Method for preparing powdery 5N high-purity diboron trioxide

A diboron trioxide, high-purity technology, applied in the direction of boron oxides, boron oxide compounds, etc., can solve the problems of incomplete fusion and dehydration of boric acid, large consumption of purified raw materials, unstable quality of boric acid, etc., and achieve high added value of products , short working hours and easy operation

Inactive Publication Date: 2017-08-18
天津市风船化学试剂科技有限公司
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Problems solved by technology

First of all, boric acid undergoes repeated recrystallization to purify raw materials, which consumes a lot of raw materials, low yield, high cost of working hours, and the quality of boric acid is unstable due to the technical level of the operator; secondly, when boric acid is vacuum dehydrated, the temperature control requirements are relatively strict, and dehydration is slow and time-consuming if the temperature is too low , the temperature is slightly higher and the boric acid fusion dehydration is not complete

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  • Method for preparing powdery 5N high-purity diboron trioxide
  • Method for preparing powdery 5N high-purity diboron trioxide

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[0015] A preparation method of powdery 5N high-purity diboron trioxide, the steps of which are:

[0016] (1) Hydrolysis: In a clean 50 ml platinum crucible, add 20 grams of high-purity trimethyl borate, then add 5 grams of pure water dropwise under stirring, continue stirring for 5 minutes after the addition, and the hydrolysis reaction is completed;

[0017] (2) Finished product: move the platinum crucible containing the reactants into a clean quartz tube, put the quartz tube into a tube furnace, and raise the temperature to 50°C for 1 hour to preheat under vacuum conditions, and then raise the temperature to 100°C for 2 hours. Take out the platinum crucible and stir the diboron trioxide in the platinum crucible with a clean polytetrafluoroethylene rod, so that the diboron trioxide is heated more evenly in the crucible, then move the platinum crucible back into the quartz tube, and continue to heat up to 200 °C under vacuum. Keep at ℃ for 2 hours, then cool to room temperatur...

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Abstract

The present invention relates to a preparation method of powdery 5N high-purity boron trioxide, the steps of which are: (1) hydrolysis: in a clean 50 ml platinum crucible, add 20 grams of high-purity trimethyl borate, and then add dropwise under stirring 5 grams of pure water, continue to stir for 5 minutes after adding, and the hydrolysis reaction is completed; (2) finished product: move the platinum crucible containing the reactant into a clean quartz tube, put the quartz tube into a tube furnace, and heat up to Keep at 100°C for 2 hours, take out the platinum crucible and stir the boron trioxide in the platinum crucible with a clean polytetrafluoroethylene rod to make the boron trioxide heated more evenly in the crucible, then move the platinum crucible back into the quartz tube, Continue to raise the temperature to 200°C for 2 hours under vacuum, then cool to room temperature, take out the platinum crucible and store it in a desiccator to obtain the finished powdery high-purity boron trioxide.

Description

technical field [0001] The invention belongs to the field of chemical reagents, in particular to a preparation method of powdery 5N high-purity boron trioxide. Background technique [0002] High-purity boron trioxide generally has two appearances, one is glass-like fragments, and the other is white powder. The 5N high-purity diboron trioxide mentioned in this application refers to a diboron trioxide product with a purity equal to or greater than 99.999%. The preparation of powdery high-purity boron trioxide has been reported in many literatures, and generally speaking the same. It is mainly obtained by repeated recrystallization and purification of boric acid, and then gradually dehydration at a certain temperature and vacuum. Years of practice have shown that there are some problems in the preparation method of this type of powdery high-purity boron trioxide. First of all, boric acid undergoes repeated recrystallization to purify raw materials, which consumes a lot of ra...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/10
CPCC01B35/1027C01P2006/80
Inventor 郝承志孔祥风于明爱
Owner 天津市风船化学试剂科技有限公司
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