CN105732860A - Expandable polystyrene beads prepared from expandable few-layer graphene and preparing method of expandable polystyrene beads - Google Patents
Expandable polystyrene beads prepared from expandable few-layer graphene and preparing method of expandable polystyrene beads Download PDFInfo
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F112/00—Homopolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
- C08F112/02—Monomers containing only one unsaturated aliphatic radical
- C08F112/04—Monomers containing only one unsaturated aliphatic radical containing one ring
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
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- C08J9/20—Making expandable particles by suspension polymerisation in the presence of the blowing agent
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Abstract
The invention relates to expandable polystyrene beads prepared from expandable few-layer graphene and a preparing method of the expandable polystyrene beads.Electrochemical intercalation is carried out on natural flake graphite with concentrated sulfuric acid, and a graphite interlayer compound with the interlayer space enlarged is obtained; few-layer graphene is obtained through ultrasonic concussion layer removing, the few-layer graphene is subjected to secondary intercalation with a chemical method, water washing and drying, and the expandable few-layer graphene is obtained; then, the expandable few-layer graphene and polystyrene monomers are subjected to suspension polymerization, and the expandable polystyrene beads prepared from the expandable few-layer graphene is obtained.According to the expandable polystyrene beads prepared from the expandable few-layer graphene and the preparing method of the expandable polystyrene beads, the expandable few-layer graphene is introduced into expandable polystyrene, and expandable graphene can be highly and uniformly dispersed in the expandable polystyrene beads, so that high infrared reflectivity in a cavity of expandable polystyrene is ensured, the heat insulation performance is good, and the expandable few-layer graphene can show the flame-retardant effects of smothering flames and insulating heat radiation.The flame retardant grade of a foam plate prepared from the expandable polystyrene beads reaches the B1 grade, and the heat conductivity value ranges from 0.028 W/(m.K) to 0.032 W/(m.K).
Description
Technical field
The present invention relates to a kind of polystyrene foamed material, especially high fire-retardance, the expandable polystyrene bead containing inflatable few layer graphene of low heat conduction and preparation method.
Background technology
Polystyrene foamed material is by the expandable polystyrene bead containing volatile fluid foaming agent, and heated pre-forms.Because it has good properties of heat preservation and energy saving, therefore it is widely used in the field such as building materials, packaging.
In order to obtain better fire-retardant, heat insulating effect:
CN104231461A discloses one " graphite EPS beadlet and production technology thereof " and granules of polystyrene, foaming agent, the graphite powder of surface modification and fire retardant is mixed graphite EPS beadlet.Graphite owing to mixing is common graphite, and the number of plies is too much, and dispersibility is not good, easily assembles, and causes it to reflect ultrared aspect deficiency, and heat insulation and preservation effect is not ideal enough.
CN103788397A discloses " preparation method of a kind of fire-retardant expandable polystyrene spherolite containing leafing graphite ", and it is characterized in that the sharply expansion of graphite layers is opened when utilizing expansible graphite to meet high temperature, thus the purpose such as the flame that reaches to suffocate, isolation heat radiation.But, mixed expansible graphite granularity excessive (generally all at tens microns), dispersibility is not good, causes anti-flaming thermal-insulation effect not satisfactory.What solve is prepare graphitiferous particle expandable polystyrene suspension polymerisation easily to reunite, the technical problem of the anti-flaming thermal-insulation poor performance of the graphite particle uneven and expandable polystyrene of dispersion in polystyrene.Preparation method is: one, claim raw material by weight;Two, the first mixture is prepared;Three, the second mixture is prepared;Four, the second mixture is under agitation added to the first mixture, after reaction, add emulsifying agent, continue reaction, it is subsequently adding pentane, pour nitrogen in a kettle., heat up and react, after having reacted, by reactor natural cooling, slowly being deflated to discharging when pressure is zero, washing is dry, obtains the fire-retardant expandable polystyrene spherolite containing leafing graphite
CN103819597A disclose one " preparation method of the expandable polystyrene polymer of graphene-containing " due to Hummers method prepare Graphene majority belong to mono-layer graphite, meet during high temperature no longer expanded (interlayer is opened), do not have the flame that suffocates, isolation heat radiation and and the effect such as contact of oxygen, so anti-flaming thermal-insulation performance is still unsatisfactory.Solve the preparation method of existing Graphene poly styrene composite material with Graphene for raw material, thus causing preparation cost height, complex process and the problem being not suitable for large-scale industrial production.
Summary of the invention
The purpose of the present invention is that for above-mentioned the deficiencies in the prior art, it is provided that a kind of high fire-retardance, low heat conduction the expandable polystyrene bead of inflatable few layer graphene;
The preparation method that it is a further object of the present invention to provide the expandable polystyrene bead of a kind of inflatable few layer graphene.
It is an object of the invention to be achieved through the following technical solutions:
The expandable polystyrene bead of inflatable few layer graphene, is be prepared from by mass percentage by following material:
The preparation method of the expandable polystyrene bead of inflatable few layer graphene, comprises the following steps:
A, compound between graphite layers preparation: with mean diameter be 1000-5000 order natural flake graphite for anode, metal titanium sheet is as negative electrode, with concentration be 98% concentrated sulphuric acid for intercalator, electrochemical intercalation is carried out under 1.8V voltage, the intercalation time is 0.5-2.0 hour, prepares compound between graphite layers;
The preparation of B, less layer graphene: above-mentioned compound between graphite layers, in the concentrated sulfuric acid solution that concentration is 98%, is implemented ultrasonic vibration under 1000W power and peeled off 05-1.5 hour, prepare few layer graphene;
C, the inflatable preparation lacking layer graphene: with the concentrated sulphuric acid of concentration 98% for intercalator, the hydrogen peroxide of concentration 30% is oxidant, carry out chemical method secondary intercalation to the few layer graphene of above-mentioned gained at ambient temperature, and the time is 30 minutes.Then, the product water after intercalation it is washed till pH value 4-6 and dries 2 hours at 100 DEG C again, namely preparing inflatable few layer graphene;
D, graphene-containing the preparation of expandable polystyrene bead: mass percent 13.8 17.3% styrene, 0.3 4.0% benzoyl peroxide and 3.5 5.5% inflatable few layer graphenes are put in reactors, mechanical agitation 30min, mixing speed keeps 210~300 revs/min;Put into 0.52 1.1% inorganic dispersant calcium hydroxy phosphate and 0.03 0.05% organic dispersing agent polyvinyl alcohol, when the temperature of charge in reactor rises to 87~90 DEG C, polyreaction 6~11 hours at this temperature;Add 0.2~0.8% calcium hydroxy phosphate and 0.35 0.55% foaming agent, continue reactor is heated;When the temperature of charge in reactor rises to 110~135 DEG C, constant temperature keeps 3~5 hours;Material in reactor taken out and is filtered, obtaining granular material;Dry 1-3 hour by pneumatic drier 30~50 DEG C, obtain the polystyrene bead of graphene-containing.
Beneficial effect: be in the synthesis by inflatable few layer graphene introducing expandable polystyrene, the nanoscale expansible graphite alkene of preparation can be dispersed at expandable polystyrene bead camber, thus ensureing the infrared reflective of cavity inner height at expandable polystyrene, obtaining good heat-proof quality, inflatable few layer graphene can show again the flame that suffocates, completely cut off thermal-radiating flame retardant effect simultaneously.
The polystyrene bead of the graphene-containing present invention prepared carries out foaming process, obtains foam board.Adopt standard GB/T 8624-2006 to carry out flame retardant rating test, adopt national military standard GJB1875-94 to carry out thermal conductivity test.The flame retardant rating of the foam board prepared by the present invention reaches B1 level, and heat conductivity value is 0.028~0.032W/ (m K).
Accompanying drawing illustrates:
Fig. 1 is the shape appearance figure of multilamellar expansible graphite alkene.
Detailed description of the invention
It is described in further detail below in conjunction with drawings and Examples:
The expandable polystyrene bead of inflatable few layer graphene, is be prepared from by mass percentage by following material:
The preparation method of the expandable polystyrene bead of inflatable few layer graphene, comprises the following steps:
A, compound between graphite layers preparation: with mean diameter be 1000-5000 order natural flake graphite for anode, metal titanium sheet is as negative electrode, with concentration be 98% concentrated sulphuric acid for intercalator, electrochemical intercalation is carried out under 1.8V voltage, the intercalation time is 0.5-2.0 hour, prepares compound between graphite layers;
The preparation of B, less layer graphene: above-mentioned compound between graphite layers, in the concentrated sulfuric acid solution that concentration is 98%, is implemented ultrasonic vibration under 1000W power and peeled off 05-1.5 hour, prepare few layer graphene;
C, the inflatable preparation lacking layer graphene: with the concentrated sulphuric acid of concentration 98% for intercalator, the hydrogen peroxide of concentration 30% is oxidant, carry out chemical method secondary intercalation to the few layer graphene of above-mentioned gained at ambient temperature, and the time is 30 minutes.Then, the product water after intercalation it is washed till pH value 4-6 and dries 2 hours at 100 DEG C again, namely preparing inflatable few layer graphene;
D, graphene-containing the preparation of expandable polystyrene bead: mass percent 13.8 17.3% styrene, 0.3 4.0% benzoyl peroxide and 3.5 5.5% inflatable few layer graphenes are put in reactors, mechanical agitation 30min, mixing speed keeps 210~300 revs/min;Put into 0.52 1.1% inorganic dispersant calcium hydroxy phosphate and 0.03 0.05% organic dispersing agent polyvinyl alcohol, when the temperature of charge in reactor rises to 87~90 DEG C, polyreaction 6~11 hours at this temperature;Add 0.2~0.8% calcium hydroxy phosphate and 0.35 0.55% foaming agent, continue reactor is heated;When the temperature of charge in reactor rises to 110~135 DEG C, constant temperature keeps 3~5 hours;Material in reactor taken out and is filtered, obtaining granular material;Dry 1-3 hour by pneumatic drier 30~50 DEG C, obtain the polystyrene bead of graphene-containing.
Embodiment 1
A, compound between graphite layers preparation: with mean diameter be 1000 orders natural flake graphite for anode, metal titanium sheet as negative electrode, with concentration be 98% concentrated sulphuric acid for intercalator, under 1.8V voltage, carry out electrochemical intercalation, the intercalation time is 2.0 hours, prepares compound between graphite layers.
The preparation of B, less layer graphene: above-mentioned compound between graphite layers, in the concentrated sulfuric acid solution that concentration is 98%, is implemented ultrasonic vibration under 1000W power and peeled off 1.5 hours, prepare few layer graphene.
C, the inflatable preparation lacking layer graphene: using the concentrated sulphuric acid of concentration 98% as intercalator, the few layer graphene of above-mentioned gained, as oxidant, is carried out chemical method secondary intercalation by the hydrogen peroxide of concentration 30% at ambient temperature, and the time is 30 minutes.Then, the product water after intercalation it is washed till pH value 6 and dries 2 hours at 100 DEG C again, namely preparing inflatable few layer graphene.
D, graphene-containing the preparation of polystyrene bead: being sequentially added into the solution of 10 grams of styrene monomers in four-hole bottle, the inflatable few layer graphene of 2g, deionized water 45 milliliters, mechanical agitation 30min, mixing speed keeps 210 revs/min.Put into 0.25g inorganic dispersant calcium hydroxy phosphate and 0.025 gram of organic dispersing agent polyvinyl alcohol and benzoyl peroxide 0.17g.When the temperature of charge in reactor rises to 90 DEG C, polyreaction 6 hours at this temperature;Add 0.2g calcium hydroxy phosphate and 0.2g foaming agent again, continue reactor is heated;When the temperature of charge in reactor rises to 110~135 DEG C, constant temperature keeps 3~5 hours;Material in reactor taken out and is filtered, obtaining granular material;Dried 3 hours by pneumatic drier 30 DEG C, obtain the polystyrene bead of graphene-containing.
Embodiment 2
A, compound between graphite layers preparation: with mean diameter be 3000 orders natural flake graphite for anode, metal titanium sheet as negative electrode, with concentration be 98% concentrated sulphuric acid for intercalator, under 1.8V voltage, carry out electrochemical intercalation, the intercalation time is 1.0 hours, prepares compound between graphite layers.
The preparation of B, less layer graphene: above-mentioned compound between graphite layers, in the concentrated sulfuric acid solution that concentration is 98%, is implemented ultrasonic vibration under 1000W power and peeled off 1.0 hours, prepare few layer graphene.
C, the inflatable preparation lacking layer graphene: using the concentrated sulphuric acid of concentration 98% as intercalator, the few layer graphene of above-mentioned gained, as oxidant, is carried out chemical method secondary intercalation by the hydrogen peroxide of concentration 30% at ambient temperature, and the time is 30 minutes.Then, the product water after intercalation it is washed till pH value 5 and dries 2 hours at 100 DEG C again, namely preparing inflatable few layer graphene.
D, graphene-containing the preparation of polystyrene bead: being sequentially added into the solution of 10 grams of styrene monomers in four-hole bottle, the inflatable few layer graphene of 3g, deionized water 50 milliliters, mechanical agitation 30min, mixing speed keeps 250 revs/min.Put into 0.35g inorganic dispersant calcium hydroxy phosphate and 0.025 gram of organic dispersing agent polyvinyl alcohol and benzoyl peroxide 2.0g.When the temperature of charge in reactor rises to 90 DEG C, polyreaction 7 hours at this temperature;Add 0.2g calcium hydroxy phosphate and 0.3g foaming agent again, continue reactor is heated;When the temperature of charge in reactor rises to 115 DEG C, constant temperature keeps 4 hours;Material in reactor taken out and is filtered, obtaining granular material;Dried 2 hours by pneumatic drier 40 DEG C, obtain the polystyrene bead of graphene-containing.
Embodiment 3
A, compound between graphite layers preparation: with mean diameter be 5000 orders natural flake graphite for anode, metal titanium sheet as negative electrode, with concentration be 98% concentrated sulphuric acid for intercalator, under 1.8V voltage, carry out electrochemical intercalation, the intercalation time is 0.5 hour, prepares compound between graphite layers.
The preparation of B, less layer graphene: above-mentioned compound between graphite layers, in the concentrated sulfuric acid solution that concentration is 98%, is implemented ultrasonic vibration under 1000W power and peeled off 0.5 hour, prepare few layer graphene.
C, the inflatable preparation lacking layer graphene: using the concentrated sulphuric acid of concentration 98% as intercalator, the few layer graphene of above-mentioned gained, as oxidant, is carried out chemical method secondary intercalation by the hydrogen peroxide of concentration 30% at ambient temperature, and the time is 30 minutes.Then, the product water after intercalation it is washed till pH value 4 and dries 2 hours at 100 DEG C again, namely preparing inflatable few layer graphene.
D, graphene-containing the preparation of polystyrene bead: being sequentially added into the solution of 10 grams of styrene monomers in four-hole bottle, the inflatable few layer graphene of 4g, deionized water 55 milliliters, mechanical agitation 30min, mixing speed keeps 280 revs/min.Put into 0.4g inorganic dispersant calcium hydroxy phosphate and 0.03 gram of organic dispersing agent polyvinyl alcohol and benzoyl peroxide 2.3g.When the temperature of charge in reactor rises to 90 DEG C, polyreaction 7 hours at this temperature;Add 0.2g calcium hydroxy phosphate and 0.4g foaming agent again, continue reactor is heated;When the temperature of charge in reactor rises to 115 DEG C, constant temperature keeps 4 hours;Material in reactor taken out and is filtered, obtaining granular material;Dried 1 hour by pneumatic drier 50 DEG C, obtain the polystyrene bead of graphene-containing.
Claims (2)
1. the expandable polystyrene bead of an inflatable few layer graphene, it is characterised in that be prepared from by mass percentage by following material:
2. the preparation method of the expandable polystyrene bead of an inflatable few layer graphene, it is characterised in that comprise the following steps:
A, compound between graphite layers preparation: with mean diameter be 1000-5000 order natural flake graphite for anode, metal titanium sheet is as negative electrode, with concentration be 98% concentrated sulphuric acid for intercalator, electrochemical intercalation is carried out under 1.8V voltage, the intercalation time is 0.5-2.0 hour, prepares compound between graphite layers;
The preparation of B, less layer graphene: above-mentioned compound between graphite layers, in the concentrated sulfuric acid solution that concentration is 98%, is implemented ultrasonic vibration under 1000W power and peeled off 05-1.5 hour, prepare few layer graphene;
C, the inflatable preparation lacking layer graphene: with the concentrated sulphuric acid of concentration 98% for intercalator, the hydrogen peroxide of concentration 30% is oxidant, carry out chemical method secondary intercalation to the few layer graphene of above-mentioned gained at ambient temperature, and the time is 30 minutes.Then, the product water after intercalation it is washed till pH value 4-6 and dries 2 hours at 100 DEG C again, namely preparing inflatable few layer graphene;
D, graphene-containing the preparation of expandable polystyrene bead: mass percent 13.8 17.3% styrene, 0.3 4.0% benzoyl peroxide and 3.5 5.5% inflatable few layer graphenes are put in reactors, mechanical agitation 30min, mixing speed keeps 210~300 revs/min;Put into 0.52 1.1% inorganic dispersant calcium hydroxy phosphate and 0.03 0.05% organic dispersing agent polyvinyl alcohol, when the temperature of charge in reactor rises to 87~90 DEG C, polyreaction 6~11 hours at this temperature;Add 0.2~0.8% calcium hydroxy phosphate and 0.35 0.55% foaming agent, continue reactor is heated;When the temperature of charge in reactor rises to 110~135 DEG C, constant temperature keeps 3~5 hours;Material in reactor taken out and is filtered, obtaining granular material;Dry 1-3 hour by pneumatic drier 30~50 DEG C, obtain the polystyrene bead of graphene-containing.
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CN106519091A (en) * | 2016-10-31 | 2017-03-22 | 无锡云亭石墨烯技术有限公司 | Oily modified graphene slurry and use thereof |
CN106519300A (en) * | 2016-10-31 | 2017-03-22 | 无锡云亭石墨烯技术有限公司 | Preparation and application method for water-based modified graphene slurry |
CN106543475A (en) * | 2016-10-31 | 2017-03-29 | 无锡云亭石墨烯技术有限公司 | A kind of preparation of modified graphene and its application in expandable polystyrene |
CN106633458A (en) * | 2016-12-29 | 2017-05-10 | 吉林省云亭节能技术有限公司 | Preparation method of low-heat-conductivity and flame-retardant graphene expanding polystyrene board |
CN106674783A (en) * | 2016-12-29 | 2017-05-17 | 吉林省云亭节能技术有限公司 | Preparation method of high-strength graphene expandable polystyrene board |
CN106752116A (en) * | 2016-11-15 | 2017-05-31 | 吉林省云亭节能技术有限公司 | The preparation method and modified graphene oxide EPS of modified graphene oxide mold the preparation method of styrofoam |
CN107337750A (en) * | 2017-05-17 | 2017-11-10 | 无锡兴达泡塑新材料股份有限公司 | A kind of expandable poly-styrene and preparation method thereof |
CN107442775A (en) * | 2017-07-14 | 2017-12-08 | 成都新柯力化工科技有限公司 | A kind of grapheme foam aluminum composite metal material and preparation method |
CN107987410A (en) * | 2017-11-29 | 2018-05-04 | 吉林云亭石墨烯技术股份有限公司 | A kind of preparation of graphene EPS master batches and the method for compound EPS |
CN109082018A (en) * | 2018-07-25 | 2018-12-25 | 无锡云亭石墨烯技术有限公司 | A kind of elastic graphite alkene EPS and preparation method thereof |
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CN106674783A (en) * | 2016-12-29 | 2017-05-17 | 吉林省云亭节能技术有限公司 | Preparation method of high-strength graphene expandable polystyrene board |
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