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Method for preparing N-(2-aminoethyl)-3-aminopropyltrimethoxysilane by adopting pipeline reactor

A technology of aminopropyltrimethoxysilane and chloropropyltrimethoxysilane is applied in the field of continuous preparation of aminopropyltriethoxysilane by using pipeline reactors, which can solve the problems of inconvenient starting and parking, complicated equipment and stable problems such as poor performance, to achieve the effects of low labor cost, shortened response time, and small liquid holding capacity

Pending Publication Date: 2021-10-15
ZHEJIANG KAIHUA SYNTHETIC MATERIAL +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, its equipment is complicated, its stability is poor, and it is inconvenient to drive and stop. It takes a considerable amount of time from driving to system stabilization, and produces a lot of intermediate materials.

Method used

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  • Method for preparing N-(2-aminoethyl)-3-aminopropyltrimethoxysilane by adopting pipeline reactor
  • Method for preparing N-(2-aminoethyl)-3-aminopropyltrimethoxysilane by adopting pipeline reactor
  • Method for preparing N-(2-aminoethyl)-3-aminopropyltrimethoxysilane by adopting pipeline reactor

Examples

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example

[0023] Device example: a continuous pipeline device for the preparation of N-(2-aminoethyl)-3-aminopropyltrimethoxysilane, its structure is as follows figure 1 Shown, including tubular reactor 7 and other equipment.

[0024] The ethylenediamine storage tank 1 is connected to the inlet of the preheating premix reactor 6 through a metering pump 4 through a pipeline, and the 3-chloropropyltrimethoxysilane storage tank 2 is connected to the preheating premix reactor 6 after the metering pump 5 The inlet is connected, the outlet of the preheating and premixing reactor 6 is connected with the inlet of the tubular reactor 7, the outlet of the tubular reactor 7 is connected with the inlet of the receiving tank 3, and a valve 13 is arranged at the outlet of the receiving tank 3; the reaction liquid passes through The outlet of the receiving tank 3 is sent to a vacuum distillation unit to obtain a refined product through distillation.

[0025] A valve 8 is provided on the pipeline betw...

Embodiment 1-1

[0030] Embodiment 1-1: A preparation method of N-(2-aminoethyl)-3-aminopropyltrimethoxysilane, comprising the following steps:

[0031] The ethylenediamine in the ethylenediamine storage tank 1 is pumped into the preheating premix reactor 6 with a flow rate of 7.5mL / min through the feed pump 4, and the 3-chloropropyltrimethoxysilane in the 3-chloropropyltrimethoxysilane storage tank 3 Propyltrimethoxysilane is pumped into the preheating premixing reactor 6 at a flow rate of 5.1 mL / min through the feed pump 5. The size of the preheating premixing reactor 6 is fixed, with a diameter of 6 mm and a length of 10 m. The preheating temperature It is generally set at 80-90°C; after preheating and mixing, the mixed solution enters the pipeline reactor 7, the diameter of the pipeline reactor 7 is 6mm, and its length is based on the set reaction time (that is, the raw material mixed solution in the pipeline reactor 7) is adjusted, and the reaction residence time of the raw material mixtu...

Embodiment 2-1～ Embodiment 2-3

[0037] Compared with Example 1-1, the tube length of the tube reactor 7 is changed, thereby changing the reaction residence time of the raw material mixed liquid in the tube reactor 7, and the rest is the same as that of Example 1-1. The product yield was detected to obtain the following data (Table 2).

[0038] Table 2, the impact of reaction residence time on N-(2-aminoethyl)-3-aminopropyltrimethoxysilane productive rate

[0039]

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Abstract

The invention discloses a method for preparing N-(2-aminoethyl)-3-aminopropyltrimethoxysilane by adopting a pipeline reactor, which comprises the steps of by taking 3-chloropropyltrimethoxysilane and ethidene diamine as raw materials, and reacting the raw materials consisting of ethidene diamine and 3-chloropropyltrimethoxysilane in the pipeline reactor, wherein the retention time of the raw materials in the pipeline reactor is 20-50 minutes, and the reaction temperature of the pipeline reactor is controlled to be 80-130 DEG C; and enabling a reaction product discharged from an outlet of the pipeline reactor to be subjected to separation treatment, and obtaining N-(2-aminoethyl)-3-aminopropyltrimethoxysilane serving as a product. The tubular reactor is adopted, so that the reaction time is greatly shortened, and the production efficiency is remarkably improved.

Description

technical field [0001] The invention relates to a synthesis method of an aminosilane coupling agent, in particular to a method for continuously preparing aminopropyltriethoxysilane by using a pipeline reactor. Background technique [0002] N-(2-aminoethyl)-3-aminopropyltrimethoxysilane is an important industrial additive widely used in the fields of ink coatings and industrial adhesives. It has the characteristics of fast hydrolysis and fast adhesion, which can meet the needs of most industrial applications. [0003] At present, the production process of N-(2-aminoethyl)-3-aminopropyltrimethoxysilane occupies a large area, and multiple reactors are started at the same time. Simultaneously, after the hydrochloric acid that this reaction generates combines with ethylenediamine to become ethylenediamine hydrochloride, the mass transfer capacity in the still body will decline, if the ethylenediamine consumption in the feed is insufficient, the ethylenediamine in the still body ...

Claims

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Application Information

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IPC IPC(8): C07F7/18
CPCC07F7/1892
Inventor 陈道伟陈禹锡黄亮兵周少东周伟钱超
Owner ZHEJIANG KAIHUA SYNTHETIC MATERIAL
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