CN108219426A - A kind of PC master batches being modified based on white graphite alkene and preparation method thereof - Google Patents
A kind of PC master batches being modified based on white graphite alkene and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to composite plastic technical fields, and in particular to a kind of PC master batches being modified based on white graphite alkene and preparation method thereof.Include by weight：100 parts of PC particles, modified 0.5~10 part of white graphite alkene, 0.05~0.2 part of fire retardant, 0.1~0.4 part of antioxidant；The modified white graphite alkene is 2~10 layers of white graphite alkene first after the processing of surface lipophile, then be modified through in-situ polymerization to obtain the white graphite alkene modified by polymer overmold.The extruded machine of above-mentioned raw materials squeezes out, then be granulated by pelleter, obtains the PC master batches of white graphite alkene modification.Addition impact modifier is not needed in this method, the heat conductivility of PC master batches, flame retardant property and the notch impact strength that the application is prepared greatly improve, and insulation performance is unaffected, and simplify technique, reduce cost.
Description
Technical field
The present invention relates to composite plastic technical fields, and in particular to a kind of PC master batches being modified based on white graphite alkene and its system
Preparation Method.
Background technology
Makrolon (PC) is the general name of a kind of polymer containing carbonate group in strand, is the main of engineering plastics
One of kind, yield are only second to nylon in five large-engineering plastics, occupy second.It has prominent impact flexibility, well
The transparency, dimensional stability and electrical insulating property, and with use temperature range is wide, creep resistance, the characteristics such as weather-proof, nontoxic,
A kind of engineering plastics of high comprehensive performance, be now widely used for automobile, electric, building, office equipment, packaging,
The fields such as sports equipment, health care.
But pure PC heat conductivilitys are poor, and flame retardant property is relatively low, limit its application in high heat conduction, flame retardant area, such as electronics
Device outer case, LED heat sinks, electrical-coil etc..Generally by adding inorganic heat filling in resin matrix, as aluminium oxide,
Silica, aluminium nitride, silicon carbide, zinc oxide etc. improve its heat conductivility, add halogen-free flame retardants such as organic phosphorus, silicon systems, sulphur
The fire retardants such as phosphate-gallate series assign its flame retardant property.But the loading of all kinds of heat fillings and fire retardant is larger, leads to the mechanics of PC
Performance, especially notch impact strength drastically decline, and insulation performance can also be affected.To solve these problems, usually add
Enter various impact modifiers, such as butadiene-styrene-methyl methacrylate (MBS) impact modifier, acrylate (ACR)
The high molecular polymer containing rubber phase, with nucleocapsid such as class impact modifier.But due to MBS resistances to oxidation and heat resistance
Difference, the weatherability and thermal stability that can cause PC products decline；ACR usually provides preferable thermal stability and weatherability, but low
Warm shock resistance is poor.And with the increase of impact-resistant modified agent content, the indexs such as stretching, bending and the case hardness of PC are
Decline, processing performance deterioration.
Therefore, as can while PC heat conduction, flame retardant property is improved, its notch impact strength and insulation performance are greatly improved
It is unaffected, it is significant to meeting the market demand and its application field of extension.
Invention content
In view of this, it is necessary to the shortcomings that for existing heat filling, it is female to provide a kind of PC being modified based on white graphite alkene
Grain and preparation method thereof, this method can reduce the dosage of fire retardant, without adding impact modifier, while make leading for PC master batches
Hot property, flame retardant property and notch impact strength greatly improve, and insulation performance is unaffected.
To achieve the above object, the present invention takes following technical solution：
The PC master batches being modified based on white graphite alkene of the present invention, are included by weight：100 parts of PC particles, modified white graphite
0.5~10 part of alkene, 0.05~0.2 part of fire retardant, 0.1~0.4 part of antioxidant；
The modified white graphite alkene first changes for 2~10 layers of white graphite alkene after the processing of surface lipophile, then through in-situ polymerization
Property obtains the white graphite alkene modified by polymer overmold.
White graphite alkene has high thermal conductivity, high mechanical properties and insulation performance, and it is excellent that a small amount of addition can assign resin
Heat conductivility, while can also improve the impact flexibility of resin, and white graphite alkene is transparence, will not after adding in resin matrix
Influence its coloring.
Further, the PC master batches, include by weight：100 parts of PC particles, modified 5 parts of white graphite alkene, fire retardant
0.2 part, 0.2 part of antioxidant.
Further, the fire retardant is at least one of organic phosphorus, silicon systems, sulfonate flame retardant；
The antioxidant is at least one of antioxidant 1010, irgasfos 168, antioxidant 2912.
Further, the grain size of the modified white graphite alkene is 5~10 μm, 300~500m of specific surface area2/ part.
Since white graphite alkene has unique structure and surface energy, with most of oiliness monomers such as styrene, metering system
Sour methyl esters is difficult to be smoothed out in white graphite alkene material surface when polymerisations, therefore, it is necessary to carry out surface oleophylic to it
Processing can make monomer that in-situ polymerization occur on its surface and form clad.
Specifically, the preparation process of the modified white graphite alkene, includes the following steps：
S1, dialogue graphene surface are modified
The white graphite alkene of 0.5~10 part of weight is dispersed in the dispersion solution of 100 parts of weight, after dispersion add in 0.1~
The stabilizer of 0.5 part of weight carries out surface modification treatment；
S2, monomer are in white graphite alkene surface aggregate
60 DEG C~100 DEG C will be warming up to through the modified white graphite alkene dispersion liquid in S1 surfaces, 0.5~5 part of weight of addition
Initiator, stirring make solution uniform, and the polymer monomer of 0.05~2 part of weight is then added dropwise, and 0.5~1h is dripped off；It is added dropwise
Afterwards, continue after keeping the temperature 30min~2h reactions, adjust pH value to 7~8, be then rapidly cooled to 20~30 DEG C；
S3, post processing
The cooled product that will be obtained by S2, washed, filtering, it is dry and grind high polymer cladding white graphite alkene.
White graphite alkene is individual layer or few layer hexagonal boron nitride, has big specific surface area, high thermal conductivity and specific strength.It is logical
It crosses dialogue graphene surface and carries out polymer overmold modification, select suitable initiator, coating thickness is controllable, coats thickness
Degree is uniform, and monomer is slowly added dropwise, cladding process is made orderly to carry out, optimizes acid-base value and temperature condition after completion of the reaction, effectively
Reaction is terminated, obtains best covered effect, can prevent white graphite alkene from reuniting, enhance its interface performance with composite substrate,
Make it that can be uniformly dispersed in PC, promote the formation of entire material system piece layered network.And large-sized white graphite alkene exists
Low content addition is lower to be easier to occur putting up a bridge to form thermal conducting path, and hot-fluid conducts faster along high heat conduction access, and it is excellent to assign PC
Heat conductivility, while do not influence insulating properties.
Further, dialogue graphene surface is modified as in S1：The white graphite alkene of 5~10 parts of weight is dispersed in 100 parts
In the dispersion solution of weight, the stabilizer that 0.1~0.5 part of weight is added in after dispersion is modified processing.
Further, modification mode described in S1 for grinding or is impregnated.
Further, solution is disperseed described in S1 to include：One or more of water, ethyl alcohol, glycerine or ethylene glycol etc.
Mixing；The stabilizer includes：It is a kind of in polyvinylpyrrolidone, sodium alkyl sulfate, sodium alkyl benzene sulfonate, oleyl amine or oleic acid etc.
It is or a variety of.
As preference, it is ethyl alcohol to disperse solution described in S1；The stabilizer is oleyl amine or oleic acid.
Further, monomer described in S2 is in white graphite alkene surface aggregate：After the surface treatment of 10~20 parts of weight
White graphite alkene dispersion liquid be warming up to 80 DEG C~90 DEG C, add in the initiator of 3~5 parts of weight, 10~30min of stirring makes solution equal
It is even, the polymer monomer of 0.5~1 part of weight is added dropwise dropwise, 0.5~1h is dripped off；After being added dropwise, continue 1~2h of heat preservation reactions
After complete, pH value is adjusted to 7~8, is then rapidly cooled to 20~30 DEG C.
Further, polymerized monomer described in S2 is：Styrene, acrylic acid, methyl acrylate, ethyl acrylate, propylene
It is one or more in the monomers such as sour hydroxyl ethyl ester, methyl methacrylate, glycidyl methacrylate.The polymerized monomer
It is all handled using preceding through vacuum distillation.
Further, initiator described in S2 is ammonium persulfate or azodiisobutyronitrile.
Further, washing, drying process described in S3, specially using ethanol wash, are done at 60~80 DEG C
It is dry.
A kind of preparation method for the PC master batches being modified based on white graphite alkene, the specific steps are：PC is done at 100-150 DEG C
Dry 6~12h；
Weigh by weight PC, modified white graphite alkene, fire retardant, antioxidant add in mixing 5 in high-speed mixer~
20min；Said mixture is added in extruder to squeeze out, then is granulated by pelleter, obtains the PC master batches of white graphite alkene modification.
Further, 180~250 DEG C of each area's temperature of the extruder, 190~250 DEG C of head temperature squeeze out machine host and turn
Speed is 250~280rpm, 8~12Hz of rate of feeding；6~12Hz of pelletizing unit frequency.
Further, the extruder is single screw extrusion machine or double screw extruder, preferably double screw extruder.
Beneficial effects of the present invention are：
1) white graphite alkene adds in the piece layered network formed after resin can effectively inhibit polymer point in combustion
The warm-up movement of subchain improves the viscosity of compound system, plays and reduces the effect of volatile fuel spilling enters with extraneous oxygen,
Auxiliary fire retardant can be used as, synergistic effect is played with fire retardant, improves flame retardant effect, while reduce the dosage of fire retardant.
2) the white graphite alkene being dispersed in PC can slow down quick orientation of PC strands when by external force, absorb
Big energy prevents generation and the Quick Extended of crazing, so as to improve the impact property of PC.Therefore it does not need to add in this method
Add impact modifier, cost can be reduced, while improve the notch of PC to avoid harmful effect is caused to matrix, and simplify technique
Impact strength.
3) white graphite alkene is insulation, transparence, after adding in resin matrix, does not interfere with the insulating properties and coloring of matrix.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention, to this hair
Bright technical solution work further clearly and completely describes.It should be noted that described embodiment is only the present invention one
Section Example, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not doing
Go out all other embodiments obtained under the premise of creative work, shall fall within the protection scope of the present invention.
Embodiment 1
The preparation of modified white graphite alkene
0.5 part of white graphite alkene powder is taken to add in into round-bottomed flask, and 100 parts of distilled water are added in into round-bottomed flask, so
Ultrasonic disperse afterwards, 0.1 part of lauryl sodium sulfate is added in into round-bottomed flask, and ultrasonic high-speed stirred obtains oleophylic and is modified white stone
Black alkene；After the white graphite alkene dispersion liquid that oleophylic is modified is heated to 60 DEG C, 0.5 part of ammonium persulfate initiator is added in, stirs 10min
After start that 0.05 part of methyl methacrylate is added dropwise, 0.5h drips off.After being added dropwise, heat preservation 0.5h treats that reaction is completed.It has reacted
It is 7 to adjust pH value with ammonium hydroxide after finishing, and is rapidly cooled to room temperature, is filtered under diminished pressure, and ethanol wash is used after being washed with distilled water filter cake 3 times
Once, and in 60 DEG C of vacuum drying grindings the white graphite alkene of polymethyl methacrylate coating decoration is obtained.
Prepare modified PC master batches
PC is dried into 12h at 100 DEG C；
100 parts of PC particles, 0.5 part of modified white graphite alkene, 0.2 part of phosphate flame retardant, 0.1 part of antioxygen are weighed by weight
Agent 1010 adds in mixing 5min in high-speed mixer；
Said mixture is added in single screw extrusion machine to squeeze out, then is granulated by pelleter, obtains the PC of white graphite alkene modification
Master batch.Wherein each area's temperature of single screw extrusion machine is at 180 DEG C, 190 DEG C of head temperature, extruder engine speed 250rpm, feeding
Rotating speed 8Hz；Pelleter speed 6Hz.
Embodiment 2
The preparation of modified white graphite alkene
2 parts of white graphite alkene powder is taken to add in into round-bottomed flask, and 100 parts of ethyl alcohol, Ran Houchao are added in into round-bottomed flask
Sound disperses, and 0.2 part of lauryl sodium sulfate is added in into round-bottomed flask, and ultrasonic high-speed stirred obtains oleophylic and is modified white graphite alkene；
After the white graphite alkene dispersion liquid that oleophylic is modified is heated to 90 DEG C, 1 part of ammonium persulfate initiator is added in, is started after stirring 15min
0.5 part of methyl acrylate is added dropwise, 0.6h is dripped off.After being added dropwise, heat preservation 1h treats that reaction is completed.It is adjusted after completion of the reaction with ammonium hydroxide
PH value is 7, is rapidly cooled to room temperature, is filtered under diminished pressure, be washed with distilled water it is primary with ethanol wash after filter cake 3~4 times, and 70
DEG C vacuum drying grinding i.e. obtain the white graphite alkene of polymethyl acrylate coating decoration.
Prepare modified PC master batches
PC is dried into 10h at 120 DEG C；
100 parts of PC, 2 parts of modified white graphite alkene, 0.15 part of oxidation phosphorus fire retardant, 0.2 part of irgasfos 168 are weighed by weight
Add in mixing 10min in high-speed mixer；
Said mixture is added in single screw extrusion machine to squeeze out, then is granulated by pelleter, obtains the PC of white graphite alkene modification
Master batch.Wherein each area's temperature of single screw extrusion machine is at 210 DEG C, 210 DEG C of head temperature, extruder engine speed 250rpm, feeding
Rotating speed 10Hz；Pelleter speed 8Hz.
Embodiment 3
The preparation of modified white graphite alkene
8 parts of white graphite alkene powder is taken to add in into round-bottomed flask, and 100 parts of glycerine are added in into round-bottomed flask, then
Ultrasonic disperse, 0.3 part of oleyl amine is added in into round-bottomed flask, and ultrasonic high-speed stirred obtains oleophylic and is modified white graphite alkene；Oleophylic is changed
Property white graphite alkene dispersion liquid be heated to 90 DEG C after, add in 2 parts of azodiisobutyronitrile initiators, stir 20min after start dropwise addition 1
Part glycidyl acrylate, 0.7h are dripped off.After being added dropwise, heat preservation 1.5h treats that reaction is completed.After completion of the reaction with ammonium hydroxide tune
It is 7 to save pH value, is rapidly cooled to room temperature, is filtered under diminished pressure, be washed with distilled water it is primary with ethanol wash after filter cake 3~4 times, and
90 DEG C of vacuum drying grindings obtain the white graphite alkene of poly (glycidyl methacrylate) coating decoration.
Prepare modified PC master batches
PC is dried into 10h at 120 DEG C；
Weigh by weight 100 parts of PC, 8 parts of modified white graphite alkene, 0.1 part of copolymerization organosiloxane fire retardant, 0.3 part it is anti-
Oxygen agent 168 adds in mixing 10min in high-speed mixer；
Said mixture is added in single screw extrusion machine to squeeze out, then is granulated by pelleter, obtains the PC of white graphite alkene modification
Master batch.Wherein each area's temperature of single screw extrusion machine squeezes out machine host and turns 260rpm in 220 DEG C, 225 DEG C of head temperature, and feeding turns
Fast 10Hz；Pelleter speed 10Hz.
Embodiment 4
The preparation of modified white graphite alkene
10 parts of white graphite alkene powder is taken to add in into round-bottomed flask, and 100 parts of glycerine are added in into round-bottomed flask, then
Ultrasonic disperse, 0.5 part of polyvinylpyrrolidone is added in into round-bottomed flask, and ultrasonic high-speed stirred obtains oleophylic and is modified white graphite
Alkene；After the white graphite alkene dispersion liquid that oleophylic is modified is heated to 100 DEG C, 5 parts of ammonium persulfate initiators are added in, after stirring 10min
Start that 2 parts of styrene are added dropwise, 1h is dripped off.After being added dropwise, heat preservation 2h treats that reaction is completed.After completion of the reaction pH value is adjusted with ammonium hydroxide
It is 7, is rapidly cooled to room temperature, be filtered under diminished pressure, is washed with distilled water primary with ethanol wash and true at 90 DEG C after filter cake 3~4 times
Empty drying and grinding obtains the white graphite alkene of polystyrene coating decoration.
Prepare modified PC master batches
PC is dried into 6h at 150 DEG C；
100 parts of PC, 10 parts of modified white graphite alkene, 0.05 part of potassium phenylsulphonyl benzene sulfonate fire retardant, 0.4 are weighed by weight
Part antioxidant 2912 adds in mixing 10min in high-speed mixer；
Said mixture is added in double screw extruder to squeeze out, then is granulated by pelleter, obtains the modification of white graphite alkene
PC master batches.Wherein at 250 DEG C, 250 DEG C of head temperature, extruder engine speed 280rpm is fed each area's temperature of single screw extrusion machine
Expect rotating speed 12Hz；Pelleter speed 12Hz.
For the technique effect of the verification present invention, the PC master batches that white graphite alkene prepared by the present invention is modified and contrast sample PC
(pure PC) is tested for the property, as shown in table 1：
The PC performance datas of 1 each embodiment of table and comparative example
As can be known from the above table, the preparation method of a kind of PC master batches being modified based on white graphite alkene provided by the invention, can subtract
The dosage of few fire retardant, without adding impact modifier, while makes heat conductivility, flame retardant property and the notch shock of PC master batches strong
Degree greatly improves.And non-modified white graphite alkene can not be added in PC.
Comparative example 1
0.5 part of white graphite alkene powder is taken to add in into round-bottomed flask, and 100 parts of distilled water are added in into round-bottomed flask, so
Ultrasonic disperse afterwards, 0.1 part of lauryl sodium sulfate is added in into round-bottomed flask, and ultrasonic high-speed stirred obtains oleophylic and is modified white stone
Black alkene.
After the white graphite alkene dispersion liquid that oleophylic is modified is heated to 60 DEG C, 0.5 part of ammonium persulfate initiator, stirring are added in
Start that 0.05 part of methyl methacrylate is added dropwise after 10min, 0.5h is dripped off.After being added dropwise, heat preservation 0.5h treats that reaction is completed.Instead
Should after the completion of pH value be 4.5, naturally cool to room temperature, be filtered under diminished pressure, be washed with distilled water after filter cake 3 times with ethanol wash one
The white graphite alkene of acrylate cladding that is secondary, and being obtained after 60 DEG C of vacuum drying grindings.
Comparative example 2
0.5 part of white graphite alkene powder is taken to add in into round-bottomed flask, and 100 parts of distilled water are added in into round-bottomed flask, so
Ultrasonic disperse afterwards, 0.1 part of lauryl sodium sulfate is added in into round-bottomed flask, and ultrasonic high-speed stirred obtains oleophylic and is modified white stone
Black alkene.
The white graphite alkene dispersion liquid that lipophile is modified heats, and temperature adds in 6 parts of ammonium persulfate initiators to after 60 DEG C,
Start that 0.05 part of methyl methacrylate is added dropwise after stirring 10min, 0.5h is dripped off.After being added dropwise, heat preservation 0.5h waits to have reacted
Into.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, after being washed with distilled water filter cake 3 times
It is primary with ethanol wash, and obtain the white graphite alkene of polymethyl methacrylate coating decoration in 60 DEG C of vacuum drying grindings.
High polymer cladding two-dimensional nano sheet material obtained by embodiment 1-4 is dispersed in alcohol, is not reunited within 10 days；Phase
Comparative example 1-2 occurred to reunite and can not apply in the product at 1 day or so under the conditions of.
Embodiment described above only expresses the several embodiments of the present invention, and description is more specific and detailed, but simultaneously
Cannot the limitation to the scope of the claims of the present invention therefore be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of PC master batches being modified based on white graphite alkene, which is characterized in that include by weight：100 parts of PC particles are modified white
0.5~10 part of graphene, 0.05~0.2 part of fire retardant, 0.1~0.4 part of antioxidant；
The modified white graphite alkene is 2~10 layers of white graphite alkene first after the processing of surface lipophile, then modified through in-situ polymerization
To the white graphite alkene modified by polymer overmold.
2. the PC master batches according to claim 1 being modified based on white graphite alkene, which is characterized in that 100 parts of PC particles, it is modified
5 parts of white graphite alkene, 0.2 part of fire retardant, 0.2 part of antioxidant.
3. the PC master batches according to claim 1 being modified based on white graphite alkene, which is characterized in that the fire retardant is organic
At least one of phosphorus system, silicon systems, sulfonate flame retardant；
The antioxidant is at least one of antioxidant 1010, irgasfos 168, antioxidant 2912.
4. the PC master batches according to claim 1 being modified based on white graphite alkene, which is characterized in that the modified white graphite alkene
Grain size for 5~10 μm, 300~500m of specific surface area2/ part.
5. the PC master batches being modified according to any one of claims 1-4 based on white graphite alkene, which is characterized in that described to change
The preparation process of property white graphite alkene, includes the following steps：
S1, dialogue graphene surface are modified
The white graphite alkene of 0.5~10 part of weight is dispersed in the dispersion solution of 100 parts of weight, 0.1~0.5 part is added in after dispersion
The stabilizer of weight carries out surface modification treatment；
S2, monomer are in white graphite alkene surface aggregate
60 DEG C~100 DEG C will be warming up to through the modified white graphite alkene dispersion liquid in S1 surfaces, add in the initiation of 0.5~5 part of weight
Agent, stirring make solution uniform, and the polymer monomer of 0.05~2 part of weight is then added dropwise, and 0.5~1h is dripped off；After being added dropwise, after
After temperature of continuing insurance 30min~2h reactions, pH value is adjusted to 7~8, is then rapidly cooled to 20~30 DEG C；
S3, post processing
The cooled product that will be obtained by S2, washed, filtering, it is dry and grind high polymer cladding white graphite alkene.
6. the PC master batches according to claim 5 being modified based on white graphite alkene, which is characterized in that disperse solution described in S1
Including：The mixing of one or more of water, ethyl alcohol, glycerine or ethylene glycol；The stabilizer includes：Polyvinylpyrrolidone,
It is one or more in sodium alkyl sulfate, sodium alkyl benzene sulfonate, oleyl amine or oleic acid.
7. the PC master batches according to claim 5 being modified based on white graphite alkene, which is characterized in that monomer is white described in S2
Graphene surface is polymerized to：White graphite alkene dispersion liquid after the surface treatment of 10~20 parts of weight is warming up to 80 DEG C~90 DEG C,
The initiator of 3~5 parts of weight is added in, 10~30min of stirring makes solution uniform, the polymer list of 0.5~1 part of weight is added dropwise dropwise
Body, 0.5~1h are dripped off；After being added dropwise, continue after 1~2h of heat preservation reacted, to adjust pH value to 7~8, be then rapidly cooled to
20~30 DEG C.
8. the PC master batches according to claim 5 being modified based on white graphite alkene, which is characterized in that polymerized monomer described in S2
For：Styrene, acrylic acid, methyl acrylate, ethyl acrylate, hydroxy-ethyl acrylate, methyl methacrylate, methacrylic acid
It is one or more in glycidyl ester monomer.
9. the PC master batches according to claim 1 being modified based on white graphite alkene, which is characterized in that initiator described in S2 is
Ammonium persulfate or azodiisobutyronitrile.
10. according to the preparation method of the PC master batches described in any one of claim 1-9 being modified based on white graphite alkene, feature
It is, the specific steps are：PC is dried into 6~12h at 100-150 DEG C；
PC, modified white graphite alkene, fire retardant, antioxidant are weighed by weight adds in 5~20min of mixing in high-speed mixer；It will
Said mixture adds in extruder and squeezes out, then is granulated by pelleter, obtains the PC master batches of white graphite alkene modification.
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