CN108384131A - White graphite alkene modified polystyrene composite material and preparation method thereof - Google Patents
White graphite alkene modified polystyrene composite material and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
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Abstract
The present invention provides a kind of white graphite alkene modified polystyrene composite material and preparation method thereof, which is mainly prepared by the raw material of following parts by weight：0.01 0.1 parts of 90 110 parts of styrene, 0.5 10 parts of high polymer modification white graphite alkene, 0.05 2 parts of fire retardant, 0.05 2 parts of antioxidant and initiator.With higher mechanical strength while above-mentioned white graphite alkene modified polystyrene composite material is with fire-retardant and smoke suppressing.
Description
Technical field
The present invention relates to field of high polymer material modification, more particularly to white graphite alkene modified polystyrene composite material
And preparation method thereof.
Background technology
Polystyrene (PS) is the polymer by styrene monomer free radical addition polymerization, has transparent, molding
Property is good, rigidity is good, electrical insulation capability is good, easy dyeing, agent of low hygroscopicity and it is cheap the advantages that, in electronics, automobile, building, packet
The industries such as dress, household electrical appliances, daily necessities, toy are widely used.But PS matter is crisp, not impact resistance, poor heat resistance, heat distortion temperature
Low (generally at 78-98 DEG C), is easy burning and raw smoke is big, belongs to combustible material, therefore application is restricted.
It is insufficient existing for PS to solve at present, it generally can be by improving toughness and resistance to stress with rubber or other resin alloys
Cracking performance, is added inorganic filler or the higher resin of glass transition temperature improves heat resistance, and addition fire retardant assigns its resistance
Fire performance.Although but all kinds of toughener, heat-proof modifier and fire retardant improve to a certain extent the toughness of PS, heat resistance and
Flame retardant property has but seriously affected the mechanical strength of PS.
Invention content
Based on this, it is necessary to provide it is a kind of while with compared with high fire-retardance, smoke suppressing with higher mechanical strength
White graphite alkene modified polystyrene composite material and preparation method thereof.
A kind of white graphite alkene modified polystyrene composite material, is mainly prepared by the raw material of following parts by weight：Gao Ju
Object modifies 0.5-10 parts of white graphite alkene, 90-110 parts of styrene, 0.05-2 parts of fire retardant, 0.05-2 parts of antioxidant and initiator
0.01-0.1 parts.
The white graphite alkene modified polystyrene composite material mainly by high polymer modification white graphite alkene, styrene, fire retardant,
Antioxidant and initiator occur polymerisation and are prepared, and by controlling raw material proportioning, make the white graphite alkene modified polyphenyl
With higher mechanical performance while ethylene composite material is with excellent fire-retardant and smoke suppressing.
High polymer modification white graphite alkene in the white graphite alkene modified polystyrene composite material forms piece layered network, makes
The warm-up movement of polystyrene strand can effectively be inhibited when combustion reaction occurs by obtaining the composite material, improve compound system
Viscosity, play hinder volatile fuel, the gas generated in combustion process, smog, solid particle overflow and extraneous oxygen into
The effect of entering can also act synergistically together with fire retardant, antioxidant, improve fire-retardant and smoke suppressing effect, promote antioxidant
Inhibition high polymer oxidative degradation effect, while controlling the dosage of antioxidant, fire retardant, avoid because of antioxidant, fire-retardant
Agent addition excessively causes the decline of mechanical performance, and cost is also reduced in certain amplitude.And the white stone of the high polymer modification
Black alkene can prevent white graphite alkene from reuniting, and enhance its interface performance with matrices of composite material, make the white graphite alkene of high polymer modification
In polystyrene can be evenly dispersed, promote the formation of entire material system piece layered network, it to a certain extent so that should
White graphite alkene modified composite material has higher mechanical strength.
In a wherein embodiment, the high polymer modification white graphite alkene is 3-10 parts, and the styrene is 95-105 parts,
The fire retardant is 0.5-2 parts, and the antioxidant is 0.5-2 parts and the initiator is 0.01-0.1 parts.
The white graphite alkene modified polystyrene composite material that raw material in the range is prepared has higher fire-retardant
And smoke suppressing.
In a wherein embodiment, the high polymer modification white graphite alkene mainly by the raw material of following parts by weight prepare and
At：0.5-10 parts of white graphite alkene, 0.05-2 parts of polymerized monomers and 0.5-5 parts of initiators；
The polymerized monomer is styrene, acrylic acid, methyl acrylate, ethyl acrylate, hydroxy-ethyl acrylate, methyl-prop
It is one or more in e pioic acid methyl ester and glycidyl methacrylate.
In a wherein embodiment, the grain size of the high polymer modification white graphite alkene is 5-10 μm, specific surface area 300-
500m2/g。
In a wherein embodiment, the fire retardant is that organic phosphorus flame retardant, silicon-series five-retardant and sulfonate system are fire-retardant
One or more of agent.
In a wherein embodiment, the antioxidant is one in antioxidant 1010, irgasfos 168 and antioxidant 2912
Kind is several.
A kind of preparation method of white graphite alkene modified polystyrene composite material, includes the following steps：
By the styrene, the high polymer modification white graphite alkene, the fire retardant, the antioxidant and described draw
It sends out agent to be uniformly mixed, under the protection of inert gas, reacts 3-6h at a temperature of 80 DEG C -90 DEG C, obtain reaction solution, then by institute
It states reaction solution to mix for 100-150 parts with decentralized medium, be subsequently poured into ethyl alcohol, collect the precipitation of generation and be drying to obtain described white
Graphene modified polystyrene composite material.
By being mixed with remaining component styrene monomer polymerisation shape occurs under the action of initiator for the above method
At modified composite material, polystyrene is modified compared to directly polystyrene and remaining component melts are blended, is had
It has the advantage that：(1) be conducive to high polymer modification white graphite alkene to spread more evenly across in PS, so that being formed by entire
The piece layered network of material system is more uniform, and manufactured modified material has higher mechanical strength.(2) post-processing simplicity etc..
In a wherein embodiment, the decentralized medium is one or more in toluene and ethylbenzene.
In a wherein embodiment, the high polymer modification white graphite alkene is prepared by following methods：
It counts in parts by weight, 0.5-10 parts of white graphite alkene is placed in ultrasonic disperse in 90-110 parts of dispersion liquids, are added
0.1-0.5 parts of stabilizers are handled, and are obtained oleophylic and are modified white graphite alkene dispersion liquid；
Oleophylic modification white graphite alkene dispersion liquid is uniformly mixed with 0.05-2 parts of polymerized monomers, 0.5-5 parts of initiators,
And 0.5-3h is reacted at 60 DEG C -100 DEG C, and neutralizer tune pH to 7-8 is added, it is cooling, it filters, be drying to obtain the high polymer and repair
Adorn white graphite alkene.
This method is prepared through polymerisation, is formed polymer covering layer on white graphite alkene surface, is repaiied to prepare high polymer
Adorn white graphite alkene.It is controllable that this method is formed by coating thickness, and thickness is uniform, is conducive to that its is evenly dispersed in PS, promotees
Into the formation of the piece layered network of entire material system.
In a wherein embodiment, the stabilizer be polyvinylpyrrolidone, sodium alkyl sulfate, sodium alkyl benzene sulfonate,
It is one or more in oleyl amine and oleic acid.
Specific implementation mode
To facilitate the understanding of the present invention, below will to invention is more fully described, and give the present invention compared with
Good embodiment.But the present invention can realize in many different forms, however it is not limited to embodiment described herein.Phase
Instead, purpose of providing these embodiments is makes the disclosure of the present invention more thorough and comprehensive.
Unless otherwise defined, all of technologies and scientific terms used here by the article and belong to the technical field of the present invention
The normally understood meaning of technical staff is identical.Used term is intended merely to description tool in the description of the invention herein
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein "and/or" includes one or more phases
Any and all combinations of the Listed Items of pass.
A kind of white graphite alkene modified polystyrene composite material, is mainly prepared by the raw material of following parts by weight：Benzene second
90-110 parts of alkene, 0.5-10 parts of high polymer modification white graphite alkene, 0.05-2 parts of fire retardant, 0.05-2 parts of antioxidant and initiator
0.01-0.1 parts.
In a wherein embodiment, high polymer modification white graphite alkene is 3-10 parts, and styrene is 95-105 parts, and fire retardant is
0.5-2 parts, antioxidant is 0.5-2 parts and initiator is 0.01-0.1 parts.
In a wherein embodiment, high polymer modification white graphite alkene is 5-10 parts, and styrene is 95-105 parts, and fire retardant is
1-2 parts, antioxidant is 1-2 parts and initiator is 0.01-0.1 parts.
Wherein, high polymer modification white graphite alkene refers to forming the white graphite alkene of high polymer clad on surface.The clad
Can be polystyrene, acroleic acid resin etc..
In one embodiment, which is polymethyl methacrylate；In one embodiment, which is polypropylene
Sour methyl esters；In one embodiment, which is poly (glycidyl methacrylate)；In one embodiment, which is
Polystyrene.
It should be noted that above-mentioned white graphite alkene modified polystyrene composite material is by mixing monomer and remaining component
It closes, polymerisation occurs under the action of initiator and is formed by modified composite material.After monomer is mixed with remaining component again
Polymerisation occurs, is had the following advantages than being directly blended with remaining component melts using polystyrene：(1) be conducive to high polymer
Modification white graphite alkene spreads more evenly across in PS, so that the piece layered network for being formed by entire material system is more equal
One, manufactured modified material has higher mechanical strength.(2) post-processing simplicity etc..
Additionally, it is preferred that the purity of above-mentioned styrene is more than 99.6%, to improve polymerisation efficiency.Decompression may be used to steam
It the modes such as evaporates to purify it.
Fire retardant is to confer to the functional aid of polymer flame retardancy.The fire retardant can be additive flame retardant, pass through
Mechanical mixture is added in above-mentioned composite material, or reactive flame retardant, as monomer, and under the action of initiator, with
Polymerisation occurs together for styrene, forms the polymer containing flame-retardant composition.In one embodiment, using additive flame retardant
Agent.The additive flame retardant can be organic phosphorus flame retardant, silicon-series five-retardant, one kind in sulfonate flame retardant or several
Kind.
Antioxidant is the substance that can inhibit or delay high molecular polymer oxidative degradation.In one embodiment, it aoxidizes
Agent is one or more of antioxidant 1010, irgasfos 168 and antioxidant 2912.
Wherein antioxidant 1010 is four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters；It is anti-oxidant
Agent 168 is three [2,4- di-tert-butyl-phenyl] phosphite esters, and antioxidant 2912 can be bought from Shanghai Jinin trade Co., Ltd.
The present invention also provides the preparation methods of above-mentioned white graphite alkene modified polystyrene composite material, including following step
Suddenly：
By 90-110 parts of styrene, 0.5-10 parts of high polymer modification white graphite alkene, 0.05-2 parts of fire retardant, antioxidant
0.05-2 parts and 0.01-0.1 parts of initiator are uniformly mixed, anti-at a temperature of 80 DEG C -90 DEG C under the protection of inert gas
3-6h is answered, reaction solution is obtained, then reaction solution is mixed for 100-150 parts with decentralized medium, is subsequently poured into atent solvent, collects production
Raw precipitation is simultaneously drying to obtain white graphite alkene modified polystyrene composite material.
The order of addition of above-mentioned material is not particularly limited, and in one embodiment, initiator is first added, in the atmosphere of inert gas
It is slow added into remaining ingredient under enclosing, the reaction was complete to promote styrene monomer.In addition, being reacted after the completion of polymerisation
Liquid can pour into reaction solution in decentralized medium, so that generated white graphite alkene modified polystyrene can be uniformly dispersed
In a dispersion medium, then the mixed liquor is poured slowly into ethyl alcohol, product is made to be precipitated again in the state of stirring.
In one embodiment, 0.01-0.1 parts of initiators are first added by weight, lead to nitrogen, condenser pipe reflux.Then exist
Remaining ingredient is added under nitrogen stream to cool down liquid in 80 DEG C of-90 DEG C of waters bath with thermostatic control after polyase 13-6h, be then added to 100-150
In part decentralized medium, it is poured slowly into ethyl alcohol under stiring, polymer fibrids is made to come out, 50 DEG C are dried under vacuum to constant weight, obtain
It is modified PS composite materials to white graphite alkene.
Wherein, decentralized medium can be one or more in toluene and ethylbenzene.
In addition, high polymer modification white graphite alkene can be prepared by following methods：
(1) it counts in parts by weight, 0.5-10 parts of white graphite alkene is placed in ultrasonic disperse in 90-110 parts of dispersion liquids, are added
0.1-0.5 parts of stabilizers are handled, and are obtained oleophylic and are modified white graphite alkene dispersion liquid；
(2) oleophylic modification white graphite alkene dispersion liquid is uniformly mixed with 0.05-2 parts of polymerized monomers, 0.5-5 parts of initiators,
And 0.5-3h is reacted at 60 DEG C -100 DEG C, and neutralizer tune pH to 7-8 is added, it is cooling, it is drying to obtain high polymer modification white graphite
Alkene.
White graphite alkene is placed in dispersion liquid carries out ultrasonic disperse first by the above method；After ultrasound, stabilizer is added, it is right
The surface of white graphite alkene is modified, and to improve its surface-active, then is polymerize under the action of initiator with polymerized monomer
Reaction, to form clad on white graphite alkene surface.Since white graphite alkene is dispersed in through ultrasound in dispersion liquid, therefore at it
The coating thickness of upper formation is uniform, can effectively improve the dispersibility of the high polymer modification white graphite alkene in PS.In addition,
It can be adjusted by the concentration to polymerized monomer, to adjust the thickness of clad, simple and convenient.
Wherein, dispersion liquid can be one or more in water, ethyl alcohol, ethylene glycol and glycerine etc..Stabilizer can be
It is one or more in polyvinylpyrrolidone, sodium alkyl sulfate, sodium alkyl benzene sulfonate, oleyl amine and oleic acid etc..
In one embodiment, polymerized monomer is styrene, acrylic acid, methyl acrylate, ethyl acrylate, acrylic acid hydroxyl second
It is one or more in ester, methyl methacrylate, glycidyl methacrylate.
In addition, used initiator is one or more in azo-initiator or peroxide initiator.
In one embodiment, initiator is ammonium persulfate or azodiisobutyronitrile.
In addition, when oleophylic modification white graphite alkene is uniformly mixed with polymerized monomer, initiator, material order of addition is without special limit
It is fixed.In one embodiment, the modified white graphite alkene dispersion liquid of oleophylic is first warming up to 60-100 DEG C of reaction temperature, 0.5- is added
5 parts of initiators, stirring 10-30min keep solution uniform, polymerized monomer are added dropwise dropwise, 0.5-1h is dripped off.
In addition, the hybrid mode in the hybrid manipulation includes one in mechanical agitation, ultrasound and ultrasound-mechanical agitation joint
Kind.In one embodiment, it is mixed using the united mode of ultrasound-mechanical agitation.
Neutralizer tune pH to 7-8 is added after the completion of polymerisation to improve the compatibility of high polymer and white graphite alkene, in this
Can be one or more in ammonium hydroxide, dimethylethanolamine, triethylamine, sodium hydroxide, potassium hydroxide with agent.In an embodiment
In, neutralizer is ammonium hydroxide.Additionally, it is preferred that being rapidly cooled to room temperature after neutralizer is added.Then dry with washing, Ke Yiyong
Ethyl alcohol is washed, to reduce subsequently dry difficulty.Furthermore it is possible to which obtained high polymer modification white graphite alkene is ground
Mill, obtains the smaller high polymer modification white graphite alkene of grain size, is conducive to the modification subsequently to composite material.
The preparation method of above-mentioned white graphite alkene modified polystyrene composite material is easy to operate, is without complicated post-processing
Target product can be obtained.The white graphite alkene modified polystyrene composite material obtained by this method has the advantage that：
(1) higher fire-retardant, smoke suppressing
High polymer modification white graphite alkene forms piece layered network, can effectively inhibit polystyrene molecule in combustion
The warm-up movement of chain improves the viscosity of compound system, play hinder volatile fuel, the gas generated in combustion process, smog,
The effect of solid particle overflows and extraneous oxygen enters, can also act synergistically together with fire retardant, antioxidant, improve fire-retardant
And smoke suppressing effect, the effect of the inhibition high polymer oxidative degradation of antioxidant is promoted, while reducing the use of antioxidant, fire retardant
Amount, avoid because antioxidant, retardant load level excessively caused by mechanical performance decline, and also in certain amplitude reduce at
This.
(2) higher mechanical performance
The white graphite alkene of the high polymer modification can prevent white graphite alkene from reuniting, and it is interface characteristics with matrices of composite material to enhance it
Can, make the white graphite alkene of high polymer modification in polystyrene can be evenly dispersed, promotes entire material system piece layered network
Formation, to a certain extent so that the white graphite alkene modified composite material have higher mechanical strength.
(3) excellent heat resistance
Above-mentioned white graphite alkene modified polystyrene composite material is modified PS by high polymer modification white graphite alkene, by
It is fire retardant under the two-dimensional slice structure that white graphite alkene is single layer or few layer, high temperature, it is specific surface area with superelevation, excellent heat-resisting
Property, therefore there is excellent heat resistance by the material of its modification.
(4) compared with high working property
High polymer modification white graphite alkene, fire retardant and antioxidant be insulation, transparence substance, be added PS matrixes after, no
It can influence the insulating properties and the transparency of PS.
With reference to specific embodiment, the present invention will be described.
Embodiment 1
The preparation of step 1) high polymer modification white graphite alkene：0.5 part of white graphite alkene powder is taken to be added into round-bottomed flask, and
100 parts of distilled water are added into round-bottomed flask, then ultrasonic disperse, 0.1 part of lauryl sodium sulfate are added into round-bottomed flask,
Ultrasonic high-speed stirred obtains oleophylic and is modified white graphite alkene；After the white graphite alkene aqueous dispersions that oleophylic is modified are heated to 60 DEG C, add
Enter 0.5 part of initiator azodiisobutyronitrile, after stirring 10min starts that 0.05 part of styrene is added dropwise, 0.5h is dripped off.It is added dropwise
Afterwards, heat preservation 0.5h waits for that reaction is completed.It is 7 to adjust pH value with ammonium hydroxide after completion of the reaction, is rapidly cooled to room temperature, is filtered under diminished pressure, and is used
Distill primary with ethanol wash after water washing filter cake 3~4 times, and vacuum drying grinding obtains polystyrene modification at 60 DEG C
White graphite alkene；
Step 2) is by weight by 100 parts of styrene, 0.5 part of high polymer modification white graphite alkene, 0.05 part of organic phosphate flame-retardant
Agent and 0.5 part of antioxidant 1010 ultrasound-mechanical agitation joint are uniformly mixed；
Step 3) takes three-necked bottle, and 0.01 part of azodiisobutyronitrile is first added by weight, leads to nitrogen, condenser pipe reflux.So
The mixed solution of step 2) is added under nitrogen flowing afterwards, in 80 DEG C of waters bath with thermostatic control after polyase 13 h, the liquid in three-necked bottle is cooled down,
It is then added in 100 parts of toluene, is poured slowly into ethyl alcohol under stiring, polymer fibrids is made to come out, 50 DEG C are dried under vacuum to
Constant weight, the white graphite alkene for obtaining embodiment 1 are modified PS composite materials.
Embodiment 2
The preparation of step 1) high polymer modification white graphite alkene：2 parts of white graphite alkene powder are taken to be added into round-bottomed flask, and to
100 parts of ethyl alcohol are added in round-bottomed flask, then ultrasonic disperse, 0.2 part of lauryl sodium sulfate, ultrasound are added into round-bottomed flask
High-speed stirred obtains oleophylic and is modified white graphite alkene；After the white graphite alkene alcohol dispersion liquid that oleophylic is modified is heated to 90 DEG C, it is added
1 part of initiator ammonium persulfate after stirring 15min starts that 0.5 part of styrene is added dropwise, and 0.6h is dripped off.After being added dropwise, heat preservation 1h is waited for
Reaction is completed.It is 7 to adjust pH value with ammonium hydroxide after completion of the reaction, is rapidly cooled to room temperature, is filtered under diminished pressure, is washed with distilled water filter cake
It is primary with ethanol wash after 3~4 times, and vacuum drying grinding obtains the white graphite alkene of polystyrene coating decoration at 70 DEG C；
Step 2) by weight by 100 parts of styrene, 2 parts of high polymer modification white graphite alkene, 0.5 part oxidation phosphorus fire retardant and
1 part of irgasfos 168 ultrasound-mechanical agitation joint is uniformly mixed；
Step 3) takes three-necked bottle, and 0.05 part of ammonium persulfate is first added by weight, leads to nitrogen, condenser pipe reflux.Then exist
The mixed solution of step 2) is added under nitrogen stream, after polymerizeing 4h in 85 DEG C of waters bath with thermostatic control, the liquid in three-necked bottle is cooled down, then adds
Enter into 120 parts of toluene, is poured slowly into ethyl alcohol under stiring, polymer fibrids is made to come out, 50 DEG C are dried under vacuum to constant weight,
The white graphite alkene for obtaining embodiment 2 is modified PS composite materials.
Embodiment 3
The preparation of step 1) high polymer modification white graphite alkene：8 parts of white graphite alkene powder are taken to be added into round-bottomed flask, and to
100 parts of glycerine are added in round-bottomed flask, then ultrasonic disperse, 0.3 part of oleyl amine, ultrasonic high-speed stirring are added into round-bottomed flask
It mixes, obtains oleophylic and be modified white graphite alkene；After the white graphite allyl triol dispersion liquid that oleophylic is modified is heated to 90 DEG C, it is added 2 parts
Initiator azodiisobutyronitrile after stirring 20min starts that 1 part of glycidyl acrylate ester is added dropwise, and 0.7h is dripped off.It is added dropwise
Afterwards, heat preservation 1.5h waits for that reaction is completed.It is 8 to adjust pH value with ammonium hydroxide after completion of the reaction, is rapidly cooled to room temperature, is filtered under diminished pressure, and is used
Distill primary with ethanol wash after water washing filter cake 3~4 times, and vacuum drying grinding obtains polymethylacrylic acid contracting at 90 DEG C
The white graphite alkene of water glyceride coating decoration；
Step 2) is by weight by 100 parts of styrene, 8 parts of high polymer modification white graphite alkene, 2 parts of copolymerization organosiloxane resistances
It fires agent and 1.5 parts of irgasfos 168 ultrasounds-mechanical agitation joint is uniformly mixed；
Step 3) takes three-necked bottle, and 0.08 part of ammonium persulfate is first added by weight, leads to nitrogen, condenser pipe reflux.Then exist
The mixed solution of step 2) is added under nitrogen stream, after polymerizeing 5h in 85 DEG C of waters bath with thermostatic control, the liquid in three-necked bottle is cooled down, then adds
Enter into 120 parts of toluene, is poured slowly into ethyl alcohol under stiring, polymer fibrids is made to come out, 50 DEG C are dried under vacuum to constant weight,
The white graphite alkene for obtaining embodiment 3 is modified PS composite materials.
Embodiment 4
The preparation of step 1) high polymer modification white graphite alkene：10 parts of white graphite alkene powder are taken to be added into round-bottomed flask, and
100 parts of distilled water are added into round-bottomed flask, then ultrasonic disperse, 0.5 part of polyvinylpyrrolidone are added into round-bottomed flask,
Ultrasonic high-speed stirred obtains oleophylic and is modified white graphite alkene；After the white graphite alkene aqueous dispersions that oleophylic is modified are heated to 100 DEG C,
5 parts of initiator idol ammonium persulfates are added, after stirring 10min start that 2 parts of styrene are added dropwise, 1h is dripped off.After being added dropwise, 2h is kept the temperature
Wait for that reaction is completed.It is 8 to adjust pH value with ammonium hydroxide after completion of the reaction, is rapidly cooled to room temperature, is filtered under diminished pressure, is washed with distilled water filter
It is primary with ethanol wash after cake 3~4 times, and vacuum drying grinding obtains the white graphite of polystyrene coating decoration at 90 DEG C
Alkene；
Step 2) is by weight by 100 parts of styrene, 10 parts of high polymer modification white graphite alkene, -1 part of benzenesulfonyl benzene sulfonic acid
Potassium fire retardant and 2 parts of 2912 ultrasounds of antioxidant-mechanical agitation joint are uniformly mixed；
Step 3) takes three-necked bottle, and 0.1 part of ammonium persulfate is first added by weight, leads to nitrogen, condenser pipe reflux.Then in nitrogen
The mixed solution of step 2) is added under air-flow, after polymerizeing 6h in 90 DEG C of waters bath with thermostatic control, the liquid in three-necked bottle is cooled down, is added
It into 150 parts of toluene, is poured slowly into ethyl alcohol under stiring, polymer fibrids is made to come out, 50 DEG C are dried under vacuum to constant weight, obtain
White graphite alkene to embodiment 4 is modified PS composite materials.
Embodiment 5
Substantially the same manner as Example 4, difference is that form the polymerized monomer of high polymer modification white graphite alkene is acrylic acid first
Ester；
Embodiment 6
Substantially the same manner as Example 4, difference is that form the polymerized monomer of high polymer modification white graphite alkene is acrylic acid hydroxyl
Ethyl ester；
Embodiment 7
Substantially the same manner as Example 4, difference is that form the polymerized monomer of high polymer modification white graphite alkene is metering system
Acid glycidyl ester；
Comparative example 1
Pure PS
It is same as Example 1 to prepare used initiator, solvent and reaction temperature and time when PS.
Comparative example 2
It is substantially the same manner as Example 4, the difference is that the white graphite alkene without high polymer modification.
Comparative example 3
It is substantially the same manner as Example 4, the difference is that white graphite alkene is without high polymer modification.
Comparative example 4
It is substantially the same manner as Example 4, the difference is that the additive amount of high polymer modification white graphite alkene is 20 parts；
Comparative example 5
Preparation method：By 100 parts of polystyrene, 0.5 part of high polymer modification white graphite alkene, 0.05 part of phosphate flame retardant and
0.5 part of antioxidant 1010, which is added in high-speed mixer, mixes 5min；
Double screw extruder is added in said mixture again to squeeze out, then is granulated by pelleter, the white graphite of comparative example 2 is obtained
Alkene modified polystyrene composite material.Wherein each area's temperature of double screw extruder squeezes out owner in 190 DEG C, 200 DEG C of head temperature
Machine rotating speed 250rpm, feeding rotating speed 8Hz；Pelleter speed 6Hz.The white graphite alkene for obtaining comparative example 5 is modified PS composite materials.
Performance test
Test method：
Simply supported beam notch impact strength：GB/T 1043.1-2008
Tensile strength：GB/T 1040.2-2006
Bending strength：GB/T 9341-2008
UL94 is fire-retardant：UL-94
Peak value gives birth to cigarette rate：GB/T 8323-1987
Heat distortion temperature：GB/T 1633-2000
Test result is as shown in table 1：
1 each embodiment of table and comparative example performance data
As known from Table 1, the white graphite alkene modified polystyrene composite material of embodiment 1- embodiments 7 has lower peak value
Raw cigarette rate, higher UL94 flame retardant ratings, illustrate it with excellent fire-retardant, smoke suppressing；With higher heat distortion temperature,
Illustrate it with stronger heat resistance；And there is higher simply supported beam notch impact strength, tensile strength and bending strength, explanation
It is with higher mechanical strength.
Comparative example 4- embodiments 7 it is found that polymerized monomer dialogue graphene modified polystyrene composite material performance
Tool has a certain impact, optimization styrene.
In addition, comparative example 1 is non-modified PS, comparative example 2 is free of the white graphite alkene of high polymer modification, comparative example 3
White graphite alkene is wrapped up without high polymer and being modified, from table 1 it follows that being compared with embodiment 4, the resistance of comparative example 1- comparative examples 3
Combustion, suppression cigarette, heat-resisting and mechanical performance have and greatly reduce, and illustrate that the presence of high polymer package modification white graphite alkene can be with
Significantly promote the flame-retardant smoke inhibition of the composite material, heat-resisting and mechanical performance.
In addition, the additive amount of the high polymer modification white graphite alkene of comparative example 4 is more than embodiment 4, as it can be seen from table 1 right
The fire-retardant of ratio 4, suppression cigarette, heat-resisting and mechanical performance are influenced to different extents, illustrate high polymer modification white graphite alkene
Additive amount needs to control in a certain range.
Comparative example 5 is the modified composite material for adding polystyrene and being prepared by the method for melt blending, can from table 1
To find out, the fire-retardant of comparative example 5, suppression cigarette, heat-resisting and mechanical performance are not so good as embodiment 1, illustrate to mix monomer and remaining component
The performance of the obtained modified composite material of polymerisation occurs after conjunction again, system is blended with remaining component melts better than polystyrene
At composite material.
Each technical characteristic of embodiment described above can be combined arbitrarily, to keep description succinct, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, it is all considered to be the range of this specification record.
Several embodiments of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of white graphite alkene modified polystyrene composite material, which is characterized in that mainly prepared by the raw material of following parts by weight
It forms：0.5-10 parts of high polymer modification white graphite alkene, 90-110 parts of styrene, 0.05-2 parts of fire retardant, antioxidant 0.05-2
0.01-0.1 parts of part and initiator.
2. white graphite alkene modified polystyrene composite material according to claim 1, which is characterized in that the high polymer is repaiied
It is 3-10 parts to adorn white graphite alkene, and the styrene is 95-105 parts, and the fire retardant is 0.5-2 parts, and the antioxidant is
0.5-2 parts and the initiator are 0.01-0.1 parts.
3. white graphite alkene modified polystyrene composite material according to claim 1 or 2, which is characterized in that described high poly-
Object modification white graphite alkene is mainly prepared by the raw material of following parts by weight：0.5-10 parts of white graphite alkene, 0.05-2 parts of polymerizations are single
Body and 0.5-5 parts of initiators；
The polymerized monomer is styrene, acrylic acid, methyl acrylate, ethyl acrylate, hydroxy-ethyl acrylate, methacrylic acid
It is one or more in methyl esters and glycidyl methacrylate.
4. white graphite alkene modified polystyrene composite material according to claim 1 or 2, which is characterized in that described high poly-
The grain size that object modifies white graphite alkene is 5-10 μm, specific surface area 300-500m2/g。
5. white graphite alkene modified polystyrene composite material according to claim 1 or 2, the fire retardant is organic phosphorus
One or more of fire retardant, silicon-series five-retardant and sulfonate flame retardant.
6. white graphite alkene modified polystyrene composite material according to claim 1 or 2, the antioxidant is antioxidant
1010, one or more of irgasfos 168 and antioxidant 2912.
7. a kind of preparation method of claim 1-6 any one of them white graphite alkene modified polystyrene composite material, special
Sign is, includes the following steps：
By the styrene, the high polymer modification white graphite alkene, the fire retardant, the antioxidant and the initiator
It is uniformly mixed, under the protection of inert gas, reacts 3-6h at a temperature of 80 DEG C -90 DEG C, obtain reaction solution, then will be described anti-
It answers liquid to be mixed for 100-150 parts with decentralized medium, is subsequently poured into ethyl alcohol, collect the precipitation of generation and be drying to obtain the white graphite
Alkene modified polystyrene composite material.
8. the method according to the description of claim 7 is characterized in that the decentralized medium is one kind or more in toluene and ethylbenzene
Kind.
9. the method according to the description of claim 7 is characterized in that the high polymer modification white graphite alkene is prepared by following methods
It forms：
It counts in parts by weight, 0.5-10 parts of white graphite alkene is placed in ultrasonic disperse in 90-110 parts of dispersion liquids, add 0.1-0.5
Part stabilizer is handled, and is obtained oleophylic and is modified white graphite alkene dispersion liquid；
Oleophylic modification white graphite alkene dispersion liquid is uniformly mixed with 0.05-2 parts of polymerized monomers, 0.5-5 parts of initiators, and in
It reacts 0.5-3h at 60 DEG C -100 DEG C, neutralizer tune pH to 7-8 is added, it is cooling, it filters, to be drying to obtain the high polymer modification white
Graphene.
10. according to the method described in claim 9, it is characterized in that, the stabilizer is polyvinylpyrrolidone, alkylsurfuric acid
It is one or more in sodium, sodium alkyl benzene sulfonate, oleyl amine and oleic acid.
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| CN102618141A (en) * | 2012-03-21 | 2012-08-01 | 青岛海信电器股份有限公司 | Modified acrylate heat-dissipation powder coating as well as preparation method and application thereof |
| CN102786815A (en) * | 2012-08-15 | 2012-11-21 | 中国科学院上海硅酸盐研究所 | Method for modifying surface of BN (boron nitride) powder, modified BN and polymer composite material |
| CN105860315A (en) * | 2016-06-14 | 2016-08-17 | 辽宁大学 | Preparing method of hexagonal boron nitride/polystyrene composite |
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2018
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102618141A (en) * | 2012-03-21 | 2012-08-01 | 青岛海信电器股份有限公司 | Modified acrylate heat-dissipation powder coating as well as preparation method and application thereof |
| CN102786815A (en) * | 2012-08-15 | 2012-11-21 | 中国科学院上海硅酸盐研究所 | Method for modifying surface of BN (boron nitride) powder, modified BN and polymer composite material |
| CN105860315A (en) * | 2016-06-14 | 2016-08-17 | 辽宁大学 | Preparing method of hexagonal boron nitride/polystyrene composite |
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Application publication date: 20180810 |