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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

AI Technical Summary

Problems solved by technology

And for the preparation method of the quaternary phosphonium salt intermediate of methylcarbonate and the quaternary phosphonium salt ionic liquid containing organic acid radicals for dimethyl carbonate for quaternary phosphonium reaction, there is no report

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

Experimental program
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Effect test

Embodiment 1

[0029] Weigh trimethylphosphine (76.1g, 1mol), dimethyl carbonate (270.2g, 3mol), ethyl acetate (34.6g, 10%) and 20%-CuO / Al 2 o 3 Catalyst (1.39g, 0.4%) joins in the stainless steel autoclave, logical N 2 The air in the reactor was replaced, and the temperature was raised to 100° C. for 12 hours of reaction. After the reaction was completed, the temperature was lowered to 70° C. with cooling water, the catalyst was recovered by filtration, and unreacted raw materials and solvents were distilled off 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 tetramethylphosphonium methyl carbonate, with a yield of about 85%. Weigh methylcarbonate quaternary phosphonium salt tetramethylmethylphosphonium carbonate (49.9g, 0.3mol) and dissolve it in acetone (59.9g), add acetic acid (21.6g, 0.36mol), and reflux reaction at 40°C under magnetic stirring 3 hours. After the reaction was completed, the solvent w...

Embodiment 2

[0031] Weigh dodecyldimethylphosphine (230.4g, 1mol), dimethyl carbonate (180.1g, 2mol), ethanol (123.2g, 30%) and 30%-BaCO 3 / ZrO 2 Catalyst (0.41g, 0.1%) joins in the stainless steel autoclave, logical N 2The air in the reactor was replaced, the initial pressure was set to 1.0 MPa, and the temperature was raised to 120° C. to react for 10 hours. After the reaction was completed, the temperature was lowered to 60° C. with cooling water, the catalyst was recovered by filtration, and unreacted raw materials and solvents were distilled off under reduced pressure. Recrystallize with acetone, then vacuum dry at 60° C. for 5 hours to obtain 256.4 g of dodecyltrimethylphosphonium methyl carbonate, and the yield is about 80%. Weigh methyl carbonate quaternary phosphonium salt dodecyl trimethyl methyl phosphonium carbonate (64.1g, 0.2mol) and dissolve in methanol (32.1g), add n-octanoic acid (30.3g, 0.21mol), at 50°C The reaction was refluxed for 2.5 hours under magnetic stirring. ...

Embodiment 3

[0033] Weigh tetradecyl diethylphosphine (143.2g, 0.5mol), dimethyl carbonate (270.2g, 3mol), dichloromethane (82.7g, 20%) and 40%-Mn (OH) 2 / TiO2 catalyst (2.07g, 0.5%) joins in the stainless steel autoclave, logical 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 was completed, the temperature was lowered to 55° C. with cooling water, the catalyst was recovered by filtration, and unreacted raw materials and solvents were distilled off 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 diethylmethyl phosphonium methyl carbonate, with a yield of about 92%. Take methyl carbonate quaternary phosphonium salt tetradecyl diethylmethyl phosphonium methyl carbonate (75.3g, 0.2mol) and dissolve in chloroform (113g), add lauric acid (42.1g, 0.21mol), The reaction was refluxed at 60° C...

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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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