CN108503972A - Composite polyethylene material and preparation method thereof - Google Patents
Composite polyethylene material and preparation method thereof Download PDFInfo
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- CN108503972A CN108503972A CN201810190922.1A CN201810190922A CN108503972A CN 108503972 A CN108503972 A CN 108503972A CN 201810190922 A CN201810190922 A CN 201810190922A CN 108503972 A CN108503972 A CN 108503972A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions 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 a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions 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 a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions 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 a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/066—LDPE (radical process)
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Abstract
The present invention relates to a kind of composite polyethylene materials and preparation method thereof.The composite polyethylene material, in parts by weight, including the following raw material component：60 100 parts of polyvinyl resin, modified 0.1 15 parts of white graphite alkene, 0.1 10 parts of white oil, 0.1 20 parts of dispersant；Wherein, the modified white graphite alkene is the white graphite alkene of polymer overmold modification, and the polymerized monomer of the polymer is styrene or acrylic ester monomer.The composite polyethylene material has both excellent mechanical strength and impact flexibility, while also having preferable ageing resistance and wearability, and the transparent easy coloring of color, need not add excessive auxiliary agent reinforcement, formula is simple, application range and wide market.
Description
Technical field
The present invention relates to plastic materials, more particularly to a kind of composite polyethylene material and preparation method thereof.
Background technology
Polyethylene (PE) is that structure is most simple in plastics, a kind of high molecular material for being most widely used, and polyethylene is because of nothing
It is smelly, nontoxic, chemical stability is good, under room temperature insoluble in common solvent, hygroscopicity is small and resistance to most of acid and alkali corrosions, insulating properties
The characteristics such as good are widely used in the industries such as plastic pipe, film, electric wire.But the intensity of polyethylene is not high, impact resistance
The defects of energy difference and poor heat-resisting anti-aging property, also limits further extensive use.Therefore raising is modified to PE plastics
Rigid toughness ageing resistance is imperative.
Previous research mostly uses elastomer or inorganic rigid particle is modified PE.It, can be with by elastomer-modified PE
Significantly improve the impact flexibility of modified PE, but mechanical strength is declined it is obvious that in addition, be modified to PE using elastomer, is
Improve processing performance, it is also necessary to be aided with antioxidant, formula is complicated and processing technology is more difficult to control；It is modified using inorganic rigid particle
PE can significantly improve PE mechanical strengths, but impact flexibility increase rate is still little, and exist when inoganic particle modified PE and fill out
Charge is big, causes expressing technique complicated, product appearance defect is more.
Also part research carries out crosslinking reinforcement by further adding coupling agent, crosslinking agent etc. in PE to PE, but rushes
Hit intensity increase rate is still limited, and is formulated and is complicated with production technology, it is difficult to adapt to market and actual production demand.
Invention content
Based on this, it is necessary to provide a kind of composite polyethylene material.It is strong that the composite polyethylene material has both excellent mechanics
Degree and impact flexibility, while also there is preferable ageing resistance and wearability, and the transparent easy coloring of color, it need not add
More auxiliary agent reinforcement, formula is simple, application range and wide market.
A kind of composite polyethylene material, in parts by weight, including the following raw material component：
Wherein, the modified white graphite alkene is the white graphite alkene of polymer overmold modification, the polymerized monomer of the polymer
For styrene or acrylic ester monomer.
The composite polyethylene material in one of the embodiments, in parts by weight, including the following raw material component：
The composite polyethylene material in one of the embodiments, in parts by weight, including the following raw material component：
In one of the embodiments, the acrylic ester monomer be acrylic acid, methyl acrylate, ethyl acrylate,
At least one of hydroxy-ethyl acrylate, butyl acrylate, methyl methacrylate, glycidyl methacrylate.
The polymerized monomer of the polymer is methyl methacrylate, methyl acrylate, third in one of the embodiments,
At least one of olefin(e) acid hydroxyl ethyl ester.
The white graphite alkene is 1-20 layers of white graphite alkene in one of the embodiments,.
The modified white graphite alkene is prepared by the method included the following steps in one of the embodiments,：
In a solvent by the dispersion of white graphite alkene, lipophilic stabilizer is added and carries out oleophylic processing, obtain the dispersion of white graphite alkene
Liquid；
The white graphite alkene dispersion liquid is warming up to 60~120 DEG C, initiator is added, stirs 10-30min；Add institute
The polymerized monomer for stating polymer, is stirred to react 0.5-2h；The pH for adjusting gained reaction solution is 7-8, and filter residue is collected in filtering；Obtain institute
State modified white graphite alkene.
The stabilizer is polyvinylpyrrolidone, sodium alkyl sulfate, alkyl benzene sulphonate in one of the embodiments,
At least one of sodium, oleyl amine, oleic acid.
The solvent is water, ethyl alcohol, ethylene glycol, glycerine, ethyl acetate, butyl acetate in one of the embodiments,
At least one of.
The initiator is at least one of ammonium persulfate, azodiisobutyronitrile in one of the embodiments,.
The polymerized monomer of the polymer first carries out vacuum distillation processing before being added in one of the embodiments,.
The modified white graphite alkene is prepared by the method included the following steps in one of the embodiments,：
In parts by weight, in a solvent by 20 parts of white graphite alkene dispersions, 0.1-5 parts of lipophilic stabilizers are added and carry out parent
Oil processing obtains white graphite alkene dispersion liquid；
In parts by weight, the 1-20 parts of white graphite alkene dispersion liquids are warming up to 60~120 DEG C, 1-5 parts of initiators are added,
Stir 10-30min；The polymerized monomer for adding the 0.1-10 parts of polymer, is stirred to react 0.5-2h；Adjust gained reaction solution
PH be 7-8, filtering, collect filter residue；Obtain the modified white graphite alkene.
The polyvinyl resin is low density polyethylene (LDPE) (LDPE), medium density polyethylene in one of the embodiments,
(MDPE), high density polyethylene (HDPE) (HDPE), linear low density polyethylene (LLDPE), crosslinked polyethylene (X-PE), the poly- second of metallocene
At least one of alkene (m-PE).Preferably low density polyethylene (LDPE) (LDPE), medium density polyethylene (MDPE), high density polyethylene (HDPE)
At least one of (HDPE).
The white oil is 1# white oils, 3# white oils, 5# white oils, 7# white oils, 10# white oils, 15# in one of the embodiments,
At least one of white oil, 26# white oils, 36# white oils, 46# white oils.Can be industrial grade white oil or food-level white oil.Preferably 7#
At least one of white oil, 15# white oils, 36# white oils.
The dispersant is paraffin, polyethylene wax, zinc stearate, calcium stearate, stearic acid in one of the embodiments,
At least one of barium, pentaerythritol stearate.Preferably at least one of polyethylene wax, calcium stearate.
The present invention also provides the preparation methods of the composite polyethylene material, include the following steps：
The polyvinyl resin, modified white graphite alkene, white oil, dispersant are premixed, gained pre-composition is through being kneaded, squeezing
Go out to get the composite polyethylene material.
The premix is carried out using high-speed mixer in one of the embodiments, the heating temperature of the high-speed mixer
Degree is 60-120 DEG C, and each material is mixed with 300-1800r/min rotating speeds to be disperseed, time 5-30min.
Described squeeze out is carried out using double screw extruder in one of the embodiments, each area of double screw extruder
Temperature range is 160-230 DEG C, and head temperature is 170-240 DEG C, engine speed 160-480r/min.
Compared with prior art, the invention has the advantages that：
The composite polyethylene material of the present invention, on the basis of reasonable preparation each raw material component forms, using polymer packet
The white graphite alkene cooperation white oil for covering modification is compound to polyvinyl resin progress, wherein uses styrene or acrylic ester monomer
The polymer dialogue graphene being polymerized carries out the modified graphene obtained by coating decoration, coordinates the addition of white oil, utilizes it
Adhesiveness improves the uniform dispersion of system, can form good compatibility with PE matrixes, and can also uniformly intercalation in PE bases
Suitable lamella network structure is formed in body, to absorb and release again while so that the compound PE materials of acquisition is reached enhancing
Impact energy is put, the mechanical strength and impact flexibility of material are improved, and then reaches and improves impact resistance purpose.In addition, after compound
PE materials while activeness and quietness, wearability and thermal oxidative aging can be also improved, and product is transparent and is easy
Color.
In addition, the composite polyethylene material of the present invention, formula is simple, without additionally adding coupling agent, crosslinking agent, antioxygen
On the basis of the auxiliary agents such as agent, you can realize excellent mechanical strength and impact flexibility, can individually carry out the preparation of plastic products
It can also be used as master batch and be further crosslinked use, application range and wide market.
Specific implementation mode
The composite polyethylene material and preparation method thereof of the present invention is made below in conjunction with specific embodiment further details of
Explanation.
Embodiment 1
A kind of composite polyethylene material of the present embodiment is grouped as by the following raw material group in parts by weight：
Wherein, the modified white graphite alkene is the white graphite alkene of polymer overmold modification, the polymerized monomer of the polymer
For methyl methacrylate；The preparation method of the modified white graphite alkene is as follows：
It takes 2-10 layers of 20 parts of white graphite alkene powder to be added into round-bottomed flask, and 100mL distillations is added into round-bottomed flask
Water, then ultrasonic disperse, 0.2 part of lauryl sodium sulfate is added into round-bottomed flask, and ultrasonic high-speed stirred obtains oleophylic modification
White graphite alkene；
After the white graphite alkene dispersion liquid that 10 parts of oleophylics are modified is heated to 85 DEG C, 1 part of initiator ammonium persulfate, stirring is added
Start that 1 part of methyl methacrylate (first carrying out vacuum distillation processing before being added dropwise) is added dropwise after 10min, 0.5h is dripped off；It is added dropwise
Afterwards, heat preservation 30min waits for that reaction is completed；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, and is used
Distill primary with ethanol wash after water washing filter cake 3~4 times, and vacuum drying grinding obtains poly-methyl methacrylate at 60 DEG C
The white graphite alkene of ester coating decoration.
The preparation method of above-mentioned composite polyethylene material is as follows：
The resin premixed conjunction dispersions of step 1) white graphite alkene/PE：High-speed mixer heating temperature is stablized after 80 DEG C, by weight
Amount number weighs 96 parts of LDPE resins, 1 part of modified white graphite alkene, 1 part of 7# industrial grade white oil, 2 parts of polyethylene waxes through high speed respectively
Blender (rotating speed 1800r/min) premixing dispersion 5min dischargings；
Step 2) composite polyethylene material preparation：By each area's stable temperature control of double screw extruder in 170-210 DEG C, machine
Head stable temperature control is added to twin-screw after 220 DEG C, by 100 parts of scattered mixtures of premixing that step 1) obtains and squeezes
Go out in machine barrel, engine speed 210r/min, it is (multiple to obtain composite polyethylene material through mixing, extrusion, water cooling, tie rod pelletizing
Close PE master batches).
Embodiment 2
A kind of composite polyethylene material of the present embodiment is grouped as by the following raw material group in parts by weight：
Wherein, the modified white graphite alkene is the white graphite alkene of polymer overmold modification, the polymerized monomer of the polymer
For methyl acrylate；The preparation method of the modified white graphite alkene is as follows：
It takes 2-10 layers of 20 parts of white graphite alkene powder to be added into round-bottomed flask, and 100mL ethyl alcohol is added into round-bottomed flask,
Then ultrasonic disperse, 0.5 part of lauryl sodium sulfate is added into round-bottomed flask, and ultrasonic high-speed stirred obtains oleophylic and is modified in vain
Graphene；
After the white graphite alkene dispersion liquid that 15 parts of oleophylics are modified is heated to 90 DEG C, 1 part of initiator ammonium persulfate, stirring is added
Start that 1 part of methyl acrylate (first carrying out vacuum distillation processing before being added dropwise) is added dropwise after 10min, 0.5h is dripped off；After being added dropwise, protect
Warm 45min waits for that reaction is completed；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, with distillation
It is primary with ethanol wash after water washing filter cake 3~4 times, and vacuum drying grinding obtains polymethyl acrylate cladding and repaiies at 70 DEG C
The white graphite alkene of decorations.
The preparation method of above-mentioned composite polyethylene material is as follows：
The resin premixed conjunction dispersions of step 1) white graphite alkene/PE：High-speed mixer heating temperature is stablized after 90 DEG C, by weight
Amount number weighs 89 parts of MDPE resins, 3 parts of modified white graphite alkene, 3 parts of 15# industrial grade white oils, 5 parts of polyethylene waxes through high speed respectively
Blender (rotating speed 1000r/min) premixing dispersion 10min dischargings；
Step 2) composite polyethylene material preparation：By each area's stable temperature control of double screw extruder in 180-220 DEG C, machine
Head stable temperature control is added to twin-screw after 225 DEG C, by 100 parts of scattered mixtures of premixing that step 1) obtains and squeezes
Go out in machine barrel, engine speed 300r/min, it is (multiple to obtain composite polyethylene material through mixing, extrusion, water cooling, tie rod pelletizing
Close PE master batches).
Embodiment 3
A kind of composite polyethylene material of the present embodiment is grouped as by the following raw material group in parts by weight：
Wherein, the modified white graphite alkene is the white graphite alkene of polymer overmold modification, the polymerized monomer of the polymer
For hydroxy-ethyl acrylate；The preparation method of the modified white graphite alkene is as follows：
It takes 20 parts of 2-10 layers of white graphite alkene powder to be added into round-bottomed flasks, and 100mL the third three is added into round-bottomed flask
Alcohol, then ultrasonic disperse, 1 part of oleyl amine is added 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 20 parts of oleophylics are modified is heated to 90 DEG C, 1 part of initiator azodiisobutyronitrile is added,
Start that 5 parts of hydroxy-ethyl acrylates (first carrying out vacuum distillation processing before being added dropwise) are added dropwise after stirring 10min, 0.5h is dripped off；It drips
Bi Hou, heat preservation 60min wait for that reaction is completed；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,
It is washed with distilled water primary with ethanol wash after filter cake 3~4 times, and vacuum drying grinding obtains polyacrylic acid hydroxyl second at 90 DEG C
The white graphite alkene of ester coating decoration.
The preparation method of above-mentioned composite polyethylene material is as follows：
The resin premixed conjunction dispersions of step 1) white graphite alkene/PE：High-speed mixer heating temperature is stablized after 90 DEG C, by weight
Amount number weighs 85 parts of HDPE resins, 5 parts of modified white graphite alkene, 4 parts of 36# food-level white oils, 6 parts of calcium stearates through high speed respectively
Blender (rotating speed 300r/min) premixing dispersion 15min dischargings；
Step 2) composite polyethylene material preparation：By each area's stable temperature control of double screw extruder in 185-225 DEG C, machine
Head stable temperature control is added to twin-screw after 225 DEG C, by 100 parts of scattered mixtures of premixing that step 1) obtains and squeezes
Go out in machine barrel, engine speed 360r/min, it is (multiple to obtain composite polyethylene material through mixing, extrusion, water cooling, tie rod pelletizing
Close PE master batches).
Comparative example 1
A kind of composite polyethylene material of this comparative example, raw material components and preparation method similar embodiment 3, difference lies in：
Described 5 parts modified white graphite alkene are substituted with 4 parts of elastomeric EP DM and 1 part of phenol antioxidant 1010.
Comparative example 2
A kind of composite polyethylene material of this comparative example, raw material components and preparation method similar embodiment 3, difference lies in：
Only to carry out oleophylic modification, the white graphite alkene for not carrying out polymer overmold modification substitutes 5 parts of modified white graphite alkene.
The composite polyethylene material of embodiment 1-3 and comparative example 1-2 are tested for the property, the results are shown in Table 1：
Table 1
Each technical characteristic of embodiment described above can be combined arbitrarily, to keep description succinct, 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, it is all considered to be the range of this specification record.
Several embodiments of the invention above described embodiment only expresses, 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 the protection of the present invention
Range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of composite polyethylene material, which is characterized in that in parts by weight, including the following raw material component：
Wherein, the modified white graphite alkene is the white graphite alkene of polymer overmold modification, and the polymerized monomer of the polymer is benzene
Ethylene or acrylic ester monomer.
2. composite polyethylene material according to claim 1, which is characterized in that in parts by weight, including the following raw material group
Point：
3. composite polyethylene material according to claim 1, which is characterized in that the polymerized monomer of the polymer is selected from first
At least one of base methyl acrylate, methyl acrylate, hydroxy-ethyl acrylate.
4. composite polyethylene material according to claim 1, which is characterized in that the white graphite alkene is 1-20 layers of white graphite
Alkene.
5. composite polyethylene material according to claim 1, which is characterized in that the modified white graphite alkene is by including as follows
The method of step is prepared：
In a solvent by the dispersion of white graphite alkene, lipophilic stabilizer is added and carries out oleophylic processing, obtain white graphite alkene dispersion liquid；
The white graphite alkene dispersion liquid is warming up to 60~120 DEG C, initiator is added, stirs 10-30min；It adds described poly-
The polymerized monomer for closing object, is stirred to react 0.5-2h；The pH for adjusting gained reaction solution is 7-8, and filter residue is collected in filtering；Obtain described change
Property white graphite alkene.
6. composite polyethylene material according to claim 5, which is characterized in that the stabilizer is polyvinylpyrrolidine
At least one of ketone, sodium alkyl sulfate, sodium alkyl benzene sulfonate, oleyl amine, oleic acid.
7. according to claim 1-6 any one of them composite polyethylene materials, which is characterized in that the polyvinyl resin is
The poly- second of low density polyethylene (LDPE), medium density polyethylene, high density polyethylene (HDPE), linear low density polyethylene, crosslinked polyethylene, metallocene
At least one of alkene；
The white oil is 1# white oils, 3# white oils, 5# white oils, 7# white oils, 10# white oils, 15# white oils, 26# white oils, 36# white oils, 46#
At least one of white oil；
The dispersant is in paraffin, polyethylene wax, zinc stearate, calcium stearate, barium stearate, pentaerythritol stearate
It is at least one.
8. the preparation method of claim 1-7 any one of them composite polyethylene materials, which is characterized in that including walking as follows
Suddenly：
The polyvinyl resin, modified white graphite alkene, white oil, dispersant are premixed, gained pre-composition through being kneaded, squeezing out,
Up to the composite polyethylene material.
9. the preparation method of composite polyethylene material according to claim 8, which is characterized in that the premix is using high speed
Mixing machine carries out, and the heating temperature of the high-speed mixer is 60-120 DEG C, and each material is with the mixing point of 300-1800r/min rotating speeds
It dissipates, time 5-30min.
10. the preparation method of composite polyethylene material according to claim 8 or claim 9, which is characterized in that the extrusion uses
Double screw extruder carries out, and each area's temperature range of double screw extruder is 160-230 DEG C, and head temperature is 170-240 DEG C,
Engine speed is 160-480r/min.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109851960A (en) * | 2019-02-19 | 2019-06-07 | 广东烯王科技有限公司 | A kind of compound PTFE material of white graphite alkene and preparation method thereof |
| CN109880222A (en) * | 2019-02-19 | 2019-06-14 | 广东烯王科技有限公司 | A kind of compound PE material of white graphite alkene, film and preparation method thereof |
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| CN105860315A (en) * | 2016-06-14 | 2016-08-17 | 辽宁大学 | Preparing method of hexagonal boron nitride/polystyrene composite |
| CN107383545A (en) * | 2016-08-22 | 2017-11-24 | 广东纳路纳米科技有限公司 | A kind of modified white graphite alkene composite polyethylene pipe and preparation method thereof |
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- 2018-03-08 CN CN201810190922.1A patent/CN108503972A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105860315A (en) * | 2016-06-14 | 2016-08-17 | 辽宁大学 | Preparing method of hexagonal boron nitride/polystyrene composite |
| CN107383545A (en) * | 2016-08-22 | 2017-11-24 | 广东纳路纳米科技有限公司 | A kind of modified white graphite alkene composite polyethylene pipe and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109851960A (en) * | 2019-02-19 | 2019-06-07 | 广东烯王科技有限公司 | A kind of compound PTFE material of white graphite alkene and preparation method thereof |
| CN109880222A (en) * | 2019-02-19 | 2019-06-14 | 广东烯王科技有限公司 | A kind of compound PE material of white graphite alkene, film and preparation method thereof |
| CN109851960B (en) * | 2019-02-19 | 2021-01-26 | 广东烯王科技有限公司 | White graphene composite PTFE material and preparation method thereof |
| CN109880222B (en) * | 2019-02-19 | 2021-07-06 | 广东烯王科技有限公司 | White graphene composite PE material, film and preparation method thereof |
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Application publication date: 20180907 |