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Technique and device for recovering tetrahydrofuran by pervaporation method

A tetrahydrofuran, pervaporation technology, applied in the chemical industry, organic chemistry, sustainable manufacturing/processing and other directions, can solve the problems of large energy consumption and equipment investment, high energy consumption and cost, high energy consumption, and ensure process safety. , the effect of improving energy utilization and reducing production energy consumption

Active Publication Date: 2015-06-17
JIANGSU NINE HEAVEN HIGH TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) Atmospheric pressure distillation: The azeotrope of tetrahydrofuran and water is obtained by distillation and separation under normal pressure. This azeotrope still contains a certain amount of water. Or the means of fractionation can no longer separate THF from the water in the azeotrope, so some extremely low moisture requirements cannot be met, and the energy consumption and cost of this process are relatively high
[0005] (2) Extractive distillation: add the extractant of the third component during the rectification process to change the relative volatility between the components to achieve the separation of the original azeotrope, but the amount of extractant used in the process of extractive distillation is relatively large , energy consumption and equipment investment are also relatively large, and the third component may be brought into THF products
However, the pressure swing rectification equipment is complex, requiring more theoretical plates and higher energy consumption

Method used

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  • Technique and device for recovering tetrahydrofuran by pervaporation method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Such as figure 1 , a device for recovering tetrahydrofuran by pervaporation, comprising a distillation kettle 1, a condenser 2, a storage tank 3, a pressurizing pump 4, a preheater 5, an evaporator 6, a pervaporation membrane separator 7 connected in sequence, and a pervaporation membrane separator 7. The permeate side of the vaporization membrane separator 7 is connected to the permeate tank 12 through the permeate condenser 10, a vacuum pump 11 is also arranged on the permeate side of the pervaporation membrane separator 7, and the retentate side of the pervaporation membrane separator 10 is connected to the preheater 5 It is connected by heat exchange, and then connected to the product tank 9 through the product condenser 8.

[0028] The crude tetrahydrofuran solvent in the production of meropenem is added to the still 1, and sodium hydroxide is added to adjust the pH to neutral, and sodium sulfite is added to remove the peroxide in the crude tetrahydrofuran, so tha...

Embodiment 2

[0030] The crude tetrahydrofuran solvent in the Grignard reaction is added to the distillation pot 1, and potassium hydroxide is added to adjust the pH to neutral, and sodium sulfite is added to remove the peroxide in the crude tetrahydrofuran, so that the peroxide mass content is lower than 0.05%. Heating and distilling, the evaporated water-containing tetrahydrofuran is condensed and collected in storage tank 3, salt, heavy organic matter and part of water are discharged from the bottom of the tank, and the flow rate is controlled to be 350kg / h. The feed liquid is preheated to 40°C and then enters the evaporator 6. The feed liquid is heated to 90°C and enters the pervaporation membrane separator 7 composed of 8 NaA molecular sieve membrane modules in series in the form of steam for dehydration and separation. The gauge pressure on the retentate side of the membrane is 0.6MPa, and the absolute pressure on the permeate side is 1000Pa. The water in the feed liquid permeates thr...

Embodiment 3

[0032] Add the crude tetrahydrofuran solvent in the production of the pharmaceutical intermediate α-methylene cyclic ketone into the distillation kettle 1, add sulfuric acid to adjust the pH to neutral, add sodium sulfite to remove the peroxide in the crude tetrahydrofuran, and make the peroxide mass content less than 0.05%. Heating and distilling, the evaporated water-containing tetrahydrofuran is condensed and collected in storage tank 3, salt, heavy organic matter and part of water are discharged from the bottom of the tank, and the flow rate is controlled to be 200kg / h. The feed liquid is preheated to 40°C and then enters the evaporator 6. The feed liquid is heated to 80°C and enters the pervaporation membrane separator 7 composed of 6 NaA molecular sieve membrane modules in series in the form of steam for dehydration and separation. The gauge pressure on the retentate side of the membrane is 0.2MPa, and the absolute pressure on the permeate side is 1500Pa. The water in t...

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Abstract

The invention relates to a technique for recovering tetrahydrofuran by a pervaporation method, which comprises the following steps: adding crude tetrahydrofuran into a distillation kettle, adding acid or alkali to regulate the pH value to a neutral state, adding a reducer to remove peroxides in the crude tetrahydrofuran, distilling by heating, condensing the distilled hydrous tetrahydrofuran, collecting the hydrous tetrahydrofuran in a storage tank, discharging salt, heavy organic substance and part of water from the kettle bottom, delivering the hydrous tetrahydrofuran to a preheater through a pressure pump, exchanging heat with high-purity tetrahydrofuran steam at the preheater, sending into an evaporator, and sending the hydrous tetrahydrofuran from the evaporator into a pervaporation membrane separator, wherein the infiltration side of the pervaporation membrane separator is connected with a vacuum system; condensing infiltration water by an infiltration liquid condenser, sending into an infiltration liquid tank, and obtaining high-purity tetrahydrofuran at the trapping side of the pervaporation membrane separator; and passing the high-purity tetrahydrofuran through a preheater, condensing through a finished product condenser, and sending into a product tank. The invention has the advantages of simple technical process, high safety factor, low equipment investment, high energy utilization efficiency and high recovery rate.

Description

technical field [0001] The invention relates to a process for recovering tetrahydrofuran, in particular to a process for recovering tetrahydrofuran by a pervaporation method, which belongs to the application field of pervaporation membranes. Background technique [0002] Tetrahydrofuran is an important organic chemical and fine chemical raw material. It has good solubility to many organic and inorganic substances. It can dissolve all compounds except polyethylene, polypropylene and fluororesin. It is widely used as a reactive solvent. "Universal solvent". [0003] In industrial production, when tetrahydrofuran is used as a solvent, impurities such as water are often brought in, so that tetrahydrofuran cannot be reused due to impurities, and it is discarded directly, which is wasteful and pollutes the environment, which does not meet the development requirements of energy saving and emission reduction. In recent years, with the increasing market demand for high-purity tetrah...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D307/08
CPCY02P20/10Y02P20/50
Inventor 顾学红石风强余丛立庆祖森
Owner JIANGSU NINE HEAVEN HIGH TECH
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