CN109735016A - Poly styrene composite material, thermal insulation material and preparation method - Google Patents
Poly styrene composite material, thermal insulation material and preparation method Download PDFInfo
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- CN109735016A CN109735016A CN201811536703.0A CN201811536703A CN109735016A CN 109735016 A CN109735016 A CN 109735016A CN 201811536703 A CN201811536703 A CN 201811536703A CN 109735016 A CN109735016 A CN 109735016A
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Abstract
The present invention relates to a kind of preparation methods of poly styrene composite material, the following steps are included: graphene dispersing solution is mixed with styrene, dispersing agent, initiator, the poly styrene composite material is obtained in 60~100 DEG C of progress polymerization reactions, the percentage that the graphene quality in the graphene dispersing solution accounts for the styrene quality is 0.1~2%.Thermal insulation material made of after the poly styrene composite material synthesized the preparation method is foamed, thermal coefficient is up to 0.027 ± 0.01W (mK)‑1, flame retardant rating reaches GB8624-2012B1 rank.
Description
Technical field
The present invention relates to field of material technology, more particularly to poly styrene composite material, thermal insulation material and preparation method.
Background technique
Expanded polystyrene (EPS) (styrofoam or EPS) has the small (1.05g/cm of relative density3), thermal conductivity it is low, moisture-proof etc. excellent
Point, and because of lower production costs, expanded polystyrene (EPS) is widely used in thermal insulation material.But due to expanded polystyrene (EPS)
Inflammable characteristic is applied to thermal insulation material after need to usually promoting the flame retardant property of expanded polystyrene (EPS) again.
And graphene is all very excellent inorganic nano material of a kind of mechanics, electric property, its Young mould at normal temperature
Amount is up to 1.0TPa, and breaking strength is up to 130GPa, and electron mobility is more than 1500cm2/ Vs, resistivity are about 10-8Ω·
M, these special performances become the ideal nanoscale fillers of polymer modification.Therefore, graphene can be used for modified poly-
The flame retardant property of styrene, modified polystyrene pass through foaming again, and flame retardant property can be obviously improved.
But common polystyrene composite graphite alkene polymerization is made composite material, and preparation process is cumbersome and poly- after foaming
Benzene composite material fire-proof and thermal-insulation effect is undesirable, its application is made to be restricted.
Summary of the invention
Based on this, it is necessary to which, for disadvantage present in above-mentioned preparation method, the embodiment provides a kind of letters
It is single, reaction condition is mild and the poly styrene composite material preparation method that can be continuously produced, the polyphenyl of preparation method production
Thermal insulation material is used as after ethylene composite material is foamed, the thermal insulation material is fire-retardant to can reach GB8624-2012B1 rank, and heat-insulated
It has excellent performance.
A kind of preparation method of poly styrene composite material, comprising the following steps:
Graphene dispersing solution is mixed with styrene, dispersing agent, initiator, is obtained in 60 DEG C~100 DEG C progress polymerization reactions
To the poly styrene composite material, the graphene quality in the graphene dispersing solution accounts for the percentage of the styrene quality
It is 0.1%~2%.
Further, the graphene dispersing solution is that ultrasonic disperse is made graphene in a solvent, ultrasonic time 1min
~10min, ultrasonic power are 100w~3000w.
Further, the solvent in the graphene dispersing solution is water, in N-Methyl pyrrolidone, dimethylbenzene, ethyl alcohol
At least two, and the mass ratio of the graphene and the solvent is (3-5): 100.
Further, the polymerization reaction is 200rpm~3000rpm progress with mixing speed.
Further, the dispersing agent in the polymerization reaction be polyvinyl alcohol, hydroxymethyl cellulose, in tricalcium phosphate extremely
Few one kind, the dispersing agent quality are the 0.1%~15% of the styrene quality.
Further, when the dispersing agent that the polymerization reaction is added includes tricalcium phosphate, may be used also in the polymerization reaction
Surfactant is added, the surfactant is at least one of stearic acid, neopelex, and the surface is living
Dynamic agent quality is the 0.1%~1% of the styrene quality.
Further, the initiator be dibenzoyl peroxide, cumyl peroxide, in azodiisobutyronitrile extremely
Few one kind, the initiator quality are the 0.1%~15% of the styrene quality.
Further, the polymerization reaction time is 6h~10h.
A kind of preparation method for poly styrene composite material that the embodiment of the present invention provides, the preparation method is due to technique
Simply, reaction condition is mild and can be continuously produced, large-scale production easy to accomplish.
The embodiment of the present invention also provides a kind of poly styrene composite material, and the poly styrene composite material is by above-mentioned
Any one method is prepared.The poly styrene composite material polymerize instead with styrene by the way that graphene dispersing solution is added
Answer, and under the synergistic effect of dispersing agent, initiator and surfactant so that graphene uniform be dispersed in finally polymerize it is poly-
In benzene composite material.
The embodiment of the present invention also provides a kind of thermal insulation material, which is sent out by above-mentioned poly styrene composite material
Brewed, and the thermal coefficient of the thermal insulation material reaches 0.027 ± 0.01W (mK)-1, the thermal coefficient of the thermal insulation material compared with
The thermal coefficient low 10%~15% of domestic excellent styrofoam.The thermal insulation material since graphene uniform is dispersed therein so that
Graphene forms one or more layers " protecting wall " in the thermal insulation material and plays trap heat (in the continuous phase of polystyrene)
The effect distributed.In addition, the thermal insulation material due to the lamellar structure of graphene itself densification of dispersed phase cause heat transfer by
Resistance reaches GB8624-2012B1 rank so that the thermal insulation material flame-retarding characteristic is promoted.
Detailed description of the invention
Fig. 1 is the scanning electron microscope (SEM) photograph (SEM) of poly styrene composite material made from the embodiment of the present invention.
Specific embodiment
Poly styrene composite material provided by the invention, thermal insulation material and preparation method will be described further below.
The preparation method of poly styrene composite material provided by the invention the following steps are included:
S1 mixes graphene dispersing solution with styrene, dispersing agent, initiator and surfactant, at 60 DEG C~100 DEG C
It carries out polymerization reaction and obtains the poly styrene composite material, the graphene quality in the graphene dispersing solution accounts for the benzene second
The percentage of alkene quality is 0.1%~2%.
Specifically, the graphene dispersing solution in step S1 is that ultrasonic disperse is made graphene in a solvent, and ultrasonic time is
1min~10min, ultrasonic power are 100w~3000w, which makes graphene uniform dispersion in a solvent.
Specifically, the solvent in the graphene dispersing solution in step S1 be water, N-Methyl pyrrolidone (NMP), dimethylbenzene,
At least two in ethyl alcohol, and the mass ratio of graphene and solvent is (3-5): 100, since benzene second can be added in graphene dispersing solution
Polymerization reaction is carried out in alkene, therefore the accounting of the graphene and solvent in graphene dispersing solution must control in a certain range,
Otherwise the dispersion effect that graphene is very few or the very few influence graphene of solvent is in thermal insulation material, so that thermal insulation material
Thermal coefficient and anti-flammability are bad.
Specifically, it is compound that common graphene product progress may be selected in above-mentioned graphene.It is also possible to modified graphite
Alkene.Modified graphene includes the one of which of watersoluble plumbago alkene, oiliness graphene, functionalization graphene, it is preferable that Neng Gou
Well dispersed functionalization graphene in organic solvent.
Specifically, polymerization reaction is 200rpm~3000rpm progress with mixing speed, and polymerization reaction is suspension polymerisation, is stirred
The effect mixed is the molecular weight that polymerisation of liquid droplets was fused together and influenced polymerization efficiency and product in order to prevent.
Specifically, dispersing agent is polyvinyl alcohol (PVA), hydroxymethyl cellulose (HEC), tricalcium phosphate (TCP) in step S1
At least one of, dispersing agent quality is the 0.1~15% of the styrene quality, and the effect of dispersing agent is to further protect
The independence for protecting polymerisation of liquid droplets, prevents the fusion between polymerisation of liquid droplets.
Specifically, polymerization reaction is carried out in order to cause styrene monomer, the initiator being added in step sl is peroxidating
Dibenzoyl (BPO), cumyl peroxide (DCP), in azodiisobutyronitrile (AIBN) at least one, initiator quality is
The 0.1%~15% of styrene quality.
Specifically, when the dispersing agent that the polymerization reaction is added includes tricalcium phosphate, table can also be added in polymerization reaction
Face activating agent, surfactant are at least one of stearic acid, neopelex (SDBS), surface activity agent quality
It is the 0.1~1% of the styrene quality.The effect of surfactant is the surface for soaking tricalcium phosphate, reduces the surface of water
Tension plays preferably isolation and protective effect.
Specifically, the polymerization reaction time of step S1 is 6h~10h.It is anti-in polymerization for the terminal for further determining that reaction
During answering, part reaction solution is taken to be cooled to, if reaction solution after cooling forms crisp and hard particle, polymerization reaction knot
Beam, cooling reaction solution, and isolate product.
A kind of preparation method for poly styrene composite material that the embodiment of the present invention provides, the preparation method is due to technique
Simply, reaction condition is mild and can be continuously produced, and can be applied to industrialized large-scale production.
The embodiment of the present invention also provides a kind of poly styrene composite material, and the poly styrene composite material is by above-mentioned any
One method is prepared.
The poly styrene composite material carries out polymerization reaction by the way that graphene dispersing solution and styrene is added, and is dispersing
Under the synergistic effect of agent, initiator and surfactant, so as to be dispersed in the polystyrene finally polymerizeing compound for graphene uniform
In material.
The present invention also provides a kind of thermal insulation material, which is foamed by above-mentioned poly styrene composite material and is made,
The thermal coefficient of the thermal insulation material reaches 0.027 ± 0.01W (mK)-1.The thermal coefficient of the thermal insulation material is more domestic excellent
The low 10%-15% of the thermal coefficient of styrofoam.Above-mentioned thermal insulation material is since graphene uniform is dispersed therein, so that graphene
One or more layers " protecting wall " is formed (in the continuous phase of polystyrene) in the thermal insulation material and plays what trap heat distributed
Effect.In addition, the thermal insulation material is since the lamellar structure of graphene itself densification of dispersed phase causes heat transfer to be obstructed, in turn
So that the thermal insulation material flame-retarding characteristic is promoted, reach GB8624-2012 B1Rank.
Hereinafter, following specific embodiments will be passed through to above-mentioned poly styrene composite material, thermal insulation material and preparation method
It is described further.
Poly styrene composite material in following embodiment is foamed by pentane, and thermal insulation material is made and carries out phase
Thermal coefficient and the flame retardant rating test answered.
Poly styrene composite material is the form of pellet before foaming.Wherein, poly- containing foaming agent in foaming process
Benzene composite material pellet can't foam before 80 DEG C, the hair being simply present in poly styrene composite material pellet
Infusion will not also be expanded to external diffusion, at this time poly styrene composite material bead formation.When temperature is greater than 80 DEG C, polystyrene is multiple
The pellet of condensation material starts to soften, and the foaming agent for being distributed in poly styrene composite material pellet interior is heated, and vaporization generates steam
Pressure causes the pellet of poly styrene composite material to start to expand and formed mutual disconnected abscess.Meanwhile steam pressure also seeps
Enter into these abscesses, increases gross pressure in hole.Over time, steam pressure deepens continuously, and pressure also constantly increases
Greatly, the volume of poly styrene composite material pellet also constantly increases, this process is sustained, and volume expansion can maintain
Until the rupture of abscess thin-walled.(wherein foaming agent is pentane, is heated to the pellet softening of poly styrene composite material until being formed
Abscess simultaneously constantly expands whole process maturing process).
Embodiment 1:
(1) 30g graphene powder is added in 500g water and 500gNMP, ultrasonic disperse 5min, 3% graphite is made
Alkene dispersion liquid;
(2) 1800g deionized water is added in 5L reaction kettle, 9gPVA is warming up to 90 DEG C, stirs with the speed of 200rpm
1000g deionized water is added after 1h, and is cooled to 60 DEG C of first reaction solutions of formation;
(3) it takes 30g graphene dispersing solution, be added in the first reaction solution in 9gBPO and 900g styrene, continue to stir 1h,
85 DEG C of reaction 1h are warming up to, then are warming up to 90 DEG C of reaction 5h, to cooling 60 DEG C or so the taking-up products of reaction solution;
(4) products therefrom is washed with deionized, then filters and dry, obtains poly styrene composite material.
Fig. 1 is the scanning electron microscope (SEM) photograph after the poly styrene composite material foaming in embodiment 1, clearly shows that graphite in the figure
Alkene laminated structure is compound into polystyrene, forms poly styrene composite material.
Embodiment 2:
(1) 30g graphene powder is added in 500g dimethylbenzene and 500g ethyl alcohol, ultrasonic disperse 5min, is made 3%
Graphene dispersing solution;
(2) 1800g deionized water, 4.5gTCP, 0.9gSDBS and 4.5gPVA are added in 5L reaction kettle, is warming up to 90
DEG C, 1000g deionized water is added after stirring 1h with the speed of 500rpm, reaction solution is cooled to 60 DEG C of first reaction solutions of formation;
(3) 30g graphene dispersing solution, 4.5gDCP, 4.5gBPO and 900g styrene is taken to be added in the first reaction solution, with
The speed of 500rpm continues to stir 1h, is warming up to 65 DEG C of reaction 1h, then be warming up to 90 DEG C of reaction 5h, to the cooling 60 DEG C of left sides of reaction solution
Right taking-up product;
(4) products therefrom is washed with deionized, then filters and dry, obtains poly styrene composite material.
Embodiment 3:
(1) 30g graphene powder is added in 500g water and 500gNMP, ultrasonic disperse 5min, 3% graphite is made
Alkene dispersion liquid;
(2) 1800g deionized water, 4.5gTCP, 0.9g stearic acid and 4.5gHEC are added in 5L reaction kettle, is warming up to 90
DEG C, after stirring 1h with the speed of 1000rpm, 1000g deionized water is added and reaction solution is made to be cooled to the first reaction of 60 DEG C of formation
Liquid;
(3) 30g graphene dispersing solution, 4.5gDCP, 4.5gAIBN and 900g styrene is taken to be added in the first reaction solution, with
The mixing speed of 1000rpm continues to stir 1h, is warming up to 65 DEG C of reaction 1h, then be warming up to 73 DEG C of reaction 5h, cooling to reaction solution
60 DEG C or so taking-up products;
(4) products therefrom is washed with deionized, then filters and dry, obtains poly styrene composite material.
Embodiment 4:
(1) 30g graphene powder is added in 500g water and 500gNMP, ultrasonic disperse 5min, 3% graphite is made
Alkene dispersion liquid;
(2) 1800g deionized water is added in 5L reaction kettle, 67.5gPVA stirs 1h in 90 DEG C of speed with 1500rpm
Afterwards, 1000g deionized water is added makes reaction solution be cooled to 60 DEG C of first reaction solutions of formation;
(3) 300g graphene dispersing solution is taken, 67.5gBPO is dissolved in 900g styrene and is added in the first reaction solution, with
The mixing speed of 1500rpm stirs 1h, is warming up to 85 DEG C of reaction 1h, then be warming up to 90 DEG C of reaction 5h, 60 DEG C cooling to reaction solution
Take out product in left and right;
(4) products therefrom is washed with deionized, then filters and dry, obtains poly styrene composite material.
Embodiment 5:
(1) 30g graphene powder is added in 500g dimethylbenzene and 500g ethyl alcohol, ultrasonic disperse 5min, is made 3%
Graphene dispersing solution;
(2) 1800g deionized water, 33.75gTCP, 4.5gSDBS and 33.75gPVA are added in 5L reaction kettle, at 90 DEG C
After stirring 1h with the speed of 2500rpm, 1000g deionized water, which is added, makes reaction solution be cooled to 60 DEG C of first reaction solutions of formation;
(3) take 300g graphene dispersing solution, 33.75gDCP, 33.75gBPO and 900g styrene that the first reaction solution is added
In, 1h is stirred with the mixing speed of 2500rpm, is warming up to 65 DEG C of reaction 1h, then be warming up to 90 DEG C of reaction 5h, it is cooling to reaction solution
60 DEG C or so taking-up products;
(4) products therefrom is washed with deionized, then filters and dry, obtains poly styrene composite material.
Embodiment 6:
(1) 30g graphene powder is added in 500g water and 500gNMP, ultrasonic disperse 5min, 3% graphite is made
Alkene dispersion liquid;
(2) 1800g deionized water, 33.75gTCP, 4.5g stearic acid and 33.75gHEC, heating are added in 5L reaction kettle
Addition 1000g deionized water is cooled to 60 DEG C and forms first instead after being completely dissolved PVA to 90 DEG C of speed stirring 1h with 3000rpm
Answer liquid;
(3) take 30g graphene dispersing solution, 33.75gDCP, 33.75gAIBN and 900g styrene that the first reaction solution is added
In, 1h is stirred with the mixing speed of 3000rpm, is warming up to 65 DEG C of reaction 1h, then be warming up to 73 DEG C of reaction 5h, it is cooling to reaction solution
60 DEG C or so taking-up products;
(4) products therefrom is washed with deionized, then filters and dry, obtains poly styrene composite material.
Embodiment 7:
(1) 50g graphene powder is added in 500g water and 500gNMP, ultrasonic disperse 10min, 5% graphite is made
Alkene dispersion liquid;
(2) 1800g deionized water, 135gPVA are added in 5L reaction kettle, is warming up to 90 DEG C of speed with 500rpm and stirs
After 1h, 1000g deionized water, which is added, makes reaction solution be cooled to 60 DEG C of first reaction solutions of formation;
(3) 360g graphene dispersing solution, 135gBPO and 900g styrene is taken to be added in the first reaction solution, with 3000rpm's
Speed continues to stir 1h, is warming up to 85 DEG C of reaction 1h, then be warming up to 90 DEG C of reaction 8h, produces to cooling 60 DEG C or so the taking-ups of reaction solution
Object;
(4) products therefrom is washed with deionized, then filters and dry, obtains poly styrene composite material.
Embodiment 8:
(1) 50g graphene powder is added in 500g dimethylbenzene and 500g ethyl alcohol, ultrasonic disperse 10min, is made 5%
Graphene dispersing solution;
(2) 1800g deionized water, 67.5gTCP, 9.0g stearic acid and 67.5gPVA are added in 5L reaction kettle, is warming up to
90 DEG C and with the speed of 1500rpm stir 1h after, be added 1000g deionized water make reaction solution be cooled to 60 DEG C formed first reaction
Liquid;
(3) 360g graphene dispersing solution, 67.5gDCP, 67.5gBPO and 900g styrene is taken to be added in the first reaction solution,
1h is stirred with the speed of 1500rpm, is warming up to 85 DEG C of reaction 1h, then be warming up to 90 DEG C of reaction 8h, to the cooling 60 DEG C of left sides of reaction solution
Right taking-up product;
(4) products therefrom is washed with deionized, then filters and dry, obtains poly styrene composite material.
Embodiment 9:
(1) 50g graphene powder is added in 500g water and 500gNMP, ultrasonic disperse 10min, 6% graphite is made
Alkene dispersion liquid;
(2) in 5L reaction kettle be added 1800g deionized water, 67.5gTCP, 9.0gSDBS and 67.5gHEC, 90 DEG C with
After the speed stirring 1h of 3000rpm, 1000g deionized water, which is added, makes reaction solution be cooled to 60 DEG C of first reaction solutions of formation;
(3) 360g graphene dispersing solution, 67.5gAIBN, 67.5gBPO and 900g styrene is taken to be added in the first reaction solution,
1h is stirred with the speed of 3000rpm, is warming up to 65 DEG C of reaction 1h, then be warming up to 73 DEG C of reaction 8h, to the cooling 60 DEG C of left sides of reaction solution
Right taking-up product;
(4) products therefrom is washed with deionized, then filters and dry, obtains poly styrene composite material.
Comparative example:
(1) in 5L reaction kettle be added 1800g deionized water, 67.5gTCP, 9.0gSDBS and 67.5gHEC, 90 DEG C with
After the speed stirring 1h of 3000rpm, 1000g deionized water, which is added, makes reaction solution be cooled to 60 DEG C of first reaction solutions of formation;
(2) it takes 67.5gAIBN, 67.5gBPO and 900g styrene to be added in the first reaction solution, is stirred with the speed of 3000rpm
1h is mixed, 65 DEG C of reaction 1h are warming up to, then is warming up to 73 DEG C of reaction 8h, to cooling 60 DEG C or so the taking-up products of reaction solution;
(3) products therefrom is washed with deionized, then filters and dry, obtains poly styrene composite material.
The performance of heat protective material of 1~embodiment of embodiment 9 is tested, test result is as shown in table 1.
Table 1
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, 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, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and 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 protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (10)
1. a kind of preparation method of poly styrene composite material, which comprises the following steps:
Graphene dispersing solution is mixed with styrene, dispersing agent, initiator, is obtained in 60~100 DEG C of progress polymerization reactions described
Poly styrene composite material, the percentage that the graphene quality in the graphene dispersing solution accounts for the styrene quality are
0.1%~2%.
2. the preparation method of poly styrene composite material according to claim 1, which is characterized in that the graphene dispersion
Liquid is that ultrasonic disperse is made graphene in a solvent, and ultrasonic time is 1~10min, and ultrasonic power is 100w~3000w.
3. the preparation method of poly styrene composite material according to claim 1, which is characterized in that the graphene dispersion
Solvent in liquid is water, N-Methyl pyrrolidone, dimethylbenzene, at least two in ethyl alcohol, and the graphene and the solvent
Mass ratio be (3-5): 100.
4. the preparation method of poly styrene composite material according to claim 1, which is characterized in that the polymerization reaction with
Mixing speed is 200rpm~3000rpm progress.
5. the preparation method of poly styrene composite material according to claim 1, which is characterized in that in the polymerization reaction
Dispersing agent be at least one of polyvinyl alcohol, hydroxymethyl cellulose, tricalcium phosphate, the dispersing agent quality be the benzene second
The 0.1%~15% of alkene quality.
6. the preparation method of poly styrene composite material according to claim 5, which is characterized in that when the addition polymerization
When the dispersing agent of reaction includes tricalcium phosphate, surfactant can also be added in the polymerization reaction, the surfactant is
At least one of stearic acid, neopelex, the surface activity agent quality are the 0.1% of the styrene quality
~1%.
7. the preparation method of poly styrene composite material according to claim 1, which is characterized in that the initiator was
At least one of dibenzoyl, cumyl peroxide, azodiisobutyronitrile are aoxidized, the initiator quality is the benzene second
The 0.1%~15% of alkene quality.
8. the preparation method of poly styrene composite material according to claim 1, which is characterized in that when the polymerization reaction
Between be 6h~10h.
9. a kind of poly styrene composite material, which is characterized in that the poly styrene composite material is any by such as claim 1-8
One method is prepared.
10. a kind of thermal insulation material, which is characterized in that the thermal insulation material is by poly styrene composite material as claimed in claim 9
Foaming is made, and the thermal coefficient of the thermal insulation material reaches 0.027 ± 0.01W (mK)-1。
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CN116023672A (en) * | 2022-12-15 | 2023-04-28 | 江阴市星宇化工有限公司 | Composite filler of tricalcium phosphate special for polymerization and preparation method thereof |
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