CN109321096A - A kind of UV modified graphite alkene polymer and preparation method thereof - Google Patents
A kind of UV modified graphite alkene polymer and preparation method thereof Download PDFInfo
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- CN109321096A CN109321096A CN201811175094.0A CN201811175094A CN109321096A CN 109321096 A CN109321096 A CN 109321096A CN 201811175094 A CN201811175094 A CN 201811175094A CN 109321096 A CN109321096 A CN 109321096A
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- graphene
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- graphite alkene
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
Abstract
The invention discloses a kind of UV modified graphite alkene polymers and preparation method thereof.The present invention is modified processing to graphene using UV irradiating machine first, obtains UV modified graphene；Modified graphene and a certain proportion of epoxy resin, decentralized medium, band epoxy group siloxanes, solvent are sufficiently mixed again；Then ball milling is carried out to mixture using planetary ball mill, obtains UV modified graphite alkene polymer.The present invention is modified modification to graphene by UV irradiation, in modifying process, graphene is exposed under ozone environment, its surface and ozone reaction generate oxygen-containing group, be grafted graphene can with coupling agent, compatibility of the graphene in epoxy-resin systems is enhanced, the dispersibility of graphene is improved, peomotes the development and application of graphene coating.
Description
Technical field
The present invention relates to graphene is modified and dispersing technology, it particularly relates to a kind of UV modified graphite alkene polymer and
Preparation method.
Background technique
Graphene is carbon atom with sp2The hexangle type two dimension carbon nanomaterial of hybridized orbit composition, with excellent light
, electricity, mechanical characteristic, in addition, graphene also has small-size effect, two-dimensional slice structure, hydrophobicity and electric conductivity.These
Excellent characteristic makes it can be used as filler for, to improve anticorrosion with coat performance, greatly enhancing anticorrosion with coat in anticorrosive paint
Ability.
But exactly because graphene is nano material, specific surface area is huge, and easily occur to reunite and then settle, thus
Influence the performance of graphene itself excellent properties.Also, the reunion of graphene be it is irreversible, which prevent graphenes to prevent again
Further applying in rotten coating.Therefore, how to solve dispersion stabilization of the graphene in coating is one very crucial
Problem, be badly in need of we explore a kind of new method prepare it is a kind of be easily dispersed, modified graphite alkene polymer not easy to reunite, solution
Certainly reunion settlement issues of the graphene in coating.
Currently, commonly solving graphene in coating there are two ways to agglomeration traits, one is use coupling agent to incite somebody to action
After graphene is modified, then with resin be grafted at compound resin, be then added in coating later；Another be then using
After graphene is modified by coupling agent, solvent is added, graphene dispersing solution is made, then dispersion liquid is added in the form of filler
Enter into coating.Both solution processes are complicated, increase the preparation step of coating, are unsuitable for industrial applications.
Summary of the invention
The purpose of the present invention is to provide a kind of UV modified graphite alkene polymer and preparation method thereof, the preparation method processes
Simply, it is suitble to industrial applications, and can solve the agglomeration traits of graphene, improves graphene stably dispersing in the epoxy
Property.
The invention is realized by the following technical scheme:
A kind of UV modified graphite alkene polymer is made of following component by mass percentage: UV modified graphene 1~
20%, epoxy resin 30~70%, decentralized medium 1~10%, band epoxy group siloxanes 0.5~3%, solvent 20~70%.
Further, the UV modified graphene obtains as follows:
(a) graphene powder is evenly laid out in the base, so that graphene can obtain in next modifying process
It is come into full contact with to uniform ultraviolet lighting and with ozone；
(b) 20~90min is irradiated to graphene powder using UV irradiating machine, obtains UV modified graphene.
The preparation method of above-mentioned modified graphite alkene polymer, comprising the following steps:
(1) freshly prepared UV modified graphene and epoxy resin, decentralized medium, band epoxy group siloxanes, solvent are pressed
Above-mentioned mass percent is uniformly mixed, and obtains mixture；
(2) mixture is put into reaction kettle, and steel ball is added, be fixed on ball mill after being sealed；
(3) 4~8h of ball milling obtains UV modified graphite alkene polymer.
Further, freshly prepared UV modified graphene is put into reaction kettle in 10min after preparation.
Further, one or more of epoxy resin CYD-011, CYD-014, E44.
Further, decentralized medium is one of n- methyl pyrrolidone (NMP), dimethylformamide (DMF).
Further, solvent is one or more of dimethylbenzene, n-butanol, cyclohexanone.
Further, band epoxy group siloxanes is one of KH-540, KH-550, AL-303.
Further, in step (2), the mass ratio of steel ball and material is 3~5:1.
Further, in step (3), ball milling carries out in planetary ball mill, and rotational speed of ball-mill should be greater than 200rpm, preferably
300~500rpm.
The preparation process of product of the present invention combines the mechanical milling process in Paint preparation technology, and preparation flow is simple, the period
It is short, it is easy to industrial applications.Wherein, to carry out surface to graphene by UV radiation instrument modified, can make graphene surface with it is smelly
Oxygen reaction generates oxygen-containing group.On the one hand, this can be such that graphene sheet layer spacing increases, and improve its dispersibility；On the other hand,
Modified graphene and coupling can be made by carrying out ball milling because there is the presence of oxygen-containing group, after modified graphene is mixed with coupling agent
Agent grafting, and chemical reaction and chemical bonding occurs with resin, enhance compatibility of the graphene in resin system, greatly changes
The dispersion of kind graphene in the polymer.
Compared with the prior art, the beneficial effects of the present invention are:
(1) present invention using UV irradiating machine to graphene carry out UV modification, under ozone environment, graphene surface with
Ozone reaction generates oxygen-containing group.This graphene method of modifying process is simple, is easy to industrial applications.
(2) modified graphene film interlamellar spacing increases, and enhances with epoxy resin compatibility, dispersed in coating
To raising.
(3) present invention is mixed by certain mass ratio by modified graphene and epoxy resin, decentralized medium, coupling agent, solvent
After conjunction put into stainless steel cauldron in carry out 7h ball milling, under the action of high-energy ball milling, realize band epoxy group siloxanes with
The grafting of modified graphene Surface oxygen-containing groups further enhances the compatibility of graphene and epoxy resin, makes modified
Graphene sheet layer is completely dispersed, and is evenly distributed in epoxy resin.
(4) present invention keeps grinding efficiency, product purity maximum by the ratio in control reaction kettle between steel ball and material
Change.
(5) addition of decentralized medium of the present invention facilitates graphene and further disperses in the epoxy, thus further
Promote polymer performance.
Detailed description of the invention
Fig. 1 is the FT-IR comparison diagram of unmodified graphene polymer and UV modified graphite alkene polymer of the present invention；
Fig. 2 is that unmodified graphene polymer carries out comparison diagram before and after 13 days sedimentation experiments.
Fig. 3 is that UV modified graphite alkene polymer of the present invention carries out comparison diagram before and after 120 days sedimentation experiments.
Specific embodiment
In the following, in order to keep those skilled in the art in the invention convenient to carry out, to UV modified graphene of the invention, UV
Modified graphene dispersing method is described in detail.Following embodiment is only to facilitate understanding the content of present invention and proposing, originally
Invention is not limited to this.
Embodiment 1
A kind of UV modified graphene, is prepared as follows:
(1) is evenly laid out on matrix by graphene powder, it is ensured that graphene is in loose condition (of surface), so that graphene exists
Uniform ultraviolet lighting can be obtained in next modifying process and is come into full contact with ozone.
(2) is modified processing to graphene: being irradiated 30min to graphene using UV irradiating machine to get described in
Modified graphene.
Embodiment 2
A kind of UV modified graphene, is prepared as follows:
(1) graphene powder is evenly laid out on matrix, it is ensured that graphene is in loose condition (of surface), so that graphene is connecing
Uniform ultraviolet lighting can be obtained in the modifying process to get off and is come into full contact with ozone.
(2) processing is modified to graphene: 60min is irradiated to get described in graphene using UV irradiating machine
Modified graphene.
Embodiment 3
A kind of preparation method of UV modified graphite alkene polymer, is prepared as follows:
Wherein formulation ratio is as follows:
Wherein modified graphene is obtained by embodiment 1 or embodiment 2.
Specific steps are as follows:
(1) by modified graphene powder according to the above ratio immediately put into 1L stainless steel cauldron in other formula materials
Mixing；
(2) is added in kettle amounts to the hard stainless shot of 0.5~0.6KG high, and kettle is placed in planetary ball mill after being sealed and is consolidated
It is fixed, reaction kettle is opened, reaction kettle revolves revolving speed as 200-480rpm, obtains UV modified graphite alkene polymer after running 7h.
Embodiment 4
A kind of preparation method of UV modified graphite alkene polymer, is prepared as follows:
Wherein formulation ratio is as follows:
Wherein modified graphene is obtained by embodiment 1 or embodiment 2.
Specific steps are as follows:
(1) by modified graphene powder according to the above ratio immediately put into 1L stainless steel cauldron in other formula materials
Mixing；
(2) is added in kettle amounts to the hard stainless shot of 0.5~0.6KG high, and kettle is placed in planetary ball mill after being sealed and is consolidated
It is fixed, reaction kettle is opened, reaction kettle revolves revolving speed as 200-480rpm, obtains UV modified graphite alkene polymer after running 7h.
Embodiment 5
A kind of preparation method of UV modified graphite alkene polymer, is prepared as follows:
Wherein formulation ratio is as follows:
Wherein modified graphene is obtained by embodiment 1 or embodiment 2.
Specific steps are as follows:
(1) obtained modified graphene powder is put into 1L stainless steel cauldron immediately according to the above ratio and is matched with other by
The mixing of square object material；
(2) is added in kettle amounts to the hard stainless shot of 0.5~0.6KG high, and kettle is placed in planetary ball mill after being sealed and is consolidated
It is fixed, reaction kettle is opened, reaction kettle revolves revolving speed as 200-480rpm, obtains UV modified graphite alkene polymer after running 7h.
Embodiment 6
A kind of preparation method of UV modified graphite alkene polymer, is prepared as follows:
Wherein formulation ratio is as follows:
Wherein modified graphene is obtained by embodiment 1 or embodiment 2.
Specific steps are as follows:
(1) obtained modified graphene powder is put into 1L stainless steel cauldron immediately according to the above ratio and is matched with other by
The mixing of square object material；
(2) is added in kettle amounts to the hard stainless shot of 0.5~0.6KG high, and kettle is placed in planetary ball mill after being sealed and is consolidated
It is fixed, reaction kettle is opened, reaction kettle revolves revolving speed as 200-480rpm, obtains UV modified graphite alkene polymer after running 7h.
By taking 3 gained UV modified graphite alkene polymer of embodiment as an example, resulting polymers of the present invention are illustrated.From Fig. 1
The FT-IR figure of product of the present invention is as can be seen that modified graphene polymer, has very compared to graphene polymer before modified
Big difference.Wherein, in 1028cm-1The absorption peak at place is the characteristic peak of Si-O-C, the peak of UV modified graphite alkene polymer here
There is significant reinforcement, this shows graphene by band epoxy group siloxanes success grafting and modifying.
Figure it is seen that unmodified graphene polymer has obvious sedimentation after 13 days, show graphite in polymer
Alkene is reunited.And from Fig. 3, it can be seen that modified graphite alkene polymer is after carrying out 120 days sedimentation experiments, do not have yet obvious
Sedimentation, shows that graphene dispersion is uniform in product of the present invention, and polymeric system is stablized.
Above to a kind of UV modified graphite alkene polymer provided by the invention schematically to the invention and its implementation
Mode is described, and description is not limiting, and shown in the drawings is also one of the embodiment of the invention, real
The structure on border is not limited thereto.So not departing from this creation objective if those of ordinary skill in the art are inspired by it
In the case where, frame mode similar with the technical solution and embodiment are not inventively designed, should belong to this patent
Protection scope.
Claims (10)
1. a kind of UV modified graphite alkene polymer, which is characterized in that be made of following component by mass percentage: UV is modified
Graphene 1~20%, epoxy resin 30~70%, decentralized medium 1~10%, band epoxy group siloxanes 0.5~3%, solvent 20
~70%.
2. UV modified graphite alkene polymer according to claim 1, which is characterized in that the UV modified graphene is by such as
Lower method obtains:
(a) graphene powder is evenly laid out in the base, so that graphene can obtain in next modifying process
Even ultraviolet lighting simultaneously comes into full contact with ozone；
(b) 20~90min is irradiated to graphene powder using UV irradiating machine, obtains UV modified graphene.
3. the preparation method of modified graphite alkene polymer of any of claims 1 or 2, which comprises the following steps:
(1) freshly prepared UV modified graphene is pressed with epoxy resin, decentralized medium, band epoxy group siloxanes, solvent above-mentioned
Mass percent is uniformly mixed, and obtains mixture；
(2) mixture is put into reaction kettle, and steel ball is added, be fixed on ball mill after being sealed；
(3) 4~8h of ball milling obtains UV modified graphite alkene polymer.
4. the preparation method of modified graphite alkene polymer according to claim 3, which is characterized in that freshly prepared UV changes
Property graphene after preparation in 10min put into reaction kettle in.
5. the preparation method of modified graphite alkene polymer according to claim 3, which is characterized in that epoxy resin CYD-
011, one or more of CYD-014, E44.
6. the preparation method of modified graphite alkene polymer according to claim 3, which is characterized in that decentralized medium is n- first
One of base pyrrolidones, dimethylformamide.
7. the preparation method of modified graphite alkene polymer according to claim 3, which is characterized in that solvent be dimethylbenzene,
One or more of n-butanol, cyclohexanone.
8. the preparation method of modified graphite alkene polymer according to claim 3, which is characterized in that band epoxy group siloxanes
For one of KH-540, KH-550, AL-303.
9. the preparation method of modified graphite alkene polymer according to claim 3, which is characterized in that in step (2), steel ball
Mass ratio with material is 3~5:1.
10. the preparation method of modified graphite alkene polymer according to claim 3, which is characterized in that in step (3), ball
Mill carries out in planetary ball mill, and rotational speed of ball-mill is greater than 200rpm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111564632A (en) * | 2020-05-20 | 2020-08-21 | 苏州柔能纳米科技有限公司 | Preparation method of electrode slurry for flexible battery |
| CN115785728A (en) * | 2022-10-27 | 2023-03-14 | 深圳市华星光电半导体显示技术有限公司 | High-refractive-index ink and preparation method thereof, and display panel and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103539106A (en) * | 2013-10-25 | 2014-01-29 | 苏州第一元素纳米技术有限公司 | Preparation method of carbon material |
| CN103965745A (en) * | 2014-05-13 | 2014-08-06 | 中国科学院宁波材料技术与工程研究所 | Epoxy resin composite coating solution, and preparation method and application method thereof |
| CN104386677A (en) * | 2014-11-10 | 2015-03-04 | 厦门凯纳石墨烯技术有限公司 | Micro-oxidized graphene and preparation method thereof |
| CN107090205A (en) * | 2017-06-06 | 2017-08-25 | 湖南邦泽科技有限公司 | A kind of electrostatic auxiliary graphene intercalation coats the preparation method of nm-class Ti polymer |
| CN108395808A (en) * | 2018-03-20 | 2018-08-14 | 湖南邦泽科技有限公司 | A kind of high heat conductance high temperature resistant heavy anti-corrosion paint and preparation method thereof |
-
2018
- 2018-10-09 CN CN201811175094.0A patent/CN109321096A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103539106A (en) * | 2013-10-25 | 2014-01-29 | 苏州第一元素纳米技术有限公司 | Preparation method of carbon material |
| CN103965745A (en) * | 2014-05-13 | 2014-08-06 | 中国科学院宁波材料技术与工程研究所 | Epoxy resin composite coating solution, and preparation method and application method thereof |
| CN104386677A (en) * | 2014-11-10 | 2015-03-04 | 厦门凯纳石墨烯技术有限公司 | Micro-oxidized graphene and preparation method thereof |
| CN107090205A (en) * | 2017-06-06 | 2017-08-25 | 湖南邦泽科技有限公司 | A kind of electrostatic auxiliary graphene intercalation coats the preparation method of nm-class Ti polymer |
| CN108395808A (en) * | 2018-03-20 | 2018-08-14 | 湖南邦泽科技有限公司 | A kind of high heat conductance high temperature resistant heavy anti-corrosion paint and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111564632A (en) * | 2020-05-20 | 2020-08-21 | 苏州柔能纳米科技有限公司 | Preparation method of electrode slurry for flexible battery |
| CN115785728A (en) * | 2022-10-27 | 2023-03-14 | 深圳市华星光电半导体显示技术有限公司 | High-refractive-index ink and preparation method thereof, and display panel and preparation method thereof |
| CN115785728B (en) * | 2022-10-27 | 2023-08-25 | 深圳市华星光电半导体显示技术有限公司 | High-refractive-index ink and preparation method thereof, display panel and preparation method thereof |
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Application publication date: 20190212 |