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Method for preparing boron-10 acid with boron-10 trifluoride

A technology of boron trifluoride and methyl acid, which is applied in the field of preparing boron-10 acid, and can solve the problems of difficult separation and large amount of by-products such as calcium fluoride

Inactive Publication Date: 2014-11-19
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method also produces by-products such as sodium chloride and calcium fluoride, which are relatively large in quantity and difficult to separate.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 1 Add 420g of methanol and 60g of calcium metal into the reactor, stir and mix evenly, then heat to 65°C under the control of a water bath. When the calcium metal is completely dissolved and mixed evenly, cool down to room temperature.

[0040] 2 Infuse boron trifluoride-10 gas at a rate of 20mL / min, and stop the aeration when the mass ratio of boron trifluoride-10 to methanol is 6:1.

[0041] 3 After reacting for 24 hours, stop heating and cool down to room temperature. The solid-liquid mixture in the reaction kettle is distilled, and the obtained distillate is a mixture of boron-10 acid methyl ester and methanol.

[0042] 4 Add distilled water to the mixture of methyl borate-10 acid and methanol, the mass ratio of the mixture to water is 1:1.5, carry out hydrolysis, mix well and cool down to room temperature.

[0043] 5 The aqueous solution of boric acid and methanol is subjected to evaporative dehydration, and the dehydration is stopped when the boiling temperature...

Embodiment 2

[0047] 1 Add 480g of methanol and 80g of calcium metal into the reactor, stir and mix evenly, then heat to 70°C under the control of a water bath. When the calcium metal is completely dissolved and mixed evenly, cool down to room temperature.

[0048] 2 Infuse boron trifluoride-10 gas at a rate of 45mL / min, and stop the aeration when the mass ratio of boron trifluoride-10 to methanol is 7:1.

[0049] 3 After reacting for 32 hours, stop heating and cool down to room temperature. The solid-liquid mixture in the reaction kettle is distilled, and the obtained distillate is a mixture of boron-10 acid methyl ester and methanol.

[0050] 4 Add distilled water to the mixture of methyl borate-10 acid and methanol, the mass ratio of the mixture to water is 1:2, carry out hydrolysis, mix well and cool down to room temperature.

[0051]5 The aqueous solution of boric acid and methanol is subjected to evaporative dehydration, and the dehydration is stopped when the boiling temperature of...

Embodiment 3

[0055] 1 Add 560g of methanol and 70g of calcium metal into the reactor, stir and mix evenly, then heat to 50°C under the control of a water bath. When the calcium metal is completely dissolved and mixed evenly, cool down to room temperature.

[0056] 2 Infuse boron trifluoride-10 gas at a rate of 80mL / min, and stop the aeration when the mass ratio of boron trifluoride-10 to methanol is 8:1.

[0057] 3 After reacting for 28 hours, stop heating and cool down to room temperature. The solid-liquid mixture in the reaction kettle is distilled, and the obtained distillate is a mixture of boron-10 acid methyl ester and methanol.

[0058] 4 Add distilled water to the mixture of methyl borate-10 acid and methanol, the mass ratio of the mixture to water is 1:2.5, carry out hydrolysis, mix well and cool down to room temperature.

[0059] 5 The aqueous solution of boric acid and methanol is subjected to evaporative dehydration, and the dehydration is stopped when the boiling temperature...

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PUM

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Abstract

The invention relates to a method for preparing boron-10 acid with boron-10 trifluoride. The method includes following steps: carrying out a reaction between the boron-10 trifluoride and calcium methoxide to obtain trimethyl borate-10 with absolute methanol being a solvent; carrying out a solid-liquid separation process to a reaction product; performing hydrolysis to a liquid mixture to obtain the boron-10 acid. The method is divided into two processes: an esterification process and a hydrolysis process, wherein methanol is used as the solvent and a reaction is carried out between the boron-10 trifluoride and the calcium methoxide to obtain the mixture composed of the trimethyl borate-10 and the methanol in the esterification process. The reaction product is subjected to a distillation process with a distillate being subjected to hydrolysis to obtain a mixed solution composed of boric acid, methanol and water. A condensation process and a crystallization process to obtain the boron-10 acid. A solid by-product obtained after the distillation is single in content, wherein a main component in the solid by-product is calcium fluoride. A yield of the boron-10 acid is more than 95.2% through the method and a purity of the boron-10 acid is more than 99.7% after the boron-10 acid being detected through a detection method in GBT12684-2006.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a method for preparing boron-10 acid with boron trifluoride-10. 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 chemical exchange distillation is mainly used as raw material to produce high-abundance boron trifluoride in the world. boron-10 acid. [0003] There are many industrial production methods of boric acid, such as ammonium bicarbonate method, sodium polyborate method, borax sulfuric acid neutralization method, hydrochloric acid method, well sa...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/10
Inventor 徐姣张卫江王祥梅张雷
Owner TIANJIN UNIV
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