CN106117606A - Red copper oxide hydridization Graphene anti-flaming smoke-inhibiting agent and preparation method thereof - Google Patents
Red copper oxide hydridization Graphene anti-flaming smoke-inhibiting agent and preparation method thereof Download PDFInfo
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- CN106117606A CN106117606A CN201610422678.8A CN201610422678A CN106117606A CN 106117606 A CN106117606 A CN 106117606A CN 201610422678 A CN201610422678 A CN 201610422678A CN 106117606 A CN106117606 A CN 106117606A
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- inhibiting agent
- copper oxide
- flaming smoke
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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
- 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
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Abstract
The invention discloses a kind of Red copper oxide hydridization Graphene anti-flaming smoke-inhibiting agent, its preparation process is as follows: be a) 0.5 1.5mg/ml mixing by graphene oxide and deionized water by graphene oxide concentration, and ultrasonic disperse obtains graphene oxide suspension;B) in graphene oxide suspension, cupric salt stirring and dissolving is added by the concentration of 0.02 0.1M, supersound process 5 15min, then it is sequentially added into precipitant and reducing agent is stirred obtaining mixture, mixture is processed by a step coprecipitation, obtains Red copper oxide hydridization Graphene anti-flaming smoke-inhibiting agent.Red copper oxide hydridization Graphene anti-flaming smoke-inhibiting agent disclosed by the invention is to integrate physical barrier effect and the catalysis carbon-forming of Red copper oxide of graphene sheet layer and press down cigarette effect, it is prepared raw material and is easy to get, preparation method is simple, low cost, environmental protection, and be applied in polymeric material to be effectively improved the flame retarding and smoke suppressing properties of polymer and mechanics mechanical performance.
Description
Technical field
The present invention relates to anti-flaming smoke-inhibiting agent technical field, be specifically related to a kind of Red copper oxide hydridization Graphene anti-flaming smoke-inhibiting agent
And preparation method thereof.
Background technology
Since 21 century, along with developing rapidly of national economy, organic polymer material in people's daily life and
The medium every field of the development of the national economy is all widely used, and organic polymer material is to the development of the life of the mankind with society
All bring huge facility.But, most of organic polymer material is all readily ignited and deflagrate, and produces
Substantial amounts of calory burning and toxic gas, also bring huge threat to the most undoubtedly human lives, therefore improves organic poly-
The combustibility of laminate material is increasingly paid attention to by researcher.
Graphene (GNS) is a kind of bi-dimensional cellular shape planar structure tightly packed by monolayer carbon atom, and it has
Bigger surface area and excellent electricity, optics, mechanics and thermal property, therefore suffered from the extensive of various fields researcher
Pay close attention to.At present, Graphene is at the energy and electronic equipment, chemical sensor, pharmaceutical carrier, catalyst and transparent conductive material etc.
Field is widely used, and it has been investigated that, it has huge in terms of improving the fire resistance of polymer equally
Potentiality.Concrete, [Gavgani J N, Adelnia H, the Gudarzi M M.Intumescent flame such as Gavgani
retardant polyurethane/reduced graphene oxide composites with improved
mechanical,thermal,and barrier properties.Journal of Materials Chemistry,
2014,49:243-254] Graphene is added in the polyurethane containing expanding fire retardant, to study Graphene to this polyurethane
The impact of fire resistance, result shows: add 2wt% Graphene and the limited oxygen index value of this polyurethane not only can be made by 29.0%
Rise to 34.0%, and the molten drop of this polyurethane can be suppressed;[Hu J, the Zhang F.Self-assembled such as Hu
fabrication and flame-retardant properties of reduced graphene oxide/
waterborne polyurethane nanocomposites.Journal of Thermal Analysis and
Calorimetry, 2014,118:1561-1568] have studied Graphene to aqueous polyurethane (being called for short WPU) heat stability and resistance
The impact of combustion performance, result shows: add 2wt% Graphene and the carbon yield of WPU can be made to be obviously improved, hence it is evident that reduce WPU
HRR and total heat release;Song etc. [Song P A, Yu Y M, Zhang T, et al.Permeability,
viscoelasticity,and flammability performances and their relationship to
polymer nanocomposites.Industrial&Engineering Chemistry Research,2012,51:
7255-7263] show after deliberation, the PP composite adding 1wt% Graphene can form effective three-dimensional net structure, pole
Reduce greatly the HRR of material;[Liu S, Yan H Y, Fang Z P, the et al.Effect of such as Liu
graphene nanosheets on morphology,thermal stability and flame retardancy of
Epoxy resin.Composites Science and Technology, 2014,90:40-47] research find Graphene receive
Rice sheet (guide number S) can give the anti-flammability that epoxy resin is excellent, add the GNS of 5wt% can make the LOI value of epoxy resin from
15.7% increases to 21.4%, and total heat release can be from 33.4kJ/m2It is reduced to 27.8kJ/m2.It practice, Graphene
The graphene sheet layer mainly due to bigger serface that promotes of composite polymeric materials fire resistance can be effective as one
Physical barriers, thus the energy between gas phase and condensed phase and the transmission of material during suppressing polymer combustion.
But, owing to there is stronger Van der Waals force between graphene sheet layer, therefore Graphene is in preparation dry run
Easily being packed together between its lamella, when causing Graphene to be used alone, its flame retarding efficiency is poor, therefore can not suppress well
The burning of polymer.Additionally, the experimental results shows, Graphene is more weak to the smoke suppressing of polymer, it is impossible to effectively suppress
The release of cigarette, it is therefore necessary to Graphene is carried out surface modification to improve its flame retarding efficiency in polymeric matrix and to press down cigarette
Performance.
Red copper oxide (Cu2O) as tradition smoke suppressant, by reduction coupling mechanism, it can promote that polymer is burned
Journey is formed more layer of charcoal, the smoke suppressing improving polymer is had the highest efficiency.And as a kind of two-dimension single layer material,
Graphene is the ideal carrier that metal-oxide is applied to catalytic field, therefore, studies Red copper oxide-graphene hybrid material,
This is significant to the flame retarding and smoke suppressing properties improving polymer.
Summary of the invention
The primary and foremost purpose of the present invention is to provide a kind of Red copper oxide hydridization Graphene anti-flaming smoke-inhibiting agent, and this anti-flaming smoke-inhibiting agent is not
It is only capable of the flame retarding and smoke suppressing properties improving polymer, the mechanics mechanical performance of polymer can also be effectively improved simultaneously.
For achieving the above object, the technical solution used in the present invention is: a kind of Red copper oxide hydridization Graphene flame-retardant smoke inhibition
Agent, it is to be dispersed on graphenic surface by covalent bond active force by Red copper oxide to obtain.
Another object of the present invention is to provide a kind of Red copper oxide hydridization Graphene anti-flaming smoke-inhibiting agent as above
Preparation method, its step is as follows:
A) it is 0.5-1.5mg/ml mixing by graphene oxide and deionized water by graphene oxide concentration, ultrasonic disperse,
Obtain graphene oxide suspension;
B) concentration pressing 0.02-0.1M adds cupric salt stirring and dissolving, supersound process in graphene oxide suspension
5-15min, is then sequentially added into precipitant and reducing agent is stirred obtaining mixture, by mixture by a step coprecipitation
Reason, obtains Red copper oxide hydridization Graphene anti-flaming smoke-inhibiting agent, and described precipitant is sodium hydroxide or potassium hydroxide, and reducing agent is
Hydrazine hydrate or ascorbic acid, Cu in described mixture2+, the mol ratio of precipitant and reducing agent be 1:2-3:0.5-1.5.Wherein walk
In rapid a, so-called is 0.5-1.5mg/ml mixing by graphene oxide and deionized water by graphene oxide concentration, say, that
Graphene oxide and deionized water are mixed, and guarantees that graphene oxide concentration therein is 0.5-1.5mg/ml;Additionally step b
In, in graphene oxide suspension, add cupric salt by the concentration of 0.02-0.1M, say, that suspend to graphene oxide
Adding cupric salt in liquid makes the concentration of wherein cupric salt between 0.02-0.1M.
Use having the beneficial effects that of technique scheme generation: compared with original metal-oxide, Graphene and gold
Belong to oxide hybridized material and demonstrate higher catalysis activity, the most metal oxide-loaded after, hold between graphene sheet layer
The problem easily piled up can be effectively suppressed.It is to say, Red copper oxide hydridization Graphene flame-retardant smoke inhibition disclosed by the invention
Agent is to integrate physical barrier effect and the catalysis carbon-forming of Red copper oxide of graphene sheet layer and press down cigarette effect, and it prepares raw material
Being easy to get, preparation method is simple, low cost, environmental protection.
Specifically, the present invention be utilize ultrasonic dispersion by dispersed for graphene oxide in deionized water, then
Add supersound process after cupric salt, make bivalent cupric ion be supported on graphenic surface, the most again by covalent bond active force
It is sequentially added into precipitant and reducing agent, prepares Red copper oxide load graphene hybrid material by coprecipitation, use this
The Red copper oxide hydridization Graphene anti-flaming smoke-inhibiting agent even particle size distribution of nano-scale prepared by bright disclosed method, it is possible to poly-
Being uniformly dispersed in compound matrix, and environmental protection, it is improving while flame retardance of polymer presses down cigarette, additionally it is possible to improve polymerization
The mechanics mechanical performance of thing.It should be noted that graphene oxide used in step a can the most commercially obtain
Arriving, or can also natural graphite powder be raw material, the Hummers method oxidation of employing prepares.
As further preferred version, in described step a, the time of ultrasonic disperse is 0.5-1.5h;In described step b
Cupric salt be copper sulphate pentahydrate or nitrate trihydrate copper.
It addition, concrete scheme is, the step that the mixture one step coprecipitation in described step b processes is: will mixing
Thing is placed in 25-65 DEG C, stirring reaction 0.5-2h under conditions of 60-100rpm, is then centrifuged for, deionized water wash, at 60-80 DEG C
Lower vacuum drying, it is, of course, preferable to be product is repeatedly centrifuged, carrying out washing treatment.Preferably, described step b adds
First stir 0.5-1h after precipitant, then add reducing agent.
Detailed description of the invention
Below by way of 3 embodiments, technical scheme disclosed by the invention is described further:
Embodiment 1: the preparation of anti-flaming smoke-inhibiting agent and performance test
One, the preparation of anti-flaming smoke-inhibiting agent
A) weigh the graphene oxide that 50mg is prepared by Hummers method, join in 100ml deionized water, ultrasonic point
Dissipate 1h, obtain graphene oxide suspension;
B) in graphene oxide suspension, 1.25g copper sulphate pentahydrate stirring and dissolving is added, supersound process 5min, then first
Add 0.4g sodium hydroxide stirring 1h and obtain uniform dispersion, add 0.88g ascorbic acid, 35 DEG C, stir under conditions of 60rpm
After mixing reaction 1h, product is centrifuged, deionized water wash, vacuum drying, obtains the resistance of Red copper oxide hydridization Graphene
Combustion smoke suppressant.
Two, the performance test of fire retardant
1, prepared by sample: the Red copper oxide hydridization Graphene anti-flaming smoke-inhibiting agent this embodiment prepared is by mass fraction
The addition of 2wt% joins in polyurethane elastomer, then mixing 6min, discharging in the mixing instrument of 180 DEG C, delivers to flat board
Produced as sheets sample on vulcanizer.
2, fire resistance test: test is carried out according to ISO5600-1:2002 standard, and sample standard size is 100 × 100
×3mm3, after testing, the maximum heat rate of release of this sample is 425, and compared with pure polyurethane elastomer, its maximum heat discharges
Speed have dropped 54.8%, illustrates that this anti-flaming smoke-inhibiting agent has the fire resistance of excellence.
3, smoke suppressing test: test is carried out according to ISO5659-2 standard, sample standard size is 75 × 75 ×
2.5mm3, after testing, radiant illumination 25kW/m of this sample2, maximum smoke density is 265, compared with pure polyurethane elastomer,
Its maximum smoke density have dropped 35.5%, illustrates that this anti-flaming smoke-inhibiting agent has the smoke suppressing of excellence.
4, Mechanics Performance Testing: test is carried out according to ISO8256-2004 standard, and after testing, the rate of extension of this sample is
300mm/min, tensile strength 35.8MPa, elongation at break is 498%, illustrates that this anti-flaming smoke-inhibiting agent can improve polymer
Mechanical property.
Embodiment 2: the preparation of anti-flaming smoke-inhibiting agent and performance test
One, the preparation of anti-flaming smoke-inhibiting agent
A) weigh the graphene oxide that 150mg is prepared by Hummers method, join in 100ml deionized water, ultrasonic point
Dissipate 1.5h, obtain graphene oxide suspension;
B) in graphene oxide suspension, 0.48g copper sulphate pentahydrate stirring and dissolving is added, supersound process 15min, then
It is initially charged 0.2g sodium hydroxide stirring 0.5h and obtains uniform dispersion, add 0.70g ascorbic acid, at 65 DEG C, the bar of 100rpm
Under part after stirring reaction 0.5h, product is centrifuged, deionized water wash, vacuum drying, obtains Red copper oxide hydridization
Graphene anti-flaming smoke-inhibiting agent.
Two, the performance test of fire retardant
1, prepared by sample: the Red copper oxide hydridization Graphene anti-flaming smoke-inhibiting agent this embodiment prepared is by mass fraction
The addition of 2wt% joins in ethylene-vinyl acetate copolymer, temperature be set 120 DEG C, rotating speed is as the stream of 40r/min
Become and instrument mixes 10min, discharging, deliver to produced as sheets sample on vulcanizing press.
2, fire resistance test: test is carried out according to ISO5600-1:2002 standard, and sample standard size is 100 × 100
×3mm3, after testing, the maximum heat rate of release of this sample is 389, and compared with pure polyurethane elastomer, its maximum heat discharges
Speed have dropped 58.2%, illustrates that this anti-flaming smoke-inhibiting agent has the fire resistance of excellence.
3, smoke suppressing test: test is carried out according to ISO5659-2 standard, sample standard size is 75 × 75 ×
2.5mm3, after testing, radiant illumination 25kW/m of this sample2, maximum smoke density is 234, compared with pure polyurethane elastomer,
Its maximum smoke density have dropped 20.2%, illustrates that this anti-flaming smoke-inhibiting agent has the smoke suppressing of excellence.
4, Mechanics Performance Testing: test is carried out according to ISO8256-2004 standard, and after testing, the rate of extension of this sample is
300mm/min, tensile strength 16.4MPa, elongation at break is 885%, illustrates that this anti-flaming smoke-inhibiting agent can improve polymer
Mechanical property.
Embodiment 3: the preparation of anti-flaming smoke-inhibiting agent and performance test
One, the preparation of anti-flaming smoke-inhibiting agent
A) weigh the graphene oxide that 100mg is prepared by Hummers method, join in 100ml deionized water, ultrasonic point
Dissipate 0.5h, obtain graphene oxide suspension;
B) in graphene oxide suspension, 2.5g copper sulphate pentahydrate stirring and dissolving is added, supersound process 8min, then first
Add 1.68g potassium hydroxide stirring 45min and obtain uniform dispersion, add 0.25g hydrazine hydrate, 25 DEG C, under conditions of 80rpm
After stirring reaction 2h, product is centrifuged, deionized water wash, vacuum drying, obtains Red copper oxide hydridization Graphene
Anti-flaming smoke-inhibiting agent.
Two, the performance test of fire retardant
1, prepared by sample: the Red copper oxide hydridization Graphene anti-flaming smoke-inhibiting agent this embodiment prepared is by mass fraction
The addition of 2wt% joins in polyurethane elastomer, and then mixing 6min in the mixing instrument of 180 DEG C, delivers to compression molding
Produced as sheets sample on machine.
2, fire resistance test: test is carried out according to ISO5600-1:2002 standard, and sample standard size is 100 × 100
×3mm3, after testing, the maximum heat rate of release of this sample is 789, and compared with pure polyurethane elastomer, its maximum heat discharges
Speed have dropped 46.7%, illustrates that this anti-flaming smoke-inhibiting agent has the fire resistance of excellence.
3, smoke suppressing test: test is carried out according to ISO5659-2 standard, sample standard size is 75 × 75 ×
2.5mm3, after testing, radiant illumination 25kW/m of this sample2, maximum smoke density is 214, compared with pure polyurethane elastomer,
Its maximum smoke density have dropped 37.6%, illustrates that this anti-flaming smoke-inhibiting agent has the smoke suppressing of excellence.
4, Mechanics Performance Testing: test is carried out according to ISO8256-2004 standard, and after testing, the rate of extension of this sample is
300mm/min, tensile strength 34.9MPa, elongation at break is 500%, illustrates that this anti-flaming smoke-inhibiting agent can improve polymer
Mechanical property.
Claims (6)
1. a Red copper oxide hydridization Graphene anti-flaming smoke-inhibiting agent, it is dispersed by covalent bond active force by Red copper oxide
Graphenic surface obtains.
2. a preparation method for Red copper oxide hydridization Graphene anti-flaming smoke-inhibiting agent as claimed in claim 1, its step is as follows:
A) it is 0.5-1.5mg/ml mixing by graphene oxide and deionized water by graphene oxide concentration, ultrasonic disperse, obtain
Graphene oxide suspension;
B) concentration pressing 0.02-0.1M adds cupric salt stirring and dissolving, supersound process 5-in graphene oxide suspension
15min, is then sequentially added into precipitant and reducing agent obtains mixture, is processed by a step coprecipitation by mixture, obtains oxygen
Changing cuprous hydridization Graphene anti-flaming smoke-inhibiting agent, described precipitant is sodium hydroxide or potassium hydroxide, reducing agent be hydrazine hydrate or
Ascorbic acid, Cu in described mixture2+, the mol ratio of precipitant and reducing agent be 1:2-3:0.5-1.5.
The preparation method of Red copper oxide hydridization Graphene anti-flaming smoke-inhibiting agent the most according to claim 2, it is characterised in that: described
In step a, the time of ultrasonic disperse is 0.5-1.5h.
The preparation method of Red copper oxide hydridization Graphene anti-flaming smoke-inhibiting agent the most according to claim 3, it is characterised in that: described
Cupric salt in step b is copper sulphate pentahydrate or nitrate trihydrate copper.
The preparation method of Red copper oxide hydridization Graphene anti-flaming smoke-inhibiting agent the most according to claim 4, it is characterised in that: described
The step that mixture one step coprecipitation in step b processes is: mixture is placed in 25-65 DEG C, under conditions of 60-100rpm
Stirring reaction 0.5-2h, is then centrifuged for, deionized water wash, is vacuum dried at 60-80 DEG C.
The preparation method of Red copper oxide hydridization Graphene anti-flaming smoke-inhibiting agent the most according to claim 5, it is characterised in that: described
First stir 0.5-1h after step b adds precipitant, then add reducing agent.
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Cited By (3)
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CN106995544A (en) * | 2017-03-30 | 2017-08-01 | 浙江大学宁波理工学院 | Polythene material containing Metal Supported fullerene and preparation method thereof |
CN111551621A (en) * | 2020-05-21 | 2020-08-18 | 天津理工大学 | Electrochemical sensor for detecting ascorbic acid and preparation method and application thereof |
CN113845695A (en) * | 2021-10-12 | 2021-12-28 | 南京工业大学 | Ternary nano composite flame retardant, flame-retardant epoxy resin and preparation method thereof |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106995544A (en) * | 2017-03-30 | 2017-08-01 | 浙江大学宁波理工学院 | Polythene material containing Metal Supported fullerene and preparation method thereof |
CN111551621A (en) * | 2020-05-21 | 2020-08-18 | 天津理工大学 | Electrochemical sensor for detecting ascorbic acid and preparation method and application thereof |
CN113845695A (en) * | 2021-10-12 | 2021-12-28 | 南京工业大学 | Ternary nano composite flame retardant, flame-retardant epoxy resin and preparation method thereof |
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