Covalent triazine skeleton doped hybrid membrane preparation method

A technology of covalent triazine skeleton and hybrid membrane, which is applied in the field of membrane separation, can solve the problem of low alcohol content, and achieve the effects of high repeatability, wide application, simple and efficient preparation and operation

Active Publication Date: 2015-06-24
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Alcohol is currently mainly obtained through fermentation, but the content of alcohol obtained by traditional fermentation technology is very low

Method used

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  • Covalent triazine skeleton doped hybrid membrane preparation method
  • Covalent triazine skeleton doped hybrid membrane preparation method
  • Covalent triazine skeleton doped hybrid membrane preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] The preparation of embodiment 1 covalent triazine framework material

[0031] Add 0.4 g of terephthalonitrile into the microwave reaction kettle, then add 2 milliliters of trifluoromethanesulfonic acid, quickly close the reaction kettle, put it into the microwave reactor and heat the reaction. The process adopts a temperature program, and the temperature is raised to 100 ° C in 3 minutes, and the temperature is raised to 100 ° C in 1 minute. The temperature was raised to 130°C in 30 seconds, then kept at 130°C for 30 minutes, and the temperature was naturally lowered after the reaction was completed. The product was washed with deionized water, ethanol, acetone, and tetrahydrofuran, respectively, and dried under vacuum at 180°C overnight to remove traces of trifluoromethanesulfonic acid.

[0032] X-ray diffraction confirms that the product has a certain crystal form (such as figure 1 ), characteristic peak packets appear at 7°, 15° and 25°, respectively. Scanning elec...

Embodiment 2

[0033] The preparation of embodiment 2 covalent triazine framework material

[0034] The same operation as in Example 1, but the addition of raw materials and the heating program are increased. 1g of terephthalonitrile powder is first added to the microwave reactor, and then 5 milliliters of trifluoromethanesulfonic acid catalyst is added. The heating program is 1 minute by room temperature. The temperature was raised to 90°C, then raised from 90°C to 110°C in 30 seconds, and then kept at 110°C for 30 minutes to allow the reaction to fully proceed, and finally the temperature was naturally lowered. X-ray diffraction confirms that the product also has a certain crystal form (such as image 3 ). This synthesis method can achieve one-time synthesis of a large number of CTF materials.

Embodiment 3

[0035] Example 3 Preparation of Covalent Triazine Framework Material Doped Silicone Rubber Hybrid Membrane

[0036] The CTF material is mixed into polymethylphenylsiloxane at a ratio of 10wt%, and the membrane solution is prepared as follows:

[0037] Solution (1): After mixing 0.2 g of CTF material and 3.3 g of isooctane, ultrasonically disperse the CTF material in a water bath for 5 minutes at room temperature;

[0038] Solution (2): Mix 0.02 g of organotin with 0.2 g of tetraethylorthosilicate, 2 g of polymethylphenylsiloxane, and 3.3 g of isooctane, and ultrasonicate in a water bath for 5 minutes.

[0039] Transfer the solution (2) into the solution (1), disperse the probe evenly by ultrasound at 0°C, immerse the prepared alumina tube or sheet in the membrane solution for 10 seconds, and then pull up to form a membrane. It is 60 mm / min; with the change of the viscosity of the film liquid, a film is pulled and prepared at regular intervals, and the film thickness becomes t...

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Abstract

A covalent triazine skeleton doped hybrid membrane preparation method comprises the steps of (1) preparation of a covalent triazine skeleton, to be more specific, the formula is organic monomer: a trifluoromethanesulfonic acid, wherein a = 5-50, the organic monomer and the trifluoromethanesulfonic acid are rapidly mixed in a microwave reactor for synthetic of CTFs material by microwave heating, the synthesis temperature is 100 to 150 DEG C, and the synthesis time is 10 to 60 minutes; (2) preparation of a hybrid membrane solution, to be more specific, the formula is b covalent triazine skeleton powder: organic matter, b = 1wt%-60wt%, the organic matter is polydimethylsiloxane, polymethylphenyl siloxane, polyimide, polysulfone and poly trimethyl silane-1-propyne; (3) preparation of the hybrid membrane on a porous carrier by a dipping method; and (4) drying of the hybrid membrane. The hybrid membrane prepared by the method has high liquid separation performance and certain gas separation performance, and the synthesis repeatability is good.

Description

technical field [0001] The invention belongs to the field of membrane separation, specifically relates to the synthesis and application of a novel hybrid membrane doped with a covalent triazine skeleton, and in particular proposes a novel hybrid membrane used in the field of pervaporation separation. Background technique [0002] Alcohols such as ethanol and butanol are widely used as solvents and precursors of compounds. In recent years, a new application field of green biofuels has been discovered, which can be blended with gasoline in any proportion or even directly replaced. Alcohol is mainly obtained through fermentation at present, but the content of alcohol obtained by traditional fermentation technology is very low. Rectification is one of the most widely used and mature separation technologies. Due to its high energy consumption and relatively low yield, it takes multiple rectifications to achieve high purity of the separated product. Therefore, pervaporation separ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D69/12B01D71/06B01D71/70B01D71/56B01D71/68B01D67/00
Inventor 杨维慎彭媛李砚硕
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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