CN104861210A - Starch-base fully biodegradable resin with steady hydrophobic property and preparation method thereof - Google Patents
Starch-base fully biodegradable resin with steady hydrophobic property and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a starch-base fully biodegradable resin with steady hydrophobic property and a preparation method thereof, belonging to the technical field of biodegradable materials. The resin comprises the following raw materials in parts by weight: 20-50 parts of modified starch, 50-80 parts of fully biodegradable polyester, 0.1-5 parts of a lubricant, and 0.1-0.5 parts of an antioxidant. The starch-base fully biodegradable resin with steady hydrophobic property is rational in design, so that the dispersity of the starch is improved greatly through pre-treatment of the starch; the moisture content is relatively low, so that degradation reaction of the resin in the processing process is also reduced. Through rational micronization function, the performance of the starch-base fully biodegradable resin is improved obviously.
Description
Technical field
The invention belongs to biodegradable material technical field, be specifically related to a kind of hydrophobic stable starch base complete biodegradable resin and preparation method thereof.
Background technology
Full-biodegradable material on current world market has quite a few to be starch base full-biodegradable material.The interpolation of starch reduces the cost of material on the one hand, on the other hand also can certain aspect performance of reinforcement material.As lancinating, the Kekelé structure count of film material.Intensity; The dimensional stability of injecting products, thermotolerance; The melt strength etc. of sheet material processing.
Current starch base full-biodegradable material all adds the plasticizing dispersion that softening agent promotes starch substantially simultaneously.Softening agent, for being mainly polyalcohols and water, causing on the one hand the adding of softening agent full-biodegradable material in the alcoholysis of the course of processing and hydrolysis, affects the stability to aging of material.Full-biodegradable material goods on the other hand containing softening agent, due to the easy moisture absorption, make product more facile hydrolysis, accelerated deterioration; Also can cause the change of film stiffness because of the change of ambient moisture for complete biodegradable film material.
CN96104325.3 discloses the thermoplastic compounds comprising starch and other components from natural source, and by starch ingredients, cellulosic ester or ether, the softening agent of starch phase and Mierocrystalline cellulose and derivative, compatilizer and matrix resin are composited.CN200810044975.9 discloses a kind of full-biodegradable plastic film and preparation method, and film raw material is thermoplastic starch, biodegradable polymers and the complementary composition of 1 ~ 9 μm is raw material.Thermoplastic starch be wherein through plasticising process comprise in the starch of W-Gum, tapioca (flour), pea starch, wheat starch, potato starch, konjak starch, canna starch starch any one.CN201210553133.2 discloses a kind of preparation method of plasticity-starch conversion PBAT biodegradable material, relate to the preparation of plasticity-starch, plasticity-starch and PBAT melt blending, material modified working method three steps, be specially at a certain temperature, with a certain proportion of composite elasticizer, plasticising is carried out to starch and prepare plasticity-starch, after vacuum drying treatment, carry out composite and extruding pelletization by the mode of melt blending and PBAT matrix at a certain temperature again, prepare plasticity-starch conversion PBAT biodegradable material; Softening agent is one or more in methane amide, glycerine, urea, deionized water mixtures of being mixed to get.CN201210185395.8 discloses a kind of degradable starch-based plastics, it is characterized by and prepare graft starch by amidin, add after being uniformly mixed in high-speed mixer again with the blending resin of 35 ~ 50 weight parts, the softening agent of 10 ~ 15 weight parts, through twin screw extruder granulation.
Although we find the goods not plasticizer-containing using starch, water and complete biodegradable resin alloy extruding pelletization out to prepare, still absorb water when contacting water very serious, the water vapor transmittance of material is also very high.So in order to make the starch base complete biodegradable goods that prepare hydrophobic stable, must improve starch and formula.
Summary of the invention
For prior art Problems existing, the object of the invention is to design the technical scheme that a kind of hydrophobic stable starch base complete biodegradable resin and preparation method thereof is provided, this Biodegradable resin has hydrophobicity, the aging character such as slowly, and processing characteristics is good, is suitable for suitability for industrialized production.
Described a kind of hydrophobic stable starch base complete biodegradable resin, is characterized in that the raw material comprising following weight part: treated starch 20 ~ 50 parts, complete biodegradable polyester 50 ~ 80 parts, lubricant 0.1 ~ 5 part, 0.1 ~ 0.5 part, oxidation inhibitor;
Described treated starch is mixed to get according to weight ratio 100:0.1 ~ 0.5 by starch and starch modifying agent.
Described a kind of hydrophobic stable starch base complete biodegradable resin, is characterized in that the raw material comprising following weight part: treated starch 25 ~ 35 parts, complete biodegradable polyester 60 ~ 70 parts, lubricant 2 ~ 3 parts, 0.2 ~ 0.4 part, oxidation inhibitor.
Described a kind of hydrophobic stable starch base complete biodegradable resin, is characterized in that described starch is one or more in W-Gum, Starch rice, yam starch, tapioca (flour), pea starch, wheat starch, green starch, sweet potato starch.
Described a kind of hydrophobic stable starch base complete biodegradable resin, is characterized in that described complete biodegradable polyester is one or more in poly terephthalic acid-tetramethylene adipate (PBAT), poly terephthalic acid-succinic acid-butanediol ester (PBST), poly-hexanodioic acid-succinic acid-butanediol ester (PBSA), poly (propylene carbonate) (PPC), poly(lactic acid) (PLA), polyglycolic acid (PGA), polyhydroxyalkanoate (PHA), poly butylene succinate (PBS).
Described a kind of hydrophobic stable starch base complete biodegradable resin, is characterized in that described starch modifying agent is one or more in stearic acid, titanate coupling agent, aluminate coupling agent, low melt point paraffin, mineral oil, alkenyl succinic acid.
Described a kind of hydrophobic stable starch base complete biodegradable resin, is characterized in that described lubricant is N, N-ethylene bis stearamide, calcium stearate, polyethylene wax, paraffin or Tegin 55G.
Described a kind of hydrophobic stable starch base complete biodegradable resin, is characterized in that described oxidation inhibitor is the two or more oxidation inhibitor in Hinered phenols, phosphorous acid esters and phosphoric acid ester oxidation inhibitor;
Described Hinered phenols antioxidant is more than one oxidation inhibitor in antioxidant 1010, antioxidant 1076, oxidation inhibitor 1098, oxidation inhibitor 1790, oxidation inhibitor 245, oxidation inhibitor 246, antioxidant BHT, antioxidant 3114 and antioxidant 330;
Described phosphite ester kind antioxidant is more than one oxidation inhibitor in irgasfos 168, antioxidant 618, oxidation inhibitor 626, oxidation inhibitor 627, trimethyl phosphite, triethyl-phosphite and triphenyl phosphite;
Described phosphoric acid ester oxidation inhibitor is more than one oxidation inhibitor in trimethyl phosphite 99, triethyl phosphate and triphenylphosphate.
The preparation method of described a kind of hydrophobic stable starch base complete biodegradable resin, is characterized in that comprising the following steps:
1) common starch is through pulverizing mill miniaturization extremely required particle diameter under 500 ~ 3000RPM condition;
2) starch through miniaturization process mixes with starch modifying agent through homogenizer;
3) starch mixed in double-cone vacuum drier, at 100 ~ 140 DEG C, reacting drying discharging in 12 ~ 24 hours under-0.07 ~-0.095MPa condition, discharging moisture is within 0.5%;
4) treated treated starch and lubricant, oxidation inhibitor, complete biodegradable mixed with resin are even;
5) material mixed through twin screw extruder 130 ~ 170 DEG C, extrude under 200 ~ 300RPM condition, cooling, dry, obtain hydrophobic stable starch base complete biodegradable resin particle.
The present invention is reasonable in design, and by the pre-treatment of starch, the dispersiveness of starch is greatly improved, lower moisture content also reduces the DeR of resin in the course of processing.By rational miniaturization effect, the property of starch base complete biodegradable resin be can significantly improve.
Embodiment
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
The W-Gum (median size is at about 3 ~ 5 μm) of the miniaturization of 100 parts, 0.3 part of titanate coupling agent are mixed under high-speed mixer 600RPM condition, be placed in double-cone vacuum drier, at 120 DEG C, dry reaction discharging in 24 hours under-0.09MPa condition, discharging moisture is 0.25%.Again by 30 parts of starch processed, 70 parts of PBAT(melting means 4.2g/10min), 0.2 part of N, N-ethylene bis stearamide, 0.4 part of composite antioxidant [1010,168 and triphenylphosphate (1:2:3)] mix in high-speed mixer, material after mixing extrudes through parallel dual-screw extruding machine that (extrusion temperature is 132 DEG C, screw speed is 260r/min), namely obtain described starch base complete biodegradable resin granular material through the pelletizing of air-cooled tie rod drag chain.Pellet blown film is good, and thickness is that the film of 0.020mm is torn very well, and face is smooth.The water vapor transmittance of starch conversion film is 1120 g/m
224 h.
Comparison example
Again by 30 parts of W-Gums, 70 parts of PBAT(melting means 4.2g/10min), 5 parts of glycerine, 0.2 part of N, N-ethylene bis stearamide, 0.4 part of composite antioxidant [1010,168 and triphenylphosphate (1:2:3)] mix in high-speed mixer, material after mixing extrudes through parallel dual-screw extruding machine that (extrusion temperature is 132 DEG C, screw speed is 260r/min), namely obtain described starch base complete biodegradable resin granular material through the pelletizing of air-cooled tie rod drag chain.Pellet blown film is good, and thickness is that the film of 0.020mm is torn very well, and face is smooth.The water vapor transmittance of starch conversion film is 3230 g/m
224 h.
Embodiment 2
The tapioca (flour) (median size is at about 10 ~ 15 μm) of the miniaturization of 100 parts, 0.2 part of aluminate coupling agent are mixed under high-speed mixer 600RPM condition, be placed in double-cone vacuum drier, at 110 DEG C, dry reaction discharging in 20 hours under-0.095MPa condition, discharging moisture is 0.3%.Again by 50 parts of starch processed, 30 parts of PLA(melting means 30.2g/10min), 20 parts of PBS(melting means 25.0g/10min), 0.5 part of paraffin, 0.5 part of composite antioxidant [1076,626 and trimethyl phosphite 99 (1:3:5)] mix in high-speed mixer, material after mixing extrudes through parallel dual-screw extruding machine that (extrusion temperature is 165 DEG C, screw speed is 230r/min), namely obtain described starch base complete biodegradable resin granular material through the pelletizing of air-cooled tie rod drag chain.Pellet surface is smooth, and injection moulding knife-fork-spoon product surface is out shinny, and toughness is better.Knife-fork-spoon goods are put into 50 DEG C of distilled water leachings and put final vacuum drying in 24 hours, the rate of weight loss of knife-fork-spoon is 0.1%
Comparison example
By 50 portions of tapioca (flour)s, 30 parts of PLA(melting means 30.2g/10min), 20 parts of PBS(melting means 25.0g/10min), 0.5 part of paraffin, 7 parts of glycerine, 0.5 part of composite antioxidant [1076,626 and trimethyl phosphite 99 (1:3:5)] mix under high-speed mixer 600RPM condition, material after mixing extrudes through parallel dual-screw extruding machine that (extrusion temperature is 165 DEG C, screw speed is 230r/min), namely obtain described starch base complete biodegradable resin granular material through the pelletizing of air-cooled tie rod drag chain.Pellet surface is more coarse, and injection moulding knife-fork-spoon product surface brightness is out general, and toughness is reported to the leadship after accomplishing a task.Knife-fork-spoon goods are put into 50 DEG C of distilled water leachings and put final vacuum drying in 24 hours, the rate of weight loss of knife-fork-spoon is 0.5%
Embodiment 3
The pea starch (median size is at about 7 ~ 9 μm) of the miniaturization of 100 parts, 0.1 part of stearic acid, 0.2 part of titanate coupling agent are mixed under high-speed mixer 600RPM condition, be placed in double-cone vacuum drier, at 125 DEG C, dry reaction discharging in 24 hours under-0.09MPa condition, discharging moisture is 0.2%.The starch again 25 parts processed, 15 parts of PHA(melting means 15.2g/10min), 60 parts of PBSA(melting means 12.3g/10min), 0.3 part of calcium stearate, 0.3 part of paraffin, 0.3 part of composite antioxidant [1098, 627 and triethyl phosphate (1:2:4)] mix in high-speed mixer, material after mixing extrudes through parallel dual-screw extruding machine that (extrusion temperature is 160 DEG C, screw speed is 240r/min) sheet material that 0.8mm is thick, sheet surface is smooth shinny, the cutlery box smooth surface blistered out, without coarse point, be placed on final vacuum drying in 24 hours in the water bath with thermostatic control of 25 DEG C, rate of weight loss is 0.25%
Comparison example
By 25 parts of pea starches, 4 parts of glycerine, 15 parts of PHA(melting means 15.2g/10min), 60 parts of PBSA(melting means 12.3g/10min), 0.3 part of calcium stearate, 0.3 part of paraffin, 0.3 part of composite antioxidant [1098, 627 and triethyl phosphate (1:2:4)] mix in high-speed mixer, material after mixing extrudes through parallel dual-screw extruding machine that (extrusion temperature is 160 DEG C, screw speed is 240r/min) sheet material that 0.8mm is thick, sheet surface slickness is general, the cutlery box blistered out to be placed in the water bath with thermostatic control of 25 DEG C 24 hours, in cutlery box, starch amount of precipitation is 1.1%.
Embodiment 4
The yam starch (median size is at about 12 ~ 14 μm) of the miniaturization of 100 parts, 0.1 part of mineral oil, 0.2 part of aluminate coupling agent are mixed under high-speed mixer 600RPM condition, be placed in double-cone vacuum drier, at 115 DEG C, dry reaction discharging in 20 hours under-0.095MPa condition, discharging moisture is 0.3%.Again by 30 parts of starch processed, 15 parts of PPC(melting means 20.7g/10min), 55 parts of PBS(melting means 25.6g/10min), 0.2 part of N, N-ethylene bis stearamide, 0.5 part of polyethylene wax, 0.3 part of composite antioxidant [1790,618 and triethyl phosphate (1:3:4)] mix in high-speed mixer, material after mixing extrudes through parallel dual-screw extruding machine that (extrusion temperature is 140 DEG C, screw speed is 210r/min), namely obtain described starch base complete biodegradable resin granular material through the pelletizing of air-cooled tie rod drag chain.Pellet surface is smooth, and injection moulding pen cap product surface is out shinny, and intensity is better.Injection moulding pen cap goods leaching is out placed in the distilled water final vacuum drying in 24 hours of 25 DEG C, claims rate of weight loss is 0.05%.
Comparison example
Again by 30 parts of yam starchs, 5 parts of glycerine, 15 parts of PPC(melting means 20.7g/10min), 55 parts of PBS(melting means 25.6g/10min), 0.2 part of N, N-ethylene bis stearamide, 0.5 part of polyethylene wax, 0.3% composite antioxidant [1790,618 and triethyl phosphate (1:3:4)] mix in high-speed mixer, material after mixing extrudes through parallel dual-screw extruding machine that (extrusion temperature is 140 DEG C, screw speed is 210r/min), namely obtain described starch base complete biodegradable resin granular material through the pelletizing of air-cooled tie rod drag chain.Pellet surface slickness is general, injection moulding pen cap goods leaching is out placed in the distilled water final vacuum drying in 24 hours of 25 DEG C, claims rate of weight loss is 0.3.
Claims (8)
1. a hydrophobic stable starch base complete biodegradable resin, is characterized in that the raw material comprising following weight part: treated starch 20 ~ 50 parts, complete biodegradable polyester 50 ~ 80 parts, lubricant 0.1 ~ 5 part, 0.1 ~ 0.5 part, oxidation inhibitor;
Described treated starch is mixed to get according to weight ratio 100:0.1 ~ 0.5 by starch and starch modifying agent.
2. a kind of hydrophobic stable starch base complete biodegradable resin as claimed in claim 1, is characterized in that the raw material comprising following weight part: treated starch 25 ~ 35 parts, complete biodegradable polyester 60 ~ 70 parts, lubricant 2 ~ 3 parts, 0.2 ~ 0.4 part, oxidation inhibitor.
3. a kind of hydrophobic stable starch base complete biodegradable resin as claimed in claim 1 or 2, is characterized in that described starch is one or more in W-Gum, Starch rice, yam starch, tapioca (flour), pea starch, wheat starch, green starch, sweet potato starch.
4. a kind of hydrophobic stable starch base complete biodegradable resin as claimed in claim 1 or 2, is characterized in that described complete biodegradable polyester is one or more in poly terephthalic acid-tetramethylene adipate (PBAT), poly terephthalic acid-succinic acid-butanediol ester (PBST), poly-hexanodioic acid-succinic acid-butanediol ester (PBSA), poly (propylene carbonate) (PPC), poly(lactic acid) (PLA), polyglycolic acid (PGA), polyhydroxyalkanoate (PHA), poly butylene succinate (PBS).
5. a kind of hydrophobic stable starch base complete biodegradable resin as claimed in claim 1 or 2, is characterized in that described starch modifying agent is one or more in stearic acid, titanate coupling agent, aluminate coupling agent, low melt point paraffin, mineral oil, alkenyl succinic acid.
6. a kind of hydrophobic stable starch base complete biodegradable resin as claimed in claim 1 or 2, is characterized in that described lubricant is N, N-ethylene bis stearamide, calcium stearate, polyethylene wax, paraffin or Tegin 55G.
7. a kind of hydrophobic stable starch base complete biodegradable resin as claimed in claim 1 or 2, is characterized in that described oxidation inhibitor is the two or more oxidation inhibitor in Hinered phenols, phosphorous acid esters and phosphoric acid ester oxidation inhibitor;
Described Hinered phenols antioxidant is more than one oxidation inhibitor in antioxidant 1010, antioxidant 1076, oxidation inhibitor 1098, oxidation inhibitor 1790, oxidation inhibitor 245, oxidation inhibitor 246, antioxidant BHT, antioxidant 3114 and antioxidant 330;
Described phosphite ester kind antioxidant is more than one oxidation inhibitor in irgasfos 168, antioxidant 618, oxidation inhibitor 626, oxidation inhibitor 627, trimethyl phosphite, triethyl-phosphite and triphenyl phosphite;
Described phosphoric acid ester oxidation inhibitor is more than one oxidation inhibitor in trimethyl phosphite 99, triethyl phosphate and triphenylphosphate.
8. the preparation method of a kind of hydrophobic stable starch base complete biodegradable resin as claimed in claim 1 or 2, is characterized in that comprising the following steps:
1) common starch is through pulverizing mill miniaturization extremely required particle diameter under 500 ~ 3000RPM condition;
2) starch through miniaturization process mixes with starch modifying agent through homogenizer;
3) starch mixed in double-cone vacuum drier, at 100 ~ 140 DEG C, reacting drying discharging in 12 ~ 24 hours under-0.07 ~-0.095MPa condition, discharging moisture is within 0.5%;
4) treated treated starch and lubricant, oxidation inhibitor, complete biodegradable mixed with resin are even;
5) material mixed through twin screw extruder 130 ~ 170 DEG C, extrude under 200 ~ 300RPM condition, cooling, dry, obtain hydrophobic stable starch base complete biodegradable resin particle.
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