CN107337750B - A kind of expandable poly-styrene and preparation method thereof - Google Patents
A kind of expandable poly-styrene 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
- 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
- C08F112/06—Hydrocarbons
- C08F112/08—Styrene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/14—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent organic
- C08J9/141—Hydrocarbons
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2203/00—Foams characterized by the expanding agent
- C08J2203/14—Saturated hydrocarbons, e.g. butane; Unspecified hydrocarbons
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2325/00—Characterised by the use of homopolymers or copolymers 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; Derivatives of such polymers
- C08J2325/02—Homopolymers or copolymers of hydrocarbons
- C08J2325/04—Homopolymers or copolymers of styrene
- C08J2325/06—Polystyrene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/006—Additives being defined by their surface area
Abstract
The invention discloses a kind of expandable poly-styrenes and preparation method thereof, wherein in the expandable poly-styrene, the amount of institute's containing graphene accounts for the 0.2wt%-1wt% for polymerizeing preceding styrene monomer total weight.Expandable poly-styrene pressing plate molding prepared by the present invention, obtains foam board.The flame retardant rating of foam board is up to B1 grades, and heat conductivity value is reduced to 0.030~0.034W/ (mK) by original 0.039~0.042W/ (mK), and drawing property is increased to 260Kpa by original 90Kpa.
Description
Technical field
The present invention relates to a kind of expandable poly-styrene and preparation method thereof, in particular to a kind of to compound with graphene
Polystyrol foam material and preparation method thereof, belong to high molecular polymer field.
Background technique
Expandable poly-styrene (EPS) is that have thermally conductive system using a kind of foamed material of physical blowing means preparation
The advantages that number is low, electrical insulating property is good, water absorption rate is low, sound insulation value is superior, antidetonation, simple moisture-proof and moulding process, therefore quilt
It is widely used in acoustic material, packing and thermal insulation material, especially in building heat preservation field, expandable poly-styrene has
Extraordinary application prospect plays the role of energy-saving and environment-friendly.
From 1949, German BASF developed the history that expandable poly-styrene has more than 60 years so far, merely
The performance of EPS be no longer satisfied the growing life and production requirement of modern society, therefore further increase the property of EPS
Can, it is most important to expand its application field.Future, EPS will be in mechanical property, flame retardant property, ageing-resistant performance and antistatics
Performance is improved, therefore the study on the modification of EPS and application study are of great significance to the development of social economy.
CN101891852A discloses a kind of " preparation of polystyrene/expanded graphite composite foaming material ", styrene 90-
110 parts, 5-10 parts of 200-500 mesh expanded graphite, 4-6 parts of nano-aluminum hydroxide, 0.3-0.5 parts of coupling agent, diphenyl peroxide first
0.1-1 parts of acyl, 0.1-0.5 parts of cumyl peroxide, 0.1-0.3 parts of polyvinyl alcohol, 1-2 parts of tricalcium phosphate, white oil 0.3-0.8
Part, 0.3-0.8 parts of polyethylene wax, 0.1-0.3 parts of stearic acid, 9-11 parts of pentane.Prepare the expandable polyphenyl second of above-mentioned flame retardant type
The method of alkene particle, comprising the following steps: (1) 0.3-0.8 parts of white oils, 0.3- are added in 90-110 parts of styrene monomer
0.8 part of polyethylene wax, 5-10 parts of expanded graphites and 4-6 parts of nano-aluminum hydroxides, 0.8-1.2 parts of coupling agents, are stirred until homogeneous；
(2) after, it is added 0.1-1 parts of dibenzoyl peroxide and 0.1-5 parts of cumyl peroxide initiators, after uniform stirring,
85 DEG C of progress pre-polymerizations are warming up to, obtain styrene/expanded graphite performed polymer, for use；(3) 90-110 parts are added in reaction kettle
Deionized water；(4) while uniform stirring, 0.1-0.3 parts of polyvinyl alcohol, 1-2 parts of calcium triphosphates is sequentially added, continue to stir
3-8 minutes；(5) after, the performed polymer that step (1) obtains is added in above-mentioned water phase, under 400-500 revs/min of revolving speed
Stirring；(6) after, when system is warming up to 90 DEG C, constant temperature is kept for 4-6 hours, and material is made to form with a certain size distribution
Grain；(7) after, pentane is added, and continues to heat reaction system.But when reacting kettle inner pressure reaches 0.9-1MPa, keep
0.5-2 hours.Then, it is allowed to naturally cool to room temperature；(8) finally, filtering off moisture, flame retardant type expandable poly-styrene is obtained
Compound particle.Graphite partial size used in this patented technology is larger (30-75um), it is not easy to be wrapped in styrene suspension particle
In, in addition, mechanical performance cannot be guaranteed under the premise of low thermal conductivity.Also, technique is extremely complex, at high cost, is difficult really
Industrial application.
On this basis, since graphene is born, people just begin one's study and replace graphite with graphene.Graphene conduct
A kind of new nano material, since being found just with excellent optical property, thermal property, mechanical property, magnetic performance with
And good chemical stability is extensively studied.Theoretically, graphene be polymer composites preferably enhance and
Functional material.But it in actual progress, is but rebuffed repeatedly.Although graphene possesses the excellent property such as single layer, conduction
Can, but itself is there is also intrinsic disadvantage, is difficult it in conjunction with other materials in application process, it is not easy to disperse,
Hinder the performance of its performance.
So far, be compounded in the EPS material technology of graphene it is close at first be CN105732860A disclose one
Kind " the expandable poly-styrene bead and preparation method of inflatable few layer graphene ".It uses the method for electrochemistry to graphite
Electrochemical intercalation is carried out, ultrasonic vibration is carried out to it, secondary intercalation is carried out to it again later, washes, is dried to obtain inflatable lack
Layer graphene.In the technology, graphene preparation process is more complex, and additive amount is more (3.5wt%-5.5wt%), at high cost, and
And the dispersibility in styrene is bad, improvement is not satisfactory.
Summary of the invention
It is an object of the invention in view of the above technical defects, provide, a kind of graphene additive amount is small, performance is more superior
Compound expandable poly-styrene；
It is a further object of the present invention to provide the preparation methods of above-mentioned material.
The purpose of the present invention is achieved by the following technical scheme:
A kind of expandable poly-styrene, the amount of institute's containing graphene account for the 0.2wt%- for polymerizeing preceding styrene monomer total weight
1wt%.
Preferably, the amount of institute's containing graphene, which accounts for, polymerize the 0.3% of preceding styrene monomer total weight.
The preparation method of above-mentioned expandable poly-styrene,
Include the following steps:
S1: first styrene, water, dispersing agent and graphene are mixed, stirs in a kettle, forms uniform suspension；
S2: will be added low temperature initiators in S1 uniformly mixed material, be warming up to 50-70 DEG C, high-temperature initiator is added, then
When being warming up to 88-92 DEG C, dispersing agent is added, after isothermal reaction 5-8h, adds foaming agent, temperature is permanent after rising to 105-130 DEG C
Warm 2-6h, end of reaction；
S3: by the material in reaction kettle take out filtering, it is dry to get.
Preferably, in the S1, water, styrene mass ratio be (1.5-3): 1, such as: 1.5:1,1.6:1,1.7:1,
1.8:1,1.9:1,2:1,2.2:1,2.3:1,2.4:1,2.5:1,2.6:1,2.7:1,2.8:1,2.9:1,3:1, etc.；It is preferred that
1.5:1；
Preferably, in the S1, the amount of dispersing agent is the 0.3wt%-0.6wt% of styrene quality, such as: 0.3wt%,
0.4wt%, 0.5wt%, 0.6wt%, etc.；It is preferred that 0.4wt%；
Preferably, in the S1, the amount of the low temperature initiators is the 1wt%-3wt% of styrene quality, such as:
1wt%, 1.1wt%, 1.3wt%, 1.5wt%, 1.6wt%, 1.7wt%, 1.9wt%, 2wt%, 2.1wt%, 2.2wt%,
2.4wt%, 2.5wt%, 2.6wt%, 2.7wt%, 2.8wt%, 2.9wt%, 2wt%, etc.；It is preferred that 1.5wt%.
Preferably, the BET value of the graphene is less than 467m2/g；It is further preferred that 187m2/ g≤BET value <
467m2/ g, such as 187m2/g、188m2/g、190m2/g、193m2/g、195m2/g、200m2/g、230m2/g、250m2/g、
270m2/g、290m2/g、300m2/g、315m2/g、337m2/g、350m2/g、356m2/g、370m2/g、384m2/g、400m2/g、
413m2/g、431m2/g、455m2/g、467m2/ g, etc..
It is further preferred that value≤10 μm D50 of the graphene, such as: 10 μm, 9 μm, 8 μm, 7 μm, 5 μm, 4 μm, 3 μ
M, 1 μm, etc..
Preferably, in the S1, the technique of the stirring are as follows: stirred 30 minutes with 180-350 revs/min of revolving speed.Revolving speed
Less than 180 revs/min graphenes disperse not open in polystyrene systems, when revolving speed is excessively high, when being greater than 350 revs/min, and stronger shearing
Power easily causes the aggregation of graphene polystyrene latex grain.
Preferably, in the S2, the amount of the high-temperature initiator is the 0.1wt%-0.5wt% of styrene, such as:
0.1wt%, 0.15wt%, 0.2wt%, 0.24wt%, 0.3wt%, 0.37wt%, 0.4wt%, 0.44wt%, 0.5wt%,
Deng；It is preferred that 0.4wt%.
Preferably, the dispersing agent is the 0.2wt%-1wt% of styrene, such as: 0.2wt%, 0.25wt%,
0.3wt%, 0.33wt%, 0.4wt%, 0.5wt%, 0.51wt%, 0.6wt%, 0.68wt%, 0.7wt%, 0.8wt%,
0.82wt%, 0.9wt%, 1wt%, etc.；It is preferred that 0.4wt%.
Preferably, the foaming agent be styrene 8wt%-12wt%, such as: 8wt%, 8.2wt%, 9wt%,
9.5wt%, 10wt%, 10.3wt%, 11wt%, 11.5wt%, 11.8wt%, 12wt%, etc.；It is preferred that 10wt%.
Preferably, in the S1 or in the S2, the dispersing agent be active calcium phosphate, neopelex,
Two or more compounding in polyvinyl alcohol or hydroxyethyl cellulose；Preferably use neopelex and work
Property calcium phosphate press 2:5 compounding dispersing agent.
Preferably, the low temperature initiators are dibenzoyl peroxide or potassium peroxydisulfate, preferably dibenzoyl peroxide.
Preferably, the high-temperature initiator is peroxidized t-butyl perbenzoate or cumyl peroxide, preferably peroxidating
T-butyl perbenzoate.
Preferably, the foaming agent is one of butane, pentane or petroleum ether or a variety of mixing, preferably pentane.
Preferably, in the step 2), low temperature initiators are added, heat up 60 DEG C, high-temperature initiator is added, is warming up to 90
DEG C, dispersing agent is added, isothermal reaction 6h adds foaming agent, reacts 5h after being warming up to 125 DEG C.
The invention has the advantages that:
(1) toxic chemical is not used using Microwave reduction method, it is environmentally protective, and the graphene size prepared is smaller,
Particle diameter distribution is uniform；
(2) graphene is introduced into polystyrene bead in the way of intercalation polymeric, the reaction time is short, technique letter
It is single, it is suitble to large-scale industrial production；
(3) graphene particle size is small, is intercalation into polystyrene bead in a manner of in-situ polymerization, and graphene is in polyphenyl
High degree of dispersion in ethylene, to ensure that good heat-insulated, the fire-retardant and mechanical property of graphene/EPS.
(4) foamable polyethylene pressing plate molding prepared by the present invention, obtains foam board.The flame retardant rating of foam board
Up to B1 grades, heat conductivity value is reduced to 0.030~0.034W/ (mK), drawing by original 0.039~0.042W/ (mK)
Performance is increased to 260Kpa by original 90Kpa.
For further instruction essence of the invention, applicant is by the deep anatomy of progress of the invention.
Application resistance limit based on current graphene in EPS, the present invention passes through multidirectional further investigation, wherein in graphite
On this direction specific surface area (BET) of alkene the experiment has found that when the specific surface area (BET) of graphene is excessive, graphene and benzene second
Alkene can not form emulsion particle, and the graphene of sheet can hinder the collision of styrene free radical, to influence the polymerization of styrene.Into one
Step, inventor catches this direction to carry out in-depth study, has further inquired into the pass between the BET of graphene and polymerization
System, makes every effort to the graphene for filtering out suitable BET and styrene is polymerize.It is found surprisingly that, BET value is less than 467m2The stone of/g
Mertenyl originally can achieve evenly dispersed purpose.For example, using SE1430 type graphene (10 μm of D50 <, specific surface area >=
240m2/ g, the hexa-atomic element in Changzhou) and SE1231 type graphene (10 μm of D50 <, specific surface area >=187m2/ g, Changzhou are hexa-atomic
Element) it can be polymerize, graphene can form stable oil-in-water state with stable dispersion into styrene；And use SE1233
Type graphene (10 μm of D50 <, specific surface area >=467m2/ g, the hexa-atomic element in Changzhou) when, graphene and styrene can not form latex
Grain, the graphene of sheet can hinder the collision of styrene free radical, to influence the polymerization of styrene.As BET value < 187m2/g
When, graphene also can generate interference to the polymerization of styrene, and polymerization effect is bad.
As shown in Figure 1, 2, SE1430 (BET >=240m2/g) and SE1233 (BET >=467m2/g) type graphene are polymerizeing
The electron micrograph of drop in the process.It can be seen that from Fig. 1, SE1430 drop is bead spheroidal particle, and graphene exists
It is wrapped in styrene droplets, it can be seen that the graphene of sheet, graphene and styrene do not form emulsion particle on Fig. 2, this
It is since the BET of graphene is excessive, the graphene of sheet can hinder the collision of styrene free radical, and graphene and styrene shape are not
At emulsion particle, to influence the polymerization of styrene.
In addition, another important wisdom contribution of the invention, introduces polystyrene for graphene in a manner of in-situ polymerization
In, and graphene additive amount is few, on the one hand reduces costs, and on the other hand may insure the evenly dispersed of graphene, to be
Excellent graphene/the polystyrol foam material of processability provides guarantee.
Detailed description of the invention
Fig. 1 is SE1430 (BET >=240m2/ g) type graphene drop in the course of the polymerization process electron micrograph；
Fig. 2 is SE1233 (BET >=467m2/ g) type graphene drop in the course of the polymerization process electron micrograph.
Specific embodiment
Hereinafter, preferred embodiments of the present invention will be described, it should be understood that preferred embodiment described herein is only used
In the description and interpretation present invention, it is not intended to limit the present invention.
Embodiment 1:
75 grams of styrene are sequentially added, 0.15 gram of SE1430 graphene, 112 grams of deionized waters, 0.3 gram of compounding dispersing agent is extremely
In reaction kettle, progress in mechanical stirring 30 minutes is pre-dispersed, and speed of agitator is 280 revs/min, and low temperature initiators benzoyl peroxide first is added
It 0.75 gram of acyl, starts to warm up, is warming up to 0.4 gram of peroxidized t-butyl perbenzoate of 60 DEG C of addition high-temperature initiators, persistently overheating is extremely
90 DEG C, 0.3 gram of dispersing agent is added after constant temperature 30min, then isothermal reaction 5.5 hours at 90 DEG C, 6 are being added into mixture
Gram pentane, continues to be heated to 120 DEG C, constant temperature 5 hours, is cooled to 40 DEG C, discharging, washs and to be dried to obtain the present invention expandable
Polystyrene bead.
Embodiment 2:
75 grams of styrene are sequentially added, 0.30 gram of SE1430 graphene, 150 grams of deionized waters, 0.3 gram of compounding dispersing agent is extremely
In reaction kettle, progress in mechanical stirring 30 minutes is pre-dispersed, and speed of agitator is 280 revs/min, and low temperature initiators benzoyl peroxide first is added
It 0.75 gram of acyl, starts to warm up, is warming up to 0.4 gram of peroxidized t-butyl perbenzoate of 60 DEG C of addition high-temperature initiators, persistently overheating is extremely
90 DEG C, 0.3 gram of dispersing agent is added after constant temperature 30min, then isothermal reaction 5.5 hours at 90 DEG C, 9 are being added into mixture
Gram pentane continues to be heated to 120 DEG C, constant temperature 5 hours, is cooled to 40 DEG C, discharging washs and is dried to obtain expandable polyphenyl second
Alkene bead.
Embodiment 3
75 grams of styrene are sequentially added, 0.15 gram of SE1231 graphene, 112 grams of deionized waters, 0.3 gram of compounding dispersing agent is extremely
In reaction kettle, progress in mechanical stirring 30 minutes is pre-dispersed, and speed of agitator is 280 revs/min, and low temperature initiators benzoyl peroxide first is added
It 0.75 gram of acyl, starts to warm up, is warming up to 0.4 gram of peroxidized t-butyl perbenzoate of 60 DEG C of addition high-temperature initiators, persistently overheating is extremely
90 DEG C, 0.3 gram of dispersing agent is added after constant temperature 30min, then isothermal reaction 5.5 hours at 90 DEG C, 6 are being added into mixture
Gram pentane continues to be heated to 120 DEG C, constant temperature 5 hours, is cooled to 40 DEG C, discharging washs and is dried to obtain expandable polyphenyl second
Alkene bead.
Embodiment 4:
75 grams of styrene are sequentially added, 0.3 gram of SE1231 graphene, 150 grams of deionized waters, 0.3 gram of compounding dispersing agent is extremely
In reaction kettle, progress in mechanical stirring 30 minutes is pre-dispersed, and speed of agitator is 280 revs/min, and low temperature initiators benzoyl peroxide first is added
It 0.75 gram of acyl, starts to warm up, is warming up to 0.4 gram of peroxidized t-butyl perbenzoate of 60 DEG C of addition high-temperature initiators, persistently overheating is extremely
90 DEG C, 0.3 gram of dispersing agent is added after constant temperature 30min, then isothermal reaction 5.5 hours at 90 DEG C, 9 are being added into mixture
Gram pentane continues to be heated to 120 DEG C, constant temperature 5 hours, is cooled to 40 DEG C, discharging washs and is dried to obtain expandable polyphenyl second
Alkene bead.
Embodiment 5:
Sequentially add 75 grams of styrene, 0.15 gram of SE1233 graphene, 112 grams of deionized waters, 0.45 gram of compounding dispersing agent
Into reaction kettle, progress in mechanical stirring 30 minutes is pre-dispersed, and speed of agitator is 280 revs/min, and low temperature initiators benzoyl peroxide is added
It 0.75 gram of formyl, starts to warm up, is warming up to 0.4 gram of peroxidized t-butyl perbenzoate of 60 DEG C of addition high-temperature initiators, persistently overheating
To 90 DEG C, add 0.3 gram of dispersing agent after constant temperature 30min, then isothermal reaction 5.5 hours at 90 DEG C, into mixture plus
Enter 6 grams of pentanes, continues to be heated to 120 DEG C, constant temperature 5 hours, be cooled to 40 DEG C, discharging is washed and is dried to obtain expandable poly-
Styrene beads.
Embodiment 6:
75 grams of styrene are sequentially added, 0.3 gram of SE1233 graphene, 150 grams of deionized waters, 0.45 gram of compounding dispersing agent is extremely
In reaction kettle, progress in mechanical stirring 30 minutes is pre-dispersed, and speed of agitator is 280 revs/min, and low temperature initiators benzoyl peroxide first is added
It 0.75 gram of acyl, starts to warm up, is warming up to 0.4 gram of peroxidized t-butyl perbenzoate of 60 DEG C of addition high-temperature initiators, persistently overheating is extremely
90 DEG C, 0.3 gram of dispersing agent is added after constant temperature 30min, then isothermal reaction 5.5 hours at 90 DEG C, 9 are being added into mixture
Gram pentane continues to be heated to 120 DEG C, constant temperature 5 hours, is cooled to 40 DEG C, discharging washs and is dried to obtain expandable polyphenyl second
Alkene bead.
Embodiment 7:
Sequentially add 75 grams of styrene, 0.225 gram of SE1231 graphene, 112 grams of deionized waters, 0.3 gram of compounding dispersing agent
Into reaction kettle, progress in mechanical stirring 30 minutes is pre-dispersed, and speed of agitator is 280 revs/min, and low temperature initiators benzoyl peroxide is added
It .125 grams of formyl chloride-1, starts to warm up, is warming up to 0.3 gram of peroxidized t-butyl perbenzoate of 60 DEG C of addition high-temperature initiators, persistently overheating
To 90 DEG C, 0.3 gram of dispersing agent is added after constant temperature 30min, then isothermal reaction 6 hours at 90 DEG C, are being added into mixture
7.5 grams of pentanes continue to be heated to 125 DEG C, constant temperature 5 hours, are cooled to 40 DEG C, discharging is washed and is dried to obtain expandable poly-
Styrene beads.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, although referring to aforementioned reality
Applying example, invention is explained in detail, for those skilled in the art, still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features.It is all in essence of the invention
Within mind and principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (23)
1. a kind of preparation method of expandable poly-styrene, it is characterised in that: include:
S1: first styrene, water, dispersing agent and graphene are mixed, stirs in a kettle, forms uniform suspension；
S2: low temperature initiators will be added in S1 uniformly mixed material, is warming up to 50-70 DEG C, high-temperature initiator is added, then heat up
When to 88-92 DEG C, it is added dispersing agent, after isothermal reaction 5-8h, adds foaming agent, constant temperature 2- after temperature rises to 105-130 DEG C
6h, end of reaction；
S3: by the material in reaction kettle take out filtering, it is dry to get；
Wherein, in the S1, the amount of dispersing agent is the 0.3wt%-0.6wt% of styrene quality, and the amount of graphene is styrene
The 0.2wt%-1wt% of quality；The BET value of the graphene is 240m2/ g≤BET value < 467m2/g；The D50 of the graphene
≤ 10 μm of value.
2. the preparation method of expandable poly-styrene according to claim 1, it is characterised in that: in the S1, water, benzene
The mass ratio of ethylene is (1.5-3): 1.
3. the preparation method of expandable poly-styrene according to claim 1, it is characterised in that: described in the S1
The amount of low temperature initiators is the 1wt%-3wt% of styrene quality.
4. the preparation method of expandable poly-styrene according to claim 2, it is characterised in that: in the S1, water, benzene
The mass ratio of ethylene is 1.5:1.
5. the preparation method of expandable poly-styrene according to claim 1, it is characterised in that: in the S1, dispersion
The amount of agent is the 0.4wt% of styrene quality.
6. the preparation method of expandable poly-styrene according to claim 3, it is characterised in that: described in the S1
The amount of low temperature initiators is the 1.5wt% of styrene quality.
7. the preparation method of expandable poly-styrene according to claim 1, it is characterised in that: described in the S1
The amount of graphene is the 0.3wt% of styrene quality.
8. the preparation method of expandable poly-styrene according to claim 1-7, it is characterised in that: the S1
In, the technique of the stirring are as follows: stirred 30 minutes with 180-350 revs/min of revolving speed.
9. the preparation method of expandable poly-styrene according to claim 1, it is characterised in that: described in the S2
The amount of high-temperature initiator is the 0.1wt%-0.5wt% of styrene.
10. the preparation method of expandable poly-styrene according to claim 1, it is characterised in that: described in the S2
Dispersing agent is the 0.2wt%-1wt% of styrene.
11. the preparation method of expandable poly-styrene according to claim 1, it is characterised in that: described in the S2
Foaming agent is the 8wt%-12wt% of styrene.
12. the preparation method of expandable poly-styrene according to claim 9, it is characterised in that: described in the S2
The amount of high-temperature initiator is the 0.4wt% of styrene.
13. the preparation method of expandable poly-styrene according to claim 10, it is characterised in that: in the S2, institute
State the 0.4wt% that dispersing agent is styrene.
14. the preparation method of expandable poly-styrene according to claim 11, it is characterised in that: in the S2, institute
State the 10wt% that foaming agent is styrene.
15. the preparation method of expandable poly-styrene according to claim 1, it is characterised in that: in the S1 or institute
It states in S2, the dispersing agent is two in active calcium phosphate, neopelex, polyvinyl alcohol or hydroxyethyl cellulose
Kind or two or more compoundings.
16. the preparation method of expandable poly-styrene according to claim 1, it is characterised in that: the low temperature causes
Agent is dibenzoyl peroxide or potassium peroxydisulfate.
17. the preparation method of expandable poly-styrene according to claim 1, it is characterised in that: the high temperature causes
Agent is peroxidized t-butyl perbenzoate or cumyl peroxide.
18. the preparation method of expandable poly-styrene according to claim 1, it is characterised in that: the foaming agent is
One of butane, pentane or petroleum ether or a variety of mixing.
19. the preparation method of expandable poly-styrene according to claim 15, it is characterised in that: in the S1 or institute
It states in S2, the dispersing agent is all made of neopelex and compounds dispersing agent by 2:5 with active calcium phosphate.
20. the preparation method of expandable poly-styrene according to claim 16, it is characterised in that: the low temperature causes
Agent is dibenzoyl peroxide.
21. the preparation method of expandable poly-styrene according to claim 17, it is characterised in that: the high temperature causes
Agent is peroxidized t-butyl perbenzoate.
22. the preparation method of expandable poly-styrene according to claim 18, it is characterised in that: the foaming agent is
Pentane.
23. the preparation method of expandable poly-styrene according to claim 1, it is characterised in that: in the step 2),
Low temperature initiators are added, heat up 60 DEG C, high-temperature initiator is added, is warming up to 90 DEG C, are added dispersing agent, isothermal reaction 6h, then plus
Enter foaming agent, reacts 5h after being warming up to 125 DEG C.
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| CN108084583B (en) * | 2017-11-29 | 2021-01-01 | 吉林云亭石墨烯技术股份有限公司 | Preparation method of graphene and preparation of sound insulation graphene EPS |
| CN109735016A (en) * | 2018-12-15 | 2019-05-10 | 宁波墨西科技有限公司 | Poly styrene composite material, thermal insulation material and preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105732860A (en) * | 2016-02-04 | 2016-07-06 | 吉林省云亭节能技术有限公司 | Expandable polystyrene beads prepared from expandable few-layer graphene and preparing method of expandable polystyrene beads |
| CN106188608A (en) * | 2016-07-25 | 2016-12-07 | 江苏利士德化工有限公司 | A kind of method of the expandable polystyrene particles of preparation of industrialization graphene-containing |
| 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 |
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| CN105732860A (en) * | 2016-02-04 | 2016-07-06 | 吉林省云亭节能技术有限公司 | Expandable polystyrene beads prepared from expandable few-layer graphene and preparing method of expandable polystyrene beads |
| CN106188608A (en) * | 2016-07-25 | 2016-12-07 | 江苏利士德化工有限公司 | A kind of method of the expandable polystyrene particles of preparation of industrialization graphene-containing |
| 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 |
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