N,N-Diisopropylethylamine CAS 7087-68-5

A kind of synthetic method of DIPEA, carry out the following steps successively:

Add 101.1g (1.0mol) diisopropylamine, 332.0g (2.0mol) tetraethylammonium chloride, 101.1g ethanol, 60g (1.5mol) sodium hydroxide to the three-necked flask of 1000ml, heat to reflux, and keep The reflux temperature (80°C) was completed after 7 hours of reaction, cooled to room temperature, and the reaction mixture was removed from the solvent on a rotary evaporator, washed with 200 mL*3 of deionized water, and the oil phase washed three times was combined and collected at normal pressure. After rectification, 124.1 g of fractions at 125-127° C. were collected, which was the product DIPEA, the yield was 96.2%, and the purity detected by gas chromatography was 99.5%.

Remarks: The reactant is a solid-liquid mixture after removing low boilers and cooling to room temperature, and becomes a water-oil two-phase after washing.

A preparation method of N,N-diisopropylethylamine, comprises the following steps:

S1. Obtain raw materials and catalysts. The raw materials are ethanol and diisopropylamine, and the catalyst is Mo-Ni-Cu/Al2O3; the composition of the Mo-Ni-Cu/Al2O3 catalyst is: Mo is 8%, Ni is 25%, and Cu is 5% %, the rest is Al2O3

The catalyst preparation steps are:

A1, Al(OH) is prepared into a sodium metaaluminate solution with 40% NaOH, neutralized and precipitated with nitric acid, after aging, filtration, and washing, rolling, drying, and roasting are carried out to obtain a spherical Al2O3 carrier with a diameter of 3mm;

A2. The nitrates of Mo, Ni and Cu are made into a mixed solution in proportion, and the Al2O3 carrier is impregnated;

A3. After drying, put it into a muffle furnace for roasting; the temperature of the muffle furnace is 490℃, and the roasting time is 6h;

After A4 and A3 are calcined, they are cooled. After cooling, they are impregnated with a nitrate mixed solution of Mo, Ni and Cu. After calcination under the same conditions, the content of Mo-Ni- Cu/Al2O3 catalyst;

A5. After loading the catalyst into the reactor, reduce the catalyst with pure hydrogen at a pressure of 0.05MPa, a temperature of 460°C, and a space velocity of 1000h-1 for 24 hours to obtain a finished catalyst;

S2, mix ethanol and diisopropylamine into a mixed solution with a molar ratio of 1.2:1, and use a metering pump to push the mixed solution into the vaporizer of the reaction system, the pressure in the vaporizer is 0.8Mpa, the reaction temperature is 180 ℃, 1000ml catalyst Feed at a rate of 30ml/h;

S3, take the hydrogen in the system with the compressor to vaporize the mixed liquid of heated ethanol and diisopropylamine in the vaporizer, enter the fixed-bed reactor to react, and the obtained material enters the separator after cooling by the condenser;

S4, the liquid phase enters a rectifying tower for rectification and purification, and the obtained ethanol and diisopropylamine are used as raw materials to continue to be mixed into a mixed solution and enter the reaction system to obtain N,N-diisopropylethylamine, diethylamine, isopropanol and triethylamine;

The N,N-diisopropylethylamine, diethylamine, isopropanol and triethylamine obtained in S5 and S4 are respectively purified by rectification;

The reaction water produced by the rectification in S6 and S5 is biochemically treated to discharge standard discharge; the gas phase continues to be circulated in the system with the compressor.

A kind of synthetic method of N,N-diisopropylethylamine, take diisopropylamine and paraldehyde as starting raw material, carry out the following steps successively:

200mL of methanol was added to the 500mL reactor, followed by adding 34.5g of paraacetaldehyde (0.261mol) and 2g of concentrated hydrochloric acid (mass concentration 30%), and under normal pressure 25 ℃, the reaction was stirred for 30 minutes. Then 72 g of diisopropylamine (100 ml, 0.713 mol) and 47 g of sodium cyanoborohydride (0.748 mol) were added, and the reaction was maintained and stirred for 20 minutes.

After the reaction, the reaction solution was decompressed (0.1MPa) to remove methanol, and then 40% (mass concentration) NaOH solution was added to pH to 13. Separate the liquid and take the upper oil phase. Through atmospheric pressure batch rectification, the fraction of 126.8～128 ℃ was collected to obtain N,N-diisopropylethylamine 88.9g, and the yield was 96.5%.

A kind of production method of diisopropylethylamine, carry out the following steps successively:

1) In a tubular reactor with an inner diameter of 8mm and a length-to-diameter ratio of 30:1, use a metering pump to inject DIPA and Et2SO4 according to the ratio, and the raw material ratio n(DIPA):n(Et2SO4)=1.25:1.0 , the pressure is 0.6Mpa, the liquid space velocity of the reaction material is 0.2h-1 (under this liquid space velocity, the reactant stays in the tubular reaction device for 5 hours), and the reaction temperature is 125°C.

2) The material after the reaction is passed through the condenser at the outlet of the tubular reactor, and the amount of cooling water in the condenser is controlled, and the temperature of the material is controlled at 35°C.

3) The condensed material enters the stratifier, and the middle of the stratifier is provided with two feed ports, one feed port is the mixture of the condensed material and the strong alkali aqueous solution with a mass concentration of 20%, and the strong alkali aqueous solution is a continuous feed , its feed flow is automatically adjusted by interlocking with the online PH meter in the stratifier, so that the mixture always maintains the pH value of 13±0.5; the other feed port is petroleum ether, and the feed flow of petroleum ether is the material flow after condensation. 50%, the upper layer obtained after layering is an organic layer, the lower layer is an inorganic layer, and the inorganic layer is the water generated by the reaction and the water contained in sodium hydroxide;

4), the organic layer (organic layer material) of step 3) gained is the 1# rectifying tower that pressure is 0.6Mpa by pumping, the middle feed, the control rectifying tower reflux ratio is 3:1, in the rectifying tower The temperature is 52°C, and the temperature difference between the two temperature measuring points at the top of the tower is 12°C;

5), 1# rectifying tower tower bottom material enters the 2# rectifying tower with a pressure of 0.1Mpa to purify through the differential pressure, and feeds in the middle, and controls the reflux ratio of the rectifying tower to be 3:1, and the temperature in the rectifying tower is 127 ℃ , the temperature difference between the two temperature measuring points at the top of the tower is ≤3 °C for extraction; the product with a boiling range of 126.5 to 127.0 °C is diisopropylethylamine, and the tower kettle material is petroleum ether, which is fed through a pump and fresh petroleum ether. The tube is returned to the stratifier for recycling. The product was chromatographically analyzed w(DIPEA) was 99.86%, and the product yield was 96.55%.