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Preparation method of boron-10 acid

A technology of lithium carbonate and boron trifluoride, which is applied in the direction of boron oxide compounds, can solve the problems of high consumption of lithium chloride, low reaction yield, hydrolysis of trimethyl borate, etc., and achieve high yield and purity of boric acid. The effect of simple process and easy industrialization

Inactive Publication Date: 2014-02-19
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method easily causes the hydrolysis of trimethyl borate in the reaction and distillation process, and the salting-out process consumes more lithium chloride, which is not conducive to industrial application, and the reaction yield is low

Method used

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  • Preparation method of boron-10 acid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Weigh powdered lithium carbonate (Li 2 CO 3 ) 55.4g (0.75mol, the ratio of boron trifluoride to lithium carbonate is 1:1.5), add 277.0g water to dissolve, forming a solid-liquid mixture of lithium carbonate and water. After heating the solid-liquid mixture to 40°C, slowly introduce enriched boron trifluoride at a rate of 10ml / min 10 BF 3 33.9 g (0.5 mol), while stirring constantly, boron trifluoride 10 BF 3 The access time is about 2h. After the completion of the boron trifluoride gas introduction, continue to maintain the water bath at 40°C for 25 hours to promote the occurrence of reaction (6).

[0029] After the reaction is completed, the pH of the solution is around 7, and the generated lithium fluoride is a solid precipitate that is very easy to filter. Filtrate at room temperature to separate the lithium fluoride from the mother liquor, and wash the solid filter cake with about 100 g of deionized water, and mix the obtained washing liquor with the mother liq...

Embodiment 2

[0033] Weigh powdered lithium carbonate (Li 2 CO 3 ) 57.3g (0.775mol, the ratio of boron trifluoride to lithium carbonate is 1:1.55), dissolved in 315.2g of water to form a solid-liquid mixture of lithium carbonate and water. After heating the solid-liquid mixture to 60°C, slowly add enriched boron trifluoride at a rate of 25ml / min 10 BF 3 33.9 g (0.5 mol), while stirring constantly, boron trifluoride 10 BF 3 The access time is about 0.8h. After the boron trifluoride gas is introduced, continue to react in a water bath at 60°C for 15 hours to promote the occurrence of reaction (6).

[0034] After the reaction is completed, the pH of the solution is around 7, and the generated lithium fluoride is a solid precipitate that is very easy to filter. Filtrate at room temperature to separate the lithium fluoride from the mother liquor, and wash the solid filter cake with about 100 g of deionized water, and mix the obtained washing liquor with the mother liquor.

[0035] All the...

Embodiment 3

[0038] Weigh powdered lithium carbonate (Li 2 CO 3 ) 59.1g (0.8mol, the ratio of boron trifluoride to lithium carbonate is 1:1.6), add 354.6g of water to dissolve, forming a solid-liquid mixture of lithium carbonate and water. After heating the solid-liquid mixture to 80°C, slowly add enriched boron trifluoride at a rate of 40ml / min 10 BF 3 33.9 g (0.5 mol), while stirring constantly, boron trifluoride 10 BF 3 The access time is about 0.5h. After the completion of the boron trifluoride gas introduction, continue to maintain the water bath at 80°C for 10 hours to promote the occurrence of reaction (6).

[0039] After the reaction is completed, the pH of the solution is around 7, and the generated lithium fluoride is a solid precipitate that is very easy to filter. Filtrate at room temperature to separate the lithium fluoride from the mother liquor, and wash the solid filter cake with about 100 g of deionized water, and mix the obtained washing liquor with the mother liquo...

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Abstract

The invention relates to a preparation method of boron-10 acid. The preparation method of the boron-10 acid comprises the following steps: heating a prepared lithium carbonate-water solid-liquid mixture to be at 40-80 DEG C, inflating boron trifluoride-10 gas into the lithium carbonate-water solid-liquid mixture, stirring so as to uniformly disperse the boron trifluoride-10 into the solid-liquid mixture, and stopping gas inflation when the mol ratio of the boron trifluoride-10 to the lithium carbonate reaches (1: 1.5)-1.6; conducting an reaction for 10-25 hours to generate the boron-10 acid; separating, and performing ion exchange and crystallization to separate out the boron-10 acid solid. The preparation method is carried out in an aqueous system, thus avoiding ester hydrolysis in the process of generating trimethyl borate; the preparation method is simple in process and can be industrialized easily; the boric acid is high in yield and purity, the yield is above 95% and the purity is above 98%.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis and separation, in particular to a method for enriching boron trifluoride 10 BF 3 Process for the preparation of boron-10 acid. 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. Among them, enriched boron-10 acid is a good neutron absorber in the nuclear industry. Compared with boric acid with natural abundance, the use of enriched boron-10 acid in nuclear reactors has two very significant advantages: one is the reactor cooling system 10 The concentration of B will increase; the second is that the overall consumption of boric acid will decrease. According to related research, 10 The benefits brought by the increase of B concentration include the enhancement...

Claims

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Application Information

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IPC IPC(8): C01B35/10
Inventor 徐姣张卫江王楠楠张雷
Owner TIANJIN UNIV
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