CN105086383A - PBAT composite film based on irradiation modification and preparation method thereof - Google Patents
PBAT composite film based on irradiation modification and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a PBAT composite film based on irradiation modification and a preparation method thereof. The composite film comprises, by weight, 100 parts of PBAT, 10-100 parts of remaining biodegradable materials, 0.1-7 parts of compatilizer, 0.1-6 parts of irradiation sensitizer, 0.1-5 parts of antioxidant, 0.1-4 parts of light stabilizer, 0.1-5 parts of anti-ultraviolet agents and 0-4 parts of lubricant. Compared with the prior art, by means of the PBAT composite film based on the irradiation modification, the biodegradability of the material is maintained, the excellent mechanical strength, barrier performance, aging resistance and the like are achieved, and the application of the biodegradable film is expanded.
Description
Technical field
The invention belongs to biodegradable composite material radiation modification field, specifically a kind of PBAT laminated film based on radiation modification and preparation method thereof, particularly a kind of radiation modification complete biodegradable PBAT laminated film and preparation method thereof, also belongs to technical field of environmental science.
Background technology
The global problem of environmental pollution brought due to petroleum-based plastics is day by day serious, and having renewable, low-carbon (LC), environmental protection feature bio-degradable plastics has become the Main Trends of The Development of macromolecular material industry.
Poly terephthalic acid-hexanodioic acid-butanediol ester (PBAT) is important Biodegradable material, belong to thermoplastic polyester, under certain environment (as temperature, pH value and oxygen), and under the nature microorganism effects such as bacterium, fungi, mould and algae, chemistry, biology or physical action can be there is and degrade or decompose, and finally become carbonic acid gas, methane, water, inorganic salt and new biomass completely, realize coming from nature, being attributed to natural Sustainable development.BASF AG is PBAT whole world largest production business, and annual production is 6.5 ten thousand tons.The existing good ductility of PBAT and elongation at break, also have good thermotolerance and shock strength.In addition, its film forming properties is excellent, and film article can use PE processing film instrument and supplies direct production.The maximum application market of PBAT is at film applications; BASF associating Shanghai is expanded farsighted chemical industry and is promoted the application of PBAT/PLA (poly(lactic acid)) laminated film at agriculture field in the whole country; find to replace conventional P E film to use, and effect of increasing production has been played to some crops.Another staple product of PBAT film class is the bag such as shopping bag, refuse bag based article, due to its puncture, anti tear, replaced PE film to be effectively applied, Jilin Province in 2015 formally implement " taboo is moulded and is made " more the application of PBAT film article lay a solid foundation.It need to recognize that, although PBAT film obtains certain application on mulch film and bag based article, but its property retention on mulch film is poor, easily break, and be limited to performance deficiency (as intensity is low, barrier is poor, resistance of aging is weak) and the higher restriction of material cost, for applying more broadly, modification need be carried out.
Radiation modification is the method for modifying of a kind of green, safety, has been applied to the modification of polymkeric substance.Polymeric inner produces free radical under irradiation, molecular chain is occurred crosslinked, changes the bodily form into, significantly can improve the multiple performance of material by linear, as wear resistance, ageing-resistant, stress crack resistant and raising mechanical strength etc.Chinese patent application 200910188653.6 discloses a kind of IXPE, improves mechanical property under high temperature, improves chemical-resistant stability and ageing resistance.Mitomo etc. disclosed a kind of method being improved PLA thermotolerance by irradiation in 2005, and irradiation post softening temperature can reach 200 DEG C.Chinese patent application 20071055475.0 utilizes cross-linking radiation and crystallization modified synergic PLA, obtains high-intensity high heat-resistance PLA matrix material.
Therefore, utilize radiation modification technology, prepare a kind of complete biodegradable PBAT laminated film, there is the performance that original material does not have, comprise excellent mechanical strength, the performance such as ageing-resistant, promoting that PBAT laminated film is applied more broadly is the problem that the present invention needs solution badly.
Summary of the invention
For defect of the prior art, the object of this invention is to provide a kind of PBAT laminated film based on radiation modification and preparation method thereof; The modified PBAT laminated film obtained not only maintains material totally biodegradable, is conducive to ecological protection, and it has excellent mechanical strength, barrier property and ageing resistance etc., has expanded the application of Biodegradable film.
The present invention is achieved by the following technical solutions:
First aspect, the invention provides a kind of PBAT laminated film based on radiation modification, described laminated film comprises following component and parts by weight:
Preferably, all the other Biodegradable materials described are one or more in PLA, polycaprolactone, poly butylene succinate, poly-succinic tetramethylene adipate, aliphatic polycarbonate, polyhydroxy-alkanoate, polysaccharide, xylogen, protein, natural rubber; Described polysaccharide comprises starch, chitosan, Mierocrystalline cellulose, chitin etc.
When all the other Biodegradable materials described are above-mentioned a certain component, the present invention is without the need to adding compatilizer, and namely compatilizer gets 0 part, when all the other Biodegradable materials described be above-mentioned two kinds and above component time, need to add compatilizer, namely the parts by weight of compatilizer are less than or equal to 5 for being greater than zero.
Preferably, described compatilizer is one or more in peroxide compounds, isocyanate ester compound, multi-group epoxy compound's (JoncrylADR series as BASF AG's production), phosphate compounds; Wherein, described peroxide compounds is one or more in dibenzoyl peroxide, dicumyl peroxide, di-t-butyl peroxide, Diisopropyl azodicarboxylate; Described isocyanate ester compound is a kind of in diphenylmethanediisocyanate, tolylene diisocyanate or combination; Described multi-group epoxy compound comprises the JoncrylADR series that BASF AG produces, and JoncrylADR series, as a kind of chainextender, based on its special reaction in system, also uses as compatilizer; Described phosphate compounds is one or more in triphenylphosphate, trisnonylphenyl phosphite.
Preferably, described irradiation sensitizing agent is one or more in cyamelide triallyl, tricarbimide methyl triallyl, Viscoat 295, trimethylolpropane trimethacrylate, triallyl cyanurate, trimethylolpropane tris allyl ethers, triallyl pentaerythritol, tetraallyl tetramethylolmethane.
Preferably, described oxidation inhibitor is one or more in MALEIC ANHYDRIDE, epoxy soybean oil, oxidation inhibitor B215, antioxidant 264, antioxidant 1010, antioxidant 1076, antioxidant 330, oxidation inhibitor 3032, anti-oxidant DLTP, irgasfos 168, oxidation inhibitor 164.
Preferably, the steady agent of described light is 2,2 '-thiobis (4-tertiary octyl phenol oxygen base) nickel, three (1,2,2,6,6-Pempiten base) phosphorous acid ester, 4-benzoyloxy-2, one or more in 2,6,6-tetramethyl piperidine, HMPA.
Preferably, described anti ultraviolet agent is salicylic acid phenyl ester, 2,4-dihydroxy benaophenonel, ESCALOL 567, Octabenzone, 2-(the 2-hydroxyl-3-tertiary butyl-5-aminomethyl phenyl)-5-chlorinated benzotriazole, or 2-(2-hydroxyl-3,5-di-tert-butyl-phenyl)-5-chlorinated benzotriazole, single phenylformic acid resorcinol, 2,4,6-tri-(2 ' n-butoxyphenyl)-1, one or more in 3,5-triazine, o-Nitraniline, p-cresol.
Preferably, described lubricant is one or more in stearic acid, aluminum stearate, calcium stearate, Zinic stearas, erucicamide, amine hydroxybenzene, oxidized polyethlene wax, stearin, paraffin, polyethylene wax.
Each material of the present invention is by commercially.
Second aspect, the invention provides a kind of described preparation method based on the PBAT laminated film of radiation modification, described preparation method comprises the steps:
Raw materials pretreatment: dry described PBAT, all the other Biodegradable materials, then mixes with other feed composition of residue, obtains raw mixture;
Extruding pelletization: by described raw mixture melt blending, extruding pelletization, obtain pellet;
Machine-shaping: dry described pellet also makes film, i.e. film article;
Radiation treatment: described film article is placed in radiation treatment under ray, obtains described radiation modification PBAT laminated film.
Preferably, in feed pretreatment step, the condition of described drying is 30 ~ 80 DEG C, 2 ~ 10h; Further, described drying adopts vacuum drying oven;
Preferably, in feed pretreatment step, described mixing specifically refers to stirring at normal temperature; Further, the time of described stirring is 2 ~ 3min, rotating speed is 600 ~ 1000r/min.
Preferably, in extruding pelletization step, the temperature of described melt blending is 100 ~ 220 DEG C; The die temperature of described extruding pelletization employing twin screw extruder is 120 ~ 200 DEG C, screw slenderness ratio is 40:1, rotating speed 100 ~ 300r/min.
Preferably, in machine-shaping step, the condition of described drying is 30 ~ 80 DEG C, 4 ~ 12h; Described drying specifically adopts vacuum drying oven.
Preferably, in machine-shaping step, described in make film technique adopt blowing or curtain coating, described in the temperature condition making film and need be 110 ~ 220 DEG C.
Preferably, in radiation treatment step, described ray is one in electron beam, gamma-rays, X-ray or combination; Further, described electron beam is produced by rumbatron, described gamma-rays by
60co or
137cs produces.
Preferably, in radiation treatment step, the irradiation dose of described ray is 1 ~ 300kGy; More preferably, the irradiation dose of described ray is 60 ~ 220kGy.
Compared with prior art, the present invention has following beneficial effect:
1, by by PBAT and other relatively low cost Biodegradable material reactive blendings, make material monolithic cost reduce by more than 20%, realize performance complement simultaneously, possess the performance that single-component does not have;
2, by the reaction of functional group between compatilizer and degradation material, can carry out chain extension to plural components, original position forms multipolymer as bridge structure, and phase interface cohesive force is improved, and material melt viscosity is also improved, and has widened process window; Improve film impelling strength and intensity;
3, in irradiation process by the initiation of free radical on sensitizing agent, promote and the combination of free radical in degradation material, cross-linking radiation density and efficiency improved;
4, oxidation inhibitor not only inhibits the oxidation of polymkeric substance in processing, and in irradiation process by and the coordinative role of the steady agent of light, and in polymkeric substance, capture sunken free radical reaction, the cracking of material radiation oxidation is effectively suppressed;
5, by radiation modification, polymer molecular chain occurs crosslinked, makes molecule change the bodily form into by linear, makes film have excellent mechanical strength, barrier property and ageing resistance etc., has expanded the application of PBAT film, had novelty.As mulch film application, can summary stability in use, reduce the generation of breaking;
6, by regulating sensitizing agent, the steady agent of light, antioxidant content, and irradiation dose, make production continuous, convenient, controlled;
7, laminated film maintains totally biodegradable performance, and medical science and environmental science have larger application potential, and alternative petroleum base general purpose film uses in a large number, alleviates environmental stress.
Embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.Following examples will contribute to those skilled in the art and understand the present invention further, but not limit the present invention in any form.It should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, some distortion and improvement can also be made.These all belong to protection scope of the present invention.
embodiment 1
The present embodiment provides a kind of PBAT laminated film based on radiation modification and preparation method thereof, and the component of described laminated film is as shown in table 1; The preparation method of described laminated film is as follows:
Raw materials pretreatment: the PBAT getting 30 DEG C of vacuum-drying 10h, by embodiment in table 11 component and content proportioning, 600r/min under normal temperature, high-speed stirring 3min;
Extruding pelletization: twin screw extruder melt blending, extruding pelletization, extrusion temperature is 100 ~ 135 DEG C, and the die temperature of screw extrusion press is 120 ~ 200 DEG C, screw slenderness ratio is 40:1, rotating speed 250r/min;
Machine-shaping: 30 DEG C of vacuum-drying 12h, 110 ~ 130 DEG C of Blown Films;
Radiation treatment: adopt the electron beam of 220kGy to film radiation treatment, obtained laminated film (sample sequence number 1).
embodiment 2
The present embodiment provides a kind of PBAT laminated film based on radiation modification and preparation method thereof, and the component of described laminated film is as shown in table 1; The preparation method of described laminated film is as follows:
Raw materials pretreatment: PBAT and PLA getting 80 DEG C of vacuum-drying 2h, by component shown in embodiment in table 12 and content proportioning, 800r/min high-speed stirring 3min under normal temperature;
Extruding pelletization: twin screw extruder melt blending, extruding pelletization, extrusion temperature is 110 ~ 180 DEG C, and the die temperature of screw extrusion press is 120 ~ 200 DEG C, screw slenderness ratio is 40:1, rotating speed 150r/min;
Machine-shaping: 80 DEG C of vacuum-drying 4h, 135 ~ 170 DEG C of Blown Films;
Radiation treatment: adopt the electron beam of 160kGy to film radiation treatment, obtained laminated film (sample sequence number 2).
embodiment 3
The present embodiment provides a kind of PBAT laminated film based on radiation modification and preparation method thereof, and the component of described laminated film is as shown in table 1; The preparation method of described laminated film is as follows:
Raw materials pretreatment: PBAT and the polyhydroxy-alkanoate of getting 60 DEG C of vacuum-drying 6h, by component shown in embodiment in table 13 and content proportioning, 1000r/min high-speed stirring 3min under normal temperature;
Extruding pelletization: twin screw extruder melt blending, extruding pelletization, extrusion temperature is 110 ~ 190 DEG C, and the die temperature of screw extrusion press is 120 ~ 200 DEG C, screw slenderness ratio is 40:1, rotating speed 150r/min;
Machine-shaping: 80 DEG C of vacuum-drying 10h, 160 ~ 190 DEG C are blown casting film-forming;
Radiation treatment: adopt the electron beam of 60kGy to film radiation treatment, obtained laminated film (sample sequence number 3).
Table 1
comparative example 1
This comparative example is the comparative example of embodiment 2, provides a kind of laminated film, the component of described laminated film and weight content identical with embodiment 2, difference is, described preparation method comprises the steps:
Raw materials pretreatment: PBAT and PLA getting vacuum-drying 4h, by embodiment 2 proportioning of component and content, 900r/min high-speed stirring 3min under normal temperature;
Extruding pelletization: twin screw extruder melt blending, extruding pelletization, extrusion temperature is 110 ~ 185 DEG C, rotating speed 150r/min;
Machine-shaping: 80 DEG C of vacuum-drying 8h, 135 ~ 170 DEG C of Blown Films;
Radiation treatment: nothing, does not namely carry out radiation treatment, prepares laminated film (sample sequence number 4).
comparative example 2
This comparative example provides a kind of laminated film and preparation method thereof, and described preparation method is with embodiment 2, and component and the weight content of described laminated film are as shown in table 2, obtained laminated film (sample sequence number 5).
comparative example 3
This comparative example is the comparative example of embodiment 2, and provide a kind of laminated film (sample sequence number 6), component and the parts by weight of described laminated film are as shown in table 2, and described preparation method is identical with embodiment 2.
Table 2
performance test
Carry out performance test to above-described embodiment and comparative example, result is as shown in table 3:
Table 3
Conclusion: can be found by the design of embodiment and reference examples and Comparative result, from component, compatilizer can carry out chain extension to component, increases phase interface cohesive force, improves film impelling strength and intensity.Sensitizing agent causes free radical in radiation treatment, with the combination of free radical in degradation material, promotes molecule crosslinked, thus changes material property.Photosensitizers and antioxidant coordinative role, with capture in polymkeric substance fall into free radical reaction, the cracking of material radiation oxidation is effectively suppressed, reduces the generation of side reaction.Radiation treatment is a kind of effective ways improving PBAT laminated film performance, changes material internal molecular chain structure, change the bodily form into by linear by irradiation, gives the performance that material does not have originally.As high strength, high-impact, high friction, high-barrier, high anti-ageing etc., expand the Application Areas of biodegradable PBAT laminated film.
Above specific embodiments of the invention are described.It is to be appreciated that the present invention is not limited to above-mentioned particular implementation, those skilled in the art can make various distortion or amendment within the scope of the claims, and this does not affect flesh and blood of the present invention.
Claims (10)
1. based on a PBAT laminated film for radiation modification, it is characterized in that, described laminated film comprises following component and parts by weight:
2. the PBAT laminated film based on radiation modification according to claim 1, it is characterized in that, all the other Biodegradable materials described are one or more in PLA, polycaprolactone, poly butylene succinate, poly-succinic tetramethylene adipate, aliphatic polycarbonate, polyhydroxy-alkanoate, polysaccharide, xylogen, protein, natural rubber.
3. the PBAT laminated film based on radiation modification according to claim 1, is characterized in that, described compatilizer is one or more in peroxide compounds, isocyanate ester compound, multi-group epoxy compound, phosphate compounds.
4. the PBAT laminated film based on radiation modification according to claim 1, it is characterized in that, described irradiation sensitizing agent is one or more in cyamelide triallyl, tricarbimide methyl triallyl, Viscoat 295, trimethylolpropane trimethacrylate, triallyl cyanurate, trimethylolpropane tris allyl ethers, triallyl pentaerythritol, tetraallyl tetramethylolmethane.
5. the PBAT laminated film based on radiation modification according to claim 1, it is characterized in that, described oxidation inhibitor is one or more in MALEIC ANHYDRIDE, epoxy soybean oil, oxidation inhibitor B215, antioxidant 264, antioxidant 1010, antioxidant 1076, antioxidant 330, oxidation inhibitor 3032, anti-oxidant DLTP, irgasfos 168, oxidation inhibitor 164.
6. the PBAT laminated film based on radiation modification according to claim 1, it is characterized in that, the steady agent of described light is 2,2 '-thiobis (4-tertiary octyl phenol oxygen base) nickel, three (1,2,2,6,6-Pempiten base) phosphorous acid ester, 4-benzoyloxy-2,2, one or more in 6,6-tetramethyl piperidine, HMPA.
7. the PBAT laminated film based on radiation modification according to claim 1, it is characterized in that, described anti ultraviolet agent is salicylic acid phenyl ester, 2, 4-dihydroxy benaophenonel, ESCALOL 567, Octabenzone, 2-(the 2-hydroxyl-3-tertiary butyl-5-aminomethyl phenyl)-5-chlorinated benzotriazole, or 2-(2-hydroxyl-3, 5-di-tert-butyl-phenyl)-5-chlorinated benzotriazole, single phenylformic acid resorcinol, 2, 4, 6-tri-(2 ' n-butoxyphenyl)-1, 3, 5-triazine, o-Nitraniline, one or more in p-cresol.
8. the PBAT laminated film based on radiation modification according to claim 1, it is characterized in that, described lubricant is one or more in stearic acid, aluminum stearate, calcium stearate, Zinic stearas, erucicamide, amine hydroxybenzene, oxidized polyethlene wax, stearin, paraffin, polyethylene wax.
9. a preparation method for the PBAT laminated film based on radiation modification according to claim 1, it is characterized in that, described preparation method comprises the steps:
Raw materials pretreatment: dry described PBAT, all the other Biodegradable materials, then mixes with other feed composition remaining, obtains raw mixture;
Extruding pelletization: by described raw mixture melt blending, extruding pelletization, obtain pellet;
Machine-shaping: dry described pellet also makes film, i.e. film article;
Radiation treatment: described film article is placed in radiation treatment under ray, obtains described radiation modification PBAT laminated film.
10. the preparation method of the PBAT laminated film based on radiation modification according to claim 9, is characterized in that, in radiation treatment step, described ray is the combination of one or more in electron beam, gamma-rays, X-ray.
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Application publication date: 20151125 |