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Technology for continuously preparing trimethyl orthoacetate by using ionic liquid as solvent

A technology of trimethyl orthoacetate and ionic liquid, applied in the field of preparing trimethyl orthoacetate, can solve the problem of high loss rate, and achieve the effects of reducing energy consumption and saving costs

Inactive Publication Date: 2014-05-14
NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method simplifies the process, the by-product ammonium chloride still needs to be separated by suction filtration before distillation, and the solvent needs to be re-purified after repeated use, and its loss rate will be as high as 27%.

Method used

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  • Technology for continuously preparing trimethyl orthoacetate by using ionic liquid as solvent
  • Technology for continuously preparing trimethyl orthoacetate by using ionic liquid as solvent
  • Technology for continuously preparing trimethyl orthoacetate by using ionic liquid as solvent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Embodiment 1: Adopt butylmethylimidazolium hexafluorophosphate as solvent

[0016] Put 41.0g (1mol) of anhydrous acetonitrile, 32.0g (1mol) of anhydrous methanol and 73.0g of butylmethylimidazolium hexafluorophosphate into the reaction kettle, stir and cool the reaction solution to -5°C, and slowly pass it through the distribution tube to dry 36.5 g (1 mol) of hydrogen chloride gas, after the completion of the passage, slowly raise the temperature to 5°C, and at the same time fully stir the reaction for 6 hours to obtain ethyleneimine methyl ether hydrochloride solution. The solution was cooled to 0°C, and 64.0 g (2 mol) of pre-cooled anhydrous methanol was added thereto, the pH of the system was adjusted to 5.5 with ammonia gas, the temperature was raised to 40°C, and the reaction was stirred for 12 hours. The reaction liquid was cooled to 0°C, and the pH of the system was adjusted to 8.0 with ammonia gas. The reaction liquid was distilled under atmospheric pressure a...

Embodiment 6

[0021] Put 41.0g (1mol) of anhydrous acetonitrile, 32.0g (1mol) of anhydrous methanol and 73.0g of hexylmethylimidazolium hexafluorophosphate into the reaction kettle, stir and cool the reaction solution to -5°C, and slowly pass it through the distribution pipe Dry 36.5 g (1 mol) of hydrogen chloride gas, and slowly raise the temperature to 5°C after passing through, and at the same time fully stir the reaction for 6 hours to obtain ethyleneimine methyl ether hydrochloride solution. The solution was cooled to 0°C, and 64.0 g (2 mol) of pre-cooled anhydrous methanol was added thereto, the pH of the system was adjusted to 5.5 with ammonia gas, the temperature was raised to 40°C, and the reaction was stirred for 12 hours. The reaction liquid was cooled to 0°C, and the pH of the system was adjusted to 8.0 with ammonia gas. The reaction liquid was distilled under atmospheric pressure and fractions at 107°C to 109°C were collected to obtain 113.52 g of trimethyl orthoacetate with a ...

Embodiment 9

[0025] Put 41.0 g (1 mol) of anhydrous acetonitrile, 32.0 g (1 mol) of anhydrous methanol and 73.0 g of octylmethylimidazolium hexafluorophosphate recovered in Example 7 into the reaction kettle, stir and cool the reaction solution to -5°C, 36.5 g (1 mol) of dry hydrogen chloride gas was slowly introduced through the distribution pipe, and after the completion of the passage, the temperature was slowly raised to 5°C, and at the same time, the reaction was fully stirred for 6 hours to obtain the ethyleneimine methyl ether hydrochloride solution. The solution was cooled to 0°C, and 64.0 g (2 mol) of pre-cooled anhydrous methanol was added thereto, the pH of the system was adjusted to 5.5 with ammonia gas, the temperature was raised to 40°C, and the reaction was stirred for 12 hours. The reaction liquid was cooled to 0°C, and the pH of the system was adjusted to 8.0 with ammonia gas. The reaction liquid was distilled under atmospheric pressure and fractions at 107°C to 109°C were...

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Abstract

The invention provides a method for preparing trimethyl orthoacetate by using hydrophobic ionic liquid as a solvent. The method comprises the following steps: feeding anhydrous acetonitrile, anhydrous methanol and the solvent into a reaction kettle, cooling to -5 DEG C, feeding dry hydrogen chloride gas into the kettle, afterwards, stirring and reacting for 6 hours, wherein the solvent is the hydrophobic ionic liquid; feeding mixed liquid into a second reaction kettle, adding precooled methanol at the temperature of 5 DEG C, stirring for 0.5 hour, adjusting the pH value of a reaction system to 5-6 by using ammonia gas, and carrying out alcoholysis on the mixed liquid for 12 hours at the temperature of 40 DEG C; cooling alcoholysis liquid to 0 DEG C, adjusting pH value to 8.0 by using ammonia gas, feeding the alcoholysis liquid into an ordinary pressure rectifying tower, and collecting 107-109 DEG C fractions so as to obtain the trimethyl orthoacetate; and feeding residue at the bottom of the rectifying tower into a washing kettle, washing, feeding lower liquid into a drying kettle, drying, and recycling the dried solvent. The method has the advantages that the cost is saved, the energy consumption is reduced, and the green production of the trimethyl orthoacetate is realized.

Description

technical field [0001] The invention relates to a method for preparing trimethyl orthoacetate using a class of hydrophobic ionic liquid as a solvent. Background technique [0002] Trimethyl orthoacetate (CAS: 11445-45-0) is a colorless transparent liquid, easily soluble in organic solvents such as alcohol and ether, and is widely used in medicine except for the synthesis of new sweetener sucralose , pesticides, spices and other chemicals. There are not many domestic and foreign literature reports on the synthesis method of trimethyl orthoacetate, mainly including the metal sodium method and the acetonitrile method, among which the acetonitrile method has the most reports, and the raw materials of this method are easy to obtain and widely used. [0003] According to related reports, low-boiling solvents are generally used in industrial production, such as anhydrous ether, petroleum ether, chloroform, carbon tetrachloride, benzene, toluene, ethanol, etc. (Peter P.T.Sah, J.Am....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C43/32C07C41/60
CPCC07C41/60C07C257/06C07C43/32Y02P20/54
Inventor 胡兴邦李旭升吴有庭张志炳
Owner NANJING UNIV