CN101824211B - Full-biodegradation high-tenacity heat-resistant type polylactic resin and preparation method thereof - Google Patents
Full-biodegradation high-tenacity heat-resistant type polylactic resin and preparation method thereof Download PDFInfo
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Abstract
The invention discloses full-biodegradation high-tenacity heat-resistant type polylactic resin and a preparation method thereof. The polylactic resin comprises polylactic resin, polybutylene succinate, dicumyl peroxide and glycidyl methacrylate; and the weight-average molecular weight of the polylactic resin is 8-13 ten thousand, and the weight-average molecular weight of the polybutylene succinate is 7-11 ten thousand. In parts by weight, the total amount of the polylactic resin and the polybutylene succinate is 100 parts, wherein the polylactic resin accounts for 70-90 parts, the polybutylene succinate accounts for 10-30 parts, the dicumyl peroxide accounts for 0.1-1 part, and the glycidyl methacrylate accounts for 1-10 parts. Compared with the prior art, the full-biodegradation high-tenacity heat-resistant type polylactic resin has good biodegradation property, mechanical property and heat-resisting property; and the preparation method has simple technique process, excellent processing performance and low cost, and can realize large-scale industrial production.
Description
Technical field
The invention belongs to technical field of polymer materials, relate in particular to a kind of full-biodegradation high-tenacity heat-resistant type polylactic resin and preparation method thereof.
Background technology
In 20th century, the appearance of synthesized polymer material has greatly improved human life with fast development.Along with the Application Areas of macromolecular material enlarges day by day, synthesized polymer material has become four big pillars of field of materials side by side with iron and steel, timber and cement.Yet the large-area applications of synthesized polymer material has also produced two significant problems: limited petroleum resource consumption is the white pollution problems that causes of problem and waste plastic totally.Therefore, the research and development to the biodegradated polymer materal that can protect environment are surging forward in worldwide.
POLYACTIC ACID (PLA) be a kind of be raw material with reproducible plant resources; Biodegradable polymer through the chemosynthesis preparation; POLYACTIC ACID can equally carry out various forming process with common polymer, as extrude, casting film-forming, blowing, injection moulding, bottle blowing, fiberizing etc.; In addition, POLYACTIC ACID also has unique biological consistency and biological degradability, and therefore, as a kind of biodegradated polymer materal, POLYACTIC ACID has become the focus of academic boundary of polymer and industrial community concern.
The intensity of POLYACTIC ACID and rigidity are high, but toughness and shock resistance are poor, are a kind of hard and crisp material under the normal temperature.Therefore the toughening modifying to POLYACTIC ACID is its market-oriented important subject always.Toughening modifying to POLYACTIC ACID mainly contains methods such as modification by copolymerization, forming process modification and blending and modifying at present.
The modification by copolymerization method is through in the polylactic acid molecule chain, introducing other monomers; The polylactic acid molecule amylose regularity is descended; Reduce even completely lose its crystallizing power, thereby reduce second-order transition temperature, fusing point and the glutinous stream temperature of POLYACTIC ACID, realize a kind of method of the toughness reinforcing purpose of POLYACTIC ACID.POLYACTIC ACID flexible comonomer kind be can be used for improving at present and lactone, alcohols or acids etc. comprised.Polyester (for example polycaprolactone etc.) and polyethers (for example POLYACTIC ACID-W 166 segmented copolymer etc.) are more typically arranged in the multipolymer that forms.For example, Chinese invention patent Shen Qing Publication specification sheets CN101134807 discloses through introducing other aliphatic polyesters and has realized the purpose that POLYACTIC ACID is toughness reinforcing as soft segment; Chinese invention patent Shen Qing Publication specification sheets CN1865321 discloses a kind of L-POLYACTIC ACID-D-polylactic-acid block copolymer, and this copolymer of poly lactic acid has improved the resistance toheat of POLYACTIC ACID effectively; Chinese invention patent Shen Qing Publication specification sheets CN101100505 discloses and in POLYACTIC ACID, has introduced the polycarbonate segment, thereby has improved the toughness and the heat resistant type of POLYACTIC ACID effectively.Modification by copolymerization method to POLYACTIC ACID mainly is to realize through the rac-Lactide ring-opening polymerization at present, therefore has the high shortcoming of cost, is unfavorable for the large-scale industrialization exploitation.
Forming process modification method is that POLYACTIC ACID is carried out stretch orientation to improve a kind of method of performances such as its shock strength, hydrolytic resistance.Forming process modification method is widely used in the film article at present.For example Chinese invention patent Shen Qing Publication specification sheets CN101397394 discloses a kind of hydrolysis resistant flexible polylactic acid orientation products and working method thereof.
Compare with forming process modification method with the modification by copolymerization method, blending modification method is a kind of method of more economic POLYACTIC ACID toughening modifying.Blending modification method is with POLYACTIC ACID and elastomerics (for example acrylonitrile-styrene-butadienecopolymer (ABS) etc.), toughness better polymerization thing (for example polycarbonate (PC), Vilaterm (PE) etc.), filler or softening agent mixed together, thereby reaches a kind of method of the toughness reinforcing purpose of POLYACTIC ACID.Blending modification method can improve the toughness of POLYACTIC ACID effectively, still, has also on the other hand that consistency between blend components is poor, a degradation problem under undesirable, the POLYACTIC ACID degradation property of the mechanical property of system after the blend.For example Chinese invention patent Shen Qing Publication specification sheets CN1250065A discloses and in POLYACTIC ACID, has added polycarbonate, Chinese invention patent Shen Qing Publication specification sheets CN1701082 and disclose and in POLYACTIC ACID, add polyoxymethylene (POM) and realize polylactic acid modified purpose; But, exist decline of POLYACTIC ACID degradation property or degraded product simultaneously and environment produced defectives such as destruction; Chinese invention patent Shen Qing Publication specification sheets CA1475530A discloses in the POLYACTIC ACID system and to have added degradable poly butylene succinate (PBS) and can in toughness reinforcing, keep the original biodegradation character of POLYACTIC ACID; But because the consistency of POLYACTIC ACID and other polymkeric substance is relatively poor, the mechanical property of system does not reach the ideal effect after the blend.
Therefore, when taking into account factor such as cost, environment protection, improve the consistency between blend components, and then improve the focus that mechanical property has become current POLYACTIC ACID marketization research.
Summary of the invention
Technical problem to be solved by this invention is to above-mentioned prior art present situation, and a kind of full-biodegradation high-tenacity heat-resistant type polylactic resin and preparation method thereof is provided, and this polylactic resin has excellent mechanical property and resistance toheat.
The present invention will solve the problems of the technologies described above the technical scheme that is adopted: a kind of full-biodegradation high-tenacity heat-resistant type polylactic resin; Comprise polylactic resin, poly butylene succinate (PBS) and additive, additive is Di Cumyl Peroxide 99 (DCP) and SY-Monomer G (GMA); The weight-average molecular weight of polylactic resin is 8～130,000; The weight-average molecular weight of poly butylene succinate is 7～110,000; In parts by weight, the parts by weight of each component are: the summation of polylactic resin and poly butylene succinate is 100 parts, and wherein polylactic resin is 70～90 parts, and poly butylene succinate is 10～30 parts; Di Cumyl Peroxide 99: 0.1～1 part; SY-Monomer G: 1～10 part.
The preparation method of full-biodegradation high-tenacity heat-resistant type polylactic resin of the present invention is: a kind of preparation method of full-biodegradation high-tenacity heat-resistant type polylactic resin comprises the steps:
Step 1, dry premix process: with mixing after polylactic resin, poly butylene succinate, Di Cumyl Peroxide 99 and the SY-Monomer G drying;
Step 2, blend extrusion: the mixture in the step 1 is extruded through the twin screw extruder blend, and the extrusion temperature in the twin screw is 160～200 ℃, and screw speed is 20～50rpm;
Step 3, injection molding process: with the moulding in injection moulding machine of the extrudate in the step 2, injection temperature is 165～200 ℃, and injection pressure is 5～12MPa;
Step 4, annealing process: the material after the injection moulding in the step 3 is 70～100 ℃ in annealing temperature annealed 30～180 minutes down, promptly obtain full-biodegradation high-tenacity heat-resistant type polylactic resin.
For optimizing technique scheme, the measure of taking also comprises: the extrusion temperature in the above-mentioned steps 2 is 185 ℃, and screw speed is 30rpm; Injection temperature in the above-mentioned steps 3 is 180 ℃, and injection pressure is 10MPa; Annealing temperature in the above-mentioned steps 4 is 80～100 ℃, and annealing time is 60～180 minutes.
Compared with prior art, each component of full-biodegradation high-tenacity heat-resistant type polylactic resin of the present invention is full-biodegradable material; Effect through Di Cumyl Peroxide 99 and SY-Monomer G; Improved the consistency of POLYACTIC ACID and poly butylene succinate component; Make a kind of full-biodegradation high-tenacity heat-resistant type polylactic resin of the present invention have excellent mechanical property; Wherein tensile strength reaches 35～55MPa, and elongation at break reaches 8.7～146%, and shock strength reaches 12～90KJ/m
2Because the crystallization of polylactic resin self and and other components between synergistic effect, a kind of full-biodegradation high-tenacity heat-resistant type polylactic resin of the present invention has the better heat-resisting performance, its vicat softening temperature reaches 69.3～82.2 ℃.Preparing method's technical process of a kind of full-biodegradation high-tenacity heat-resistant type polylactic resin of the present invention is simple, and processing characteristics is good, and cost is low and can realize large-scale industrial production; The blend that obtains can be used for preparing film, sheet material, sheet material, foaming and injection-molded plastic product.
Embodiment
A kind of full-biodegradation high-tenacity heat-resistant type polylactic resin of the present invention comprises polylactic resin, poly butylene succinate and additive; Additive is made up of oxide compound and coupling agent; Wherein oxide compound is a Di Cumyl Peroxide 99, and coupling agent is a SY-Monomer G.The weight-average molecular weight of polylactic resin is 8～130,000; The weight-average molecular weight of poly butylene succinate is 7～110,000.In parts by weight, the parts by weight of each component are: the summation of polylactic resin and poly butylene succinate is 100 parts, and wherein polylactic resin is 70～90 parts, and poly butylene succinate is 10～30 parts; Di Cumyl Peroxide 99 is 0.1～1 part; SY-Monomer G is 1～10 part.
Embodiment 1:
Get weight-average molecular weight and be 80 parts of 130,000 polylactic resin parts by weight, weight-average molecular weight is 20 parts of 80,000 poly butylene succinate parts by weight, 0.1 part of Di Cumyl Peroxide 99 parts by weight, 1 part of SY-Monomer G parts by weight.After impeller stirred, blend was extruded in twin screw extruder with above-mentioned substance, and extrusion temperature is 185 ℃, and screw speed is 30rpm; Resin after extruding is 180 ℃ at injection temperature, and injection pressure is injection moulding under the injecting condition of 5MPa, and the 60min that under 80 ℃ annealing temperature, anneals then promptly obtains full-biodegradation high-tenacity heat-resistant type polylactic resin.
Embodiment 2:
Get weight-average molecular weight and be 80 parts of 130,000 polylactic resin parts by weight, weight-average molecular weight is 20 parts of 70,000 poly butylene succinate parts by weight, 0.2 part of Di Cumyl Peroxide 99 parts by weight, 1 part of SY-Monomer G parts by weight.After impeller stirred, blend was extruded in twin screw extruder with above-mentioned substance, and extrusion temperature is 185 ℃, and screw speed is 20rpm; Resin after extruding is 180 ℃ at injection temperature, and injection pressure is under the 10MPa after the injection moulding, and the 60min that under 80 ℃ annealing temperature, anneals promptly obtains full-biodegradation high-tenacity heat-resistant type polylactic resin.
Embodiment 3:
Get weight-average molecular weight and be 80 parts of 130,000 polylactic resin parts by weight, weight-average molecular weight is 20 parts of 80,000 poly butylene succinate parts by weight, 0.25 part of Di Cumyl Peroxide 99 parts by weight, 2.5 parts of SY-Monomer G parts by weight.After impeller stirred, blend was extruded in twin screw extruder with above-mentioned substance, and extrusion temperature is 185 ℃, and screw speed is 20rpm; Resin after extruding is 180 ℃ at injection temperature, and injection pressure is under the 10MPa after the injection moulding, and the 60min that under 80 ℃ annealing temperature, anneals promptly obtains full-biodegradation high-tenacity heat-resistant type polylactic resin.
Embodiment 4:
Get weight-average molecular weight and be 80 parts of 130,000 polylactic resin parts by weight, weight-average molecular weight is 20 parts of 80,000 poly butylene succinate parts by weight, 0.3 part of Di Cumyl Peroxide 99 parts by weight, 1 part of SY-Monomer G parts by weight.After impeller stirred, blend was extruded in twin screw extruder with above-mentioned substance, and extrusion temperature is 185 ℃, and screw speed is 30rpm; Resin after extruding is 180 ℃ at injection temperature, and injection pressure is under the 12MPa after the injection moulding, and the 60min that under 90 ℃ annealing temperature, anneals promptly obtains full-biodegradation high-tenacity heat-resistant type polylactic resin.
Embodiment 5:
Get weight-average molecular weight and be 80 parts of 80,000 polylactic resin parts by weight, weight-average molecular weight is 20 parts of 100,000 poly butylene succinate parts by weight, 0.3 part of Di Cumyl Peroxide 99 parts by weight, 1 part of SY-Monomer G parts by weight.After impeller stirred, blend was extruded in twin screw extruder with above-mentioned substance, and extrusion temperature is 200 ℃, and screw speed is 30rpm; Resin after extruding is 180 ℃ at injection temperature, and injection pressure is under the 10MPa after the injection moulding, and the 60min that under 80 ℃ annealing temperature, anneals promptly obtains full-biodegradation high-tenacity heat-resistant type polylactic resin.
Embodiment 6:
Get weight-average molecular weight and be 80 parts of 100,000 polylactic resin parts by weight, weight-average molecular weight is 20 parts of 110,000 poly butylene succinate parts by weight, 0.3 part of Di Cumyl Peroxide 99 parts by weight, 1 part of SY-Monomer G parts by weight.After impeller stirred, blend was extruded in twin screw extruder with above-mentioned substance, and extrusion temperature is 185 ℃, and screw speed is 50rpm; Resin after extruding is 180 ℃ at injection temperature, and injection pressure is under the 10MPa after the injection moulding, and the 30min that under 70 ℃ annealing temperature, anneals promptly obtains full-biodegradation high-tenacity heat-resistant type polylactic resin.
Embodiment 7:
Get weight-average molecular weight and be 70 parts of 130,000 polylactic resin parts by weight, weight-average molecular weight is 30 parts of 80,000 poly butylene succinate parts by weight, 0.3 part of Di Cumyl Peroxide 99 parts by weight, 1 part of SY-Monomer G parts by weight.After impeller stirred, blend was extruded in twin screw extruder with above-mentioned substance, and extrusion temperature is 160 ℃, and screw speed is 30rpm; Resin after extruding is 165 ℃ at injection temperature, and injection pressure is 12MPa, and the 180min that under 80 ℃ annealing temperature, anneals promptly obtains full-biodegradation high-tenacity heat-resistant type polylactic resin.
Embodiment 8:
Get weight-average molecular weight and be 70 parts of 130,000 polylactic resin parts by weight, weight-average molecular weight is 30 parts of 80,000 poly butylene succinate parts by weight, 0.2 part of Di Cumyl Peroxide 99 parts by weight, 1 part of SY-Monomer G parts by weight.After impeller stirred, blend was extruded in twin screw extruder with above-mentioned substance, and extrusion temperature is 185 ℃, and screw speed is 30rpm; Resin after extruding is 180 ℃ at injection temperature, and injection pressure is under the 10MPa after the injection moulding, and the 180min that under 100 ℃ annealing temperature, anneals promptly obtains full-biodegradation high-tenacity heat-resistant type polylactic resin.
Embodiment 9:
Get weight-average molecular weight and be 70 parts of 130,000 polylactic resin parts by weight, weight-average molecular weight is 30 parts of 110,000 poly butylene succinate parts by weight, 0.3 part of Di Cumyl Peroxide 99 parts by weight, 2 parts of SY-Monomer G parts by weight.After impeller stirred, blend was extruded in twin screw extruder with above-mentioned substance, and extrusion temperature is 185 ℃, and screw speed is 30rpm; Resin after extruding is 180 ℃ at injection temperature, and injection pressure is under the 10MPa after the injection moulding, and the 180min that under 80 ℃ annealing temperature, anneals promptly obtains full-biodegradation high-tenacity heat-resistant type polylactic resin.
Embodiment 10:
Get weight-average molecular weight and be 70 parts of 130,000 polylactic resin parts by weight, weight-average molecular weight is 30 parts of 80,000 poly butylene succinate parts by weight, 1 part of Di Cumyl Peroxide 99 parts by weight, 5 parts of SY-Monomer G parts by weight.After impeller stirred, blend was extruded in twin screw extruder with above-mentioned substance, and extrusion temperature is 185 ℃, and screw speed is 30rpm; Resin after extruding is 180 ℃ at injection temperature, and injection pressure is under the 10MPa after the injection moulding, and the 180min that under 80 ℃ annealing temperature, anneals promptly obtains full-biodegradation high-tenacity heat-resistant type polylactic resin.
Embodiment 11:
Get weight-average molecular weight and be 90 parts of 130,000 polylactic resin parts by weight, weight-average molecular weight is 10 parts of 80,000 poly butylene succinate parts by weight, 1 part of Di Cumyl Peroxide 99 parts by weight, 10 parts of SY-Monomer G parts by weight.After impeller stirred, blend was extruded in twin screw extruder with above-mentioned substance, and extrusion condition is 200 ℃, and screw speed is 30rpm; Resin after extruding is 200 ℃ at injection temperature, and injection pressure is under the 10MPa after the injection moulding, and the 180min that under 80 ℃ annealing temperature, anneals promptly obtains full-biodegradation high-tenacity heat-resistant type polylactic resin.
Embodiment 12:
Get weight-average molecular weight and be 90 parts of 130,000 polylactic resin parts by weight, weight-average molecular weight is 10 parts of 80,000 poly butylene succinate parts by weight, 0.3 part of Di Cumyl Peroxide 99 parts by weight, 1 part of SY-Monomer G parts by weight.After impeller stirred, blend was extruded in twin screw extruder with above-mentioned substance, and extrusion condition is 185 ℃, and screw speed is 30rpm; Resin after extruding is 180 ℃ at injection temperature, and injection pressure is under the 10MPa after the injection moulding, and the 180min that under 80 ℃ annealing temperature, anneals promptly obtains full-biodegradation high-tenacity heat-resistant type polylactic resin.
The full-biodegradation high-tenacity heat-resistant type polylactic resin that obtains in the foregoing description 1～12 is carried out Mechanics Performance Testing and resistance toheat test, and the Mechanics Performance Testing project comprises tensile property test and impact property test.Selected testing method and operative norm are following among the present invention: tensile property test execution GB/T 1040-2006, and rate of extension is 5mm/min; Impact property test execution GB/T 1043-1993 adopts simple beam non-notch sample impact method; Resistance toheat test execution GB/T 1633-2000, B
120Method.
The test result of embodiment 1～12 is following:
Overload
*: the Charpy shock strength surpasses 90KJ/m
2
Most preferred embodiment of the present invention is illustrated, and various variations or the remodeling made by those of ordinary skills can not depart from the scope of the present invention.
Claims (5)
1. a full-biodegradation high-tenacity heat-resistant type polylactic resin comprises polylactic resin, poly butylene succinate and additive, it is characterized in that: described additive is Di Cumyl Peroxide 99 and SY-Monomer G; The weight-average molecular weight of described polylactic resin is 8～130,000; The weight-average molecular weight of described poly butylene succinate is 7～110,000; In parts by weight, the parts by weight of each component are: the summation of polylactic resin and poly butylene succinate is 100 parts, and wherein polylactic resin is 70～90 parts, and poly butylene succinate is 10～30 parts; Di Cumyl Peroxide 99: 0.1～1 part; SY-Monomer G: 1～10 part;
The tensile strength of described full-biodegradation high-tenacity heat-resistant type polylactic resin is 35～55MPa, and elongation at break is 8.7～146%, and shock strength is 12～90KJ/m
2, vicat softening temperature is 69.3～82.2 ℃.
2. the preparation method of a kind of full-biodegradation high-tenacity heat-resistant type polylactic resin as claimed in claim 1 is characterized in that: comprise the steps:
Step 1, dry premix process: with mixing after polylactic resin, poly butylene succinate, Di Cumyl Peroxide 99 and the SY-Monomer G drying;
Step 2, blend extrusion: the mixture in the step 1 is extruded through the twin screw extruder blend, and the extrusion temperature in the twin screw is 160～200 ℃, and screw speed is 20～50rpm;
Step 3, injection molding process: with the moulding in injection moulding machine of the extrudate in the step 2, injection temperature is 165～200 ℃, and injection pressure is 5～12MPa;
Step 4, annealing process: the material after the injection moulding in the step 3 is 70～100 ℃ in annealing temperature annealed 30～180 minutes down, promptly obtain full-biodegradation high-tenacity heat-resistant type polylactic resin.
3. the preparation method of a kind of full-biodegradation high-tenacity heat-resistant type polylactic resin according to claim 2, it is characterized in that: the extrusion temperature in the described step 2 is 185 ℃, and screw speed is 30rpm.
4. the preparation method of a kind of full-biodegradation high-tenacity heat-resistant type polylactic resin according to claim 2, it is characterized in that: the injection temperature in the described step 3 is 180 ℃, and injection pressure is 10MPa.
5. according to the preparation method of the described a kind of full-biodegradation high-tenacity heat-resistant type polylactic resin of the arbitrary claim of claim 2 to 4, it is characterized in that: the annealing temperature in the described step 4 is 80～100 ℃, and annealing time is 60～180 minutes.
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| CN102295825A (en) * | 2011-07-08 | 2011-12-28 | 金发科技股份有限公司 | Biodegradable composition and preparation method thereof |
| SE538364C2 (en) | 2014-01-24 | 2016-05-31 | Stora Enso Oyj | Use of polylactide and process for making a heat-sealed container or packaging of paper or cardboard |
| SE538363C2 (en) | 2014-01-24 | 2016-05-31 | Stora Enso Oyj | Process for improving heat sealability of polyester, and for making a heat-sealed container or package |
| CN105860457A (en) * | 2016-05-11 | 2016-08-17 | 上海馨星环保科技有限公司 | Novel polylactic film |
| CN109666271B (en) * | 2018-12-11 | 2020-11-24 | 中国科学院理化技术研究所 | Micro-foaming degradable mulching film and preparation method thereof |
| CN110341271A (en) * | 2019-07-12 | 2019-10-18 | 青岛周氏塑料包装有限公司 | A kind of high strength Fully-biodegradable composite membrane and its production technology and application |
| CN112406150B (en) * | 2020-11-06 | 2023-07-18 | 贵州黔峰实业有限公司 | Preparation and production process of nano modified high-density polyethylene alloy pipe |
| CN113265129B (en) * | 2020-11-26 | 2022-10-11 | 汕头市三马塑胶制品有限公司 | Foaming-grade polylactic acid with excellent processing fluidity and preparation method thereof |
| CN112694703A (en) * | 2020-12-24 | 2021-04-23 | 无锡殷达尼龙有限公司 | Toughened polylactic acid blend and preparation method thereof |
| CN113321909A (en) * | 2021-05-28 | 2021-08-31 | 山西省化工研究所（有限公司） | Heat-resistant polylactic acid composition and preparation method thereof |
| CN114957937B (en) * | 2021-11-01 | 2023-10-20 | 深圳市联辉科技创新有限公司 | One-step injection molding high polymer material |
| CN114085483B (en) * | 2021-11-26 | 2022-09-02 | 安徽江南医疗器械股份有限公司 | Preparation method of completely biodegradable disposable infusion hose |
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| CN1400092A (en) * | 2001-08-01 | 2003-03-05 | 富士胶片株式会社 | Manufacture of resin forming part |
| CN1793227A (en) * | 2005-12-28 | 2006-06-28 | 中国科学院长春应用化学研究所 | Process for preparing thermal resistant easy processed polylactic resin |
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| CN1400092A (en) * | 2001-08-01 | 2003-03-05 | 富士胶片株式会社 | Manufacture of resin forming part |
| CN1793227A (en) * | 2005-12-28 | 2006-06-28 | 中国科学院长春应用化学研究所 | Process for preparing thermal resistant easy processed polylactic resin |
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