CN101195273A - Method for improving polyglycol plasticization polylactic acid strength of materials capability by process - Google Patents
Method for improving polyglycol plasticization polylactic acid strength of materials capability by process Download PDFInfo
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- CN101195273A CN101195273A CNA2007101708741A CN200710170874A CN101195273A CN 101195273 A CN101195273 A CN 101195273A CN A2007101708741 A CNA2007101708741 A CN A2007101708741A CN 200710170874 A CN200710170874 A CN 200710170874A CN 101195273 A CN101195273 A CN 101195273A
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Abstract
The invention relates a press-working and solid forming method for improving the mechanical properties of polylactic acid (PLA) material plasticized with polyethylene glycol (PEG). The steps include: (1) preparation of PLA spline plasticized with PEG; (2) press-working and solid forming of the PLA spline plasticized with PEG; (3) heat treatment after the forming. The impacting property of PLA plactics plasticized with PEG can be increased by dozens of times, the stretching property can be increased by two times, solid motion of samples occurs by employing the method to give force on the samples, and in the process of solid motion, the internal microstructure of the material is improved, thereby achieving the purpose of improving the mechanical properties.
Description
Technical field
The invention belongs to the PLA field, particularly relate to the method that the pressure processing formed solid improves polyethylene glycol plasticized poly lactic acid mechanical property.
Background technology
PLA is as biodegradable macromolecular material, owing to degradable, the friendly performance of reproducible biology have obtained a large amount of research.But, can only limit as packaging material widely and use because the crystalline rate of PLA own is slow, the strand rigidity has caused toughness of material poor by force.Generally can make impact property improve by the method for plasticising, blending and modifying.But in the time of modification, tensile property descends and has acutely limited the use of material.The method of Recent study blending toughening is a lot, and a large amount of toughness reinforcing models occurred.
For the application of various high polymer materials, toughness is an extremely important mechanical performance index, and the toughening modifying of polymer is the major issue in the material modification always.Since the technical patent appearance of first toughness reinforcing PS of nineteen twenty-seven, the ABS plastic that utilizes rubber toughened technological development to go out to first, the application of macromolecular material is constantly expanded.And along with 70, toughness reinforcing high-impact investigation of materials and the research of inorganic rigid particle toughened system in recent years of the various rigidity organic fillers eighties, various toughening mechanism propose in succession.
Injection mo(u)lding is the processing method of extensive use, in recent years the injection mo(u)lding Study on Self-reinforcement is emerged in an endless stream.(Bayer R K such as BayerR K, et al.Polymer Engineering and Science 1989,29,186) reported the elongational flow injection moulding method, on common injection machine, realize poly self-reinforcing, made the sample that hot strength reaches 150MPa.In addition, roll-forming also is a kind of effectively processing method.(D.C.Sun such as D.C.Sun, E.M.Berg, J.H.Magill.Polym.Eng.Sci., 1990,30,635) reported the roll-forming of polypropylene, high density polyethylene (HDPE), Kynoar and polyethylene-polypropylene block copolymer, found that the mechanical strength of the sample behind all roll-formings all has raising on three axial directions, and disclosed the relation of structure and performance.But the toughening effect of material work in-process and mechanism are also seldom.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of pressure processing formed solid to improve the method for polyethylene glycol (PEG) plasticized poly lactic acid (PLA) material mechanical performance, mix PEG, PLA at first by a certain percentage, by the double screw extruder granulation, use injection machine to obtain the PLA batten of the PEG plasticising of certain size at last then.The batten of suitable dimension is put in the homemade mould under different pressures, temperature and time effect, and sandwich structure appears in macromolecule.And by heat treatment elimination material internal stress, the structure of formation has improved the mechanical property of material.
Under pressure, carry out the pressure processing formed solid by polymer, thereby form sandwich structure, reach toughness reinforcing purpose at material internal.
Pressure processing formed solid of the present invention improves the method for PEG plasticising PLA material mechanical performance, comprises the following steps:
(1) the PLA batten of PEG plasticising preparation
The PEG and the PLA of preliminary blend are carried out the blend extruding pelletization by double screw extruder, and injection mo(u)lding prepares the PLA batten of PEG plasticising (80mm * 10mm * 4mm), injection temperature is 150 ℃～200 ℃, and injection pressure is 60bar～160bar then;
(2) the pressure processing formed solid of the PLA batten of PEG plasticising
The injection moulding batten is processed into certain shape, as be cut into rectangular shape (35mm * 10mm * 4mm), the crystallization different time, put into homemade mould (the mould internal cavity is the cuboid of 80mm * 10mm * 4mm) then, under 0～170 ℃ temperature conditions, pressure limit is 0MPa～900MPa, compacting 0-150min, the pressure processing formed solid of the PLA batten of realization PEG plasticising;
(3) heat treatment after the moulding
The PLA batten of the PEG plasticising after the moulding is put into thermostatic equipment, be set in 50 ℃～160 ℃ and heat-treat, the time is 1min～120min, to improve the anti-impact structure of material internal.
Polyethylene glycol (PEG) molecular weight in the described step (1) is 200～20,000, and the intrinsic viscosity of PLA (PLA) is 1.08736dL/g, and fusing point is 168 ℃;
Preferred 160～180 ℃ of injection temperature in the described step (1), the preferred 80～120bar of injection pressure.
Preferred 50～150 ℃ of temperature in the described step (2), the preferred 200MP～800Mpa of pressure, 100-800Mpa most preferably, preferred 5～20min of press time;
Flow direction and compression ratio in the described step (2) can be controlled;
Preferred 60 ℃～120 ℃ of temperature in the described step (3), preferred 1～20min of time.
Beneficial effect of the present invention:
The technology of the present invention by a kind of pressure processing formed solid formed high-impact and got sandwich structure in the PLA of PEG plasticising batten, this structure not only several times has improved the bending property of material, tensile property has improved twice, and tens times raising the impact strength of material.This method processing temperature has reduced the palliating degradation degree of material near Tg, improved the apparent property of goods, has promoted the combination property of the PLA of PEG plasticising comprehensively.This method can be processed by methods such as mold pressing, punching press or continous ways on vulcanizer, forcing press equal pressure equipment.
This method makes sample solid-state flowing occur by sample is exerted pressure, the internal microstructure of material improves in solid-state flowing, thereby has reached the purpose of improving mechanical property.
Description of drawings
Fig. 1 is the form of PLA batten of PEG plasticising of injection moulding preparation and the form after the processing;
Fig. 2 is a pressure processing formed solid schematic diagram;
Fig. 3 is the impact section of the PLA batten of undressed PEG plasticising;
Fig. 4 be the PLA batten of PEG plasticising behind crystallization 2.5min at 70 ℃ of pressurized 250MPa, the sandwich structure in the impact section of the material of time 10min.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
The form of the PLA batten of the PEG plasticising of injection moulding preparation and the form (as Fig. 1) after the processing and self-control Mould Machining process schematic diagram (as Fig. 2), the impact section (as Fig. 3) of the PLA batten of undressed PEG plasticising.
Embodiment 2
Press embodiment 1 described method, at 70 ℃, the pressure condition of 250MPa kept 5 minutes down with the PLA batten of the PEG plasticising of 80 ℃ of different crystallization times, and the mechanical property without the heat treatment batten after the moulding sees Table 1.
After the moulding under the table 180 ℃ different crystallization times without the mechanical property of heat treatment batten
| The crystallization time that batten is 80 ℃ (min) | Impact strength (the kJ/m of original batten 2) | Impact strength (the kJ/m of processing back batten 2) |
| 2.5 5 7 10 14 | 1.24 1.37 1.52 1.77 1.3 | 43.29 37.74 33.29 21.13 14.89 |
Embodiment 3
Press embodiment 1 described method, under condition of different temperatures, 250MPa kept 5 minutes down with the PLA batten of the PEG plasticising of crystallization 2.5min, and the mechanical property without the heat treatment batten after the moulding sees Table 2.
Behind the different processing temperature compacted unders of table 2 without the mechanical property of heat treatment batten
| The processing temperature of batten (℃) | Impact strength (the kJ/m of batten 2) |
| 30 50 70 90 110 | 3.56791 5.67307 29.23382 16.49121 7.74971 |
Embodiment 4
Press embodiment 1 described method, at 70 ℃, the 250MPa pressure condition keeps different time (impact section such as Fig. 4 of the material of pressurized time 10min) down with the PLA batten of the PEG plasticising of crystallization 2.5min, and the mechanical property without the heat treatment batten after the moulding sees Table 3.
Behind table 3 different process time of the compacted under without the mechanical property of heat treatment batten
| The process time of batten (min) | Impact strength (the kJ/m of batten 2) |
| 0 1 3 5 7 15 | 1.48619 8.99106 15.44667 34.48375 29.93279 30.67779 |
Embodiment 5
Press embodiment 1 described method, the PLA batten of the PEG plasticising of crystallization 2.5min at 70 ℃, is kept 5min under the different pressures condition, the mechanical property without the heat treatment batten after the moulding sees Table 4.
Behind the different tonnage compacted unders of table 4 without the mechanical property of heat treatment batten
| The tonnage of batten (MPa) | Impact strength (the kJ/m of batten 2) |
| 0 50 150 300 500 600 | 1.49 2.83 8.45 29.89 30.29 30.4 |
Embodiment 6
Press embodiment 1 described method, the PLA batten of the PEG plasticising of crystallization 2.5min at 70 ℃, is implemented 5min under the different pressures condition, the mechanical property at the batten of 80 ℃ of heat treatment different times after the moulding sees Table 4.
The mechanical property of batten under the table 4 different heat treatment time
| The heat treatment time of batten (min) | Impact strength (the kJ/m of batten 2) |
| 1 2.5 5 7 10 15 | 23.82 24.71 29.9 39.21 51.53 50.78 |
Claims (9)
1. the pressure processing formed solid improves the method for polyethylene glycol PEG plasticized poly lactic acid PLA material mechanical performance, comprises the following steps:
(1) the PLA batten of PEG plasticising preparation
The PEG and the PLA of preliminary blend are carried out the blend extruding pelletization by double screw extruder, and injection mo(u)lding prepares the PLA batten of PEG plasticising then, and injection temperature is 150 ℃～200 ℃, and injection pressure is 60bar～160bar;
(2) the pressure processing formed solid of the PLA batten of PEG plasticising
The injection moulding batten is sheared shaping, and the crystallization different time is put into mould then, and under 0～170 ℃ temperature conditions, pressure limit is 0MPa～900MPa, compacting 0～150min, the pressure processing formed solid of the PLA batten of realization PEG plasticising;
(3) heat treatment after the moulding
The PLA batten of the PEG plasticising after the moulding is put into thermostatic equipment, heat-treat 1min～120min, improve the anti-impact structure of material internal at 50 ℃～160 ℃.
2. method according to claim 1 is characterized in that: the polyethylene glycol PEG molecular weight in the described step (1) is 200～20,000, and the intrinsic viscosity of polylactic acid PLA is 1.08736dL/g, and fusing point is 168 ℃.
3. method according to claim 1 is characterized in that: the injection temperature in the described step (1) is 160～180 ℃, and injection pressure is 80～120bar.
4. method according to claim 1 is characterized in that: the temperature in the described step (2) is 50～150 ℃, and pressure is 200MP～800Mpa, and the press time is 5～20min.
5. method according to claim 4 is characterized in that: the pressure in the described step (2) is 100-800Mpa.
6. method according to claim 1 is characterized in that: flow direction and compression ratio in the described step (2) can be controlled.
7. method according to claim 1 is characterized in that: the treatment temperature in the described step (3) is 60 ℃～120 ℃, and the time is 1～20min.
8. method according to claim 1 is characterized in that: the internal cavity of mould is the cuboid of 80mm * 10mm * 4mm in the described step (2).
9. method according to claim 1 is characterized in that: injection moulding batten shearing shaping is that PLA batten 80mm * 10mm * 4mm cuts into rectangular shape 35mm * 10mm * 4mm in the described step (2).
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2007101708741A CN101195273A (en) | 2007-11-23 | 2007-11-23 | Method for improving polyglycol plasticization polylactic acid strength of materials capability by process |
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| CNA2007101708741A CN101195273A (en) | 2007-11-23 | 2007-11-23 | Method for improving polyglycol plasticization polylactic acid strength of materials capability by process |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100183834A1 (en) * | 2007-08-14 | 2010-07-22 | Huhtamaki Forchheim, Zweigniederlassung Der Huhtamaki Deutschland Gmbh & Co. Kg | Film arrangement |
| CN102069590A (en) * | 2009-11-25 | 2011-05-25 | 中原工学院 | Method for toughening and enhancing crystalline polypropylene |
| CN102189618A (en) * | 2010-03-16 | 2011-09-21 | 中原工学院 | Method for increasing mechanical property of PA66 by forced solid flow |
| CN102941640A (en) * | 2012-10-09 | 2013-02-27 | 四川大学 | High pressure forming method for increasing crystallinity of polylactic acid |
| CN105269738A (en) * | 2014-06-27 | 2016-01-27 | 中山市益建兴塑胶制品有限公司 | Method for producing plastic box |
| CN105885374A (en) * | 2016-06-29 | 2016-08-24 | 郑州大学 | High-toughness polylactic acid based composite material and preparation method thereof |
| CN107756736A (en) * | 2017-11-15 | 2018-03-06 | 成都美益达医疗科技有限公司 | A kind of crystalline material injection self-reinforcing process and equipment |
-
2007
- 2007-11-23 CN CNA2007101708741A patent/CN101195273A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100183834A1 (en) * | 2007-08-14 | 2010-07-22 | Huhtamaki Forchheim, Zweigniederlassung Der Huhtamaki Deutschland Gmbh & Co. Kg | Film arrangement |
| US8846202B2 (en) * | 2007-08-14 | 2014-09-30 | Huhtamaki Films Germany Gmbh & Co. Kg | Film arrangement |
| CN102069590A (en) * | 2009-11-25 | 2011-05-25 | 中原工学院 | Method for toughening and enhancing crystalline polypropylene |
| CN102189618A (en) * | 2010-03-16 | 2011-09-21 | 中原工学院 | Method for increasing mechanical property of PA66 by forced solid flow |
| CN102941640A (en) * | 2012-10-09 | 2013-02-27 | 四川大学 | High pressure forming method for increasing crystallinity of polylactic acid |
| CN105269738A (en) * | 2014-06-27 | 2016-01-27 | 中山市益建兴塑胶制品有限公司 | Method for producing plastic box |
| CN105885374A (en) * | 2016-06-29 | 2016-08-24 | 郑州大学 | High-toughness polylactic acid based composite material and preparation method thereof |
| CN107756736A (en) * | 2017-11-15 | 2018-03-06 | 成都美益达医疗科技有限公司 | A kind of crystalline material injection self-reinforcing process and equipment |
| CN107756736B (en) * | 2017-11-15 | 2023-08-22 | 成都美益达医疗科技有限公司 | Self-reinforcing process and equipment for injection molding of crystalline material |
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Open date: 20080611 |