A kind of 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 and graphite oxide. Due to the low density of fluorosilicon on the surface of olefin and the limited toughening effect of epoxy resin, the effects of process optimization, avoiding competitive reaction and increasing fluorosilicon content are achieved.

Inactive Publication Date: 2016-08-31
HOHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 modified group, and most of the different single modification schemes have disadvantages such as low raw material utilization rate, low product yield, and high preparation cost: the use of silane coupling agent to modify graphene oxide The method has the disadvantages of poor practicability; the method of modifying graphene oxide with short-chain fluorine-containing siloxane has the disadvantages of low fluorine-silicon density on the surface of graphene and low siloxane utilization; because the ring-closing reaction of POSS is Reversible reaction, POSS modified graphene oxide also has the disadvantage of low POSS conversion rate
These reasons lead to the poor effect of the final graphene surface modification.

Method used

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  • A kind of preparation method of dodecafluoroheptyl propyl poss modified graphene oxide
  • A kind of preparation method of dodecafluoroheptyl propyl poss modified graphene oxide
  • A kind of preparation method of dodecafluoroheptyl propyl poss modified graphene oxide

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Embodiment 1

[0045] A kind of preparation method of dodecafluoroheptylpropyl POSS modified graphene oxide provided by the invention, the preparation steps are as follows:

[0046] (1) Add 1.2mol silane coupling agent KH560 dropwise to 1.0molT 7 In the dodecafluoro POSS DMF solution, add 0.06 mol of triethylamine as a catalyst, stir, heat and react at 25°C for 4.5 hours to prepare KH560 end-capped POSS and T containing single epoxy functional group 7 The mixed solution of dodecafluoro POSS, the chemical reaction formula is as follows Figure 4 shown;

[0047] (2) add the surface carboxyl content that is made by Hummers method at 0.25kg of graphene oxide 5.0wt.% to above-mentioned mixed solution, and ultrasonic dispersion makes it react with KH560 end-capping POSS, adds the triethylamine of 0.06mol as catalyst, Stir, heat and react at 20°C for 3 hours, stop heating and continue stirring, the chemical reaction formula is as follows Figure 5 shown;

[0048] (3) Add 0.05mol and 0.03mol of ...

Embodiment 2-7

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

[0055] Table 1 Preparation T 7 Raw material dosage table for dodecafluoroheptylpropyl POSS modified graphene oxide

[0056]

[0057] Preparation method is with embodiment 1, has parameter as shown in table 2, wherein the amount of the substance of the catalyzer of step (1) and step (2) is 5% of the amount of the KH560 substance that adds in the step (1):

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

[0059]

[0060] Measure the water contact angle of embodiment 2-7 product with electronic water drop angle tester, the result is as shown in table 3:

[0061] Table 3 Preparation T 7 Water Contact A...

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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 invention belongs to the technical field of chemical industry, in particular to a preparation method of dodecafluoroheptylpropyl POSS modified graphene oxide, especially using T 7 Preparation method of modified graphene oxide prepared by dodecafluoroheptylpropyl POSS. Background technique [0002] Graphene is a new carbon material in which carbon atoms are closely packed into a single-layer two-dimensional honeycomb lattice structure. The thickness of this graphite crystal film is only 0.335nm, which is the basic unit for constructing 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 makes it have a series of properties such as half-integer quantum Hall effect and never-disappearing electrical conductivity, so it has att...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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