089]

[0090]

Embodiment 2

[0096] In the microreactor (including 4 inlets) in series of six microreactor units, the active hydrogen compound and the catalyst mixture are used as fluid A, and the epoxy compound is used as fluid B, so that the two are mixed in the microreactor reaction. The microreactor is placed in a bath at a certain temperature, and the temperature is regulated through the outer wall of the microreactor unit. The microreactors of Examples 2.1 to 2.10 comprise a reaction zone of 30 ml, and the minimum equivalent diameter of the cross section is 0.1 mm. The flow rate adopted by fluid A is 3g / min, and fluid B is put into the microreactor from three inlets (each 1 / 3) in a certain molar ratio. Table 3 shows the molecular weights, distribution coefficients and residual amount of epoxy compounds collected after the reaction of different active hydrogen compounds and epoxy compounds in Examples 2.1 to 2.10.

[0097] table 3

[0098]

Embodiment 3

[0104] In the microreactor (containing 5 inlets) that eight microreactor units are connected in series, reclaim the product that obtains in embodiment 2 as fluid A, and with epoxy compound as fluid B, make both carry out in microreactor Mixed reactions. The microreactor is placed in a bath at a certain temperature, and the temperature is regulated through the outer wall of the microreactor unit. The microreactors of Examples 3.1 to 3.6 comprise a reaction zone of 40 ml, and the minimum equivalent diameter of the cross section is 0.5 mm. The flow rate adopted by fluid A is 6g / min, and fluid B is put into the microreactor from four inlets (each 1 / 4) in a certain molar ratio. Table 5 shows the molecular weights, distribution coefficients and residual amounts of epoxy compounds collected after the reactions of different active hydrogen compounds and epoxy compounds in Examples 3.1 to 3.6.

[0105] table 5

[0106]

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PUM

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Abstract

The invention relates to a method for performing alkoxylation reaction in a microreactor, which comprises the following steps: adding a composite system composed of an active-hydrogen-containing compound, an epoxy compound and a catalyst into the microreactor, and carrying out alkoxylation reaction, wherein the microreactor is provided with a plurality of microchannels of which the cross section equivalent diameter is 0.001-10mm. The method can save resources and enhance the control safety in the alkoxylation reaction process, and is stable in process control. The obtained alkoxylation product has the advantages of light color, narrow distribution and low epoxy compound content.

Description

technical field [0001] The alkoxylation reaction of the present invention particularly relates to a method for carrying out the alkoxylation reaction in a microreactor. Background technique [0002] The reaction of the active hydrogen-containing compound with the alkoxy group of the epoxy compound is a stepwise addition reaction. Taking ethylene oxide as an example, the reaction with active hydrogen-containing compounds is as follows: [0003] [0004] It can be seen that the reaction process is a typical stepwise addition reaction, and the final product is a mixture of a series of different polymerization degrees, that is, there is a relative molecular mass distribution in the product. The width of the relative molecular mass distribution of ethoxylated products is one of the main factors affecting its physical and chemical properties and post-processing performance. The wider the relative molecular mass distribution of the product, the more unfavorable it is for the ra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07B41/04C07C43/13C07C43/178C07C43/23C07C41/03C07C213/04C07C215/14C07C215/24C07C69/54C07C67/26
Inventor 朱建民刘兆滨董振鹏周立明李雪峰
Owner LIAONING OXIRANCHEM INC
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