CN105111723B - A kind of preparation method of the orderly magnetic boron nitride nanosheet/compound polyurethane material of surface micro-structure - Google Patents

A kind of preparation method of the orderly magnetic boron nitride nanosheet/compound polyurethane material of surface micro-structure Download PDF

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CN105111723B
CN105111723B CN201510627752.5A CN201510627752A CN105111723B CN 105111723 B CN105111723 B CN 105111723B CN 201510627752 A CN201510627752 A CN 201510627752A CN 105111723 B CN105111723 B CN 105111723B
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boron nitride
nitride nanosheet
polyurethane material
compound polyurethane
preparation
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CN105111723A (en
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矫维成
袁凤
王荣国
刘文博
杨帆
郝立峰
徐忠海
赫晓东
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Harbin Institute of Technology
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Harbin Institute of Technology
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Abstract

A kind of preparation method of the orderly magnetic boron nitride nanosheet/compound polyurethane material of surface micro-structure, is related to a kind of preparation method of magnetic boron nitride nanosheet/compound polyurethane material.It is an object of the invention to provide a kind of preparation method of the orderly magnetic boron nitride nanosheet/compound polyurethane material of surface micro-structure.The present invention method be:First, intercalation boron nitride is prepared;2nd, boron nitride nanosheet is prepared;3rd, the boron nitride nanosheet of area load ferroferric oxide magnetic nano-particles is prepared;4th, the orderly magnetic boron nitride nanosheet/compound polyurethane material of surface micro-structure is prepared.The ordered composite material that the present invention is obtained has excellent erosive resistance, relative to unordered boron nitride/compound polyurethane material, pure polyurethane, and its erosive resistance has been respectively increased 31.9%, 51.5%, available for Anti-erosion protective coating.The present invention is applied to nano material processing and applied technical field.

Description

A kind of orderly magnetic boron nitride nanosheet/compound polyurethane material of surface micro-structure Preparation method
Technical field
The present invention relates to a kind of preparation method of magnetic boron nitride nanosheet/compound polyurethane material.
Background technology
Liquid or gas medium carry small solids with certain speed and impact the surface of material and produce Abrasion be referred to as erosive wear.Ore dressing part, flow passage components, main easily worn part, Residue extraction pipeline, the turbine blade of ship Etc. all suffer from serious erosion attack.Relevant information is counted, and the loss that China is caused due to erosion attack every year is up to 40000000000 yuan, therefore, it is badly in need of the knowledge of comprehensive promotion and application erosive wear.
Such as with industrialized process, polymer and its composite gradually show their superiority, excellent Corrosion resistance, high chemical stability, damping sound absorption, low-friction coefficient, water lubrication and non-corrosive etc..These excellent performances make Polymer and composite are gradually applied to Anti-erosion abrasion field, and the gesture of big substituted metal material.
The influence factor of erosive wear is numerous, formation mechenism complex.Metal being directed to current existing research more And its erosive wear behavior of composite, and establish corresponding Erosion Wear Mechanisms model, but for polymer and its The research of the Erosive Properties of composite is then considerably less, and need further explore and research.
It can form that micro-structural is orderly, composite with specific function by aligning for packing material, this The orderly composite of micro-structural is planted to be expected to preferably be applied to Anti-erosion abrasion field.At present, filler is aligned as polymerization The Strengthening and Toughening of thing, which is modified, provides broader space, it has also become the study hotspot of field of nanocomposite materials.The present invention can be The design of composite propeller surface micro-structure, Strengthening and Toughening are applied in terms of being modified, and are also applicable in micro-structural ordered composite material Preparation, bionic composite material design of material etc..
The content of the invention
It is an object of the invention to provide a kind of orderly magnetic boron nitride nanosheet/polyurethane composite of surface micro-structure The preparation method of material.
A kind of preparation method of the orderly magnetic boron nitride nanosheet/compound polyurethane material of surface micro-structure of the invention It is to carry out according to the following steps:
First, 2~6g hexagonal boron nitride powder is added in 100mL~500mL nitration mixture, is 30 DEG C~100 in temperature DEG C, rotating speed is under 1000rpm~2000rpm, continuously stirs 10h~50h, then cooled down, diluted with deionized water, and repetition is taken out Filter, washing to filtrate obtain intercalation boron nitride in neutrality;Wherein, described nitration mixture by mass concentration be 98% dense H2SO4With Mass concentration is 95% dense HNO3It is 1~3 by volume:1 composition;
2nd, the intercalation boron nitride that step one is obtained is scattered in isopropanol, at room temperature, ultrasonically treated 10h~30h, so 15min~50min is centrifuged under rotating speed is 1500rpm~6000rpm, supernatant liquor is taken, and be washed with deionized To neutral, product is placed at 80 DEG C~100 DEG C and dried, boron nitride nanosheet is obtained;The intercalation nitrogen that described step one is obtained It is 1mg to change the quality of boron and the volume ratio of isopropanol:0.5~2mL;
3rd, the boron nitride nanosheet and FeCl obtained step 22·4H2O is scattered in deionized water, is placed in ultrasonic clear It is 60kHz~80kHz to wash in device in hertz, and ultrasonically treated 3h~6h under power 180W~200W obtains boron nitride nanosheet point Dispersion liquid, then at room temperature, in the case where rotating speed is 1000rpm~2000rpm, is slowly added dropwise into boron nitride nanosheet dispersion liquid 5mL~20mL concentration is the 5mg/mL NaOH aqueous solution, and the H that mass concentration is 5.0mg/mL is then added dropwise again2O2The aqueous solution, When solution is changed into black by dusty blue, stops being added dropwise, be then sonicated 5min~30min, carry out Magneto separate, by product point Do not cleaned with deionized water 2~4 times, washes of absolute alcohol 2~5 times, be finally placed in 80 DEG C~100 DEG C of vacuum drying oven and carry out Dry, obtain the boron nitride nanosheet of area load ferroferric oxide magnetic nano-particles;Wherein, described step two is obtained Boron nitride nanosheet and FeCl2·4H2O mass ratio is 1:(0.4~4);The boron nitride nanosheet that described step two is obtained Quality and deionized water volume ratio be (0.001~0.02) g:1mL;
4th, the boron nitride nanosheet that step 3 is obtained into area load ferroferric oxide magnetic nano-particles is dispersed in In DMF, the ultrasound in the case where hertz is 60kHz~80kHz, power 180W~200W is placed in ultrasonic cleaning machine 2h~6h is handled, under nitrogen protection, the polybutylene glyool adipate of dehydration is added in above-mentioned dispersion liquid, in High speed shear 30min~60min under conditions of 8000rpm~15000rpm, then adds 4,4`- diphenylmethane diisocyanates Ester, is 50~80 DEG C in temperature, rotating speed is stirring reaction 0.5h~3h under 1000rpm~2000rpm, finally, into reactor BDO is added, continues to react 0.5h~2h, stops stirring, nitrogen protection is released, reaction solution is poured into warmed-up mark Quasi-mode has, and is placed in 0.4T~1T uniform magnetic field standing 2h~8h, under conditions of 60 DEG C~80 DEG C evaporation solvent 12h~ 24h, then heats to 120 DEG C~150 DEG C, cures 10~20h, and room temperature is placed 1 week, obtains the orderly magnetic nitrogen of surface micro-structure Change boron nanometer sheet/compound polyurethane material;Wherein, described step three obtains area load ferroferric oxide magnetic nano grain The quality of the boron nitride nanosheet of son and the volume ratio of N,N-dimethylformamide are 1~20g:10~50mL;Described step Three obtain the boron nitride nanosheet and the poly adipate succinic acid ester of dehydration of area load ferroferric oxide magnetic nano-particles The mass ratio of glycol is 1~20:40~80;Described step three obtains area load ferroferric oxide magnetic nano-particles The mass ratio of boron nitride nanosheet and 4,4`- '-diphenylmethane diisocyanates is 1~20:100;Described step three obtains surface The mass ratio of the boron nitride nanosheet and 1,4- butanediols that have loaded ferroferric oxide magnetic nano-particles is 1~20:20~60.
The present invention includes following beneficial effect:
The method for the orderly boron nitride/compound polyurethane material of preparation micro-structural that the present invention is provided, technique is simple, power consumption It is few, and obtained ordered composite material has excellent erosive resistance, it is compound relative to unordered boron nitride/polyurethane Material, pure polyurethane, its erosive resistance have been respectively increased 31.9%, 51.5%, available for Anti-erosion protective coating.
Brief description of the drawings
Fig. 1 is to prepare the orderly magnetic boron nitride nanosheet/compound polyurethane material schematic diagram of surface micro-structure;Wherein, 1 For magnetic boron nitride nanosheet;2 be polyurethane;
Fig. 2 is that surface micro-structure prepared by pure polyurethane, unordered boron nitride/compound polyurethane material and experiment one is orderly The Wear rate of boron nitride/compound polyurethane material with the angle of shock change curve;Wherein, 1 ground for the erosion of pure polyurethane Loss rate with the angle of shock change curve;1 for unordered boron nitride/compound polyurethane material Wear rate with the angle of shock change Curve;The Wear rate of the 3 orderly boron nitride/compound polyurethane materials of surface micro-structure prepared for experiment one is with the angle of shock Change curve.
Embodiment
Embodiment one:A kind of orderly magnetic boron nitride nanosheet/poly- ammonia of surface micro-structure of present embodiment The preparation method of ester composite is to carry out according to the following steps:
First, 2~6g hexagonal boron nitride powder is added in 100mL~500mL nitration mixture, is 30 DEG C~100 in temperature DEG C, rotating speed is under 1000rpm~2000rpm, continuously stirs 10h~50h, then cooled down, diluted with deionized water, and repetition is taken out Filter, washing to filtrate obtain intercalation boron nitride in neutrality;Wherein, described nitration mixture by mass concentration be 98% dense H2SO4With Mass concentration is 95% dense HNO3It is 1~3 by volume:1 composition;
2nd, the intercalation boron nitride that step one is obtained is scattered in isopropanol, at room temperature, ultrasonically treated 10h~30h, so 15min~50min is centrifuged under rotating speed is 1500rpm~6000rpm, supernatant liquor is taken, and be washed with deionized To neutral, product is placed at 80 DEG C~100 DEG C and dried, boron nitride nanosheet is obtained;The intercalation nitrogen that described step one is obtained It is 1mg to change the quality of boron and the volume ratio of isopropanol:0.5~2mL;
3rd, the boron nitride nanosheet and FeCl obtained step 22·4H2O is scattered in deionized water, is placed in ultrasonic clear It is 60kHz~80kHz to wash in device in hertz, and ultrasonically treated 3h~6h under power 180W~200W obtains boron nitride nanosheet point Dispersion liquid, then at room temperature, in the case where rotating speed is 1000rpm~2000rpm, is slowly added dropwise into boron nitride nanosheet dispersion liquid 5mL~20mL concentration is the 5mg/mL NaOH aqueous solution, and the H that mass concentration is 5.0mg/mL is then added dropwise again2O2The aqueous solution, When solution is changed into black by dusty blue, stops being added dropwise, be then sonicated 5min~30min, carry out Magneto separate, by product point Do not cleaned with deionized water 2~4 times, washes of absolute alcohol 2~5 times, be finally placed in 80 DEG C~100 DEG C of vacuum drying oven and carry out Dry, obtain the boron nitride nanosheet of area load ferroferric oxide magnetic nano-particles;Wherein, described step two is obtained Boron nitride nanosheet and FeCl2·4H2O mass ratio is 1:(0.4~4);The boron nitride nanosheet that described step two is obtained Quality and deionized water volume ratio be (0.001~0.02) g:1mL;
4th, the boron nitride nanosheet that step 3 is obtained into area load ferroferric oxide magnetic nano-particles is dispersed in In DMF, the ultrasound in the case where hertz is 60kHz~80kHz, power 180W~200W is placed in ultrasonic cleaning machine 2h~6h is handled, under nitrogen protection, the polybutylene glyool adipate of dehydration is added in above-mentioned dispersion liquid, in High speed shear 30min~60min under conditions of 8000rpm~15000rpm, then adds 4,4`- diphenylmethane diisocyanates Ester, is 50~80 DEG C in temperature, rotating speed is stirring reaction 0.5h~3h under 1000rpm~2000rpm, finally, into reactor BDO is added, continues to react 0.5h~2h, stops stirring, nitrogen protection is released, reaction solution is poured into warmed-up mark Quasi-mode has, and is placed in 0.4T~1T uniform magnetic field standing 2h~8h, under conditions of 60 DEG C~80 DEG C evaporation solvent 12h~ 24h, then heats to 120 DEG C~150 DEG C, cures 10~20h, and room temperature is placed 1 week, obtains the orderly magnetic nitrogen of surface micro-structure Change boron nanometer sheet/compound polyurethane material;Wherein, described step three obtains area load ferroferric oxide magnetic nano grain The quality of the boron nitride nanosheet of son and the volume ratio of N,N-dimethylformamide are 1~20g:10~50mL;Described step Three obtain the boron nitride nanosheet and the poly adipate succinic acid ester of dehydration of area load ferroferric oxide magnetic nano-particles The mass ratio of glycol is 1~20:40~80;Described step three obtains area load ferroferric oxide magnetic nano-particles The mass ratio of boron nitride nanosheet and 4,4`- '-diphenylmethane diisocyanates is 1~20:100;Described step three obtains surface The mass ratio of the boron nitride nanosheet and 1,4- butanediols that have loaded ferroferric oxide magnetic nano-particles is 1~20:20~60.
Present embodiment includes following beneficial effect:
The method for the orderly boron nitride/compound polyurethane material of preparation micro-structural that present embodiment is provided, technique is simple, consumption Can be few, and obtained ordered composite material has excellent erosive resistance, it is multiple relative to unordered boron nitride/polyurethane Condensation material, pure polyurethane, its erosive resistance have been respectively increased 31.9%, 51.5%, available for Anti-erosion protective coating.
Embodiment two:Present embodiment from unlike embodiment one:In step one temperature be 60 DEG C, rotating speed be 2000rpm under, continuously stir 30h.It is other identical with embodiment one.
Embodiment three:Present embodiment from unlike embodiment one or two:Described in step one Nitration mixture by mass concentration be 98% dense H2SO4With the dense HNO that mass concentration is 95%3It is 3 by volume:1 composition.It is other with Embodiment one or two is identical.
Embodiment four:Unlike one of present embodiment and embodiment one to three:In step 2 in Rotating speed be 5000rpm under centrifuge 15min.It is other identical with one of embodiment one to three.
Embodiment five:Unlike one of present embodiment and embodiment one to four:Institute in step 2 The quality for the intercalation boron nitride that the step of stating one obtains and the volume ratio of isopropanol are 1mg:0.5mL.Other and specific embodiment party One of formula one to four is identical.
Embodiment six:Unlike one of present embodiment and embodiment one to five:Put in step 3 In hertz it is 80kHz in ultrasonic cleaning machine, ultrasonically treated 3h under power 200W.One of other and embodiment one to five It is identical.
Embodiment seven:Unlike one of present embodiment and embodiment one to six:Institute in step 3 Boron nitride nanosheet and FeCl that the step of stating two obtains2·4H2O mass ratio is 1:3.It is other with embodiment one to One of six is identical.
Embodiment eight:Unlike one of present embodiment and embodiment one to seven:Institute in step 3 The boron nitride nanosheet and the mass ratio of deionized water that the step of stating two obtains are 0.006g:1g.Other and embodiment One of one to seven is identical.
Embodiment nine:Unlike one of present embodiment and embodiment one to eight:Institute in step 4 The step of stating three obtains the quality and N, N- diformazan of the boron nitride nanosheet of area load ferroferric oxide magnetic nano-particles The volume ratio of base formamide is 1g:50mL.It is other identical with one of embodiment one to eight.
Embodiment ten:Unlike one of present embodiment and embodiment one to nine:Institute in step 4 The step of stating three obtains the boron nitride nanosheet and the polyadipate of dehydration of area load ferroferric oxide magnetic nano-particles The mass ratio of butyl glycol ester diol is 1:80.It is other identical with one of embodiment one to nine.
Embodiment 11:Unlike one of present embodiment and embodiment one to ten:In step 4 Described step three obtains the boron nitride nanosheet and 4,4`- diphenyl-methanes of area load ferroferric oxide magnetic nano-particles The mass ratio of diisocyanate is 1:100.It is other identical with one of embodiment one to ten.
Embodiment 12:Present embodiment from unlike embodiment one to one of 11:Step 4 Described in the step of three obtain the boron nitride nanosheets of area load ferroferric oxide magnetic nano-particles and 1,4- butanediols Mass ratio be 1:20.It is other identical with embodiment one to one of 11.
Beneficial effects of the present invention are verified by tests below:
Experiment one:A kind of orderly magnetic boron nitride nanosheet/compound polyurethane material of surface micro-structure of this experiment Preparation method is to realize according to the following steps:
First, 3g hexagonal boron nitride powder is added in 200mL nitration mixture, is 60 DEG C in temperature, rotating speed is 2000rpm Under, 30h is continuously stirred, is then cooled down, is diluted with deionized water, suction filtration is repeated, washs to filtrate in neutrality, obtain intercalation nitridation Boron;Wherein, described nitration mixture by mass concentration be 98% dense H2SO4With the dense HNO that mass concentration is 95%3It is by volume 3:1 composition;
2nd, the intercalation boron nitride that 0.2g steps one are obtained is scattered in 100mL isopropanol, it is at room temperature, ultrasonically treated 12h, then centrifuges 15min under rotating speed is 5000rpm, takes supernatant liquor, and is washed with deionized to neutrality, will produce Thing is placed at 80 DEG C and dried, and obtains boron nitride nanosheet;
3rd, the boron nitride nanosheet and 0.36g FeCl obtained the step of 0.12g two2·4H2O is scattered in going for 20mL In ionized water, the ultrasonically treated 3h in the case where hertz is 80kHz, power 200W is placed in ultrasonic cleaning machine, boron nitride nanosheet is obtained Dispersion liquid, then at room temperature, in the case where rotating speed is 1500rpm, the dense of 15mL is slowly added dropwise into boron nitride nanosheet dispersion liquid The NaOH aqueous solution for 5mg/mL is spent, the H that mass concentration is 5.0mg/mL is then added dropwise again2O2The aqueous solution, when solution is by dusty blue When being changed into black, stop being added dropwise, be then sonicated 30min, carry out Magneto separate, product is cleaned 4 times with deionized water respectively, It is dried in washes of absolute alcohol 5 times, the vacuum drying oven for being finally placed in 80 DEG C, obtains area load Fe 3 O 4 magnetic The boron nitride nanosheet of nano-particle;
4th, the step of 1g three boron nitride nanosheets for obtaining area load ferroferric oxide magnetic nano-particles are disperseed 50mL DMF in, it is 80kHz to be placed in ultrasonic cleaning machine in hertz, ultrasonically treated under power 200W 5h, under nitrogen protection, the polybutylene glyool adipate of 80g dehydration is added in above-mentioned dispersion liquid, in 8000rpm Under conditions of high speed shear 30min, then add 100g 4,4`- '-diphenylmethane diisocyanates, temperature be 70 DEG C, rotating speed For stirring reaction 1.5h under 2000rpm, finally, 20g BDO is added into reactor, continue to react 1h, stop stirring Mix, release nitrogen protection, reaction solution is poured into warmed-up Standard Module, 3h is stood in the uniform magnetic field for being placed in 0.4T, 70 Evaporation solvent 24h under conditions of DEG C, then heats to 120 DEG C, cures 20h, and room temperature is placed 1 week, obtains surface micro-structure orderly Magnetic boron nitride nanosheet/compound polyurethane material.
Fig. 1 is to prepare the orderly magnetic boron nitride nanosheet/compound polyurethane material schematic diagram of surface micro-structure;
The nitridation of surface micro-structure prepared by pure polyurethane, unordered boron nitride/compound polyurethane material and this experiment in order The Wear rate of boron/compound polyurethane material is as shown in Figure 2 with the change curve of the angle of shock;Wherein, 1 rushing for pure polyurethane Lose change curve of the wear rate with the angle of shock;2 for unordered boron nitride/compound polyurethane material Wear rate with the angle of shock Change curve;3 be the Wear rate of the orderly boron nitride/compound polyurethane material of surface micro-structure of this experiment preparation with punching Hit the change curve at angle;Figure it is seen that relative to unordered boron nitride/compound polyurethane material, pure polyurethane, surface is micro- The erosive resistance of structurally ordered boron nitride/compound polyurethane material has been respectively increased 31.9%, 51.5%, can be used for Anti-erosion protective coating.

Claims (10)

1. a kind of preparation method of the orderly magnetic boron nitride nanosheet/compound polyurethane material of surface micro-structure, its feature exists In the preparation method of the orderly magnetic boron nitride nanosheet/compound polyurethane material of surface micro-structure be to carry out according to the following steps:
First, 2~6g hexagonal boron nitride powder is added in 100mL~500mL nitration mixture, is 30 DEG C~100 DEG C in temperature, turns Speed repeats suction filtration, washing under 1000rpm~2000rpm, to continuously stir 10h~50h, then cooling down, diluted with deionized water To filtrate in neutrality, intercalation boron nitride is obtained;Wherein, described nitration mixture by mass concentration be 98% dense H2SO4And mass concentration For 95% dense HNO3It is 1~3 by volume:1 composition;
2nd, the intercalation boron nitride that step one is obtained is scattered in isopropanol, at room temperature, ultrasonically treated 10h~30h, Ran Houyu Rotating speed is centrifugation 15min~50min under 1500rpm~6000rpm, takes supernatant liquor, and be washed with deionized into Property, product is placed at 80 DEG C~100 DEG C and dried, boron nitride nanosheet is obtained;The intercalation boron nitride that described step one is obtained Quality and isopropanol volume ratio be 1mg:0.5~2mL;
3rd, the boron nitride nanosheet and FeCl obtained step 22·4H2O is scattered in deionized water, is placed in ultrasonic cleaning machine In in hertz be 60kHz~80kHz, ultrasonically treated 3h~6h under power 180W~200W obtains boron nitride nanosheet dispersion liquid, Then at room temperature, rotating speed be 1000rpm~2000rpm under, be slowly added dropwise into boron nitride nanosheet dispersion liquid 5mL~ 20mL concentration is the 5mg/mL NaOH aqueous solution, and the H that mass concentration is 5.0mg/mL is then added dropwise again2O2The aqueous solution, works as solution When being changed into black by dusty blue, stop being added dropwise, be then sonicated 5min~30min, carry out Magneto separate, product is spent respectively Ionized water is cleaned 2~4 times, washes of absolute alcohol 2~5 times, is dried in the vacuum drying oven for being finally placed in 80 DEG C~100 DEG C, Obtain the boron nitride nanosheet of area load ferroferric oxide magnetic nano-particles;Wherein, the nitrogen that described step two is obtained Change boron nanometer sheet and FeCl2·4H2O mass ratio is 1:(0.4~4);The matter for the boron nitride nanosheet that described step two is obtained The volume ratio of amount and deionized water is (0.001~0.02) g:1mL;
4th, the N that the boron nitride nanosheet that step 3 is obtained into area load ferroferric oxide magnetic nano-particles is dispersed in, N- In dimethylformamide, it is placed in ultrasonic cleaning machine ultrasonically treated in the case where hertz is 60kHz~80kHz, power 180W~200W 2h~6h, under nitrogen protection, the polybutylene glyool adipate of dehydration is added in above-mentioned dispersion liquid, in 8000rpm High speed shear 30min~60min under conditions of~15000rpm, then adds 4,4`- '-diphenylmethane diisocyanates, in temperature For 50~80 DEG C, rotating speed is stirring reaction 0.5h~3h under 1000rpm~2000rpm, finally, and Isosorbide-5-Nitrae-fourth is added into reactor Glycol, continues to react 0.5h~2h, stops stirring, releases nitrogen protection, reaction solution is poured into warmed-up Standard Module, is placed in 2h~8h is stood in 0.4T~1T uniform magnetic field, evaporation solvent 12h~24h, then heats up under conditions of 60 DEG C~80 DEG C To 120 DEG C~150 DEG C, cure 10~20h, room temperature place 1 week, obtain the orderly magnetic boron nitride nanosheet of surface micro-structure/ Compound polyurethane material;Wherein, described step three obtains the boron nitride of area load ferroferric oxide magnetic nano-particles The quality of nanometer sheet and the volume ratio of N,N-dimethylformamide are 1~20g:10~50mL;Described step three obtains surface The quality of the boron nitride nanosheet and the polybutylene glyool adipate of dehydration of ferroferric oxide magnetic nano-particles is loaded Than for 1~20:40~80;Described step three obtains the boron nitride nanometer of area load ferroferric oxide magnetic nano-particles The mass ratio of piece and 4,4`- '-diphenylmethane diisocyanates is 1~20:100;Described step three obtains the oxygen of area load four The mass ratio of the boron nitride nanosheet and 1,4- butanediols of changing three ferromagnetism nanometer particles is 1~20:20~60.
2. a kind of orderly magnetic boron nitride nanosheet/compound polyurethane material of surface micro-structure according to claim 1 Preparation method, it is characterised in that in step one temperature be 60 DEG C, rotating speed be 2000rpm under, continuously stir 30h.
3. a kind of orderly magnetic boron nitride nanosheet/compound polyurethane material of surface micro-structure according to claim 1 Preparation method, it is characterised in that nitration mixture described in step one is by dense H that mass concentration is 98%2SO4It is with mass concentration 95% dense HNO3It is 3 by volume:1 composition.
4. a kind of orderly magnetic boron nitride nanosheet/compound polyurethane material of surface micro-structure according to claim 1 Preparation method, it is characterised in that the quality and the volume of isopropanol of one obtained intercalation boron nitride the step of described in step 2 Than for 1mg:0.5mL.
5. a kind of orderly magnetic boron nitride nanosheet/compound polyurethane material of surface micro-structure according to claim 1 Preparation method, it is characterised in that two obtained boron nitride nanosheets and FeCl the step of described in step 32·4H2O quality Than for 1:3.
6. a kind of orderly magnetic boron nitride nanosheet/compound polyurethane material of surface micro-structure according to claim 1 Preparation method, it is characterised in that two obtained boron nitride nanosheets and the mass ratio of deionized water the step of described in step 3 For 0.006g:1g.
7. a kind of orderly magnetic boron nitride nanosheet/compound polyurethane material of surface micro-structure according to claim 1 Preparation method, it is characterised in that three obtain area load ferroferric oxide magnetic nano-particles the step of described in step 4 Boron nitride nanosheet quality and N,N-dimethylformamide volume ratio be 1g:50mL.
8. a kind of orderly magnetic boron nitride nanosheet/compound polyurethane material of surface micro-structure according to claim 1 Preparation method, it is characterised in that three obtain area load ferroferric oxide magnetic nano-particles the step of described in step 4 Boron nitride nanosheet with dehydration polybutylene glyool adipate mass ratio be 1:80.
9. a kind of orderly magnetic boron nitride nanosheet/compound polyurethane material of surface micro-structure according to claim 1 Preparation method, it is characterised in that three obtain area load ferroferric oxide magnetic nano-particles the step of described in step 4 Boron nitride nanosheet and 4,4`- '-diphenylmethane diisocyanates mass ratio be 1:100.
10. a kind of orderly magnetic boron nitride nanosheet/compound polyurethane material of surface micro-structure according to claim 1 Preparation method, it is characterised in that three obtain area load ferroferric oxide magnetic nano-particles the step of described in step 4 The mass ratio of boron nitride nanosheet and 1,4- butanediols be 1:20.
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Publication number Priority date Publication date Assignee Title
US10059585B2 (en) * 2016-06-28 2018-08-28 Nanoco Technologies Ltd. Formation of 2D flakes from chemical cutting of prefabricated nanoparticles and van der Waals heterostructure devices made using the same
CN106475129B (en) * 2016-09-24 2019-04-16 上海大学 Using hexagonal boron nitride as the preparation method of the composite oxides denitrating catalyst of carrier
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
CN110563981A (en) * 2019-05-22 2019-12-13 青岛科技大学 Preparation method of oriented boron nitride composite film
CN111471156A (en) * 2020-05-11 2020-07-31 黎哲华 Insulating high-thermal-conductivity modified polyurethane film and preparation method thereof
CN111875764A (en) * 2020-08-03 2020-11-03 合肥万力轮胎有限公司 Novel nanometer hybrid flame-retardant polyurethane elastomer and preparation method thereof
CN113913074A (en) * 2021-11-10 2022-01-11 齐威 Waterproof coating and application method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103333465A (en) * 2013-07-10 2013-10-02 西北工业大学 Preparation method of FeCo@MWNTs/epoxy resin based wave absorbing composite material
CN103602041A (en) * 2013-11-15 2014-02-26 哈尔滨工业大学 Method for preparing microstructural ordered porous composite material for improving wear-resisting property of edge of pore of porous composite material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103333465A (en) * 2013-07-10 2013-10-02 西北工业大学 Preparation method of FeCo@MWNTs/epoxy resin based wave absorbing composite material
CN103602041A (en) * 2013-11-15 2014-02-26 哈尔滨工业大学 Method for preparing microstructural ordered porous composite material for improving wear-resisting property of edge of pore of porous composite material

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
eld induced alignment.《Composites Science and Technology》.2014,第99卷第124-130页. *
Weicheng Jiao et al..Improving the gas barrier properties of Fe3O4/graphite nanoplatelet reinforced nanocomposites by a low magnetic &#64257 *
氮化硼纳米管/聚氨酯复合材料的合成与表征;张弛等;《2015年中西部地区无机化学化工学术研讨会会议论文集》;20150422;第241-215页 *

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