CN108948703A - A kind of weather-proof degradation plastic bottle and preparation method thereof - Google Patents
A kind of weather-proof degradation plastic bottle and preparation method thereof Download PDFInfo
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- 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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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08K2003/2241—Titanium dioxide
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Abstract
The invention discloses a kind of weatherability degradation plastic bottles and preparation method thereof, component comprising following parts by weight: 50-70 parts of polylactic acid, attapulgite/15-25 parts of polymethyl methacrylate hybrid particle, 1-5 parts of nano-titanium dioxide, 1-5 parts of nano zine oxide, 5-10 parts of glass fibre, 0.01-1 parts of plasticizer, 0.05-1.2 parts of compatilizer.The plastic bottle that the present invention is prepared is environmentally protective, it is degradable, it can be applied to outdoor, test through climate, pass through the introducing of attapulgite modified grafting polymethyl methacrylate, mechanical performance, the weatherability of polylactic acid are improved, meanwhile, the plastic bottle that joined nano particle has the excellent characteristics such as uvioresistant, sterilization, antifouling.
Description
Technical field
The present invention relates to plastic products production technical field more particularly to a kind of weather-proof degradation plastic bottles.
Background technique
Polylactic acid production process is pollution-free, and product can be biodegradable, realizes circulation in nature, therefore is ideal
Green Polymer Material.However pure crystallization of polylactic acid resin speed is slow, moulded products shrinking percentage is big, poor dimensional stability, this
Stature matter is crisp, and processing heat stability difference etc. limits its application as engineering plastics.Plastic products shine vulnerable to sunlight simultaneously
It penetrates, temperature change, the influence of the external conditions such as wind and weather, occurs fading, discoloration, be cracked, a system such as dusting and intensity decline
Column aging phenomenon, furthermore the growth of bacterium also affects the preservation of food.
In recent decades, a large amount of research, attapulgite are had been carried out using the filling-modified poly-lactic acid material of attapulgite
Nano effect make it often to be unfavorable for the promotion of system performance when biggish stick crystalline substance aggregation presence, directly addition, therefore it is logical
Crossing chemical means to change its surface property is a kind of common modified method.
Polymethyl methacrylate (PMMA) is a kind of exploitation important thermoplastic earlier, is had preferable transparent
Property, chemical stability and weatherability, different dyeing, easy processing, attractive appearance have in construction industry and kind are widely applied.By PMMA
Strand is grafted to attapulgite single stick crystalline substance surface, can get a kind of blank particle of hybrid material, and is effectively improved bumps
The agglomeration of stick soil stick crystalline substance in the polymer realizes nano-dispersion.
Nanoparticle is a kind of new inorganic material of multifunctionality, and nano-titanium dioxide, nano zine oxide are in light
Sterilized for a long time under the action of ultraviolet light, to bacillus subtilis black variety gemma, Pseudomonas aeruginosa, Escherichia coli, gold-coloured staphylococci,
The killing rate of salmonella, tooth branch bacterium and aspergillus reaches 98% or more；Can absorb ultraviolet light and reflection, scatter it is ultraviolet
Line, moreover it is possible to penetrate visible light, be the ultra-violet protecting agent of superior performance, extremely promising physical shielding type.
A kind of attapulgite/poly lactic acid nano composite material of 201610931603.2 invention of Chinese patent and its preparation side
Method, attapulgite obtained/poly lactic acid nano composite material performance are significantly promoted, biodegradable membrane material, sheet material, injection molding,
Packaging material field has wide application prospect.But attapulgite is extremely difficult to reinforcing effect in polylactic acid poor dispersion
It maximizes, and there is no ultraviolet-resistent property, weatherability is poor.
Summary of the invention
In order to solve the deficiencies in the prior art, it is an object of that present invention to provide a kind of weather-proof degradation plastic bottle and its systems
Preparation Method, it is compound using attapulgite modified grafting polymethyl methacrylate and PLA, and nanoparticle and other auxiliary agents is added
The degradation plastic bottle with very good mechanical properties, weatherability, uvioresistant and biocidal property is prepared.
Weather-proof degradation plastic bottle of the invention be include following raw material composition:
50-70 parts of polylactic acid, attapulgite/15-25 parts of polymethyl methacrylate hybrid particle, nano-titanium dioxide 1-
5 parts, 1-5 parts of nano zine oxide, 5-10 parts of glass fibre, 0.01-1 parts of plasticizer, 0.05-1.2 parts of compatilizer.
The purity and partial size of attapulgite and the degree of polymerization of polymethyl methacrylate influence whether plastic bottle raw material
Composition, and then to influence the mechanical property, light transmission and weatherability of lactic acid composite material.
Attapulgite partial size is 30-100 μm, and the attapulgite is the attapulgite after purification.
Preparing the weather-proof degradation plastic bottle includes following preparation step: the method for purification of attapulgite are as follows: by 1 part
Sodium pyrophosphate be dissolved in 100 parts of deionized waters, 20 parts of attapulgites are added, stir 1h at 30-60 DEG C, when standing one section
Between after take upper layer suspension, HCl solution is added, stirs 1h at 30-60 DEG C.Centrifuge separation, dries after being washed with water to neutrality, obtains
Attapulgite after to purification.
Preparing the weather-proof degradation plastic bottle includes following preparation step: attapulgite/polymethyl methacrylate
Hybrid particle preparation step are as follows: (1) in attapulgite a certain amount of purification after addition amino silicane coupling agent solution, 50 DEG C
Stir 2h, after being washed and wash with alcohol respectively dry, obtain it is amination modified after attapulgite.(2) by modified concave convex rod
It is added a certain amount of dimethylbenzene, methyl methacrylate, initiator in soil, ultrasonic disperse 10-20min, in a nitrogen environment, 80
DEG C magnetic agitation 3-5h, washs drying after the reaction was completed, obtains attapulgite/polymethyl methacrylate hybrid particle.
It is amination modified by being carried out to attapulgite, so that modifying agent is adsorbed on attapulgite's surface, is formed and wrapped on surface
Coating reduces interparticle reunion to reduce surface tension.To modified attapulgite, cause activity using initiator
Site is grafted polymethyl methacrylate using surface grafting polymerization method, improves the tensile resistance and resistance to ag(e)ing of material
Energy.
Further preferably weather-proof degradation plastic bottle of the invention be include that following raw material forms: polylactic acid 60
Part, attapulgite/20 parts of polymethyl methacrylate hybrid particle, 3 parts of nano-titanium dioxide, 2 parts of nano zine oxide, glass fibers
5 parts, 0.02 part of plasticizer, 0.1 part of compatilizer of dimension.
The nano-titanium dioxide partial size is 30-100nm, and the nano titanium dioxide crystal form is Detitanium-ore-type, institute
The Particle Size of Nanometer ZnO stated is 30-100nm.
For the selected nanoparticle of the present invention since size is smaller, activity is big, can reflect, scatters ultraviolet and suction
Ultraviolet light is received, to have stronger obstructing capacity to ultraviolet light, while can effectively kill harmful bacteria, plays and resists antibacterial effect
Fruit.
The plasticizer is in triacetyl glycerine, citrate ether, aliphatic ester ether and 2-Butoxyethyl acetate
One or two.
Although additive amount is less in the present invention for plasticizer, each component dispersion in recombination process can be improved,
Increase the connectivity between each component, improves the mechanical performance of composite material.
The compatilizer is octadecyl bromination ammonium, p-hydroxybenzoate, diisocyanate and septichen
One of this ester.
The selected compatilizer of the present invention can improve attapulgite/polymethyl methacrylate hybrid particle, nano particle
Dispersibility in polylactic acid, prevents particle from reuniting.
The hydrochloric acid solution is concentration 1-3mol/L.
The amino silicane coupling agent is gamma-aminopropyl-triethoxy-silane, γ-aminopropyltrimethoxysilane, N- β
(aminoethyl)-γ-aminopropyltrimethoxysilane, N- β (aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane and γ-ammonia third
One of ylmethyl diethoxy silane is a variety of.
Interaction between the adjustable attapulgite of silane coupling agent and methyl methacrylate improves polymerization process
The dispersibility and the degree of polymerization of middle particle, to improve the comprehensive performance of lactic acid composite material.
The mass ratio of attapulgite, dimethylbenzene, methyl methacrylate and initiator after the purification is 3-8:50:
10-15:0.5-2, the initiator are azo-initiator.
Weather-proof degradation plastic bottle of the invention the preparation method comprises the following steps:
Polylactic acid by weight, attapulgite/polymethyl methacrylate hybrid particle, nano-titanium dioxide, nano oxygen
Change zinc, glass fibre, plasticizer, compatilizer is added in high-speed mixer, after mixing using double screw extruder in 190-
It is squeezed out at 240 DEG C, finally carries out blow molding, obtain weather-proof degradation plastic bottle.
It is had the advantage that using the preparation-obtained weather-proof degradation plastic bottle of above technical scheme
1, the attapulgite grafting polymethyl methacrylate of modification used herein and polylactic acid carry out compound, significantly
Improve weatherability, the mechanical performance of polylactic acid.
2, the present invention joined nano-titanium dioxide and zinc oxide in the feed, the nano-titanium dioxide of Detitanium-ore-type and receive
Rice zinc oxide so that plastic bottle has the function of eliminating peculiar smell, antibacterial, antibacterial, while having absorption and barrier property to ultraviolet light,
Improve uvioresistant, the performances such as ageing-resistant of polylactic acid plastic bottle.
Specific embodiment
The following examples are further described to of the invention.
Embodiment 1
A kind of weather-proof degradation plastic bottle, preparation method include the next steps:
(1) 1 part of sodium pyrophosphate is dissolved in 100 parts of deionized waters, 20 parts of attapulgites is added, at 30-60 DEG C
1h is stirred, upper layer suspension is taken after standing a period of time, HCl solution is added, stirs 1h at 30-60 DEG C.Centrifuge separation, uses water
It is dried after being washed till neutrality, the attapulgite after being purified；
(2) the addition gamma-aminopropyl-triethoxy-silane solution in the attapulgite after the purification that step (1) obtains, 50
DEG C stirring 2h, washed and washed with alcohol respectively and dried afterwards three times, obtain it is amination modified after attapulgite；
(3) a certain amount of dimethylbenzene, methyl methacrylate is added in the modified attapulgite that step (2) obtains
Ester, initiator, ultrasonic disperse 10-20min, in a nitrogen environment, 80 DEG C of magnetic agitation 3-5h wash drying after the reaction was completed,
Obtain attapulgite/polymethyl methacrylate hybrid particle, wherein attapulgite, dimethylbenzene, methacrylic acid after purification
The mass ratio of methyl esters and initiator is 3:50:10:0.5；
(4) it weighs by weight in 15 parts of steps (3) and obtains attapulgite/polymethyl methacrylate hybrid particle, gather
50 parts of lactic acid, 1 part of nano-titanium dioxide, 1 part of nano zine oxide, 5 parts of glass fibre, 0.01 part of triacetyl glycerine, octadecane
It 0.05 part of base ammonium bromide, is added in high-speed mixer, is squeezed out at 190-240 DEG C using double screw extruder after mixing,
Blow molding is finally carried out, weather-proof degradation plastic bottle is obtained.
Embodiment 2
A kind of weather-proof degradation plastic bottle, preparation method include the next steps:
(1) 1 part of sodium pyrophosphate is dissolved in 100 parts of deionized waters, 20 parts of attapulgites is added, at 30-60 DEG C
1h is stirred, upper layer suspension is taken after standing a period of time, HCl solution is added, stirs 1h at 30-60 DEG C.Centrifuge separation, uses water
It is dried after being washed till neutrality, the attapulgite after being purified；
(2) amino silicane coupling agent solution, 50 DEG C of stirrings are added in the attapulgite after the purification that step (1) obtains
2h is washed and is washed with alcohol respectively and dried afterwards three times, obtain it is amination modified after attapulgite；
(3) a certain amount of dimethylbenzene, methyl methacrylate is added in the modified attapulgite that step (2) obtains
Ester, initiator, ultrasonic disperse 10-20min, in a nitrogen environment, 80 DEG C of magnetic agitation 3-5h wash drying after the reaction was completed,
Obtain attapulgite/polymethyl methacrylate hybrid particle, wherein attapulgite, dimethylbenzene, methacrylic acid after purification
The mass ratio of methyl esters and initiator is 4:50:12:0.7；
(4) it weighs by weight in 20 parts of steps (3) and obtains attapulgite/polymethyl methacrylate hybrid particle, gather
55 parts of lactic acid, 2 parts of nano-titanium dioxide, 1 part of nano zine oxide, 6 parts of glass fibre, 0.03 part of plasticizer, 0.07 part of compatilizer,
It is added in high-speed mixer, is squeezed out at 190-240 DEG C using double screw extruder, be finally blow molded into after mixing
Shape obtains weather-proof degradation plastic bottle.
Embodiment 3
A kind of weather-proof degradation plastic bottle, preparation method include the next steps:
(1) 1 part of sodium pyrophosphate is dissolved in 100 parts of deionized waters, 20 parts of attapulgites is added, at 30-60 DEG C
1h is stirred, upper layer suspension is taken after standing a period of time, HCl solution is added, stirs 1h at 30-60 DEG C.Centrifuge separation, uses water
It is dried after being washed till neutrality, the attapulgite after being purified；
(2) N- β (aminoethyl)-γ-aminopropyl trimethoxy is added in the attapulgite after the purification that step (1) obtains
Solution of silane, 50 DEG C of stirring 2h, is washed and is washed with alcohol respectively and dried afterwards three times, obtain it is amination modified after attapulgite；
(3) a certain amount of dimethylbenzene, methyl methacrylate is added in the modified attapulgite that step (2) obtains
Ester, initiator, ultrasonic disperse 10-20min, in a nitrogen environment, 80 DEG C of magnetic agitation 3-5h wash drying after the reaction was completed,
Obtain attapulgite/polymethyl methacrylate hybrid particle, wherein attapulgite, dimethylbenzene, methacrylic acid after purification
The mass ratio of methyl esters and initiator is 5:50:14:0.8；
(4) it weighs by weight in 15 parts of steps (3) and obtains attapulgite/polymethyl methacrylate hybrid particle, gather
60 parts of lactic acid, 3 parts of nano-titanium dioxide, 2 parts of nano zine oxide, 7 parts of glass fibre, 0.03 part of plasticizer, 0.08 part of compatilizer,
It is added in high-speed mixer, is squeezed out at 190-240 DEG C using double screw extruder, be finally blow molded into after mixing
Shape obtains weather-proof degradation plastic bottle.
Embodiment 4
A kind of weather-proof degradation plastic bottle, preparation method include the next steps:
(1) 1 part of sodium pyrophosphate is dissolved in 100 parts of deionized waters, 20 parts of attapulgites is added, at 30-60 DEG C
1h is stirred, upper layer suspension is taken after standing a period of time, HCl solution is added, stirs 1h at 30-60 DEG C.Centrifuge separation, uses water
It is dried after being washed till neutrality, the attapulgite after being purified；
(2) it is molten that γ-aminopropyltriethoxy diethoxy silane is added in the attapulgite after the purification that step (1) obtains
Liquid, 50 DEG C of stirring 2h, is washed and is washed with alcohol respectively and dried afterwards three times, obtain it is amination modified after attapulgite；
(3) a certain amount of dimethylbenzene, methyl methacrylate is added in the modified attapulgite that step (2) obtains
Ester, initiator, ultrasonic disperse 10-20min, in a nitrogen environment, 80 DEG C of magnetic agitation 3-5h wash drying after the reaction was completed,
Obtain attapulgite/polymethyl methacrylate hybrid particle, wherein attapulgite, dimethylbenzene, methacrylic acid after purification
The mass ratio of methyl esters and initiator is 6:50:15:1.2；
(4) it weighs by weight in 15 parts of steps (3) and obtains attapulgite/polymethyl methacrylate hybrid particle, gather
65 parts of lactic acid, 3 parts of nano-titanium dioxide, 3 parts of nano zine oxide, 8 parts of glass fibre, 0.05 part of plasticizer, 0.09 part of compatilizer,
It is added in high-speed mixer, is squeezed out at 190-240 DEG C using double screw extruder, be finally blow molded into after mixing
Shape obtains weather-proof degradation plastic bottle.
Comparative example 1
A kind of weather-proof degradation plastic bottle, preparation method include the next steps:
60 parts of polylactic acid are weighed by weight, 3 parts of nano-titanium dioxide, 2 parts of nano zine oxide, 7 parts of glass fibre, are plasticized
It 0.03 part of agent, 0.08 part of compatilizer, is added in high-speed mixer, after mixing using double screw extruder at 190-240 DEG C
Under be extruded into embryo, finally carry out blow molding, obtain weather-proof degradation plastic bottle.
Comparative example 2
A kind of weather-proof degradation plastic bottle, preparation method include the next steps:
(1) 1 part of sodium pyrophosphate is dissolved in 100 parts of deionized waters, 20 parts of attapulgites is added, at 30-60 DEG C
1h is stirred, upper layer suspension is taken after standing a period of time, HCl solution is added, stirs 1h at 30-60 DEG C.Centrifuge separation, uses water
It is dried after being washed till neutrality, the attapulgite after being purified；
(2) N- β (aminoethyl)-γ-aminopropyl trimethoxy is added in the attapulgite after the purification that step (1) obtains
Solution of silane, 50 DEG C of stirring 2h, is washed and is washed with alcohol respectively and dried afterwards three times, obtain it is amination modified after attapulgite；
(3) a certain amount of dimethylbenzene, methyl methacrylate is added in the modified attapulgite that step (2) obtains
Ester, initiator, ultrasonic disperse 10-20min, in a nitrogen environment, 80 DEG C of magnetic agitation 3-5h wash drying after the reaction was completed,
Obtain attapulgite/polymethyl methacrylate hybrid particle, wherein attapulgite, dimethylbenzene, methacrylic acid after purification
The mass ratio of methyl esters and initiator is 5:50:14:0.8；
(4) it weighs by weight in 15 parts of steps (3) and obtains attapulgite/polymethyl methacrylate hybrid particle, gather
It 60 parts of lactic acid, 7 parts of glass fibre, 0.03 part of plasticizer, 0.08 part of compatilizer, is added in high-speed mixer, adopts after mixing
It is squeezed out at 190-240 DEG C with double screw extruder, finally carries out blow molding, obtain weather-proof degradation plastic bottle.
Comparative example 3
A kind of weather-proof degradation plastic bottle, preparation method include the next steps:
60 parts of polylactic acid are weighed by weight, and 7 parts of glass fibre, 0.03 part of plasticizer, 0.08 part of compatilizer, high speed is added
In mixing machine, is squeezed out at 190-240 DEG C using double screw extruder after mixing, finally carry out blow molding, obtain resistance to
Time type degradation plastic bottle.
Using plastics ultraviolet light exposure test method ASTM D4329-05, sample is put and is irradiated in the UV lamp,
The degree of aging (table 1) of sample is observed under different time sections.
1 ultraviolet irradiation of table influences (UV intensity 3000uW/cm to ageing of plastics2)
According to GB/T1040-1992, GB/T1040.1-2006 and GB/T1043-1993, tensile strength is carried out, fracture is stretched
Long rate, impact strength detection, using JC/T897-2014 improved method test sample anti-microbial property, the results are shown in Table 2:
Table 2
By Tables 1 and 2 it is found that the degradable poly lactic acid composite that embodiment 1-4 is prepared has preferable mechanicalness
Energy and ageing-resistant performance, with the increase of hybrid particle and nano-particle content, the uviolresistance of composite material is stretched by force
Degree, impact strength and antibiotic property also increase accordingly.It is multiple by comparative example 1-3 it is found that when being added without hybrid particle or nano particle
Condensation material various aspects of performance is declined, and when being added without nano particle, does not have antibiotic property.
Claims (10)
1. a kind of weather-proof degradation plastic bottle, it is characterised in that: it is made of the raw material of following parts by weight, 50-70 parts of polylactic acid,
Attapulgite/15-25 parts of polymethyl methacrylate hybrid particle, 1-5 parts of nano-titanium dioxide, 1-5 parts of nano zine oxide, glass
5-10 parts of glass fiber, 0.01-1 parts of plasticizer, 0.05-1.2 parts of compatilizer.
2. a kind of weather-proof degradation plastic bottle as described in claim 1, it is characterised in that: the attapulgite partial size is
10-50 μm, the attapulgite is the attapulgite after purification, the method for purification of the attapulgite are as follows: by pyrophosphoric acid
Sodium is dissolved in deionized water, and attapulgite is added, and 1-2h is stirred at 30-60 DEG C, takes upper layer to suspend after standing a period of time
Liquid is added HCl solution, 1h is stirred at 30-60 DEG C, is centrifugated, dries after being washed with water to neutrality, the bumps after being purified
Stick soil.
3. a kind of weather-proof degradation plastic bottle as described in claim 1, it is characterised in that: the attapulgite/poly- first
Base methyl acrylate hybrid particle preparation step are as follows: (1) it is even that amino silane is added in the attapulgite after a certain amount of purification
Join agent solution, 50 DEG C of stirring 2h, after being washed and washed with alcohol respectively dry, obtain it is amination modified after attapulgite.(2) will change
It is added a certain amount of dimethylbenzene, methyl methacrylate, initiator in attapulgite after property, ultrasonic disperse 10-20min,
Under nitrogen environment, 80 DEG C of magnetic agitation 3-5h wash drying after the reaction was completed, obtain attapulgite/polymethyl methacrylate
Hybrid particle.
4. a kind of weather-proof degradation plastic bottle as described in claim 1, it is characterised in that: the nano-titanium dioxide grain
Diameter is 30-100nm, and the nano titanium dioxide crystal form is Detitanium-ore-type.
5. a kind of weather-proof degradation plastic bottle as described in claim 1, it is characterised in that: the plasticizer is three acetic acid
One of glyceride, citrate ether, aliphatic ester ether and 2-Butoxyethyl acetate are a variety of.
6. a kind of weather-proof degradation plastic bottle as described in claim 1, it is characterised in that: the compatilizer is octadecane
One of base ammonium bromide, p-hydroxybenzoate, diisocyanate and septichen this ester are a variety of.
7. a kind of weather-proof degradation plastic bottle as claimed in claim 2, it is characterised in that: hydrochloric acid solution is concentration 1-
3mol/L。
8. a kind of weather-proof degradation plastic bottle as claimed in claim 3, it is characterised in that: amino silicane coupling agent is γ-
Aminopropyl triethoxysilane, γ-aminopropyltrimethoxysilane, N- β (aminoethyl)-γ-aminopropyltrimethoxysilane, N-
One of β (aminoethyl)-γ-aminopropyltriethoxy dimethoxysilane or γ-aminopropyltriethoxy diethoxy silane are a variety of.
9. a kind of weather-proof degradation plastic bottle according to claim 3, it is characterised in that: attapulgite after purification,
The mass ratio of dimethylbenzene, methyl methacrylate and initiator is 3-8:50:10-15:0.5-2, and the initiator is azo
Class initiator.
10. a kind of preparation method of such as described in any item weather-proof degradation plastic bottles of claim 1-9, it is characterised in that:
It should be the preparation method comprises the following steps: polylactic acid, attapulgite/polymethyl methacrylate hybrid particle, nano-titanium dioxide be received by weight
Rice zinc oxide, glass fibre, plasticizer, compatilizer are added in high-speed mixer, are existed after mixing using double screw extruder
It is squeezed out at 190-240 DEG C, finally carries out blow molding, obtain weather-proof degradation plastic bottle.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112409733A (en) * | 2020-11-22 | 2021-02-26 | 颍上县龙裕扬工贸有限公司 | Composite corrosion-resistant plastic product and processing method thereof |
| CN114773646A (en) * | 2022-05-26 | 2022-07-22 | 悟锐新材料科技(江苏)有限公司 | Fully-degradable high-toughness polyvinyl alcohol composite material and preparation method thereof |
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