CN107841107A - Heat-resistant fireproof lactic acid composite material and preparation method thereof - Google Patents
Heat-resistant fireproof lactic acid composite material and preparation method thereof Download PDFInfo
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- CN107841107A CN107841107A CN201610834263.1A CN201610834263A CN107841107A CN 107841107 A CN107841107 A CN 107841107A CN 201610834263 A CN201610834263 A CN 201610834263A CN 107841107 A CN107841107 A CN 107841107A
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- lactic acid
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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
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/006—Additives being defined by their surface area
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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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
- C08L2201/02—Flame or fire retardant/resistant
-
- 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
Abstract
The invention provides a kind of heat-resistant fireproof lactic acid composite material, it is characterised in that it is made up of the raw material of following parts by weight:50~100 parts of PLA, 8~16 parts of chitosan, 2~8 parts of graphene nanometer sheet, 5~14 parts of carbon fiber, 8~14 parts of glass fibre, 5~10 parts of calcined kaolin, 1~5 part of Ludox, 10~18 parts of expanded graphite, 2~6 parts of attapulgite, 1~5 part of four glycidyl amine of MDA, 1~3 part of silane coupler;Wherein, the specific surface area of the graphene nanometer sheet reaches 80~100m2/ g, and treated by the glycidyl amine of MDA four.The present invention also provides a kind of preparation method of above-mentioned heat-resistant fireproof lactic acid composite material.Heat-resistant fireproof lactic acid composite material provided by the invention has the advantages of excellent fire-retardancy, excellent toughness, resistance to elevated temperatures are good, comprehensive mechanical intensity is high.
Description
Technical field
The present invention relates to a kind of lactic acid composite material, and in particular to a kind of heat-resistant fireproof lactic acid composite material and its
Preparation method.
Background technology
PLA(English abbreviation:PLA)It is a kind of thermoplastic aliphatic's polyester, produces the lactic acid and third required for PLA
Lactide can be fermented by renewable resource, be dehydrated, be obtained after purification, resulting PLA typically have good machinery and
Processing characteristics, and poly-lactic acid products it is discarded after can be that one kind possesses good performance by various mode fast degradations
Green plastic.But PLA material is more crisp in itself, and heat resistance is poor, and this significantly limit its application.
The content of the invention
In view of this, it is a kind of good, comprehensive with excellent fire-retardancy, excellent toughness, resistance to elevated temperatures it is necessory to provide
Heat-resistant fireproof lactic acid composite material of high mechanical strength and preparation method thereof, to solve the above problems.
The present invention provides a kind of heat-resistant fireproof lactic acid composite material, is made up of the raw material of following parts by weight:PLA
50~100 parts, 8~16 parts of chitosan, 2~8 parts of graphene nanometer sheet, 5~14 parts of carbon fiber, 8~14 parts of glass fibre, calcining
5~10 parts of kaolin, 1~5 part of Ludox, 10~18 parts of expanded graphite, 2~6 parts of attapulgite, MDA four contract
1~5 part of water glyceramine, 1~3 part of silane coupler;Wherein, the specific surface area of the graphene nanometer sheet reaches 80~100m2/
G, and treated by the glycidyl amine of MDA four.
Based on above-mentioned, it is made up of the raw material of following parts by weight:70~90 parts of PLA, 10~14 parts of chitosan, graphite
It is 3~6 parts of alkene nanometer sheet, 7~11 parts of carbon fiber, 9~12 parts of glass fibre, 6~9 parts of calcined kaolin, 2~4 parts of Ludox, swollen
Swollen 12~16 parts of graphite, 3~5 parts of attapulgite, 2~4 parts of four glycidyl amine of MDA, silane coupler 1~3
Part.
Based on above-mentioned, the silane coupler is Silane coupling agent KH550, silane coupler KH560, silane coupler
KH570 or silane coupler KH792.
Based on above-mentioned, the weight average molecular weight of the PLA is 100,000~800,000, and fusing point is 60 DEG C.
Based on above-mentioned, the carbon fiber is treated through silane coupler.
Based on above-mentioned, the glass fibre is treated through silane coupler.
Wherein, the particle diameter of the silicon dioxide granule in the Ludox is 580nm, and the content of silicon dioxide granule is
20%~30%.
Based on above-mentioned, the particle diameter of the calcined kaolin is less than 40 μm.
The present invention also provides a kind of preparation method of above-mentioned heat-resistant fireproof lactic acid composite material, specific preparation method step
It is rapid as follows:
(1)The processing of graphene nanometer sheet
Graphene nanometer sheet is positioned in DMF solvent together with the glycidyl amine of MDA four, mechanical agitation is held
It is continuous 1~3 hour, the rpm of rotating speed 500~1500, after being well mixed, it is positioned in drying oven, temperature control is at 45 DEG C~55 DEG C
Persistently dry 6 hours, obtain the graphene nanometer sheet of surface modification;
(2)The graphene nanometer sheet that the surface is modified and PLA mix particles is uniform, in three-roll grinder grind 20~
30 min, obtain PLA graphene mixture;
(3)By the PLA graphene mixture and chitosan, calcined kaolin, silane coupler, Ludox, expansion stone
Ink, attapulgite, the glycidyl amine of MDA four in the min of high-speed mixer and mixing 10~30, mix according to said ratio
Added after closing uniformly in the hopper of double screw extruder, by carbon fiber and glass fibre by a certain percentage from double screw extruder
Plus added in fine mouth, extruded through melt blending, extruded material dries up pelletizing after cold go, and the poly- breast of the heat-resistant fireproof is made
Sour composite.
Compared with prior art, heat-resistant fireproof lactic acid composite material provided by the invention has advantages below:First,
The graphene nanometer sheet of the glycidyl amine of MDA four surface treatment is prepared using solution blended process, stone can be made
Black alkene nanometer sheet has good compatibility with matrix resin;Secondly, the glycidyl amine of MDA four possesses larger
Relative molecular mass, but show very low viscosity, thus be used to reduce polymer melt viscosity, improve polymer
Fluidity of molten;In addition, having active hydroxyl and amino in chitosan macromolecular, they have stronger chemical reaction ability,
By producing interaction with other radical reactions or with matrix, toughening effect is splendid;The addition of calcined kaolin can then carry
The mechanical strength of high polymer;Ludox can increase the heat resistance and intensity of polymer;Expanded graphite is expansion type flame-retarding
The phyllosilicate nano material compositional flame-retardant such as agent and attapulgite, kaolin, it can be formed in matrix surface continuous and fine and close
Layer of charcoal, and will not produce and melt drop;Graphene has the advantages that high temperature resistant, excellent pliability and high intensity;Therefore, this hair
The heat-resistant fireproof lactic acid composite material of bright offer has that excellent fire-retardancy, excellent toughness, resistance to elevated temperatures be good, integrated machine
The advantages that tool intensity is high.
Embodiment
Below by embodiment, technical scheme is described in further detail.
Embodiment 1
The embodiment of the present invention provides a kind of heat-resistant fireproof lactic acid composite material, and it is made up of the raw material of following parts by weight:It is poly-
50 parts of lactic acid, 8 parts of chitosan, 2 parts of graphene nanometer sheet, 5 parts of carbon fiber, 8 parts of glass fibre, 5 parts of calcined kaolin, Ludox
1 part, 10 parts of expanded graphite, 2 parts of attapulgite, 1 part of four glycidyl amine of MDA and Silane coupling agent KH550 1
Part;Wherein, the weight average molecular weight of the PLA is 100,000, and fusing point is 60 DEG C;Carbon fiber and glass fibre are all by silane
What coupling agent KH550 was treated.
The preparation method for the above-mentioned heat-resistant fireproof lactic acid composite material that the present embodiment provides comprises the following steps:
(1)Graphene nanometer sheet is positioned in DMF solvent together with the glycidyl amine of MDA four, mechanical agitation
Continue 1 hour, the rpm of rotating speed 700, after being well mixed, be positioned in drying oven, temperature control 45 DEG C persistently drying it is 6 small
When, the graphene nanometer sheet of surface modification is obtained, and its specific surface area reaches 86 m2/g;
(2)The graphene nanometer sheet that the surface is modified and PLA mix particles is uniform, 20 are ground in three-roll grinder
Min, obtain PLA graphene mixture;
(3)By the PLA graphene mixture and chitosan, calcined kaolin, Silane coupling agent KH550, Ludox, swollen
Swollen graphite, attapulgite, the glycidyl amine of MDA four in the min of high-speed mixer and mixing 10, mix according to said ratio
Added after closing uniformly in the hopper of double screw extruder, by carbon fiber and glass fibre by a certain percentage from double screw extruder
Plus added in fine mouth, extruded through melt blending, extruded material dries up pelletizing after cold go, and the poly- breast of the heat-resistant fireproof is made
Sour composite.
Embodiment 2
The embodiment of the present invention provides a kind of heat-resistant fireproof lactic acid composite material, and it is made up of the raw material of following parts by weight:It is poly-
70 parts of lactic acid, 10 parts of chitosan, 3 parts of graphene nanometer sheet, 7 parts of carbon fiber, 9 parts of glass fibre, 7 parts of calcined kaolin, silicon are molten
2 parts of glue, 12 parts of expanded graphite, 3 parts of attapulgite, 2 parts of four glycidyl amine of MDA, silane coupler KH560
2 parts;Wherein, the weight average molecular weight of the PLA is 300,000, and fusing point is 60 DEG C;Carbon fiber and glass fibre are all by silane
What coupling agent KH560 was treated.
The preparation method for the above-mentioned heat-resistant fireproof lactic acid composite material that the present embodiment provides comprises the following steps:
(1)Graphene nanometer sheet is positioned in DMF solvent together with the glycidyl amine of MDA four, mechanical agitation
Continue 2 hours, the rpm of rotating speed 800, after being well mixed, be positioned in drying oven, temperature control 50 DEG C persistently drying it is 6 small
When, the graphene nanometer sheet of surface modification is obtained, and its specific surface area reaches 92 m2/g;
(2)The graphene nanometer sheet that the surface is modified and PLA mix particles is uniform, 20 are ground in three-roll grinder
Min, obtain PLA graphene mixture;
(3)By the PLA graphene mixture and chitosan, calcined kaolin, silane coupler KH560, Ludox, swollen
Swollen graphite, attapulgite, the glycidyl amine of MDA four in the min of high-speed mixer and mixing 15, mix according to said ratio
Added after closing uniformly in the hopper of double screw extruder, by carbon fiber and glass fibre by a certain percentage from double screw extruder
Plus added in fine mouth, extruded through melt blending, extruded material dries up pelletizing after cold go, and the poly- breast of the heat-resistant fireproof is made
Sour composite.
Embodiment 3
The embodiment of the present invention provides a kind of heat-resistant fireproof lactic acid composite material, and it is made up of the raw material of following parts by weight:It is poly-
80 parts of lactic acid, 12 parts of chitosan, 5 parts of graphene nanometer sheet, 9 parts of carbon fiber, 11 parts of glass fibre, 8 parts of calcined kaolin, silicon are molten
3 parts of glue, 14 parts of expanded graphite, 3 parts of attapulgite, 4 parts of four glycidyl amine of MDA, silane coupler KH570
2 parts;Wherein, the weight average molecular weight of the PLA is 500,000, and fusing point is 60 DEG C;Carbon fiber and glass fibre are all by silane
What coupling agent KH570 was treated.
The preparation method for the above-mentioned heat-resistant fireproof lactic acid composite material that the present embodiment provides comprises the following steps:
(1)Graphene nanometer sheet is positioned in DMF solvent together with the glycidyl amine of MDA four, mechanical agitation
Continue 2 hours, the rpm of rotating speed 1000, after being well mixed, be positioned in drying oven, temperature control 50 DEG C persistently drying it is 6 small
When, the graphene nanometer sheet of surface modification is obtained, and its specific surface area reaches 99 m2/g;
(2)The graphene nanometer sheet that the surface is modified and PLA mix particles is uniform, 25 are ground in three-roll grinder
Min, obtain PLA graphene mixture;
(3)By the PLA graphene mixture and chitosan, calcined kaolin, silane coupler KH570, Ludox, swollen
Swollen graphite, attapulgite, the glycidyl amine of MDA four in the min of high-speed mixer and mixing 20, mix according to said ratio
Added after closing uniformly in the hopper of double screw extruder, by carbon fiber and glass fibre by a certain percentage from double screw extruder
Plus added in fine mouth, extruded through melt blending, extruded material dries up pelletizing after cold go, and the poly- breast of the heat-resistant fireproof is made
Sour composite.
Embodiment 4
The embodiment of the present invention provides a kind of heat-resistant fireproof lactic acid composite material, and it is made up of the raw material of following parts by weight:It is poly-
90 parts of lactic acid, 14 parts of chitosan, 6 parts of graphene nanometer sheet, 11 parts of carbon fiber, 12 parts of glass fibre, 9 parts of calcined kaolin, silicon
4 parts of colloidal sol, 16 parts of expanded graphite, 4 parts of attapulgite, 4 parts of four glycidyl amine of MDA, silane coupler
3 parts of KH792;Wherein, the weight average molecular weight of the PLA is 700,000, and fusing point is 60 DEG C;Carbon fiber and glass fibre be all through
Cross what silane coupler KH792 was treated.
The preparation method for the above-mentioned heat-resistant fireproof lactic acid composite material that the present embodiment provides comprises the following steps:
(1)Graphene nanometer sheet is positioned in DMF solvent together with the glycidyl amine of MDA four, mechanical agitation
Continue 2 hours, the rpm of rotating speed 1100, after being well mixed, be positioned in drying oven, temperature control 50 DEG C persistently drying it is 6 small
When, the graphene nanometer sheet of surface modification is obtained, and its specific surface area reaches 89 m2/g;
(2)The graphene nanometer sheet that the surface is modified and PLA mix particles is uniform, 30 are ground in three-roll grinder
Min, obtain PLA graphene mixture;
(3)By the PLA graphene mixture and chitosan, calcined kaolin, silane coupler KH792, Ludox, swollen
Swollen graphite, attapulgite, the glycidyl amine of MDA four in the min of high-speed mixer and mixing 25, mix according to said ratio
Added after closing uniformly in the hopper of double screw extruder, by carbon fiber and glass fibre by a certain percentage from double screw extruder
Plus added in fine mouth, extruded through melt blending, extruded material dries up pelletizing after cold go, and the poly- breast of the heat-resistant fireproof is made
Sour composite.
Embodiment 5
The embodiment of the present invention provides a kind of heat-resistant fireproof lactic acid composite material, and it is made up of the raw material of following parts by weight:It is poly-
100 parts of lactic acid, 16 parts of chitosan, 8 parts of graphene nanometer sheet, 14 parts of carbon fiber, 14 parts of glass fibre, 10 parts of calcined kaolin,
5 parts of Ludox, 18 parts of expanded graphite, 5 parts of attapulgite, 5 parts of four glycidyl amine of MDA, silane coupler
3 parts of KH560;Wherein, the weight average molecular weight of the PLA is 800,000, and fusing point is 60 DEG C;Carbon fiber and glass fibre be all through
Cross what silane coupler KH560 was treated.
The preparation method for the above-mentioned heat-resistant fireproof lactic acid composite material that the present embodiment provides comprises the following steps:
(1)Graphene nanometer sheet is positioned in DMF solvent together with the glycidyl amine of MDA four, mechanical agitation
Continue 3 hours, the rpm of rotating speed 1400, after being well mixed, be positioned in drying oven, temperature control 55 DEG C persistently drying it is 6 small
When, the graphene nanometer sheet of surface modification is obtained, and its specific surface area reaches 93 m2/g;
(2)The graphene nanometer sheet that the surface is modified and PLA mix particles is uniform, 30 are ground in three-roll grinder
Min, obtain PLA graphene mixture;
(3)By the PLA graphene mixture and chitosan, calcined kaolin, silane coupler KH560, Ludox, swollen
Swollen graphite, attapulgite, the glycidyl amine of MDA four in the min of high-speed mixer and mixing 30, mix according to said ratio
Added after closing uniformly in the hopper of double screw extruder, by carbon fiber and glass fibre by a certain percentage from double screw extruder
Plus added in fine mouth, extruded through melt blending, extruded material dries up pelletizing after cold go, and the poly- breast of the heat-resistant fireproof is made
Sour composite.
According to national standard, items are carried out to the heat-resistant fireproof lactic acid composite material that above-described embodiment 1~5 provides
It can test, test result is as shown in the table:
Project | Tensile strength(MPa) | Bending strength(MPa) | Unnotched impact strength (KJ/m2) | Heat distortion temperature (0.18MPa/ DEG C) | Strength retention(%) | Oxygen index (OI) |
Embodiment 1 | 91.2 | 82.7 | 31.7 | 83.9 | 84.5 | 30 |
Embodiment 2 | 95.6 | 88.4 | 34.9 | 87.5 | 80.1 | 31 |
Embodiment 3 | 119.1 | 92.2 | 40.2 | 90.9 | 78.8 | 33 |
Embodiment 4 | 117.3 | 93.3 | 40.9 | 89.5 | 78.4 | 34 |
Embodiment 5 | 107.8 | 87.9 | 37.5 | 86.7 | 78.7 | 35 |
Note:It is strong that strength retention refers to that obtained composite soaks 24 h drying process post-tensioning in 80 DEG C of waters bath with thermostatic control
Spend the rate of change relative to untreated composite.
Finally it should be noted that:The above embodiments are merely illustrative of the technical scheme of the present invention and are not intended to be limiting thereof;To the greatest extent
The present invention is described in detail with reference to preferred embodiments for pipe, those of ordinary skills in the art should understand that:Still
The embodiment of the present invention can be modified or equivalent substitution is carried out to some technical characteristics;Without departing from this hair
The spirit of bright technical scheme, it all should cover among the claimed technical scheme scope of the present invention.
Claims (7)
1. a kind of heat-resistant fireproof lactic acid composite material, it is characterised in that it is made up of the raw material of following parts by weight:PLA
50~100 parts, 8~16 parts of chitosan, 2~8 parts of graphene nanometer sheet, 5~14 parts of carbon fiber, 8~14 parts of glass fibre, calcining
5~10 parts of kaolin, 1~5 part of Ludox, 10~18 parts of expanded graphite, 2~6 parts of attapulgite, MDA four contract
1~5 part of water glyceramine, 1~3 part of silane coupler;Wherein, the specific surface area of the graphene nanometer sheet reaches 80~100m2/
G, and treated by the glycidyl amine of MDA four.
2. heat-resistant fireproof lactic acid composite material according to claim 1, it is characterised in that it is by following parts by weight
Raw material is made:70~90 parts of PLA, 10~14 parts of chitosan, 3~6 parts of graphene nanometer sheet, 7~11 parts of carbon fiber, glass
9~12 parts of fiber, 6~9 parts of calcined kaolin, 2~4 parts of Ludox, 12~16 parts of expanded graphite, 3~5 parts of attapulgite, two
2~4 parts of four glycidyl amine of diaminodiphenylmethane, 1~3 part of silane coupler.
3. heat-resistant fireproof lactic acid composite material according to claim 1 or 2, it is characterised in that described silane coupled
Agent is Silane coupling agent KH550, silane coupler KH560, silane coupler KH570 or silane coupler KH792.
4. heat-resistant fireproof lactic acid composite material according to claim 1 or 2, it is characterised in that the PLA
Weight average molecular weight is 100,000~800,000, and fusing point is 60 DEG C.
5. heat-resistant fireproof lactic acid composite material according to claim 1 or 2, it is characterised in that the carbon fiber and
The glass fibre is treated through silane coupler.
6. heat-resistant fireproof lactic acid composite material according to claim 1 or 2, it is characterised in that the calcining kaolinite
The particle diameter of soil is less than 40 μm.
7. a kind of preparation method of the heat-resistant fireproof lactic acid composite material described in any one of claim 1~6, specific to prepare
Method and step is as follows:
(1)Graphene nanometer sheet is positioned in DMF solvent together with the glycidyl amine of MDA four, mechanical agitation
Continue 1~3 hour, the rpm of rotating speed 500~1500, after being well mixed, be positioned in drying oven, temperature control is 45 DEG C~55
DEG C persistently dry 6 hours, obtain the graphene nanometer sheet of surface modification;
(2)The graphene nanometer sheet that the surface is modified and PLA mix particles is uniform, in three-roll grinder grind 20~
30 min, obtain PLA graphene mixture;
(3)By the PLA graphene mixture and chitosan, calcined kaolin, silane coupler, Ludox, expansion stone
Ink, attapulgite, the glycidyl amine of MDA four in the min of high-speed mixer and mixing 10~30, mix according to said ratio
Added after closing uniformly in the hopper of double screw extruder, by carbon fiber and glass fibre by a certain percentage from double screw extruder
Plus added in fine mouth, extruded through melt blending, extruded material dries up pelletizing after cold go, and the poly- breast of the heat-resistant fireproof is made
Sour composite.
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Cited By (1)
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CN111576089A (en) * | 2020-05-06 | 2020-08-25 | 泾县艺宣阁宣纸工艺品有限公司 | Rice paper for ink-jet printing and preparation method thereof |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111576089A (en) * | 2020-05-06 | 2020-08-25 | 泾县艺宣阁宣纸工艺品有限公司 | Rice paper for ink-jet printing and preparation method thereof |
CN111576089B (en) * | 2020-05-06 | 2021-12-31 | 泾县艺宣阁宣纸工艺品有限公司 | Rice paper for ink-jet printing and preparation method thereof |
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Application publication date: 20180327 |