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Continuous production reaction device and continuous production reaction method for N-(beta-aminoethyl)-gamma-aminopropyltrimethoxysilane

A technology of aminopropyltrimethoxysilane and reaction device, which is applied in the field of silane coupling agent, can solve the problems of reducing output, increasing consumption, increasing product consumption, etc., so as to reduce labor intensity and amount of labor, increase reaction rate, and simplify The effect of applying steps

Active Publication Date: 2013-11-27
淄博市临淄齐泉工贸有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Repeated waste of manpower and material resources
[0004] And after the reaction of the traditional production process is completed, the mutual insolubility of the product itself of N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane is not as obvious as that of oil and water, so it is difficult to separate layers in the settling tank. slower
It is necessary to release the lower by-product ethylenediamine hydrochloride from the bottom of the kettle after a long period of rest, and then release the reaction supernatant; the separation time between the upper and lower layers needs to be controlled manually by the operator. If the rest time is insufficient, there will still be The mixed layer of ethylenediamine hydrochloride and the supernatant in the middle not only wastes a long time but also causes high operational difficulty for the operator. Two situations may occur if the salt separation is not handled properly: one is the supernatant Containing ethylenediamine hydrochloride will affect rectification, and the residue of rectification still increases, which increases consumption; second, ethylenediamine hydrochloride contains clear liquid, which is also a loss to clear liquid, and the final product consumption increases
Because it takes a long time to stand still, and the product has to be processed in batches, the liquid cannot be separated continuously, which directly slows down the production efficiency and reduces the output.

Method used

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  • Continuous production reaction device and continuous production reaction method for N-(beta-aminoethyl)-gamma-aminopropyltrimethoxysilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 1. Vaporization of ethylenediamine: pump the raw material ethylenediamine into the ethylenediamine vaporization kettle 6, raise the temperature to 120°C, control the pressure of the kettle to 0.06MPa, open the inlet valve of the tower ethylenediamine vaporization liquid and control it through the flowmeter 10 The flow rate is 150 Kg / h; observe the ethylenediamine reflux in the gas-liquid separator 5, open the reflux valve of the reactor 3; slowly raise the temperature of the reactor 3 to 150°C; control the top temperature to 121°C, and the bottom temperature to 150°C;

[0040] 2. Premix: Pump ethylenediamine and 400 Kg chloropropyltrimethoxysilane into the premix kettle 1 respectively by the pump, and the mixed solution enters the reaction tower 2 from the overflow port 9, and the ethylenediamine and chlorine The pumping rates of propyltrimethoxysilane are 45Kg / h and 100Kg / h respectively;

[0041] 3. Continuous discharge at the bottom of the tank: Observe the reaction l...

Embodiment 2

[0045] 1. Vaporization of ethylenediamine: pump the raw material ethylenediamine into the ethylenediamine vaporization kettle 6, raise the temperature to 120°C, control the pressure of the kettle to 0.07 MPa, open the inlet valve of the tower ethylenediamine vaporization liquid and control it through the flowmeter 10 The flow rate is 145Kg / h; observe the ethylenediamine reflux in the gas-liquid separator 5, open the reflux valve of the reactor 3; slowly raise the temperature of the reactor 3 to 150°C; control the top temperature to 120~122°C, and the bottom temperature to 150~152°C ;

[0046] 2. Premix: Pump ethylenediamine and 400 Kg chloropropyltrimethoxysilane into the premix kettle 1 respectively by the pump, and the mixed solution enters the reaction tower 2 from the overflow port 9, and the ethylenediamine and chlorine The pumping rates of propyltrimethoxysilane are 48Kg / h and 100Kg / h respectively;

[0047] 3. Continuous discharge at the bottom of the tank: Observe the ...

Embodiment 3

[0051] 1. Ethylenediamine vaporization: pump the raw material ethylenediamine into the ethylenediamine vaporization kettle 6, raise the temperature to 120°C, control the pressure of the kettle to 0.08 MPa, open the inlet valve of the tower ethylenediamine vaporization liquid and control it through the flow meter 10 The flow rate is 155 Kg / h; observe the ethylenediamine reflux in the gas-liquid separator 5, open the reflux valve of the reactor 3; slowly raise the temperature of the reactor 3 to 150°C; control the top temperature to 122~123°C, and the bottom temperature to 152~153°C ℃;

[0052] 2. Premix: Pump ethylenediamine and 400 Kg chloropropyltrimethoxysilane into the premix kettle 1 respectively by the pump, and the mixed solution enters the reaction tower 2 from the overflow port 9, and the ethylenediamine and chlorine The pumping rates of propyltrimethoxysilane are 42Kg / h and 100Kg / h respectively;

[0053] 3. Continuous discharge at the bottom of the tank: Observe the ...

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Abstract

The invention discloses a continuous production reaction device and a continuous production reaction method for N-(beta-aminoethyl)-gamma-aminopropyltrimethoxysilane, which belong to the technical field of silane coupling agents. The invention designs a tower-type continuous reaction device, wherein a mixed solution of ethylenediamine and chloropropyl trimethoxysilane, which is sprayed downwards from the top of a reaction tower (2) finishes reaction in a falling process in the reaction tower (2) under the excessive protection of ascending ethylenediamine vaporization liquid, and is automatically pumped into a continuous sedimentation liquid separator by a material transfer pump (12) for automatically controlling the amount of a reaction liquid in a reaction kettle (3) to perform continuous liquid separation; the obtained clear liquid is rectified to obtain N-(beta-aminoethyl)-gamma-aminopropyltrimethoxysilane. The device disclosed by the invention is matched with the process, and continuous reaction and continuous liquid separation can be performed to realize production; the consumption of ethylenediamine is effectively reduced, and both purity and yield are high; the production efficiency is improved while the reaction continuity is ensured, and no ethylenediamine hydrochloride in the separated clear liquid can also be ensured.

Description

technical field [0001] The invention relates to a continuous production reaction device and method of N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane, belonging to the technical field of silane coupling agents. Background technique [0002] Silane coupling agent is a kind of organic compound containing silicon atoms, which can enhance the affinity between organic and inorganic compounds, and can strengthen and improve the physical and chemical properties of composite materials, known as industrial monosodium glutamate. N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane is a very representative silane coupling agent. However, there are still many problems in its actual production and application. [0003] For a long time, the production of N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane is mostly batch reaction, single-pot batch production, long reaction cycle, high energy consumption, low efficiency, and requires high manpower Labor and operation are complicated. In batch produ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 孔德强张宇峰齐峰全杨义会齐泮锋
Owner 淄博市临淄齐泉工贸有限公司
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