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Oxidized graphene modified polyamide composite nano-filtration membrane and preparation method thereof

A composite nanofiltration membrane and polyamide technology, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., can solve the problems of graphene oxide shedding, not really using graphene oxide filtration effect, etc., to achieve improved separation performance effect

Active Publication Date: 2016-11-09
TIANJIN POLYTECHNIC UNIV
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

However, the above treatment methods for graphene oxide often face the defect that the water flux increases while the salt interception decreases. At the same time, the graphene oxide is prone to fall off during the long-term use of the membrane, and the graphene oxide sheets are not distributed in the membrane. The polyamide layer is piled up on the bottom or surface, which does not really take advantage of the filtering effect of graphene oxide

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  • Oxidized graphene modified polyamide composite nano-filtration membrane and preparation method thereof
  • Oxidized graphene modified polyamide composite nano-filtration membrane and preparation method thereof
  • Oxidized graphene modified polyamide composite nano-filtration membrane and preparation method thereof

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preparation example Construction

[0020] Preparation of acyl chloride graphene oxide: under nitrogen protection, disperse 0.1 g of graphene oxide in absolute ethanol, mix with tetrachloromethane solution dissolved in 30 g of triphosgene, stir under ice bath; then add dropwise 20 milliliters of triethylamine-carbon tetrachloride solution (a catalyst for triphosgene), stirred until the triethylamine mist disappeared completely, removed the ice bath and nitrogen protection, and refluxed at 65° C. for 10 hours; the resulting mixture was filtered, The product is suction-filtered and washed with absolute ethanol for 2-3 times to remove by-products of glycolyl chloride esters (diethyl carbonate, a by-reaction product of glycolyl chloride, soluble in ethanol), to obtain the graphene oxide product of acid chloride.

[0021] In the graphene oxide modified polyamide composite nanofiltration membrane of the present invention, the ultrafiltration membrane base membrane of its interfacial polymerization is a flat membrane, a...

Embodiment 1

[0028] The specific preparation process of acyl chloride graphene oxide is as follows: under the protection of nitrogen, 0.1 gram of graphene oxide is dispersed in absolute ethanol, mixed with tetrachloromethane solution that is dissolved with 30 grams of triphosgene, stirred under ice bath; then Add 20 ml of triethylamine-carbon tetrachloride solution (a catalyst for triphosgene) dropwise, stir until the mist of triethylamine disappears completely, remove the ice bath and nitrogen protection, and reflux at 65°C for 10 hours; Filtrate, and use absolute ethanol to filter and wash the product 2-3 times to remove the by-products of glycolyl chloride esters (diethyl carbonate, a by-reaction product of glycolyl chloride, soluble in ethanol), to obtain graphene oxide of acid chloride product.

[0029] The obtained product was characterized by infrared spectroscopy, and it was found that the characteristic peak of graphene oxide C=O stretching vibration shifted to the low frequency d...

Embodiment 2

[0031] Soak the clean polysulfone ultrafiltration basement membrane in a 1% piperazine aqueous solution by mass percentage, take it out after 5 minutes, roll with a rubber roller to remove the excess aqueous solution on the surface of the basement membrane, and continue to immerse it in 0.10 % trimesoyl chloride organic solution (mass percentage is 2% ethanol as dispersant and cosolvent), carry out interfacial polymerization reaction, take out after 60 seconds; The polyamide composite membrane that will obtain is placed in 60 ℃ of environments and continues crosslinking 1 minute.

[0032] Use pure water and 1000ppm sodium sulfate, magnesium sulfate and sodium chloride aqueous solution to test the performance of graphene oxide modified polyamide composite nanofiltration membrane under the pressure of 0.6MPa. The results show that the pure water flux of the composite membrane 34.6L·m -2 h -1 , the rejection rates of sodium sulfate, magnesium sulfate and sodium chloride were 93...

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Abstract

The invention relates to an oxidized graphene modified polyamide composite nano-filtration membrane. Water flux and salt interception of a traditional polyamide nano-filtration membrane can be simultaneously improved. The composite membrane takes an ultra-filtration membrane as a base membrane, oxidized graphene or modified oxidized graphene and co-solvents are added into oil-phase solution in the traditional interfacial polymerization preparation process of the polyamide composite membrane, and the composite membrane is prepared by interfacial polymerization. The oxidized graphene modified polyamide composite nano-filtration membrane has the remarkable advantages that an upper ultrathin polyamide layer and a lower ultrathin polyamide layer are formed on the composite nano-filtration membrane, an orderly arranged oxidized graphene or modified oxidized graphene sheet structure is clamped between the upper ultrathin polyamide layer and the lower ultrathin polyamide layer, a loose polyamide layer link is arranged between sheets, surface charge of the ultrathin polyamide layer and the oxidized graphene sheets gives the composite membrane a high salt interception rate, the ultrathin layer is thinner than a functional layer of the traditional polyamide nano-filtration membrane, membrane resistance is effectively reduced, and the water flux is improved.

Description

technical field [0001] The invention relates to a graphene oxide modified polyamide nanofiltration membrane, belonging to the technical field of separation membrane preparation. Its preparation is characterized in that the composite nanofiltration membrane is based on an ultrafiltration membrane, and graphene oxide or modified graphene oxide and a cosolvent are added to the oil phase solution in the process of preparing a polyamide composite membrane by traditional interfacial polymerization, and the interfacial polymerization And prepared. Its notable feature is that graphene oxide sheets exist in the middle of the polyamide layer in an orderly manner instead of stacking on the bottom or surface, which reduces the effective filtration thickness of the functional layer, and doubles the water flux while improving the salt concentration to a certain extent. retention rate. Background technique [0002] Due to its unique structure and performance, separation membranes have em...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/82B01D71/56B01D71/02B01D69/12B01D69/02B01D67/00
CPCB01D67/0079B01D67/0088B01D69/02B01D69/12B01D71/024B01D71/56B01D71/82
Inventor 陈英波文鹏胡晓宇张宇峰
Owner TIANJIN POLYTECHNIC UNIV
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