CN101649072A - Full-degradable biological material and film product thereof - Google Patents
Full-degradable biological material and film product thereof Download PDFInfo
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Abstract
The invention discloses a full-degradable biological material and a film product thereof. The material is prepared by mixing main materials of starch with good biological degradation property and polyester mixture under the conditions of specific temperature, rotation speed, processing time and the like, adding other auxiliary agents, and finishing and self compounding molecular structures under the melting condition. The processing property and the using property are good. The film product made of degradable materials has the advantages of wear resistance, oil resistance, leakage resistance,large tensile strength and high flexibility, and can be applied in the temperature range of -20 DEG C to 70 DEG C. The invention has the advantages of novel component, no toxic additives, scientific compounding, simple process, low energy consumption, large-scale industrial production, no toxicity or harmfulness and complete biological degradation, can be used as compost after being discarded, andespecially used as an environmental-protection substitution product of various disposable film products.
Description
Technical field
The present invention relates to a kind of full-degradable biological material and film article thereof, particularly a kind of is full-degradable biological material and its film article of base-material with starch, and the preparation method of this material and film thereof.
Technical background
The petrochemical industry plastics are penetrated into the human being's production various fields in life already, when bringing people's convenience and practicality, because itself, bring problems such as energy consumption and environmental pollution inevitably.Especially use film class the most widely in the plastics, as various non-returnable container bags, shopping bag, refuse bag, agricultural mulching etc., volume is little, in light weight, cost is low, has caused arbitrarily to abandon after using, and is difficult for reclaiming, day by day worsen in energy shortage and environment, and the today of advocating the sustainability harmonious development, caused that common people more and more pay close attention to, also become one of hot subject of scientific circles' challenges.People strive to find the substitute of plastics, and last century the seventies the notion of degradative plastics has been proposed.Even to this day, there is many degradative plastics product to come out, but the overwhelming majority wherein, belongs to the plastics of filled-type or modification.Natural polymers such as these so-called degradative plastics utilizations interpolation starch improve the degradation property of plastics, still contain traditional PE in the material component, PP, and PS etc. can't fundamentally accomplish to degrade fully, recycle.In addition, the degradable material industry has also been developed complete novel, degradable material fully, as PLA, PCL, green macromolecular material such as PBS, but cost costliness, this material not as miscellaneous plastic prod, has hindered its industrialized popularization and market and has used on processing characteristics and use properties simultaneously.
Summary of the invention
The objective of the invention is to disclose a kind of full-degradable biological material and by the high-fall biofilm of separating that can be used for the substituted for plastic film article of this material preparation; The present invention also aims to disclose the preparation method of this material and film thereof.
The present invention is achieved through the following technical solutions.
The raw material of full-degradable biological material of the present invention consists of:
Base-material: starch 30～50 weight parts, ethylene/vinyl alcohol copolymer (EVOH) 3～7 weight parts and ethylene acrylic acid co polymer (EAA) 2～4 weight parts;
Modified component: Fully-degradable ester mixture 9.5～19.5 weight parts;
Other auxiliary agents: expanding material, oxidation inhibitor, antifreezing agent, lubricant and/or releasing agent amount to 9.1～24.2 weight parts.
Wherein, the Fully-degradable ester mixture in the modified component is poly(lactic acid) (PLA), polycaprolactone
(PCL), terephthalic acid, hexanodioic acid, 1,4-butyleneglycol three-element copolymerized ester (PBAT), succsinic acid fourth diester (PBS), polybutylene terephthalate (PBT) and/or poly-3 butyric esters (PHB), preferred: PCL 2～5 weight parts, PBAT 4～9 weight parts and PBT 3.5～5.5 weight parts.
Other auxiliary agents are preferably: carboxymethyl cellulose 0.5～2 weight part, sorbyl alcohol 3～8 weight parts; Triphenyl phosphite 1.5～3 weight parts, glycerine 2.5～5.5 weight parts, epoxy soybean oil 0.1～0.8 weight part, liquid wax 0.1～0.4 weight part, Zinic stearas 0.6～1.8 weight part, talcum powder 0.2～0.9 weight part and calcium stearate 0.6～1.8 weight part.
The raw material composition of film of the present invention is preferably:
Base-material: starch 35 weight parts, ethylene/vinyl alcohol copolymer (EVOH) 6 weight parts, ethylene acrylic acid co polymer (EAA) 3 weight parts;
Modified component: polycaprolactone (PCL) 3.5 weight parts, PBAT 4.5 weight parts, polybutylene terephthalate (PBT) 4.5 weight parts;
Other auxiliary agents: carboxymethyl cellulose 1.25 weight parts, sorbyl alcohol 6 weight parts, triphenyl phosphite 2.25 weight parts, glycerine 4 weight parts, epoxy soybean oil 0.45 weight part, liquid wax 0.25 weight part, Zinic stearas 1.2 weight parts, talcum powder 0.55 weight part and calcium stearate 1.2 weight parts.
The raw material composition of film of the present invention is preferably:
Base-material: starch 40 weight parts, ethylene/vinyl alcohol copolymer (EVOH) 4 weight parts, ethylene acrylic acid co polymer (EAA) 4 weight parts;
Modified component: polycaprolactone (PCL) 4 weight parts, PBAT 8 weight parts, polybutylene terephthalate (PBT) 4 weight parts;
Other auxiliary agents: carboxymethyl cellulose 0.7 weight part, sorbyl alcohol 7 weight parts, triphenyl phosphite 2.8 weight parts, glycerine 3 weight parts, epoxy soybean oil 0.7 weight part, liquid wax 0.3 weight part, Zinic stearas 0.8 weight part, talcum powder 0.3 weight part and calcium stearate 1.6 weight parts.
The raw material composition of film of the present invention is preferably:
Base-material: starch 45 weight parts, ethylene/vinyl alcohol copolymer (EVOH) 5 weight parts, ethylene acrylic acid co polymer (EAA) 4 weight parts;
Modified component: polycaprolactone (PCL) 3 weight parts, PBAT 6 weight parts, polybutylene terephthalate (PBT) 5 weight parts;
Other auxiliary agents: carboxymethyl cellulose 1.8 weight parts, sorbyl alcohol 4 weight parts, triphenyl phosphite 1.7 weight parts, glycerine 5 weight parts, epoxy soybean oil 0.2 weight part, liquid wax 0.2 weight part, Zinic stearas 1.6 weight parts, talcum powder 0.8 weight part and calcium stearate 0.8 weight part.
The preparation method of film of the present invention comprises the steps:
Earlier the dusty raw materials in the raw material is crossed 120 mesh sieves, standby; The starch that pre-treatment is good, EVOH and EAA put in the high-speed mixer, and in 60～70 ℃ of mixing 3～4 minutes, rotating speed was made as 220～260 rev/mins; The modification auxiliary material is put in the high-speed mixer again, be warming up to 90～110 ℃, rotating speed rises to 320～460 rev/mins, moves 8～12 minutes; The powder in other auxiliary agents, liquid material are put in the high-speed mixer successively at last, it is 150～170 ℃ that temperature is set, high-speed mixing 4～6 minutes again; After the mixed raw materials cooling, put in the twin screw extruder, it is 120～180 rev/mins that rotating speed is set, and it is 90～160 ℃ that processing covers temperature, goes through dehydration, exhaust, plasticizing, shears, extrudes, discharging, makes full-degradable biological material of the present invention.
Can be used as the further preparation cost invention of masterbatch film with full-degradable biological material of the present invention: according to actual needs, full-degradable biological material is passed through single screw rod blown film unit, pass through fusion, plasticizing, supercharging, cooling, traction, rolling successively, can make the thin-film material of different size, thickness is 0.005～0.060mm; Tensile strength vertically is 28.5～37.5MP, laterally is 22.6～30.2MP; Elongation at break vertically is 291%～374%, laterally is 352%～486%; Angle tear strength vertically is 86～112KN/m, laterally is 72～88KN/m.
Full-degradable biological material of the present invention and film article thereof be under the condition of specific temperature, rotating speed and process period, will have good biodegradability properties can starch and polyester mixture be that main raw material is mixing, add other reaction promoters, be composited by the molecular structure alteration under the molten state and from group, processing and use properties excellence, made film class finished product is water-fast, oil resistant, anti-seepage, tensile strength are big, the snappiness height can be used in-20 ℃～70 ℃ temperature range.Component novelty of the present invention does not contain poisonous additive, the batching science, and technology is simple, energy consumption is low, is fit to large-scale industrial production, and is particularly nontoxic, harmless, fully biodegradable can be used as compost after discarding, and is particularly useful for the environment-friend substitution product of each kind disposable film article.
Following experimental example and embodiment further specify but are not limited to the present invention.
Full-degradable biological material of the present invention that experimental example 1 embodiment 1 prepares and the experiment of the performance parameter test of film article thereof
According to the Specifeca tion speeification of following standard testing full-degradable biological material of the present invention and film article thereof, the result is as shown in table 1.
According to method described in the GB/T 5009.60-2003 product appearance is estimated;
According to ISO-14855-2004, the testing method of biological degradation rate and disintegration under the composting conditions, the disintegration situation of testing the biodegradation intensity and the film of feed particles and film article;
Carry out the mensuration of feed particles density according to GB/T 1033.1-2008;
Carry out the finished film Determination of thickness according to GB/T 6672-2001;
Carry out the mensuration of feed particles molten state current downflow speed according to the described method of GB 3682-2000;
Raw material and finished film are carried out the detection of heavy metal and sanitary index according to the described method of GB 18006-1999;
Finished film is carried out the mensuration of the angle tear strength of vertical and horizontal according to the described method of QB/T1130-1991;
According to the described method of GB/T13022-1991 finished film is carried out the tensile strength of vertical, horizontal and the mensuration of fracture extensibility respectively;
Finished film is carried out the mensuration of heat sealing strength according to the described method of QBT 2358-1998.
The Specifeca tion speeification table of table 1 full-degradable biological material of the present invention and film article thereof
Following embodiment is used to further specify but is not limited to the present invention.
Embodiment
Embodiment 1: full-degradable biological material of the present invention and film article thereof
Base-material: starch 35Kg, ethylene/vinyl alcohol copolymer (EVOH) 6Kg and ethylene acrylic acid co polymer (EAA) 3Kg;
Modification auxiliary material: polycaprolactone (PCL) 3.5Kg, PBAT 4.5Kg and polybutylene terephthalate (PBT) 4.5Kg;
Other auxiliary agents: carboxymethyl cellulose 1.25Kg, sorbyl alcohol 6Kg, triphenyl phosphite 2.25Kg, glycerine 4Kg, epoxy soybean oil 0.45Kg, liquid wax 0.25Kg, Zinic stearas 1.2Kg, talcum powder 0.55Kg and calcium stearate 1.2Kg.
Earlier the dusty raw materials in the raw material is crossed 120 mesh sieves, standby; The starch that pre-treatment is good, EVOH and EAA put in the high-speed mixer, and in 65 ℃ of mixing 3 minutes, rotating speed was made as 240 rev/mins; The modification auxiliary material is put in the high-speed mixer again, be warming up to 100 ℃, rotating speed rises to 390 rev/mins, moves 10 minutes; The powder in other auxiliary agents, liquid material are put in the high-speed mixer successively at last, it is 165 ℃ that temperature is set, high-speed mixing 5 minutes again; With after the mixed raw materials cooling, to put in the twin screw extruder, it is 150 rev/mins that rotating speed is set, it is 90～160 ℃ that processing covers temperature, goes through dehydration, exhaust, plasticizing, shears, extrudes, discharging, makes full-degradable biological material of the present invention;
Above-mentioned full-degradable biological material is passed through single screw rod blown film unit as the film masterbatch, pass through fusion, plasticizing, supercharging, cooling, traction, rolling successively, can make thin-film material, thickness 0.020mm; Tensile strength vertically is 30.1MP, laterally is 26.4MP; Elongation at break vertically is 322%, laterally is 415%; Angle tear strength vertically is 90.4N/mm, laterally is 77.1N/mm; Can degrade fully, application of temperature is-20 ℃～70 ℃.
Embodiment 2: full-degradable biological material of the present invention and film article thereof
Base-material: starch 40Kg, ethylene/vinyl alcohol copolymer (EVOH) 4Kg and ethylene acrylic acid co polymer (EAA) 4Kg;
Modification auxiliary material: polycaprolactone (PCL) 4Kg, PBAT 8Kg and polybutylene terephthalate (PBT) 4Kg;
Other auxiliary agents: carboxymethyl cellulose 0.7Kg, sorbyl alcohol 7Kg, triphenyl phosphite 2.8Kg, glycerine 3Kg, epoxy soybean oil 0.7Kg, liquid wax 0.3Kg, Zinic stearas 0.8Kg, talcum powder 0.3Kg and calcium stearate 1.6Kg.
Earlier the dusty raw materials in the raw material is crossed 120 mesh sieves, standby; The starch that pre-treatment is good, EVOH and EAA put in the high-speed mixer, and in 70 ℃ of mixing 3 minutes, rotating speed was made as 230 rev/mins; The modification auxiliary material is put in the high-speed mixer again, be warming up to 105 ℃, rotating speed rises to 450 rev/mins, moves 9 minutes; The powder in other auxiliary agents, liquid material are put in the high-speed mixer successively at last, it is 160 ℃ that temperature is set, high-speed mixing 6 minutes again; After the mixed raw materials cooling, drop in the twin screw extruder, it is 170 rev/mins that rotating speed is set; It is 90～160 ℃ that processing covers temperature, goes through dehydration, exhaust, plasticizing, shears, extrudes, discharging, makes full-degradable biological material of the present invention;
Above-mentioned full-degradable biological material is passed through single screw rod blown film unit as the film masterbatch, pass through fusion, plasticizing, supercharging, cooling, traction, rolling successively, can make thin-film material, thickness 0.010mm; Tensile strength vertically is 35.2MP, laterally is 28.7MP; Elongation at break vertically is 348%, laterally is 453%; Angle tear strength vertically is 101KN/m, laterally is 80KN/mm; Can degrade fully, application of temperature is-20 ℃～70 ℃.
Embodiment 3: full-degradable biological material of the present invention and film article thereof
Base-material: starch 45Kg, ethylene/vinyl alcohol copolymer (EVOH) 5Kg and ethylene acrylic acid co polymer (EAA) 4Kg;
Modification auxiliary material: polycaprolactone (PCL) 3Kg, PBAT 6Kg and polybutylene terephthalate (PBT) 5Kg;
Other auxiliary agents: carboxymethyl cellulose 1.8Kg and sorbyl alcohol 4Kg, triphenyl phosphite 1.7Kg, glycerine 5Kg, epoxy soybean oil 0.2Kg, liquid wax 0.2Kg, Zinic stearas 1.6Kg, talcum powder 0.8Kg and calcium stearate 0.8Kg.
Earlier the dusty raw materials in the raw material is crossed 120 mesh sieves, standby; The starch that pre-treatment is good, EVOH and EAA put in the high-speed mixer, and in 60 ℃ of mixing 4 minutes, rotating speed was made as 250 rev/mins; The modification auxiliary material is put in the high-speed mixer again, be warming up to 95 ℃, rotating speed rises to 330 rev/mins, moves 11 minutes; The powder in other auxiliary agents, liquid material are put in the high-speed mixer successively at last, it is 155 ℃ that temperature is set, high-speed mixing 6 minutes again; With after the mixed raw materials cooling, to put in the twin screw extruder, it is 130 rev/mins that rotating speed is set, it is 90～160 ℃ that processing covers temperature, goes through dehydration, exhaust, plasticizing, shears, extrudes, discharging, makes full-degradable biological material of the present invention;
Above-mentioned full-degradable biological material is passed through single screw rod blown film unit as the film masterbatch, pass through fusion, plasticizing, supercharging, cooling, traction, rolling successively, can make the thin-film material of different size, thickness 0.050mm; Tensile strength vertically is 29.6MP, laterally is 25.3MP; Elongation at break vertically is 297%, laterally is 387%; Angle tear strength vertically is 89KN/m, laterally is 75N/mm; Can degrade fully, application of temperature is-20 ℃～70 ℃.
Claims (11)
1, a kind of full-degradable biological material is characterized in that the raw material of this material consists of:
Base-material: starch 30～50 weight parts, ethylene/vinyl alcohol copolymer (EVOH) 3～7 weight parts and ethylene acrylic acid co polymer (EAA) 2～4 weight parts;
Modified component: Fully-degradable ester mixture 9.5～19.5 weight parts;
Other auxiliary agents: expanding material, oxidation inhibitor, antifreezing agent, lubricant and/or releasing agent amount to 9.1～24.2 weight parts.
2, full-degradable biological material as claimed in claim 1, it is characterized in that the Fully-degradable ester mixture in the modified component wherein is poly(lactic acid) (PLA), polycaprolactone (PCL), terephthalic acid, hexanodioic acid, 1,4-butyleneglycol three-element copolymerized ester (PBAT), succsinic acid fourth diester (PBS), polybutylene terephthalate (PBT) and/or poly-3 butyric esters (PHB).
3, as claim 1 and 2 described full-biodegradable materials, it is characterized in that wherein
Modified component is: polycaprolactone (PCL) 2～5 weight parts, 1,4-butyleneglycol three-element copolymerized ester (PBAT) 4～9 weight parts and polybutylene terephthalate (PBT) 3.5～5.5 weight parts;
Other auxiliary agents are: carboxymethyl cellulose 0.5～2 weight part, sorbyl alcohol 3～8 weight parts; Triphenyl phosphite 1.5～3 weight parts, glycerine 2.5～5.5 weight parts, epoxy soybean oil 0.1～0.8 weight part, liquid wax 0.1～0.4 weight part, Zinic stearas 0.6～1.8 weight part, talcum powder 0.2～0.9 weight part and calcium stearate 0.6～1.8 weight part.
4, full-degradable biological material as claimed in claim 3 is characterized in that the raw material of this material consists of:
Base-material: starch 35 weight parts, ethylene/vinyl alcohol copolymer (EVOH) 6 weight parts, ethylene acrylic acid co polymer (EAA) 3 weight parts;
Modified component: polycaprolactone (PCL) 3.5 weight parts, PBAT 4.5 weight parts, polybutylene terephthalate (PBT) 4.5 weight parts;
Other auxiliary agents: carboxymethyl cellulose 1.25 weight parts, sorbyl alcohol 6 weight parts, triphenyl phosphite 2.25 weight parts, glycerine 4 weight parts, epoxy soybean oil 0.45 weight part, liquid wax 0.25 weight part, Zinic stearas 1.2 weight parts, talcum powder 0.55 weight part and calcium stearate 1.2 weight parts.
5, full-degradable biological material as claimed in claim 3 is characterized in that the raw material of this material consists of:
Base-material: starch 40 weight parts, ethylene/vinyl alcohol copolymer (EVOH) 4 weight parts, ethylene acrylic acid co polymer (EAA) 4 weight parts;
Modified component: polycaprolactone (PCL) 4 weight parts, PBAT 8 weight parts, polybutylene terephthalate (PBT) 4 weight parts;
Other auxiliary agents: carboxymethyl cellulose 0.7 weight part, sorbyl alcohol 7 weight parts, triphenyl phosphite 2.8 weight parts, glycerine 3 weight parts, epoxy soybean oil 0.7 weight part, liquid wax 0.3 weight part, Zinic stearas 0.8 weight part, talcum powder 0.3 weight part and calcium stearate 1.6 weight parts.
6, full-degradable biological material as claimed in claim 3 is characterized in that the raw material of this material consists of:
Base-material: starch 45 weight parts, ethylene/vinyl alcohol copolymer (EVOH) 5 weight parts, ethylene acrylic acid co polymer (EAA) 4 weight parts;
Modified component: polycaprolactone (PCL) 3 weight parts, PBAT 6 weight parts, polybutylene terephthalate (PBT) 5 weight parts;
Other auxiliary agents: carboxymethyl cellulose 1.8 weight parts, sorbyl alcohol 4 weight parts, triphenyl phosphite 1.7 weight parts, glycerine 5 weight parts, epoxy soybean oil 0.2 weight part, liquid wax 0.2 weight part, Zinic stearas 1.6 weight parts, talcum powder 0.8 weight part and calcium stearate 0.8 weight part.
7,, it is characterized in that this method comprises the steps: as the preparation method of claim 1,2,4,5 or 6 described full-degradable biological materials
Earlier the dusty raw materials in the raw material is crossed 120 mesh sieves, standby; The starch that pre-treatment is good, EVOH and EAA put in the high-speed mixer, and in 60～70 ℃ of mixing 3～4 minutes, rotating speed was made as 220～260 rev/mins; The modification auxiliary material is put in the high-speed mixer again, be warming up to 90～110 ℃, rotating speed rises to 320～460 rev/mins, moves 8～12 minutes; The powder in other auxiliary agents, liquid material are put in the high-speed mixer successively at last, it is 150～170 ℃ that temperature is set, high-speed mixing 4～6 minutes again; After the mixed raw materials cooling, put in the twin screw extruder, it is 120～180 rev/mins that rotating speed is set, and it is 90～160 ℃ that processing covers temperature, goes through dehydration, exhaust, plasticizing, shears, extrudes, discharging, makes full-degradable biological material.
8, the preparation method of full-degradable biological material as claimed in claim 3 is characterized in that this method comprises the steps:
Earlier the dusty raw materials in the raw material is crossed 120 mesh sieves, standby; The starch that pre-treatment is good, EVOH and EAA put in the high-speed mixer, and in 60～70 ℃ of mixing 3～4 minutes, rotating speed was made as 220～260 rev/mins; The modification auxiliary material is put in the high-speed mixer again, be warming up to 90～110 ℃, rotating speed rises to 320～460 rev/mins, moves 8～12 minutes; The powder in other auxiliary agents, liquid material are put in the high-speed mixer successively at last, it is 150～170 ℃ that temperature is set, high-speed mixing 4～6 minutes again; After the mixed raw materials cooling, put in the twin screw extruder, it is 120～180 rev/mins that rotating speed is set, and it is 90～160 ℃ that processing covers temperature, goes through dehydration, exhaust, plasticizing, shears, extrudes, discharging, makes full-degradable biological material.
9, as the arbitrary described full-degradable biological material of claim 1-6, it is characterized in that this full-degradable biological material is made film.
10, full-degradable biological material as claimed in claim 9, the preparation method who it is characterized in that wherein said film is: use full-degradable biological material as masterbatch, full-degradable biological material is passed through single screw rod blown film unit, pass through fusion, plasticizing, supercharging, cooling, traction, rolling successively, make the film of different size.
11, as claim 9 or 10 described films, the thickness that it is characterized in that this film is 0.005～0.060mm; Tensile strength vertically is 28.5～37.5MP, laterally is 22.6～30.2MP; Elongation at break vertically is 291%～374%, laterally is 352%～486%; Angle tear strength vertically is 86～112KN/m, laterally is 72～88KN/m; Can degrade fully, application of temperature is-20 ℃～70 ℃.
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| CN102276906B (en) * | 2011-07-07 | 2012-11-28 | 刘立文 | Modified ethane-vinyl alcohol copolymer composite material and preparation technology thereof |
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