CN108503890A - The preparation method of organosilicon functionalization boron nitride nanosheet - Google Patents
The preparation method of organosilicon functionalization boron nitride nanosheet Download PDFInfo
- Publication number
- CN108503890A CN108503890A CN201810326080.8A CN201810326080A CN108503890A CN 108503890 A CN108503890 A CN 108503890A CN 201810326080 A CN201810326080 A CN 201810326080A CN 108503890 A CN108503890 A CN 108503890A
- Authority
- CN
- China
- Prior art keywords
- boron nitride
- organosilicon
- preparation
- amination
- functionalization
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The invention discloses a kind of preparation methods of organosilicon functionalization boron nitride nanosheet, and this method comprises the following steps：By boron nitride powder amination, amination boron nitride is obtained；The amination boron nitride and organosilicon reaction that will be obtained obtain organosilicon functionalization boron nitride nanosheet.Solubility and dispersibility of the boron nitride nanosheet in matrix are further improved simultaneously, improves doping concentration of the boron nitride nanosheet in matrix.
Description
Technical field
The present invention relates to the preparation fields of boron nitride nanosheet.More particularly, to a kind of organosilicon functionalization boron nitride
The preparation method of nanometer sheet.
Background technology
Boron nitride (BN), a kind of important iii-v chemical combination being made of triels boron and pentels nitrogen
Object.Boron nitride has the excellent physical and chemical performance such as broad-band gap, high heat conductance, inoxidizability, high temperature, high frequency, it is high-power,
Photoelectron and radioresistance etc. have huge application prospect.Therefore, the preparation of boron nitride nanosheet, the survey of nanostructure
Amount, the assembling of nano-device, test of boron nitride enhancing ceramics and light, electric property etc. are as current field of inorganic nano material
Important research direction.Boron nitride nanometer material includes quantum dot, nano wire, nanobelt, nanotube, nanometer sheet, nanocrystalline etc.,
Traditional preparation method includes mechanical stripping method, arc discharge method, laser ablation method, ball-milling method, plasma jet method, chemistry
Vapour deposition process etc..Because single nano material can not put into actual use in, it is therefore desirable to by nano material with have
Machine or inorganic matrix are doped, and are prepared into composite material and device.If directly carrying out physical blending, doping can be caused uneven
The drawbacks such as even, bad dispersibility.Therefore it needs to carry out suitable functionalization to nano material to improve its solubility in matrix
And dispersion degree.
Accordingly, it is desirable to provide a kind of new method by boron nitride functionalization, to improve above-mentioned problem.
Invention content
The purpose of the present invention is to provide a kind of preparation methods of organosilicon functionalization boron nitride nanosheet, realize nitrogen
Change boron nanometer sheet organic functional, improves solubility and dispersibility of the boron nitride nanosheet in matrix, improve the nitrogen
Change doping concentration of the boron nanometer sheet in matrix.
In order to achieve the above objectives, the present invention provides a kind of preparation method of organosilicon functionalization boron nitride nanosheet, the party
Method includes the following steps：
By boron nitride powder amination, amination boron nitride is obtained；
The amination boron nitride and organosilicon reaction that will be obtained obtain organosilicon functionalization boron nitride nanosheet.
In above-mentioned preparation method, boron nitride powder granularity is preferably between 2-5 μm, by first by boron nitride in this method
Amination, then by amination boron nitride and organosilicon reaction, obtained organosilicon functionalization boron nitride nanosheet has in matrix
There is high doping concentration.Wherein, the matrix may include and be not limited to vinyl alcohol, methyl methacrylate, methyl triethoxy
Silane, aminopropyl triethoxysilane etc..
Preferably, described by the amidized method of boron nitride powder includes but not limited to one of the following two kinds method：
Boron nitride powder is mixed, the ball milling under inert protective gas atmosphere with amino organic compounds, washed, after dry
Obtain the amination boron nitride；Or,
Boron nitride powder is subjected to microwave treatment in 0.3Pa or less under ammonia atmosphere, obtains the amination boron nitride.
In the above method, boron nitride powder amination can be improved by yield using ball-milling method.
Preferably, the mass ratio of the amino organic compounds and boron nitride powder is more than 1:1.
Preferably, the amino organic compounds are selected from one or more of urea, tetraethylenepentamine, triphenylamine；
Preferably, the time of the ball milling is more than 6h, and ball milling temperature is 0-150 DEG C；
Preferably, preferably but do not include selected from epoxy group, carboxylic containing the group that can be reacted with amino on the organosilicon
One or more of base, isocyanate groups.
Preferably, the isocyanate groups are selected from 3- isocyanate group propyl trimethoxy silicane, 3- isocyanate group
One or more of propyl-triethoxysilicane.
Preferably, the amination boron nitride includes the following steps with reacting for organosilicon：By the amination boron nitride
Back flow reaction is carried out under inert protective gas atmosphere in solvent with organosilicon, after reaction, purified, centrifugation is had
The dispersion liquid of machine functional silicon boron nitride nanosheet.It is appreciated that after removal solvent, pure organosilicon functionalization boron nitride is obtained
Nanometer sheet.Wherein, the removal of solvent can be the conventional means of this field, such as evaporation, and this will not be repeated here.
Preferably, the inert protective gas is selected from nitrogen, argon gas.
Preferably, the condition of the back flow reaction is：25-100 DEG C of temperature, time 3-24h.
Preferably, by weight, the additive amount of the amination boron nitride is 1-50 parts, the additive amount of the organosilicon
It is 10-100 parts.
Preferably, the solvent is selected from the mixing of one or more of acetone, petroleum ether, ethyl alcohol.
It is highly preferred that by weight, the additive amount of the amination boron nitride is 1-50 parts, the addition of the organosilicon
Amount is 10-100 parts, and the additive amount of the solvent is 10-200 parts.
Beneficial effects of the present invention are as follows：
The present invention removes boron nitride powder at boron nitride nanosheet, can obtain a large amount of boron nitride nanosheets.
The preparation method of the present invention is realized boron nitride nanosheet organic functional, is improved the boron nitride nanosheet and is existed
Solubility in matrix and dispersibility improve doping concentration of the boron nitride nanosheet in matrix.
The method provided by the present invention for preparing organosilicon functionalization boron nitride nanosheet has preparation method applicability
Extensively, the features such as easy to operate.
Description of the drawings
Specific embodiments of the present invention will be described in further detail below in conjunction with the accompanying drawings.
Fig. 1 shows the schematic diagram that organosilicon functionalization boron nitride nanosheet is prepared in embodiment 1.
Fig. 2 shows the Fourier of the amination boron nitride prepared in embodiment 1, organosilicon functionalization boron nitride nanosheet
Infrared spectrum.
Fig. 3 shows amination boron nitride nanosheet (a) and organosilicon functionalization boron nitride nanosheet (b) in embodiment 1
Transmission electron microscope photo.
Fig. 4 shows dispersion liquid photo of the organosilicon functionalization boron nitride nanosheet in petroleum ether in embodiment 1.
Fig. 5 shows the organic glass of the obtained doping 0.1wt% organosilicon functionalization boron nitride nanosheets of embodiment 1
Composite material photo.
Fig. 6 shows the dispersion liquid photo of 2 organosilicon functionalization boron nitride nanosheet of embodiment in ethanol.
Fig. 7 shows the organic glass of the obtained doping 0.5wt% organosilicon functionalization boron nitride nanosheets of embodiment 3
Composite material photo.
Fig. 8 shows the photo of the dispersion liquid of 1 boron nitride powder of comparative example in water.
Fig. 9 shows that comparative example 5 adulterates the organic glass composite material photo of non-functionalization boron nitride nanosheet.
Figure 10 shows that comparative example 6 adulterates the organic glass composite material photograph of the non-functionalization boron nitride nanosheets of 0.5wt%
Piece.
Specific implementation mode
In order to illustrate more clearly of the present invention, the present invention is done further with reference to preferred embodiments and drawings
It is bright.Similar component is indicated with identical reference numeral in attached drawing.It will be appreciated by those skilled in the art that institute is specific below
The content of description is illustrative and be not restrictive, and should not be limited the scope of the invention with this.
Embodiment 1
The preparation method of organosilicon functionalization boron nitride nanosheet, includes the following steps：
In a nitrogen atmosphere, boron nitride powder 40g, urea 80g are added in 1# ball mills, ball milling 15h at 0 DEG C takes out
Mixture after ball milling；Make to be washed with deionized, it is dry, obtain amination boron nitride.
25g amination boron nitride is weighed, 100ml petroleum ethers and the amination boron nitride weighed are added in reactor 2#,
Ultrasonic 60min obtains milk-white coloured suspension, 50g 3- isocyanate group propyl-triethoxysilicanes is added, in 100 DEG C of temperature
Under the conditions of persistently stir, reflow treatment is for 24 hours；After reaction, it with petroleum ether, centrifuges, obtains under 12000rpm rotating speeds
The petroleum ether dispersion liquid of the boron nitride nanosheet of organosilicon functionalization, solubility 0.5mg/ml.Nanometer sheet grain size is 100nm,
Lamellar spacing is 3nm.It is as shown in Figure 1 to react schematic diagram.
Referring to attached drawing 2, it is the amination boron nitride prepared in embodiment 1, organosilicon functionalization boron nitride nanosheet
Fourier's infrared spectrum；It can be seen from the figure that in 1373.6cm-1Place and 816.5cm-1The characteristic absorption peak at place corresponds to respectively
The out-of-plane bending vibration of stretching vibration and B-N-B in the faces B-N of boron nitride；In 3443cm-1It is due to sample to locate corresponding absorption peak
Caused by water in product adsorption air；For the infrared spectrum of amination boron nitride, it can be seen that in the absorption peak in water
Neighbouring 3240cm-1There are one absorption peaks at place, are caused by N-H key stretching vibrations；For the infrared of organosilicon functionalization boron nitride
Spectrum, it can be seen that in 3240cm-1The absorption peak at place disappears, and in 1081cm-1、1695cm-1、2927cm-1Locate the absorption occurred
Peak corresponds to Si-O keys, amido bond and alkane bond respectively, this demonstrate that the presence of 3- isocyanates propyl diester triethoxysilanes, and
It does not find in 2272cm-1Nearby there is the absorption peak of isocyanate group, illustrates thoroughly to eliminate unreacted organosilicon, go out simultaneously
The corresponding absorption peak of amido bond is showed, has illustrated that the amino on boron nitride is chemically reacted with isocyanate group, show successfully to make
The boron nitride nanosheet of organosilicon functionalization is obtained, nanometer sheet grain size is 130nm, lamellar spacing 5nm.
Referring to attached drawing 3, it is the transmission electron microscope of amination boron nitride nanosheet and organosilicon functionalization boron nitride nanosheet
Photo；The boron nitride nanosheet prepared as can be seen from Figure is two-dimensional slice structure, and lamellar spacing is smaller, the edge of nanometer sheet
Place crimps.
Referring to attached drawing 4, it is dispersion liquid photo of the organosilicon functionalization boron nitride nanosheet in petroleum ether.It is shone in laser
It penetrates down it can be seen that apparent Tyndall effect, it was demonstrated that form stable dispersion liquid.
Organosilicon functionalization boron nitride nanosheet is doped to methyltriethoxysilane matrix by sol-gel method
In, the specific method is as follows：
Obtained dispersion liquid is mixed with methyltriethoxysilane monomer, after reaction, reaction product curing molding obtains
To the organic glass composite material for adulterating organic functional silicon boron nitride nanosheet.
Referring to attached drawing 5, it is that the obtained organic glass for adulterating 0.1wt% organosilicon functionalization boron nitride nanosheets is multiple
Condensation material photo, it can be seen that organosilicon functionalization boron nitride nanosheet is uniformly dispersed in the composite, does not observe nanometer
The clustering phenomena of piece.The haze value of organic glass can be used for weighing degree of scatter of the nano material in matrix, and haze value is got over
The dispersibility of low then material is better.The haze value of this glass is 13.1%.It is to be appreciated that in this attached drawing, English alphabet is only to carry on the back
Word on scape paper, can be used for the degree of scatter of the light transmission and nano material of intuitive observation glass in matrix, and nothing
Other meanings.Similarly hereinafter attached drawing 7,9 and 10.
Embodiment 2
The preparation method of organosilicon functionalization boron nitride nanosheet, includes the following steps：
In a nitrogen atmosphere, boron nitride powder 20g, tetraethylenepentamine 100g are added in 1# ball mills, ball milling at 150 DEG C
20h takes out mixture after ball milling；Make to be washed with deionized, it is dry, obtain amination boron nitride.
10g amination boron nitride is weighed, 50ml petroleum ethers and the amination boron nitride weighed are added in reactor 2#, is surpassed
Sound 40min obtains milk-white coloured suspension, 40g 3- isocyanate group propyl trimethoxy silicanes is added, in 70 DEG C of temperature strip
It is persistently stirred under part, reflow treatment 10h；After reaction, solvent petroleum ether is removed by rotating device, after being washed with ethyl alcohol,
It is centrifuged under 5000rpm rotating speeds, obtains the alcohol dispersion liquid of the boron nitride nanosheet of organosilicon functionalization, solubility 1.3mg/
Ml, nanometer sheet grain size are 90nm, lamellar spacing 2nm.
Organosilicon functionalization boron nitride nanosheet obtained by embodiment 2 is entrained in as sol-gel method identical poly-
In polymer matrix, the effect reached is close with embodiment 1, and haze value is 11.4% when doping concentration is 0.1wt%.
Referring to attached drawing 6, it is the dispersion liquid photo of organosilicon functionalization boron nitride nanosheet in ethanol.In laser irradiation
Down it can be seen that apparent Tyndall effect, it was demonstrated that form stable dispersion liquid.
Embodiment 3
The preparation method of organosilicon functionalization boron nitride nanosheet, includes the following steps：
In a nitrogen atmosphere, boron nitride powder 2g, triphenylamine 20g are added in 1# ball mills, ball milling 10h, takes at room temperature
Go out mixture after ball milling；Using deionized water, wash, it is dry, obtain amination boron nitride.
1g amination boron nitride is weighed, 10ml acetone and the amination boron nitride weighed are added in reactor 2#, ultrasound
10min obtains milk-white coloured suspension, 10g 3- isocyanate group propyl-triethoxysilicanes is added, in 25 DEG C of temperature condition
Lower lasting stirring, reflow treatment 3h；After reaction, it is washed using acetone, is centrifuged under 500rpm rotating speeds, obtain organosilicon work(
The acetone dispersion liquor of the boron nitride nanosheet of energyization, solubility 1.4mg/ml.Nanometer sheet grain size is 110nm, and lamellar spacing is
1nm。
Organosilicon functionalization boron nitride nanosheet is doped to aminopropyl triethoxysilane matrix by sol-gel method
In, method is the same as embodiment 2.
Referring to attached drawing 7, it is that the obtained organic glass for adulterating 0.5wt% organosilicon functionalization boron nitride nanosheets is multiple
Condensation material photo, it can be seen that the concentration of the organosilicon functionalization boron nitride nanosheet of doping reaches 0.5wt%, and nanometer sheet exists
Evenly dispersed in matrix, glass haze value is 16.2%.
Embodiment 4
The preparation method of organosilicon functionalization boron nitride nanosheet, includes the following steps：
It takes 2g boron nitride powders to be placed in micro-wave oven, and is evacuated to low pressure 0.1Pa, be passed through 30sccm ammonias, microwave treatment
Amination boron nitride is obtained after 20min.
2g amination boron nitride is weighed, 20ml acetone and the amination boron nitride weighed are added in reactor 2#, ultrasound
15min obtains milk-white coloured suspension, 15g 3- isocyanate group propyl-triethoxysilicanes is added, in 50 DEG C of temperature condition
Lower lasting stirring, reflow treatment 5h；After reaction, it is washed using acetone, is centrifuged under 1000rpm rotating speeds, obtain organosilicon
The acetone dispersion liquor of the boron nitride nanosheet of functionalization, solubility 1.8mg/ml.Nanometer sheet grain size is 130nm, lamellar spacing
For 1.4nm.
4 gained organosilicon functionalization boron nitride nanosheet of embodiment is doped to three ethoxy of methyl by sol-gel method
In base silane matrix, for method with embodiment 1, the effect reached is close with embodiment 1, and when doping concentration is 0.1wt%
Haze value is 10.3%.
Comparative example 1
Embodiment 1 is repeated, difference lies in, change organosilicon functionalization boron nitride nanosheet into boron nitride powder, remaining
Part is constant, and boron nitride powder is dissolved in water.
The solubility of the boron nitride powder of the non-functionalization of gained in water is 0.002mg/ml.
Referring to attached drawing 8, it is the photo of the dispersion liquid of boron nitride powder in water.It can see from picture, boron nitride
The solubility of powder in water is extremely low, and most of powder is all precipitated.
Comparative example 2
Embodiment 1 is repeated, difference lies in the boron nitride that organosilicon functionalization boron nitride nanosheet is changed into non-functionalization is received
Rice piece, remaining condition is constant, and the boron nitride nanosheet of non-functionalization is dissolved in petroleum ether.Wherein, the nitrogen of non-functionalization
The preparation method for changing boron nanometer sheet is as follows：
A certain amount of boron nitride powder is taken, is disperseed in a solvent, in high-power lower ultrasound a period of time.Obtained by after ultrasound
Dispersion liquid centrifuged under certain rotating speed, finally obtain non-functionalization boron nitride nanosheet dispersion liquid.Solvent can pass through revolving
Or be distilled off, obtain nanometer sheet powder.
Solubility of the boron nitride nanosheet of the non-functionalization of gained in petroleum ether is 0.13mg/ml.
Comparative example 3
Embodiment 2 is repeated, difference lies in the boron nitride that organosilicon functionalization boron nitride nanosheet is changed into non-functionalization is received
Rice piece, remaining condition is constant, and in ethanol by the dissolving of the boron nitride nanosheet of non-functionalization.Wherein, the nitridation of non-functionalization
The preparation method of boron nanometer sheet is the same as comparative example 1.The solubility of organosilicon functionalization boron nitride nanosheet in ethanol is more than non-work(
Its solubility of the boron nitride nanosheet of energyization is 1mg/ml.
Comparative example 4
Embodiment 3 is repeated, difference lies in the boron nitride that organosilicon functionalization boron nitride nanosheet is changed into non-functionalization is received
Rice piece, remaining condition is constant, and in acetone by the dissolving of the boron nitride nanosheet of non-functionalization.Wherein, the nitridation of non-functionalization
The preparation method of boron nanometer sheet is the same as comparative example 1.The solubility of organosilicon functionalization boron nitride nanosheet in acetone is more than non-work(
The boron nitride nanosheet of energyization, corresponding solubility are 0.7mg/ml.
Comparative example 5
Embodiment 1 is repeated, difference lies in adulterate 1 non-functionalization boron nitride nanosheet of comparative example by sol-gel method
Into methyltriethoxysilane matrix, specific method is the same as embodiment 1.
Referring to attached drawing 9, it is the organic glass composite material photo for adulterating non-functionalization boron nitride nanosheet, it can be seen that
Nanometer sheet has apparent clustering phenomena in the composite, and doping concentration only has 0.1wt%.Haze value is 54.7%.
Comparative example 6
Embodiment 3 is repeated, difference lies in be doped to ammonia third by non-functionalization boron nitride nanosheet by sol-gel method
In ethyl triethoxy silicane alkyl matter, specific method is the same as embodiment 3.
Referring to attached drawing 10, it is the organic glass composite material photo for adulterating the non-functionalization boron nitride nanosheets of 0.5wt%,
It can be seen that nanometer sheet has apparent clustering phenomena in the composite.Haze value is 70.6%.
Obviously, the above embodiment of the present invention be only to clearly illustrate example of the present invention, and not be pair
The restriction of embodiments of the present invention may be used also on the basis of the above description for those of ordinary skill in the art
To make other variations or changes in different ways, all embodiments can not be exhaustive here, it is every to belong to this hair
Row of the obvious changes or variations that bright technical solution is extended out still in protection scope of the present invention.
Claims (10)
1. the preparation method of organosilicon functionalization boron nitride nanosheet, which is characterized in that include the following steps：
By boron nitride powder amination, amination boron nitride is obtained；
The amination boron nitride and organosilicon reaction that will be obtained obtain organosilicon functionalization boron nitride nanosheet.
2. preparation method according to claim 1, which is characterized in that described to be selected from the amidized method of boron nitride powder
One of the following two kinds method：
Boron nitride powder is mixed, the ball milling under inert protective gas atmosphere with amino organic compounds, washed, institute is obtained after dry
State amination boron nitride；Or,
Boron nitride powder is subjected to microwave treatment in 0.3Pa or less under ammonia atmosphere, obtains the amination boron nitride.
3. preparation method according to claim 2, which is characterized in that the amino organic compounds and boron nitride powder
Mass ratio is more than 1:1.
4. preparation method according to claim 2, which is characterized in that the amino organic compounds are selected from urea, tetrem
One or more of five amine of alkene, triphenylamine.
5. preparation method according to claim 2, which is characterized in that the time of the ball milling is more than 6h, and ball milling temperature is
0-150℃。
6. preparation method according to claim 1, which is characterized in that contain the base that can be reacted with amino on the organosilicon
Group；Preferably, the group that can be reacted with amino is selected from one or more of isocyanate groups, epoxy group, carboxyl；More
Preferably, the isocyanate groups are selected from 3- isocyanate group propyl trimethoxy silicane, three second of 3- isocyanate group propyl
One or more of oxysilane.
7. preparation method according to claim 1, which is characterized in that the amination boron nitride reacts packet with organosilicon
Include following steps：The amination boron nitride and organosilicon under inert protective gas atmosphere flow back instead in solvent
It answers, after reaction, purified, centrifugation obtains the dispersion liquid of organosilicon functionalization boron nitride nanosheet.
8. preparation method according to claim 7, which is characterized in that the condition of the back flow reaction is：Temperature 25-100
DEG C, time 3-24h.
9. preparation method according to claim 1 or claim 7, which is characterized in that by weight, the amination boron nitride
Additive amount is 1-50 parts, and the additive amount of the organosilicon is 10-100 parts.
10. preparation method according to claim 7, which is characterized in that the solvent is in acetone, petroleum ether, ethyl alcohol
One or more of mixing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810326080.8A CN108503890B (en) | 2018-04-12 | 2018-04-12 | Preparation method of organic silicon functionalized boron nitride nanosheet |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810326080.8A CN108503890B (en) | 2018-04-12 | 2018-04-12 | Preparation method of organic silicon functionalized boron nitride nanosheet |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108503890A true CN108503890A (en) | 2018-09-07 |
| CN108503890B CN108503890B (en) | 2021-04-02 |
Family
ID=63381961
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810326080.8A Active CN108503890B (en) | 2018-04-12 | 2018-04-12 | Preparation method of organic silicon functionalized boron nitride nanosheet |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108503890B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109810544A (en) * | 2018-12-29 | 2019-05-28 | 厦门大学 | A kind of amination hexagonal boron nitride and its preparation method and application |
| CN109852044A (en) * | 2018-12-06 | 2019-06-07 | 安徽集虹材料科技有限公司 | Thermally conductive nylon of a kind of boron nitride orientation and preparation method thereof |
| CN112679801A (en) * | 2020-12-15 | 2021-04-20 | 中国科学院理化技术研究所 | Organic silicon functionalized antimonene nanosheet and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002161A (en) * | 2010-09-21 | 2011-04-06 | 中国科学院长春应用化学研究所 | Preparation method of aminosilane-functionalized graphene reinforced silica gel |
| CN102351174A (en) * | 2011-08-23 | 2012-02-15 | 华南理工大学 | Preparation method of dispersible silane functionalized graphene |
| CN107501610A (en) * | 2017-08-30 | 2017-12-22 | 桂林电子科技大学 | A kind of composite heat interfacial material based on boron nitride and preparation method thereof |
| CN110016227A (en) * | 2019-05-05 | 2019-07-16 | 合肥工业大学 | A kind of nylon composite materials and preparation method thereof containing secondary surface modifying stuffing |
-
2018
- 2018-04-12 CN CN201810326080.8A patent/CN108503890B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102002161A (en) * | 2010-09-21 | 2011-04-06 | 中国科学院长春应用化学研究所 | Preparation method of aminosilane-functionalized graphene reinforced silica gel |
| CN102351174A (en) * | 2011-08-23 | 2012-02-15 | 华南理工大学 | Preparation method of dispersible silane functionalized graphene |
| CN107501610A (en) * | 2017-08-30 | 2017-12-22 | 桂林电子科技大学 | A kind of composite heat interfacial material based on boron nitride and preparation method thereof |
| CN110016227A (en) * | 2019-05-05 | 2019-07-16 | 合肥工业大学 | A kind of nylon composite materials and preparation method thereof containing secondary surface modifying stuffing |
Non-Patent Citations (1)
| Title |
|---|
| WEIWEI LEI 等: "Boron nitride colloidal solutions, ultralight aerogels and freestanding membranes through one-step exfoliation and functionalization", 《NATURE COMMUNICATIONS》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109852044A (en) * | 2018-12-06 | 2019-06-07 | 安徽集虹材料科技有限公司 | Thermally conductive nylon of a kind of boron nitride orientation and preparation method thereof |
| CN109810544A (en) * | 2018-12-29 | 2019-05-28 | 厦门大学 | A kind of amination hexagonal boron nitride and its preparation method and application |
| CN112679801A (en) * | 2020-12-15 | 2021-04-20 | 中国科学院理化技术研究所 | Organic silicon functionalized antimonene nanosheet and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108503890B (en) | 2021-04-02 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108503890A (en) | The preparation method of organosilicon functionalization boron nitride nanosheet | |
| CN110093680B (en) | Graphene/cage type polysilsesquioxane modified polyester fiber and preparation method thereof | |
| CN105980307B (en) | Silica particles, resin composition containing the same, and use thereof | |
| CN105542228A (en) | Preparation method of functionalized nano-silica based on graphene | |
| CN109778335B (en) | Modified polypropylene fiber and preparation method thereof | |
| CN109913968B (en) | Antibacterial polypropylene fiber and preparation method thereof | |
| CN101475179B (en) | Preparation of organic-inorganic hybridization silicon oxide nanosphere | |
| CN110343406A (en) | A kind of fluorine containing silane modified graphene oxide and its preparation method and application | |
| CN106832707A (en) | The preparation method of copper metal organic frame/polyvinyl alcohol nano composite membrane | |
| CN112662354A (en) | Silicon dioxide filler, preparation method thereof and epoxy resin composite material | |
| CN112608565A (en) | High-thermal-conductivity graphene heat dissipation film and preparation method thereof | |
| CN106589390A (en) | Modification method for nano-crystalline cellulose crystal hydrophobic grafting | |
| CN103059343B (en) | Modified carbon nanotube and preparation method thereof | |
| CN113683818A (en) | Core-shell structure modified boron nitride and preparation method thereof | |
| CN102875844B (en) | Modified carbon nano tube and preparation method thereof | |
| CN108192137B (en) | Preparation method of high-dispersion carbon nano tube used as rubber filler | |
| CN108409591B (en) | Star-shaped carboxylic acid group zwitterionic compound and preparation method and application thereof | |
| CN112876685B (en) | Tetraepoxy group liquid cage type silsesquioxane as well as preparation method and application thereof | |
| CN108912334A (en) | A kind of preparation method of the hydrophobic silicone nanoparticle containing vinyl | |
| CN111534130B (en) | Heat-conducting powder modifier, heat-conducting silica gel and preparation method thereof | |
| CN105802488A (en) | Coating containing composite silicone rubber and preparation method of coating | |
| CN114874453B (en) | BN nanosheet modified polycarbosilane and synthesis method thereof | |
| CN111073347A (en) | Preparation method of ultra-dispersed nano white carbon black for rubber filler | |
| CN102875843B (en) | Modified carbon nanotube and preparation method thereof | |
| Kang et al. | A novel surface modification of Sb2O3 nanoparticles with a combination of cationic surfactant and silane coupling agent |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |