CN106752116A - The preparation method and modified graphene oxide EPS of modified graphene oxide mold the preparation method of styrofoam - Google Patents
The preparation method and modified graphene oxide EPS of modified graphene oxide mold the preparation method of styrofoam Download PDFInfo
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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Abstract
The invention belongs to Graphene synthesis technical field, it is related to a kind of preparation method of modified graphene oxide and modified graphene oxide EPS to mold the preparation method of styrofoam, specially：The pre-dispersed rear modified dispersion for adding modifying agent, dispersant and dispersion aids to carry out graphene oxide in deionized water by graphene oxide, activator and stabilizer, add alkali and adjust pH value, then be modified the grinding of graphene oxide, terminate rear ultrasound filtration it is dry modified graphene powder；Modified graphene carries out suspension polymerisation in being added to white material EPS.The preparation of modified graphene oxide of the present invention material based on graphene oxide, aims at EPS applications and develops.Emphasis of the present invention is modified graphene oxide, and modified graphene EPS molding styrofoam strength ratio national standards improve 160% 200%, 032 grade of national standard reduction of thermal conductivity ratio 9% 13%, with more excellent comprehensive mechanical property.The method process is simple that the present invention is provided, low cost, it is easy to the industrialized production of modified graphene.
Description
Technical field
The invention belongs to Graphene synthesis technical field, it is related to a kind of preparation method of modified graphene oxide and modified oxygen
Graphite alkene EPS molds the preparation method of styrofoam.
Background technology
Graphene is a kind of two dimensional crystal material tightly packed by carbon atom, excellent because of its unique structure
Electricity, mechanics, optics, chemistry and thermal property turn into the focus of scientific research personnel's research.The preparation method of Graphene has a lot, mesh
Before possess industrialized production only oxidation-reduction method, it has production efficiency high, technological process, the advantage of scale.
The method is, by native graphite and strong acid Strong oxdiative thing reaction generation graphite oxide, oxidation to be processed into by ultrasound or microwave bulking
Graphene, then the oxygen-containing functional group of reduction removal surface of graphene oxide is carried out, obtain Graphene.Due to graphite oxide or oxidation
Graphenic surface group is numerous, is suitably modified and can be widely applied to other industries.
Expandable polystyrene (EPS) is used as building heat preservation heat-barrier material because of its excellent heat insulation property, and with every
The quantity of year few hundred thousand tonnes of is applied to commodity packaging.At present, the EPS products of in the market are divided into white material EPS and two kinds of graphite EPS.
Standard GB/T/T 29906-2013《Molding exterior insulation system for polyphenyl plate thin plastering exterior wall material》Middle EPS moldings styrofoam resists
Tensile strength >=0.1Mpa, 039 grade of thermal conductivity factor≤0.039W/ (mK), 032 grade of thermal conductivity factor≤0.032W/ (mK), its
In, white material EPS thermal conductivity factors are 039 grade, and graphite EPS thermal conductivity factors are 032 grade.Research finds that Graphene is not modified directly
It is added to polymerization in EPS systems, is easily caused inhibition effect and knot kettle phenomenon even occur, EPS particles is polymerize reluctantly, it is foamed to beat
Plate surveys performance, though though tensile strength can improve 5%-20% than national standard 0.1Mpa, and thermal conductivity factor is substantially without substantially reduction.
As the continuous improvement of national building energy conservation professional standard is, it is necessary to develop that thermal conductivity factor is lower, the more preferable EPS of heat-insulating property is produced
Product.Meanwhile, it is also problem demanding prompt solution that the mechanical strength of EPS products is too low.
The content of the invention
The purpose of the present invention is directed to above-mentioned the deficiencies in the prior art, there is provided a kind of preparation side of modified graphene oxide
Method.It is a further object of the present invention to provide the preparation method that modified graphene oxide EPS molds styrofoam.
The purpose of the present invention is achieved through the following technical solutions：
A kind of preparation method of modified graphene oxide, comprises the following steps：
A, graphene oxide, activator and stabilizer are carried out pre-dispersed, wherein activator and stabilization in deionized water
Agent is respectively 2-6wt% and 2-8wt% with the percentage by weight of graphene oxide；
B, it is subsequently adding coupling agent, dispersant and dispersion aids and carries out the modified dispersion of graphene oxide, adds alkali tune
The weight of graphene oxide modification liquid, the coupling agent, dispersant and dispersion aids and graphene oxide is obtained to neutrality for section pH value
Amount percentage is respectively 1-5wt%, 5-10wt% and 0.1-0.5wt%；
C, the number of plies that above-mentioned graphene oxide modification liquid is ground to modified graphene oxide<10 layers, particle diameter：D50 is 5-
10um, D90 are 10-20um；
After D, modified end, carry out ultrasound filtration, dry prepared modified graphene powder.
The graphene oxide is prepared in accordance with the following methods：In concentrated sulfuric acid system, to adding permanganic acid in native graphite
Potassium, sodium nitrate add potassium permanganate, hydrogen peroxide for strong oxidizer reaction prepares graphite oxide, and reusable heat plavini will aoxidize stone
Ink in 1000 DEG C or so of high-temperature heat treatment, then using the continuous impact peel graphite oxide of ultrasonic wave.
The graphene oxide can also be prepared in accordance with the following methods：Under concentrated nitric acid, concentrated sulfuric acid system, potassium chlorate is added
For oxidant reacts, prepare graphite oxide, reusable heat plavini by graphite oxide in 1000 DEG C or so of high-temperature heat treatment,
Then the continuous impact peel graphite oxide of ultrasonic wave is utilized.
The activator is sodium alkyl benzene sulfonate, molecular formula R-C6H4-SO3Na。
Preferably, the activator is neopelex, cetyl benzenesulfonic acid sodium, octadecyl benzenesulfonic acid sodium
In at least one.
The stabilizer be Tissuemat E, ethene-beta-unsaturated esters copolymer (EAA, EMAA, EEA, EMA, EMMA, EMAH),
At least one in ethylene-vinyl acetate copolymer (EVA).
The coupling agent is at least in silane coupler, titanate coupling agent, aluminate coupling agent, aluminum-zirconium coupling agent
Kind.
The dispersant is at least one in active calcium phosphate, activated Calcium carbonate.
The dispersion aids is at least one in methylcellulose (MC), carboxymethylcellulose calcium (CMC).
A kind of modified graphene oxide EPS molds the preparation method of styrofoam, comprises the following steps：The above method is obtained
Modified graphene be added to white material EPS systems in carry out suspension polymerisation, then the prepared expandable polystyrene molding that re-packs that foams
Styrofoam；The white material EPS systems include pure water, styrene, initiator B PO, dispersant active calcium phosphate and foaming agent pentane；
In polymerization system, pure water is 1-4 with the weight ratio of styrene:1, modified graphene, BPO, active calcium phosphate, pentane and styrene
Percentage by weight be respectively 0.5%wt, 0.2-0.5wt%, 0.5-1wt% and 7-10wt%, polymerization time is 10-12h.
Compared with prior art, the beneficial effects of the present invention are：The preparation method of modified graphene of the present invention is reliable, raw
Produce low cost, production efficiency high, be adapted to industrialized production；The present invention solves that Graphene is not modified to be directly appended to EPS
Polymerization-filling can cause to inhibit and tie the problem of kettle, and gained modified graphene EPS molding styrofoam strength ratio national standards are improved
160-200%, 032 grade of national standard reduction 9%-13% of thermal conductivity ratio, can be widely applied to the neck such as packaging, building energy conservation
Domain, and had broad application prospects in fields such as road construction, anti-collision system for automobile.
Brief description of the drawings
Fig. 1 is that modified graphene oxide of the present invention is added to EPS foaming and re-packs the styrofoam that is made and standard GB/T/T
The tensile strength comparison diagram of 29906-2013；
Fig. 2 is that modified graphene oxide of the present invention is added to EPS foaming and re-packs the styrofoam that is made and standard GB/T/T
The thermal conductivity factor comparison diagram of 29906-2013.
Specific embodiment
The present invention will be further described with reference to the embodiment in accompanying drawing below：
A kind of preparation method of modified graphene oxide, comprises the following steps：
A, graphene oxide, activator and stabilizer are carried out pre-dispersed, wherein activator and stabilization in deionized water
Agent is respectively 2-6wt% and 2-8wt% with the percentage by weight of graphene oxide；
B, it is subsequently adding coupling agent, dispersant and dispersion aids and carries out the modified dispersion of graphene oxide, adds alkali tune
The weight of graphene oxide modification liquid, the coupling agent, dispersant and dispersion aids and graphene oxide is obtained to neutrality for section pH value
Amount percentage is respectively 1-5wt%, 5-10wt% and 0.1-0.5wt%；
C, the number of plies that above-mentioned graphene oxide modification liquid is ground to modified graphene oxide<10 layers, particle diameter：D50 is 5-
10um, D90 are 10-20um；
After D, modified end, carry out ultrasound filtration, dry prepared modified graphene powder.
The graphene oxide is prepared in accordance with the following methods：In concentrated sulfuric acid system, to adding permanganic acid in native graphite
Potassium, sodium nitrate add potassium permanganate, hydrogen peroxide for strong oxidizer reaction prepares graphite oxide, and reusable heat plavini will aoxidize stone
Ink in 1000 DEG C or so of high-temperature heat treatment, then using the continuous impact peel graphite oxide of ultrasonic wave.
The graphene oxide can also be prepared in accordance with the following methods：Under concentrated nitric acid, concentrated sulfuric acid system, potassium chlorate is added
For oxidant reacts, prepare graphite oxide, reusable heat plavini by graphite oxide in 1000 DEG C or so of high-temperature heat treatment,
Then the continuous impact peel graphite oxide of ultrasonic wave is utilized.
The activator is sodium alkyl benzene sulfonate, molecular formula R-C6H4-SO3Na。
Preferably, the activator is neopelex, cetyl benzenesulfonic acid sodium, octadecyl benzenesulfonic acid sodium
In at least one.
The stabilizer be Tissuemat E, ethene-beta-unsaturated esters copolymer (EAA, EMAA, EEA, EMA, EMMA, EMAH),
At least one in ethylene-vinyl acetate copolymer (EVA).
The coupling agent is at least in silane coupler, titanate coupling agent, aluminate coupling agent, aluminum-zirconium coupling agent
Kind.
The dispersant is at least one in active calcium phosphate, activated Calcium carbonate.
The dispersion aids is at least one in methylcellulose (MC), carboxymethylcellulose calcium (CMC).
A kind of modified graphene oxide EPS molds the preparation method of styrofoam, comprises the following steps：The above method is obtained
Modified graphene be added to white material EPS systems in carry out suspension polymerisation, then the prepared expandable polystyrene molding that re-packs that foams
Styrofoam；The white material EPS systems include pure water, styrene, initiator B PO, dispersant active calcium phosphate and foaming agent pentane；
In polymerization system, pure water is 1-4 with the weight ratio of styrene:1, modified graphene, BPO, active calcium phosphate, pentane and styrene
Percentage by weight be respectively 0.5%wt, 0.2-0.5wt%, 0.5-1wt% and 7-10wt%, polymerization time is 10~12h.
Embodiment 1
A kind of preparation method of modified graphene oxide, comprises the following steps：
A, 50g graphene oxide powders, 1g neopelexes, 4g Tissuemat Es are carried out in deionized water it is pre-
Dispersion；
B, it is subsequently adding 0.5g Silane coupling agent KH550s, 5g active calcium phosphates, 0.18g MC and completes graphene oxide and change
Property dispersion, stirring shearing dispersion 1h adds NaOH and adjusts pH value to neutrality；
C, by above-mentioned graphene oxide modification liquid be ground to D50 be 10um, D90 is 20um；
D, it is modified terminate after, carry out ultrasound filtration it is dry modified graphene powder.
Embodiment 2
A kind of preparation method of modified graphene oxide, comprises the following steps：
A, by 50g graphene oxide powders, 1.5g cetyl benzenesulfonic acid sodiums, 2g EAA, 1g EMAA in deionized water
Carry out pre-dispersed；
B, it is subsequently adding modified point that 1g aluminum-zirconium coupling agents, 4g activated Calcium carbonates, 0.25g CMC complete graphene oxide
Dissipate, stirring shearing dispersion 1h adds potassium hydroxide and adjusts pH value to neutrality；
C, by above-mentioned graphene oxide modification liquid be ground to D50 be 8um, D90 is 17um；
D, it is modified terminate after, carry out ultrasound filtration it is dry modified graphene powder.
Embodiment 3
A kind of preparation method of modified graphene oxide, comprises the following steps：
A, by 50g graphene oxide powders, 1g neopelexes, 1g octadecyl benzenesulfonic acids sodium, 1gEVA,
1gEMAH carries out pre-dispersed in deionized water；
B, be subsequently adding 1.2g aluminate coupling agent DL-411,0.5g titanate coupling agent 101,1.2g active calcium phosphates,
2g activated Calcium carbonates, 0.1g CMC complete the modified dispersion of graphene oxide, and stirring shearing dispersion 1h adds potassium hydroxide tune
PH value is to neutrality；
C, by above-mentioned graphene oxide modification liquid be ground to D50 be 6um, D90 is 13um；
D, it is modified terminate after, carry out ultrasound filtration it is dry modified graphene powder.
Embodiment 4
A kind of preparation method of modified graphene oxide, comprises the following steps：
A, by 50g graphene oxide powders, 3g cetyl benzenesulfonic acid sodiums, 0.5gEEA, 0.3gEMMA, 0.2gEMA are in going
Carried out in ionized water pre-dispersed；
B, be subsequently adding 2g silane coupler KH570,0.5g aluminum-zirconium coupling agent TL-4,1.5g active calcium phosphate, 1g activity
Calcium carbonate, 0.02g CMC, 0.03gMC complete the modified dispersion of graphene oxide, and stirring shearing dispersion 1h adds bicarbonate
Sodium adjusts pH value to neutrality；
C, by above-mentioned graphene oxide modification liquid be ground to D50 be 5um, D90 is 10um；
D, it is modified terminate after, carry out ultrasound filtration it is dry modified graphene powder.
Embodiment 5
A kind of modified graphene oxide EPS molds the preparation method of styrofoam, comprises the following steps：Will be by the side of embodiment 1
Modified graphene oxide powder obtained in method carries out suspension polymerisation in being added to white material EPS systems, then foam re-pack be obtained can send out
Property polystyrene molding styrofoam；The white material EPS systems include pure water, styrene, BPO, active calcium phosphate and pentane；Polymerization
In system, pure water is 4 with the weight ratio of styrene:1, styrene 20wt%, pure water 80wt%, BPO 0.04wt%, active phosphorus
Sour calcium 0.1wt%, modified graphene oxide 0.1wt%, pentane 1.4wt%, polymerization time is 11h.Mold the density of styrofoam
It is 16kg/m3, tested for tensile strength and thermal conductivity factor, it is tensile strength 0.265MPa to test, thermal conductivity factor 0.0282W/ (m
K)。
Embodiment 6
A kind of modified graphene oxide EPS molds the preparation method of styrofoam, comprises the following steps：Will be by the side of embodiment 2
Modified graphene oxide powder obtained in method carries out suspension polymerisation in being added to white material EPS systems, then foaming re-pack be obtained can
Hair property polystyrene molding styrofoam；The white material EPS systems include pure water, styrene, BPO, active calcium phosphate, pentane；It is poly-
In zoarium system, pure water is 3 with the weight ratio of styrene:1, styrene 25wt%, pure water 75wt%, BPO 0.075wt%, activity
Calcium phosphate 0.175wt%, Graphene 0.125wt%, pentane 2.0wt%, polymerization time is 10h.Mold styrofoam density be
16kg/m3, tested for tensile strength and thermal conductivity factor, it is tensile strength 0.277MPa to test, thermal conductivity factor 0.0284W/ (mK).
Embodiment 7
A kind of modified graphene oxide EPS molds the preparation method of styrofoam, comprises the following steps：Will be by the side of embodiment 3
Modified graphene oxide powder obtained in method carries out suspension polymerisation in being added to white material EPS systems, then foaming re-pack be obtained can
Hair property polystyrene molding styrofoam；The white material EPS systems include pure water, styrene, BPO, active calcium phosphate, pentane；Its
In, pure water is 2 with the weight ratio of styrene:1, styrene 33wt%, pure water 66wt%, BPO 0.132wt%, active calcium phosphate
0.265wt%, Graphene 0.165wt%, pentane 2.97wt%, polymerization time is 12h.The density for molding styrofoam is 16kg/
m3, tested for tensile strength and thermal conductivity factor, it is tensile strength 0.289MPa to test, thermal conductivity factor 0.0283W/ (mK).
Embodiment 8
A kind of modified graphene oxide EPS molds the preparation method of styrofoam, comprises the following steps：Will be by the side of embodiment 4
Modified graphene oxide powder obtained in method carries out suspension polymerisation in being added to white material EPS systems, then foaming re-pack be obtained can
Hair property polystyrene molding styrofoam；The white material EPS systems include pure water, styrene, BPO, active calcium phosphate, pentane；Its
In, pure water is 1 with the weight ratio of styrene:1, styrene 50wt%, pure water 50wt%, BPO 0.25wt%, active calcium phosphate
0.5wt%, Graphene 0.25wt%, pentane 5wt%, polymerization time is 11.5h.The density for molding styrofoam is 16kg/m3, survey
Examination tensile strength and thermal conductivity factor, it is tensile strength 0.285MPa to test, thermal conductivity factor 0.0281W/ (mK).
The gained modified graphene oxide EPS of embodiment 5- embodiments 8 molding styrofoam tensile strength and thermal conductivity factor with
The contrast of national standard is shown in Table 1.
Table 1
Claims (10)
1. a kind of preparation method of modified graphene oxide, it is characterised in that comprise the following steps：
A, graphene oxide, activator and stabilizer are carried out in deionized water it is pre-dispersed, wherein activator and stabilizer with
The percentage by weight of graphene oxide is respectively 2-6wt% and 2-8wt%；
B, it is subsequently adding coupling agent, dispersant and dispersion aids and carries out the modified dispersion of graphene oxide, adds alkali regulation PH
The weight hundred of graphene oxide modification liquid, the coupling agent, dispersant and dispersion aids and graphene oxide is obtained to neutrality for value
Divide than respectively 1-5wt%, 5-10wt% and 0.1-0.5wt%；
C, the number of plies that above-mentioned graphene oxide modification liquid is ground to modified graphene oxide<10 layers, particle diameter：D50 is 5-10um,
D90 is 10-20um；
After D, modified end, carry out ultrasound filtration, dry prepared modified graphene powder.
2. a kind of preparation method of modified graphene oxide according to claim 1, it is characterised in that the graphite oxide
Alkene is prepared in accordance with the following methods：In concentrated sulfuric acid system, to addition potassium permanganate, sodium nitrate or addition permanganic acid in native graphite
Potassium, hydrogen peroxide prepare graphite oxide for strong oxidizer reaction, and reusable heat plavini is by graphite oxide in 1000 DEG C or so of high temperature
Heat treatment, then using the continuous impact peel graphite oxide of ultrasonic wave.
3. a kind of preparation method of modified graphene oxide according to claim 1, it is characterised in that the graphite oxide
Alkene can also be prepared in accordance with the following methods：Under concentrated nitric acid, concentrated sulfuric acid system, add potassium chlorate for oxidant reacts, make
Standby graphite oxide, reusable heat plavini by graphite oxide in 1000 DEG C or so of high-temperature heat treatment, it is then continuous using ultrasonic wave
Impact peel graphite oxide.
4. the preparation method of a kind of modified graphene oxide according to claim 1, it is characterised in that：The activator is
Sodium alkyl benzene sulfonate, molecular formula R-C6H4-SO3Na。
5. the preparation method of a kind of modified graphene oxide according to claim 4, it is characterised in that：The activator is
At least one in neopelex, cetyl benzenesulfonic acid sodium, octadecyl benzenesulfonic acid sodium.
6. the preparation method of a kind of modified graphene oxide according to claim 1, it is characterised in that：The stabilizer is
At least one in Tissuemat E, ethene-beta-unsaturated esters copolymer, ethylene-vinyl acetate copolymer.
7. the preparation method of a kind of modified graphene oxide according to claim 1, it is characterised in that：The coupling agent is
At least one in silane coupler, titanate coupling agent, aluminate coupling agent, aluminum-zirconium coupling agent.
8. the preparation method of a kind of modified graphene oxide according to claim 1, it is characterised in that：The dispersant is
At least one in active calcium phosphate, activated Calcium carbonate.
9. the preparation method of a kind of modified graphene oxide according to claim 1, it is characterised in that：The dispersion aids
It is at least one in methylcellulose, carboxymethylcellulose calcium.
10. a kind of modified graphene oxide EPS molds the preparation method of styrofoam, it is characterised in that comprise the following steps：Will power
Profit requires that the modified graphene that any one of 1-9 claim methods describeds are obtained is suspended in being added to white material EPS systems
Polymerization, then the prepared expandable polystyrene molding styrofoam that re-packs that foams；The white material EPS systems include pure water, styrene, draw
Hair agent BPO, dispersant active calcium phosphate and foaming agent pentane；In polymerization system, pure water is 1-4 with the weight ratio of styrene:1,
The percentage by weight of modified graphene, BPO, active calcium phosphate, pentane and styrene be respectively 0.5%wt, 0.2-0.5wt%,
0.5-1wt% and 7-10wt%, polymerization time is 10-12h.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611026588.3A CN106752116A (en) | 2016-11-15 | 2016-11-15 | The preparation method and modified graphene oxide EPS of modified graphene oxide mold the preparation method of styrofoam |
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