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Method for Separating Small Molecule Solvents from Aprotic Polar Solvents

A polar solvent and small molecule technology, applied in the field of separation of small molecule solvents in aprotic polar solvents, can solve the problems of poor solvent resistance, high cost and short service life of membranes

Active Publication Date: 2021-11-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is that the separation device for aprotic polar solvents in the prior art has high energy consumption, high cost, and complex recovery equipment and processes. Ordinary polymer membranes have poor solvent resistance and low separation efficiency, resulting in thin The service life is short, and it is difficult to separate and purify aprotic polar organic solvents; the present invention provides a method for separating small molecule solvents in aprotic polar solvents, using polyimide pervaporation membranes, which can stably and effectively separate Small molecule solvent in aprotic polar solvent, resistant to high pressure difference and not easy to break, high separation efficiency, simple process, compared with the characteristics of low cost of the existing separation technology, the application prospect is broad

Method used

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  • Method for Separating Small Molecule Solvents from Aprotic Polar Solvents

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] 1. Stock solution preparation: Dissolve 14.7g 2,2'-bis[4-(4-aminophenoxyphenyl)]propane (BAPP) and 1.8g 3,-diaminobenzoic acid (DABA) in 146.1g N , N-dimethylacetamide, after stirring until completely dissolved, add 15.5g of benzophenone dianhydride (BTDA) powder (the molar ratio of dianhydride to diamine is 1:1), continue stirring until fully reacted, and the table The apparent viscosity is 5×10 3 cP (25°C) homogeneous transparent viscous polyamic acid solution.

[0055] 2. Preparation of pervaporation membrane:

[0056] a) Coat a layer of PAA solution on the inorganic ceramic support by spin coating, immerse it horizontally in ethanol for 10 minutes to make the solvent diffuse completely, take it out and keep it in an oven at 100°C for 20 minutes, and keep it at 260°C for 30 minutes for imidization Thus, the prepared PI pervaporation membrane a covered with a dense layer of PI is obtained.

[0057] b) Coat a layer of PAA solution on the prepared PI pervaporation me...

Embodiment 2

[0061] 1. Stock solution preparation: Dissolve 22.1g of 4,4-biphenylenediamine (BZD) in 250.8g of N,N-dimethylacetamide, stir until completely dissolved, then add 40.6g of benzophenone dianhydride (BTDA) powder (the molar ratio of dianhydride to diamine is 1.05:1), and continue to stir until fully reacted to obtain an apparent viscosity of 4.8×10 5 cP (25°C) homogeneous transparent viscous polyamic acid solution.

[0062] 2. Preparation of pervaporation membrane:

[0063] a) Coat a layer of PAA solution on the inorganic ceramic support by spin coating, immerse it horizontally in ethanol for 10 minutes to make the solvent diffuse completely, take it out, keep it in an oven at 50°C for 60 minutes, and keep it at 240°C for 60 minutes for imidization Thus, the prepared PI pervaporation membrane a covered with a dense layer of PI is obtained.

[0064] b) Coat a layer of PAA solution on the preliminary PI pervaporation membrane a obtained in step a) by spin coating method, immerse...

Embodiment 3

[0069] 1. Stock solution preparation: Dissolve 24.0g 4,4-diaminodiphenyl ether (ODA) in 220.9g N-methyl-2-pyrrolidone, stir until completely dissolved, then add 39.3g benzophenone dianhydride (BTDA) powder (the molar ratio of dianhydride to diamine is 0.99:1), continue to stir until fully reacted, and obtain an apparent viscosity of 3.6×10 5 cP (25°C) homogeneous transparent viscous polyamic acid solution.

[0070] 2. Preparation of pervaporation membrane:

[0071] a) Apply a layer of PAA solution on the inorganic ceramic support by scraping method, immerse it horizontally in N-methyl-2-pyrrolidone aqueous solution (20wt%) for 10min to make the solvent diffuse completely, take it out and put it in an oven at 80°C Insulate for 40 minutes, and then imidize at 300°C for 10 minutes to obtain a preliminary PI pervaporation membrane a covered with a dense layer of PI.

[0072] b) Coating a layer of PAA solution on the prepared PI pervaporation membrane a obtained in step a) by spi...

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Abstract

The invention relates to a method for separating small-molecule solvents from aprotic polar solvents, which mainly solves the problems of high equipment requirements for aprotic polar solvent separation, high energy consumption, and complex devices and processes in the existing separation technology. The method for separating small-molecule solvents in aprotic polar solvents provided by the present invention adopts a pervaporation membrane separation device, which includes a feed liquid filled with a mixture of aprotic polar solvents and small-molecule solvents on the upper part of the pervaporation membrane, and the lower part of the pervaporation membrane The cavity is connected to a vacuum device, so that the small molecule solvent in the feed liquid diffuses to the lower cavity through the pervaporation membrane, wherein the pervaporation membrane is a polyimide pervaporation membrane including a support layer and a separation layer, and the separation layer Located on the support layer, the separation layer is a multi-layer polyimide membrane, which better solves this problem and can be used in industrial processes such as recovery and purification of aprotic polar organic solvents.

Description

technical field [0001] The invention relates to a method for separating small molecule solvents from aprotic polar solvents. Background technique [0002] Aprotic polar solvents such as dimethylformamide (DMF) and dimethylacetamide (DMAc) are widely used in the fields of pesticides, medicine, organic synthesis, and synthetic leather. The separation, recovery and treatment of used aprotic polar solvents such as amide solvents has become an important research content in the industrial field. However, the distillation and rectification separation methods commonly used in the existing separation and recovery technologies have problems such as high energy consumption, complicated recovery equipment and processes, and at the same time, in order to improve the tolerance of the separation device to aprotic polar solvents, the separation has also been greatly improved. Cost recovery. As a new type of membrane separation technology, pervaporation (PV) technology has been well applie...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D61/36B01D71/64B01D69/10C08G73/10
CPCB01D61/362B01D69/10B01D71/64C08G73/1042C08G73/105C08G73/1053C08G73/1067C08G73/1071
Inventor 刘京妮孙旭阳崔晶钟璟马文中
Owner CHINA PETROLEUM & CHEM CORP