CN109181207B - Molybdenum-antimony brominated graphene oxide modified ABS composite flame-retardant material and preparation method thereof - Google Patents
Molybdenum-antimony brominated graphene oxide modified ABS composite flame-retardant material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a molybdenum-antimony brominated graphene oxide modified ABS composite flame retardant material and a preparation method thereof, and the ABS nano composite flame retardant material is prepared by melting and blending Sb-Mo/Br-RGO and ABS, wherein the Sb-Mo/Br-RGO is uniformly dispersed in an ABS matrix, and graphene nanosheets are connected with each other to form a barrier layer, so that the flame retardant property of the ABS can be obviously improved, and meanwhile, the tensile strength of the material is improved, particularly, when the addition of the Sb-Mo/Br-RGO reaches 5.0 wt%, compact carbon residue can be generated, and when the material meets flame or heat flow, the heat transfer and oxygen isolation can be effectively inhibited, so that the heat transfer and the escape of pyrolysis volatile matters are delayed, the flame retardant property is greatly improved, and the tensile strength can reach 68.4 MPa.
Description
Technical Field
The invention belongs to the technical field of flame retardant material preparation, relates to an ABS flame retardant material and a preparation method thereof, and particularly relates to a molybdenum-antimony brominated graphene oxide modified ABS composite flame retardant material and a preparation method thereof.
Background
ABS resin is an indispensable part of today's life. It has the various performances of Polystyrene (PS), styrene-acrylonitrile copolymer (SAN) and butadiene-styrene copolymer (BS), so that it has excellent comprehensive performance. The thermoplastic polymer material has excellent impact strength, strong toughness, wear resistance and easy forming and machining, and is widely applied to the fields of packaging, furniture, automobiles, electronic and electric appliances, building materials and the like. However, ABS is easily combustible and emits black smoke and toxic gases. Thus bringing serious property loss to the production and life of people and destroying the environment. The flame retardancy and smoke suppression of ABS resins should be improved.
In actual production, the flame retardant property of the material is often improved by adding a flame retardant. The common flame retardant comprises a hydroxide flame retardant and an intumescent flame retardant, wherein the flame retardant mechanism of the hydroxide flame retardant is that a charring protective layer is generated on the outer surface of a polymer during combustion, and oxygen in air can be isolated from the reaction with the polymer; the traditional intumescent flame retardant has a similar flame retardant mechanism to that of a hydroxide flame retardant, and a dense foam carbon layer is formed on the surface of a polymer when the traditional intumescent flame retardant is heated, so that the interior of the polymer can be isolated from oxygen. However, since they are merely physically mixed with the polymer, the mechanical properties and processability of the polymer are affected.
Disclosure of Invention
The invention aims to provide a molybdenum-antimony brominated graphene oxide modified ABS composite flame retardant material and a preparation method thereof, aiming at the defects of the prior art.
The technical scheme adopted by the invention is as follows:
a preparation method of a molybdenum-antimony brominated graphene oxide modified ABS composite flame retardant material comprises the following steps:
1) synthesis of Sb-Mo/Br-RGO
Firstly, graphite oxide, carbon tetrabromide and triphenylphosphine are mixed, heated and stirred for at least 5 hours, and Br-GO powder is obtained after filtration, cleaning and drying;
dispersing the prepared Br-GO powder in deionized water to obtain a suspension, adding antimony trichloride and ammonium molybdate into the suspension, and reacting to obtain Sb-Mo/Br-GO powder;
thirdly, adding Sb-Mo/Br-GO powder into deionized water, performing ultrasonic treatment for at least 60min, and then dropwise adding a hydrazine hydrate solution under an alkaline condition to obtain antimony molybdate-loaded brominated reduced graphene Sb-Mo/Br-RGO;
2) synthesis of composite materials
And adding the prepared Sb-Mo/Br-RGO into ABS resin, melting, placing the mixture into an internal mixer with the rotating speed of 50rpm, stirring and mixing at 200 ℃ for at least 12min, and then placing the mixture into a mold for molding to obtain the molybdenum-antimony brominated graphene oxide modified ABS composite flame-retardant material.
In the above technical scheme, further, the mass ratio of the graphite oxide, the carbon tetrabromide and the triphenylphosphine in the step 1) is usually 1: 20-100: 4-20.
In the step II, the molar ratio of the antimony trichloride to the ammonium molybdate is usually 1: 1-1.2.
Further, in the step 2), Sb-Mo/Br-RGO is added into the ABS resin, and the addition amount is usually 0.5-10 wt% of the ABS resin.
The invention has the beneficial effects that:
the invention develops a novel Sb-Mo and Br-RGO composite synergistic flame-retardant system, wherein Br-RGO is synergistic with Sb, so that the flame-retardant efficiency of the flame-retardant system is greatly improved, and Br-RGO is synergistic with Mo, so that the smoke suppression effect of the flame-retardant system is effectively improved, and the flame retardant Sb-Mo/Br-RGO has double functions of flame retardance and smoke suppression. As a modifier of the high molecular material, Sb-Mo/Br-RGO has a good reinforcing effect on a polymer matrix, and can effectively improve the mechanical property of the high molecular material. Sb-Mo/Br-RGO also has the following advantages compared with conventional bromine-antimony-based flame retardants. Firstly, bromine is grafted on the surface of graphene through chemical grafting, so that the bromine is difficult to separate out from a matrix material, and secondary pollution to the environment is reduced. Secondly, the enhancement and the barrier effect of the graphene sheet layer are beneficial to improving the mechanical property, the thermal property, the flame retardant property and the like of the matrix material. And thirdly, the antimony molybdate loaded on the surface of the graphene can play a good isolation role, the agglomeration tendency of the graphene is effectively reduced, the problem of dispersibility of the graphene in the processing process is solved, and the nano-reinforcing effect of the graphene is fully exerted. In addition, the flame-retardant system is used as a nano additive, can be used for flame-retardant modification of polymers by melt blending, in-situ polymerization and other methods, and has good applicability. The GO used for preparing the flame retardant is easy to obtain raw materials and low in price, and the problem of economy of graphene in engineering application is well solved. Although the conventional bromine-antimony flame retardant has higher flame retardant efficiency, the smoke generation amount is larger, and a molybdenum-containing compound (such as ammonium molybdate) is usually selected as a smoke suppressant, but the ammonium molybdate is water-soluble and is easy to precipitate when being added into a polymer. As the Sb-Mo/Br-RGO and the ABS are fused and blended to prepare the ABS nano composite flame-retardant material, the Sb-Mo/Br-RGO can be uniformly dispersed in an ABS matrix, the flame retardant property of the ABS can be obviously improved, and the ABS nano composite flame-retardant material has good mechanical property; particularly, when the addition amount of Sb-Mo/Br-RGO reaches 5.0 wt%, compact carbon residue can be generated, and when the material encounters flame or heat flow, the material can effectively inhibit heat transfer and isolate oxygen, thereby delaying heat transfer and pyrolysis volatile substance escape, greatly improving flame retardant property and having tensile strength as high as 68.4 MPa.
Drawings
FIG. 1 is a schematic diagram of the synthesis of Sb-Mo/Br-RGO;
FIG. 2 is a TEM image of an ABS composite flame retardant material; (a) low magnification, (b) high magnification;
FIG. 3 is a TGA curve (a) and a DTG curve (b) of ABS and ABS composite at room temperature;
FIG. 4 is a heat release rate curve (a), a total heat release curve (b), a mass loss curve (c), a smoke generation rate curve (d) of ABS and ABS composite;
FIG. 5 is an electron photograph of carbon residue after cone calorimeter testing of (a) ABS and an ABS composite with the addition of (b)0.1 wt%, (c)1.0 wt%, and (d)5.0 wt% Sb-Mo/Br-RGO.
FIG. 6 is an SEM image of (a) ABS, (b) ABS/SbMo-BrG0.5, (c) ABS/SbMo-BrG5 carbon residue and an EDX spectrum (d) of carbon residue.
FIG. 7 is a graph of the tensile properties of ABS and its composites.
Detailed Description
The synthesis of Sb-Mo/Br-RGO consists essentially of three steps, as shown in FIG. 1:
the first step is the bromination of graphene oxide.
Graphene Oxide (GO) can be prepared by a modified Hummers method and dried under vacuum at room temperature for more than one week under a phosphorus pentoxide atmosphere. 250mg of graphene oxide is weighed, placed into a 100mL dry flask with a magnetic stirring rod, added with 15g of carbon tetrabromide and 3g of triphenylphosphine, heated to 150 ℃ after the addition is finished, stirred and reacted for 5 hours, and after the reaction mixture is cooled to room temperature, added with 30mL of ethanol. And filtering a mixture obtained by the reaction, repeatedly washing the mixture for 3 times by using methanol, and drying the mixture in vacuum to obtain brominated graphene (Br-GO).
The second step is to load the antimony molybdate on Br-GO.
Adding 1.0g of Br-GO into 100mL of deionized water, ultrasonically dispersing for 60min at room temperature, gradually adding a dilute hydrochloric acid solution containing 0.19g of antimony chloride and 0.44g of ammonium molybdate into the suspension, and continuously adding a dilute ammonia solution. And after stirring for 8 hours, repeatedly washing the prepared product by using deionized water, and performing suction filtration and separation by using a nylon membrane to obtain the antimony molybdate loaded brominated graphene (Sb-Mo/Br-GO).
The last step is the reduction of Sb-Mo/Br-GO with hydrazine hydrate.
Weighing 1.0g of Sb-Mo/Br-GO powder, adding the Sb-Mo/Br-GO powder into 250mL of deionized water, gradually adding 3.5mL of ammonia water with the concentration of 28% and 0.8mL of hydrazine hydrate after ultrasonic dispersion is carried out for 60min, heating the suspension to 60 ℃, continuing ultrasonic dispersion for 4h, washing a product obtained by reaction with deionized water, repeatedly washing the product with methanol for three times, and measuring to obtain the product, namely, antimony molybdate-loaded brominated reduced graphene (Sb-Mo/Br-RGO), wherein the density of the product is 2.84g/cm by measuring3。
0, 0.1, 0.5, 1.0 and 5.0 wt% of Sb-Mo/Br-RGO were added to an equal amount of ABS resin, respectively, and after melting, they were put into an internal mixer rotating at 50rpm and stirred and mixed at 200 ℃ for 12 min. And then putting the product into a die, preheating at 180 ℃ for 6min, and then extruding at 12MPa for 8min to finally obtain a sheet with the thickness of about 4.0 mm. The samples were designated ABS, ABS/Sb-Mo/Br-G0.1, ABS/Sb-Mo/Br-G0.5, ABS/Sb-Mo/Br-G1, and ABS/Sb-Mo/Br-G5, respectively.
FIG. 2 is a TEM image of a composite sample, which shows that the Sb-Mo/Br-RGO particles are uniformly dispersed in the ABS polymer matrix as a whole, and the high molecular material with a difference layer structure formed by the dispersion of dark gray or black graphene sheets in the matrix can be clearly seen. Through Fourier transform infrared spectroscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS) measurement and analysis, Sb and Mo elements in a composite material sample are successfully loaded on the brominated graphene.
Performing thermogravimetric analysis by using Q600SDT thermogravimetric analyzer, and heating to 600 ℃ from room temperature at a heating rate of 10 ℃/min; TGA curves, DTG curves (fig. 3) and test data (table 1) were obtained for ABS and ABS composites at room temperature;
TABLE 1 TGA test data for ABS and ABS composites
Ti aAnd Tmax aRespectively, the initial decomposition temperature and the maximum decomposition temperature.
It can be seen that the initial decomposition temperature of the material is higher and higher with the increase of the addition amount of Sb-Mo/Br-RGO, the residual amount of ABS is greatly increased with the increase of the addition amount of Sb-Mo/Br-RGO, the weight loss rate is obviously reduced, the thermal stability of ABS can be obviously improved, and the decomposition of ABS is delayed.
The test is carried out by using a cone calorimeter (ICONE), and the test is preheated for more than 2 hours before the test. Using aluminum foil at a thickness of 100X 4mm3The dimensions of (a) were to wrap the sides and bottom of the sample, leaving only the top surface exposed. Moving to a ventilation position after the last sample is burnt, and taking the next sample after at least 10 min. The three repeated measurements were averaged, and the flame retardant properties of each sample are shown in fig. 4, with the data shown in the following table:
TABLE 2 ABS and ABS composite materials Experimental data in Cone calorimeter testing
TTIa: the ignition time; PHRRa: peak heat release rate; THRa(ii) a Total amount of heat release; PSPRa: a peak smoke generation rate; TSPa: the total amount of smoke generated;
Chara: rate of carbon residue
It can be seen that the addition of Sb-Mo/Br-RGO can reduce the total heat release THR of ABS, and as the addition amount of Sb-Mo/Br-RGO is larger, the ignition time is prolonged, the THR is reduced more obviously, and simultaneously the mass loss rate of the ABS composite material is reduced, the carbon residue rate is increased, and the smoke generation rate peak value (PSPR) and the total smoke content (TSP) are both reduced obviously, especially when 5.0 wt% of Sb-Mo/Br-RGO is added, the TTI is prolonged by 12s, the PHRR is reduced by 38.26%, the THR is reduced by 27.4%, the PSPR is reduced by 61.4%, and the TSP is reduced by 53.6%. The flame retardance of ABS is improved obviously.
An electron photograph of carbon residue after cone calorimeter testing is shown in fig. 5, and a corresponding SEM image and EDX analysis are shown in fig. 6, it can be seen that for the ABS sample, it has completely burned, the remaining residue is negligible (fig. 5a), and the coke layer surface has a certain porous structure (fig. 6 a); while the composite sample has significant carbon residue, and when the addition amount of ABS/SbMo-BrG5 reaches 5.0 wt%, the carbon residue after combustion is at most and more compact, the SEM image can observe that a plurality of graphene nano sheets have good dispersibility and are connected with each other to form a barrier layer, the residue is continuous and compact, the C content is 51.9 wt%, the O content is 21.5 wt%, the Br content is 4.5 wt%, the Sb content is 12.7 wt%, and the Mo content is 11.4 wt%.
In addition, as shown in FIG. 7 and Table 3, the tensile strength of ABS and its composite material is 52.2MPa, the elongation at break is 35.1%, and with the increasing content of Sb-Mo/Br-RGO, the tensile strength of the obtained composite material is increased, but the elongation at break value is decreased. Namely, Sb-Mo/Br-RGO not only can obviously improve the flame retardant property of ABS, but also can enhance the tensile strength of the ABS composite material and reduce the elongation at break thereof.
TABLE 3 tensile Properties of ABS and its composites
Claims (5)
1. A preparation method of a molybdenum-antimony brominated graphene oxide modified ABS composite flame retardant material is characterized by comprising the following steps:
1) synthesis of Sb-Mo/Br-RGO
Firstly, graphite oxide, carbon tetrabromide and triphenylphosphine are mixed, heated and stirred for at least 5 hours, and Br-GO powder is obtained after filtration, cleaning and drying;
dispersing the prepared Br-GO powder in deionized water to obtain a suspension, adding antimony trichloride and ammonium molybdate into the suspension, and reacting to obtain Sb-Mo/Br-GO powder;
thirdly, adding Sb-Mo/Br-GO powder into deionized water, performing ultrasonic treatment for at least 60min, and then dropwise adding a hydrazine hydrate solution under an alkaline condition to obtain antimony molybdate-loaded brominated reduced graphene Sb-Mo/Br-RGO;
2) synthesis of composite materials
And adding the prepared Sb-Mo/Br-RGO into ABS resin, melting, placing the mixture into an internal mixer with the rotating speed of 50rpm, stirring and mixing at 200 ℃ for at least 12min, and then placing the mixture into a mold for molding to obtain the molybdenum-antimony brominated graphene oxide modified ABS composite flame-retardant material.
2. The preparation method of the molybdenum-antimony brominated graphene oxide modified ABS composite flame retardant material as claimed in claim 1, wherein the mass ratio of graphite oxide, carbon tetrabromide and triphenylphosphine in the step (i) is 1: 20-100: 4-20.
3. The preparation method of the molybdenum-antimony brominated graphene oxide modified ABS composite flame retardant material according to claim 1, wherein the molar ratio of antimony trichloride to ammonium molybdate in the step (II) is 1: 1-1.2.
4. The preparation method of the molybdenum-antimony brominated graphene oxide modified ABS composite flame retardant material according to claim 1, wherein in the step 2), Sb-Mo/Br-RGO is added into the ABS resin, and the addition amount is 0.5-10 wt% of the ABS resin.
5. The molybdenum-antimony brominated graphene oxide modified ABS composite flame retardant material is characterized by being prepared by the method of any one of claims 1-4.
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| CN105153564A (en) * | 2015-10-21 | 2015-12-16 | 山东科技大学 | Graphene-molybdenum oxide nano flame-retardant composite material |
| CN106220893A (en) * | 2015-12-27 | 2016-12-14 | 黄国波 | Antimony oxide load bromination Graphene fire retardant and its preparation method and application |
| CN106916337A (en) * | 2015-12-27 | 2017-07-04 | 黄国波 | Antimony oxide loads bromination Graphene fire retardant |
| CN106987109A (en) * | 2017-04-13 | 2017-07-28 | 郭峰 | The method that a kind of nanometer of dawsonite/stannic acid lanthanum/graphene oxide composite flame-proof is modified PC/ABS alloys |
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| CN105153564A (en) * | 2015-10-21 | 2015-12-16 | 山东科技大学 | Graphene-molybdenum oxide nano flame-retardant composite material |
| CN106220893A (en) * | 2015-12-27 | 2016-12-14 | 黄国波 | Antimony oxide load bromination Graphene fire retardant and its preparation method and application |
| CN106916337A (en) * | 2015-12-27 | 2017-07-04 | 黄国波 | Antimony oxide loads bromination Graphene fire retardant |
| CN106987109A (en) * | 2017-04-13 | 2017-07-28 | 郭峰 | The method that a kind of nanometer of dawsonite/stannic acid lanthanum/graphene oxide composite flame-proof is modified PC/ABS alloys |
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