CN107880502A - A kind of biological whole degradation plastic and preparation method thereof - Google Patents
A kind of biological whole degradation plastic and preparation method thereof Download PDFInfo
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- CN107880502A CN107880502A CN201711187422.4A CN201711187422A CN107880502A CN 107880502 A CN107880502 A CN 107880502A CN 201711187422 A CN201711187422 A CN 201711187422A CN 107880502 A CN107880502 A CN 107880502A
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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
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B3/00—Preparation of cellulose esters of organic acids
- C08B3/08—Preparation of cellulose esters of organic acids of monobasic organic acids with three or more carbon atoms, e.g. propionate or butyrate
- C08B3/10—Preparation of cellulose esters of organic acids of monobasic organic acids with three or more carbon atoms, e.g. propionate or butyrate with five or more carbon-atoms, e.g. valerate
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- 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
- C08K2201/018—Additives for biodegradable polymeric composition
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
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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
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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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
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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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
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
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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
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Abstract
The invention discloses a kind of biological whole degradation plastic and preparation method thereof, is related to plastics preparing technical field;It is prepared from the following raw materials in parts by weight:40~60 parts of polycaprolactone, 10~20 parts of stalk fibre, 10~20 parts of wheat bran, 5~15 parts of chitosan, biuret modified 4~10 parts of epoxy resin, 2~8 parts of methyl diphenylene diisocyanate, 1~7 part of tributyl 2-acetylcitrate, 2,2 pairs of 0.1~0.5 part of (4 hydroxy phenyl) propane, 1~8 part of polypropylene grafted maleic anhydride, 1~5 part of silane coupler, 1~5 part of stearic acid, 1~5 part of carragheen, 1~7 part of glycerine;Preparation method includes the pre-treatment of wheat bran, the modification of stalk fibre, mixing, extrusion blow etc.;The plastics of the present invention can carry out fully bio-degradable, and can all degrade completion for 3~9 months in outdoor, will not pollute environment;The structural strength and mechanical strength, its tensile strength for improving the present invention simultaneously are 9~18N/mm2, fracture strength is 10~28N/mm2, elongation at break is 100~240%.
Description
Technical field
The present invention relates to plastics preparing technical field, is especially a kind of biological whole degradation plastic and preparation method thereof.
Background technology
As the problems such as environmental pollution and energy shortage is on the rise, the development and application of environmentally friendly material, which turns into, grinds
The emphasis studied carefully.For environmentally friendly material using renewable resource as raw material, product has a biodegradability, raw material sources are abundant,
Its Devoting Major Efforts To Developing application of product degraded is pollution-free etc. advantage boosting.During product development, degradable polymer is due to making
Prepared with non-petroleum class raw material and widely paid close attention to.
Natural fiber is commonly used to replace some synthesis fine due to its cheap and easy to get, renewable and good biocompatibility
Tie up to serve as reinforcing agent and filler.In recent years, have increasing natural fiber be used for degradation plastic it is filling-modified with
Improve its mechanical property, hot property, crystal property and degradation property.Rice and wheat are as basic primary product, annual production
Amount is very big, the byproduct stalk of rice and wheat except packing ring, pasture is used on a small quantity, partly made compost for heap it is outer, it is most of
All abandoned or burnt up as fuel;The byproduct wheat bran of wheat is primarily used to feed or discarded, causes very big resource
Waste;Research at present focuses primarily upon some compositions of wheat bran or the functional study of component, in the research of other side
It is less;Therefore rice straw and wheat bran are not utilized rationally.
But in string containing substantial amounts of hydroxyl, phenolic hydroxyl group, hydrophily is strong, at the same thermoplastic resin hydrophobicity compared with
By force, make the interface compatibility of the two poor, simultaneously because the presence of hydroxyl and phenolic hydroxyl group, fiber is easily reunited in process,
Dispersiveness is poor, thus the two simple mixing is difficult to reach and should required, so improving its interface compatibility turns into research
With the key for preparing natural plant fibre composite.
The content of the invention
The technical problems to be solved by the invention are the shortcomings that overcoming above prior art:A kind of fully bio-degradable is provided
Plastics and preparation method thereof.
The technical solution of the present invention is as follows:
A kind of biological whole degradation plastic:It is prepared from the following raw materials in parts by weight:40~60 parts of polycaprolactone, stalk fibre
10~20 parts, 10~20 parts of wheat bran, 5~15 parts of chitosan, biuret modified 4~10 parts of epoxy resin, diphenyl methane two is different
2~8 parts of cyanate, 1~7 part of tributyl 2-acetylcitrate, 2,2- double 0.1~0.5 part of (4- hydroxy phenyls) propane, polypropylene connects
1~8 part of maleic anhydride of branch, 1~5 part of silane coupler, 1~5 part of stearic acid, 1~5 part of carragheen, 1~7 part of glycerine.
A kind of preparation method of biological whole degradation plastic:Comprise the following steps:
(1) pre-treatment of wheat bran:It is 100~150 mesh that wheat bran is crushed into granularity, by the wheat bran after crushing with
Water is 1~2 according to mass body:10 are mixed, and the sulphur acid for adjusting pH for adding 1mol/L is 5~6, are heated to 60~80 DEG C of placements
3~4h;Then 5~10 are ultrasonically treated under the conditions of 200~400W of ultrasonic power until after neutral with absolute ethyl alcohol and water washing
Minute;It is 4~5 with 1mol/L sulphur acid for adjusting pH, adds alpha-amylase, 20~30min is digested at 40~60 DEG C;Add
1mol/L sodium hydroxide regulation pH is 7.5~8.5, adds at protease is 30~40 DEG C in temperature and digests 20~30min, does
It is dry;
(2) modification of stalk fibre:By stalk fibre and silane coupler, chitosan, biuret modified epoxy resin, hard
Resin acid is mixed, and input high-speed mixer mixes 5~10 minutes, is dried after taking-up at 20~40 DEG C, produces modified straw
Fiber;
(3) mix:The stalk fibre modified with step (2) of wheat bran enzymolysis liquid made from step (1) is mixed, so
Polycaprolactone, polypropylene grafted maleic anhydride, methyl diphenylene diisocyanate are added afterwards to be well mixed, and add acetyl lemon
Double (4- hydroxy phenyls) the propane carragheens of sour tributyl, 2,2-, glycerine are well mixed, and melting extrusion is carried out with double screw extruder
It is granulated, obtains masterbatch;
(4) masterbatch is added in inflation film manufacturing machine through heating up, extruding, being blow molded, upper traction, lower traction and winding film forming, that is, obtain
The product of the present invention.
The preparation method of stalk fibre of the present invention is:Water intaking rice or wheat stalk, it is 5~8cm to cut into length, uses clear water
Clean, dry or dry at 30~50 DEG C, 5~10min of crushing in pulverizer is then put into, through 2~3h of ball milling in ball mill;
Rice straw powder after ball milling and mass percent concentration are handled into 1~2h for 10% sodium hydroxide solution in 40~50 DEG C,
It is with absolute ethyl alcohol and water washing until neutral;It is 95 that rice straw after alkali process is added into mass ratio:2:3 NaOH, K2S2O4With
And K2In S mixed solutions, filtered with the nylon filter bag of 400 mesh, then with absolute ethyl alcohol and water washing up to neutral, so as to be made
Stalk fibre;
The beneficial effects of the invention are as follows:
1st, the present invention in order to solve the problems, such as that the compatibility between stalk fibre and polyester is poor, using silane coupler,
Chitosan, biuret modified epoxy resin, stearic acid are surface-treated to stalk fibre, and first, silane coupler can improve
The hydrophobicity of fiber surface;Secondly, physical entanglement effect can occur with fiber macromolecular for chitosan, and the amino of chitosan is with gathering
The ester group of caprolactone can produce hydrogen bond, and good bridging effect is played to the compatibility of composite, while again because it is day
Right macromolecule, therefore the water imbibition of modified obtained composite is also larger;Stearic carboxyl is esterified with hydroxyl in fiber
Reaction, reduces fibrous hydrophobic, improves the dispersiveness of fiber, while stearic backbone one side and polycaprolactone
There is preferable compatibility, on the other hand can be deep into polycaprolactone phase, mutually wind, enhance with the strand of polycaprolactone
The toughness of composite;Excessive epoxy radicals strengthens the polarity of modified fibre in biuret modified epoxy resin, so as to influence
Compatibility between fiber and plastic substrate;Therefore by the synergy of these four materials, stalk fibre is substantially increased
Compatibility between polyester, so as to improve the mechanical property of composite.
2nd, the present invention uses NaOH, K2S2O4And K2S is handled stalk fibre, and NaOH is in dissolving hemicellulose, wood
While plain, cellulose has also inevitably been decomposed, has caused the reduction of fiber self-strength, therefore the present invention is in NaOH processing
During, add K2S2O4And K2S auxiliary agents can occur certain with the aldehyde terminal groups of the carbohydrate such as cellulose, hemicellulose
Chemical reaction (oxidation, reduction), it is suppressed that " peeling reaction " of carbohydrate, so as to play a part of protecting cellulose.
3rd, a variety of processing aids, such as tributyl 2-acetylcitrate carragheen, glycerine are also added with the present invention, carried significantly
Water resistance, hot-workability and the life-span of high polybag of the present invention.Added with double (4- hydroxy phenyls) propane of 2,2- in the present invention
The degraded of plastics can be promoted.
4th, the present invention adds stalk fibre of degradable, wheat bran, chitosan etc. in polycaprolactone, so as to improve it is poly- oneself
The degradability of lactone, meanwhile, the structural strength and mechanical strength, its tensile strength for improving the present invention are 9~18N/
mm2, fracture strength is 10~28N/mm2, elongation at break is 100~240%.The plastics of the present invention can carry out fully bio-degradable,
Can degrade completion for 3~9 months substantially in outdoor, therefore protect environment.
Embodiment
The present invention is described in further details with specific embodiment below, but the present invention is not only limited in detail below in fact
Apply example.
Embodiment one
The raw material for weighing following weight proportion is made:40 parts of polycaprolactone, 10 parts of stalk fibre, 10 parts of wheat bran, chitosan 5
Part, biuret modified 4 parts of epoxy resin, 2 parts of methyl diphenylene diisocyanate, 1 part of tributyl 2-acetylcitrate, 2,2- is double
0.1 part of (4- hydroxy phenyls) propane, 1 part of polypropylene grafted maleic anhydride, 1 part of silane coupler, 1 part of stearic acid, carragheen 1
Part, 1 part of glycerine.
Prepare in accordance with the following methods:
(1) pre-treatment of wheat bran:It is 100 mesh that wheat bran is crushed into granularity, and the wheat bran after crushing is pressed with water
It is 1 according to mass body:10 are mixed, and the sulphur acid for adjusting pH for adding 1mol/L is 5, are heated to 60 DEG C of placement 4h;Then with anhydrous
Ethanol washs and water washing is until after neutral, is ultrasonically treated 10 minutes under the conditions of ultrasonic power 200W;With 1mol/L sulfuric acid
It is 4 to adjust pH, adds alpha-amylase, 30min is digested at 40 DEG C;The sodium hydroxide regulation pH for adding 1mol/L is 7.5, is added
Protease digests 30min at being 30 DEG C in temperature, dries;
(2) preparation of stalk fibre:Water intaking rice or wheat stalk, it is 5~8cm to cut into length, is cleaned with clear water, 30
Dry or dry at DEG C, be then put into pulverizer and crush 10min, through ball milling 2h in ball mill;By the rice straw after ball milling
Powder handles 2h with the sodium hydroxide solution that mass percent concentration is 10% in 40 DEG C, with absolute ethyl alcohol and water washing in
Property;It is 95 that rice straw after alkali process is added into mass ratio:2:3 NaOH, K2S2O4And K2In S mixed solutions, with 400 mesh
Nylon filter bag filtering, then with absolute ethyl alcohol and water washing until neutral, so as to which stalk fibre be made;
(3) modification of stalk fibre:By stalk fibre and silane coupler, chitosan, biuret modified epoxy resin, hard
Resin acid is mixed, and input high-speed mixer mixes 5 minutes, is dried after taking-up at 20 DEG C, produces modified straw fiber;
(4) mix:The stalk fibre modified with step (3) of wheat bran enzymolysis liquid made from step (1) is mixed, so
Polycaprolactone, polypropylene grafted maleic anhydride, methyl diphenylene diisocyanate are added afterwards to be well mixed, and add acetyl lemon
Double (4- hydroxy phenyls) the propane carragheens of sour tributyl, 2,2-, glycerine are well mixed, and melting extrusion is carried out with double screw extruder
It is granulated, obtains masterbatch;
(5) masterbatch is added in inflation film manufacturing machine through heating up, extruding, being blow molded, upper traction, lower traction and winding film forming, that is, obtain
The product of the present invention.
Embodiment two
The raw material for weighing following weight proportion is made:60 parts of polycaprolactone, 20 parts of stalk fibre, 20 parts of wheat bran, chitosan
15 parts, biuret modified 10 parts of epoxy resin, 8 parts of methyl diphenylene diisocyanate, 7 parts of tributyl 2-acetylcitrate, 2,2-
Double 0.5 part of (4- hydroxy phenyls) propane, 8 parts of polypropylene grafted maleic anhydride, 5 parts of silane coupler, 5 parts of stearic acid, carragheen 5
Part, 7 parts of glycerine.
Prepare in accordance with the following methods:
(1) pre-treatment of wheat bran:It is 150 mesh that wheat bran is crushed into granularity, and the wheat bran after crushing is pressed with water
It is 2 according to mass body:10 are mixed, and the sulphur acid for adjusting pH for adding 1mol/L is 6, are heated to 40 DEG C of placement 3h;Then with anhydrous
Ethanol washs and water washing is until after neutral, is ultrasonically treated 5 minutes under the conditions of ultrasonic power 400W;Adjusted with 1mol/L sulfuric acid
It is 5 to save pH, adds alpha-amylase, 30min is digested at 40 DEG C;The sodium hydroxide regulation pH for adding 1mol/L is 7.5, adds egg
White enzyme digests 30min at being 30 DEG C in temperature, dries;
(2) preparation of stalk fibre:Water intaking rice or wheat stalk, it is 5~8cm to cut into length, is cleaned with clear water, 30
Dry or dry at DEG C, be then put into pulverizer and crush 10min, through ball milling 2h in ball mill;By the rice straw after ball milling
Powder handles 2h with the sodium hydroxide solution that mass percent concentration is 10% in 40 DEG C, with absolute ethyl alcohol and water washing in
Property;It is 95 that rice straw after alkali process is added into mass ratio:2:3 NaOH, K2S2O4And K2In S mixed solutions, with 400 mesh
Nylon filter bag filtering, then with absolute ethyl alcohol and water washing until neutral, so as to which stalk fibre be made;
(3) modification of stalk fibre:By stalk fibre and silane coupler, chitosan, biuret modified epoxy resin, hard
Resin acid is mixed, and input high-speed mixer mixes 10 minutes, is dried after taking-up at 40 DEG C, produces modified straw fiber;
(4) mix:The stalk fibre modified with step (3) of wheat bran enzymolysis liquid made from step (1) is mixed, so
Polycaprolactone, polypropylene grafted maleic anhydride, methyl diphenylene diisocyanate are added afterwards to be well mixed, and add acetyl lemon
Double (4- hydroxy phenyls) the propane carragheens of sour tributyl, 2,2-, glycerine are well mixed, and melting extrusion is carried out with double screw extruder
It is granulated, obtains masterbatch;
(5) masterbatch is added in inflation film manufacturing machine through heating up, extruding, being blow molded, upper traction, lower traction and winding film forming, that is, obtain
The product of the present invention.
The plastics that embodiment one to two is prepared carry out performance detection, and wherein degradation rate uses composting process;Specific knot
Fruit such as table one:
Table one
Embodiment one | Embodiment two | |
Tensile strength (N/nm2) | 9.3 | 14.2 |
Fracture strength (N/nm2) | 10.5 | 14.3 |
Elongation at break (%) | 106.9 | 142.8 |
60 days degradation rates (%) | 99.5% | 99.9% |
Therefore, by performance test it can be found that the plastics mechanical property for preparing of the present invention is preferable, and can drop completely
Solution, the degradation rate of 60 days is more than 99%, greatly reduces the pollution to environment.
It the above is only the feature implementation example of the present invention, the scope of the present invention be not limited in any way.It is all to use together
The technical scheme formed Deng exchange or equivalence replacement, all falls within rights protection scope of the present invention.
Claims (2)
- A kind of 1. biological whole degradation plastic:It is characterized in that:It is prepared from the following raw materials in parts by weight:Polycaprolactone 40~60 Part, 10~20 parts of stalk fibre, 10~20 parts of wheat bran, 5~15 parts of chitosan, biuret modified 4~10 parts of epoxy resin, hexichol 2~8 parts of dicyclohexylmethane diisocyanate, 1~7 part of tributyl 2-acetylcitrate, 2,2- double (4- hydroxy phenyls) propane 0.1~0.5 Part, 1~8 part of polypropylene grafted maleic anhydride, 1~5 part of silane coupler, 1~5 part of stearic acid, 1~5 part of carragheen, glycerine 1 ~7 parts.
- A kind of 2. preparation method of biological whole degradation plastic:It is characterized in that:Comprise the following steps:(1) pre-treatment of wheat bran:It is 100~150 mesh that wheat bran is crushed into granularity, and the wheat bran after crushing is pressed with water It is 1~2 according to mass body:10 are mixed, add 1mol/L sulphur acid for adjusting pH be 5~6, be heated to 60~80 DEG C place 3~ 4h;Then 5~10 points are ultrasonically treated under the conditions of 200~400W of ultrasonic power until after neutral with absolute ethyl alcohol and water washing Clock;It is 4~5 with 1mol/L sulphur acid for adjusting pH, adds alpha-amylase, 20~30min is digested at 40~60 DEG C;Add 1mol/L sodium hydroxide regulation pH is 7.5~8.5, adds at protease is 30~40 DEG C in temperature and digests 20~30min, does It is dry;(2) modification of stalk fibre:By stalk fibre and silane coupler, chitosan, biuret modified epoxy resin, stearic acid Mixed, input high-speed mixer mixes 5~10 minutes, is dried after taking-up at 20~40 DEG C, produces modified straw fiber;(3) mix:The stalk fibre modified with step (2) of wheat bran enzymolysis liquid made from step (1) is mixed, Ran Houjia Enter polycaprolactone, polypropylene grafted maleic anhydride, methyl diphenylene diisocyanate to be well mixed, add acetyl tributyl citrate three Double (4- hydroxy phenyls) the propane carragheens of butyl ester, 2,2-, glycerine are well mixed, and carrying out melting extrusion with double screw extruder makes Grain, obtains masterbatch;(4) masterbatch is added in inflation film manufacturing machine through heating up, extruding, being blow molded, upper traction, lower traction and winding film forming, that is, obtain this hair Bright product;The preparation method of stalk fibre is:Water intaking rice or wheat stalk, it is 5~8cm to cut into length, is cleaned with clear water, 30 Dry or dry at~50 DEG C, 5~10min of crushing in pulverizer is then put into, through 2~3h of ball milling in ball mill;After ball milling Rice straw powder and mass percent concentration be 10% sodium hydroxide solution handle 1~2h in 40~50 DEG C, with anhydrous second Alcohol and water washing is until neutral;It is 95 that rice straw after alkali process is added into mass ratio:2:3 NaOH, K2S2O4And K2S is mixed Close in solution, filtered with the nylon filter bag of 400 mesh, then with absolute ethyl alcohol and water washing until neutrality, fine so as to which stalk be made Dimension.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109337128A (en) * | 2018-09-05 | 2019-02-15 | 安徽新翔包装材料有限公司 | A kind of decomposable environmentally-friendly plastic packaging bag of high tenacity |
CN113733278A (en) * | 2021-05-25 | 2021-12-03 | 付生 | Raw material mixing treatment process of degradable drainage plate |
GB2604624A (en) * | 2021-03-10 | 2022-09-14 | Kristina Magnhild Nameth Mira | Plant-based flexible material, process for preparation, and uses thereof |
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CN106349669A (en) * | 2016-09-26 | 2017-01-25 | 中国热带农业科学院农产品加工研究所 | Bagasse biodegradable plastic and preparation method thereof |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109337128A (en) * | 2018-09-05 | 2019-02-15 | 安徽新翔包装材料有限公司 | A kind of decomposable environmentally-friendly plastic packaging bag of high tenacity |
GB2604624A (en) * | 2021-03-10 | 2022-09-14 | Kristina Magnhild Nameth Mira | Plant-based flexible material, process for preparation, and uses thereof |
GB2604624B (en) * | 2021-03-10 | 2023-05-24 | Kristina Magnhild Nameth Mira | Plant-based flexible material, process for preparation, and uses thereof |
CN113733278A (en) * | 2021-05-25 | 2021-12-03 | 付生 | Raw material mixing treatment process of degradable drainage plate |
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Application publication date: 20180406 |