CN105837616A

CN105837616A - Method for preparing N,N-diethyl-3-aminopropyl trimethoxy silane

Info

Publication number: CN105837616A
Application number: CN201610332357.9A
Authority: CN
Inventors: 车鈜; 席亚男; 钟奇军
Original assignee: Nanjing Chemical Co Ltd Of Strategy Software Systems Co Ltd (sss)
Current assignee: Nanjing Chemical Co Ltd Of Strategy Software Systems Co Ltd (sss)
Priority date: 2016-05-19
Filing date: 2016-05-19
Publication date: 2016-08-10

Abstract

The invention discloses a method for preparing N,N-diethyl-3-aminopropyl trimethoxy silane. The method comprises the following steps: in the presence of a high boiling point solvent N,N-diethyl formamide, heating to be 110-130 DEG C to enable diethylamine and 3-chloropropy trimethoxy silane to react at normal pressure, performing refluxing reaction for 6-10 hours, cooling to be 20 DEG C, filtering off solid diethylamine hydrochloride, and leaching once by using the solvent N,N-diethyl formamide; performing vacuum concentration on the filtrate, recycling the solvent N,N-diethyl formamide, and rectifying so as to obtain a 99% product; dissolving the solid diethylamine hydrochloride in a solution, dripping into a sodium hydroxide solution, distilling so as to recycle diethylamine, absorbing the gas generated in the reaction and aftertreatment process by using the solvent N,N-diethyl formamide, and reusing in the production process. By adopting the method, not only is the reaction time great shortened, but also the waste gas generated when the low boiling point raw material diethylamine is used can be effectively treated, so that the environment can be protected, and the content of the product is equal to or higher than 99%.

Description

The preparation method of N, N-diethyl-3-aminopropyl trimethoxysilane

Technical field

The present invention relates to the preparation method of N, N-diethyl-3-aminopropyl trimethoxysilane.

Background technology

Organo silane coupling agent, as a kind of new material, is increasingly widely used in construction material, weaving, in coating, in fiberglass surfacing processes, improve bond properties, in filler processes, improve dispersiveness and the bonding force of resin, it is additionally operable to sealant, coating and bonding agent.Demand both domestic and external just steps up.

N, N-dimethyl-3-aminopropyl trimethoxysilane must have been gone abroad as a kind of silane coupler therein the accreditation of most of client, it is therefore desirable to strengthen the development of this product and production, the method purity of existing this product of production is relatively low and the reaction time longer typically need to have a strong impact on industrialized production at about 20 hours.

Summary of the invention

It is an object of the invention to overcome above deficiency; provide N; the preparation method of N-diethyl-3-aminopropyl trimethoxysilane; the present invention is greatly shortened in the reaction time; and making low boiling raw material diethylamine (normal pressure 55 DEG C) waste gas in use obtain effective governance and protection environment, product content is more than 99%.

The technical scheme that the present invention provides is:

A kind of preparation method of N, N-diethyl-3-aminopropyl trimethoxysilane, the method comprises the following steps:

A) N is put in a kettle., N-DEF and diethylamine, at room temperature react after stirring 1 hour, dropping liquid 3-r-chloropropyl trimethoxyl silane, start after dripping slowly to heat up, finally being warmed up to backflow and be maintained at 115 DEG C of reactions 6 hours, in course of reaction, sampling terminates reaction when the material content of 3-r-chloropropyl trimethoxyl silane being detected less than 0.5%；

B) after the reaction of step a) terminates, take out product when reactor is cooled to 20 DEG C and be filtrated to get diethylamine hydrochloride, the diethylamine hydrochloride solvent N that will obtain, N-DEF rinses, the filtrate of rinsing is merged concentration and recovery diethylamine and solvent N, N-DEF, and rectifying obtains N, N-diethyl-3-aminopropyl trimethoxysilane；

C) it is dissolved in water is made into 50% aqueous solution by step b) reacts remaining diethylamine hydrochloride solid, drip in 30% sodium hydrate aqueous solution and heat temperature raising, use collection tower to go out diethylamine in gas phase temperature rectifying at 55 DEG C-60 DEG C and recycle course of reaction.

Preferably, in the preparation method of described N, N-diethyl-3-aminopropyl trimethoxysilane, in described step a), N, N-DEF is 1:2-5 with the mol ratio of the input of diethylamine.

Preferably, in the preparation method of described N, N-diethyl-3-aminopropyl trimethoxysilane, described step a) vacuumizes during stirring in making reactor and keep negative pressure.

Preferably, in the preparation method of described N, N-diethyl-3-aminopropyl trimethoxysilane, open tail gas absorption pump during the reaction of described step a) and protect with nitrogen.

The invention has the beneficial effects as follows that the present invention is greatly shortened in the reaction time, and make low boiling raw material diethylamine (normal pressure 55 DEG C) waste gas in use obtain effective governance and protection environment, product content is more than 99%.Detailed description of the invention

Below in conjunction with embodiment, the invention will be further described, but should not limit the scope of the invention with this.

C) it is dissolved in water is made into 50% aqueous solution by step b) reacts remaining diethylamine hydrochloride solid, drip in 30% sodium hydrate aqueous solution and heat temperature raising, use collection tower to go out diethylamine in gas phase temperature rectifying at 55 DEG C-60 DEG C and recycle course of reaction.Wherein N in step a), N-DEF is 1:2-5 with the mol ratio of the input of diethylamine, vacuumizes in making reactor and keep negative pressure during stirring, opens tail gas absorption pump and protect with nitrogen during reaction.

Example one

The N of 1200Kg is put in the reactor of 3000L; N-DEF (DEF) and diethylamine 450Kg(6.15Kmol) also open tail gas absorption N simultaneously; N-DEF (DEF) pump is protected with nitrogen; within after reactor stirs at room temperature about 1 hour, drip 600Kg(3.03Kmol) 3-r-chloropropyl trimethoxyl silane; dripping and begin to warm to backflow afterwards and be maintained at 115 DEG C react 6 hours, sampling makes raw material 3-r-chloropropyl trimethoxyl silane terminate less than 0.5% reaction.

Cooling makes temperature in the kettle to 20 DEG C blowing leach diethylamine hydrochloride, and rinsing solid with solvent N, the N-DEF of 100Kg, filtrate merges concentration and recovery diethylamine and solvent N, N-DEF (DEF) rectifying obtain 620Kg product, content 99.5%.

Diethylamine hydrochloride solid is dissolved in water and is made into 50% aqueous solution, is added drop-wise in 30% sodium hydrate aqueous solution of 500Kg and heat temperature raising collection top gaseous phase temperature is that qualified diethylamine is back in course of reaction at 55 DEG C of-60 DEG C of fractions.

Example two

The N of 1200Kg is put in the reactor of 3000L; N-DEF (DEF) and diethylamine 550Kg(7.52Kmol) also open tail gas absorption N simultaneously; N-DEF (DEF) pump is protected with nitrogen; within after reactor stirs at room temperature about 1 hour, drip 600Kg(3.03Kmol) 3-r-chloropropyl trimethoxyl silane; dripping and begin to warm to backflow afterwards and be maintained at 125 DEG C react 6 hours, sampling makes raw material 3-r-chloropropyl trimethoxyl silane terminate less than 0.5% reaction.

Cooling makes temperature in the kettle to 20 DEG C blowing leach diethylamine hydrochloride, and with solvent N, the N-DEF of 100Kg

Rinsing solid, filtrate merges concentration and recovery diethylamine and solvent N, and N-DEF (DEF) rectifying obtain 635Kg product, content 99.2%.

Example three

The N of 1200Kg is put in the reactor of 3000L; N-DEF (DEF) and diethylamine 665Kg(9.09Kmol) also open tail gas absorption N simultaneously; N-DEF (DEF) pump is protected with nitrogen; within after reactor stirs at room temperature about 1 hour, drip 600Kg(3.03Kmol) 3-r-chloropropyl trimethoxyl silane; dripping and begin to warm to backflow afterwards and be maintained at 110 DEG C react 4 hours, sampling makes raw material 3-r-chloropropyl trimethoxyl silane terminate less than 0.5% reaction.

Rinsing solid, filtrate merges concentration and recovery diethylamine and solvent N, and N-DEF (DEF) rectifying obtain 656Kg product, content 99.7%.

Although the embodiment of invention is disclosed as above, but it is not restricted in specification and embodiment listed utilization, it can be applied to various applicable the field of the invention completely, for those skilled in the art, it is easily achieved other amendment, therefore, under the universal limited without departing substantially from claim and equivalency range, the present invention is not limited to specific details and shown here as the proportioning example with description.

Claims

1. the preparation method of a N, N-diethyl-3-aminopropyl trimethoxysilane, it is characterised in that the method comprises the following steps:

2. the preparation method of N, N-diethyl-3-aminopropyl trimethoxysilane as claimed in claim 1, it is characterised in that in described step a), N, N-DEF is 1:2-5 with the mol ratio of the input of diethylamine.

3. the preparation method of N, N-diethyl-3-aminopropyl trimethoxysilane as claimed in claim 1, it is characterised in that vacuumize during stirring in described step a) in making reactor and keep negative pressure.

4. the preparation method of N, N-diethyl-3-aminopropyl trimethoxysilane as claimed in claim 1, it is characterised in that open tail gas absorption pump during the reaction of described step a) and protect with nitrogen.