CN103275408B - The preparation method of a kind of Graphene/layered double-hydroxide composite fire retardant and pipe/polyhenylethylene nano flame-proof composite material - Google Patents
The preparation method of a kind of Graphene/layered double-hydroxide composite fire retardant and pipe/polyhenylethylene nano flame-proof composite material Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
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Abstract
The preparation method of a kind of Graphene/layered double-hydroxide composite fire retardant and pipe/polyhenylethylene nano flame-proof composite material: comprise and carbon nanotube is dissolved in graphene oxide colloid, stir and utilize ultrasonic wave disperse make it be uniformly dispersed after add M
2+salt and Al
3+add urea after salt, obtain graphene/carbon nano-tube/layered double-hydroxide after back flow reaction composite assembled, by composite assembled mix with polystyrene resin after melt extrude and obtain pipe/polyhenylethylene nano flame-proof composite material.The present invention utilizes stannic oxide/graphene nano sheet dispersing Nano carbon tubes, and while utilizing urea to regulate and control the pH value of solution graphene oxide being reduced to Graphene, to prepare graphene/carbon nano-tube/layered double-hydroxide composite assembled.The polystyrene nano composite material utilizing extrusion by melting to prepare has good flame retardant properties and mechanical property.
Description
Technical field
The present invention relates to a kind of preparation method of halogen free nanometer composite flame-retardant agent, belong to the technical field of the preparations and applicatio of inorganic composite flame retardants.
Background technology
Polystyrene is one of five large general-purpose plastics, and its goods are widely used among the every profession and trades such as electrical equipment, decoration, building, traffic, military project.But polystyrene is very easy to burning, in combustion processes, melting drippage is serious and discharge a large amount of black smoke, be therefore necessary very much to its carry out fire-retardant, press down cigarette process to improve the security of its application.The material fire-retardant due to halogenated flame retardant can produce poisonous, mordant smog in a large number when burning, and has pollution, corrosive nature to environment, mould.Based on the requirement of environment protection and Sustainable development, halogen-free flame-retardant system will have vast potential for future development.The halogen-free flame retardants system being usually used in polymkeric substance mainly comprises phosphorus system, nitrogen system, silicon system, metal hydroxides etc., if nanoparticle can be scattered in polymeric matrix well form the flame retardant properties that nano composite material can improve polymkeric substance.Halogen free nanometer composite fire retardant demonstrates the tempting prospect as flame-proofed polymer material, particularly in reduction material Thermal release performance and to meet in environmental requirement more for people favors.
Graphene is by a kind of carbonaceous novel material of monolayer carbon atom tightly packed one-tenth bi-dimensional cellular shape crystalline structure, there is such as lower production cost, the advantages such as high-specific surface area, good mechanical property and superior conductivity, these superior characteristics make this novel material of Graphene demonstrate tempting application prospect (Shi Y in the flame retardant area of polymkeric substance, Li LJ. Chemically modified graphene:flame retardant or fuel for combustion J. Mater. Chem. 2011,21:3277-3279.).Very easily reunite between Graphene blade in graphene/polymer nano composite material, this is unfavorable for its fire-retardant to polymkeric substance.Layered double-hydroxide (LDH) is the compound piled up by interlayer anion and positively charged laminate, and its chemical constitution can be expressed as [M
2+ 1-xm
3+ x(OH)
2] (A
n-)
x/nmH
2o, wherein M
2+represent divalent metal, as Mg
2+, Zn
2+, Cu
2+, Ni
2+deng; M
3+for trivalent metal cation, as Al
3+, Cr
3+, Fe
3+, Ga
3+deng; A
n-for the tradable negatively charged ion of interlayer, as Cl
-, NO
3 -, CO
3 2-, OH
-, SO
4 2-deng; x=M
3+/ (M
2++ M
3+) the ratio of amount of substance, usually can obtain pure LDH in 0.2 ~ 0.33 scope, m is middle water Molecules.The metal ion existed in LDH synusia is the active principle eliminated smoke; Product after decomposition is Alkaline porous material, and specific surface is large, can adsorb obnoxious flavour particularly sour gas.Thus LDH can be used as the fire-retardant and smoke suppressant of polymkeric substance.But inorganic combustion inhibitor needs larger loading level just can reach desirable flame retardant effect usually, but the extremely lower degradation problem of processing caused by large addition and product mechanical property is all more serious.Therefore develop low loading level and little composite efficient fire retardant is affected on material mechanical performance and have important practical significance and scientific research value.
Propose in patent CN20110425506.3 and CN201110425497.8 to utilize electrochemistry and hydrothermal method to prepare the method for graphene/nickel aluminium LDH matrix material, prepared matrix material is mainly used in electrode material for super capacitor, adopt hydrothermal method (Wang Z, Zhang X, Wang JH, Zou L, Liu ZT, Hao ZP. Preparation and capacitance properties of graphene/NiAl layered double-hydroxide nanocomposite. Journal of Colloid and Interface Science, 2013, 396:251-257.), coprecipitation method (Li MX, Zhu JE, Zhang LL, Chen X, Zhang HM, Zhagn FZ, Xu SL, Evans DG. Facile synthesis of NiAl-layered double hydroxide/graphene hybrid with enhanced electrochemical properties for detection of dopamine. Nanoscale, 2011, Graphene 3:4240-4246.) prepared/(cobalt aluminium, nickel aluminium) LDH matrix material can be used for electrode material for super capacitor and detects Dopamine HCL etc.So far, yet there are no Graphene/LDH matrix material and be used as the report of fire retardant, and the matrix material adopting aforesaid method to prepare still exists and yields poorly, the shortcomings such as graphene nano lamella, the reunion of LDH lamella, this is unfavorable for the performance of its flame retarding efficiency in the polymeric material.
Summary of the invention
For the problems referred to above, technical problem to be solved by this invention finds a kind of polystyrene fire retardant, meets halide-free smokeless simultaneously, burning does not produce toxic gas, addition is little, to objects such as the Effect on Mechanical Properties of material are less.
In order to solve the problem, the invention provides a kind of Graphene/layered double-hydroxide halogen free nanometer composite flame-retardant agent, one dimension carbon nanotube (CNTs) is introduced in advance the accumulation suppressing graphene film between two-dimensional graphene sheet, utilize Graphene, carbon nanotube, layered double-hydroxide to carry out cooperative flame retardant polymer materials.
The technical solution adopted in the present invention is:
A preparation method for Graphene/layered double-hydroxide composite fire retardant and pipe/polyhenylethylene nano flame-proof composite material, comprises the following steps:
1. compound concentration is graphene oxide (GO) colloid of 0.05-1g/L, after being added by the one dimension carbon CNTs of acidifying, mixture is carried out ultrasonic disperse 2-12h under condition of ice bath, obtains the colloidal dispersion of light/dark balance; The mass ratio of GO and CNTs is 1:1-1:20.
2. by M
2+salt and Al
3+salt (mol ratio is 2:1) successively adds the GO/CNTs colloidal dispersion that step (1) obtains, and adds urea (urea and Al after Keep agitation 10-30min
3+the mol ratio of salt is 10:1-20:1), mixing solutions refluxes after 24h at 80-100 DEG C, is cooled by suspension and uses distilled water and ethanol repetitive scrubbing, then in 60 DEG C of vacuum drying ovens dry 24h to prepare GO/CNTs/LDH composite assembled.Described M is any one in Mg, Zn, Co, Ni, Ca.
3., by composite assembled for GO/CNTs/LDH 1-10 part, polystyrene 100 parts mixing, with homogenizer mixing, obtains raw mixture, melt extrudes shaping by raw mixture through twin screw extruder, obtain pipe/polyhenylethylene nano flame-proof composite material.
The processing parameter of described twin screw extruder is, length-to-diameter ratio is 20, and screw diameter is 40mm, and screw speed is 200-220rpm; Barrel temperature is 180-200 DEG C, and head temperature is 190-200 DEG C, and extruder temperature is 180-190 DEG C.
Positively effect of the present invention is as follows:
1, one dimension carbon nanotube is introduced in advance GO colloid and prepare the effect that Graphene/CNTs/LDH assembly can play prevention graphene film and the reunion of LDH blade, play the effect that synergistic is fire-retardant simultaneously.
What 2, prepared by the present invention is composite assembled compared with halogen flame, decreases and endangers the secondary of environment, thus reach the requirement of environmental protection.
3, the splicing structure of composite assembled the formed lamella prepared of the present invention and one-dimensional nano line, present flame retarding efficiency when fire retardant polystyrene high, addition is little, has the effect pressing down cigarette simultaneously, and less to the Effect on Mechanical Properties of matrix material.
Accompanying drawing explanation
Table 1 gives the mechanical property of pure polystyrene resin and each embodiment matrix material, from table, compared with polystyrene resin, tensile strength, the shock strength change of matrix material are little, illustrate that adding the Effect on Mechanical Properties of matrix material of Graphene/layered double-hydroxide composite fire retardant is less.
Fig. 1 is the SEM figure that the embodiment of the present invention 1 prepares polystyrene nano composite material, and as seen from Figure 1, in polystyrene nano composite material, compact layer distributes homogeneous in polystyrene matrix, there is not agglomeration (magnification is 5000 times) significantly.
Fig. 2 is the XRD figure of polystyrene nano composite material prepared by the embodiment of the present invention 1, as seen from Figure 2, there is not the charateristic avsorption band of LDH and Graphene in matrix material, illustrate that nanometer sheet is peeled off in the composite compared with polystyrene, forms exfoliated polystyrene nano composite material.
Fig. 3 is the polystyrene nano composite material of embodiment 1 preparation and the heat release rate curve of pure polystyrene, as seen from Figure 3, compared with pure polystyrene, the peak heat release rate of polystyrene nano composite material declines about 45%, and the flame retardant properties of matrix material significantly improves.
Fig. 4 is the polystyrene nano composite material of embodiment 1 preparation and the raw cigarette rate curve of pure polystyrene, as seen from Figure 4, compared with pure polystyrene, the raw cigarette speed of polystyrene nano composite material has obvious decline, wherein the raw cigarette speed in peak declines about 25%, and composite material exhibits is good smoke suppressing effect.
Fig. 5 is the photo after the polystyrene nano composite material burning of the embodiment of the present invention 1 preparation, and left figure is polystyrene, and right figure is polystyrene nano composite material, as seen from the figure, almost burnouts after polystyrene burns, does not have resistates; After polystyrene nano composite material burning compared with polystyrene resistates showed increased, illustrate and composite assembledly serve good protection polystyrene matrix and fire-retardant effect.
Embodiment
Below by way of specific embodiment, foregoing of the present invention is described in further detail.But this should be interpreted as content of the present invention is only limitted to following example.
Embodiment 1
A preparation method for Graphene/layered double-hydroxide composite fire retardant and pipe/polyhenylethylene nano flame-proof composite material, step is as follows:
(1) (preparation method is see Hummers W S to prepare the GO colloid of 1L 0.05g/L, Offeman R E. Preparation of graphite oxide. J Am Chem Soc, 1958, 80:1339), by 0.2g CNTs(purchased from Chengdu Organical Chemical Co., Ltd., Chinese Academy of Sciences) (souring method is see Han YQ after acidifying, Shen MX, Lin XC, Ding B, Zhang LJ, Tong H, Zhang XG. Ternary phase interfacial polymerization of polypyrrole/MWCNT nanocomposites with core-shell structure. Synthetic Metals, 2012, 162:753-758.) add, mixture is carried out ultrasonic disperse 2h under condition of ice bath, obtain the colloidal dispersion of light/dark balance.
(2) by 0.2 mol MgCl
2(purchased from Nanjing Chemistry Reagent Co., Ltd.) and 0.1molAlCl
3(purchased from company limited of Nanjing Chemistry Reagent Co., Ltd.) successively adds in the GO/CNTs dispersion liquid that step (1) obtains, the urea of 1mol is added after Keep agitation 10min, mixing solutions refluxes after 24h at 80-100 DEG C, suspension is cooled and uses distilled water and ethanol repetitive scrubbing, then in 60 DEG C of vacuum drying ovens dry 24h to prepare GO/CNTs/LDH composite assembled.
(3) by composite assembled for GO/CNTs/LDH 5 parts, general purpose polystyrene resin (PG-383, purchased from Taiwan Qimei Industry Co., Ltd.) 100 parts of mixing, mix with homogenizer, obtain raw mixture, raw mixture is melt extruded through twin screw extruder shaping, obtains pipe/polyhenylethylene nano flame-proof composite material.The processing parameter of twin screw extruder is length-to-diameter ratio is 20, and screw diameter is 40mm, and screw speed is 200-220rpm, and barrel temperature is 180-200 DEG C, and head temperature is 190-200 DEG C, and extruder temperature is 180-190 DEG C.
The preparation method of embodiment 2 one kinds of Graphenes/layered double-hydroxide composite fire retardant and pipe/polyhenylethylene nano flame-proof composite material, its place different from embodiment 1 is that the concentration of GO colloid becomes 0.1g/L, the quality of CNTs becomes 1g, and ultrasonic disperse 2h becomes 6h; MgCl in step 2
2become ZnCl
2; Composite assembledly in step 3 become 2 parts from 5 parts.
The preparation method of embodiment 3. 1 kinds of Graphenes/layered double-hydroxide composite fire retardant and pipe/polyhenylethylene nano flame-proof composite material, its place different from embodiment 1 is that the volume of GO colloid in step one becomes 4L from 1L, the quality of CNTs becomes 4g, ultrasonic disperse 2h becomes 12h, composite assembledly in step 3 becomes 1 part from 5 parts.
The preparation method of embodiment 4. 1 kinds of Graphenes/layered double-hydroxide composite fire retardant and pipe/polyhenylethylene nano flame-proof composite material, its place different from embodiment 1 is MgCl in step 2
2mole number become become 0.5mol from 0.2mol, MgCl
2become CoCl
2, AlCl
3mole number become 0.25mol from 0.1mol, the mole number of urea becomes 3mol from 1mol, composite assembledly in step 3 becomes 8 parts from 5 parts.
The preparation method of embodiment 5. 1 kinds of Graphenes/layered double-hydroxide composite fire retardant and pipe/polyhenylethylene nano flame-proof composite material, its place different from embodiment 1 is that the volume of GO colloid in step one becomes 5L from 1L, the quality of CNTs becomes 1.5g from 0.2g, and ultrasonic disperse 2h becomes 12h.MgCl in step 2
2mole number become 1mol from 0.2mol, MgCl
2become NiCl
2, AlCl
3mole number become 0.5mol from 0.1mol, the mole number of urea becomes 10mol from 1mol, composite assembledly in step 3 becomes 1 part from 5 parts.
The preparation method of embodiment 6. 1 kinds of Graphenes/layered double-hydroxide composite fire retardant and pipe/polyhenylethylene nano flame-proof composite material, its place different from embodiment 1 is that the volume of GO colloid in step one becomes 2L from 1L, and the quality of CNTs becomes 0.1g from 0.2g.MgCl in step 2
2mole number become 0.4mol from 0.2mol, MgCl
2become CaCl
2, AlCl
3mole number become 0.2mol from 0.1mol, the mole number of urea becomes 2mol from 1mol, composite assembledly in step 3 becomes 10 parts from 5 parts.
The composite flame-proof material that embodiment 2-6 obtains shows after testing afterwards: the composite material nanometer sheet prepared is peeled off in the composite, forms exfoliated polystyrene nano composite material; And compact layer distributes homogeneous in polystyrene matrix in polystyrene nano composite material, there is not agglomeration significantly; Compared with pure polystyrene, the raw cigarette speed of polystyrene nano composite material has obvious decline, and wherein the raw cigarette speed in peak declines about 25-50%, and composite material exhibits is good smoke suppressing effect, and flame retardant properties significantly improves; And after polystyrene nano composite material burning compared with polystyrene resistates showed increased, illustrate and composite assembledly serve good protection polystyrene matrix and fire-retardant effect.
The mechanical property of the pure polystyrene resin of table 1 and each embodiment matrix material
| Material | Tensile strength (MPa) | Izod notched impact strength (KJ/m2) |
| Pure polystyrene | 18.5 | 1.2 |
| Embodiment 1 | 20.5 | 1.3 |
| Embodiment 2 | 19.5 | 1.5 |
| Embodiment 3 | 18.8 | 1.6 |
| Embodiment 4 | 17.8 | 1.0 |
| Embodiment 5 | 21.2 | 1.8 |
| Embodiment 6 | 18.2 | 0.9 |
Claims (5)
1. a preparation method for pipe/polyhenylethylene nano composite flame-proof material, is characterized in that step is as follows:
(1) carbon nanotube of acidifying is added in graphene oxide colloid, stirring, the ultrasonic colloidal dispersion obtaining black under condition of ice bath, for subsequent use;
(2) by M
2+salt and Al
3+salt is successively added in step (1) gained colloidal dispersion, stir and add urea, after mixing solutions refluxes, cooled by gained suspension and to use distilled water and ethanol repetitive scrubbing, drying to prepare graphene/carbon nano-tube/layered double-hydroxide composite assembled, for subsequent use, M is Mg, Zn, any one in Co, Ni, Ca;
(3) composite assembled in step (2) is mixed with polystyrene resin, with homogenizer mixing, obtain raw mixture, raw mixture is melt extruded through twin screw extruder shaping, obtain pipe/polyhenylethylene nano composite flame-proof material.
2. the preparation method of pipe/polyhenylethylene nano composite flame-proof material according to claim 1, it is characterized in that the concentration of graphene oxide colloid is 0.05-1g/L in step (1), the mass ratio of the carbon nanotube of graphene oxide and acidifying is 1:1-1:20, and the ultrasonic disperse time is 2-12h.
3. the preparation method of pipe/polyhenylethylene nano composite flame-proof material according to claim 1, is characterized in that step (2) M
2+salt and Al
3+the mol ratio of salt is 2:1, urea and Al
3+the mol ratio of salt is 10:1-20:1, and mixing solutions return time is 24h.
4. the preparation method of pipe/polyhenylethylene nano composite flame-proof material according to claim 1, it is characterized in that mass fraction composite assembled in step (3) is 1-10 part, the mass fraction of polystyrene resin is 100 parts.
5. the preparation method of pipe/polyhenylethylene nano composite flame-proof material according to claim 1, it is characterized in that the processing parameter of the twin screw extruder described in step (3) is, length-to-diameter ratio is 20, and screw diameter is 40mm, and screw speed is 200-220rpm; Barrel temperature is 180-200 DEG C, and head temperature is 190-200 DEG C, and extruder temperature is 180-190 DEG C.
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| CN107163289B (en) * | 2017-06-20 | 2020-04-07 | 安徽建筑大学 | Layered double hydroxide-molybdate ion modified graphene flame-retardant smoke suppressant and preparation method thereof |
| CN108559225B (en) * | 2018-04-28 | 2020-09-15 | 济宁学院 | Preparation method of graphene/epoxy resin flame-retardant composite material |
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