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
View PDF4 Cites 3 Cited by
  • 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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

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...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

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

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Applications(China)
IPC IPC(8): C01B35/10
Inventor 徐姣张卫江王祥梅张雷
Owner TIANJIN UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap