Process for separating ethane nitrile wastewater with combination of abstraction and distillation

A process method and combined technology, applied in the field of separation of acetonitrile wastewater by combining extraction and rectification, can solve the problems of complex treatment methods, low separation efficiency, high equipment cost, etc., achieve improved recovery rate and acetonitrile product quality, and improve economic benefits , The effect of reducing energy consumption and production costs

Active Publication Date: 2013-06-19
TIANJIN PULAI CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Both of these two methods use two steps of rough distillation and rectification, and use a special rectification method for separation treatment, which has problems such as complicated treatment methods, high equipment costs and low separation efficiency.

Method used

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  • Process for separating ethane nitrile wastewater with combination of abstraction and distillation

Examples

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Effect test

Embodiment 1

[0020] A pharmaceutical factory produces acetonitrile waste water in the production process, the acetonitrile weight content in this acetonitrile waste water is about 20%, and the rest is a small amount of pharmaceutical by-products and water, and its treatment steps are as follows:

[0021] (1). Under normal temperature and pressure, use a 3L glass cup as the extraction tank, add 1L of acetonitrile waste water in each batch, and then add 0.8L of dichloromethane. After fully stirring for half an hour, the mixture will be extracted; the mixture will be allowed to stand Half an hour later, the mixture was divided into two layers: the lower layer was the extract phase, which was a heavy phase with a volume of about 1.1 L and acetonitrile weight content of about 13%; the upper layer was a raffinate phase, and the raffinate phase was a light phase. The volume is about 0.7L, mainly water, and the weight content of acetonitrile is about 2.2%;

[0022] (2). Put the extract phase of th...

Embodiment 2

[0027] A pharmaceutical factory produces 5m per day in the production process 3 Acetonitrile waste water, the acetonitrile weight content in this acetonitrile waste water is about 28%, and all the other are a small amount of pharmaceutical by-products and water, and its treatment steps are as follows:

[0028] (1). At normal temperature and pressure, use 6.3m 3 The enamel stirring tank is used as the extraction tank, and each batch is added with 2.5m 3 Acetonitrile wastewater, then add 2.5m 3 Dichloromethane, fully stirred for 2 hours, the mixed solution was extracted; then the mixed solution was left to stand for half an hour, and the mixed solution was divided into two layers: the lower layer was the extraction phase, and the extraction phase was the heavy phase, with a volume of about 3.2m 3 , the weight content of acetonitrile is about 15%; the upper layer is the raffinate phase, and the raffinate phase is the light phase with a volume of about 1.8m 3 , mainly water, th...

Embodiment 3

[0035] A pharmaceutical factory produces 2m per day in the production process 3 Acetonitrile waste water, the acetonitrile weight content in this acetonitrile waste water is about 15%, all the other are a small amount of pharmaceutical by-products and water, and solution is acidic, and its processing steps are as follows:

[0036] (1). At normal temperature and pressure, use 6.3m 3 The enamel stirring tank is used as the extraction tank, and the acetonitrile wastewater is added to the extraction tank at one time, and then 1.8m 3 Dichloromethane, fully stirred for 2 hours, and the mixture was extracted; then the mixture was left to stand for half an hour, and the mixture was divided into two layers: the lower layer was the extraction phase, and the extraction phase was the heavy phase, with a volume of about 2.2m 3 , the weight content of acetonitrile is about 11%; the upper layer is the raffinate phase, and the raffinate phase is the light phase with a volume of about 1.6m 3...

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Abstract

The invention relates to a technical method of separating acetonitrile wastewater by combining extraction and distillation, belonging to the technical field of pharmaceutical chemicals. In the method, the acetonitrile waste water and dichloromethane are successively put into an extraction pot for the extraction function, and then mixed liquid is stratified; an extract phase is added into a distillation tower reactor, and after the distillation treatment, the dichloromethane containing water and the dichloromethane containing acetonitrile are successively separated and put into the extraction pot; when the tower top temperature of the distillation tower reaches 81-82 DEG C, the acetonitrile is separated after the dichloromethane is collected; extraction raffinate in an extraction raffinatepot is added into the distillation tower reactor, and after the distillation treatment, the dichloromethane-acetonitrile in extraction raffinate is separated and added into the extraction pot to be treated together with acetonitrile waste water of the next batch. The technical method solves common problems existing in the production of pharmaceutical industry, reduces menstruum losses and equipment investment, lowers the energy consumption and the production cost, improves the recovery rate and the product quality of the acetonitrile and obviously improves the economic benefits.

Description

technical field [0001] The invention belongs to the technical field of medicine and chemical industry, in particular to a process method for separating acetonitrile wastewater by combining extraction and rectification. Background technique [0002] Acetonitrile is an important solvent in the pharmaceutical production process. In the production process, it is inevitable to mix acetonitrile with water and other impurities to produce acetonitrile wastewater. In the actual production process, it is often necessary to separate acetonitrile from acetonitrile wastewater for reuse. However, acetonitrile and water form an azeotrope under normal pressure, and it is difficult to completely separate them by ordinary distillation methods. At present, there are two kinds of conventional methods for separating the acetonitrile-water mixture: 1. Pressure swing rectification: the first step acetonitrile-water mixture is roughly steamed to obtain an azeotrope with acetonitrile content of 85%;...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C255/03C07C253/34C02F1/26C02F101/30
Inventor 徐仁萍刘翠茹李建慈
Owner TIANJIN PULAI CHEM TECH
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