CN102464873A - Bidirectional stretching polylactic acid / montmorillonoid, and preparation method and application thereof - Google Patents
Bidirectional stretching polylactic acid / montmorillonoid, and preparation method and application thereof Download PDFInfo
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- CN102464873A CN102464873A CN2010105330495A CN201010533049A CN102464873A CN 102464873 A CN102464873 A CN 102464873A CN 2010105330495 A CN2010105330495 A CN 2010105330495A CN 201010533049 A CN201010533049 A CN 201010533049A CN 102464873 A CN102464873 A CN 102464873A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
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Abstract
The invention provides a bidirectional stretching polylactic acid / montmorillonoid, and a preparation method and application thereof. The invention composite membrane of the invention comprises a mixture of 100 weight parts of polylactic acid and 1-10 weight parts of montmorillonoid, is prepared by a bidirectional stretching method and has a thickness of 10-100 mum. The composite membrane of the invention has low preparation cost, excellent barrier property and good biodegradability, and can be applied to the filed of package having high demand on oxygen permeability.
Description
Technical field
The present invention relates to a kind of poly (lactic acid) composition, more specifically, the present invention relates to a kind of biodegradable polylactic acid membrane.
Background technology
Along with the raising of industrialization degree, the consumption of plastics film is increasing, is raw-material Vilaterm with oil and gas, and Vestolen PP 7052 is the main raw material of plastics film, and these materials are discarded in the nature and can not degrade, and can produce serious " white pollution ".And along with the worsening shortages of petroleum resources, oil price rises steadily, and the raw-material cost of this type also rises steadily.
In order to solve this a series of problems, a kind ofly utilize the POLYACTIC ACID that biotechnology makes (polylactic acid, PLA) plant plastics arises at the historic moment.POLYACTIC ACID is to be basic raw material, to make through the ring-opening polymerization of polycondensation or its lactide dimer with the lactic acid that corn or potato starch make through fermentation, and is at biodegradable generation carbonic acid gas of occurring in nature and water, environmentally friendly.Thereby be widely used in fields such as wrapping material, plastic sheeting for farm use, bio-medical material.But,, only be applicable to the food that packing is less demanding to barrier, shelf-life is relatively short because POLYACTIC ACID is higher to the transmitance of oxygen in the food product pack field.
Add polynite POLYACTIC ACID is carried out the effective means that modification is a raising POLYACTIC ACID barrier property.Being dispersed in montmorillonite layer in the POLYACTIC ACID matrix has increased the path of gaseous diffusion, and the POLYACTIC ACID gas barrier property is improved.According to Chang (Polym Sci Part B:Polym Phys, 2003,41 (1): 94-103.) and Tellen (Polymer; 2005,46 (25): 11715-11727.) people's such as grade research, the method for employing pressed film method and solution film forming; The poly-lactic acid/montmorillonite composite package of preparation polynite content 1～6wt%; The purer POLYACTIC ACID of the transmission rates of oxygen in matrix material reduces by 15～30%, and under the polynite addition of 10wt%, transmission rates can reduce about 50%.The present invention has used the film forming method of two-way stretch, be more suitable for large-scale industrial production, and barriering effect is better.
Summary of the invention
Defective to prior art exists the invention provides a kind of biaxially stretched polylactic acid/montmorillonite Composite film.Two-way stretch composite package of the present invention, preparation cost is cheap, have excellent barrier property, and its biodegradable is good, can be applied to oxygen-permeable is required than higher packaging field.
One of the object of the invention is biaxially stretched polylactic acid/Nano composite material of montmorillonite film (BOPLA film) of providing a kind of barrier property good.
Described composite package includes following component: POLYACTIC ACID, polynite, in POLYACTIC ACID by 100 weight parts, polynite 1～10 weight part, preferred 3～5 weight parts.Composite package is through the preparation of two-way stretch method, and thickness is 10～100 μ m.
Wherein, the POLYACTIC ACID as composite package main body of the present invention is selected from oneself disclosed polylactic resin in the prior art.
Polynite described in the two-way stretch composite package of the present invention is selected from least a in inorganic polynite of the prior art and the organic modification montmonrillonite.
Described organic modification montmonrillonite is that inorganic polynite obtains after organic intercalation agent is handled modification.Can select various organic modification montmonrillonite of the prior art for use.Preferred said organic intercalation agent is selected from least one type in following two types: the first kind is the quaternary ammonium salt of C6～C24, the quaternary ammonium salt of preferred C6～C18; More preferred examples of compounds comprises at least a in the following material: octadecyl trimethylammonium bromide, OTAC, cetyl trimethylammonium bromide, palmityl trimethyl ammonium chloride, double hexadecyl ammonium salt, two octadecyl ammonium salt, DTAC, dodecylbenzyl alkyl dimethyl ammonium chloride, ammonium lauryl sulfate; Wherein, preferred octadecyl trimethylammonium bromide.Second type is selected from the special intercalator that an end that is not connected with polynite behind the intercalation has polar group, and described polar group comprises amino, hydroxyl, carboxyl; More concrete examples of compounds comprises: hexanolactam, hexanediamine, decamethylene diamine etc.
Said inorganic polynite and organic modification montmonrillonite can pass through commercially available getting; Wherein organic modification montmonrillonite can also obtain through self-control.The preferred powder size of described polynite is 170～230 orders, average lamellar spacing 1～10nm, interlamellar spacing 1.5～4nm.Among the present invention, the adding of this kind polynite can improve the tensile property of POLYACTIC ACID, and the stable pulling multiplying power can be increased to 1.5 times.
In order to increase the consistency of each component in the composite package; Also comprise compatilizer in the poly-lactic acid/montmorillonite composite package of the present invention, described compatilizer can be selected at least a in polycaprolactone (PCL), polyhydroxyalkanoate (PHA), polyoxyethylene glycol (PEG), the epoxy resin for use.Adopt polyoxyethylene glycol compatilizers such as (PEG), can improve barrier property with the matrix material of inorganic polynite of equal size and organo montmorillonite; Adopt not with the barrier property of the polynite of terminal polar group intercalator and POLYACTIC ACID compound film quite with the polynite of amino end group treatment agent, on performance and cost, arrived balance with POLYACTIC ACID compound film with employing.In POLYACTIC ACID by 100 weight parts, compatilizer 0～5 weight part, preferred 2～4 weight parts.
In addition; In the course of processing of poly-lactic acid/montmorillonite composite package; The needs of the concrete processing of available basis add processing aid commonly used in the polylactic resin modification technology, for example: oxidation inhibitor, softening agent, toughener, fire retardant, static inhibitor, dispersion agent, nucleator, weighting agent, pigment etc. in the blend material; Its consumption is conventional amount used, or adjusts according to practical requirements.
Two of the object of the invention is to provide the preparation method of this kind biaxially stretched polylactic acid/montmorillonite Composite film, said method comprising the steps of:
Comprise that the each component that will include said POLYACTIC ACID, polynite mixes by said content, melt blending carries out two-way stretch again after curtain coating, make described biaxially stretched polylactic acid/montmorillonite Composite film.
In the course of processing of polylactic acid resin composition of the present invention; Material melt blending temperature is used blending temperature in the common polylactic resin processing; Should select not only guaranteeing the complete fusion of matrix resin but also can not make in the scope of its decomposition, be generally 155 ℃～200 ℃.In addition, according to the processing needs, can in the blend material, add some auxiliary agents commonly used in the polylactic resin course of processing such as compatilizer, dispersion agent, surface treatment agent etc. in right amount, its consumption is conventional amount used, or adjusts according to practical requirements.
More concrete, its step of preparation method of the present invention normally mixes all components earlier, carries out melt blending, curtain coating and two-way stretch then, and more concrete preparation process is following:
(1) with POLYACTIC ACID, polynite in vacuum drying oven 80 ℃, dry 8 hours, add or do not add compatilizer, put in the twin screw extruder 155～200 ℃ of processing temperatures, screw speed 50～400rpm.
(2), dry 10 hours, put into the casting machine curtain coating with prepared composite material pellet in vacuum drying oven 80 ℃.160～195 ℃ of curtain coating temperature, curtain coating screw speed 6～20rpm.
(3) two-way stretch is carried out in the sheet material cut-parts that curtain coating gone out on biaxial orientation stretching machine, the cross directional stretch multiplying power is 3～7 times, and longitudinal tensile strength is 3～7 times, and film thickness is 15～40 μ m.
In the preparation method of the invention described above, the mixing equipment of mixing of materials can adopt various mixing equipments used in the prior art, like stirrer, kneading machine etc.Employed melt blending equipment is the general blending equipment in the rubber and plastic processing industry, can be twin screw extruder, single screw extrusion machine, mill or Banbury mixer etc.Employed casting apparatus can adopt in the prior art general various casting apparatus, like casting machine etc.Employed stretcher is general various stretchers, as: biaxial orientation stretching machine etc.
Three of the object of the invention is to provide the application of this kind biaxially stretched polylactic acid/montmorillonite Composite film.
Composite package of the present invention is used for the wrapping material field of high obstructing performance; As: food fresh-keeping film, medical packaging film, electronic product packing film etc.
Through experiment showed, that the adding polynite is carried out modification to POLYACTIC ACID is an effective means that improves the POLYACTIC ACID barrier property, thus the excellent property of the BOPLA film of poly-lactic acid/montmorillonite Composite Preparation of the present invention.Being dispersed in montmorillonite layer in the POLYACTIC ACID matrix has increased the path of gaseous diffusion, and the POLYACTIC ACID gas barrier property is improved.According to method provided by the invention, add the 3wt% polynite, the purer POLYACTIC ACID of the rate of permeation of oxygen in matrix material reduces about 50%, and when addition is increased to 10wt%, oxygen permeability can reduce nearly about 70%.
The biaxially oriented film complete processing is that macromolecule melt is at first processed sheet material or thick film through long and narrow head; Then in the drawing machine of special use; Under the speed of certain temperature and setting; Simultaneously or the stretching on vertical both direction (vertically, laterally), carried out of substep, and the film of processing through suitable cooling or thermal treatment or special processing (like corona, coating etc.).This film is because the orientation effect of molecular chain is being superior to non-oriented film aspect the transparency and the mechanical property.It is that the biaxial stretching film BOPLA of raw material preparing not only can have good barrier that good degradation property and tensility can also be arranged that the present invention adopts poly-lactic acid/montmorillonite.The film forming method of two-way stretch of the present invention is more suitable for large-scale industrial production, and the barriering effect of product is better.
Embodiment
Below in conjunction with specific embodiment the present invention is further specified.But the present invention is not limited in following embodiment.
Testing method: according to ASTM E 96, adopt MOCON oxygen flow appearance that film is carried out the oxygen-permeable test: oxygen purity is 99.9%, and carrier gas is N
2/ H
2Mixed gas (H
2Content 1.0%), 23 ℃ of probe temperatures, relative humidity is 0.
Raw material:
POLYACTIC ACID (PLA): the positive biomaterial limited-liability company in sea, REVODE201, (190 ℃/2.16Kg) 10～30g/10min of MFR;
Inorganic polynite: fill level, Zhejiang Feng Hong clay chemical industry ltd;
Organic modification montmonrillonite A:DK1, octadecyl trimethylammonium bromide are the intercalator modification, Zhejiang Feng Hong clay chemical industry ltd;
Organic modification montmonrillonite B:DK5, hexanolactam is the intercalator modification, contains the polar group of amino end group, Zhejiang Feng Hong clay chemical industry ltd;
Polyoxyethylene glycol (PEG): molecular weight 6000, Japanese import packing.
Embodiment 1
With 100 parts of POLYACTIC ACIDs, add 3 parts of inorganic polynites, in vacuum drying oven, after dry 8 hours and 1.5 parts of polyoxyethylene glycol (PEG) put into high-speed stirring together and stirred 2 minutes.Put into the forcing machine granulation, each section temperature is set at 180-190-190-190-190-195 ℃ from the barrel to the head, and screw speed is 350rpm.After the granulation pellet was put into 80 ℃ of dryings of vacuum drying oven 10 hours.Adopt the casting machine curtain coating, the temperature of each section of casting machine barrel from the hopper to the head is followed successively by 175-170-170-180-180 ℃, and screw speed is 8.5rpm.With the sheet material that curtain coating obtains, be cut into the square sheet of 9.3 * 9.3cm, the preparation BOPLA film that in biaxial orientation stretching machine, stretches, 75 ℃ of stretching furnace furnace temperature are carried out longitudinal stretching earlier, stretching ratio 3.5.Carry out cross directional stretch then, stretching ratio 4.Its oxygen-permeable test result is seen table 1.
Embodiment 2
Other conditions are with embodiment 1, but replace inorganic polynite with 3 parts of organic modification montmonrillonite A.Its oxygen-permeable test result is seen table 1.
Embodiment 3
Other conditions are with embodiment 1, but replace inorganic polynite with 3 parts of organic modification montmonrillonite B, do not add compatilizer.Its oxygen-permeable test result is seen table 1.
Embodiment 4
Other conditions are with embodiment 3, but organic modification montmonrillonite B content is reduced to 1 part.Its oxygen-permeable test result is seen table 1.
Embodiment 5
Other conditions are with embodiment 3, but organic modification montmonrillonite B content is increased to 5 parts.Its oxygen-permeable test result is seen table 1.
Embodiment 6
Other conditions are with embodiment 3, but organic modification montmonrillonite B content is increased to 10 parts.Its oxygen-permeable test result is seen table 1.
Embodiment 7
Other conditions are with embodiment 1, but the compatilizer addition is brought up to 3 parts.Its oxygen-permeable test result is seen table 1.
Embodiment 8
Other conditions are with embodiment 6, but horizontal and vertical stretching ratio is all brought up to 7 times.Investigate the tensility ability of this PLA film.
Comparative Examples 1
Pure PLA pellet was put into 80 ℃ of dryings of vacuum drying oven 10 hours.Adopt the casting machine curtain coating, the temperature of each section of casting machine barrel from the hopper to the head is followed successively by 175-170-170-180-180 ℃, and screw speed is 8.5rpm.With the sheet material that curtain coating obtains, be cut into the square sheet of 9.3 * 9.3cm, the preparation BOPLA that in biaxial orientation stretching machine, stretches, 75 ℃ of stretching furnace furnace temperature are carried out longitudinal stretching earlier, stretching ratio 3.5.Carry out cross directional stretch then, stretching ratio 4.Its oxygen-permeable test result is seen table 1.
Comparative Examples 2
With 100 parts of POLYACTIC ACIDs, add 10 parts of organo montmorillonite B, after dry 8 hours and through granulation in the forcing machine, each section temperature is set at 180-190-190-190-190-195 ℃ from the barrel to the head in vacuum drying oven, and screw speed is 350rpm.After the granulation pellet was put into 80 ℃ of dryings of vacuum drying oven 10 hours.Preheating 12min under 150 ℃ of temperature adds 3MPa pressure compacting 1min, 25 ℃ of pressurization cooling 10min.Its oxygen-permeable test result is seen table 1.
Comparative Examples 3
Other conditions are with Comparative Examples 1, but laterally the longitudinal stretching multiplying power all is increased to 4.5 times.Investigate the tensility ability of this PLA film.
The oxygen transmission rate of table 1 BOPLA film
Comparison through Comparative Examples 2 and embodiment; Can find out, add the barrier that polynite can significantly improve POLYACTIC ACID, even the same in the polynite kind; Under the identical situation of addition, the barrier through two-way stretch method prepared composite film obviously is better than compression molding.Being equipped with polynite content through the two-way stretch legal system is that the barrier property of 3wt% composite package is superior to compression molding and prepares the composite package that polynite content is 10wt%.
Can find out the contribution that the barrier property of composite package is improved: polarity organo montmorillonite＞nonpolar polynite＞inorganic polynite through embodiment 1～3.Comparative example 3～6 can find out that along with the increase of polynite content, the barrier of composite package improves gradually.
In investigating the tensility ability process of film, according to embodiment 8 said technologies, no rupture of membranes phenomenon in the course of processing; And Comparative Examples 3 said technologies, polylactic acid membrane can be pulled open, and explains that the adding of polynite can improve the tensile property of polylactic acid membrane, and its stretching ratio improves 1.5 times.
Claims (10)
1. biaxially stretched polylactic acid/montmorillonite Composite film includes following component: POLYACTIC ACID, polynite; In POLYACTIC ACID by 100 weight parts, polynite 1～10 weight part; Described composite package is through the preparation of two-way stretch method, and thickness is 10～100 μ m.
2. poly-lactic acid/montmorillonite composite package according to claim 1 is characterized in that including following component:
In POLYACTIC ACID by 100 weight parts, polynite 1～10 weight part.
3. poly-lactic acid/montmorillonite composite package according to claim 1 is characterized in that:
Described polynite is selected from least a in inorganic polynite and the organic modification montmonrillonite; Its powder size is 170～230 orders, average lamellar spacing 1～10nm, interlamellar spacing 1.5～4nm.
4. like the said poly-lactic acid/montmorillonite composite package of claim 3, it is characterized in that:
The intercalator of described organic modification montmonrillonite is selected from the quaternary ammonium salt of C6～C24, or is selected from the special intercalator that an end that is not connected with polynite behind the intercalation has polar group.
5. like the said poly-lactic acid/montmorillonite composite package of claim 4, it is characterized in that:
In the described intercalator, the quaternary ammonium salt of C6～C24 is selected from least a in octadecyl trimethylammonium bromide, OTAC, cetyl trimethylammonium bromide, palmityl trimethyl ammonium chloride, double hexadecyl ammonium salt, two octadecyl ammonium salt, DTAC, dodecylbenzyl alkyl dimethyl ammonium chloride, the ammonium lauryl sulfate.
6. like the said poly-lactic acid/montmorillonite composite package of claim 5, it is characterized in that,
The quaternary ammonium salt of described C6～C24 is the octadecyl trimethylammonium bromide.
7. like the said poly-lactic acid/montmorillonite composite package of claim 4, it is characterized in that,
In the described intercalator, the special intercalator lactan of selecting oneself, hexanediamine, at least a in the decamethylene diamine; Said polar group is selected from amino, hydroxyl or carboxyl.
8. poly-lactic acid/montmorillonite composite package according to claim 1 is characterized in that:
Comprise compatilizer; In POLYACTIC ACID by 100 weight parts, compatilizer 0～5 weight part;
Described compatilizer is selected from least a in polycaprolactone, polyhydroxyalkanoate, polyoxyethylene glycol, the epoxy resin.
9. like the preparation method of the arbitrary described biaxially stretched polylactic acid/montmorillonite Composite film of claim 1～8, it is characterized in that:
Comprise that the each component that will include said POLYACTIC ACID, polynite mixes by said content, melt blending, again through curtain coating after the two-way stretch method makes described biaxially stretched polylactic acid/montmorillonite Composite film.
10. like the application on the wrapping material of high obstructing performance of the arbitrary described a kind of biaxially stretched polylactic acid/montmorillonite Composite film of claim 1～8.
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Cited By (7)
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| CN105419262A (en) * | 2014-09-02 | 2016-03-23 | 允友成(宿迁)复合新材料有限公司 | Polylactic acid/montmorillonite nanometer composite material preparation method |
| CN106495175A (en) * | 2016-12-23 | 2017-03-15 | 仲恺农业工程学院 | A kind of preparation method of organic modification montmonrillonite |
| CN109929228A (en) * | 2019-04-17 | 2019-06-25 | 谷水英 | Green biodegradable plastics film and its processing technology |
| CN111086181A (en) * | 2019-12-28 | 2020-05-01 | 北京星和众工设备技术股份有限公司 | Preparation method of lithium battery diaphragm |
| CN112457639A (en) * | 2020-11-17 | 2021-03-09 | 杨勇 | Polylactic resin prepared from corn and preparation method thereof |
| CN115058032A (en) * | 2022-07-20 | 2022-09-16 | 扬州惠通生物新材料有限公司 | Preparation method of polylactic acid film opening master batch |
| CN115975355A (en) * | 2022-12-29 | 2023-04-18 | 广州市信联包装容器实业有限公司 | High-barrier-toughness PET (polyethylene terephthalate) -based composite film and preparation method and application thereof |
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| JP2003082212A (en) * | 2001-09-13 | 2003-03-19 | Unitika Ltd | Biodegradable resin film |
| JP2003261695A (en) * | 2002-03-11 | 2003-09-19 | Unitika Ltd | Polylactic acid based biaxially stretched film |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105419262A (en) * | 2014-09-02 | 2016-03-23 | 允友成(宿迁)复合新材料有限公司 | Polylactic acid/montmorillonite nanometer composite material preparation method |
| CN106495175A (en) * | 2016-12-23 | 2017-03-15 | 仲恺农业工程学院 | A kind of preparation method of organic modification montmonrillonite |
| CN109929228A (en) * | 2019-04-17 | 2019-06-25 | 谷水英 | Green biodegradable plastics film and its processing technology |
| CN111086181A (en) * | 2019-12-28 | 2020-05-01 | 北京星和众工设备技术股份有限公司 | Preparation method of lithium battery diaphragm |
| CN112457639A (en) * | 2020-11-17 | 2021-03-09 | 杨勇 | Polylactic resin prepared from corn and preparation method thereof |
| CN115058032A (en) * | 2022-07-20 | 2022-09-16 | 扬州惠通生物新材料有限公司 | Preparation method of polylactic acid film opening master batch |
| CN115058032B (en) * | 2022-07-20 | 2024-01-26 | 扬州惠通生物新材料有限公司 | Preparation method of polylactic acid film opening master batch |
| CN115975355A (en) * | 2022-12-29 | 2023-04-18 | 广州市信联包装容器实业有限公司 | High-barrier-toughness PET (polyethylene terephthalate) -based composite film and preparation method and application thereof |
| CN115975355B (en) * | 2022-12-29 | 2024-05-07 | 广州市信联包装容器实业有限公司 | PET-based composite film with high barrier strength and toughness, and preparation method and application thereof |
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