CN109054189A - A kind of plant composite fibre filling polypropylene composite material and preparation method thereof - Google Patents
A kind of plant composite fibre filling polypropylene composite material and preparation method thereof Download PDFInfo
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- CN109054189A CN109054189A CN201810935961.XA CN201810935961A CN109054189A CN 109054189 A CN109054189 A CN 109054189A CN 201810935961 A CN201810935961 A CN 201810935961A CN 109054189 A CN109054189 A CN 109054189A
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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
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/14—Copolymers of propene
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
- C08L2205/16—Fibres; Fibrils
Abstract
The present invention relates to a kind of plant composite fibre filling polypropylene composite materials and preparation method thereof.A kind of plant composite fibre filling polypropylene composite material, raw material is grouped as by following group by weight percentage: 42~64% copolymer polypropylene, 6~18% homopolypropylene, 5~18% plant powders, 0~5% inorganic mineral filler, 1~5% elastomer, 0.8~3% expanding material, 0.2~0.6% coupling agent, 0.1~0.3% antioxidant, 10~28% polyester resin, 0.01~0.03% epoxy resin, 0.03~0.08% graphene.
Description
Technical field
The present invention relates to a kind of plant composite fibre filling polypropylene composite material and preparation method thereof, belong to polypropylene and its
Composite material environmental protection, Lightweight Technology field.
Background technique
There is the improperly processing mode such as discarded, burning with wood structure agricultural crop straw the most similar, for environment
Protection and the utilization of resource have negative consequence.Plant fiber is due to itself fatal defects, such as in irregular shape, fault of construction
It is more, it is very poor with polymer-based compatability, cause composite material combination property poor, is of limited application.
Mainstream polypropylene composites defect is big at present, poor mechanical property, poor fluidity, rough surface, only
It can apply to low-end product.
The present invention develops while ensuring excellent mechanical property and appearance, has lower density, more stable
The polypropylene composites of fluidity of molten realize automobile-used high molecular material environmental protection, light-weighted purpose.
Summary of the invention
To solve the above problems, the purpose of the present invention is to provide a kind of plant composite fibre filled polypropylene composite woods
Material, it is ensured that while excellent mechanical property and appearance, there is lower density, more stable fluidity of molten.
Another object of the present invention is to provide a kind of preparation methods of plant composite fibre filling polypropylene composite material.
The technical solution used in the present invention is:
A kind of plant composite fibre filling polypropylene composite material, it is characterised in that raw material is by as follows by weight percentage
Group is grouped as: 42~64% copolymer polypropylene, 6~18% homopolypropylene, 5~18% plant powders, 0~5% inorganic mineral
Filler, 1~5% elastomer, 0.8~3% expanding material, 0.2~0.6% coupling agent, 0.1~0.3% antioxidant, 10~28% are gathered
Ester resin, 0.01~0.03% epoxy resin, 0.03~0.08% graphene.
Further, the plant powder is at least one of straw powder, bamboo powder, wood powder.
Further, the inorganic mineral filler is hollow glass micropearl, and average grain diameter is 0.8~85 micron, specific surface
9~17m2/g of product.
Further, the elastomer is at least one of POE, EPDM, SBS, SEBS.
Further, the expanding material is at least one of SEBS-g-MAH, PP-g-MAH, POE-g-MAH.
Further, the coupling agent is silane coupling agent KH560.
Further, the antioxidant is antioxidant 1010.
A kind of preparation method of plant composite fibre filling polypropylene composite material as described in claim 1, feature exist
In including the following steps:
(1) plant powder is added in high-speed mixer with the ethanol solution containing 1~3wt% coupling agent and is mixed, gradually
The solution containing 1% epoxy resin and 3% graphene is added, continues to stir 30 minutes under the conditions of 85 DEG C, obtains stone after dry
Black alkene coats plant powder filler, and the graphene coated plant powder packing material size range is 15 microns -110 microns;
(2) graphene coated plant powder filler and polyester resin are subjected to melt blending, by blend dimethyl methyl
Spinning, drying are carried out after amide solvent dissolution, composite fibre is formed, composite fibre is ground in ball mill, is fabricated to
Plant composite fibre powder, the length range of the plant composite fibre powder are 22 microns -285 microns, draw ratio 130:1
~240:1;
(3) when there is inorganic mineral filler in raw material, by inorganic mineral filler, polypropylene, elastomer with containing 1~
The ethanol solution of 3wt% coupling agent mixes 3~8 minutes in high speed mixer, and 50~70 DEG C of temperature;When not inorganic in raw material
When mineral filler, polypropylene, elastomer are mixed 3~8 minutes in high speed mixer, 50~70 DEG C of temperature;
(4) material and expanding material, antioxidant that step (2), (3) obtain are placed in double screw extruder, are squeezed through melting
Out, it is granulated.
Further, by weight, plant powder in step (1): solution 5:1.
Further, by weight, graphene coated plant powder filler in step (2): polyester resin: dimethyl methyl
Amide solvent is 1:2:12.
The beneficial effects of the present invention are: having lower while ensuring composite material excellent mechanical property and appearance
Density, more stable fluidity of molten, density be lower than 0.99g/cm3.It is handled by the spinning of plant fiber, it is overcome not advise
Then bring fills problem the disadvantages of shape, defect, has not only improved the intensity of PP composite material, but also reduce polypropylene composite materials
The density of material;Plant fiber powder with certain draw ratio, so that composite material shrinking percentage obtains control and modulus obtains
It is promoted;Plant fiber powder aligns the mobility enhanced under PP composite material molten condition;Hollow glass is micro-
The nucleating effect of pearl makes composite material strength get a promotion.
Specific embodiment
The present invention is further illustrated combined with specific embodiments below, and however, it is not limited to this.
Embodiment 1
Plant composite fibre filling polypropylene composite material is as follows:
(1) 3 grams of silane coupling agent KH560 are configured to the coupling agent ethanol solution of 1~3wt%;By 100 grams of straw powder with
Mixing, is gradually added into containing 1% epoxy resin and 3% in 150 grams of addition high-speed mixers of prepared coupling agent ethanol solution
20 grams of the solution (epoxy resin is uncured resin, and solvent is butanol, it is also possible to cyclohexanone or dehydrated alcohol etc.) of graphene, holds
Continue and stirred 30 minutes under the conditions of 85 DEG C, obtains graphene coated plant powder filler, the graphene coated plant after dry
Powder filler particle size range is 15 microns -110 microns;
(2) graphene coated plant powder filler and 200 grams of polyester resin are subjected to melt blendings, by blend with 1200
Spinning, drying are carried out after the dissolution of gram solvent dimethylformamide, forms composite fibre;Composite fibre is ground in ball mill
Mill, is fabricated to plant composite fibre powder, the plant composite fibre powder length range is 22 microns -285 microns, draw ratio
For 130:1~240:1's;
(3) 700 grams of copolymer polypropylene, 150 grams of homopolypropylene, 30 grams of POE are mixed 3~8 points in high speed mixer
Clock, 50~70 DEG C of temperature;
(4) material and 15 grams of POE-g-MAH, 2 grams of antioxidant 1010s that step (2), (3) obtain are placed in twin-screw extrusion
In machine, through melting extrusion, it is granulated.
Wherein, the screw slenderness ratio of all double screw extruders is 48:1, in the double screw extruder of point nine area's temperature controls into
Row extruding pelletization, one to nine area's processing temperature is successively are as follows: and 185 DEG C, 191 DEG C, 187 DEG C, 190 DEG C, 193 DEG C, 197 DEG C, 192 DEG C,
195 DEG C, 198 DEG C, 202 DEG C of head temperature, host 28~38HZ of frequency, feeding 22~28HZ of frequency, melt pressure 2.9~
3.8MPa, vacuum degree -0.03~-0.06MPa, 370~470rpm of pelleter revolving speed.
Embodiment 2
Plant composite fibre filling polypropylene composite material is as follows:
(1) 4.5g silane coupling agent KH560 is configured to the coupling agent ethanol solution of 1~3wt%;By 105 grams of straw powders,
30 grams of bamboo powders, 15 grams of wood powders are added in high-speed mixer with prepared coupling agent ethanol solution and mix, and are gradually added into containing 1%
Epoxy resin and 3% graphene 30 grams of solution (epoxy resin is uncured resin, and solvent is butanol, it is also possible to cyclohexanone or
Dehydrated alcohol etc.), continue to stir 30 minutes under the conditions of 85 DEG C, obtains graphene coated plant powder filler after dry, it is described
Graphene coated plant powder packing material size range is 15 microns -110 microns;
(2) graphene coated plant powder filler and 300 grams of polyester resin are subjected to melt blendings, by blend with 1800
Spinning, drying are carried out after the dissolution of gram solvent dimethylformamide, forms composite fibre;Composite fibre is ground in ball mill
Mill, being fabricated to length range is 22 microns -285 microns, and draw ratio is the plant composite fibre powder of 130:1~240:1;
(3) 1.5 grams of silane coupling agent KH560 are configured to the coupling agent ethanol solution of 1~3wt%;By 50 grams of hollow glass
Glass microballon, 630 grams of copolymer polypropylene, 100 grams of homopolypropylene, 32 grams of EPDM and prepared coupling agent ethanol solution are in high speed
It is mixed in batch mixer 3~8 minutes, 50~70 DEG C of temperature;
(4) material and 30 grams of PP-g-MAH, 2 grams of antioxidant 1010s that step (2), (3) obtain are placed in twin-screw extrusion
In machine, through melting extrusion, it is granulated.
Wherein, the screw slenderness ratio of all double screw extruders is 48:1, in the double screw extruder of point nine area's temperature controls into
Row extruding pelletization, one to nine area's processing temperature is successively are as follows: and 185 DEG C, 191 DEG C, 187 DEG C, 190 DEG C, 193 DEG C, 197 DEG C, 192 DEG C,
195 DEG C, 198 DEG C, 202 DEG C of head temperature, host 28~38HZ of frequency, feeding 22~28HZ of frequency, melt pressure 2.9~
3.8MPa, vacuum degree -0.03~-0.06MPa, 370~470rpm of pelleter revolving speed.
Embodiment 3
Plant composite fibre filling polypropylene composite material is as follows:
(1) 2.4 grams of silane coupling agent KH560 are configured to the ethanol solution containing 1~3wt% coupling agent;By 64 grams of straw
Is mixed in stalk powder, 16 grams of wood powders and 120 grams of addition high-speed mixers of prepared coupling agent ethanol solution, be gradually added into containing
(epoxy resin is uncured resin to 16 grams of the solution of 1% epoxy resin and 3% graphene, and solvent is butanol, it is also possible to cyclohexanone
Or dehydrated alcohol etc.), continue to stir 30 minutes under the conditions of 85 DEG C, obtains graphene coated plant powder filler, institute after dry
Stating graphene coated plant powder packing material size range is 15 microns -110 microns;
(2) graphene coated plant powder filler and 160 grams of polyester resin are subjected to melt blendings, by blend with 960
Spinning, drying are carried out after the dissolution of gram solvent dimethylformamide, forms composite fibre;Composite fibre is ground in ball mill
Mill, is fabricated to plant composite fibre powder, the length range of the plant composite fibre powder is 22 microns -285 microns, major diameter
Than for 130:1~240:1;
(3) 0.6 gram of silane coupling agent KH560 is configured to the coupling agent ethanol solution of 1~3wt%, by 20 grams of hollow glass
Glass microballon, 740 grams of copolymer polypropylene, 120 grams of homopolypropylene, 22 grams of SEBS and prepared coupling agent ethanol solution are in high speed
It is mixed in batch mixer 3~8 minutes, 50~70 DEG C of temperature;
(4) material and 13 grams of SEBS-g-MAH, 2 grams of antioxidant 1010s that step (2), (3) obtain twin-screw is placed in squeeze
Out in machine, through melting extrusion, it is granulated.
Wherein, the screw slenderness ratio of all double screw extruders is 48:1, in the double screw extruder of point nine area's temperature controls into
Row extruding pelletization, one to nine area's processing temperature is successively are as follows: and 185 DEG C, 191 DEG C, 187 DEG C, 190 DEG C, 193 DEG C, 197 DEG C, 192 DEG C,
195 DEG C, 198 DEG C, 202 DEG C of head temperature, host 28~38HZ of frequency, feeding 22~28HZ of frequency, melt pressure 2.9~
3.8MPa, vacuum degree -0.03~-0.06MPa, 370~470rpm of pelleter revolving speed.
Embodiment 4
Plant composite fibre filling polypropylene composite material is as follows:
(1) 5.4 grams of silane coupling agent KH560 are configured to the ethanol solution containing 1~3wt% coupling agent;By 108 grams of straw
It is mixed in stalk powder, 39.6 grams of bamboo powders, 32.4 grams of wood powders and 270 grams of addition high-speed mixers of prepared coupling agent ethanol solution,
Be gradually added into containing 1% epoxy resin and 3% graphene 36 grams of solution (epoxy resin is uncured resin, and solvent is butanol,
Cyclohexanone or dehydrated alcohol etc. can also be used), continue to stir 30 minutes under the conditions of 85 DEG C, obtains graphene coated plant after dry
Powder filler;The graphene coated plant powder packing material size range is 15 microns -110 microns;
(2) graphene coated plant powder filler and 360 grams of polyester resin are subjected to melt blendings, by blend with 2160
Spinning, drying are carried out after the dissolution of gram solvent dimethylformamide, forms composite fibre;Composite fibre is ground in ball mill
Mill, is fabricated to plant composite fibre powder, the length range of the plant composite fibre powder is 22 microns -285 microns, major diameter
Than for 130:1~240:1;
(3) 0.6 gram of silane coupling agent KH560 is configured to the coupling agent ethanol solution of 1~3wt%, by 20 grams of hollow glass
Glass microballon, 580 grams of copolymer polypropylene, 140 grams of homopolypropylene, 42 grams of POE and prepared coupling agent ethanol solution are in high speed
It is mixed in batch mixer 3~8 minutes, 50~70 DEG C of temperature;
(4) material and 30 grams of POE-g-MAH, 2 grams of antioxidant 1010s that step (2), (3) obtain are placed in twin-screw extrusion
In machine, through melting extrusion, it is granulated.
Wherein, the screw slenderness ratio of all double screw extruders is 48:1, in the double screw extruder of point nine area's temperature controls into
Row extruding pelletization, one to nine area's processing temperature is successively are as follows: and 185 DEG C, 191 DEG C, 187 DEG C, 190 DEG C, 193 DEG C, 197 DEG C, 192 DEG C,
195 DEG C, 198 DEG C, 202 DEG C of head temperature, host 28~38HZ of frequency, feeding 22~28HZ of frequency, melt pressure 2.9~
3.8MPa, vacuum degree -0.03~-0.06MPa, 370~470rpm of pelleter revolving speed.
Embodiment 5
Plant composite fibre filling polypropylene composite material is as follows:
(1)) 1.8 grams of silane coupling agent KH560 are configured to the ethanol solution containing 1~3wt% coupling agent;By 60 grams of straw
It mixes, is gradually added into containing 1% epoxy resin in stalk powder and 90 grams of addition high-speed mixers of prepared coupling agent ethanol solution
(epoxy resin is uncured resin, and solvent is butanol, it is also possible to cyclohexanone or dehydrated alcohol with 12 grams of the solution of 3% graphene
Deng), continue to stir 30 minutes under the conditions of 85 DEG C, obtains graphene coated plant powder filler after dry;The graphene packet
Covering plant powder packing material size range is 15 microns -110 microns;
(2) graphene coated plant powder filler and 120 grams of polyester resin are subjected to melt blendings, by blend with 720
Spinning, drying are carried out after the dissolution of gram solvent dimethylformamide, forms composite fibre;Composite fibre is ground in ball mill
Mill, is fabricated to plant composite fibre powder, the length range of the plant composite fibre powder is 22 microns -285 microns, major diameter
Than for 130:1~240:1;
(3) 1.2 grams of silane coupling agent KH560 are configured to the coupling agent ethanol solution of 1~3wt%, by 40 grams of hollow glass
Glass microballon, 660 grams of copolymer polypropylene, 180 grams of homopolypropylene, 45 grams of SBS and prepared coupling agent ethanol solution are in high speed
It is mixed in batch mixer 3~8 minutes, 50~70 DEG C of temperature;
(4) material and 10 grams of PP-g-MAH, 2 grams of antioxidant 1010s that step (2), (3) obtain are placed in twin-screw extrusion
In machine, through melting extrusion, it is granulated.
Wherein, the screw slenderness ratio of all double screw extruders is 48:1, in the double screw extruder of point nine area's temperature controls into
Row extruding pelletization, one to nine area's processing temperature is successively are as follows: and 185 DEG C, 191 DEG C, 187 DEG C, 190 DEG C, 193 DEG C, 197 DEG C, 192 DEG C,
195 DEG C, 198 DEG C, 202 DEG C of head temperature, host 28~38HZ of frequency, feeding 22~28HZ of frequency, melt pressure 2.9~
3.8MPa, vacuum degree -0.03~-0.06MPa, 370~470rpm of pelleter revolving speed.
The composite material of preparation is tested for the property, as a result as described in Table 1.
The method for carrying out various performance tests to the sample prepared in above-described embodiment 1~5 is as follows:
Specific gravity is detected by ASTM D792 standard;
Shrinking percentage (MD) is detected by ASTM D995 standard;
Melt index is detected by ASTM D1238 (230 DEG C/2.16kg) standard;
Rockwell hardness is detected by ASTM D785 standard;
Tensile strength and elongation at break are detected by ASTM D638 standard;
Bending strength and bending modulus are detected by ASTM D790 standard;
Izod notched impact strength is detected by ASTM D256 standard;
Heat distortion temperature is detected by ASTM D648 standard;
Smog requirement, odor requirements, aldoketones material requirement, VOC test value, by BT/SGMWJ0872-2016 standard into
Row test.
The performance and comparison of the composite material of each embodiment of table 1 preparation
As can be seen from Table 1, when the sum of plant powder and inorganic mineral filler are no more than 10%, density domination is in 0.93g/
Cm3 or less.When the sum of plant powder and inorganic mineral filler are no more than 20%, density domination is in 0.99g/cm3Below.Plant is fine
It is ideal for the density domination for controlling PP composite material to tie up powder.Plant fiber powder with certain draw ratio has
Conducive to the promotion of composite material bending strength and bending modulus, hollow glass micropearl has very big side for the increase of melt index
It helps.Plant fiber powder and hollow glass micropearl are used cooperatively, and the two passes through different shape, various sizes of synergistic effect pair
It is ideal in the control of PP composite material smell smog.
Claims (10)
1. a kind of plant composite fibre filling polypropylene composite material, it is characterised in that raw material is by such as the following group by weight percentage
Be grouped as: 42~64% copolymer polypropylene, 6~18% homopolypropylene, 5~18% plant powders, 0~5% inorganic mineral are filled out
Material, 1~5% elastomer, 0.8~3% expanding material, 0.2~0.6% coupling agent, 0.1~0.3% antioxidant, 10~28% polyester
Resin, 0.01~0.03% epoxy resin, 0.03~0.08% graphene.
2. a kind of plant composite fibre filling polypropylene composite material according to claim 1, it is characterised in that: the plant
Object powder is at least one of straw powder, bamboo powder, wood powder.
3. a kind of plant composite fibre filling polypropylene composite material according to claim 1, it is characterised in that: the nothing
Machine mineral filler is hollow glass micropearl, and average grain diameter is 0.8~85 micron, 9~17m2/g of specific surface area.
4. a kind of plant composite fibre filling polypropylene composite material according to claim 1, it is characterised in that: the bullet
Property body be at least one of POE, EPDM, SBS, SEBS.
5. a kind of plant composite fibre filling polypropylene composite material according to claim 1, it is characterised in that: the increasing
Holding agent is at least one of SEBS-g-MAH, PP-g-MAH, POE-g-MAH.
6. a kind of plant composite fibre filling polypropylene composite material according to claim 1, it is characterised in that: the idol
Connection agent is silane coupling agent KH560, and the antioxidant is antioxidant 1010.
7. a kind of preparation method of plant composite fibre filling polypropylene composite material as described in claim 1, it is characterised in that
Include the following steps:
(1) plant powder is added in high-speed mixer with the ethanol solution containing 1~3wt% coupling agent and is mixed, is gradually added into
Solution containing 1% epoxy resin and 3% graphene continues to stir 30 minutes under the conditions of 85 DEG C, obtains graphene after dry
Plant powder filler is coated, the graphene coated plant powder packing material size range is 15 microns -110 microns;
(2) graphene coated plant powder filler and polyester resin are subjected to melt blending, by blend dimethylformamide
Spinning, drying are carried out after solvent dissolution, composite fibre is formed, composite fibre is ground in ball mill, is fabricated to plant
Composite fibre powder, the length range of the plant composite fibre powder are 22 microns -285 microns, draw ratio be 130:1~
240:1;
(3) when there is inorganic mineral filler in raw material, by inorganic mineral filler, polypropylene, elastomer and contain 1~3wt% idol
The ethanol solution of connection agent mixes 3~8 minutes in high speed mixer, and 50~70 DEG C of temperature;When there is no inorganic mineral to fill out in raw material
When material, polypropylene, elastomer are mixed 3~8 minutes in high speed mixer, 50~70 DEG C of temperature;
(4) material and expanding material, antioxidant that step (2), (3) obtain are placed in double screw extruder, through melting extrusion, are made
Grain.
8. a kind of preparation method of plant composite fibre filling polypropylene composite material according to claim 7, feature
Be: coupling agent dosage is the 3% of plant powder total weight in step (1);Coupling agent dosage is filled out in step (3) for inorganic mineral
Expect the 3% of total weight.
9. a kind of preparation method of plant composite fibre filling polypropylene composite material according to claim 7, feature
It is by weight, the ratio between plant powder and solution are 5:1 in step (1).
10. a kind of preparation method of plant composite fibre filling polypropylene composite material according to claim 7, feature
It is by weight, graphene coated plant powder filler in step (2): polyester resin: solvent dimethylformamide 1:
2:12.
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Cited By (3)
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CN111925594A (en) * | 2020-08-17 | 2020-11-13 | 新奥(内蒙古)石墨烯材料有限公司 | Graphene reinforced polypropylene composite material, preparation method thereof and heat conduction product |
CN111961284A (en) * | 2020-08-26 | 2020-11-20 | 安徽国泰智能科技有限公司 | Light high-strength air guide sleeve for light truck |
CN112111105A (en) * | 2020-08-28 | 2020-12-22 | 安徽越洋达新能源科技有限公司 | High strength power support |
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CN112111105A (en) * | 2020-08-28 | 2020-12-22 | 安徽越洋达新能源科技有限公司 | High strength power support |
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