CN103304851A - High-starch-content waterproof totally-decomposed composite material and preparation method thereof - Google Patents
High-starch-content waterproof totally-decomposed composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-starch-content waterproof totally-decomposed composite material and a preparation method thereof. The method comprises the steps of: firstly dispersing nanosilicon dioxide particles in a plasticizer in advance to obtain nano sol; secondly, evenly blending the sol and starch in a high-speed mixer, and then kneading the mixture together with polyvinyl alcohol in a kneading machine to obtain starch-based master batch; and finally carrying out melt blending on the starch-based master batch and polylactic acid through one of or a combination of more of an open mill, an internal mixer and an extruder to obtain the high-starch-content waterproof totally-decomposed composite material. Compared with the ordinary biology-based composite material, the high-starch-content waterproof totally-decomposed composite material is high in starch content, low in cost, and good in ingredient compatibility, the mechanical property and waterproof property of the material can be both obviously improved, and all ingredients can be totally decomposed, so that the excellent sustainable development characteristic can be achieved; and meanwhile, the high-starch-content waterproof totally-decomposed composite material can be machined by adopting die pressing, extrusion, injection molding and other technologies on general plastic machining equipment.
Description
Technical field
The present invention relates to water-fast biodegradable composites of a kind of high-content of starch and preparation method thereof, be specifically related to utilize nano silicon that starch is carried out modification, and prepare water-fast biodegradable composites of high-content of starch and preparation method thereof with degradation material blend such as poly(lactic acid), polyvinyl alcohol, belong to technical field of polymer materials.
Background technology
Based on the pressure of environment and social sustainable development, national governments have all given great attention to the white pollution of plastics, thus to the research and development of degradable plastics give and support energetically.
Starch (St) is polysaccharide compound, is now widely used biodegradable natural polymer, and it is decomposed into glucose under the effect of microorganism, be degraded at last CO
2And H
2O.Although starch has been widely used in a lot of fields such as papermaking, weaving, medicine, oil, food and fermentation industry, but starch belongs to and contains polyhydric rigidity natural macromolecular material, and the defectives such as intensity is low hamper the broader applications of starch material always after plasticizing difficulty and the moisture absorption.Since 20 century 70s, people have developed a series of degradative plastics products with starch and synthetic plastic blend, wherein how starch is applied as the filler that reduces cost, but starch content is lower in these kind of starch base plastics, how to exist as the filler that reduces cost, these type of plastics are owing to can not be degradable, to solving having little significance of environmental pollution.
Poly(lactic acid) (PLA) is that more biodegradable material is used in research at present, and it must be hydrolyzed first, just can carry out enzymolysis after being hydrolyzed into to a certain degree, and degraded product is CO
2And H
2O, free from environmental pollution, have simultaneously good biocompatibility, hydrophobicity, workability and good physical and mechanical properties.The matrix material of poly(lactic acid) and starch blending preparation can effectively improve the processing characteristics of starch-based material, significantly improves mechanical strength and the water tolerance of material, and can be degradable, should and possess the good characteristic of Sustainable development.
Although but the starch/polylactic acid blended compound material has certain consistency, can't be fully compatible, the elongation at break of made matrix material is low, toughness is not enough.Polyvinyl alcohol (PVA) is a kind of biodegradable polymer that is rich in hydroxyl, can be used as the interfacial compatibilizer of starch/polylactic acid mixture, when improving starch/polylactic acid blended compound material consistency, can further improve the mechanical strength of this matrix material.
Nano silicon (nano-SiO
2) be a kind of three-dimensional structure nano particle of rich surface hydroxyl, after starch/polylactic acid/polyvinyl alcohol composite material blend, can be preferentially and the hydroxy combining on starch, poly(lactic acid) or polyvinyl alcohol surface form hydrogen bond, the consistency of this matrix material is further improved, stop simultaneously the combination of free state water molecules and composite material surface hydroxyl, thereby promoted the water tolerance of matrix material.
Summary of the invention
The object of the invention is to address the deficiencies of the prior art, water-fast biodegradable composites of high-content of starch that a kind of high strength, high-content of starch, water tolerance have larger improvement and preparation method thereof is provided.The method at first is dispersed in nano-silicon dioxide particle in advance and makes Nano sol in the softening agent, then this colloidal sol and starch are mixed in high-speed mixer, and then mediate in kneader with polyvinyl alcohol and to make starch-based master batch, at last this masterbatch and poly(lactic acid) are carried out melt blending by a kind of or more than one combinations in mill, Banbury mixer or the forcing machine, make the water-fast biodegradable composites of high-content of starch.The consistency of each component of matrix material is good, and mechanical property, water tolerance all are significantly increased, and can adopt mold pressing at general device of plastic processing, extrudes, the processes such as injection moulding becomes goods.
The present invention is achieved by the following technical solutions:
Water-fast biodegradable composites of a kind of high-content of starch and preparation method thereof is characterized in that the water-fast biodegradable composites of described high-content of starch is according to the mass fraction, fills a prescription composed as follows:
Described starch is one or more combinations in the esterification starchs such as phosphate ester starch, acetate starch and octene succinate starch.
Described poly(lactic acid) is one or more combinations in D-poly(lactic acid), PLLA and the meso poly(lactic acid).
Described polyvinyl alcohol is one or more combinations in the polyvinyl alcohol with low alcoholysis level of different polymerization degree.
Described softening agent is one or more combinations in polypropylene glycol, polyoxyethylene glycol, glycerol and the tri-n-butyl citrate.
The particle diameter of described nano silicon is between the 7-12 nanometer.
The preparation method of the water-fast biodegradable composites of high-content of starch, specifically at first adopt a kind of in high-shear emulsion machine, emulsification pump or the hypervelocity stirrer that 1-4 part nano silicon is scattered in 20-40 part softening agent, time is 1-3h, rotating speed is 700-3000rpm, adopt again ultrasonic generator expeling bubble wherein, time is 1-2h, makes Nano sol; Secondly 20-40 part Nano sol is mixed in high-speed mixer with 50-80 part starch, the time is 30min, mediates in kneader with 10-30 part polyvinyl alcohol and makes starch-based master batch, and the time is 10min; At last 80-150 part starch-based master batch and 20-50 part poly(lactic acid) are carried out melt blending by one or more combinations in mill, Banbury mixer or the forcing machine, make the water-fast biodegradable composites of high-content of starch.Adopting the mixing temperature of mill is 170-210 ℃, and the time is 10-20min; Adopting the banburying temperature of Banbury mixer is 180-210 ℃, and the time is 5-15min, and rotating speed is 50-150rpm; When adopting forcing machine, the barrel temperature of forcing machine is 140-210 ℃, and screw speed is 50-150rpm.
The present invention has the following advantages:
Compare with common bio-based composite material, the starch content of the water-fast biodegradable composites of high-content of starch is high, with low cost, component compatibility is good, mechanical property, the water tolerance of material all are significantly increased, and all components can be degradable, thereby the good characteristic that possesses Sustainable development simultaneously can adopt mold pressing, extrudes, the processes such as injection moulding becomes goods at general device of plastic processing.
Embodiment:
Now in conjunction with specific embodiments content of the present invention is described in detail, but described embodiment only is used for the present invention rather than restriction the present invention.
Embodiment 1
Material provided by the invention is formulated by weight by following raw material:
At first the nano silicon in the above-mentioned raw materials and polypropylene glycol are mixed with the hypervelocity stirrer, the time is 1h, and rotating speed is 700-3000rpm, adopts ultrasonic generator expeling bubble wherein again, and the time is 1h, makes Nano sol; Secondly Nano sol is mixed in high-speed mixer with acetate starch, the time is 30min, mediates in kneader with the polyvinyl alcohol of the polymerization degree 1700, alcoholysis degree 88% again, makes starch-based master batch, and the time is 10min; At last starch-based master batch and PLLA are carried out melt blending by Banbury mixer, the banburying temperature is 180 ℃, and the time is 6min, and rotating speed is 60rpm, makes the water-fast biodegradable composites of high-content of starch.
Embodiment 2
Material provided by the invention is formulated by weight by following raw material:
At first the nano silicon in the above-mentioned raw materials and glycerol are mixed with high-shear emulsion machine, the time is 1.5h, and rotating speed is 700-3000rpm, adopts ultrasonic generator expeling bubble wherein again, and the time is 1.5h, makes Nano sol; Secondly Nano sol is mixed in high-speed mixer with acetate starch, the time is 30min, mediates in kneader with the polyvinyl alcohol of the polymerization degree 500, alcoholysis degree 88% again, makes starch-based master batch, and the time is 10min; At last starch-based master batch and PLLA are carried out melt blending by Banbury mixer, the banburying temperature is 180 ℃, and the time is 8min, and rotating speed is 60rpm, makes the water-fast biodegradable composites of high-content of starch.
Embodiment 3
Material provided by the invention is formulated by weight by following raw material:
At first the nano silicon in the above-mentioned raw materials and tri-n-butyl citrate are mixed with emulsification pump, the time is 1.5h, and rotating speed is 700-3000rpm, adopts ultrasonic generator expeling bubble wherein again, and the time is 2h, makes Nano sol; Secondly Nano sol is mixed in high-speed mixer with phosphate ester starch, the time is 30min, mediates in kneader with the polyvinyl alcohol of the polymerization degree 500, alcoholysis degree 88% again, makes starch-based master batch, and the time is 10min; At last starch-based master batch and D-poly(lactic acid) are carried out melt blending by mill, mixing temperature is 190 ℃, and the time is 10min, makes the water-fast biodegradable composites of high-content of starch.
Embodiment 4
Material provided by the invention is formulated by weight by following raw material:
At first the nano silicon in the above-mentioned raw materials and tri-n-butyl citrate are mixed with high-shear emulsion machine, the time is 2.5h, and rotating speed is 700-3000rpm, adopts ultrasonic generator expeling bubble wherein again, and the time is 2h, makes Nano sol; Secondly Nano sol is mixed in high-speed mixer with the octene succinate starch, the time is 30min, mediates in kneader with the polyvinyl alcohol of the polymerization degree 1700, alcoholysis degree 88% again, makes starch-based master batch, and the time is 10min; At last starch-based master batch and PLLA are carried out melt blending by forcing machine, the barrel temperature of forcing machine is 170-210 ℃, and screw speed is 60rpm, makes the water-fast biodegradable composites of high-content of starch.
Embodiment 5
Material provided by the invention is formulated by weight by following raw material:
At first the nano silicon in the above-mentioned raw materials and polyoxyethylene glycol are mixed with the hypervelocity stirrer, the time is 2.5h, and rotating speed is 700-3000rpm, adopts ultrasonic generator expeling bubble wherein again, and the time is 2h, makes Nano sol; Secondly Nano sol is mixed in high-speed mixer with acetate starch, the time is 30min, is 500 with the polymerization degree again, the polyvinyl alcohol of alcoholysis degree 88% mediates in kneader, makes starch-based master batch, and the time is 10min; At last starch-based master batch and PLLA are carried out melt blending by Banbury mixer, the banburying temperature is 190 ℃, and the time is 10min, and rotating speed is 60rpm, makes the water-fast biodegradable composites of high-content of starch.
Embodiment 6
Material provided by the invention is formulated by weight by following raw material:
At first the nano silicon in the above-mentioned raw materials and glycerol are mixed with high-shear emulsion machine, the time is 3h, and rotating speed is 700-3000rpm, adopts ultrasonic generator expeling bubble wherein again, and the time is 2h, makes Nano sol; Secondly Nano sol is mixed in high-speed mixer with the octene succinate starch, the time is 30min, is 2400 with the polymerization degree again, the polyvinyl alcohol of alcoholysis degree 88% mediates in kneader, makes starch-based master batch, and the time is 10min; At last starch-based master batch and D-poly(lactic acid) are carried out melt blending by Banbury mixer, the banburying temperature is 200 ℃, and the time is 10min, and rotating speed is 60rpm, makes the water-fast biodegradable composites of high-content of starch.
Claims (10)
1. the water-fast biodegradable composites of high-content of starch is characterized in that the water-fast biodegradable composites of described a kind of high-content of starch according to the mass fraction, fills a prescription composed as follows:
2. material according to claim 1 is characterized in that starch is one or more combinations in the esterification starchs such as phosphate ester starch, acetate starch and octene succinate starch.
3. material according to claim 1 is characterized in that poly(lactic acid) is one or more combinations in D-poly(lactic acid), PLLA and the meso poly(lactic acid).
4. material according to claim 1 is characterized in that polyvinyl alcohol is one or more combinations in the polyvinyl alcohol with low alcoholysis level of different polymerization degree.
5. material according to claim 1 is characterized in that softening agent is one or more combinations in polypropylene glycol, polyoxyethylene glycol, glycerol and the tri-n-butyl citrate.
6. material according to claim 1, the particle diameter that it is characterized in that nano silicon is between the 7-12 nanometer.
7. material according to claim 1, it is characterized in that after nano silicon and the softening agent weighing, with a kind of in high-shear emulsion machine, emulsification pump or the hypervelocity stirrer nano silicon is scattered in the softening agent, and adopt ultrasonic generator expeling bubble wherein, make Nano sol.
8. material according to claim 1 is characterized in that mixing in high-speed mixer after starch and the Nano sol weighing, mediates in kneader with polyvinyl alcohol again, makes starch-based master batch.
9. material according to claim 1 is characterized in that starch-based master batch and poly(lactic acid) are carried out melt blending by one or more combinations in mill, Banbury mixer or the forcing machine, makes the water-fast biodegradable composites of high-content of starch.
10. material according to claim 1, it is characterized in that comparing with common bio-based composite material, the water-fast biodegradable composites of high-content of starch with low cost, component compatibility good, mechanical property, the water tolerance of material all are significantly increased, and all components can be degradable, can adopt mold pressing at general device of plastic processing, extrudes, the processes such as injection moulding becomes goods.
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| CN103865275A (en) * | 2014-04-11 | 2014-06-18 | 山东理工大学 | Method for improving the water resistance of polyethylene glycol film modified by polylactic acid and polyvinyl alcohol |
| CN103937269A (en) * | 2014-03-24 | 2014-07-23 | 山东理工大学 | Method for modifying water proofness of polyvinyl alcohol membrane by polypeptide and polycaprolactone |
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Application publication date: 20130918 |