Preparation method of diethyl aluminum hydride

A technology of diethylaluminum hydride and diethylaluminum chloride, applied in the field of preparation of alkylaluminum hydride, can solve the problems of low synthesis yield, expensive raw materials and unsuitable purchase, and achieves high purity, good use value, reduction strong effect

Inactive Publication Date: 2015-07-15
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the problems of the traditional preparation of diethylaluminum hydride that raw materials are expensi...

Method used

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  • Preparation method of diethyl aluminum hydride
  • Preparation method of diethyl aluminum hydride
  • Preparation method of diethyl aluminum hydride

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specific Embodiment approach 1

[0021] Specific Embodiment 1: This embodiment provides a method for preparing diethylaluminum hydride. The following steps are all carried out under strict anhydrous and oxygen-free conditions. The specific steps are as follows:

[0022] (1) Add 100ml of Et to a 500ml three-neck round bottom flask 2 AlCl, slowly add 180ml of toluene under stirring condition, continue stirring for 30min;

[0023] (2) Slowly add 41g LiAlH when the temperature does not exceed 60°C 4 , after fully mixing, the oil bath controls the reaction temperature at 100°C for 4 hours;

[0024] (3) Cool to room temperature after the reaction, and then remove the solvent toluene by rotary evaporation at 55°C, and then filter to remove the gray solid substance;

[0025] (4) The filtrate was distilled under reduced pressure again, and the fraction was collected at 102°C to obtain a colorless transparent liquid.

[0026] The raw material Et2AlCl used in the present embodiment 1 H NMR as figure 1 As shown, the...

specific Embodiment approach 2

[0027] Specific embodiment two: This embodiment provides a method for preparing diethylaluminum hydride, the following steps are all carried out under anaerobic conditions, and the specific steps are as follows:

[0028] (1) Add 100ml of Et to a 500ml three-neck round bottom flask 2 AlCl, slowly add 180ml of benzene under stirring condition, continue stirring for 30min;

[0029] (2) Slowly add 41g LiAlH when the temperature does not exceed 60°C 4 , after fully mixing, the oil bath controls the reaction temperature at 100°C for 4 hours;

[0030] (3) After the reaction is completed, cool to room temperature, then distill off the solvent under reduced pressure at 55°C, and then filter to remove the gray solid substance;

[0031] (4) The filtrate was distilled under reduced pressure again, and the fraction was collected at 102°C to obtain a colorless transparent liquid.

[0032] Raw material Et used in this embodiment 2 AlCl 1 H NMR as figure 1 As shown, the prepared Et 2 T...

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Abstract

The invention discloses a preparation method of diethyl aluminum hydride. The preparation method comprises the following steps: (1) adding 80-120ml of diethyl aluminum hydride (Et2AlCl) to 500ml of three-mouth round-bottom flask, slowly adding 160-200ml of solvent under a stirring condition, and then further stirring for 20-40 minutes; (2) controlling the temperature to be not greater than 60 DEG C, slowly adding 40-42g of LiAlH4, fully mixing, heating in an oil bath, controlling the reaction temperature to be 100-110 DEG C and reacting for 3-5 hours; (3) after reacting, cooling, carrying out rotary evaporation at 50-60 DEG C until no liquid is evaporated, and then filtering to remove grey solid substances; and (4) carrying out reduced pressure distillation on filtrate, and collecting fractions at 102 DEG C, thereby obtaining a colorless transparent liquid as a target product. The diethyl aluminum hydride prepared by the method is high in purity and high in yield and has great potential industrial value.

Description

technical field [0001] The present invention relates to a kind of preparation method of alkyl aluminum hydride, in particular to a kind of diethyl aluminum hydride (Et 2 AlH) preparation method. Background technique [0002] Alkyl aluminum is a large class of metal aluminum organic compounds formed by the direct combination of alkyl and aluminum, the general formula is AlR 3 , RnAlX 3-n or R 3 Al 2 x 2 (R is an alkyl group, X is a halo group, n=1, 2, 3). Alkyl aluminum can be used as ignition fuel in high-energy fuels, and the compound formed by linking with halo group is called alkylaluminium halide, which is a representative organoaluminum compound and can be used in Ziegler-Natta (Ziegler-Natta) Natta) reaction catalyst, organic synthesis intermediate. However, these alkylaluminums are easily oxidized and hydrolyzed in the air, and are naturally irritating and can cause skin and mucous membrane ulcers in the air. The alkylaluminum hydride is prepared by reducing t...

Claims

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Application Information

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IPC IPC(8): C07F5/06
CPCC07F5/065
Inventor 杨玉林高跃岳王华威范瑞清朱朝阳
Owner HARBIN INST OF TECH
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