Preparation method of dodecafluoroheptyl-propyl-POSS modified graphene oxide

A technology of dodecafluoroheptylpropyl and fluoroheptylpropyl is applied in the field of preparation of dodecafluoroheptylpropyl POSS-modified graphene oxide, and can solve the problem of poor surface modification effect of final graphene, cyclic Due to the limited toughening effect of oxygen resin and the low density of fluorine and silicon on the surface of graphene, the effects of process optimization, avoidance of competitive reactions, and improvement of hydrophobic and oleophobic properties are achieved.

Inactive Publication Date: 2015-04-01
HOHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

POSS was successfully grafted on the prepared graphene oxide sheet, realizing the complementary advantages of graphene oxide and POSS structure, but due to the thermodynamic control of the reaction, the number of POSS grafted with graphene was greatly affected by the increase of temperature. Restricted, the toughening effect of modified epoxy resin is also limited
[0012] Although modifying graphene can produce high-performance materials and expand its application range, the existing graphene modification technology is mainly a single group modification, and the yield of the product and the modified graphene oxide The properties mainly depend on the degree of reaction and the nature of the modifie...

Method used

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  • Preparation method of dodecafluoroheptyl-propyl-POSS modified graphene oxide

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Embodiment 1

[0045] The invention provides a method for preparing dodecafluoroheptylpropyl POSS modified graphene oxide, the preparation steps are as follows:

[0046] (1) Add 1.2mol silane coupling agent KH560 dropwise to 1.0molT 7 Add 0.06 mol of triethylamine as a catalyst to the dodecafluoro POSS DMF solution, stir and heat at 25°C for 4.5 hours to prepare KH560-terminated POSS and T with monoepoxy functional groups. 7 Dodecafluoro POSS mixed solution, the chemical reaction formula is as follows Figure 4 Shown

[0047] (2) Add 0.25 kg of graphene oxide prepared by Hummers method with a surface carboxyl group content of 5.0wt.% to the above mixed solution, and ultrasonically disperse it to react with KH560-terminated POSS, add 0.06mol of triethylamine as a catalyst, Stir, heat the reaction at 20°C for 3 hours, stop heating and continue stirring, the chemical reaction formula is as follows Figure 5 Shown

[0048] (3) Add 0.05 mol and 0.03 mol of KH560 to the above reaction system to react for...

Embodiment 2-7

[0054] T 7 The preparation method of configuration dodecafluoroheptyl propyl POSS modified graphene oxide, the specific steps are the same as in Example 1, the amount of each raw material in the preparation process is shown in Table 1, wherein, T is added in each example 7 Dodecafluoro POSS is 0.10mol.

[0055] Table 1 Preparation T 7 The raw material consumption table of the configuration dodecafluoroheptyl propyl POSS modified graphene oxide

[0056]

[0057] The preparation method is the same as that of Example 1, with the parameters shown in Table 2, where the amount of the catalyst in step (1) and step (2) is 5% of the amount of KH560 added in step (1):

[0058] Table 2 Preparation T 7 Preparation process of modified graphene oxide with configuration dodecafluoroheptylpropyl POSS

[0059]

[0060] The water contact angle of the products of Examples 2-7 was measured with an electronic water drop angle tester, and the results are shown in Table 3:

[0061] Table 3 Preparation T 7 Wat...

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Abstract

A preparation method of dodecafluoroheptyl-propyl-POSS modified graphene oxide belongs to the technical filed of materials. The preparation process comprises three stages, wherein the first stage is a primary blocking stage, in which a silane coupling agent is added dropwise into T7 dodecafluoroheptyl-propyl-POSS to be subjected to blocking reaction to obtain a solution; the second stage is a grafting reaction stage, in which graphene oxide is added into the solution; the third stage in a secondary blocking ring-closure reaction stage, in which the silane coupling agent and dodecafluoroheptyl-propyl-siloxane are added and react to obtain the dodecafluoroheptyl-propyl-POSS modified graphene oxide with a higher grafting rate. The preparation method provided by the invention adopts three-time blocking and a one-pot synthetic process, greatly improves the grafting efficiency and increases the utilization ratio of fluorine-containing POSS, effectively reduces the dosage of T7 dodecafluoroheptyl-propyl-POSS, increases the density of fluorine and silicone on the surface of graphene, and further improves the surface property of water and oil repellency of graphene, the preparation process is simple, product purity is high and the production cost is low.

Description

Technical field [0001] The present invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of dodecafluoroheptylpropyl POSS modified graphene oxide, especially using T 7 Preparation method of modified graphene oxide prepared with dodecafluoroheptylpropyl POSS. Background technique [0002] Graphene is a new carbon material in which carbon atoms are densely packed into a single-layer two-dimensional honeycomb lattice structure. The thickness of this graphite crystal film is only 0.335nm. It is the basic unit for the construction of other dimensional carbon materials. Good crystallinity and electrical properties. Graphene has a high theoretical specific surface area, outstanding thermal conductivity and mechanical properties, and high electron mobility at room temperature. In addition, its special structure gives it a series of properties such as the half-integer quantum Hall effect and the never-disappearing conductivity, w...

Claims

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Application Information

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IPC IPC(8): C01B31/04
Inventor 何辉高超蒋亚清汪米琪程沁灵
Owner HOHAI UNIV
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