Preparation method of 2-amino-2-methyl-1-propanol

Abstract

The preparation process of 2-amino-2-methyl-1-propanol includes the following steps: combination reaction of isobutene, chlorine and methyl cyanide in the weight ratio of 1 to 0.5-5 to 1-100 to obtain N-[1-(chloromethyl)propyl] acetyl chloroamine; and subsequent adding water for the first hydrolysis reaction of N-[1-(chloromethyl)propyl] acetyl chloroamine to obtain N-[1-(chloromethyl)propyl] acetamide and the second hydrolysis reaction of N-[1-(chloromethyl)propyl] acetamide to obtain the 2-amino-2-methyl-1-propanol. The preparation process of 2-amino-2-methyl-1-propanol has the beneficial effects of cheap facile material, less steps, low cost, high product purity and being suitable for industrial production.

Description

(1) Technical field

[0001] The present invention relates to the preparation method of 2-amino-2-methyl-1-propanol. (2) Background technology

[0002] 2-Amino-2-methyl-1-propanol, referred to as AMP for short, is a multifunctional additive for the deployment of environmentally friendly latex paints, and can also be used as organic bases and pharmaceutical intermediates for other neutralization and buffering purposes, such as biochemical diagnostic reagents Buffer and Activator. 2-Amino-2-methyl-1-propanol can improve and strengthen many coating components, and enhance the function and performance of other additives. AMP can improve the scrub resistance, hiding power, viscosity stability, color development and so on of the coating. The addition of ammonia to paint in place of ammonia can provide many benefits such as reduced system odor, reduced tank corrosion and flash rust.

[0003] AMP is a primary amine, which mainly acts as a dispersant as follows:

[0004] a) Electro...

Examples

Embodiment 1

[0025] 205.5g of acetonitrile (5mol) is loaded into a 500ml glass tube reactor, the two ports of the reaction bottle are connected to the bottom tube, one is connected to the chlorine gas source, the other is connected to the isobutylene source, and the other is equipped with a thermometer. Put it into an ice-water bath at 0°C, start magnetic stirring, wait until the temperature of the system drops to 0°C, and at the same time, pass 63.8g (0.9mol) of chlorine gas and 50.5g (0.9mol) of isobutene into the reaction flask according to the same ratio. Continue to stir for half an hour after ventilating, then add 11 g of water (0.6 mol) dropwise, stir for half an hour after the dropwise addition, then filter, and vacuum concentrate the filtrate at about 45° C. to obtain 83 g of a slightly yellow concentrate. Dissolve the concentrated solution obtained in the previous step with 41.5 g of ethanol solution with a volume concentration of 95%, heat and stir until it refluxes, then add 29....

Embodiment 2

[0028]205.5g of acetonitrile (5mol) is loaded into a 500ml glass tube reactor, the two ports of the reaction bottle are connected to the bottom tube, one is connected to the chlorine gas source, the other is connected to the isobutylene source, and the other is equipped with a thermometer. into a 30°C water bath, and at the same time 39g (0.55mol) of chlorine and 30.86g (0.55mol) of isobutene were slowly passed into the reaction flask. Continue to stir for half an hour after ventilating, then add 11g of water (0.6mol) dropwise, (hydrolysis reaction exotherm) and stir for half an hour after dropwise addition, then filter, and vacuum concentrate the filtrate at about 45°C to obtain 57g of a yellowish concentrate. Dissolve the concentrated solution obtained in the previous step with 28.5 g of ethanol with a volume concentration of 95%, heat and stir until it refluxes, then add 19.95 g of concentrated hydrochloric acid with a mass concentration of 37%, heat and reflux for about 2 h...

Embodiment 3

[0031] In the glass reactor of 500ml, the acetonitrile (7.23mol) of packing 297g, two ports of reaction flask are connected with inserting bottom pipe, one connects chlorine gas source, one connects isobutylene source, another mouth is equipped with thermometer, puts reaction flask into- In an ice-salt bath at 10°C, 34.8g (0.62mol) of chlorine gas and 46g (0.65mol) of isobutene were slowly passed into the reaction flask at the same time. Continue to stir for half an hour after ventilating, add 15g of water (0.833mol) dropwise, (hydrolysis reaction exotherm) and stir for half an hour after dropwise addition, then filter, and vacuum concentrate the filtrate at about 45°C to obtain 93g of slightly yellow concentrate. Dissolve the concentrated solution obtained in the previous step with 46.5 g of ethanol with a volume concentration of 95%, then heat and stir until reflux, then add 32.55 g of concentrated hydrochloric acid with a mass concentration of 37%, heat to reflux for about 2...

(1) Technical field

[0001] The present invention relates to the preparation method of 2-amino-2-methyl-1-propanol. (2) Background technology

[0002] 2-Amino-2-methyl-1-propanol, referred to as AMP for short, is a multifunctional additive for the deployment of environmentally friendly latex paints, and can also be used as organic bases and pharmaceutical intermediates for other neutralization and buffering purposes, such as biochemical diagnostic reagents Buffer and Activator. 2-Amino-2-methyl-1-propanol can improve and strengthen many coating components, and enhance the function and performance of other additives. AMP can improve the scrub resistance, hiding power, viscosity stability, color development and so on of the coating. The addition of ammonia to paint in place of ammonia can provide many benefits such as reduced system odor, reduced tank corrosion and flash rust.

[0003] AMP is a primary amine, which mainly acts as a dispersant as follows:

[0004] a) Electro...

Examples

Embodiment 1

[0025] 205.5g of acetonitrile (5mol) is loaded into a 500ml glass tube reactor, the two ports of the reaction bottle are connected to the bottom tube, one is connected to the chlorine gas source, the other is connected to the isobutylene source, and the other is equipped with a thermometer. Put it into an ice-water bath at 0°C, start magnetic stirring, wait until the temperature of the system drops to 0°C, and at the same time, pass 63.8g (0.9mol) of chlorine gas and 50.5g (0.9mol) of isobutene into the reaction flask according to the same ratio. Continue to stir for half an hour after ventilating, then add 11 g of water (0.6 mol) dropwise, stir for half an hour after the dropwise addition, then filter, and vacuum concentrate the filtrate at about 45° C. to obtain 83 g of a slightly yellow concentrate. Dissolve the concentrated solution obtained in the previous step with 41.5 g of ethanol solution with a volume concentration of 95%, heat and stir until it refluxes, then add 29....

Embodiment 2

[0028]205.5g of acetonitrile (5mol) is loaded into a 500ml glass tube reactor, the two ports of the reaction bottle are connected to the bottom tube, one is connected to the chlorine gas source, the other is connected to the isobutylene source, and the other is equipped with a thermometer. into a 30°C water bath, and at the same time 39g (0.55mol) of chlorine and 30.86g (0.55mol) of isobutene were slowly passed into the reaction flask. Continue to stir for half an hour after ventilating, then add 11g of water (0.6mol) dropwise, (hydrolysis reaction exotherm) and stir for half an hour after dropwise addition, then filter, and vacuum concentrate the filtrate at about 45°C to obtain 57g of a yellowish concentrate. Dissolve the concentrated solution obtained in the previous step with 28.5 g of ethanol with a volume concentration of 95%, heat and stir until it refluxes, then add 19.95 g of concentrated hydrochloric acid with a mass concentration of 37%, heat and reflux for about 2 h...

Embodiment 3

[0031] In the glass reactor of 500ml, the acetonitrile (7.23mol) of packing 297g, two ports of reaction flask are connected with inserting bottom pipe, one connects chlorine gas source, one connects isobutylene source, another mouth is equipped with thermometer, puts reaction flask into- In an ice-salt bath at 10°C, 34.8g (0.62mol) of chlorine gas and 46g (0.65mol) of isobutene were slowly passed into the reaction flask at the same time. Continue to stir for half an hour after ventilating, add 15g of water (0.833mol) dropwise, (hydrolysis reaction exotherm) and stir for half an hour after dropwise addition, then filter, and vacuum concentrate the filtrate at about 45°C to obtain 93g of slightly yellow concentrate. Dissolve the concentrated solution obtained in the previous step with 46.5 g of ethanol with a volume concentration of 95%, then heat and stir until reflux, then add 32.55 g of concentrated hydrochloric acid with a mass concentration of 37%, heat to reflux for about 2...