CN106243388A - A kind of metal oxide-loaded nano-particle of graphite phase carbon nitride with flame-retardant smoke inhibition function and preparation method and application - Google Patents
A kind of metal oxide-loaded nano-particle of graphite phase carbon nitride with flame-retardant smoke inhibition function and preparation method and application Download PDFInfo
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- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
Abstract
The invention discloses a kind of metal oxide-loaded nano-particle of graphite phase carbon nitride with flame-retardant smoke inhibition function and preparation method and application.The method prepares g C for raw material by high temperature pyrolytic cracking (HTP) with carbamide or tripolycyanamide3N4；Then select metal oxide precursor, use the methods such as co-precipitation, Hydrothermal Synthesis or high temperature sintering to be carried on g C3N4On lamella, prepare the functionalization g C of a kind of metal oxide-loaded nano-particle3N4.By this functionalization g C3N4It is applied in polymeric matrix, thus is formed and there is the flame-proofed polymer material pressing down cigarette attenuated nature.The present invention have selected a class two-dimensional nanoparticle g C3N4As supporting carrier, nano-metal-oxide deposition is dispersed in g C3N4Surface, prepares functionalization g C3N4.The preparation technology that the present invention provides is simple, and raw material sources are extensive, have vast potential for future development in flame-retardant smoke inhibition field.
Description
Technical field
The invention belongs to material preparation and energetic material field, be specifically related to a kind of graphite-phase with flame-retardant smoke inhibition function
Metal oxide-loaded nano-particle of carbonitride and preparation method and application.
Background technology
Class Graphene lamellar compound g-C3N4As the polymer of a kind of excellent performance, have that density is low, chemical stability
Height, the advantages such as calorifics, good in optical property, wearability are strong, drive thing, catalyst carrier, organic reaction catalyst and light before the reaction
The fields such as catalyst have broad application prospects, thus get more and more people's extensive concerning for a long time.Additionally, as carbonitride
Most stable of allotrope, g-C3N4There is the two-dimensional structure of stacking, simultaneously because its huge specific surface area, can be in polymerization
Thing melt is formed network structure, forms effective Physical barriers at intrinsic silicon, reach heat insulation, oxygen barrier and suppression pyrolysis gas
The effect of the escape of body, thus reduce material combustion HRR and reach flame retardant effect.
Polymer not only can discharge heat also can discharge toxic gas when burning, and in fire process, smog and
Poisonous gas is maximum to the harm of people, according to statistics, in building fire about 75～85% the dead be owing to flue gas is lethal
's.Containing substantial amounts of CO, CO in this dense smoke2, the toxic gas such as HCHO, HCN, this constitutes pole to our personal safety
Big threat.And the catalysis for these poison gas is attenuated one of study hotspot being always catalytic field.Research finds, gold
Belong to oxide nano particles and include that transition metal oxide, rare-earth oxide etc. have excellent oxygen storage capacity, it is easy to
Converting between oxidized and reduced, thermodynamically oxidative dehydrogenation is favourable, can be catalyzed into carbon, reduces carbonization reaction
Required temperature.Additionally, metal oxide nanoparticles has stronger catalysis activity and selectivity to the gas such as CO, formaldehyde,
Therefore the burst size decomposing or reducing poison gas of the gas such as CO, formaldehyde can be effectively catalyzed.
g-C3N4Physical barrier effect is functioned only as when polymeric material burns, so single g-C3N4Flame retarding efficiency
Very limited, it is impossible to reach the flame retardant effect being more satisfied with, it would be desirable to it is carried out functional modification..Due to g-C3N4Have
Huge specific surface area, can occur effective interaction with metal oxide nanoparticles, be metal oxide nanoparticles
Excellent carrier.Therefore, functionalization g-C of metal oxide-loaded nano-particle is introduced3N4It is to reduce polymer combustion to have toxic smoke
Gas burst size, the effective ways of lifting fire resistance.
There is many metal-oxides such as Fe at present2O3, CuO, La2O3, TiO2Deng being successfully carried on g-C3N4Surface,
But they great majority are applied to other fields such as photocatalysis, and at flame retardance of polymer, to press down the research in terms of cigarette attenuation current
Report is less both at home and abroad.
Above with class Graphene lamellar compound g-C3N4As a example by, to functionalization g-C3N4Nano composite material is at polymer
In fire-retardant application present situation be briefly described and dissected.
Summary of the invention
It is an object of the invention to overcome the deficiencies in the prior art, it is provided that a kind of graphite-phase nitridation with flame-retardant smoke inhibition function
Metal oxide-loaded nano-particle of carbon and preparation method and application, i.e. functionalization g-C3N4, by this functionalization g-C3N4Application
In polymeric matrix, thus formed and there is the flame-proofed polymer material pressing down cigarette attenuated nature.
It is a further object to provide a kind of above-mentioned graphite phase carbon nitride gold-supported with flame-retardant smoke inhibition function
Belong to the easy preparation method of oxide nano particles.
For solving above technical problem, the present invention takes techniques below scheme.
A kind of preparation method of the metal oxide-loaded nano-particle of graphite phase carbon nitride with flame-retardant smoke inhibition function, institute
Method of stating prepares g-C for raw material by high temperature pyrolytic cracking (HTP) with carbamide or tripolycyanamide3N4；Then suitable metal-oxide is selected
Presoma, uses the methods such as co-precipitation, Hydrothermal Synthesis or high temperature sintering to be carried on g-C3N4On lamella, prepare a kind of tool
Having the metal oxide-loaded nano-particle of graphite phase carbon nitride of flame-retardant smoke inhibition function, concrete preparation process is as follows:
(1) it is firstly placed to tripolycyanamide or carbamide in baking oven dry, is subsequently adding in crucible and calcines in Muffle furnace, it
By supercooling, grind and prepare graphite phase carbon nitride g-C3N4。
(2) by the g-C of preparation in step (1)3N4It is dispersed in ultrasonic agitation in distilled water, makes g-C3N4In water, dispersion is all
Even.
(3) configure certain density metal salt solution, be slowly dropped in step (2) gained dispersion liquid continuation ultrasonic agitation
Until mix homogeneously, instilling a small amount of ammonia regulation pH value afterwards is 10～11.
(4) gained mixed solution in step (3) is joined in there-necked flask in thermostatical oil bath, it is stirred at reflux one section
Time, reaction carries out repeatedly centrifuge washing after terminating until gained filtrate is neutrality.
(5) product is put into after baking oven is dried, calcine in Muffle furnace and i.e. can get one there is flame-retardant smoke inhibition function
The metal oxide-loaded nano-particle of graphite phase carbon nitride.
Further, in step (1), the temperature of described baking oven is 60～80 DEG C, and drying time is 8～10h.
Further, in step (1), the temperature of described calcining is 500～600 DEG C, and the time of calcining is 4～6h.
Further, in step (2), the described ultrasonic time is 3～5h.
Further, in step (3), the slaine in described metal salt solution is in transition metal salt and rare earth metal salt
One or more；The concentration of described metal salt solution is 0.05～0.15mol/L.
Further, one or more during described transition metal salt is cobalt salt, iron salt and mantoquita；Described rare earth metal
Salt is cerium salt.
Further, in step (3), the described ultrasonic time is 1～2h.
Further, in step (4), the temperature of described reaction is 90～100 DEG C, and the time of reaction is 6～10h.
Further, in step (4), described centrifugal rotating speed is 6000～8000r/min, the centrifugal time be 10～
20min；Described washing is repeatedly to wash with water and ethanol successively.
Further, in step (5), the temperature of described baking oven is 70～90 DEG C, and the time being dried is 6～8h；Described forge
The temperature burnt is 250～350 DEG C, and the time of calcining is 2～4h.
There is a kind of graphite phase carbon nitride carried metal oxygen with flame-retardant smoke inhibition function that made as described above method prepares
Compound nano-particle, have selected the two-dimensional nano particle g-C that a class is novel3N4As supporting carrier, nano-metal-oxide is sunk
Integration is dispersed in g-C3N4Surface, prepares a kind of metal oxide-loaded nanometer of graphite phase carbon nitride with flame-retardant smoke inhibition function
Granule, i.e. functionalization g-C3N4。
Above-described a kind of metal oxide-loaded nano-particle of graphite phase carbon nitride with flame-retardant smoke inhibition function exists
Application in flame-proofed polymer material.
Compared with prior art, present invention have the advantage that
1. in the research of forefathers, g-C3N4Application at fire protection field is not yet developed.Although additionally, having had many gold
Belong to oxide such as Fe2O3, CuO, La2O3, TiO2Deng being successfully carried on g-C3N4Surface, but they great majority are applied to light
Other fields such as catalysis, and at flame retardance of polymer, press down the research in terms of cigarette attenuation and report less the most both at home and abroad.
2. the present invention combines nano combined with cooperative flame retardant, will have the metal oxide nano pressing down cigarette Attenuation
Granule and g-C3N4Combine formation functionalization g-C3N4, it is applied in polymer prepare fire proofing.
3. functionalization g-C3N4Nano composite material can play physical barrier effect, can reduce again polymer combustion speed
With poison gas burst size, in terms of two, improve the fire resistance of material.
4. the preparation technology that the present invention provides is simple, and raw material sources are extensive, have wide development in flame-retardant smoke inhibition field
Prospect.
Accompanying drawing explanation
Fig. 1 is the structure that the present invention has the metal oxide-loaded nano-particle of graphite phase carbon nitride of flame-retardant smoke inhibition function
Schematic diagram.
Fig. 2 is the chemical principle figure that the present invention is concrete.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described in detail, but the invention is not restricted to following enforcement
Example.
Number in following example, unless otherwise indicated, refers to parts by weight and percentage by weight.
Embodiment 1
(1) weigh carbamide and be positioned in the baking oven of 80 DEG C dry 8h, after being dried, carbamide is joined in crucible horse
Not 550 DEG C of calcining 5h in stove, prepare graphite phase carbon nitride g-C through supercooling, grinding afterwards3N4。
(2) by 0.2g g-C3N4It is dispersed in ultrasonic agitation 3h in 80mL distilled water, makes g-C3N4Dispersion is all in aqueous
Even.
(3) cobalt nitrate solution of 10mL 0.1mol/L is added dropwise to g-C3N4Dispersion liquid continues ultrasonic agitation 2h until mixing
Closing uniformly, instilling ammonia regulation pH value afterwards is 10.5.
(4) step (3) gained mixed solution is joined there-necked flask is warmed up in thermostatical oil bath 95 DEG C of stirrings
Backflow 8h, reaction is carrying out repeatedly centrifuge washing with water and ethanol after terminating respectively, centrifugal 10min under 8000r/min, until
Gained filtrate is neutral.
(5) being put into by step (4) products therefrom after being dried 8h in the baking oven of 80 DEG C, in Muffle furnace, 350 DEG C of calcining 2h are i.e.
Available Co3O4/g-C3N4Nano composite material.
What the present invention prepared has the knot of the metal oxide-loaded nano-particle of graphite phase carbon nitride of flame-retardant smoke inhibition function
Structure schematic diagram is as shown in Figure 1；As in figure 2 it is shown, wherein, R is metal ion to concrete chemical principle；M is 1,2 or 3.
Embodiment 2
(1) weigh tripolycyanamide and be positioned in the baking oven of 80 DEG C dry 10h, after being dried, tripolycyanamide is joined earthenware
In crucible in Muffle furnace 500 DEG C calcining 6h, afterwards through supercooling, grind prepare graphite phase carbon nitride g-C3N4。
(2) by 0.3g g-C3N4It is dispersed in ultrasonic agitation 5h in 120mL distilled water, makes g-C3N4Dispersion is all in aqueous
Even.
(3) cerous nitrate solution of 10mL 0.15mol/L is added dropwise to g-C3N4In dispersion liquid continue ultrasonic agitation 1h until
Mix homogeneously, instilling ammonia regulation pH value afterwards is 10.
(4) step (3) gained mixed solution is joined there-necked flask is warmed up in thermostatical oil bath 90 DEG C of stirrings
Backflow 10h, reaction carries out repeatedly centrifuge washing with water and ethanol after terminating respectively, centrifugal 20min under 6000r/min, until
Gained filtrate is neutral,
(5) being put into by step (4) products therefrom after being dried 8h in the baking oven of 70 DEG C, in Muffle furnace, 350 DEG C of calcining 3h are i.e.
Available CeO2/g-C3N4Nano composite material.
Embodiment 3
(1) weigh tripolycyanamide and be positioned in the baking oven of 70 DEG C dry 9h, after being dried, tripolycyanamide is joined earthenware
In crucible in Muffle furnace 600 DEG C calcining 4h, afterwards through supercooling, grind prepare graphite phase carbon nitride g-C3N4。
(2) by 0.3gg-C3N4It is dispersed in ultrasonic agitation 4h in 120mL distilled water, makes g-C3N4Dispersion is all in aqueous
Even.
(3) cerous nitrate of 5mL 0.1mol/L and the cobalt nitrate solution of 5mL 0.1mol/L are added dropwise to g-C3N4Dispersion liquid
Middle continuation ultrasonic agitation 1.5h is until mix homogeneously, and instilling ammonia regulation pH value afterwards is 10.
(4) step (3) gained mixed solution is joined there-necked flask is warmed up in thermostatical oil bath 95 DEG C of stirrings
Backflow 8h, reaction carries out repeatedly centrifuge washing with water and ethanol after terminating respectively, centrifugal 15min under 7000r/min, until institute
It is neutral for obtaining filtrate.
(5) being put into by step (4) products therefrom after being dried 6h in the baking oven of 90 DEG C, in Muffle furnace, 300 DEG C of calcining 3h are i.e.
Available Co3O4/CeO2/g-C3N4Nano composite material.
Embodiment 4
(1) weigh carbamide and be positioned in the baking oven of 60 DEG C dry 10h, after being dried, carbamide is joined in crucible horse
Not 500 DEG C of calcining 6h in stove, prepare graphite phase carbon nitride g-C through supercooling, grinding afterwards3N4。
(2) by 0.2g g-C3N4It is dispersed in ultrasonic agitation 4h in 80mL distilled water, makes g-C3N4Dispersion is all in aqueous
Even.
(3) ferric chloride solution of 20mL 0.05mol/L is added dropwise to g-C3N4In dispersion liquid continue ultrasonic agitation 2h until
Mix homogeneously, instilling ammonia regulation pH value afterwards is 11.
(4) step (3) gained mixed solution is joined there-necked flask is warmed up in thermostatical oil bath 100 DEG C of stirrings
Backflow 6h, reaction carries out repeatedly centrifuge washing with water and ethanol after terminating respectively, centrifugal 10min under 8000r/min, until institute
It is neutral for obtaining filtrate.
(5) step (4) products therefrom is put into and i.e. can get Fe after the baking oven of 70 DEG C is dried 8h2O3/g-C3N4Nanometer is multiple
Condensation material.
Embodiment 5
(1) weigh carbamide and be positioned in the baking oven of 80 DEG C dry 8h, after being dried, carbamide is joined in crucible horse
Not 550 DEG C of calcining 5h in stove, prepare graphite phase carbon nitride g-C through supercooling, grinding afterwards3N4。
(2) by 0.3g g-C3N4It is dispersed in ultrasonic agitation 5h in 120mL distilled water, makes g-C3N4Dispersion is all in aqueous
Even.
(3) iron chloride of 10mL 0.05mol/L and the cobalt chloride solution of 5mL 0.05mol/L are added dropwise to g-C3N4Dispersion
Continuing ultrasonic agitation 1.5h in liquid until mix homogeneously, instilling ammonia regulation pH value afterwards is 10.
(4) step (3) gained mixed solution is joined there-necked flask is warmed up in thermostatical oil bath 95 DEG C of stirrings
Backflow 8h, reaction carries out repeatedly centrifuge washing with water and ethanol after terminating respectively, centrifugal 10min under 8000r/min, until institute
It is neutral for obtaining filtrate.
(5) step (4) products therefrom is put into and i.e. can get CoFeO after the baking oven of 80 DEG C is dried 7h4/g-C3N4Nanometer
Composite.
Embodiment 6
In order to investigate the g-C of the present invention3N4Metal oxide-loaded nano-particle flame-retardant smoke inhibition in the polymeric material is made
With, a kind of conventional inflammable polymeric material polyurethane elastomer (TPU) of the present embodiment selection is as matrix, by embodiment
The fire retardant formula as below (being shown in Table 1) that 1-5 prepares joins in TPU resin, adds double screw extruder after mix homogeneously
In unit temperature 200 DEG C, die head temperature 185 DEG C, screw speed 230rpm, extruding pelletization, drying, cooling, obtain fire-retardant
TPU.Obtain standard specimen by hot-forming and machine cuts, these standard specimens are carried out fire resistance (taper calorimetric
Analysis reference standard: ISO 5660-1；Smoke density analyzes reference standard: ISO 5659-2 (2006)；UL94 reference standard: ASTM
D3801-10；LOI reference standard: ASTMD2863-06A), its test result is shown in Table 1.
Table 1
As can be seen from the above embodiments, the present invention combines nano combined with cooperative flame retardant, it is provided that one has
The preparation method of the metal oxide-loaded nano-particle of graphite phase carbon nitride of flame-retardant smoke inhibition function, and it is poly-to be applied to PS etc.
Compound finds its preferable flame-retardant smoke inhibition effect.The preparation technology that the present invention provides is simple, and raw material sources are extensive, press down fire-retardant
Cigarette field has vast potential for future development.
Above the present invention is described in detail, its object is to allow the personage being familiar with this art will appreciate that this
Invention content and be carried out, can not limit the scope of the invention with this, all spirit institutes according to the present invention
The equivalence change made or modification, all should contain within the scope of the present invention.
Claims (10)
1. having a preparation method for the metal oxide-loaded nano-particle of graphite phase carbon nitride of flame-retardant smoke inhibition function, it is special
Levying and be, described method prepares g-C for raw material by high temperature pyrolytic cracking (HTP) with carbamide or tripolycyanamide3N4；Then metal oxygen is selected
Compound presoma, uses co-precipitation, Hydrothermal Synthesis or high temperature sintering methods by metal oxide supported in g-C3N4On lamella, system
For going out a kind of metal oxide-loaded nano-particle of graphite phase carbon nitride with flame-retardant smoke inhibition function, concrete preparation process is such as
Under:
(1) it is firstly placed to tripolycyanamide or carbamide in baking oven dry, is subsequently adding in crucible and calcines in Muffle furnace, afterwards
Through supercooling, grind and prepare graphite phase carbon nitride g-C3N4；
(2) by the g-C of preparation in step (1)3N4It is dispersed in ultrasonic agitation in distilled water, makes g-C3N4Water is uniformly dispersed；
(3) configuration metal salt solution, is added dropwise in the dispersion liquid of step (2) gained to continue ultrasonic agitation until mix homogeneously, it
Rear instillation ammonia regulation pH is 10 ~ 11；
(4) being joined in there-necked flask by step (3) gained mixed solution and be stirred at reflux in thermostatical oil bath, reaction terminates
After carry out repeatedly centrifuge washing until gained filtrate for neutrality；
(5) step (4) products therefrom is put into after baking oven is dried, calcine in Muffle furnace and i.e. can obtain that there is flame-retardant smoke inhibition
The metal oxide-loaded nano-particle of graphite phase carbon nitride of function.
A kind of metal oxide-loaded nanometer of graphite phase carbon nitride with flame-retardant smoke inhibition function the most according to claim 1
The preparation method of granule, it is characterised in that: in step (1), the temperature of described baking oven is 60 ~ 80 ° of C, and drying time is 8 ~ 10
h；The temperature of described calcining is 500 ~ 600 ° of C, and the time of calcining is 4 ~ 6 h.
A kind of metal oxide-loaded nanometer of graphite phase carbon nitride with flame-retardant smoke inhibition function the most according to claim 1
The preparation method of granule, it is characterised in that: in step (2), the described ultrasonic time is 3 ~ 5 h；In step (3), described ultrasonic
Time be 1 ~ 2 h.
A kind of metal oxide-loaded nanometer of graphite phase carbon nitride with flame-retardant smoke inhibition function the most according to claim 1
The preparation method of granule, it is characterised in that: in step (3), the slaine in described metal salt solution is transition metal salt and dilute
One or more in earth metal salt；The concentration of described metal salt solution is 0.05 ~ 0.15 mol/L.
A kind of metal oxide-loaded nanometer of graphite phase carbon nitride with flame-retardant smoke inhibition function the most according to claim 4
The preparation method of granule, it is characterised in that: described transition metal salt is one or more in cobalt salt, iron salt and mantoquita；Described
Rare earth metal salt is cerium salt.
A kind of metal oxide-loaded nanometer of graphite phase carbon nitride with flame-retardant smoke inhibition function the most according to claim 1
The preparation method of granule, it is characterised in that: in step (4), the temperature of described reaction is 90 ~ 100 ° of C, the time of reaction is 6 ~
10 h。
A kind of metal oxide-loaded nanometer of graphite phase carbon nitride with flame-retardant smoke inhibition function the most according to claim 1
The preparation method of granule, it is characterised in that: in step (4), described centrifugal rotating speed is 6000 ~ 8000 r/min, time centrifugal
Between be 10 ~ 20 min；Described washing is repeatedly to wash with water and ethanol successively.
A kind of metal oxide-loaded nanometer of graphite phase carbon nitride with flame-retardant smoke inhibition function the most according to claim 1
The preparation method of granule, it is characterised in that: in step (5), the temperature of described baking oven is 70 ~ 90 ° of C, and the dry time is 6 ~ 8
h；The temperature of described calcining is 250 ~ 350 ° of C, and the time of calcining is 2 ~ 4 h.
9. a kind of graphite-phase nitridation with flame-retardant smoke inhibition function prepared by the preparation method described in any one of claim 1-8
The metal oxide-loaded nano-particle of carbon, it is characterised in that: this has the graphite phase carbon nitride carried metal of flame-retardant smoke inhibition function
Oxide nano particles is with a class two-dimensional nanoparticle g-C3N4As supporting carrier, nano-metal-oxide deposition is dispersed in
g-C3N4Surface.
10. a kind of metal oxide-loaded nanometer of graphite phase carbon nitride with flame-retardant smoke inhibition function described in claim 9
Grain application in flame-proofed polymer material.
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