CN113121882A - Functionalized graphene oxide-aluminum hypophosphite flame retardant and preparation method and application thereof - Google Patents

Functionalized graphene oxide-aluminum hypophosphite flame retardant and preparation method and application thereof Download PDF

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CN113121882A
CN113121882A CN202110249677.9A CN202110249677A CN113121882A CN 113121882 A CN113121882 A CN 113121882A CN 202110249677 A CN202110249677 A CN 202110249677A CN 113121882 A CN113121882 A CN 113121882A
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flame retardant
graphene oxide
functionalized graphene
polystyrene
aluminum hypophosphite
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CN113121882B (en
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邓贞贞
戴康
刘古月
吴雨彤
赵楚雯
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Guangdong University of Technology
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Abstract

The invention discloses a functionalized graphene oxide-aluminum hypophosphite flame retardant, and a preparation method and application thereof. The preparation method of the functionalized graphene oxide-aluminum hypophosphite flame retardant comprises the following steps: s1, uniformly mixing graphene oxide, phosphorus oxychloride and triethylamine in a dimethylformamide solution under an inert gas atmosphere, reacting for 5-8 h at 0-5 ℃, mixing DOPO-OH, reacting for 5-8 h at 40-60 ℃, and performing aftertreatment to obtain FGO; s2, uniformly mixing sodium hypophosphite and an aqueous solution of FGO, dropwise adding an aluminum sulfate aqueous solution of octadecahydrate at the temperature of 80-90 ℃, reacting for 6-8 h, and performing aftertreatment to obtain the functionalized graphene oxide-aluminum hypophosphite flame retardant. The functionalized graphene oxide-aluminum hypophosphite flame retardant developed by the invention has an excellent flame retardant effect, and the functionalized graphene oxide-aluminum hypophosphite flame retardant is added into polystyrene in a melt blending mode, so that the polystyrene nano composite flame retardant material can be prepared.

Description

Functionalized graphene oxide-aluminum hypophosphite flame retardant and preparation method and application thereof
Technical Field
The invention relates to the field of hybrid materials, and particularly relates to a functionalized graphene oxide-aluminum hypophosphite flame retardant, and a preparation method and application thereof.
Background
Polystyrene (PS) is prepared by radical polycondensation of styrene monomers, is easy to process and form, is a polymer with wide application, and is widely applied to the fields of packaging materials, electronic industry, buildings, household appliances, transportation and the like. But PS is only composed of two elements of carbon and hydrogen, has low limiting oxygen index and high peak value of heat release rate, can release a large amount of toxic gas and black smoke during combustion, can also generate serious melting and dripping, and is very easy to cause fire hazard; if the flame retardant treatment is not carried out, the application is limited.
Graphene is a carbon material with a special structure, and is prepared from sp2The carbon atoms of the hybrid orbitals are stacked and the thickness is only one carbon atom. The characteristics of the graphene such as large surface area and excellent heat conductivity make the research of the graphene/polymer nanocomposite prepared by adding the graphene into the polymer material attract attention. However, the single addition of graphene easily causes an aggregation phenomenon due to strong van der waals attraction in graphene sheets, so that the graphene is unevenly dispersed in a polymer matrix, the performance of the graphene-based nanocomposite is weakened, and the development and utilization of the graphene are limited to a great extent. Graphene Oxide (GO) is the most common derivative of graphene, and the surface of the graphene oxide contains a plurality of active reaction sites, namely a large number of oxygen-containing functional groups such as-COOH, -OH, -COC and the like; the active sites can react with small molecules or polymer molecules containing specific active functional groups to graft the small molecules or the polymer molecules onto graphene oxide, so that the dispersibility of the graphene in a polymer matrix is improved, and the interaction with the polymer matrix is improved.
The phosphorus flame retardant is widely applied to flame retardance of polymer materials due to the characteristics of no halogen, high efficiency and the like. Wherein 9, 10-dihydro-9-oxa-10-phosphaphenanthrene-10 oxide (DOPO) is a phosphaphenanthrene compound in the phosphorus flame retardant; the DOPO flame retardant is based on a gas-phase flame retardant mechanism, and a phosphorus-oxygen free radical formed by phosphorus elements in the DOPO flame retardant can be used as a flame quencher for polymer combustion during combustion, so that the chain reaction of the combustion is interrupted, and the DOPO flame retardant has an obvious flame retardant effect. The P-H bond in the molecular structure of DOPO has high activity, and can be bonded into a plurality of flame retardants or curing agents with better performance. The research finds that when DOPO-GO is added in an amount of 3%, the carbon residue rate of the EP composite material is improved by 1.8% compared with that of pure EP, so that a certain flame retardant effect is achieved. But the flame retardant efficiency is low, and the flame retardant effect of the flame retardant in a polystyrene system is not researched.
Therefore, it is required to develop a flame retardant material with better flame retardant effect when applied to polystyrene.
Disclosure of Invention
The invention provides a functionalized graphene oxide-aluminum hypophosphite flame retardant for overcoming the defect of low flame retardant efficiency in the prior art, and the flame retardant has a good flame retardant effect.
The invention also aims to provide a preparation method of the functionalized graphene oxide-aluminum hypophosphite flame retardant.
The invention also aims to provide application of the functionalized graphene oxide-aluminum hypophosphite flame retardant in preparation of a polystyrene nano composite flame-retardant material.
The invention also aims to provide a preparation method of the polystyrene nano composite flame retardant material.
In order to solve the technical problems, the invention adopts the technical scheme that:
a preparation method of a functionalized graphene oxide-aluminum hypophosphite flame retardant comprises the following steps:
s1, preparing phosphorus-containing Functionalized Graphene Oxide (FGO):
uniformly mixing graphene oxide, phosphorus oxychloride and triethylamine in a dimethylformamide solution under an inert gas atmosphere, and reacting at 0-5 ℃ for 5-8 h to obtain a mixed solution;
uniformly mixing DOPO-OH with the mixed solution, reacting for 5-8 h at 40-60 ℃, and performing aftertreatment to obtain FGO;
s2, preparing a functionalized graphene oxide-aluminum hypophosphite flame retardant (FGO-AHP):
uniformly mixing sodium hypophosphite and an aqueous solution of FGO, dropwise adding an aluminum sulfate octadecahydrate aqueous solution at the temperature of 80-90 ℃, reacting for 6-8 h, and performing aftertreatment to obtain the functionalized graphene oxide-aluminum hypophosphite flame retardant.
The aluminum hypophosphite is an efficient phosphorus-containing flame retardant, has high phosphorus content, can play a role of catalytic char formation in a condensed phase in a high polymer matrix, and simultaneously captures free radicals in a gas phase to cut off a combustion chain reaction, so that the aluminum hypophosphite has excellent flame retardant effect.
The inventor finds that after the phosphorus-containing functional group is grafted to the surface of GO to prepare FGO, the functionalized graphene oxide is further subjected to flame retardant modification by using aluminum hypophosphite by using a chemical deposition method, and the functionalized graphene oxide is modified by chemical bond combination, so that the obtained FGO-AHP has the specific functionality of graphene, the phosphorus-containing grafting group and aluminum hypophosphite; meanwhile, by the synergistic effect of the three, the FGO-AHP has more excellent flame retardant effect.
Preferably, in the step S1, the mass ratio of the graphene oxide to the triethylamine to the DOPO-OH to the phosphorus oxychloride is 1: (16.24-25.1): (11.6-17.5): (8.2-11.7).
Preferably, the mass ratio of the FGO, the sodium hypophosphite and the aluminum sulfate octadecahydrate in step S2 is 1: (7.9-8.6): (4.5-5.6).
Preferably, the inert atmosphere is a nitrogen or argon atmosphere.
The post-treatments in S1 and S2 are filtration, washing, drying.
Preferably, the washing is washing with deionized water.
Preferably, the drying is vacuum freeze drying for 10-20 h.
Preferably, the particle sizes of the GO, the FGO and the FGO-AHP are all 100nm to 500 nm.
The invention also discloses a functionalized graphene oxide-aluminum hypophosphite flame retardant, which is prepared by the preparation method.
The invention also protects the application of the functionalized graphene oxide-aluminum hypophosphite flame retardant in the preparation of the polystyrene nano composite flame-retardant material.
The invention also provides a preparation method of the polystyrene nano composite flame retardant material, which comprises the following steps:
m1, dispersing the functionalized graphene oxide-aluminum hypophosphite flame retardant and polystyrene in a dimethylformamide solution, uniformly mixing, drying, and granulating to obtain polystyrene nano material master batches;
and M2, blending the polystyrene nano material master batch and polystyrene to obtain the polystyrene nano composite flame retardant material.
Preferably, the weight ratio of the functionalized graphene oxide-aluminum hypophosphite flame retardant to the polystyrene is 1: (3.6-9).
Preferably, the blending weight ratio of the polystyrene nano material master batch to the polystyrene is 1: (1-5).
Preferably, the drying in the step M1 is carried out by blowing at 100-120 ℃.
Preferably, the blending in the step M2 is carried out by using a double-mixing internal mixer at a rotation speed of 50-55 rpm/min, a blending temperature of 180-190 ℃ and a blending time of 8-10 min.
By introducing FGO-AHP into the PS matrix in a melt blending mode, the multiphase flame retardant effect can be realized: the DOPO structure can play a role in gas-phase flame retardance and is combined with active free radicals H & in gas-phase combustion reaction during combustion, so that the chain reaction of combustion is interrupted, and the combustion flame is reduced; the phosphorus-containing molecular chain segment can also form polymers such as metaphosphoric acid and the like to form a stable barrier on the surface of the material, thereby preventing oxygen required by continuous combustion from entering and preventing combustible gas from overflowing and further improving the flame retardant effect; the phosphorus-containing component of AHP catalyzes polystyrene to degrade into carbon in gas phase and condensed phase, inhibit the spread of fire during combustion, the inflaming retarding is high in efficiency; the graphene can effectively improve the heat insulation and heat insulation of the flame-retardant material, and obviously improve the comprehensive performance of the polystyrene. The synergistic flame-retardant effect of the three components ensures that the polystyrene nano composite flame-retardant material has excellent flame-retardant performance.
Compared with the prior art, the invention has the beneficial effects that:
(1) the FGO-AHP developed by the invention is stably and uniformly dispersed in a PS system, a DOPO structure and an aluminum hypophosphite phosphorus-containing flame retardant group are grafted on the surface, the specific functionality of graphene, the phosphorus-containing grafting group and the aluminum hypophosphite is realized, and the FGO-AHP has an excellent flame retardant effect under the synergistic effect of the graphene, the phosphorus-containing grafting group and the aluminum hypophosphite.
(2) FGO-AHP is introduced into a PS matrix in a melt blending mode, the heat release peak value of the prepared polystyrene nano composite flame retardant material is reduced by about 39.9 percent compared with that of pure PS, and the flame retardant property of the polystyrene nano composite flame retardant material is obviously improved.
Drawings
Fig. 1 is an infrared detection spectrum of Graphene Oxide (GO), phosphorus-containing Functionalized Graphene Oxide (FGO), and functionalized graphene oxide-aluminum hypophosphite flame retardant (FGO-AHP) prepared in example 1.
FIG. 2 is SEM images of blending GO, FGO-AHP with PS respectively prepared in example 1, wherein FIG. 2a is PS/GO, FIG. 2b is PS/FGO, and FIG. 2c is FGO-AHP/PS.
FIG. 3 is a thermogravimetric analysis of GO, FGO-AHP prepared in example 1.
FIG. 4 is a heat release rate curve of the polystyrene nanocomposite flame retardant material prepared in example 1 with pure PS.
Fig. 5 is an SEM image of a polystyrene nanocomposite flame retardant material prepared in example 1 and carbon residue after PS/GO combustion, where fig. 5a is an SEM image of the polystyrene nanocomposite flame retardant material carbon residue, and fig. 5b is an SEM image of the PS/GO carbon residue.
Fig. 6 is a diagram of a polystyrene nanocomposite flame retardant material prepared in example 1 and carbon residue obtained after PS/GO combustion, where fig. 6a is a diagram of a polystyrene nanocomposite flame retardant material carbon residue and fig. 6b is a diagram of a PS/GO carbon residue.
Detailed Description
The present invention will be further described with reference to the following embodiments.
The raw materials in the examples are all commercially available;
graphene oxide is prepared by taking graphite powder as a raw material and utilizing an improved Hummers method;
graphite powder 800 mesh Shanghai Merlin biochemistry, Inc.;
polystyrene 158K basf (china) ltd;
DOPO-OH takes DOPO as a raw material, and adopts polymerization reaction to synthesize the DOPO-OH;
DOPO analysis pure Shenzhen Jinlong chemical Co., Ltd;
dimethylformamide analytical pure Guangzhou chemical reagent works;
POCl3analytical pure Shanghai Meclin biochemistry, Inc.;
triethylamine was analyzed in a pure Tianjin Damao chemical reagent plant;
NaH2PO2analytical pure Guangzhou chemical reagent works;
Al2(SO4)3·18H2o analytically pure Shanghai Merlin biochemistry, Inc.
Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Example 1
The embodiment provides a functionalized graphene oxide-aluminum hypophosphite flame retardant and a polystyrene nano composite flame-retardant material prepared from the same.
The preparation method of the functionalized graphene oxide-aluminum hypophosphite flame retardant comprises the following steps:
s1, preparing phosphorus-containing Functionalized Graphene Oxide (FGO):
40ml of Dimethylformamide (DMF) were added to a 500ml three-necked flask under a nitrogen atmosphere, and POCl was rapidly added3(0.06mol, 9.252g) is stirred evenly and triethylamine is added(TEA) (0.2mol, 20.258g), stirring for 20min, dispersing 1g of Graphene Oxide (GO) in 60ml of DMF, performing ultrasonic treatment for 1h to form a uniform mixed solution, slowly dropping the mixed solution into a three-neck flask, and stirring at 0-5 ℃ for 4h to obtain a mixed solution;
and (3) moving the three-neck flask filled with the mixed solution into an oil bath kettle at 60 ℃, slowly adding DOPO-OH (0.06mol, 14.772g) into the three-neck flask, stirring for 6h at 60 ℃, filtering and washing a product by using deionized water, refrigerating for 12h, and carrying out vacuum freeze drying for 12h to obtain black powder FGO.
S2, preparing a functionalized graphene oxide-aluminum hypophosphite flame retardant (FGO-AHP):
1g FGO and 7.922g NaH2PO2Dispersing in 40ml deionized water, ultrasonically stirring and mixing for 1h, transferring to a 90 ℃ oil bath pot, and stirring for half an hour; 4.504g of Al2(SO4)3·18H2Dissolving O in 20ml of deionized water, dropwise adding the mixed solution, and mechanically stirring at 90 ℃ for 6 hours; washing with deionized water, filtering, and vacuum drying at 70 deg.C for 12 hr to obtain black powder FGO-AHP.
The preparation method of the polystyrene nano composite flame-retardant material comprises the following steps:
m1, dispersing 12.6g of polystyrene in a three-neck flask filled with 50ml of DMF, and carrying out ultrasonic treatment for 1 hour while mechanically stirring; ultrasonically treating 1.4g of FGO-AHP in 20ml of DMF for 30min, slowly dripping into a three-neck flask, ultrasonically treating for 2h while mechanically stirring to obtain uniform black slurry, drying by air blowing at 120 ℃ for 12h, taking out, cutting into small particles, and further drying at 130 ℃ for 6h to obtain the polystyrene nano material master batch.
And M2, adding 10g of polystyrene nano material master batch and 40g of polystyrene into an XSS-300 double-mixing internal mixer for blending, wherein the temperature of the internal mixer is 180 ℃, the rotating speed is 50rpm/min, and the blending time is 8min, so as to obtain the polystyrene nano composite flame retardant material.
Example 2
The embodiment provides a functionalized graphene oxide-aluminum hypophosphite flame retardant and a polystyrene nano composite flame-retardant material prepared from the flame retardant, and is different from the embodiment 1 in that the mass of FGO-AHP in M1 is 2.1 g.
Example 3
The embodiment provides a functionalized graphene oxide-aluminum hypophosphite flame retardant and a polystyrene nano composite flame-retardant material prepared from the flame retardant, and is different from the embodiment 1 in that the mass of FGO-AHP in M1 is 2.8 g.
Example 4
The embodiment provides a functionalized graphene oxide-aluminum hypophosphite flame retardant and a polystyrene nano composite flame-retardant material prepared from the flame retardant, and is different from the embodiment 1 in that the mass of FGO-AHP in M1 is 3.5 g.
Example 5
This example provides a functionalized graphene oxide-aluminum hypophosphite flame retardant and a polystyrene nanocomposite flame retardant material prepared therefrom, which is different from example 1 in that the mass of polystyrene in M2 is 10 g.
Example 6
This example provides a functionalized graphene oxide-aluminum hypophosphite flame retardant and a polystyrene nanocomposite flame retardant material prepared therefrom, which is different from example 1 in that the mass of polystyrene in M2 is 50 g.
Example 7
The embodiment provides a functionalized graphene oxide-aluminum hypophosphite flame retardant and a polystyrene nanocomposite flame retardant material prepared from the same, and is different from the embodiment 1 in that the addition amounts of graphene oxide, triethylamine, DOPO-OH and phosphorus oxychloride in S1 are 1g, 22.2g, 12.5g and 11.2g respectively.
Example 8
The embodiment provides a functionalized graphene oxide-aluminum hypophosphite flame retardant and a polystyrene nano composite flame retardant material prepared from the same, and is different from the embodiment 1 in that the addition amounts of FGO, sodium hypophosphite and aluminum sulfate octadecahydrate in S2 are 1g, 8.2g and 5.6g respectively.
Performance testing
The functionalized graphene oxide-aluminum hypophosphite flame retardant prepared in the above embodiment is subjected to a performance test, and the test method is as follows:
fourier infrared spectroscopy (FTIR): infrared spectrum analyzer using Nicolet 6700Testing the functionalized graphene oxide-aluminum hypophosphite flame retardant, mixing a proper amount of sample with KBr powder according to the ratio of 1: 100, uniformly grinding, pressing into a sheet to be tested, wherein the testing range is 500cm-1-4000cm-1The wave number of (c).
Thermogravimetric analysis (TGA): the samples were tested for thermal stability using a model TGA4000 analyzer (Perkin Elmer, usa) with the experimental parameters set as: the temperature rise range is between room temperature and 800 ℃, the temperature rise rate is 20 ℃/min, and the mass of the sample is 5-10 mg.
Microscopic morphology: scanning was performed using a Scanning Electron Microscope (SEM) (model: S-3400N (II) Hitachi, Japan).
The test results were as follows:
from the infrared spectrum of FIG. 1, it can be found that the wave number is 3408cm-1The peak is the-OH vibration peak of water molecules, and the GO and FGO can be judged to contain a small amount of water, which is caused by that the GO surface contains a large amount of hydrophilic groups to adsorb water. The infrared spectrum of GO shows the presence of oxygen-containing functional groups, 1728cm-1Where is C ═ O cm-11624cm of telescopic vibration peak-1The peak is C ═ C, 1384cm-1The absorption vibration peak of C-OH is shown. The FGO spectra show some new characteristic peaks compared to the GO spectra. Wherein the length of the groove is 3000cm-1～2600cm-1The absorption peak is C-H stretching vibration peak at 2490cm-1For the P-H bond of DOPO at 1204cm-1A new vibration peak appears, which indicates that P ═ O exists in GO and also indicates that DOPO-OH is grafted on the GO surface.
In addition, at 1000-1470cm-1The newly appeared vibration peaks are P-O-Ph and the stretching vibration of aromatic rings respectively, which proves that DOPO-OH is successfully grafted on the surface of GO and marks that FGO is successfully synthesized. The characteristic peak of AHP comprises, 2405cm-1(stretching vibration of P-H bond), 1190cm-1(P ═ vibration peak of O bond), 763cm-1And 908cm-1(bending vibration peak of P-H bond) and 1080cm-1(vibration peak of P-O bond). For the FGO-AHP spectrum at 3408cm-1The absorption peak at the-OH bond is significantly reduced and is 1384cm-1The characteristic peak of C-OH bond disappears, tableIt is clear that FGO-AHP has hydrophobicity. Furthermore, the IR spectrum of FGO-AHP was shown to be 2405cm-1、1190cm-1And 1080cm-1The peaks at (a) correspond to the absorption peaks for P-H, P ═ O and P-O, respectively, further indicating that AHP has been successfully deposited on the FGO surface. In conclusion, the FGO-AHP nano hybrid is shown to be successfully synthesized.
FIG. 2 is SEM images of GO, FGO prepared in example 1, FGO-AHP blended with PS, respectively. As can be seen from FIG. 2a, a large amount of agglomeration phenomenon exists in PS/GO, and due to the fact that Van der Waals force between GO nano-sheets is strong, compatibility between GO and PS molecular chains is weak, and a rough fracture surface with a small wrinkle shape is presented. FIG. 2b shows that the fracture surface of PS/FGO is smooth, FGO can be better dispersed in the PS matrix, and the FGO and PS have ideal compatibility, because the carbon-carbon double bond of the covalent functionalized molecule on the surface of FGO can be chemically combined with the polystyrene double bond, thereby improving the comprehensive performance of the material. It can be observed from fig. 2c that FGO-AHP is embedded and well dispersed in PS matrix without aggregation and obvious stacking of nanosheets, indicating that the interfacial compatibility between FGO-AHP and PS matrix is better, which is beneficial to improving the flame retardant performance of the composite material.
FIG. 3 is a thermogravimetric analysis of GO, FGO-AHP prepared in example 1. As can be seen from fig. 3, the residual carbon content of FGO-AHP is 73 wt.%, the residual carbon content of FGO is 57 wt.%, and the residual carbon content of GO is 43 wt.%, which indicates that the thermal stability of FGO-AHP is significantly improved compared to FGO and GO.
FIG. 4 is a heat release rate curve of the polystyrene nanocomposite flame retardant material prepared in example 1 with pure PS. It can be seen that, compared with pure PS, the heat release peak value of the polystyrene nano composite flame retardant material is reduced by about 39.9%, and the flame retardant property of the composite flame retardant material is obviously improved.
Fig. 5 and 6 are SEM images and physical images of the polystyrene nanocomposite flame retardant material prepared in example 1 and carbon residue after PS/GO combustion, respectively. As can be seen from fig. 5a and 6a, the surface structure of the carbon layer of the polystyrene nanocomposite flame retardant material is compact and smooth, which indicates that the gas product can be blocked by the dense carbon layer, thereby effectively preventing the internal material from being exposed to the heat source; as can be seen from FIGS. 5b and 6b, the PS/GO residual carbon appears on irregular surface and has loose structure, and the residual carbon with many small holes can transmit oxygen and air during the combustion process. Therefore, the FGO-AHP has good air isolation effect on PS, reduces the volatilization of combustible gas, further controls mass transfer and heat transfer, prevents the degradation of internal polystyrene and achieves the flame retardant effect.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.

Claims (10)

1. A preparation method of a functionalized graphene oxide-aluminum hypophosphite flame retardant is characterized by comprising the following steps:
s1, preparing phosphorus-containing functionalized graphene oxide:
uniformly mixing graphene oxide, phosphorus oxychloride and triethylamine in a dimethylformamide solution under an inert gas atmosphere, and reacting at 0-5 ℃ for 5-8 h to obtain a mixed solution;
uniformly mixing DOPO-OH with the mixed solution, reacting at 40-60 ℃ for 5-8 h, and performing aftertreatment to obtain phosphorus-containing functionalized graphene oxide;
s2, preparing a functionalized graphene oxide-aluminum hypophosphite flame retardant:
uniformly mixing sodium hypophosphite and the aqueous solution of the phosphorus-containing functionalized graphene oxide, dropwise adding an aluminum sulfate aqueous solution of octadecahydrate at the temperature of 80-90 ℃, reacting for 6-8 h, and performing post-treatment to obtain the functionalized graphene oxide-aluminum hypophosphite flame retardant.
2. The preparation method according to claim 1, wherein in step S1, the mass ratio of graphene oxide to triethylamine to DOPO-OH to phosphorus oxychloride is 1: (16.24-25.1): (11.6-17.5): (8.2-11.7).
3. The preparation method according to claim 1, wherein the mass ratio of the phosphorus-containing functionalized graphene oxide, the sodium hypophosphite and the aluminum sulfate octadecahydrate in the step S1 is 1: (7.9-8.6): (4.5-5.6).
4. The method according to claim 1, wherein the post-treatment is filtration, washing, drying; the drying is vacuum freeze drying for 10-20 h.
5. A functionalized graphene oxide-aluminum hypophosphite flame retardant is characterized in that the functionalized graphene oxide-aluminum hypophosphite flame retardant is prepared by the preparation method of any one of claims 1-5.
6. The functionalized graphene oxide-aluminum hypophosphite flame retardant as claimed in claim 5, wherein the functionalized graphene oxide-aluminum hypophosphite has a particle size of 100-500 nm.
7. Use of the functionalized graphene oxide-aluminum hypophosphite flame retardant as defined in claim 5 or 6 for preparing polystyrene nanocomposite flame retardant materials.
8. The method for preparing the polystyrene nanocomposite flame retardant material of claim 7, which is characterized by comprising the following steps:
m1, dispersing the functionalized graphene oxide-aluminum hypophosphite flame retardant and polystyrene in a dimethylformamide solution, uniformly mixing, drying, and granulating to obtain polystyrene nano material master batches;
and M2, blending the polystyrene nano material master batch and polystyrene to obtain the polystyrene nano composite flame retardant material.
9. The preparation method of claim 8, wherein the weight ratio of the functionalized graphene oxide-aluminum hypophosphite flame retardant to the polystyrene is 1: (3.6-9).
10. The preparation method of claim 8, wherein the blending weight ratio of the polystyrene nanomaterial masterbatch to polystyrene is 1: (1-5).
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