Preparation method of fluorozirconate

A technology of fluorozirconate and pentafluorozirconate, which is applied in electrical components, electrolytic capacitors, capacitors, etc., can solve the problems of unachieved, and achieve the effects of high yield, easy purification and cheap raw materials

Active Publication Date: 2016-11-16
NANJING YUANSHU MEDICAL TECH CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This invention provides an effective way to produce chemicals that are costly but can be easily obtained from natural sources or produced by other methods without causing harmful environmental impact. It also allows for efficient separation processes with minimal contaminants during processing.

Problems solved by technology

This patented technical problem addressed by this patents relates to developing novel types of chemical substances that are more effective at storing or releasing electrical charges than current materials such as TEAs/BFO4.

Method used

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  • Preparation method of fluorozirconate
  • Preparation method of fluorozirconate
  • Preparation method of fluorozirconate

Examples

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Effect test

Embodiment 1

[0024] Embodiment 1 A kind of preparation method of fluorozirconate

[0025] 1) Weigh 7.1g of pyrrolidine and 14g of potassium carbonate, dissolve it in 1000mL of acetone, add it to a three-neck flask, adjust the temperature to 15-20°C, and slowly add 10mL of 1-bromo-3-chloropropane dropwise for 5 minutes , the temperature of the whole dropwise addition reaction was kept at 15-20°C. After the dropwise addition was completed, the temperature was raised to 35°C, and the reaction was continued for 24 hours. After the reaction was completed, the reaction solution was directly filtered, and the organic solvent was distilled off under reduced pressure to obtain 13.8g 1-(3-chloro Propane) pyrrole, the yield (calculated as pyrrolidine) is 94%.

[0026] 2) Weigh 13.8g of 1-(3-chloropropane)pyrrolidine and dissolve it in 850mL of acetonitrile, then add it into a three-neck flask, the temperature rises to 60-65°C, the whole reaction temperature is kept at 60°C-65°C, and the reaction is c...

Embodiment 2

[0029] 1) Weigh 7.1g of pyrrolidine and 14g of potassium carbonate, dissolve it in 1000mL of acetone, add it to a three-neck flask, adjust the temperature to 15°C, and slowly add 13.4mL of 1,4-diiodobutane dropwise. At 15°C to 20°C, after the addition, the temperature was raised to 35°C, and the reaction was continued for 24 hours. After the reaction was completed, the reaction solution was directly filtered, and the organic solvent was distilled under reduced pressure to obtain 24.5g of 1-(4-iodobutane)pyrrole. The yield ( Based on pyrrolidine) was 97%.

[0030] 2) Weigh 24.5g of 1-(4-iodobutane)pyrrole and dissolve it in 850mL of acetonitrile, add it into a three-neck flask, raise the temperature to 60°C, keep the whole reaction temperature at 60°C-65°C, and continue the reaction for 16 hours. After the reaction is completed, the temperature is down to room temperature, and the reaction solution is directly filtered, and the organic solvent is distilled under reduced pressur...

Embodiment 3

[0033] 1) Weigh 7.1g of pyrrolidine and 10.8g of sodium carbonate and dissolve them in 1000mL of acetone, add them to a three-neck flask, adjust the temperature to 15°C and slowly add 13.8mL of 1,5-dibromopentane, and keep the entire reaction temperature at 15°C ℃~20℃, after the addition is completed, the temperature is raised to 35℃, and the reaction is continued for 24h. After the reaction is completed, the reaction solution is directly filtered, and the organic solvent is distilled under reduced pressure to obtain 21.5g of 1-(5-bromopentane)pyrrole. The yield (calculated as pyrrolidine Count) is 98%.

[0034] 2) Weigh 24.5g of 1-(5-bromopentane)pyrrole and dissolve it in 850mL of acetonitrile, add it into a three-neck flask, raise the temperature to 60°C, keep the whole reaction temperature at 60°C~65°C, continue the reaction for 16h, wait After completion of the reaction, the temperature is down to room temperature, and the reaction solution is directly filtered, and the o...

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Abstract

The invention discloses a preparation method of fluorozirconate. The preparation method comprises the following steps of A, enabling a nitrogen-containing heterocyclic compound and halogenating alkane to be subjected to a reaction in an organic solvent under alkaline conditions, so as to obtain heterocyclic amine based alkane halogen; B, enabling the heterocyclic amine based alkane halogen obtained in the step A to be dissolved in an organic solvent, and performing heating so as to obtain nitrogen spirane halide salt; and C, enabling nitrogen spirane halide salt which is obtained in the step B and as shown in a formula iv to be dissolved in the organic solvent, and performing ion exchange on the nitrogen spirane halide salt dissolved in the organic solvent with pentafluoro sodium zirconate or pentafluoro zirconic acid so as to obtain nitrogen spirane pentafluoro zirconic acid as shown in a formula vi, or performing ion exchange on the nitrogen spirane halide salt dissolved in the organic solvent with hexafluorozirconic acid or hexafluorozirconic acid sodium so as to obtain dinitrogen spirane hexafluorozirconic acid salt as shown in a formula vi. According to the method disclosed by the invention, raw materials are cheap and easy to obtain, reaction steps are simple, the yield is high, pollution is hardly generated, strict and dangerous reaction conditions are not used, products are easy to refine, and the method disclosed by the invention is suitable for national mass production.

Description

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Claims

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Application Information

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Owner NANJING YUANSHU MEDICAL TECH CO LTD
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