CN109181207A - A kind of molybdenum-antimony bromination graphene oxide modified ABS composite flame-proof material and preparation method thereof - Google Patents
A kind of molybdenum-antimony bromination graphene oxide modified ABS composite flame-proof material and preparation method thereof Download PDFInfo
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- CN109181207A CN109181207A CN201811154054.8A CN201811154054A CN109181207A CN 109181207 A CN109181207 A CN 109181207A CN 201811154054 A CN201811154054 A CN 201811154054A CN 109181207 A CN109181207 A CN 109181207A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The invention discloses a kind of molybdenum-antimony bromination graphene oxide modified ABS composite flame-proof materials and preparation method thereof, ABS nanometer flame retardent materials are prepared using Sb-Mo/Br-RGO and ABS melt blending, Sb-Mo/Br-RGO is dispersed in ABS matrix, graphene nanometer sheet is connected to each other to form barrier layer, the flame retardant property of ABS can be significantly improved, the tensile strength of material is promoted simultaneously, especially when the additive amount of Sb-Mo/Br-RGO reaches 5.0wt%, it can produce fine and close carbon residue, when material encounters flame or hot-fluid, heat transfer and isolation oxygen can be effectively suppressed, to delay heat transfer and the evolution of pyrolysis devolatilization object, greatly improve flame retardant property, and tensile strength is up to 68.4MPa.
Description
Technical field
The invention belongs to fire proofing preparation technical field, it is related to a kind of ABS fire proofing and preparation method thereof, especially relates to
And a kind of molybdenum-antimony bromination graphene oxide modified ABS composite flame-proof material and preparation method thereof.
Background technique
ABS resin is a part indispensable in current life.It has polystyrene (PS), styrene-the third simultaneously
Alkene lonitrile copolymer (SAN), the various performances of butadiene-styrene copolymer (BS), so there is excellent comprehensive performance.It is
A kind of to have fabulous impact strength, toughness is strong, wear-resisting, the thermoplastic, polymeric materials of processing and machining easy to form, extensively
It is general to be applied to the fields such as packaging, furniture, automobile, electronic apparatus and building materials.But ABS is easy burning, can release black smog
And toxic gas.Serious property loss is brought to the production and living of people in this way, also destroys environment.So should improve
The flame retardant property and smoke suppressing of ABS resin.
Flame Retardancy energy is improved often through addition fire retardant when actual production.Common fire retardant has hydroxide
Fire retardant and expansion type flame retardant, the fire retardant mechanism of hydroxide flame retardant make polymeric outer surface generate charing guarantor when being burning
Sheath can completely cut off oxygen and polymer reaction in air；The fire retardant mechanism and hydroxide of conventional expanded type fire retardant hinder
Combustion agent is similar, and the surface of polymer will form one layer of dense foam layer of charcoal when it is heated, can make inside and the oxygen of polymer
It is isolated.But because they are only mixed with polymer simple physical, the mechanical property and processing performance meeting of polymer
It is affected.
Summary of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide a kind of molybdenum-antimony bromination graphene oxide modified ABS
Composite flame-proof material and preparation method thereof.
The technical solution adopted by the invention is as follows:
A kind of preparation method of molybdenum-antimony bromination graphene oxide modified ABS composite flame-proof material, includes the following steps:
1) synthesis of Sb-Mo/Br-RGO
1. by graphite oxide, carbon tetrabromide and triphenylphosphine Hybrid Heating and stirring at least 5h, is filtered, is cleaned and dried
To Br-GO powder；
2. Br-GO powder obtained dispersion is obtained suspension in deionized water, trichlorine is added in above-mentioned suspension
Change antimony and ammonium molybdate, reaction obtains Sb-Mo/Br-GO powder；
3. simultaneously ultrasound at least 60min is added in deionized water in Sb-Mo/Br-GO powder, then under alkaline condition by water
It closes hydrazine solution to be added dropwise wherein, molybdic acid antimony is made and loads bromination reduced graphene Sb-Mo/Br-RGO；
2) synthesis of composite material
Sb-Mo/Br-RGO obtained is added into ABS resin, melting is placed in the mixer that revolving speed is 50rpm,
It is stirred at least 12min at 200 DEG C, places into die for molding, it is multiple to obtain molybdenum-antimony bromination graphene oxide modified ABS
Close fire proofing.
In above-mentioned technical proposal, further, 1) the step of described in 1. in graphite oxide, carbon tetrabromide and triphenylphosphine
Mass ratio be usually 1:20~100:4~20.
2. the molar ratio of middle antimony trichloride and ammonium molybdate is usually 1:1~1.2 to the step.
Further, Sb-Mo/Br-RGO is added into ABS resin in the step 2), and additive amount is usually ABS tree
0.5~10wt% of rouge.
The beneficial effects of the present invention are:
The present invention develops novel Sb-Mo and the compound cooperative flame retardant system of Br-RGO, and wherein Br-RGO is cooperateed with Sb, greatly
The flame retarding efficiency of the flame-retardant system is improved greatly, and Br-RGO is cooperateed with Mo, and the suppression cigarette for effectively improving the flame-retardant system is acted on, is made
Fire retardant Sb-Mo/Br-RGO has fire-retardant, suppression cigarette dual function concurrently.As the modifying agent of high molecular material, Sb-Mo/Br-RGO pairs
Polymeric matrix has good humidification, can effectively improve the mechanical property of high molecular material.It is hindered compared to conventional bromo- antimony system
Agent is fired, Sb-Mo/Br-RGO has further the advantage that.First, bromo element passes through chemical graft on the surface of graphene, make it difficult to
It is precipitated, reduces caused by environment " secondary pollution " from basis material.Second, the enhancing of graphene sheet layer, barrier action have
Help improve basis material mechanical property, hot property and flame retardant property etc..Third, the molybdic acid antimony of load on the surface of graphene can rise
To good buffer action, graphene reunion tendency is effectively reduced, solves the dispersion problem of graphene in process,
Give full play to its nanometer of enhancement effect.In addition, the flame-retardant system can pass through melt blending, original position as a kind of nanometer additive
The methods of polymerization is modified for flame retardance of polymer, has good applicability.Be used to prepare the GO of the fire retardant, raw material be easy to get and
Price is lower, solves economy problems of the graphene in engineer application very well.Although conventional bromo- Sb system fire retardant have compared with
High flame retarding efficiency, but smoke amount is larger usually selects the compound (such as ammonium molybdate) containing molybdenum to be used as smoke suppressant, but ammonium molybdate by
In having water solubility, it is added in macromolecule and is easy precipitation, the present invention utilizes coprecipitation method by water-insoluble molybdenum-antimony chemical combination
Object loads to graphene surface, and makes molybdenum-antimonial uniform fold on the surface of graphene by the control of process conditions, reaches
Good buffer action, this is the key technology and difficult point that the present invention prepares fire retardant Sb-Mo/Br-RGO.Due to benefit of the invention
ABS nanometer flame retardent materials are prepared with Sb-Mo/Br-RGO and ABS melt blending, Sb-Mo/Br-RGO may be uniformly dispersed in
In ABS matrix, and the flame retardant property of ABS can be significantly improved, while there is good mechanical property；Especially work as Sb-Mo/Br-
When the additive amount of RGO reaches 5.0wt%, can produce fine and close carbon residue can be effectively suppressed heat when material encounters flame or hot-fluid
Amount transmitting and isolation oxygen greatly improve flame retardant property, and have up to delay heat transfer and the evolution of pyrolysis devolatilization object
68.4MPa tensile strength.
Detailed description of the invention
Fig. 1 is the synthesis schematic diagram of Sb-Mo/Br-RGO；
Fig. 2 is the TEM image of ABS composite flame-proof material；(a) low magnification, (b) high-amplification-factor；
Fig. 3 is the TGA curve (a) of ABS and ABS composite material at room temperature and DTG curve (b)；
Fig. 4 is the heat release rate curve (a) of ABS and ABS composite material, hot total volume curve (b), mass loss song
Line (c), raw cigarette rate curve (d)；
Fig. 5 is (a) ABS and addition (b) 0.1wt%, and (c) ABS of 1.0wt% and (d) 5.0wt%Sb-Mo/Br-RGO is multiple
The electronic photo of condensation material breeze after cone calorimetry test.
Fig. 6 is (a) ABS, (b) ABS/SbMo-BrG0.5's, (c) SEM image of ABS/SbMo-BrG5 carbon residue and breeze
EDX spectrum (d).
Fig. 7 is the graph of stretch performance of ABS and its composite material.
Specific embodiment
The synthesis of Sb-Mo/Br-RGO is mainly made of three steps, as shown in Figure 1:
The first step is the bromination of graphene oxide.
Graphene oxide (GO) can be prepared by improved Hummers method, and room temperature is true under phosphorus pentoxide atmosphere
More than sky is dried for a week.250mg graphene oxide is weighed, is put into the dry flask of the 100mL with magnetic stirring bar, 15g is added
Carbon tetrabromide and 3g triphenylphosphine, are warming up to 150 DEG C, while being stirred to react 5h, are cooled to reaction mixture after addition
After room temperature, 30ml ethyl alcohol is added into solution.The mixture filtering that reaction is obtained, is washed 3 times with methanol, then repeatedly in vacuum
Middle drying to get arrive bromination graphene (Br-GO).
Second step is that molybdic acid antimony is supported on Br-GO.
Take 1.0g Br-GO to be added in 100mL deionized water, ultrasonic disperse 60min at room temperature, then in suspension by
The dilute hydrochloric acid solution and 0.44g ammonium molybdate of the antimony chloride containing 0.19g is gradually added, continuously adds dilute ammonia solution.After stirring 8h, spend
Ionized water washs obtained product repeatedly, and carries out filtering separation to get molybdic acid antimony load bromination graphene is arrived with nylon membrane
(Sb-Mo/Br-GO)。
Final step is to restore Sb-Mo/Br-GO using hydrazine hydrate.
1.0g Sb-Mo/Br-GO powder is weighed to be added in the deionized water of 250mL, after ultrasonic disperse 60min, by
The hydrazine hydrate of 3.5mL ammonium hydroxide and 0.8mL that concentration is 28% is gradually added, after suspension is warming up to 60 DEG C, continues ultrasonic disperse
4h will react resulting product and be washed with deionized, and be washed repeatedly three times with methanol, and resulting product is that molybdic acid antimony is negative
It carries bromination reduced graphene (Sb-Mo/Br-RGO), measurement can obtain the density 2.84g/cm of product3。
Add 0,0.1,0.5,1.0 and 5.0wt%Sb-Mo/Br-RGO respectively into equivalent ABS resin, melting is placed on
Revolving speed is to be stirred at 200 DEG C, time 12min in the mixer of 50rpm.Next product is put into mold, first
6min is preheated at 180 DEG C, squeezes 8min under 12MPa, the sheet material that last available thickness is about 4.0mm.It orders respectively
Entitled ABS, ABS/Sb-Mo/Br-G0.1, ABS/Sb-Mo/Br-G0.5, ABS/Sb-Mo/Br-G1 and ABS/Sb-Mo/Br-G5
Five samples.
Fig. 2 is the TEM image of composite sample, it can be seen that Sb-Mo/Br-RGO particle is integrally dispersed in ABS
In polymer substrate, it may be clearly seen that the graphene sheet layer of Dark grey or black, which is dispersed in, forms poor layer structure in matrix
High molecular material.It is fourier transformed infrared spectroscopy (FT-IR), x-ray photoelectron spectroscopy (XPS) measurement analysis, composite material
Sb and Mo element is successfully supported on bromination graphene in sample.
Thermogravimetric analysis is carried out using Q600SDT thermogravimetric analyzer, is heated to 600 from room temperature with the heating rate of 10 DEG C/min
℃；Obtain TGA curve, DTG curve (Fig. 3) and the test data (table 1) of ABS and ABS composite material at room temperature；
The TGA test data of 1 ABS of table and ABS composite material
Ti aAnd Tmax aRespectively refer to initial decomposition temperature and maximum decomposition temperature.
As can be seen that the initial decomposition temperature of material is higher and higher with the increase of Sb-Mo/Br-RGO additive amount, and with
The increase of Sb-Mo/Br-RGO additive amount, the residual volume of ABS be significantly increased, weight loss rate is substantially reduced, and is remarkably improved ABS
Thermal stability and delay the decomposition of ABS.
It is tested using cone calorimetry (ICONE), preheats 2h or more before testing.With aluminium foil with 100 × 100 × 4mm3Rule
Lattice encase the side and bottom surface of sample, only exposed upper surface.Move to ventilation after a upper sample combustion, at least every
Next sample is made after 10min.Duplicate measurements is averaged three times, and each sample flame retardant property is as shown in figure 4, data are as follows:
The experimental data of 2 ABS of table and ABS composite material in cone calorimetry test
TTIa: the duration of ignition；PHRRa: heat release rate peak value；THRa；Hot total volume；PSPRa: raw cigarette rate peak value；
TSPa: raw cigarette total amount；
Chara: carbon yield
It can be seen that the addition of Sb-Mo/Br-RGO can be such that the total heat release THR of ABS is reduced, and with Sb-Mo/
Br-RGO additive amount is more, and the duration of ignition extends, and THR reduces to be more obvious, while the mass loss rate of ABS composite material subtracts
Small, carbon yield increases, and raw cigarette rate peak value (PSPR) and total smoke (TSP) are all substantially reduced, especially addition 5.0wt%Sb-Mo/
TTI can be made to extend 12s when Br-RGO, PHRR, which reduces 38.26%, THR and reduces 27.4%, PSPR, reduces 61.4%, TSP
Reduce 53.6%.The anti-flammability of ABS is significantly improved.
The electronic photo of carbon residue is as shown in figure 5, corresponding SEM image and EDX are analyzed such as Fig. 6 institute after cone calorimetry test
Show, it can be seen that for ABS sample, completely burned, the residue left be can be ignored (Fig. 5 a), coke layer surface
It is upper that there is certain porous structure (Fig. 6 a)；And composite sample then has obvious carbon residue, and adding as ABS/SbMo-BrG5
When dosage reaches 5.0wt%, the carbon left after burning is most and more compact in contrast, and many graphenes can be observed in SEM figure
Nanometer sheet has good dispersion, and is connected to each other and to form barrier layer, and residue is continuously fine and close, C content 51.9wt%,
O content is 21.5wt%, and Br content is 4.5wt%, and the content of Sb is 12.7wt%, and the content of Mo is 11.4wt%.
In addition, ABS and its Tensile Properties of Composites, as shown in Fig. 7 and table 3, the tensile strength of ABS is 52.2MPa, break
Splitting elongation is 35.1%, and with gradually increasing for addition Sb-Mo/Br-RGO content, the tensile strength of gained composite material is not
Disconnected enhancing, but extension at break rate score is on a declining curve.That is Sb-Mo/Br-RGO is not only remarkably improved the flame retardant property of ABS,
Simultaneously can also reinforced ABS composite material tensile strength, reduce its elongation at break.
The tensile property parameter of 3 ABS of table and its composite material
Claims (5)
1. a kind of molybdenum-antimony bromination graphene oxide modified ABS composite flame-proof material preparation method, which is characterized in that including such as
Lower step:
1) synthesis of Sb-Mo/Br-RGO
1. by graphite oxide, carbon tetrabromide and triphenylphosphine Hybrid Heating and stirring at least 5h, is filtered, is cleaned and dried to obtain
Br-GO powder；
2. Br-GO powder obtained dispersion is obtained suspension in deionized water, antimony trichloride is added in above-mentioned suspension
And ammonium molybdate, reaction obtain Sb-Mo/Br-GO powder；
3. simultaneously ultrasound at least 60min is added in deionized water in Sb-Mo/Br-GO powder, then under alkaline condition by hydrazine hydrate
Solution is added dropwise wherein, and molybdic acid antimony is made and loads bromination reduced graphene Sb-Mo/Br-RGO；
2) synthesis of composite material
Sb-Mo/Br-RGO obtained is added into ABS resin, melting is placed in the mixer that revolving speed is 50rpm, 200
It is stirred at least 12min at DEG C, places into die for molding, obtains molybdenum-antimony bromination graphene oxide modified ABS composite flame-proof
Material.
2. molybdenum according to claim 1-antimony bromination graphene oxide modified ABS composite flame-proof material preparation method,
Be characterized in that, the step 1. in graphite oxide, carbon tetrabromide and triphenylphosphine mass ratio be 1:20~100:4~20.
3. molybdenum according to claim 1-antimony bromination graphene oxide modified ABS composite flame-proof material preparation method,
It is characterized in that, 2. the molar ratio of middle antimony trichloride and ammonium molybdate is 1:1~1.2 to the step.
4. molybdenum according to claim 1-antimony bromination graphene oxide modified ABS composite flame-proof material preparation method,
Be characterized in that, Sb-Mo/Br-RGO is added into ABS resin in the step 2), additive amount be ABS resin 0.5~
10wt%.
5. a kind of molybdenum-antimony bromination graphene oxide modified ABS composite flame-proof material, which is characterized in that using such as claim 1-4
Described in any item methods are made.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2024036756A1 (en) * | 2022-08-19 | 2024-02-22 | 台州学院 | Multifunctional phosphorus and nickel doped graphite-like carbon nitride nanosheet, preparation method therefor, and abs material |
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| US20170260389A1 (en) * | 2012-06-29 | 2017-09-14 | Frx Polymers, Inc. | Polyester co-phosphonates |
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| US20170260389A1 (en) * | 2012-06-29 | 2017-09-14 | Frx Polymers, Inc. | Polyester co-phosphonates |
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| CN106220893A (en) * | 2015-12-27 | 2016-12-14 | 黄国波 | Antimony oxide load bromination Graphene fire retardant and its preparation method and application |
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| 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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| WO2024036756A1 (en) * | 2022-08-19 | 2024-02-22 | 台州学院 | Multifunctional phosphorus and nickel doped graphite-like carbon nitride nanosheet, preparation method therefor, and abs material |
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