Preparation method and device of trimethyl borate-10

Abstract

The invention relates to a preparation method and device of trimethyl borate-10. The preparation method comprises the steps of adding reactants into a reaction kettle, taking methanol as a solvent, and stirring for reacting for 30-45h; setting the reaction temperature to be 50-70 DEG C, and performing esterification reaction to generate trimethyl borate-10; performing azeotropic distillation on an esterification reaction product, and setting the temperature to be 70-90 DEG C; collecting a fraction at the temperature of 50-60 DEG C, then continuously heating, and recovering methanol; adding the fraction collected in azeotropic distillation into an extraction and distillation tower kettle; heating the tower kettle, controlling the heating voltage to be 120-150V and controlling the total reflux time to be 20-30min according to the total reflux speed to meet a heat load of a system, adding an extraction agent N, N-dimethylformamide or dimethyl sulfoxide or a mixed extraction agent into a high-level tank at the tower top of a distillation tower, and collecting trimethyl borate at the temperature of 67-68.5 DEG C at the tower top. The operation of the method is stable, and the purity of trimethyl borate-10 obtained by the method can be above 99%.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a method and equipment for preparing trimethyl boron-10 acid from boron trifluoride-10 and the application of trimethyl boron-10 acid. Background technique [0002] Boron has two stable isotopes, 10 B and 11 B, Their relative abundances are 19.78% and 80.22%, respectively. Boron 10 has a very strong ability to absorb neutrons, and it is widely used in nuclear power, modern industry, military equipment, and medicine. in order to get 10 Boron isotope with higher B content, and make it have a production-scale device. At present, boron trifluoride containing high-abundance boron-10 isotope produced by the chemical exchange method of rectification tower is mainly used as raw material to produce boron-10 in the world. 10 boric acid with higher purity and direct application. [0003] Trimethyl borate in natural abundance can be used as a solvent, dehydrating a...

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Problems solved by technology

[0006] Wu Changmei, Liaoning Research Institute of Chemical Industry, published an article in 2000, using industrial boron trifluoride-10 ether complex as raw material, using calcium chloride as defluorinating agent, using methanol as the medium for reaction, and adding quantitative catalyst to prepare boron-10 The process of acid produces trimethyl boron-10 acid, but the loss of trimethyl borate during the distillation process is relatively large

[0007] Patent CN102774846A provides a boron trifluoride-anisole complex as the main raw material in the process of producing boron-10 acid, which also needs to go through the step of generating trimethyl boron-10 acid. The process of this method is relatively complicated. The equipment requires very good airtightness, and the side reaction products are various mixtures, which are difficult to single-handle

[0008] In the literature, the separation of trimethyl borate and methanol adopts the method of salting out or the method of extractive distillation. Shi Xinyu used the salting out method to separate trimethyl borate and methanol azeotrope in 1995. Lithium chloride, zinc chloride and calcium chloride are used as comparative research methods, but although the process of salting out in industrial production is relatively short, the salt cycle is relatively inconvenient; Bai Liying and others from Liaoning Chemical Industry Research Institute studied the separation of trimethyl borate The method adopts the method of extraction and rectification. The extraction agent is N,N-dimethylformamide, and the purity can reach 98%. In order to obtain a higher purity, the separation effect of other extraction agents can be considered

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