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Phosphate ionic liquids as well as synthetic method and application thereof

A technology of phosphate esters and ionic liquids, which is applied in chemical instruments and methods, liquid solution solvent extraction, compounds of group 5/15 elements of the periodic table, etc., can solve the problem of strong corrosion of extraction equipment and high concentration of tributyl phosphate , organic phase dissolution loss and other problems, to achieve the effect of favorable promotion and industrial production, feasible process, and reduced viscosity

Inactive Publication Date: 2018-04-24
青海柴达木兴华锂盐有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The main problems are that the concentration of tributyl phosphate in the system is high, which is extremely corrosive to the extraction equipment, and the solubility of brine in the organic phase is large, and the dissolution loss of the organic phase is large

Method used

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  • Phosphate ionic liquids as well as synthetic method and application thereof
  • Phosphate ionic liquids as well as synthetic method and application thereof
  • Phosphate ionic liquids as well as synthetic method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Synthesis of dibutyl (2-(trimethyl-amino) ethyl) phosphonic acid hexafluorophosphate, the structural formula is as follows:

[0033]

[0034] Add 58.28g of dibutyl phosphite, 23.25g of trichloroisocyanuric acid and 270mL of acetonitrile into a 500mL three-necked flask, place the system on a constant temperature stirrer, react at room temperature, and stop the reaction within 15 minutes.

[0035] After suction filtration, the filter cake was washed three times with 50 mL of acetonitrile to obtain 65.12 g of the product with a yield of 95%.

[0036] Add 57.08g of phosphorus oxychloride, 180mL of 1,2-dichloroethane and 25.25g of triethylamine into a 500mL three-necked flask. The system is lowered to below zero in the ice-salt bath, and 60ml containing 24.38g of N,N - 1,2-dichloroethane solution of dimethylethylenediamine, the rate of addition is controlled to ensure that the reaction temperature is maintained within 10°C. After the dropwise addition, the reaction syste...

Embodiment 2

[0042] Synthesis of diethyl (2-(trimethyl-amino)butyl) phosphonic acid hexafluorophosphate, the structural formula is as follows:

[0043]

[0044] Add 41.45g of diethyl phosphite, 23.25g of trichloroisocyanuric acid and 240mL of acetonitrile into a 500mL three-neck flask, place the system on a constant temperature stirrer, react at room temperature, and stop the reaction within 15 minutes.

[0045] After suction filtration, the filter cake was washed three times with 45 mL of acetonitrile to obtain 47.87 g of the product with a yield of 93.5%.

[0046] Add 43.17g of phosphorus oxychloride, 150mL of 1,2-dichloroethane and 25.25g of triethylamine into a 500mL three-necked flask. The system is lowered to below zero in an ice-salt bath, and 90ml containing 29.75g of N,N - 1,2-dichloroethane solution of dimethylethylenediamine, the rate of addition is controlled to ensure that the reaction temperature is maintained within 10°C. After the dropwise addition, the reaction system ...

Embodiment 3

[0052] Synthesis of diethyl(2-(trimethyl-amino)propyl)phosphonic acid hexafluorophosphate, the structural formula is as follows:

[0053]

[0054] Add 57.98g of dibutyl phosphite, 22.95g of trichloroisocyanuric acid and 270mL of acetonitrile into a 500mL three-necked flask, place the system on a constant temperature stirrer, react at room temperature, and stop the reaction within 15 minutes.

[0055] After suction filtration, the filter cake was washed three times with 50 mL of acetonitrile to obtain 64.78 g of the product with a yield of 94.7%.

[0056] Add 56.98g of phosphorus oxychloride, 180mL of 1,2-dichloroethane and 25.31g of triethylamine into a 500mL three-necked flask, and the system is lowered to below zero in an ice-salt bath, and 25.56g of N,N- 60mL 1,2-dichloroethane solution of dimethylpropanediamine, the acceleration is controlled to ensure that the reaction temperature is maintained within 10°C. After the dropwise addition, the reaction system was transfer...

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Abstract

The invention discloses phosphate ionic liquids, a synthetic method thereof and an application as a lithium extraction agent. According to the method, the functional ionic liquids containing phosphamide groups are prepared from dibutyl phosphite, trichloroisocyanuric acid, N,N'-dimethylethanediamine and potassium hexafluorophosphate taken as raw materials through phosphoryl chlorination reaction,amidation with amine, salt forming reaction and exchange reaction. Compared with the prior art, the ionic liquids and the synthetic method thereof have the characteristics that operation is simple, industrial popularization and application are facilitated and the like, and have important application values.

Description

technical field [0001] The invention relates to a phosphoric acid ester ionic liquid and its synthesis method and application. Background technique [0002] As a new type of energy and strategic resource, lithium is known as "the energy metal of the 21st century". Its development and utilization have attracted much attention, and its demand is increasing year by year. Due to the cost and scale advantages of extracting lithium from salt lakes, the development and utilization of lithium resources in salt lakes has become an inevitable trend. my country is rich in lithium resources, mainly distributed in Qinghai and Tibet. By the end of 2014, the cumulative proven reserves of lithium chloride resources in Qinghai Qaidam Basin reached 18.31 million tons, accounting for about 80% of lithium resources reserves in China's salt lake brine. [0003] Magnesium and lithium are "diagonal elements" in the periodic table of chemical elements. They have similar radii and similar physical ...

Claims

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Application Information

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IPC IPC(8): C07F9/24B01D11/04
CPCC07F9/2454B01D11/04
Inventor 孟庆芬王延风赵朋龙张晓梅席田兴娇春鹏薛林
Owner 青海柴达木兴华锂盐有限公司
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