Room-temperature quaternary phosphonium salt ionic liquid and preparation method thereof

A technology of ionic liquid and quaternary phosphonium salt, which is applied in the field of room temperature quaternary phosphonium salt ionic liquid and its preparation, and achieves the effect of avoiding toxicity

Inactive Publication Date: 2018-08-24
CHINA RES INST OF DAILY CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

And for the preparation method of the quaternary phosphonium salt intermediate of methylcarbonate and the quaternary phosphonium

Method used

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  • Room-temperature quaternary phosphonium salt ionic liquid and preparation method thereof
  • Room-temperature quaternary phosphonium salt ionic liquid and preparation method thereof
  • Room-temperature quaternary phosphonium salt ionic liquid and preparation method thereof

Examples

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Example Embodiment

[0028] Example 1

[0029] Weigh trimethylphosphine (76.1g, 1mol), dimethyl carbonate (270.2g, 3mol), ethyl acetate (34.6g, 10%) and 20%-CuO / Al 2 O 3 The catalyst (1.39g, 0.4%) was added to the stainless steel autoclave and passed N 2 The air in the reactor was replaced, and the temperature was raised to 100°C for 12 hours. After the completion of the reaction, cooling water was passed to cool to 70°C, the catalyst was recovered by filtration, and unreacted raw materials and solvent were removed by distillation under reduced pressure. The product was washed with ethyl acetate, and then vacuum dried at 60°C for 5 hours to obtain 141.2 g of tetramethyl methyl carbonate phosphonium, with a yield of about 85%. Weigh methyl carbonate quaternary phosphonium salt tetramethyl methyl carbonate phosphonium (49.9g, 0.3mol) and dissolve it in acetone (59.9g), add acetic acid (21.6g, 0.36mol), and react under reflux at 40°C under magnetic stirring 3 hours. After the reaction, the solvent was...

Example Embodiment

[0030] Example 2

[0031] Weigh out dodecyl dimethyl phosphine (230.4g, 1mol), dimethyl carbonate (180.1g, 2mol), ethanol (123.2g, 30%) and 30%-BaCO 3 / ZrO 2 The catalyst (0.41g, 0.1%) was added to the stainless steel autoclave and passed N 2 The air in the reactor was replaced, the initial pressure was set to 1.0 MPa, and the temperature was raised to 120°C for 10 hours. After the reaction, the temperature was cooled to 60°C through cooling water, the catalyst was recovered by filtration, and the unreacted raw materials and solvent were removed by distillation under reduced pressure. It was recrystallized with acetone, and then dried under vacuum at 60° C. for 5 hours to obtain 256.4 g of dodecyl trimethyl phosphonium carbonate with a yield of about 80%. Weigh methyl carbonate quaternary phosphonium salt dodecyl trimethyl methyl carbonate (64.1g, 0.2mol) and dissolve it in methanol (32.1g), add n-octanoic acid (30.3g, 0.21mol), and heat at 50℃ The reaction was refluxed for 2.5 ...

Example Embodiment

[0032] Example 3

[0033] Weigh tetradecyl diethyl phosphine (143.2g, 0.5mol), dimethyl carbonate (270.2g, 3mol), dichloromethane (82.7g, 20%) and 40%-Mn(OH) 2 / TiO2 catalyst (2.07g, 0.5%) was added to the stainless steel autoclave, and N 2 The air in the reactor was replaced, the initial pressure was set to 0.2 MPa, and the temperature was raised to 140°C for 10 hours. After the reaction, the temperature was cooled to 55°C through cooling water, the catalyst was recovered by filtration, and the unreacted raw materials and solvent were removed by distillation under reduced pressure. The product was washed with dichloromethane, and then vacuum dried at 60°C for 5 hours to obtain 173.2 g of tetradecyl diethyl methyl methyl carbonate phosphonium, with a yield of about 92%. Weigh the methyl carbonate quaternary phosphonium salt tetradecyl diethyl methyl methyl carbonate phosphonium (75.3g, 0.2mol) and dissolve it in chloroform (113g), add lauric acid (42.1g, 0.21mol), The reaction w...

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Abstract

The structural formula of a room-temperature quaternary phosphonium salt ionic liquid is shown in the description; and in the formula, R1, R2 and R3 are a C1-22 alkyl group, a phenyl group or an arylgroup, R1, R2 and R3 are the same group or different groups, and A<-> is an acid radical. The ionic liquid has the advantages of non-toxicity, no pollution and high device corrosivity.

Description

technical field [0001] The invention relates to a room temperature quaternary phosphonium salt ionic liquid and a preparation method thereof. Background technique [0002] Ionic liquids refer to salts that are liquid at or near room temperature and are composed entirely of anions and cations, also known as room temperature molten salts. Ionic liquids are widely used in catalysis, organic synthesis, electrochemistry, biomedicine, separation science, nano materials, antibacterial materials, optical materials, lubricating materials and other fields. [0003] According to different cation structures, ionic liquids can be divided into four categories: alkyl-substituted imidazolium ammonium salts, alkyl-substituted pyridinium ammonium salts, quaternary ammonium salts, and quaternary phosphonium salts. In recent years, due to the better chemical stability and thermal stability of quaternary phosphonium salt ionic liquids, researchers have gradually attracted attention. The prepa...

Claims

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Application Information

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IPC IPC(8): C07F9/54
CPCC07F9/5407C07F9/5435C07F9/5442
Inventor 耿涛段升富姜亚洁鞠红斌王亚魁
Owner CHINA RES INST OF DAILY CHEM IND
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