CN108864759A - A kind of method of modifying of the graphene suitable for methyl phenyl silicone oil material - Google Patents
A kind of method of modifying of the graphene suitable for methyl phenyl silicone oil material Download PDFInfo
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
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- C01B32/15—Nano-sized carbon materials
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- C01B32/194—After-treatment
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- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- C08K9/00—Use of pretreated ingredients
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- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/12—Treatment with organosilicon compounds
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Abstract
The invention discloses a kind of method of modifying of graphene suitable for methyl phenyl silicone oil material, include the following steps：By certain mass component, by graphene ultrasonic disperse in dimethylbenzene, graphene slurries are formed；Dehydrated alcohol, phenyl triethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy silicane, nonylphenol polyoxyethylene ether, polyalcohol are added into graphene slurries, after stirring, deionized water is added and adjusts pH value, is again stirring for；After dry, modified graphene is made to neutrality in washing.Its preparation process is simple, efficiently solve the dispersion of the graphene in methyl phenyl silicone oil, realize graphene purpose evenly dispersed in methyl phenyl silicone oil, and there is very good stability, it can long-term preservation, so that the conduction and heating conduction of graphene are given full play in methyl phenyl silicone oil material, there is very strong practicability and wide applicability.
Description
Technical field
The present invention relates to a kind of method of modifying, and in particular to a kind of graphene suitable for methyl phenyl silicone oil material changes
Property method.
Background technique
Organic silicon rubber and silicone resin are widely used in power industry Material Field, and graphene has excellent lead
Electricity and the capacity of heat transmission, the combination of two kinds of materials can play respective advantage, using graphene as filler addition organic silicon rubber and
Silicone material can significantly improve its thermally conductive, electric conductivity.
Since graphene is inorganic matter, chemical bond directly can not be formed between organosilicon material, therefore directly by graphite
After organic rubber or silicone material is added in alkene, grapheme material can reunite, it is evenly dispersed to be difficult to.
Summary of the invention
To solve the deficiencies in the prior art, the purpose of the present invention is to provide one kind to enable graphene in aminomethyl phenyl silicon
The method of modifying of uniform and stable dispersion in light wood material.
In order to achieve the above objectives, the present invention adopts the following technical scheme that：
A kind of method of modifying of the graphene suitable for methyl phenyl silicone oil material, includes the following steps：
S1, certain mass component is pressed, by graphene ultrasonic disperse in dimethylbenzene, forms graphene slurries；
S2, certain mass component is pressed, dehydrated alcohol, phenyl triethoxysilane, γ-shrink is added into graphene slurries
Glycerol ether oxygen propyl trimethoxy silicane, nonylphenol polyoxyethylene ether, polyalcohol after stirring, are added deionized water and adjust pH
Value, is again stirring for；
After dry, modified graphene is made in S3, washing to neutrality.
Above-mentioned supersonic frequency is 40-50KHz, jitter time 10-30min.
The revolving speed stirred in above-mentioned steps S2 is 1800r/min, mixing time 3-5min, and the time being again stirring for is
20-40min。
PH value in above-mentioned steps S2 is adjusted to 4-5.
Detergent in above-mentioned steps S3 is dimethylbenzene, depressurizes filtering and washing, and pass is 4-6 times.
Drying temperature in above-mentioned steps S3 is 120-140 DEG C, is evacuated to -0.09MPa, drying time 1-4h.
Drying in above-mentioned steps S3, environment are -0.09MPa vacuum state.
Quality component in above-mentioned steps S1 includes：100 parts of graphene, 1600-1900 parts of dimethylbenzene；Matter in step S2
Measuring component includes：100-400 parts of dehydrated alcohol, 1-4 parts of phenyl triethoxysilane, γ-glycidyl ether oxygen propyl trimethoxy
1-3 parts of base silane, 1-3 parts of nonylphenol polyoxyethylene ether, 1-5 parts of deionized water.
Above-mentioned graphene is the graphene of reduction method preparation.
The invention has the beneficial effects that：
For the present invention by each quality component raw material, having reached keeps graphene uniform and stable in vinyl silicone oil material
The purpose of dispersion：
Contain phenyl ring in dimethylbenzene, be good nonpolar solvent, graphene has good dispersion effect in dimethylbenzene
Fruit, therefore dispersing agent of the dimethylbenzene as graphene can be used.
The graphene surface of reduction method preparation usually contains a small amount of hydroxyl (- OH) or epoxy groupPhenyl
Triethoxysilane and γ-glycidyl ether oxygen propyl trimethoxy silicane are silane coupling agent, can be with the hydroxyl of graphene surface
Base reacts, and vinyl is contained on the modified graphene surface of formationEpoxy group (Ether (-
O-), wherein the pi bond collective effect of the pi bond of phenyl and graphene itself, enriched move freely electronics, weaken modified pair
The negative effect of the graphene conductive capacity of heat transmission, enhances the compatibility with phenyl siloxane rubber, and epoxy group can pass through with ether
The interaction force of effect the enhancing graphene and organosilicon macromolecule of hydrogen bond, and then increase point of the graphene in silicon rubber
Dissipate stability.
Nonylphenol polyoxyethylene ether is emulsifier, and deionized water can be made evenly dispersed in dimethylbenzene (oily phase).
The hydroxyl of phenyl triethoxysilane and γ-glycidyl ether oxygen propyl trimethoxy silicane and graphene surface is anti-
Answer it is removable be divided into two steps, the first step is phenyl triethoxysilane and γ-glycidyl ether oxygen propyl trimethoxy silicane and water
Hydrolysis occurs and generates silanol, contains silicone hydroxyl (- Si-OH) in silanol, second step is the hydroxyl of silanol and graphene surface
Reaction, realize graphene surface grafted-organosilicon segment, emulsifier nonylphenol polyoxyethylene ether make deionized water with it is silane coupled
Agent and graphene uniform contact, and the modified related chemistry reaction of graphene can uniformly occur in mixed system, can be reduced and do not changed
Property graphene residual.
Modified graphene need to pass through filtering and washing, to remove non-grafted silane coupling agent on the surface of graphene, emulsification
Agent, the remaining water of hydrochloric acid and part, are finally dried, and phosphorus pentoxide, five oxidations need to be added when dry in vacuum drying oven
Two phosphorus and water have high reactivity, can absorb a small amount of water evaporated from modified graphene because vacuum is heated
Point.It finally can get pure vinyl triethoxysilane and γ-glycidyl ether oxygen propyl trimethoxy silicane modified graphite
Alkene.
A kind of method of modifying of graphene suitable for methyl phenyl silicone oil material provided by the invention, preparation process letter
It is single, the dispersion of the graphene in methyl phenyl silicone oil is efficiently solved, it is equal in methyl phenyl silicone oil to realize graphene
The purpose of even dispersion, and have very good stability, can long-term preservation so that the conduction of graphene and heating conduction are in first
It is given full play in base phenyl silicone oil material, there is very strong practicability and wide applicability.
Detailed description of the invention
Fig. 1 is the schematic diagram of modification theory of the invention.
Specific embodiment：
Specific introduce is made to the present invention below in conjunction with the drawings and specific embodiments.
Reagent used in the embodiment of the present invention is commercially available.
Dimethylbenzene used in the present embodiment is to analyze pure dimethylbenzene, and ethyl alcohol is to analyze pure dehydrated alcohol, and all reagents are equal
It is commercially available.
Ultrasonic dispersing machine, model：TJS-300, producer：Hangzhou Success Ultrasonic Equipment Co., Ltd
Planetary stirrer, model：15L, producer：Shandong Long Xing chemical machinery Group Co., Ltd
The present invention will be described combined with specific embodiments below, so that those skilled in the art's reference book being capable of evidence
To implement.
A kind of method of modifying of the graphene suitable for methyl phenyl silicone oil material, includes the following steps：
S1, dispersion：It takes 100g graphene to be placed in 5L beaker, 1900g dimethylbenzene is added, is put into ultrasonic wave dispersing apparatus
In, supersonic frequency is set as 40-50KHz, disperses 10min, is formed and is starched by uniform, the stable graphene of dispersing agent of dimethylbenzene
Liquid；
S2, modification：400 parts of dehydrated alcohols, 3.5g phenyl triethoxysilane, 1.5g parts of γ-glycidyl ether oxygens are added
Propyl trimethoxy silicane, 2g part nonylphenol polyoxyethylene ether, using planetary stirrer under the speed of 1800r/min, high speed
Disperse 3-5min, 4g deionized water is added and continues with the Rate Dispersion 3-5min of 1800r/min, it will using the dilute hydrochloric acid of 1mol/L
PH value is adjusted to 5, is again stirring for 30min, obtains modified graphene mixed liquor；
PH value is adjusted to 5, under acid condition, H+Phenyl triethoxysilane and γ-glycidyl ether oxygen third can be catalyzed
Base trimethoxy silane is reacted with the hydroxyl of graphene surface, is accelerated reaction rate, is modified graphene sufficiently.
S3, using dimethylbenzene as detergent, filtering and washing 4-6 is carried out all over to neutral to modified graphene mixed liquor, it is every all over using
500g dimethylbenzene；100g dehydrated alcohol is added in the 5th time filtrate, 10g deionized water is added to be uniformly mixed, measures pH value, if
Neutrality can then carry out next step, then continue to wash if acidity；
PH value is the effect of neutrality：Modified graphene under acid condition, is entrained in high molecular material, can accelerate high score
The cracking aging of sub- material, influences the operation stability of material, therefore to restore after the completion of being modified to neutrality.
After completing washing, it is put into vacuum drying oven, is put into phosphorus pentoxide 20g in an oven, phosphorus pentoxide and water have pole
High reactivity can absorb a small amount of moisture evaporated from modified graphene because vacuum is heated.Temperature, which is arranged, is
120-140 DEG C, it is evacuated to -0.09MPa, keeps 1h；Vacuum degree situation of change is observed, if vacuum degree declines, continues to take out true
Empty extremely -0.09MPa, holding 1-3h, closing temperature after the retention time, to prevent modified graphene from aoxidizing at high temperature, to
Vacuum is bled off near 60 DEG C of temperature or less, modified graphene is made.
Preferably, graphene is the graphene of reduction method preparation.
The graphene surface that method of the invention is modified contains epoxy group and phenyl, can be in the benzene of ultraviolet ageing resisting
Disperse in base silica gel or silicone resin, while the synergistic effect between phenyl can also play the conductive and heat-conductive characteristic of graphene, it can and can
For methyl phenyl silicone resin and the ageing-resistant corrosion-inhibiting coating of methyl phenyl silicone rubber class.
Centrefuge experiment：
The modified graphene that embodiment is obtained, is dispersed in methyl phenyl silicone oil, after being uniformly dispersed, is centrifuged
Experiment, investigates dispersion stabilization of the graphene in corresponding system, and experimental result is as shown in table 1.
Table 1 is dispersion of the modified graphene under organosilicon systems
| Xiang Lie | Centrifugal speed | Centrifugation time | Organosilicon systems | Discrete state |
| Parameter | 10000r/min | 20min | Methyl phenyl silicone oil | Without layering |
Seen from table 1, the dispersion stabilization that can be used to characterize graphene by centrefuge experiment, the revolving speed that centrifuge is arranged are
10000r/min, time 10min, if graphene disperses unstable in organosilicon, the different compounding substances of specific gravity exist
Will appear layering under the action of centrifugal force, illustrate that the system of graphene and organosilicon is not sufficiently stable at this time, if graphene with it is organic
The mixed system of polymeric silicon is stablized, then is still uniform substance after being centrifuged.
Dispersion stabilization of the graphene in organosilicon is excellent, illustrates that graphene and organosilicon macromolecule pass through intermolecular work
Firmly and covalent bond effect forms the entirety of stable homogeneous, can make graphene-based organosilicon macromolecule composite material long term storage
Still there is excellent stability afterwards：
It such as, can be to phenyl in high temperature resistant that graphene uniform was stable be entrained in, low temperature resistant, radiation hardness type phenyl siloxane rubber
The characteristics of silicon rubber plays reinforcing effect, makes up phenyl siloxane rubber bad mechanical property.
In of the invention and the present embodiment,
Contain phenyl ring in dimethylbenzene, be good nonpolar solvent, graphene has good dispersion effect in dimethylbenzene
Fruit, therefore dispersing agent of the dimethylbenzene as graphene can be used.
The graphene that graphene takes reduction method to prepare, surface usually contain a small amount of hydroxyl (- OH) or epoxy group (Phenyl triethoxysilane and γ-glycidyl ether oxygen propyl trimethoxy silicane are silane coupling agent, can be with
The hydroxyl of graphene surface reacts, and vinyl is contained on the modified graphene surface of formationEpoxy group (Ether (- O-), wherein the pi bond collective effect of the pi bond of phenyl and graphene itself, enriched move freely electricity
Son weakens the modified negative effect to the graphene conductive capacity of heat transmission, enhances the compatibility with phenyl siloxane rubber, epoxy group
Can be by the interaction force of effect the enhancing graphene and organosilicon macromolecule of hydrogen bond with ether, and then increase graphene
Dispersion stabilization in silicon rubber.
Using nonylphenol polyoxyethylene ether as emulsifier, deionized water can be made evenly dispersed in dimethylbenzene (oily phase).
The hydroxyl of phenyl triethoxysilane and γ-glycidyl ether oxygen propyl trimethoxy silicane and graphene surface is anti-
Answer it is removable be divided into two steps, the first step is phenyl triethoxysilane and γ-glycidyl ether oxygen propyl trimethoxy silicane and water
Hydrolysis occurs and generates silanol, contains silicone hydroxyl (- Si-OH) in silanol, second step is the hydroxyl of silanol and graphene surface
Reaction, realize graphene surface grafted-organosilicon segment, emulsifier nonylphenol polyoxyethylene ether make deionized water with it is silane coupled
Agent and graphene uniform contact, and the modified related chemistry reaction of graphene can uniformly occur in mixed system, can be reduced and do not changed
Property graphene residual.
Modified graphene need to pass through filtering and washing, to remove non-grafted silane coupling agent on the surface of graphene, emulsification
Agent, the remaining water of hydrochloric acid and part, are finally dried, and phosphorus pentoxide, five oxidations two are added when dry in vacuum drying oven
Phosphorus and water have high reactivity, can absorb a small amount of moisture evaporated from modified graphene because vacuum is heated.
It finally can get pure vinyl triethoxysilane and γ-glycidyl ether oxygen propyl trimethoxy silicane modified graphene.
The basic principles, main features and advantages of the invention have been shown and described above.The technical staff of the industry should
Understand, the above embodiments do not limit the invention in any form, all obtained by the way of equivalent substitution or equivalent transformation
Technical solution is fallen within the scope of protection of the present invention.
Claims (9)
1. a kind of method of modifying of the graphene suitable for methyl phenyl silicone oil material, which is characterized in that include the following steps：
S1, certain mass component is pressed, by graphene ultrasonic disperse in dimethylbenzene, forms graphene slurries；
S2, certain mass component is pressed, dehydrated alcohol, phenyl triethoxysilane, γ-glycidol is added into graphene slurries
Ether oxygen propyl trimethoxy silicane, nonylphenol polyoxyethylene ether, polyalcohol after stirring, are added deionized water and adjust pH value, then
Secondary stirring；
After dry, modified graphene is made in S3, washing to neutrality.
2. a kind of method of modifying of graphene suitable for methyl phenyl silicone oil material according to claim 1, feature
It is, the supersonic frequency is 40-50KHz, jitter time 10-30min.
3. a kind of method of modifying of graphene suitable for methyl phenyl silicone oil material according to claim 1, feature
It is, the revolving speed stirred in the step S2 is 1800r/min, and mixing time 3-5min, the time being again stirring for is 20-
40min。
4. a kind of method of modifying of graphene suitable for methyl phenyl silicone oil material according to claim 1, feature
It is, the pH value in the step S2 is adjusted to 4-5.
5. a kind of method of modifying of graphene suitable for methyl phenyl silicone oil material according to claim 1, feature
It is, the detergent in the step S3 is dimethylbenzene, depressurizes filtering and washing, and pass is 4-6 times.
6. a kind of method of modifying of graphene suitable for methyl phenyl silicone oil material according to claim 1, feature
It is, the drying temperature in the step S3 is 120-140 DEG C, is evacuated to -0.09MPa, drying time 1-4h.
7. a kind of method of modifying of graphene suitable for methyl phenyl silicone oil material according to claim 1, feature
It is, the drying in the step S3, environment is -0.09MPa vacuum state.
8. a kind of method of modifying of graphene suitable for methyl phenyl silicone oil material according to claim 1, feature
It is, the quality component in the step S1 includes：100 parts of graphene；
Quality component in the step S2 includes：1600-1900 parts of dimethylbenzene, 100-400 parts of dehydrated alcohol, three ethoxy of phenyl
1-4 parts of base silane, γ -1-3 parts of glycidyl ether oxygen propyl trimethoxy silicane, 1-3 parts of nonylphenol polyoxyethylene ether, deionization
1-5 parts of water.
9. a kind of method of modifying of the graphene suitable for methyl phenyl silicone oil material according to right 1, which is characterized in that
The graphene is the graphene of reduction method preparation.
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| CN111378208A (en) * | 2020-02-19 | 2020-07-07 | 广州奥翼材料与器件研究院有限公司 | Graphene heat conduction material and preparation method thereof |
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