CN109294089A - A kind of construction wall polystyrene foam graphene enhancing masterbatch and preparation method - Google Patents
A kind of construction wall polystyrene foam graphene enhancing masterbatch and preparation method Download PDFInfo
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
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- 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
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Abstract
The invention belongs to the technical field of construction material, a kind of construction wall polystyrene foam graphene enhancing masterbatch and preparation method are provided.This method is by being filled in porous SiO for Graphene powder2Inside microballoon, and oleophylic processing is carried out, then polymerization reaction forms polystyrene/ultra high molecular weight polyethylene alloy, coated porous SiO2Complex microsphere, further with polystyrene carrier resin, activating agent mixed at high speed and extruding pelletization, graphene, which is made, enhances masterbatch.It is compared with the traditional method, the graphene of preparation of the invention enhances masterbatch, when enhancing modified for polystyrene foam, effectively improve the dispersibility of graphene, and then the mechanical property of material can be obviously improved, ensure modified reinforcing effect, gained polystyrene foam is suitable for the engineering fields such as construction wall.
Description
Technical field
The invention belongs to the technical field of construction material, provides a kind of construction wall polystyrene foam and increased with graphene
Strong masterbatch and preparation method.
Background technique
Polystyrene (PS) foam be by the expandable polystyrene bead containing volatile fluid foaming agent, it is heated pre-
The white object of hot briquetting in a mold after hair, there is the design feature of fine closed pore, is mainly used for construction wall, and roofing is protected
Temperature, composite plate heat preservation, freezer, air-conditioning, vehicle, ship insulation, floor heating, decoration engraving etc. purposes it is very extensive.
Become an important topic of building field lower than the research of base styrenic foams material and application in recent years.
Graphene possesses many excellent special natures as a kind of novel nano material, and especially it has very high
Strength and stiffness, be currently known it is highest in material.Its structure is the graphite synusia of single layer, it is graphite, carbon nanometer
The basic component units of pipe, fullerene.Graphene have so excellent strength and stiffness be because graphene atomic structure in,
Formed key is strongest chemical bond σ key between carbon atom and carbon atom.Graphene is in addition to possessing very excellent intensity and just
Other than degree, also there is excellent toughness and some special deformation mechanisms.
Enhancing modification is carried out to polystyrene foam using graphene and has become the technical method generallyd use.Polyphenyl second
The manufacture of alkene-graphene complex can be by carrying out as follows: by Polystyrene powder and graphene for example by shear-mixed skill
Art is further foamed by grinding physical mixed.However, the shortcomings that these methods is that graphene is not good in polystyrene
Good dispersion, graphene dispersion is ineffective, easily reunites, so that the polystyrene prepared will appear mechanical property unevenness
It is even, the unconspicuous phenomenon of reinforcing effect.
One especially has been achieved in terms of graphene enhancing polystyrene foam in polystyrene foam technology both at home and abroad at present
Determine effect.Wherein Hu Zhen et al. has invented a kind of preparation method (the middle promulgated by the State Council of the expandable polystyrene polymer of containing graphene
Bright number of patent application 201410056491.1), which will solve the preparation side of existing graphene poly styrene composite material
Method is using graphene as raw material, the high, complex process and the problem of unsuitable large-scale industrial production so as to cause preparation cost, system
Preparation Method: (1) graphite oxide is prepared using Hummers method;The preparation of (2) first mixtures;The preparation of (3) second mixtures;
(4) preparation of the expandable polystyrene polymer of graphene to get containing graphene expandable polystyrene polymer.Separately
Outside, Liu Lili et al. has invented a kind of expandable poly-styrene and preparation method thereof (Chinese invention patent application number
201710349183.1), wherein in the expandable poly-styrene, the amount of institute's containing graphene accounts for styrene monomer before polymerization
0.2 ~ 1wt% of total weight;The expandable poly-styrene pressing plate molding of invention preparation, obtains foam board.
As it can be seen that the technical method in the prior art using graphene modified polystyrene foamed material, there are graphenes
It is difficult to evenly dispersed, the serious phenomenon of reuniting, causes polystyrene foamed material there are mechanical property reinforcing effect is bad, it is comprehensive
The non-uniform defect of performance.
Summary of the invention
In response to this, it is proposed that a kind of construction wall polystyrene foam enhances masterbatch and preparation side with graphene
Method can be effectively improved distribution characteristics of the graphene in polystyrene foam, and be obviously improved to foamed product mechanical property
The reinforcing effect of energy.
To achieve the above object, specific technical solution of the present invention is as follows:
A kind of construction wall polystyrene foam enhances the preparation method of masterbatch with graphene, more by the way that Graphene powder to be filled in
Hole SiO2Inside microballoon, and oleophylic processing is carried out, then polymerization reaction forms polystyrene/ultra high molecular weight polyethylene alloy,
Coated porous SiO2Stone is made further with polystyrene carrier resin, activating agent mixed at high speed and extruding pelletization in complex microsphere
Black alkene enhances masterbatch, and specific step is as follows for preparation:
(1) by Graphene powder and porous SiO2Microballoon mixing, is adsorbed in circulating air driven mixer, fills out Graphene powder
It fills in porous SiO2Inside microballoon, surfactant is then added, oleophylic processing is carried out to microsphere surface in ultrasound field,
Porous SiO is made2Complex microsphere;
It (2) will treated porous SiO2Complex microsphere moves into reaction kettle, and it is poly- that styrene activated monomer, super high molecular weight is added
Ethylene staple fiber, initiator are passed through nitrogen protection, while carrying out isothermal reaction, shape under the activation of ultrasound field, initiation
At the porous SiO of polystyrene/ultra high molecular weight polyethylene alloy cladding2Complex microsphere;
(3) complex microsphere made from step (2) and polystyrene carrier resin, activating agent are mixed point in a high speed mixer
It dissipates, is granulated through screw extruder, graphene, which is made, enhances masterbatch.
Preferably, step (1) surfactant is alkyl glucoside, in fatty glyceride, fatty acid sorbitan
At least one.
Preferably, the parts by weight of step (1) each raw material are 5 ~ 20 parts by weight of Graphene powder, porous SiO2Microballoon 77 ~
94 parts by weight, 1 ~ 3 parts by weight of surfactant.
Preferably, the ultrasonic frequency of step (1) described ultrasound field is 80 ~ 150kHz, and power density is 0.5 ~ 1w/
cm2。
Preferably, step (2) initiator is azodiisobutyronitrile, azobisisoheptonitrile, two isobutyric acid diformazan of azo
At least one of ester.
Preferably, the parts by weight of step (2) each raw material are porous SiO276 ~ 88 parts by weight of complex microsphere, styrene
5 ~ 10 parts by weight of activated monomer, 6 ~ 12 parts by weight of ultra-high molecular weight polyethylene staple fiber, 1 ~ 2 parts by weight of initiator.
Preferably, step (2) ultrasonic frequency is 60 ~ 120kHz, and power density is 0.5 ~ 0.8w/cm2, reaction temperature
Degree is 90 ~ 130 DEG C.
Preferably, step (3) activating agent is potassium stearate, odium stearate, zinc stearate, calcium stearate, stearic acid
At least one of magnesium.
Preferably, the parts by weight of step (3) each raw material are 10 ~ 30 parts by weight of complex microsphere, polystyrene support tree
67 ~ 89 parts by weight of rouge, 1 ~ 3 parts by weight of activating agent.
The innovation of the invention consists in that passing through the porous SiO that will load graphene2Microballoon is dispersed in superhigh molecular weight polyethylene
In the mixed system of alkene staple fiber and styrene monomer, and polystyrene is generated by causing polymerization, with superhigh molecular weight polyethylene
Simultaneously masterbatch is made in alkene staple fiber mixing composition plastic alloy cladding microballoon, can be effectively improved stone when modified for polystyrene foam
The compatibility of black alkene and polystyrene overcomes graphene in the prior art and disperses in polystyrene foam plastics process
Effect difference fails to effectively improve the technological deficiency of performance.
The present invention also provides a kind of construction wall polystyrene foam graphenes that above-mentioned preparation method is prepared
Enhance masterbatch.Graphene powder is first filled in porous SiO when enhancing masterbatch by the graphene2Inside microballoon, then in ultrasound field
With surfactant to porous SiO2Microsphere surface carries out oleophylic processing, then moves into reaction kettle and styrene activity list is added
Body, ultra-high molecular weight polyethylene staple fiber, initiator etc. are passed through nitrogen protection, while more in the activation of ultrasound field, initiation etc.
SiO is realized in the lower isothermal reaction of recast2Microballoon disperses in reaction medium, while causing styrene monomer in porous SiO2Microballoon
Surface carries out polymerization reaction, collectively forms polystyrene/ultra high molecular weight polyethylene alloy alloy with ultra-high molecular weight polyethylene
Coated porous SiO2Complex microsphere mixes gained complex microsphere and polystyrene carrier resin, activating agent etc. in high mixer
After dispersion, it is granulated and is made through screw extruder.
The present invention provides a kind of construction wall polystyrene foam graphenes to enhance masterbatch and preparation method, and existing
Technology is compared, and the feature and excellent effect protruded is:
1. graphene prepared by the present invention enhances masterbatch, obvious to the reinforcing effect of construction wall polystyrene foam, it is worth pushing away
Wide application.
2. preparation method of the invention passes through polystyrene/ultra high molecular weight polyethylene alloy cladding load graphene
Porous SiO2Complex microsphere effectively improves dispersibility of the graphene in polystyrene foam matrix, avoids agglomeration.
3. preparation method of the invention, the graphene enhancing masterbatch of preparation can be obviously improved the mechanical property of material, to poly-
Styrenic foams play excellent humidification, and gained enhances modified polystyrene foam and is suitable for the engineerings such as construction wall neck
Domain.
Specific embodiment
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
By 9kg Graphene powder and the porous SiO of 89kg2Microballoon mixing, is adsorbed in circulating air driven mixer, makes graphene
Powder is filled in porous SiO2Inside microballoon, 2kg alkyl glucoside is then added is with ultrasonic frequency in ultrasound field
110kHz, power density 0.7w/cm2Ultrasonic wave to microsphere surface carry out oleophylic processing, porous SiO is made2It is compound micro-
Ball;Then by 83kg treated porous SiO2Complex microsphere moves into reaction kettle, and it is super that 7kg styrene activated monomer, 9kg is added
High molecular weight polyethylene staple fiber, 1kg azodiisobutyronitrile are passed through nitrogen protection, while being 90kHz, function in ultrasonic frequency
Rate density is 0.7w/cm2Ultrasound field activation, initiation isothermal reaction at 110 DEG C, formed polystyrene/superelevation
The porous SiO of molecular weight polyethylene alloy-coated2Complex microsphere;Then by 19kg complex microsphere and 79kg polystyrene support tree
Rouge, 2kg potassium stearate mix dispersion in a high speed mixer, are granulated through screw extruder, and graphene, which is made, enhances masterbatch.
Test method:
Graphene produced by the present invention enhancing masterbatch is prepared into polystyrene foam article according to 20% addition of mass ratio, is made
50mm × 50mm × 50mm standard sample,
Mechanical strength: carrying out on triaxial apparatus plus unloading test, confining pressure 20kPa, test speed 0.4mm/min, proving ring
Border temperature is 23 DEG C, and relative humidity 55% measures the compressive strength and elasticity modulus of material;It is measured and is tried using universal testing machine
The tensile strength of sample;It tests 3 times and obtains average value.
The data obtained is as shown in table 1.
Embodiment 2
By 5kg Graphene powder and the porous SiO of 94kg2Microballoon mixing, is adsorbed in circulating air driven mixer, makes graphene
Powder is filled in porous SiO2Inside microballoon, 1kg fatty glyceride is then added is with ultrasonic frequency in ultrasound field
80kHz, power density 0.5w/cm2Ultrasonic wave to microsphere surface carry out oleophylic processing, porous SiO is made2Complex microsphere;
Then by 88kg treated porous SiO2Complex microsphere moves into reaction kettle, and 5kg styrene activated monomer, 6kg superelevation is added
Molecular weight polyethylene staple fiber, 1kg azobisisoheptonitrile are passed through nitrogen protection, while being 60kHz, power in ultrasonic frequency
Density is 0.5w/cm2Ultrasound field activation, initiation isothermal reaction at 90 DEG C, formed polystyrene/supra polymer
The porous SiO of weight polyethylene alloy cladding2Complex microsphere;Then by 10kg complex microsphere and 89kg polystyrene carrier resin,
1kg odium stearate mixes dispersion in a high speed mixer, is granulated through screw extruder, and graphene, which is made, enhances masterbatch.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Embodiment 3
By 20kg Graphene powder and the porous SiO of 77kg2Microballoon mixing, is adsorbed in circulating air driven mixer, makes graphite
Alkene powder is filled in porous SiO2Inside microballoon, 3kg fatty acid sorbitan is then added, in ultrasound field, with ultrasonic frequency
For 150kHz, power density 0.1w/cm2Ultrasonic wave to microsphere surface carry out oleophylic processing, porous SiO is made2It is compound micro-
Ball;Then by 76kg treated porous SiO2Complex microsphere moves into reaction kettle, and 10kg styrene activated monomer, 12kg is added
Ultra-high molecular weight polyethylene staple fiber, 2kg azo-bis-iso-dimethyl are passed through nitrogen protection, while being in ultrasonic frequency
120kHz, power density 0.8w/cm2Ultrasound field activation, initiation isothermal reaction at 130 DEG C, formed polyphenyl
The porous SiO of ethylene/ultra high molecular weight polyethylene alloy cladding2Complex microsphere;Then by 30kg complex microsphere and 67kg polyphenyl
Ethylene vector resin, 3kg zinc stearate mix dispersion in a high speed mixer, are granulated through screw extruder, and graphene is made and increases
Strong masterbatch.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Embodiment 4
By 10kg Graphene powder and the porous SiO of 88kg2Microballoon mixing, is adsorbed in circulating air driven mixer, makes graphite
Alkene powder is filled in porous SiO2Inside microballoon, 2kg alkyl glucoside is then added is with ultrasonic frequency in ultrasound field
90kHz, power density 0.6w/cm2Ultrasonic wave to microsphere surface carry out oleophylic processing, porous SiO is made2Complex microsphere;
Then by 85kg treated porous SiO2Complex microsphere moves into reaction kettle, and 6kg styrene activated monomer, 8kg superelevation is added
Molecular weight polyethylene staple fiber, 1kg azodiisobutyronitrile are passed through nitrogen protection, while being 70kHz, power in ultrasonic frequency
Density is 0.6w/cm2Ultrasound field activation, initiation isothermal reaction at 100 DEG C forms polystyrene/superelevation point
The porous SiO of sub- weight polyethylene alloy cladding2Complex microsphere;Then by 15kg complex microsphere and 84kg polystyrene support tree
Rouge, 1kg calcium stearate mix dispersion in a high speed mixer, are granulated through screw extruder, and graphene, which is made, enhances masterbatch.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Embodiment 5
By 16kg Graphene powder and the porous SiO of 81kg2Microballoon mixing, is adsorbed in circulating air driven mixer, makes graphite
Alkene powder is filled in porous SiO2Inside microballoon, 3kg fatty glyceride is then added, in ultrasound field, with ultrasonic frequency
For 140kHz, power density 0.9w/cm2Ultrasonic wave to microsphere surface carry out oleophylic processing, porous SiO is made2It is compound micro-
Ball;Then by 80kg treated porous SiO2Complex microsphere moves into reaction kettle, and 8kg styrene activated monomer, 10kg is added
Ultra-high molecular weight polyethylene staple fiber, 2kg azobisisoheptonitrile are passed through nitrogen protection, while being in ultrasonic frequency
110kHz, power density 0.7w/cm2Ultrasound field activation, initiation isothermal reaction at 120 DEG C, formed polyphenyl
The porous SiO of ethylene/ultra high molecular weight polyethylene alloy cladding2Complex microsphere;Then by 25kg complex microsphere and 72kg polyphenyl
Ethylene vector resin, 3kg magnesium stearate mix dispersion in a high speed mixer, are granulated through screw extruder, and graphene is made and increases
Strong masterbatch.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Embodiment 6
By 12kg Graphene powder and the porous SiO of 86kg2Microballoon mixing, is adsorbed in circulating air driven mixer, makes graphite
Alkene powder is filled in porous SiO2Inside microballoon, 2kg fatty acid sorbitan is then added, in ultrasound field, with ultrasonic frequency
For 110kHz, power density 0.8w/cm2Ultrasonic wave to microsphere surface carry out oleophylic processing, porous SiO is made2It is compound micro-
Ball;Then by 82kg treated porous SiO2Complex microsphere moves into reaction kettle, and it is super that 8kg styrene activated monomer, 9kg is added
High molecular weight polyethylene staple fiber, 1kg azo-bis-iso-dimethyl are passed through nitrogen protection, while being in ultrasonic frequency
90kHz, power density 0.6w/cm2Ultrasound field activation, initiation isothermal reaction at 110 DEG C, formed polyphenyl second
The porous SiO of alkene/ultra high molecular weight polyethylene alloy cladding2Complex microsphere;Then by 20kg complex microsphere and 78kg polyphenyl second
Alkene vector resin, 2kg potassium stearate mix dispersion in a high speed mixer, are granulated through screw extruder, and graphene enhancing is made
Masterbatch.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Comparative example 1
Graphene enhances in masterbatch preparation process, non-synthetic polystyrene clad, other preparation conditions and embodiment 6 are consistent.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Comparative example 2
Graphene enhances in masterbatch preparation process, is not added with ultra-high molecular weight polyethylene staple fiber clad, other preparation conditions
It is consistent with embodiment 6.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Table 1:
Performance indicator | Compressive strength (kPa) | Elasticity modulus (MPa) | Tensile strength (MPa) |
Embodiment 1 | 665 | 5.62 | 0.23 |
Embodiment 2 | 656 | 5.65 | 0.21 |
Embodiment 3 | 668 | 5.64 | 0.22 |
Embodiment 4 | 662 | 5.66 | 0.24 |
Embodiment 5 | 669 | 5.62 | 0.24 |
Embodiment 6 | 658 | 5.59 | 0.23 |
Comparative example 1 | 345 | 3.98 | 0.12 |
Comparative example 2 | 465 | 4.15 | 0.16 |
Claims (10)
1. the preparation method that a kind of construction wall polystyrene foam enhances masterbatch with graphene, which is characterized in that by by stone
Black alkene powder is filled in porous SiO2Inside microballoon, and oleophylic processing is carried out, then polymerization reaction forms polystyrene/supra polymer
Weight polyethylene alloy, coated porous SiO2Complex microsphere, further with polystyrene carrier resin, activating agent mixed at high speed and squeeze
It is granulated out, graphene, which is made, enhances masterbatch, and specific step is as follows for preparation:
(1) by Graphene powder and porous SiO2Microballoon mixing, is adsorbed in circulating air driven mixer, fills out Graphene powder
It fills in porous SiO2Inside microballoon, surfactant is then added, oleophylic processing is carried out to microsphere surface in ultrasound field,
Porous SiO is made2Complex microsphere;
It (2) will treated porous SiO2Complex microsphere moves into reaction kettle, and it is poly- that styrene activated monomer, super high molecular weight is added
Ethylene staple fiber, initiator are passed through nitrogen protection, while carrying out isothermal reaction, shape under the activation of ultrasound field, initiation
At the porous SiO of polystyrene/ultra high molecular weight polyethylene alloy cladding2Complex microsphere;
(3) complex microsphere made from step (2) and polystyrene carrier resin, activating agent are mixed point in a high speed mixer
It dissipates, is granulated through screw extruder, graphene, which is made, enhances masterbatch.
2. a kind of construction wall polystyrene foam enhances the preparation method of masterbatch with graphene according to claim 1,
Be characterized in that: step (1) surfactant be alkyl glucoside, fatty glyceride, in fatty acid sorbitan at least
It is a kind of.
3. a kind of construction wall polystyrene foam enhances the preparation method of masterbatch with graphene according to claim 1,
Be characterized in that: the parts by weight of step (1) each raw material are 5 ~ 20 parts by weight of Graphene powder, porous SiO277 ~ 94 weight of microballoon
Part, 1 ~ 3 parts by weight of surfactant.
4. a kind of construction wall polystyrene foam enhances the preparation method of masterbatch with graphene according to claim 1,
Be characterized in that: the ultrasonic frequency of step (1) described ultrasound field is 80 ~ 150kHz, and power density is 0.5 ~ 1w/cm2。
5. a kind of construction wall polystyrene foam enhances the preparation method of masterbatch with graphene according to claim 1,
Be characterized in that: step (2) initiator is azodiisobutyronitrile, in azobisisoheptonitrile, azo-bis-iso-dimethyl
It is at least one.
6. a kind of construction wall polystyrene foam enhances the preparation method of masterbatch with graphene according to claim 1,
Be characterized in that: the parts by weight of step (2) each raw material are porous SiO276 ~ 88 parts by weight of complex microsphere, styrene activity are single
5 ~ 10 parts by weight of body, 6 ~ 12 parts by weight of ultra-high molecular weight polyethylene staple fiber, 1 ~ 2 parts by weight of initiator.
7. a kind of construction wall polystyrene foam enhances the preparation method of masterbatch with graphene according to claim 1,
Be characterized in that: step (2) ultrasonic frequency is 60 ~ 120kHz, and power density is 0.5 ~ 0.8w/cm2, reaction temperature 90
~130℃。
8. a kind of construction wall polystyrene foam enhances the preparation method of masterbatch with graphene according to claim 1,
Be characterized in that: step (3) activating agent is potassium stearate, in odium stearate, zinc stearate, calcium stearate, magnesium stearate
It is at least one.
9. a kind of construction wall polystyrene foam enhances the preparation method of masterbatch with graphene according to claim 1,
Be characterized in that: the parts by weight of step (3) each raw material are, 10 ~ 30 parts by weight of complex microsphere, polystyrene carrier resin 67 ~
89 parts by weight, 1 ~ 3 parts by weight of activating agent.
10. the construction wall polystyrene foam that any one of claim 1 ~ 9 preparation method is prepared is increased with graphene
Strong masterbatch.
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US12116702B2 (en) * | 2019-07-18 | 2024-10-15 | Xingyu Safety Protection Technology Co., Ltd | Ultra-high molecular weight polyethylene fiber with ultra-high cut resistance and preparation method thereof |
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2018
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---|---|---|---|---|
US20210363666A1 (en) * | 2019-07-18 | 2021-11-25 | Xingyu Safety Protection Technology Co., Ltd | Ultra-high molecular weight polyethylene fiber with ultra-high cut resistance and preparation method thereof |
US12116702B2 (en) * | 2019-07-18 | 2024-10-15 | Xingyu Safety Protection Technology Co., Ltd | Ultra-high molecular weight polyethylene fiber with ultra-high cut resistance and preparation method thereof |
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