A kind of preparation method of stable isotope reagent sodium borodeuteride

Abstract

The invention relates to a preparation method for a stable isotope reagent sodium borodeuteride. The method comprises the following steps: (1) pre-treating a boron-containing substance and quartz sand for complete dehydration, loading the boron-containing substance and the quartz sand in a sealed reaction kettle, adding a pretreated active metal from which a surface oxide layer is removed, connecting a deuterium bag to the sealed reaction kettle, performing heating and stirring, and sucking deuterium for reaction until the volume of the deuterium bag is kept unchanged; (2) after reaction is ended, performing cooling to obtain a sodium borodeuteride product. Compared with the prior art, the preparation method has the advantages that a preparation process route is simple, a preparation condition is mild, less waste gas, wastewater and industrial residues are generated by reaction, and moreover, the prepared sodium borodeuteride has purity capable of reaching 99 percent or above, abundance of 99.9atom% or above and the like.

Description

technical field [0001] The invention relates to a preparation method of a stable isotope reagent sodium borodeuteride, in particular to a preparation method of a high-purity stable isotope reagent sodium borodeuteride. Background technique [0002] Sodium borohydride (NaBH 4 ) also known as sodium borohydride, white to off-white fine crystalline powder or block, decomposes at 300°C in dry air, 400°C in vacuum, 503°C in nitrogen, and 512°C in hydrogen. It has strong hygroscopicity and strong of restoration. Sodium borohydride is widely used in organic chemistry and inorganic chemistry. It is called "universal reducing agent" in organic synthesis and can be used as reducing agent for aldehydes, ketones and acid chlorides, foaming agent for plastics, manufacturing Hydrogenating agent for dihydrostreptomycin, intermediate for manufacturing potassium borohydride, raw material for synthesizing borane, and used in paper industry and mercury-containing sewage treatment agent and o...

AI Technical Summary

Problems solved by technology

[0004] At present, the preparation method of isotope-labeled sodium borodeuteride abroad is trimethylaminopropane in D 2 SO 4 with D 2 Stirred under O condition for 24h, separated D 2 O, repeat the same operation more than 9 times, use D for the ether phase 2 O washed, dried with anhydrous sodium carbonate, and evaporated to prepare trimethylaminoborane-D 3 , by trimethylaminoborane-D 3 Mix with alcohol sodium methoxide and diethylene glycol dimethyl ether, stir under nitrogen atmosphere, and release trimethylamine through condensation recovery, isopropylamine extraction and other operations. This method has a long route and consumes a large amount of deuterated reagent D 2 SO 4 with D 2 O, produce a large number of pollutants and other disadvantages

There have been synthetic literature and patents on sodium borohydride in China, but no literature on the preparation of isotope sodium borodeuteride has been seen. The more mature method, such as the Nankai University patent literature, mentions the use of improved borax method to prepare sodium borohydride, but because the preparation of this method is common Sodium borohydride, so the use of hydrogen is an excessive reaction. After the reactor is fed, vacuumize, fill with hydrogen, and then vacuumize and fill with hydrogen. Repeat the above operation until the received tail gas is ignited without detonation.

If this method is adopted, the amount of deuterium used will be very large, and it is not suitable for the preparation of deuterated reagents.