阅读说明：本技术 甲胺溴的制备方法 (Preparation method of methylamine bromide ) 是由 凌周驰 于 2018-06-21 设计创作，主要内容包括：本发明提供了化学领域内的甲胺溴的制备方法,包括以下步骤,(1)量取24mL甲胺醇溶液(浓度33wt%)放入冰水浴中搅拌,10min内缓慢将10mL的HBr水溶液(浓度45wt%)滴入甲胺醇溶液中,保持其在冰水浴中反应2h,用鼓风干燥箱干燥上述溶液,干燥温度为60℃,干燥时间为24h,得到淡黄色的粉末；(2)用乙醇将该粉末溶解,加入大量乙醚析出白色的沉淀,将该步骤(溶解-析出)反复进行三次,最后将得到的沉淀60℃真空干燥24h,即得CH3NH3Br粉体；本发明有利于提高电池的热稳定性。(The invention provides a preparation method of methylamine bromide in the chemical field, which comprises the following steps of (1) measuring 24mL of methylamine alcohol solution (with the concentration of 33 wt%) and placing the methylamine alcohol solution into an ice water bath for stirring, slowly dropping 10mL of HBr aqueous solution (with the concentration of 45 wt%) into the methylamine alcohol solution within 10min, keeping the methylamine alcohol solution to react for 2h in the ice water bath, drying the solution by using an air-blast drying oven, wherein the drying temperature is 60 ℃, and the drying time is 24h, so that light yellow powder is obtained; (2) dissolving the powder with ethanol, adding a large amount of diethyl ether to precipitate white precipitate, repeating the step (dissolving-precipitating) for three times, and vacuum drying the obtained precipitate at 60 deg.C for 24 hr to obtain CH3NH3Br powder; the invention is beneficial to improving the thermal stability of the battery.)

1. The preparation method of methylamine bromide is characterized by comprising the following steps:

(1) weighing 24mL of methylamine alcohol solution (with the concentration of 33 wt%) and putting the methylamine alcohol solution into an ice water bath to be stirred, slowly dropping 10mL of HBr aqueous solution (with the concentration of 45 wt%) into the methylamine alcohol solution within 10min, keeping the methylamine alcohol solution to react in the ice water bath for 2h, and drying the solution by using an air-blast drying oven at the drying temperature of 60 ℃ for 24h to obtain light yellow powder;

(2) dissolving the powder with ethanol, adding a large amount of diethyl ether to precipitate white precipitate, repeating the step (dissolving-precipitating) for three times, and vacuum drying the obtained precipitate at 60 deg.C for 24h to obtain CH3NH3Br powder.

Technical Field

The invention belongs to the field of chemistry, and particularly relates to a preparation method of methylamine bromide.

Background

At present, a novel organic-inorganic hybrid perovskite solar cell with high efficiency and low cost is receiving great attention, the photoelectric conversion efficiency of the novel organic-inorganic hybrid perovskite solar cell reaches the level of commercialization preliminarily, but the traditional perovskite material is poor in thermal stability, and organic groups are easy to absorb moisture and decompose, so that the further application of the novel organic-inorganic hybrid perovskite solar cell is limited. In the process of preparing the battery, the material methylamine bromide, methylamine iodide or stannous iodide which needs to be used plays a crucial role in the preparation of the battery.

Disclosure of Invention

Aiming at the defects in the prior art, the invention aims to overcome the defects in the prior art, and provides a preparation method of methylamine bromide, which improves the thermal stability of a battery.

The purpose of the invention is realized as follows: the preparation method of methylamine bromide comprises the following steps:

(1) weighing 24mL of methylamine alcohol solution (with the concentration of 33 wt%) and putting the methylamine alcohol solution into an ice water bath to be stirred, slowly dropping 10mL of HBr aqueous solution (with the concentration of 45 wt%) into the methylamine alcohol solution within 10min, keeping the methylamine alcohol solution to react in the ice water bath for 2h, and drying the solution by using an air-blast drying oven at the drying temperature of 60 ℃ for 24h to obtain light yellow powder;

(2) dissolving the powder with ethanol, adding a large amount of diethyl ether to precipitate white precipitate, repeating the step (dissolving-precipitating) for three times, and vacuum drying the obtained precipitate at 60 deg.C for 24h to obtain CH3NH3Br powder.

Detailed Description

The preparation method of methylamine bromide comprises the following steps:

(1) weighing 24mL of methylamine alcohol solution (with the concentration of 33 wt%) and putting the methylamine alcohol solution into an ice water bath to be stirred, slowly dropping 10mL of HBr aqueous solution (with the concentration of 45 wt%) into the methylamine alcohol solution within 10min, keeping the methylamine alcohol solution to react in the ice water bath for 2h, and drying the solution by using an air-blast drying oven at the drying temperature of 60 ℃ for 24h to obtain light yellow powder;

(2) dissolving the powder with ethanol, adding a large amount of diethyl ether to precipitate white precipitate, repeating the step (dissolving-precipitating) for three times, and vacuum drying the obtained precipitate at 60 deg.C for 24h to obtain CH3NH3Br powder.

The present invention is not limited to the above embodiments, and based on the technical solutions disclosed in the present invention, those skilled in the art can make some substitutions and modifications to some technical features without creative efforts based on the disclosed technical solutions, and these substitutions and modifications are all within the protection scope of the present invention.