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Synthetic method for spiro quaternary ammonium tetrafluoroborate

A technology of tetrafluoroborate spiro and spirocyclic quaternary ammonium salts, which is applied in the direction of organic chemistry, can solve the problems of difficult industrial production, reduced yield, and instability of spirocyclic quaternary ammonium bases, and achieve cost savings and pollution reduction. Effect

Inactive Publication Date: 2015-01-14
HUNAN ZHENGYUAN ENERGY STORAGE MATERIALS & DEVICE INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this method, the spirocyclic quaternary ammonium base obtained by heating to reflux is unstable in the heating process and is prone to decomposition, resulting in a reduction in yield and affecting product purity, making it difficult to achieve industrial production.

Method used

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  • Synthetic method for spiro quaternary ammonium tetrafluoroborate
  • Synthetic method for spiro quaternary ammonium tetrafluoroborate
  • Synthetic method for spiro quaternary ammonium tetrafluoroborate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Step 2: Dissolve 10.9g of chlorospirocyclic quaternary ammonium salt in 150ml of ethanol in a 250ml reaction kettle, then add 2.7g of sodium hydroxide, and stir at -10°C for 0.5h. Then it was filtered with suction, and the filtrate was evaporated to dryness to obtain 11.1 g (yield rate: 80%) of spirocyclic quaternary ammonium base.

[0021] Step 3: Add 11.1g of spirocyclic quaternary ammonium base, 50g of deionized water, and 11.8g of fluoboric acid (40% aqueous solution) into a 100ml reactor, and stir at 0°C for 0.5h. Then add activated carbon and heat to reflux for 2h. Cool, filter with suction, and evaporate the filtrate to dryness to obtain 10.3 g of the final product (yield: 90%, purity ≥ 99%) spirocyclic ammonium tetrafluoroborate.

[0022]

[0023] Example 2:

[0024]

Embodiment 2

[0026] Step 2: Dissolve 21.5g of chlorospirocyclic quaternary ammonium salt in 150ml of ethanol in a 250ml reactor, then add 8.0g of sodium hydroxide, and stir at 20°C for 3h. Then it was filtered with suction, and the filtrate was evaporated to dryness to obtain 26.8 g (yield rate: 98%) of spirocyclic quaternary ammonium base.

[0027] Step 3: Add 26.8g of spirocyclic quaternary ammonium base, 50g of deionized water, and 42.8g of fluoboric acid (40% aqueous solution) into a 100ml reactor, and stir at 15°C for 3h. . Then add activated carbon and heat to reflux for 2h. Cool, filter with suction, and evaporate the filtrate to dryness to obtain 27.2 g (yield: 98%, purity ≥ 99%) of the final product, spirocyclic ammonium tetrafluoroborate.

[0028] Example 3:

[0029]

Embodiment 3

[0031] Step 2: Dissolve 19.2g of chlorospirocyclic quaternary ammonium salt in 150ml of ethanol in a 250ml reactor, then add 9.5g of sodium hydroxide, and stir at 60°C for 5h. Then it was filtered with suction, and the filtrate was evaporated to dryness to obtain 20.1 g (yield rate: 82%) of spirocyclic quaternary ammonium base.

[0032] Step 3: Add 20.1g of spirocyclic quaternary ammonium base, 50g of deionized water, and 42.8g of fluoboric acid (40% aqueous solution) into a 100ml reactor, and stir at 30°C for 5h. . Then add activated carbon and heat to reflux for 2h. Cool, filter with suction, and evaporate the filtrate to dryness to obtain 19.1 g (yield: 92%, purity ≥ 99%) of the final product, spirocyclic ammonium tetrafluoroborate.

[0033] Example 4:

[0034]

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Abstract

The invention discloses a rapid simple efficient method for synthesizing a high-purity spiro quaternary ammonium tetrafluoroborate. The method comprises the following steps: step 1, adding a carbonate, 1,4-dichlorobutane, tetrahydro pyrrole, sodium iodide and a methanol solvent into a reaction kettle to perform reaction, so as to obtain a chloro spiro quaternary ammonium salt; step 2, dissolving the chloro spiro quaternary ammonium salt into ethanol in a reaction kettle, then adding sodium hydroxide to perform ion exchange, and evaporating the solvent to finally obtain a spiro quaternary ammonium base; and step 3, dissolving the spiro quaternary ammonium base into deionized water in a reaction kettle, then adding fluorboric acid for neutralization, then adding active carbon for refluxing decoloring, and then performing pumping filtration, evaporation condensation and drying, so as to finally obtain the high-purity spiro quaternary ammonium tetrafluoroborate with extremely low water content. The step 1 also can be performed as following: adding the raw materials into a ball milling tank for ball milling reaction, so as to obtain the chloro spiro quaternary ammonium salt. The provided synthetic method for the spiro quaternary ammonium tetrafluoroborate is relatively suitable for industrial large-scale production.

Description

technical field [0001] The invention relates to a chemical synthesis method of spirocyclic quaternary ammonium tetrafluoroborate, belonging to the field of new materials. Background technique [0002] Due to the increasing shortage of oil resources and the increasingly serious environmental pollution caused by the exhaust emissions of internal combustion engines burning oil (especially in large and medium-sized cities), people are studying new energy devices to replace internal combustion engines. Research and development of hybrid power, fuel cells, and chemical battery products and applications have been carried out, and certain results have been achieved. However, due to their inherent shortcomings such as short service life, poor temperature characteristics, environmental pollution by chemical batteries, complex systems, and high cost, there has been no good solution. Supercapacitors are widely used in hybrid electric vehicles and various electric energy recovery system...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D487/10
CPCC07D487/10
Inventor 李荐周宏明刘明
Owner HUNAN ZHENGYUAN ENERGY STORAGE MATERIALS & DEVICE INST
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