Method for preparing 2-amido-1-alkyl alcohol and catalyst preparation method

A technology of alkyl alcohol and catalyst, which is applied in the field of catalyst preparation, can solve problems such as poor catalytic effect, and achieve the effects of low cost, high economic benefit and simple process

Inactive Publication Date: 2009-03-25
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalytic effect is very poor in the continuous reaction of the fixed bed reactor. The catalyst of Co-Cu (90:10) component is selected, and the reaction is carried out at 180 °C in the fixed bed, and the conversion rate of 1,2-butanediol is 50%. , the selectivity of (R, S)-2-aminobutanol is only 8%

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0026] Embodiment 1: the production method of 2-amino-1-propanol:

[0027] 15 grams of an oxidative solid-supported catalytic amination catalyst was packed in a single-tube fixed-bed reactor with a diameter of 15 mm and a length of 1.0 m, and the filling height of the catalyst layer was 0.3 m. The catalyst in the reactor is kept in a hydrogen-facing state with a hydrogen flow passing through it, and the temperature is maintained at 400° C. for 5 hours for reduction to make the catalyst active. After the reduction, the temperature is lowered to 130°C, the hydrogen pressure is raised to 5.0MPa, and the 1,4-dioxane solution of 1,2-propylene glycol with a volume percentage of 30% and liquid ammonia enter the catalytic amine from the upper end through the preheater In the reactor, the flow rate of 1,2-propylene glycol solution is 60 milliliters per hour, and the feed rate of liquid ammonia is 20 milliliters per hour. The catalytic amination reaction product flows out from the lo...

Embodiment 2

[0031] Embodiment 2: the production method of 2-amino-1-butanol:

[0032] 15 grams of an oxidative solid-supported catalytic amination catalyst was packed in a single-tube fixed-bed reactor with a diameter of 15 mm and a length of 1.0 m, and the filling height of the catalyst layer was 0.3 m. The catalyst in the reactor is kept in a hydrogen-facing state with a hydrogen flow passing through it, and the temperature is maintained at 400° C. for 5 hours for reduction to make the catalyst active. Cool down to 160 DEG C after reduction finishes, hydrogen pressure rises to 5.0MPa, 1,4-dioxane and toluene mixed solution (1,4-dioxane Six rings: toluene volume ratio 1:2) and liquid ammonia enter the catalytic amination reactor from the upper end through the preheater, the flow rate of 1,2-butanediol solution is 60 ml per hour, and the feed rate of liquid ammonia is 20 ml per hour . The catalytic amination reaction product flows out from the lower end of the fixed-bed reactor, and t...

Embodiment 3

[0036] Embodiment 3: the production method of 2-amino-1-butanol:

[0037] 15 grams of an oxidative solid-supported catalytic amination catalyst was packed in a single-tube fixed-bed reactor with a diameter of 15 mm and a length of 1.0 m, and the filling height of the catalyst layer was 0.3 m. The catalyst in the reactor is kept in a hydrogen-facing state with a hydrogen flow passing through it, and the temperature is maintained at 400° C. for 5 hours for reduction to make the catalyst active. Cool down to 160 DEG C after reduction finishes, hydrogen pressure rises to 5.0MPa, 1,4-dioxane and toluene mixed solution (1,4-dioxane Six rings: toluene volume ratio 1:2) and liquid ammonia enter the catalytic amination reactor from the upper end through the preheater, the flow rate of 1,2-butanediol solution is 60 ml per hour, and the feed rate of liquid ammonia is 20 ml per hour . The catalytic amination reaction product flows out from the lower end of the fixed-bed reactor, and t...

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Abstract

The invention relates to methods for preparing 2-amino-1-alkyl alcohol and catalyst. The solid catalyst is filled in a single-tube type or double-tube type fixed bed reactor, the temperature in a preheater and the reactor is kept between 130 to 250 DEG C, the hydrogen pressure is kept between 1.0 to 10.0MPa; 1, 2-diol solution with the volume ratio of 10 to 30 percent and ammonia gas are led into the fixed bed reactor from the upper end, the mol ratio between 1, 2-diol and ammonia gas is 1:3 to 1:15, the volume airspeed of the 1, 2-o-diol solution is 30 to 300h<-1>, the obtained liquid is added with methanol for being regulated to homogeneous phase, and transferred into a still after being filtered, and then rectified to obtain the product after the solvent is removed by evaporation. The preparation method of the catalyst adopts the immersion method or the extruding method. The quality of the products of the invention meets the standards of the first class of the industrial products, the content of 2-amino-1-butyl is equal to or more than 99.0 percent; the prepared catalyst for catalysis and amination has long service life; the technology is simple and suitable for continuous industrial production; the cost is low, and the economic benefit is high.

Description

technical field [0001] The invention relates to a method suitable for preparing 2-amino-1-alkanol through selective catalytic dehydrogenation, amination and catalytic hydrogenation with 1,2-vicinal diol as the main raw material and a catalyst preparation method. Background technique [0002] 2-Amino-1-alkyl alcohol compounds are a class of compounds that are widely used, especially as drugs or pharmaceutical intermediates. For example, (S)—(+)—2-aminopropanol is a key intermediate for the synthesis of the fourth-generation quinolone antibacterial drug levofloxacin, and (S)—(+)—2—aminobutanol is An important intermediate for the synthesis of anti-tuberculosis drug ethambutol hydrochloride. [0003] US Patent No. 4151204 uses a hydrogenation catalyst to selectively dehydrogenate the 2-position hydroxyl of a series of 1,2-o-diols in an autoclave, and obtain 2-amino-1-alkyl alcohols after amination reduction. Among them, Co-ThO 2 (99:1) component catalyst is the best for cata...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C213/02C07C215/08C07C215/28B01J23/70
Inventor 闫喜龙李阳王东华陈立功赵广乐张月成
Owner TIANJIN UNIV
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