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A kind of method that reclaims triethylamine from aqueous solution

A technology of triethylamine and aqueous solution, applied in the field of pharmaceutical synthesis, can solve the problems of high cost, high energy consumption, low efficiency, etc., and achieve the effects of low environmental pressure, simple operation, and no environmental pollution

Active Publication Date: 2017-01-11
SHANGHAI NEW HUALIAN PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention provides a kind of method that reclaims triethylamine from aqueous solution, and this method can reduce the moisture of system during distillation greatly, can reduce the waste of resource, do not pollute environment again, can also reduce production cost, thereby solved The problems of high energy consumption, high cost and low efficiency in recovering triethylamine from aqueous solution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Embodiment 1, reclaim triethylamine from the aqueous solution of synthetic hydrocortisone

[0022] The content of triethylamine in the triethylamine aqueous solution of this embodiment is 30%, which comes from the aqueous solution of synthetic hydrocortisone.

[0023] 1. Adjust acidity

[0024] In a 5L beaker, put 3.5L of 30% triethylamine aqueous solution, add 30% hydrochloric acid to adjust pH=1;

[0025] 2. Cyclohexane extraction

[0026] Add the solution in step 1 to a 5L separatory funnel, extract with 500ml cyclohexane each time until the triethylamine content in the aqueous layer is less than 0.5%, and collect the obtained organic phase for later use;

[0027] 3. Alkali adjustment and liquid separation

[0028] Combine the organic phases in step 2, adjust the pH to greater than 12 with 45% sodium hydroxide solution, separate the alkaline aqueous layer, and apply mechanically;

[0029] 4. Backflow water separation

[0030] Put the solution of step 3 into a 1L...

Embodiment 2

[0031] Embodiment 2, reclaim triethylamine from the aqueous solution of synthetic hydrocortisone

[0032] The content of triethylamine in the triethylamine aqueous solution of this embodiment is 30%, which comes from the aqueous solution of synthetic hydrocortisone.

[0033] 1. Adjust acidity

[0034] In a 500L reactor, put 300L of 30% aqueous solution of triethylamine into it, and add 30% hydrochloric acid to adjust the pH to 1;

[0035] 2. Cyclohexane extraction

[0036] Extract the solution in step 1 with 30-50L cyclohexane each time until the content of triethylamine in the aqueous layer is less than 0.5%, and collect the obtained organic phase for later use;

[0037] 3. Alkali adjustment and liquid separation

[0038] Combine the organic phases in step 2, adjust the pH to greater than 12 with 50% sodium hydroxide solution, separate the alkaline water layer, and apply mechanically;

[0039] 4. Backflow water separation

[0040] After the solution in step 3 was refluxe...

Embodiment 3

[0041] Embodiment 3, reclaim triethylamine from the aqueous solution of synthetic hydrocortisone

[0042] The content of triethylamine in the triethylamine aqueous solution of this embodiment is 30%, which comes from the aqueous solution of synthetic hydrocortisone.

[0043] 1. Adjust acidity

[0044] In a 2000L reactor, put 1600L of 30% triethylamine aqueous solution into it, and add 30% hydrochloric acid to adjust the pH=1;

[0045] 2. Cyclohexane extraction

[0046] Extract the solution in step 1 with 100-200L cyclohexane each time until the content of triethylamine in the water layer is less than 0.5%, and collect the obtained organic phase for later use;

[0047] 3. Alkali adjustment and liquid separation

[0048] Combine the organic phases in step 2, adjust the pH to greater than 12 with 45% sodium hydroxide solution, separate the alkaline aqueous layer, and apply mechanically;

[0049] 4. Backflow water separation

[0050] After the solution of step 3 is refluxed t...

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PUM

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Abstract

The invention relates to a method for recovering triethylamine from an aqueous solution. the method comprises the following steps: adjusting pH value of a triethylamine aqueous solution system to 1 by the use of hydrochloric acid, extracting triethylamine by the use of cyclohexane, adjusting pH value to more than 12 by the use of sodium hydroxide, carrying out backflow and water division after division of an alkaline water layer until there is no obvious moisture, carrying out atmospheric distillation, distilling to obtain high-purity triethylamine, and recovering cyclohexane. The method has advantages of simple operation, high efficiency and less environment stress, and is suitable for recovery of a triethylamine aqueous solution with the concentration of 5-50%.

Description

technical field [0001] The invention relates to the technical field of medicine synthesis, in particular to a method for recovering triethylamine from an aqueous solution. Background technique [0002] Triethylamine (molecular formula: N(CH2CH3)3) is an amine organic compound. It is a colorless to light yellow transparent liquid with a strong ammonia odor. It fumes slightly in the air and is slightly soluble in water. It is soluble in ethanol and ether, and its aqueous solution is alkaline. It is an organic base, catalyst, solvent and raw material commonly used in drug synthesis. [0003] Because triethylamine is expensive and highly toxic, it must be recycled in drug synthesis. However, the solubility of triethylamine in aqueous solution is relatively large, so when the content of triethylamine in aqueous solution is low, the recovery energy consumption by distillation is large and the cost is very high. Contents of the invention [0004] The object of the present inven...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C211/05C07C209/82C07C13/18C07C7/04
Inventor 宣闵吴庆安周秋火
Owner SHANGHAI NEW HUALIAN PHARMA