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

A technology of boron trifluoride and lithium hydroxide, applied in the directions of boron oxyacids, boron halide compounds, boron oxy compounds, etc., can solve the problems of high consumption of lithium chloride, difficult industrialization, complicated process, etc. The effect of high yield and purity, simple treatment process and easy industrialization

Inactive Publication Date: 2016-06-01
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process is too complicated, the equipment needs to be completely sealed, and the salting out process consumes more lithium chloride, the industrialization is difficult, and the reaction yield is low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Weigh powdered lithium hydroxide crystals (LiOH·H 2 O, analytically pure 90%) 34.95g (0.75mol, boron trifluoride and lithium hydroxide molar ratio is 1:3), add 244.65g water (the mass ratio of lithium hydroxide crystal and water is 1:7) dissolving, A mixture of lithium hydroxide and water is formed.

[0026] (2) Slowly feed 16.95 g (0.25 mol) of boron trifluoride-10 gas at a gas rate of about 5 mL / min while stirring continuously. After the feeding is completed, heat the mixture in an oil bath until the mixture boils, and react for 15 hours.

[0027] (3) Filter the reacted mixture, and wash the solid filter cake with about 100 g of deionized water, and the filtrate is boric acid solution.

[0028] (4) all filtrates carry out ion exchange by 732 type strongly acidic cation exchange resins with the line speed of 3cm / min, after all filtrates pass through ion exchange resins, wash resin with 150g deionized water to reclaim the mother liquor adsorbed by resins.

[0029]...

Embodiment 2

[0031] (1) Weigh powdered lithium hydroxide crystals (LiOH·H 2 O, analytically pure 90%) 46.60g (1mol, boron trifluoride and lithium hydroxide molar ratio is 1:4), add 372.80g water (the mass ratio of lithium hydroxide crystal and water is 1:8) dissolve, form A mixture of lithium hydroxide and water.

[0032] (2) Slowly feed 16.95 g (0.25 mol) of boron trifluoride-10 gas at a gas rate of about 15 mL / min while stirring continuously. After the feeding is completed, heat the mixture in an oil bath until the mixture boils, and react for 20 hours.

[0033] (3) Filter the reacted mixture, and wash the solid filter cake with about 100 g of deionized water, and the filtrate is boric acid solution.

[0034] (4) all filtrates carry out ion exchange by 732 type strongly acidic cation exchange resins with the line speed of 4cm / min, after all filtrates pass through ion exchange resins, wash the resin with 150g deionized water to reclaim the mother liquor adsorbed by the resins.

[0035] ...

Embodiment 3

[0037] (1) Weigh powdered lithium hydroxide crystals (LiOH·H 2 (2, analytically pure 90%) 58.25g (1.25mol, boron trifluoride and lithium hydroxide molar ratio is 1:5), adds 524.25g water (the mass ratio of lithium hydroxide crystal and water is 1:9) dissolving, A mixture of lithium hydroxide and water is formed.

[0038] (2) Slowly feed 16.95 g (0.25 mol) of boron trifluoride-10 gas at a gas rate of about 25 mL / min while stirring continuously. After the feeding is complete, heat the mixture in an oil bath until the mixture boils, and react for 25 hours.

[0039] (3) Filter the reacted mixture, and wash the solid filter cake with about 100 g of deionized water, and the filtrate is boric acid solution.

[0040] (4) all filtrates carry out ion exchange by 732 type strongly acidic cation exchange resins with the line speed of 5cm / min, after all filtrates pass through ion exchange resins, wash the resin with 150g deionized water to reclaim the mother liquor adsorbed by the resins....

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Abstract

The invention relates to a method for preparing boron-10 acid from boron trifluoride-10. The method comprises the following steps: by taking a boron trifluoride-10 gas or a boron trifluoride-10 low-carbon alcohol complex as a raw material, reacting with lithium hydroxide to generate boron-10 acid in a water medium, filtering, performing ion exchange and crystallizing a mixed liquid so as to separate boron-10 solid. The method is performed in water, so that the loss of yield caused by the fact that a middle product boric acid ester generated in a conventional esterification hydrolysis method is hydrolyzed as the system contains water is avoided. The treatment process is simple, industrialization is relatively easy to achieve, the boric acid yield and the purity are relatively high, the boric acid yield is greater than 97%, and the purity is greater than 99%.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis and separation, in particular to a method for preparing boron-10 acid from boron trifluoride-10 gas or boron trifluoride-10 lower alcohol complex. Background technique [0002] Boron B has two stable isotopes, 10 B and 11 B, their abundance in nature is about 19.8% and 80.2%. Boron 10 has a very strong ability to absorb neutrons, and it is widely used in nuclear power, modern industry, military equipment, and medicine. Compared with naturally abundant boric acid, the use of enriched boron-10 acid in nuclear reactors can enhance the capacity of reactors, increase the use of MOX fuel (mixed oxides), increase fuel combustion and cycle times, and reduce fuel consumption per cycle. As a result, waste liquid treatment costs, final required fuel costs, intermediate and final storage costs will be greatly reduced. [0003] At present, the mature boric acid industrial production methods incl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B35/06C01B35/10
CPCC01B35/1045
Inventor 徐姣张卫江张雷
Owner TIANJIN UNIV
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