CN108641261A - Amido modified graphene/class graphene MoSe2/ Bismaleimide composites and preparation method - Google Patents

Amido modified graphene/class graphene MoSe2/ Bismaleimide composites and preparation method Download PDF

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CN108641261A
CN108641261A CN201810475744.7A CN201810475744A CN108641261A CN 108641261 A CN108641261 A CN 108641261A CN 201810475744 A CN201810475744 A CN 201810475744A CN 108641261 A CN108641261 A CN 108641261A
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graphene
mose
bismaleimide
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颜红侠
陈争艳
郭留龙
李林
杨鹏飞
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Northwestern Polytechnical University
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    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F212/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
    • C08F212/34Monomers containing two or more unsaturated aliphatic radicals
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    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F222/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
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    • C08F222/40Imides, e.g. cyclic imides
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    • C08K3/02Elements
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    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
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Abstract

The present invention relates to a kind of amido modified graphene/class graphene MoSe2/ Bismaleimide composites and preparation method, belong to advanced compound materials science domain.Carrying out modification to surface of graphene oxide first with silane coupling agent KH 550 makes it take active amino, then by itself and Na2MoO4·2H2O and it is dissolved in N2H4·H2Selenium powder in O is uniformly mixed, and two selenizing molybdenum nano-complex particle of amido modified graphene/class graphene is prepared using one pot of hydro-thermal method.Finally, prepared nano-complex particle is mixed with composite material with certain proportion and diphenyl-methane type bismaleimide and diallyl bisphenol.Prepared composite material has good interface bond strength, excellent mechanical property and tribological property.

Description

Amido modified graphene/class graphene MoSe2/ Bismaleimide composites and Preparation method
Technical field
The invention belongs to advanced compound materials science domains, are related to a kind of amido modified graphene/class graphene MoSe2/ Bismaleimide composites and preparation method.
Background technology
Bismaleimide (BMI) resin has the characteristics that cheap, thermal stability is good, and it is multiple to be normally used for high-performance The resin matrix of condensation material.It is widely used in key areas such as aviation, transport, machinery, electronics.But span carrys out acyl The crosslink density of imines itself is higher, therefore especially crisp after its solidification, and some fine fisssures are easy tod produce in friction process Line, this just greatly limits application of the bimaleimide resin as friction reducing abrasion resistant material in many fields.Recently, research hair Now by nano particle be added in resin matrix can effective reinforced resin matrix frictional behaviour.
Two-dimentional carbon material and graphene-based material due to its excellent performance (such as good hot property, electrical property and its His excellent properties) cause the extensive concern of people.The presence of carbon material can increase substantially resin according to the literature The intensity and toughness of matrix, but also the extension of micro-crack can be effectively inhibited, therefore high performance friction material can be obtained Material.In particular, grapheme material is easy to shear due to its unique soft graphite layer, high intensity and on intensive shiny surface Characteristic, so that it is shown remarkable self-lubricating property, it also made to show huge dive in many fields as kollag Power.[the J.Colloid Interf.Sci.2015 such as Fan;452:98-108] by chemical method and electrochemical method in alkyl The graphene sheet layer that can in high volume process is prepared in imidazole solution, and finding can be significantly using graphene sheet layer as additive The properties of antifriction and wear resistance of enhancing alkylation pentamethylene, friction and wear reduce 27% and 74% respectively.Min etc. [Tribol.Int.2014;80:131-40] by situ aggregation method synthesized graphite oxide it is dilute/composite polyimide material, and It was found that the composite material prepared shows excellent properties of antifriction and wear resistance in brine.[the Polymer.2013 such as Shen;54(3): 1234-42] it has studied when graphene oxide content is only 0.05-0.5wt.%, graphene oxide/epoxide resin nano is compound The frictional behaviour of material;The result shows that compared with pure epoxy resin, the wear rate of the composite material of 0.5wt.% reduces 90.0-94.1%.Therefore, graphene or the grapheme material of modification can be widely used in polymeric matrix as kollag In.
After the discovery and research of graphene excellent properties, two-dimensional layer transient metal sulfide (TMDs) has weighed Newly start the interest by scholars and concern, because it can remove into class graphene-structured.Two selenizing molybdenums are similar to two sulphur Change molybdenum, is Typical Representative therein, the sandwich structure being made of two selenium atom layers and a molybdenum atom layer.It is adjacent Se-Mo-Se layers between be to be connected by weak Van der Waals force, therefore the friction coefficient between interface is relatively low.Zhang etc. [Micro.Nano Lett.,2015,10(7):339-342.] it is successfully made by mild hydro-thermal method using molybdate and selenium powder For two selenizing molybdenum nano flowers, and its friction and wear behavior is had studied as oil additive;As a result, it has been found that in base oil The two selenizing molybdenums of addition 1.0wt.% can reach best frictional behaviour.Based on the above analysis, two selenizing molybdenums can also be used as A kind of important kollag is added in resin matrix to enhance its frictional behaviour.Due to Van der Waals weak between layers Power so that two selenizing molybdenums are easy to happen sliding in process of friction and wear between lamella, and are easy to be formed between interface and turn Film is moved, this is considered as a key factor for reducing friction loss.Although graphene is a kind of widely used solid lubrication Agent, but due to its high surface energy cause its in a solvent dispersibility it is poor, this just greatly limits graphene in crowd Extensive use in multi-field.If can be compound by two selenizing molybdenum of class graphene and graphene progress, make the two that collaboration occur and make With the performance of the composite material of preparation will be better than one component of any of which.But the selenizing molybdenum of graphene/bis- is received at present The preparation of nano composite material and the research of frictional behaviour have not been reported.
Invention content
Technical problems to be solved
In order to avoid the shortcomings of the prior art, the present invention proposes a kind of amido modified graphene/class graphene MoSe2/ Bismaleimide composites and preparation method, solve graphene nano particle it is dispersed poor in a solvent and The poor problem with the compatibility of resin matrix.The dispersibility of graphene in organic solvent can be not only improved, but also can To be effectively improved graphene/class graphene MoSe2Interfacial bonding property between bimaleimide resin so that preparation is answered Condensation material has the features such as high mechanical strength and good anti-friction wear-resistant.
Technical solution
A kind of amido modified graphene/class graphene MoSe2/ Bismaleimide composites, it is characterised in that group Part it is:0.1~10 part of amido modified graphene/class graphene MoSe2Composite nanoparticle, 30~70 parts of diphenyl-methane types Bismaleimide and 30~70 parts of diallyl bisphenols.
The amido modified graphene/class graphene MoSe2Composite nanoparticle is to prepare amino using hydro-thermal method to repair The graphene of decorations/class graphene MoSe2Composite nanoparticle, wherein:Graphene and class graphene MoSe2Mass ratio be 1: (0.1~10);Amino grafting rate is the 0.1~30% of compound particle gross mass;The amino is with silane resin acceptor kh-550 It is formed with the hydroxyl condensation of surface of graphene oxide.
It is a kind of to prepare the amido modified graphene/class graphene MoSe2The side of/Bismaleimide composites Method, it is characterised in that steps are as follows:
Step 1:By 0.1~3g graphene oxides and 2.5mL KH-550 be dissolved in by 25~200mL absolute ethyl alcohols and 1~ In the mixed solution of 20mL distilled water composition, it is warming up to 78 DEG C and reacts 4h;Later, reaction solution filter and utilize nothing Water-ethanol and deionized water, washing for several times, are dried in baking oven, are labeled as NH2-GO;
Step 2:By the NH of 0.6~1.8g2The Na of-GO and 0.3~1.2g2MoO4·2H2O is dissolved in 50~80mL ionized waters In and 15~60min of ultrasonic disperse, be labeled as solution A;The selenium powder of 0.2~0.8g is dissolved in the N of 10~25mL2H4·H2O is in sky Blood-red solution B is formed in gas;Then, solution B is slowly added into solution A, and 1~4h is stirred at room temperature.Later, will Reaction mixture is transferred in high-temperature high-pressure reaction kettle 180~230 DEG C of reactions 10~for 24 hours;After being cooled to room temperature, by reaction product It is washed for several times with deionized water and absolute ethyl alcohol, freeze-drying, products therefrom is labeled as NH2-rGO/MoSe2
Step 3:By 0.1~10 part of NH2-rGO/MoSe2, 30~70 parts of diphenyl-methane type bismaleimide and 30~ 70 parts of diallyl bisphenols after 10~80min of ultrasonic disperse, heat molten under the power of 120~300W at 130~150 DEG C Melt, 15~80min of pre-polymerization is poured into the mold of preheating, is put into 130~150 DEG C of vacuum tank, is vacuumized removing bubble, is put Enter air dry oven and carry out step-up temperature solidification, curing process is 150 DEG C/2h+180 DEG C/2h+220 DEG C/4h+250 DEG C/4h, so Natural cooling afterwards demoulds up to NH2-rGO/MoSe2/ Bismaleimide composites;
Above-mentioned is to prepare portion NH2-rGO/MoSe2The proportioning of/Bismaleimide composites.
Advantageous effect
A kind of amido modified graphene/class graphene MoSe proposed by the present invention2/ Bismaleimide composites and Preparation method first prepares the GO (NH of silane coupling agent modification2- GO), then with two molybdic acid hydrate sodium, selenium powder, hydrazine hydrate etc. High-temperature high-pressure reaction kettle prepares NH2-rGO/MoSe2.The advantages of the invention, is:Class graphene MoSe2Incorporation can effectively press down Stacking between graphene sheet layer processed and reunion, effectively to solve the problems, such as that graphene is dispersed poor in a solvent;Utilize ammonia Base is to rGO/MoSe2Modified, active amino on nanoparticle surface band can be made, thus can and bismaleimide Resin carries out Michael addition reaction, can enhance the interface bond strength between nano-particle and resin in this way, can be obtained one Kind high mechanical strength, the two selenizing molybdenum of graphene/class graphene that properties of antifriction and wear resistance is good, interface bond strength is high are nano combined Material.
In the present invention, graphene and two selenizing molybdenum of class graphene are carried out compound to prepare graphene/two selenizing of class graphene Molybdenum compound particle solves the problems, such as that the dispersibility of nano-complex particle in a solvent is poor, and considers nano-particle and tree The interface cohesion sex chromosome mosaicism of aliphatic radical body, this method design prepare a kind of two selenizing molybdenum compound particle of graphene/class graphene, are used in combination Silane resin acceptor kh-550 modifies its surface, it is made to take active amino, allows for nano-particle so in a solvent With good dispersibility, and there is good interfacial bonding property between resin matrix so that composite material not only has Excellent machinery, frictional behaviour but also there is good interface bond strength, in Aeronautics and Astronautics field as solid lubrication material Material or dynamic sealing coating have a wide range of applications.
Description of the drawings
Fig. 1:The preparation process schematic diagram of amido modified graphene/class graphene MoSe2 nano-particles
Fig. 2:Diphenyl-methane type bimaleimide resin structural schematic diagram
Fig. 3:Diallyl bisphenol structural schematic diagram
Specific implementation mode
In conjunction with embodiment, attached drawing, the invention will be further described:
The technical solution adopted by the present invention is:
First, carrying out modification to surface of graphene oxide using silane resin acceptor kh-550 makes it take active amino, so Afterwards by itself and Na2MoO4·2H2O and it is dissolved in suitable N2H4·H2The selenium powder of O is uniformly mixed, and is prepared using one pot of hydro-thermal method Two selenizing molybdenum nano-complex particle (NH of amido modified graphene/class graphene2-rGO/MoSe2).Finally, by 0.1~10 part Amido modified graphene/class graphene MoSe2, 30~70 parts of diphenyl-methane type bismaleimide and 30~70 parts of diene Propyl bisphenol-A is prepared with casting moulding.
Preparation method includes the following steps:
The first step, carrying out modification to the surface graphene oxide (GO) using silane resin acceptor kh-550 makes it take active ammonia Base is labeled as NH2-GO。
Second step, by NH2- GO and Na2MoO4·2H2O is dissolved in appropriate amount of deionized water and ultrasonic disperse 30min, is labeled as Solution A;Selenium powder is dissolved in a certain amount of N2H4·H2O forms blood-red solution B in air;Then, solution B is slowly added to Into solution A, and it is stirred at room temperature to being uniformly dispersed.Later, reaction mixture is transferred to close in high-temperature high-pressure reaction kettle Seal pyroreaction a few hours.After being cooled to room temperature, reaction product is washed for several times with deionized water and absolute ethyl alcohol, then freezes dry Dry, products therefrom is labeled as NH2-rGO/MoSe2.Its reaction process such as Fig. 1;
Third walks, with certain proportion by NH2-rGO/MoSe2, diphenyl-methane type bismaleimide and diallyl bisphenol Pre-polymerization is heated in mixing, is vacuumized to be poured into be put into baking oven in preheated mold after bubble removing and is cured.
Graphene is easy to cause reunion since surface energy is higher, this allow in organic solvent dispersibility compared with Graphene and two selenizing molybdenum of class graphene are carried out compound and acted synergistically by difference, consideration, two selenizing molybdenum of such class graphene Incorporation can effectively inhibit stacking and the reunion of graphene, at the same time, the incorporation of graphene is also possible to prevent stripping Two selenizing molybdenum of class graphene further stacks, and can thus improve the dispersion of nano-complex particle in organic solvent Property.In addition, being modified nano-complex particle surface using the KH-550 with active amino can just make it with active Amino, and Michael addition reaction can occur with bimaleimide resin.Nano-particle can be improved and span carrys out acyl Interface bond strength between imide resin.The invention firstly uses silane resin acceptor kh-550s to carry out surface of graphene oxide Modification, then prepares NH by itself and two molybdic acid hydrate sodium, selenium powder, hydrazine hydrate etc. in high-temperature high-pressure reaction kettle2-rGO/MoSe2It receives Rice compound particle.Then using nano-particle as solid lubrication additive, with certain proportion with diphenyl-methane type bismaleimide Amine and diallyl bisphenol mixing prepare composite material using casting method curing molding.
The specific method is as follows:
The first step, by 0.1~3g graphene oxides and 2.5mL KH-550 be dissolved in by 25~200mL absolute ethyl alcohols and 1~ In the mixed solution of 20mL distilled water composition, it is warming up to 78 DEG C and reacts 4h.Later, reaction solution filter and utilize nothing For several times, drying is labeled as NH for water-ethanol and deionized water washing2-GO。
Second step, by the NH of 0.6~1.8g2The Na of-GO and 0.3~1.2g2MoO4·2H2O is dissolved in suitable deionized water In and 15~60min of ultrasonic disperse, be labeled as solution A;The selenium powder of 0.2~0.8g is dissolved in the N of 10~25mL2H4·H2O is in sky Blood-red solution B is formed in gas;Then, solution B is slowly added into solution A, and 1~4h is stirred at room temperature.Later, will Reaction mixture is transferred in high-temperature high-pressure reaction kettle 180~230 DEG C of reactions 10~for 24 hours.After being cooled to room temperature, by reaction product It is washed for several times with deionized water and absolute ethyl alcohol, freeze-drying, products therefrom is labeled as NH2-rGO/MoSe2
Third walks, by 0.1~10 part of NH2-rGO/MoSe2, 30~70 parts of diphenyl-methane type bismaleimide and 30~ 70 parts of diallyl bisphenols after 10~80min of ultrasonic disperse, heat molten under the power of 120~300W at 130~150 DEG C Melt, 15~80min of pre-polymerization is poured into the mold of preheating, is put into 130~150 DEG C of vacuum tank, is vacuumized removing bubble, is put Enter air dry oven and carry out step-up temperature solidification, curing process is 150 DEG C/2h+180 DEG C/2h+220 DEG C/4h+250 DEG C/4h, so Natural cooling afterwards demoulds up to NH2-rGO/MoSe2/ Bismaleimide composites.
Implement example 1:
The first step, 0.6~2.5g graphene oxides and 2.5mL KH-550 are dissolved in by 100~180mL absolute ethyl alcohols and In the mixed solution of 10~20mL distilled water composition, it is warming up to 78 DEG C and reacts 4h.Later, reaction solution filter simultaneously profit It is washed for several times with absolute ethyl alcohol and deionized water, drying is labeled as NH2-GO。
Second step, by the NH of 0.6g2The Na of-GO and 0.3g2MoO4·2H2O is dissolved in appropriate amount of deionized water and ultrasonic disperse 15min is labeled as solution A;The Se powder of 0.2g is dissolved in the N of 10mL2H4·H2O forms blood-red solution B in air;Then, Solution B is slowly added into solution A, and 1h is stirred at room temperature.Later, reaction mixture is transferred to high-temperature high-voltage reaction 180 DEG C of reaction 22h in kettle.After being cooled to room temperature, reaction product deionized water and absolute ethyl alcohol are washed for several times, freezing is dry Dry, products therefrom is labeled as NH2-rGO/MoSe2
Third walks, by 0.1 part of NH2-rGO/MoSe2The ultrasonic disperse 10min under the power of 120W, 30 parts of diphenyl-methanes Type bismaleimide and 40 parts of diallyl bisphenols heat melting at 130 DEG C, and pre-polymerization 15min pours into the mold of preheating In, it is put into 130 DEG C of vacuum tank, vacuumizes removing bubble, be put into air dry oven and carry out step-up temperature solidification, curing process For 150 DEG C/2h+180 DEG C/2h+220 DEG C/4h+250 DEG C/4h, then natural cooling, demoulds up to NH2-rGO/MoSe2/ span Carry out acid imide composite material.
Implement example 2:
The first step, with implementation example 1.
Second step, by the NH of 0.9g2The Na of-GO and 0.6g2MoO4·2H2O is dissolved in appropriate amount of deionized water and ultrasonic disperse 30min is labeled as solution A;The Se powder of 0.4g is dissolved in the N of 15mL2H4·H2O forms blood-red solution B in air;Then, Solution B is slowly added into solution A, and 2h is stirred at room temperature.Later, reaction mixture is transferred to high-temperature high-voltage reaction 200 DEG C of reaction 20h in kettle.After being cooled to room temperature, reaction product deionized water and absolute ethyl alcohol are washed for several times, freezing is dry Dry, products therefrom is labeled as NH2-rGO/MoSe2
Third walks, by 1 part of NH2-rGO/MoSe2The ultrasonic disperse 30min under the power of 150W, 57 parts of diphenyl-methane types Bismaleimide and 43 parts of diallyl bisphenols heat melting at 140 DEG C, and pre-polymerization 50min is poured into the mold of preheating, It is put into 140 DEG C of vacuum tank, vacuumizes removing bubble, be put into air dry oven and carry out step-up temperature solidification, curing process is 150 DEG C/2h+180 DEG C/2h+220 DEG C/4h+250 DEG C/4h, then natural cooling, demoulds up to NH2-rGO/MoSe2/ span comes Acid imide composite material.
Implement example 3:
The first step, with implementation example 1.
Second step, by the NH of 1.2g2The Na of-GO and 0.9g2MoO4·2H2O is dissolved in appropriate amount of deionized water and ultrasonic disperse 45min is labeled as solution A;The Se powder of 0.6g is dissolved in the N of 20mL2H4·H2O forms blood-red solution B in air;Then, Solution B is slowly added into solution A, and 3h is stirred at room temperature.Later, reaction mixture is transferred to high-temperature high-voltage reaction 220 DEG C of reaction 20h in kettle.After being cooled to room temperature, reaction product deionized water and absolute ethyl alcohol are washed for several times, freezing is dry Dry, products therefrom is labeled as NH2-rGO/MoSe2
Third walks, by 3 parts of NH2-rGO/MoSe2The ultrasonic disperse 60min under the power of 200W, 43 parts of diphenyl-methane types Bismaleimide and 57 parts of diallyl bisphenols heat melting at 150 DEG C, and pre-polymerization 70min is poured into the mold of preheating, It is put into 150 DEG C of vacuum tank, vacuumizes removing bubble, be put into air dry oven and carry out step-up temperature solidification, curing process is 150 DEG C/2h+180 DEG C/2h+220 DEG C/4h+250 DEG C/4h, then natural cooling, demoulds up to NH2-rGO/MoSe2/ span comes Acid imide composite material.
Implement example 4:
The first step, with implementation example 1.
Second step, by the NH of 1.8g2The Na of-GO and 1.2g2MoO4·2H2O is dissolved in appropriate amount of deionized water and ultrasonic disperse 60min is labeled as solution A;The Se powder of 0.8g is dissolved in the N of 25mL2H4·H2O forms blood-red solution B in air;Then, Solution B is slowly added into solution A, and 4h is stirred at room temperature.Later, reaction mixture is transferred to high-temperature high-voltage reaction 230 DEG C of reaction 18h in kettle.After being cooled to room temperature, reaction product deionized water and absolute ethyl alcohol are washed for several times, freezing is dry Dry, products therefrom is labeled as NH2-rGO/MoSe2
Third walks, by 5 parts of NH2-rGO/MoSe2The ultrasonic disperse 80min under the power of 300W, 57 parts of diphenyl-methane types Bismaleimide and 43 parts of diallyl bisphenols heat melting at 150 DEG C, and pre-polymerization 80min is poured into the mold of preheating, It is put into 150 DEG C of vacuum tank, vacuumizes removing bubble, be put into air dry oven and carry out step-up temperature solidification, curing process is 150 DEG C/2h+180 DEG C/2h+220 DEG C/4h+250 DEG C/4h, then natural cooling, demoulds up to NH2-rGO/MoSe2/ span comes Acid imide composite material.
Implement example 5:
The first step, with implementation example 1.
Second step, by the NH of 2.0g2The Na of-GO and 1.2g2MoO4·2H2O is dissolved in appropriate amount of deionized water and ultrasonic disperse 60min is labeled as solution A;The Se powder of 0.8g is dissolved in the N of 25mL2H4·H2O forms blood-red solution B in air;Then, Solution B is slowly added into solution A, and 4h is stirred at room temperature.Later, reaction mixture is transferred to high-temperature high-voltage reaction 230 DEG C of reaction 23h in kettle.After being cooled to room temperature, reaction product deionized water and absolute ethyl alcohol are washed for several times, freezing is dry Dry, products therefrom is labeled as NH2-rGO/MoSe2
Third walks, by 7 parts of NH2-rGO/MoSe2The ultrasonic disperse 80min under the power of 300W, 57 parts of diphenyl-methane types Bismaleimide and 43 parts of diallyl bisphenols heat melting at 150 DEG C, and pre-polymerization 80min is poured into the mold of preheating, It is put into 150 DEG C of vacuum tank, vacuumizes removing bubble, be put into air dry oven and carry out step-up temperature solidification, curing process is 150 DEG C/2h+180 DEG C/2h+220 DEG C/4h+250 DEG C/4h, then natural cooling, demoulds up to NH2-rGO/MoSe2/ span comes Acid imide composite material.

Claims (3)

1. a kind of amido modified graphene/class graphene MoSe2/ Bismaleimide composites, it is characterised in that component For:0.1~10 part of amido modified graphene/class graphene MoSe2Composite nanoparticle, 30~70 parts of diphenyl-methane types are double Maleimide and 30~70 parts of diallyl bisphenols.
2. amido modified graphene/class graphene MoSe according to claim 12/ Bismaleimide composites, It is characterized in that:The amido modified graphene/class graphene MoSe2Composite nanoparticle is to prepare amino using hydro-thermal method to repair The graphene of decorations/class graphene MoSe2Composite nanoparticle, wherein:Graphene and class graphene MoSe2Mass ratio be 1: (0.1~10);Amino grafting rate is the 0.1~30% of compound particle gross mass;The amino is with silane resin acceptor kh-550 It is formed with the hydroxyl condensation of surface of graphene oxide.
3. a kind of preparing graphene amido modified described in claims 1 or 2/class graphene MoSe2/ bismaleimide is compound The method of material, it is characterised in that steps are as follows:
Step 1:0.1~3g graphene oxides and 2.5mL KH-550 are dissolved in by 25~200mL absolute ethyl alcohols and 1~20mL steamings In the mixed solution of distilled water composition, it is warming up to 78 DEG C and reacts 4h;Later, reaction solution filter and utilize absolute ethyl alcohol And deionized water, washing for several times, are dried in baking oven, are labeled as NH2-GO;
Step 2:By the NH of 0.6~1.8g2The Na of-GO and 0.3~1.2g2MoO4·2H2O is dissolved in 50~80mL ionized waters and surpasses Sound disperses 15~60min, is labeled as solution A;The selenium powder of 0.2~0.8g is dissolved in the N of 10~25mL2H4·H2O shapes in air At blood-red solution B;Then, solution B is slowly added into solution A, and 1~4h is stirred at room temperature.Later, reaction is mixed It closes object and is transferred in high-temperature high-pressure reaction kettle 180~230 DEG C of reactions 10~for 24 hours;After being cooled to room temperature, by reaction product spend from For several times, freeze-drying, products therefrom is labeled as NH for sub- water and absolute ethyl alcohol washing2-rGO/MoSe2
Step 3:By 0.1~10 part of NH2-rGO/MoSe2, 30~70 parts of diphenyl-methane type bismaleimide and 30~70 parts Diallyl bisphenol after 10~80min of ultrasonic disperse, heats melting, in advance under the power of 120~300W at 130~150 DEG C Poly- 15~80min is poured into the mold of preheating, is put into 130~150 DEG C of vacuum tank, is vacuumized removing bubble, is put into air blast Drying box carries out step-up temperature solidification, and curing process is 150 DEG C/2h+180 DEG C/2h+220 DEG C/4h+250 DEG C/4h, then natural It is cooling, it demoulds up to NH2-rGO/MoSe2/ Bismaleimide composites;
Above-mentioned is to prepare portion NH2-rGO/MoSe2The proportioning of/Bismaleimide composites.
CN201810475744.7A 2018-05-17 2018-05-17 Amido modified graphene/class graphene MoSe2/ Bismaleimide composites and preparation method Pending CN108641261A (en)

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CN109713156A (en) * 2018-11-30 2019-05-03 云谷(固安)科技有限公司 Display panel and preparation method thereof and display terminal
CN114479453A (en) * 2021-12-20 2022-05-13 西安理工大学 Preparation method of MXene-based hyperbranched polysiloxane reinforced resin composite material
CN114639810A (en) * 2022-03-23 2022-06-17 哈尔滨师范大学 Preparation method of molybdenum diselenide @ RGO composite material with adjustable heterostructure and multiple microwave absorption bands

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109713156A (en) * 2018-11-30 2019-05-03 云谷(固安)科技有限公司 Display panel and preparation method thereof and display terminal
CN109713156B (en) * 2018-11-30 2021-03-30 云谷(固安)科技有限公司 Display panel, preparation method thereof and display terminal
CN114479453A (en) * 2021-12-20 2022-05-13 西安理工大学 Preparation method of MXene-based hyperbranched polysiloxane reinforced resin composite material
CN114639810A (en) * 2022-03-23 2022-06-17 哈尔滨师范大学 Preparation method of molybdenum diselenide @ RGO composite material with adjustable heterostructure and multiple microwave absorption bands
CN114639810B (en) * 2022-03-23 2024-02-09 哈尔滨师范大学 Preparation method of molybdenum diselenide@RGO composite material with adjustable heterostructure and multiple microwave absorption bands

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Application publication date: 20181012