CN106832801A - A kind of lignin modification PBAT biodegradable plastics and preparation method thereof - Google Patents
A kind of lignin modification PBAT biodegradable plastics and preparation method thereof Download PDFInfo
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- CN106832801A CN106832801A CN201611193434.3A CN201611193434A CN106832801A CN 106832801 A CN106832801 A CN 106832801A CN 201611193434 A CN201611193434 A CN 201611193434A CN 106832801 A CN106832801 A CN 106832801A
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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
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2497/00—Characterised by the use of lignin-containing materials
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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
- C08L2201/06—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
- C08L2205/03—Polymer mixtures characterised by other features containing three 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
- C08L2205/05—Polymer mixtures characterised by other features containing polymer components which can react with one another
Abstract
The invention discloses a kind of preparation method of lignin modification PBAT biodegradable plastics, comprise the following steps：(1) poly terephthalic acid/tetramethylene adipate, lignin are vacuum dried respectively；(2) dried poly terephthalic acid/tetramethylene adipate, lignin and chain extender, antioxidant, plasticizer, lubricant, heat stabilizer are added in high mixer, is sufficiently mixed；(3) by gained mixed material through twin-screw extrusion machine extruding pelletization；(4) lignin PBAT composite plastics grain is carried out into blown film at a certain temperature, lignin modification PBAT biodegradable plastics is obtained.The present invention prepares biodegradable plastic using a large amount of biomass lignin for existing of nature are compound with PBAT, while meeting degradable requirement after composite modified, the mechanical property of pure PBAT resins is enhanced, and effectively reduces production cost, be allowed to be more beneficial for marketing.
Description
Technical field
The present invention relates to degradative plastics technical field, more particularly to a kind of lignin modification PBAT biodegradable plastics and its
Preparation method.
Background technology
At present, continuing to develop with national economy, the consumption figure of plastic products is constantly increasing, and synthetic plastic is in production
With more and more important role is play in life.But cannot be degraded after being discarded due to most plastic products, deposited for a long time
, constantly accumulation causes serious white pollution, with the continuous exacerbation and the continuous enhancing of people's environmental consciousness of pollution,
Seek it is a kind of can meet people's use demand and can meet the plastic products of ecological requirements again seem more and more urgent and cause
The broad interest of researcher, wherein degradable resin have become the heat of research due to its degradation characteristic and economic performance
Point,
Poly terephthalic acid/tetramethylene adipate (PBAT) is a kind of polyester material of complete biodegradable, in nature
Under the conditions of can by multiple-microorganism and animal and plant body enzyme dispersion metabolism, finally be degraded to water and carbon dioxide.Gather to benzene
Dioctyl phthalate/tetramethylene adipate has a characteristic of poly adipate succinic acid ester and poly terephthalic acid simultaneously, existing good
Ductility and elongation at break, also there is preferably heat resistance and shock resistance, substantially improve original binary polyester material
Performance.
Lignin be in a kind of unformed, molecular structure being widely present in plant containing oxo phenylpropanol or its
The armaticity high polymer of derivant structure unit.Because the molecular structure of lignin has aromatic radical.Phenolic hydroxyl group, alcoholic extract hydroxyl group,
Carbon-based conjugated double bond isoreactivity group, thus can by oxidation, reduction, hydrolysis, alcoholysis, acidolysis methoxyl group, carboxyl, phthalein,
Various reactive modes such as sulfonation, alkylation, halogenation, polycondensation or graft copolymerization are modified.Lignin has preferable mechanics
Performance and wooden appearance attribute, while from biomass resource, while having degradability quickly under composting conditionses
Can, it is a kind of following material for comparing environmental protection.
The content of the invention
It is an object of the invention to provide a kind of lignin modification PBAT biodegradable plastics and preparation method thereof.
The invention provides a kind of preparation method of lignin modification PBAT biodegradable plastics, it is by biodegradation
Biological material lignin obtained quality modified PBAT biodegradable plastic after composite modified is introduced on the basis of material PBAT,
While degradable requirement is met, the mechanical property of pure PBAT resins is enhanced, and effectively reduce this kind of plastics
Cost is obtained, is allowed to be more beneficial for marketing.
Present invention also offers a kind of lignin modification PBAT biodegradable plastics, by the various functions auxiliary agent for adding
Synergy, can effectively by the reactive group on lignin surface and the feature of PBAT polymer segments on microcosmic
Group can be combined together, and macroscopically both materials are preferably being merged so as to excellent wooden of processability
Plain modified PBAT biodegradation membrane material, is widely portable to the membrane materials such as shopping bag, refuse bag, mulch film, awning film.
To achieve the above object, the present invention uses following technical scheme：
The first aspect of the invention is to provide a kind of preparation method of lignin modification PBAT biodegradable plastics, including
Following steps：
(1) a certain amount of poly terephthalic acid/tetramethylene adipate, lignin are vacuum dried respectively；
(2) dried poly terephthalic acid/tetramethylene adipate and lignin and chain extension is added in high mixer
Agent, antioxidant, plasticizer, lubricant, heat stabilizer, after being sufficiently mixed, obtain mixed material；
(3) by gained mixed material through double screw extruder extruding pelletization, lignin-PBAT composite plastics grain is obtained；
(4) lignin-PBAT composite plastics grain is carried out into blown film at a certain temperature, lignin modification PBAT is obtained
Biodegradable plastic.
Further, the poly terephthalic acid/tetramethylene adipate is by gathering that petroleum-based feedstock route synthesizes
Terephthalic acid (TPA)/tetramethylene adipate；Preferably, the raw material poly terephthalic acid/tetramethylene adipate uses Xinjiang
The trade mark of Tun He companies of Lanshan County production is the poly terephthalic acid/tetramethylene adipate (PBAT) of 801T.
Further, lignin is former powder in the step (1), and its particle diameter is 100~800 mesh；Its particle diameter is preferably 150
~600 mesh；Preferably 200~500 mesh；More preferably 300~400 mesh.
Further, the drying process in the step (1) is：Drying temperature is 25~40 DEG C, and drying time is 1.5h
~3h, vacuum is 0~5000Pa (absolute pressure)；Preferably, drying temperature be 28~36 DEG C, drying time be 2h~
2.5h, vacuum is 100~3000Pa (absolute pressure)；It is further preferable that drying temperature is 30~32 DEG C, drying time is
2.3h, vacuum is 1000~2000Pa (absolute pressure).
Further, in the step (2), the heat stabilizer is selected from maleic anhydride, epoxidized soybean oil
Kind；The lubricant is selected from one or two or more kinds mixture in calcium stearate, zinc stearate, oleamide series lubricant agent；
The plasticizer is selected from ATBC, triethyl citrate, ATBC, triacetyl glycerine, the last of the ten Heavenly stems two
One or two or more kinds compound in dibutyl phthalate；The antioxidant is selected from butylated hydroxy anisole, butylated hydroxy-a
Benzene, butyl are to biphenol, the isodecyl ester of phosphorous acid benzene two, pentaerythritol bis-phosphite, 3- (3,5- di-t-butyl -4- hydroxy benzenes
Base) propionate, phosphorous acid three (2,4- di-tert-butyl-phenyl) ester, 3,5- di-tert-butyl-hydroxy phenyls propionic acid ten
One or more compounds in caprylate；The chain extender is selected from hydroquinone two hydroxy ethyl ether, resorcinol two
One or more compoundings in hydroxyethyl ether, bisphenol-A, ethylene glycol, 1,4- butanediols, 1,6-HD, diethylene glycol
Thing.
Further, the mixing temperature of high mixer described in the step (3) be 100~110 DEG C, rotating speed be 800~
1000r/min, incorporation time is 10~20min.
Further, the extrusion temperature of double screw extruder is 120~190 DEG C in the step (3)；Preferably 130~
170℃；More preferably 140~160 DEG C.
Further, blown film temperature is 125~160 DEG C in the step (4)；Preferably 130~150 DEG C；More preferably
135~145 DEG C.
Further, in the preparation method of lignin modification PBAT biodegradable plastics, count by weight, each original
Material consumption proportion is as follows：
Preferably, in the preparation method of lignin modification PBAT biodegradable plastics, count by weight, each raw material
Consumption proportion is as follows：
Further, wherein the parts by weight of each raw material are 100% calculating, actual amount according to the effective content of raw material
Need to be converted according to the actually active content of raw material.
The second aspect of the invention is to provide lignin modification PBAT biodegradations prepared by a kind of use above method
Plastics.
The third aspect of the invention is to provide a kind of above-mentioned lignin modification PBAT biodegradable plastics and is preparing life
Application in thing degraded shopping bag, refuse bag, mulch film, green house of vegetables film.
The present invention uses above-mentioned technical proposal, compared with prior art, have the following technical effect that：
The lignin original powder that the inventive method is prepared by use from the biomass that nature is widely present, to PBAT
Biodegradable resin is modified modification and lignin-PBAT composite biological degradation plastics is obtained, and can be widely used for shopping bag, rubbish
The membrane materials such as bag, mulch film, awning film；The lignin-PBAT composite biological degradation plastics are relative to traditional pure PBAT resin-mades
While same solution white pollution, (raw material of PBAT is to benzene two can effectively to reduce petroleum based material for standby membrane material
Formic acid, adipic acid, butanediol are all formed from petroleum refining) consumption, and the mechanical property for effectively improving membrane material；
Raw material of the present invention are cheap and easy to get, and preparation process is simple is easy to operate, and low production cost is conducive to marketing.
Specific embodiment
The present invention is described in more detail below by specific embodiment, for a better understanding of the present invention,
But following embodiments are not intended to limit the scope of the invention.
The preparation of the lignin modification PBAT biodegradable plastics of embodiment 1
(1) count by weight, each raw material dosage proportioning of use is as follows：
(2) specific preparation method, comprises the following steps：
(1) a certain amount of PBAT, lignin powder (150 mesh) are dried into 2.5h under the conditions of 25 DEG C, 0~5000Pa；
(2) dried PBAT, lignin powder and bisphenol-A, dibutyl hydroxy toluene, citric acid are added in high mixer
Triethyl, epoxidized soybean oil, zinc stearate, control material temperature are 100-105 DEG C, are mixed 15 minutes, and rotating speed is 900r/min；
(3) by gained mixed material by double screw extruder extruding pelletization, extrusion temperature is controlled for 120~140 DEG C, system
Obtain lignin-PBAT composite plastic particles；
(4) by the lignin-PBAT composite plastics by blown film, control blown film temperature for 125~130 DEG C, be made various
Lignin modification PBAT biodegradable plastics.
The preparation of the lignin modification PBAT biodegradable plastics of embodiment 2
(1) count by weight, each raw material dosage proportioning of use is as follows：
(2) specific preparation method, comprises the following steps：
(1) a certain amount of PBAT, lignin (150 mesh) are dried into 3h under the conditions of 25 DEG C, 0~5000Pa；
(2) dried PBAT, lignin and ATBC, resorcinol two are added in high mixer
, to biphenol, epoxidized soybean oil, calcium stearate, control material temperature is 110 DEG C, is mixed 20 minutes, rotating speed for hydroxyethyl ether, butyl
It is 1000r/min；
(3) by gained mixed material by double screw extruder extruding pelletization, extrusion temperature is controlled for 130~150 DEG C, system
Obtain lignin-PBAT composite plastic particles；
(4) by the lignin-PBAT composite plastics by blown film, control blown film temperature for 135~140 DEG C, be made various
Lignin modification PBAT biodegradable plastics.
The preparation of the lignin modification PBAT biodegradable plastics of embodiment 3
(1) count by weight, each raw material dosage proportioning of use is as follows：
(2) specific preparation method, comprises the following steps：
(1) a certain amount of PBAT, lignin (200 mesh) are dried into 3h under the conditions of 25 DEG C, 0~5000Pa；
(2) dried PBAT, lignin, maleic anhydride, triacetyl glycerine, butyl pair are added in high mixer
Biphenol, BDO, zinc stearate, control material temperature are 105 DEG C, are mixed 25 minutes, and rotating speed is 1000r/min；
(3) by gained mixed material by double screw extruder extruding pelletization, extrusion temperature is controlled for 150~160 DEG C, system
Obtain lignin-PBAT composite plastic particles；
(4) by the lignin-PBAT composite plastics by blown film, control blown film temperature for 140~150 DEG C, be made various
Lignin modification PBAT biodegradable plastics.
The preparation of the lignin modification PBAT biodegradable plastics of embodiment 4
(1) count by weight, each raw material dosage proportioning of use is as follows：
(2) specific preparation method, comprises the following steps：
(1) a certain amount of PBAT, lignin (300 mesh) are dried into 3h under the conditions of 25 DEG C, 0~5000Pa；
(2) add dried PBAT, lignin, triacetyl glycerine, bisphenol-A, phosphorous acid benzene two different in high mixer
Last of the ten Heavenly stems ester, epoxidized soybean oil, zinc stearate, control material temperature are 105 DEG C, are mixed 25 minutes, and rotating speed is 800r/min；
(3) by gained mixed material by double screw extruder extruding pelletization, extrusion temperature is controlled for 185~190 DEG C, system
Obtain lignin-PBAT composite plastic particles；
(4) by the lignin-PBAT composite plastics by blown film, control blown film temperature for 130~135 DEG C, be made various
Lignin modification PBAT biodegradable plastics.
Comparative example 1 is by the poly terephthalic acid/tetramethylene adipate of unmodified Xinjiang Lanshan County village river trade mark 801T
(PBAT) as a comparison case 1.
Performance test
Using universal electrical tensile testing machine (SUN500 types are manufactured by Italian GALDABINI companies) to above-mentioned implementation
Example 1-4, the tensile strength of the material of comparative example 1, elongation at break are measured, and according to GB GB/T16716.7-2012 standards
Biological compost degradation experiment is carried out to above-mentioned material, specific testing result is as shown in table 1：
Each performance applications test data of the embodiment 1~4 of table 1 and comparative example 1
| Tensile strength/MPa | Elongation at break/% | 6 months compost degradation rate % | |
| Embodiment 1 | 30 | 330 | 99 |
| Embodiment 2 | 35 | 328 | 98 |
| Embodiment 3 | 38 | 335 | 98 |
| Embodiment 4 | 40 | 340 | 97 |
| Comparative example 1 | 23 | 332 | 99 |
Be can be seen that by the application test result in above-mentioned table 1：With the non-modified pure poly terephthalic acid of degradable material/
Tetramethylene adipate comparative example 1 is compared, by the situation that the embodiment 1~4 of lignin modification is basically unchanged in degradation property
Under, there is lifting in mechanical property by the PBAT of lignin modification, the growth rate of tensile strength is respectively 30.4%,
52.2%th, 65.2% and 73.9%, obtain significantly strengthening；Wherein understood with lignin by above-mentioned tensile strength enhancing rate
The increase of content, this enhancing is more and more obvious.Therefore, the obtained lignin modification PBAT biodegradable plastics of the present invention are in symbol
While closing degradable requirement, the mechanical property of pure PBAT resins is effectively enhanced, and reduce production cost, be allowed to more
Be conducive to marketing, relatively existing unmodified pure poly terephthalic acid/tetramethylene adipate has obvious technology
Advantage.
Specific embodiment of the invention has been described in detail above, but it is intended only as example, and the present invention is not limited
It is formed on particular embodiments described above.To those skilled in the art, any equivalent modifications carried out to the present invention and
Replacement is also all among scope of the invention.Therefore, the impartial conversion made without departing from the spirit and scope of the invention and
Modification, all should be contained within the scope of the invention.
Claims (10)
1. a kind of preparation method of lignin modification PBAT biodegradable plastics, it is characterised in that comprise the following steps：
(1) a certain amount of poly terephthalic acid/tetramethylene adipate, lignin are vacuum dried respectively；
(2) dried poly terephthalic acid/tetramethylene adipate and lignin and chain extender, anti-are added in high mixer
Oxygen agent, plasticizer, lubricant, heat stabilizer, after being sufficiently mixed, obtain mixed material；
(3) by gained mixed material through double screw extruder extruding pelletization, lignin-PBAT composite plastics grain is obtained；
(4) lignin-PBAT composite plastics grain is carried out into blown film at a certain temperature, lignin modification PBAT is obtained biological
Degradative plastics.
2. preparation method according to claim 1, it is characterised in that the poly terephthalic acid/tetramethylene adipate
It is the poly terephthalic acid/tetramethylene adipate synthesized by petroleum-based feedstock route.
3. preparation method according to claim 1, it is characterised in that in the step (1) particle diameter of lignin be 100~
800 mesh.
4. preparation method according to claim 1, it is characterised in that the drying process in the step (1) is：Dry temperature
It is 25~40 DEG C to spend, and drying time is 1.5h~3h, and vacuum is 0~5000Pa.
5. preparation method according to claim 1, it is characterised in that in the step (2), the heat stabilizer is selected from suitable
One kind in anhydride maleique, epoxidized soybean oil；The lubricant is selected from calcium stearate, zinc stearate, oleamide class lubrication
One or two or more kinds mixture in agent；The plasticizer is selected from ATBC, triethyl citrate, acetyl tributyl citrate
One or two or more kinds compound in tri-n-butyl, triacetyl glycerine, dibutyl sebacate；The antioxidant is selected from fourth
Base BHA, dibutyl hydroxy toluene, butyl to biphenol, the isodecyl ester of phosphorous acid benzene two, pentaerythritol bis-phosphite,
3- (3,5- di-tert-butyl-hydroxy phenyl) propionate, phosphorous acid three (2,4- di-tert-butyl-phenyl) ester, 3,5- bis-
One or more compounds in the caprylate of tert-butyl-hydroxy phenyl propionic acid ten；The chain extender is selected to benzene two
Phenol dihydroxyethyl ether, resorcinol dihydroxyethyl ether, bisphenol-A, ethylene glycol, 1,4- butanediols, 1,6-HD, diethylene glycol
In one or more compounds.
6. preparation method according to claim 1, it is characterised in that the extrusion of double screw extruder in the step (3)
Temperature is 120~190 DEG C.
7. preparation method according to claim 1, it is characterised in that blown film temperature is 125~160 in the step (4)
℃。
8. the preparation method according to claim any one of 1-7, it is characterised in that count by weight, each raw material dosage
Proportioning is as follows：
9. the lignin modification PBAT biodegradable plastics that prepared by a kind of preparation method as described in claim any one of 1-8.
10. a kind of lignin modification PBAT biodegradable plastics as claimed in claim 9 are preparing biodegradable shopping bag, rubbish
Application in rubbish bag, mulch film, green house of vegetables film.
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107141826A (en) * | 2017-07-05 | 2017-09-08 | 江苏旭华圣洛迪建材有限公司 | A kind of degradable lignin-base composite and preparation method thereof |
| CN108359224A (en) * | 2018-02-13 | 2018-08-03 | 南京工业大学 | A kind of degradable mulch and preparation method thereof with slow-release nitrogen fertilizer |
| CN108485207A (en) * | 2018-02-13 | 2018-09-04 | 南京工业大学 | A kind of degradable mulch and preparation method thereof with slow-release phosphate fertilizer |
| CN109535667A (en) * | 2018-11-01 | 2019-03-29 | 刘辉 | A kind of biology base degradative tableware |
| CN109735067A (en) * | 2018-09-25 | 2019-05-10 | 北京林业大学 | A kind of lignin-base biodegradable plastics and preparation method thereof |
| CN109943039A (en) * | 2019-02-15 | 2019-06-28 | 北京林业大学 | A kind of methylation lignin/PBAT biodegradable plastics and preparation method thereof |
| CN111978692A (en) * | 2020-09-11 | 2020-11-24 | 苏州威瑞成新材料有限公司 | Degradable plastic and preparation method thereof |
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| CN113402857A (en) * | 2021-06-09 | 2021-09-17 | 华南理工大学 | Lignin/PBAT composite material and preparation method and application thereof |
| CN113831518A (en) * | 2021-11-15 | 2021-12-24 | 中核华纬工程设计研究有限公司 | Method for modifying PBAT (poly (butylene adipate-co-terephthalate)) by using small-molecular phenol |
| CN113881195A (en) * | 2021-09-30 | 2022-01-04 | 宜宾天亿新材料科技有限公司 | Biodegradable resin composition and preparation method thereof |
| CN114213816A (en) * | 2022-01-13 | 2022-03-22 | 周元康 | Green environment-friendly degradable plastic and preparation method thereof |
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| CN116102854A (en) * | 2022-12-13 | 2023-05-12 | 湖北宜化降解新材料有限公司 | Preparation method of polybutylene adipate-terephthalate with high lignin content |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107141826A (en) * | 2017-07-05 | 2017-09-08 | 江苏旭华圣洛迪建材有限公司 | A kind of degradable lignin-base composite and preparation method thereof |
| CN108359224A (en) * | 2018-02-13 | 2018-08-03 | 南京工业大学 | A kind of degradable mulch and preparation method thereof with slow-release nitrogen fertilizer |
| CN108485207A (en) * | 2018-02-13 | 2018-09-04 | 南京工业大学 | A kind of degradable mulch and preparation method thereof with slow-release phosphate fertilizer |
| CN109735067A (en) * | 2018-09-25 | 2019-05-10 | 北京林业大学 | A kind of lignin-base biodegradable plastics and preparation method thereof |
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