CN103627151B - Polyester full-biodegradable mulch film - Google Patents
Polyester full-biodegradable mulch film Download PDFInfo
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Abstract
The present invention relates to mulch film, be specifically related to a kind of Polyester full-biodegradable mulch film.This mulch film is made up of the raw material of following mass percent: 40-80% flexibility degraded polyester, the degraded of 10-55% rigidity polyester, 0.5-1.5% reactive compatibilizer, 1-2% heat preserving agent, 1-2% wetting Agent for Printing Inks, 0.5-1.5% antiager, 0.5-1% slipping agent and 0.5-3% opening agent.Biodegradable mulch of the present invention, not containing any non-biodegradable common plastics, not starch-containing yet, can on common LDPE inflation film manufacturing machine Blown Film, without the need to carrying out any transformation to equipment, this mulch film transparency is good, and snappiness is good, intensity is high, water vapor transmittance is low, is beneficial to moisturizing and good heat preservation performance.
Description
Technical field
The present invention relates to mulch film, be specifically related to a kind of Polyester full-biodegradable mulch film.
Background technology
The sixties in 20th century, film-mulching technique rises in the country such as Japanese, American-European, and is popularized.Since 1979, plastic mulching cultivation technology obtains in China and widelys popularize, and nowadays membrane covering area has reached 2.1 hundred million mu, and Year's consumption is more than 1,200,000 tons.The popularization and application of mulch film, especially for arid, that weather condition are severe area, farm crop are served to the key effect of insulation soil moisture conservation, crop yield is obviously increased, and mulch film has become indispensable producer goods in agricultural gradually.
Meanwhile, mulch film remains and is also on the rise to the pollution of soil, because commonly lepthymenia being difficult to reclaims, within 100 years in soil, also do not degrade, use through accumulation for many years, in soil, mulch film residual quantity gets more and more, according to statistics, in Cotton Fields in Xinjiang mulch film residual quantity up to 17.5-39.8kg/ mu." white pollution " in soil makes soil compaction, poor air permeability, and liquid manure circulation is poor, root system development is poor, affects Crop moisture content nutrient, and planting seed to mulch film relic also cannot germinate, if can not administer Plastic-film pollution problem in time, our soil can not have been planted soon.
Have a lot about the report of degradative plastic film in document in the past, can be much almost all utilize common plastics LDPE or PVAC polyvinylalcohol, add starch, calcium carbonate or photosensitizers, it is made to become fragment, reach the object of " disintegration ", instead of real degraded, the fragment of this disintegration is still common plastics, and the pollution of fragment to soil is even more serious.We know, starch molecule amount chain has a large amount of hydroxyls, is the good material of a kind of wetting ability, even if pass through modified method, by starch upper part hydroxy esterification or etherificate, but a large amount of hydroxyls still makes it have good water absorbability, and starch and resin alloy blown film, can micropore be there is in film microcosmic, therefore, add starch, not only can affect thin-film transparent, also can reduce its water-retentivity.
Simultaneously, polyvinyl alcohol (PVA) is a kind of water-soluble material, and the biodegradable material of really, good consistency is had with starch, water, glycerine, a lot of people often utilizes its water-soluble and good with starch consistency feature, by PVA and starch blending film forming, thinks that it is exactly complete biodegradable, in fact really not so, and this film is more difficult to ensure the good water-retentivity of card.
The LDPE(MG70 of 3-4.2% is added respectively in the degradative plastic film that CN101812187A and CN101831097A, CN101828495A propose) and 30-65%LDPE(7042).Also 10-20% polyethylene, 10-20% polypropylene, 2-3% polyvinyl alcohol is added in the degradative plastic film of CN102850626A report.The polyvinyl alcohol of 5-2% and 25-35% is added respectively in the degradative plastic film of CN1197091 and CN103289132A report.CN1260115 reports a kind of containing agricultural chemicals Clomazone and the polyethylene ground film of slaughtering green bristlegrass amine.The degradative plastic film of CN103242561A, CN101280116, CN101589681 and CN101362862 report is all be membrane-forming agent with polyvinyl alcohol, adds the blended film forming such as starch.The degradative plastic film of CN102964669A and CN102660068A report is respectively containing 95-99% and 98.3-99.77% linear low density polyethylene LLDPE7042.The degradative plastic film that CN102599030A mentions with common not degradative plasticss such as acrylic ester emulsion, silicone fluid or urethane for carrier.
CN170395 report mulch film with waste and old cotton, cotton, waste paper, cardboard etc. for raw material, the mulch film that CN101884292A and CN101712805A mentions with powdery soil, black humic acid powder for raw material, carry out pulverizing mixing roll mixing after make and be pressed into mulch film, although this mulch film is complete biodegradable, can production method is difficult, poor repeatability, the transparency is poor, heat retaining property and poor water retention property, and degradation rate is difficult to control, and is difficult to spread.The degradative plastic film that it is raw material that although CN101565514 and CN102475046A reports with treated starch or thermoplastic starch, degradable polymer or poly-alkyl fatty acid ester (PHA) respectively, but degradable polymer is not described further in claims, and take starch as the mulch film of main raw, the same existence transparency is poor, heat retaining property and the shortcoming such as poor water retention property, the difficult control of degradation rate, is difficult to popularization.
At present, general biological degradation standard is EN13432 and ASTM D6400, meet these degraded standards, biodegradable material has poly terephthalic acid-hexanodioic acid-butanediol ester (PBAT), poly(lactic acid) (PLA), PHA (PHAs), carbon dioxide copolymer (PPC) etc.Utilize biodegradable plastic to substitute traditional PE and PVA material, be prepared into the mulch film of complete biodegradable, the problem of white pollution in farmland can be solved, be significant.
Have 4 requirements to film material in prior art: the first, snappiness is good, can have certain tensile deformation in plastic film mulch process; The second, intensity is good, and can not break in plastic film mulch process film; 3rd, water vapor transmittance is low, is beneficial to moisturizing; 4th, good heat preservation performance.
The biodegradable material of single variety is difficult to the performance requriements meeting mulch film, and therefore, we have carried out formulating of recipe to mulch film, to meet various index demand.
First, in order to reach the mechanical property requirements close with PE, can ensure the snappiness of mulch film, can ensure ground film strength again, we select flexible degraded polyester and rigidity degraded polyester to carry out composite modified.
Secondly, in order to improve consistency between differing materials, we have selected oxazoline compounds is compatilizer, this compounds and carboxyl have very high reactive behavior, and we degrade, the content of carboxyl end group of polyester material is higher, and end carboxyl can accelerate again the degradation with aging of material, and the introducing of oxazoline compounds not only can improve the consistency of storeroom, termination process can also be carried out to end carboxyl simultaneously, improve its resistance of aging.
Moreover, we find to add layered inorganic compound in system, the soil moisture can be significantly improved, in order to ensure the heat retaining property of mulch film excellence, we have selected the lamellar compound such as hydrotalcite, mica powder as heat preserving agent, in order to not affect the transmittance of film, the particle diameter of heat preserving agent is enough little, more than order number 3000 order.
Finally, the water vapor transmittance of degraded polyester material is higher, and the water vapor transmittance of such as PBST is 170g/m
2* d(film thickness: 0.05mm), the water vapor transmittance of PLA is 90g/m
2* d(film thickness: 0.05mm), and the water vapor transmittance of PE is only 1.7g/m
2* d(film thickness: 0.05mm), the water vapor transmittance of PBAT is 100 times of PE, and therefore, we introduce wetting Agent for Printing Inks in system, substantially improve the moisture retention of film.
The present invention has following beneficial effect:
Biodegradable mulch of the present invention, not containing any non-biodegradable common plastics, not starch-containing yet, can on common LDPE inflation film manufacturing machine Blown Film, without the need to carrying out any transformation to equipment, this mulch film transparency is good, and snappiness is good, intensity is high, water vapor transmittance is low, is beneficial to moisturizing and good heat preservation performance.
Summary of the invention
The object of this invention is to provide a kind of Polyester full-biodegradable mulch film, this mulch film transparency, heat retaining property and good water-retaining property, can complete biodegradable.
Polyester full-biodegradable mulch film of the present invention, be made up of the raw material of following mass percent:
40-80% flexibility degraded polyester, the degraded of 10-55% rigidity polyester, 0.5-1.5% reactive compatibilizer, 1-2% heat preserving agent, 1-2% wetting Agent for Printing Inks, 0.5-1.5% antiager, 0.5-1% slipping agent and 0.5-3% opening agent.
Elongation at break >=100% of described flexibility degraded polyester, comprises one or more in poly terephthalic acid-succinic acid-butanediol ester (PBST), poly-succinic-butanediol ester (PBS), poly-succinic-hexanodioic acid-butanediol ester (PBSA).
The elongation at break < 100% of described rigidity degraded polyester, comprises one or more in poly(lactic acid) (PLA), polyglycolic acid (PGA), polyhydroxybutyrate-valeric acid copolyesters (PHBV).
Described reactive compatibilizer is oxazoline compounds, preferred 2-methyl-2-oxazoline, 2-ethyl-2-oxazoline, 2,2'-(1,3-phenylene)-bisoxazoline, 4,4-dimethyl oxazoline quinoline, 2-ethyl-4,4-dimethyl-2-oxazoline, 2-phenyl-4,4-dimethyl-2-oxazoline, 2,2 '-bis-(2-oxazoline), 2,2'-isopropyl subunit two (4-phenyl-2-oxazoline), 2,2-(Isosorbide-5-Nitrae-phenylene) bisoxazoline or 2,4,5-trimethylammonium-3-oxazoline.
Described heat preserving agent is layered inorganic compound, and be one or more in hydrotalcite, polynite or mica powder, order number is 3000-10000 order.
Described wetting Agent for Printing Inks is sodium cellulose glycolate, Xylo-Mucine, Vltra tears sodium or sodium starch glycolate.
Described antiager is the mixture of oxidation inhibitor, UV light absorber and photostabilizer, and the mass ratio of three is 0.5-2:0.5-2:1.
Described oxidation inhibitor is that Hinered phenols antioxidant and phosphite ester kind antioxidant are according to mass ratio 1:1 mixture;
Hinered phenols antioxidant: mainly comprise 1010(tetra-[β-(3, 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester), 1076(β-(3, 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid), 1024(N, N '-bis-[β-(3, 5-di-tert-butyl-hydroxy phenyl) propionyl] hydrazine), 1098(N, N'-pair-(3-(3, 5-di-tert-butyl-hydroxy phenyl) propionyl) hexanediamine), 245(Triethylene glycol two [β-(3-tertiary butyl-4-hydroxy-5-aminomethyl phenyl) propionic ester]), 3114(1, 3, 5-tri-(3, 5-di-tert-butyl-4-hydroxyl benzyl) tricarbimide), 1135(β-(3, 5-di-tert-butyl-hydroxy phenyl) propionic acid isooctyl alcohol ester), 1330(1, 3, 5-trimethylammonium-2, 4, 6-(3, 5-di-t-butyl-4-hydroxyphenylmethyl) benzene), 1520(2, 4-bis-(n-octylthiomethylene)-6-methylphenol),
Phosphite ester kind antioxidant: mainly comprise trimethyl phosphite 99, triethyl phosphate, tributyl phosphate, triphenylphosphate, trimethyl phosphite, triethyl-phosphite, triisopropyl phosphite, triphenyl phosphite, 168(tri-[2.4-di-tert-butyl-phenyl] phosphorous acid ester), two (2,4-DTBP) pentaerythritol diphosphites of 626().
Described UV light absorber is benzophenone or phenylpropyl alcohol triazole class;
Benzophenone: mainly comprise UV-O(2,4-dihydroxy benaophenonel), UV-9(2-hydroxyl-4-methoxy benzophenone), UV-531(2-hydroxyl-4-oxy-octyl benzophenone);
Phenylpropyl alcohol triazole class: mainly comprise UV-P(2-(2 ˊ-hydroxyl-5 ˊ-aminomethyl phenyl) benzotriazole), UV-326(2-(the 2'-hydroxyl-3'-tertiary butyl-5'-aminomethyl phenyl)-5-chlorinated benzotriazole), UV-327(2-(2 '-hydroxyl-3 ', 5 '-two tertiary phenyl)-5-chlorination benzotriazole), UV-328(2-[2-hydroxyl-3, 5-bis-(1, 1-dimethyl propyl phenyl)]-2H-benzotriazole), UV-329(2-(the special octyl phenyl of 2'-hydroxyl-5'-) benzotriazole), UV-360(2, 2'-methylene-bis (the tertiary octyl group of 4--6-benzotriazole phenol)), UV-234(2-(2'-hydroxyl-3', two (a of 5', a-dimethyl benzyl) phenyl) benzotriazole).
Described photostabilizer mainly comprises 622(succinic acid and (4-hydroxyl-2, the polymkeric substance of 2,6,6-tetramethyl--1-piperidine alcohols)), 770(two (2,2,6,6-tetramethyl--4-piperidyl) sebate), the poly-[[6-[(1,1 of 944(, 3,3-tetramethyl butyl) amine]-1,3,5-triazines-2,4-bis-base] [(2,2,6,6-tetramethyl--4-piperidines) imines]-1,6-bis-dihexyl [(2,2,6,6-tetramethyl--4-piperidines) imines]]).
Described slipping agent is one or more in stearates, organic carboxyl acid amides or wax class;
Stearates is: calcium stearate, Magnesium Stearate, Zinic stearas, barium stearate;
Organic carboxyl acid amides is: erucicamide, amine hydroxybenzene, N, N-ethylene bis stearamide;
Wax class is: polyethylene wax, oxidized polyethlene wax, paraffin;
Described opening agent is: the one in silicon-dioxide, talcum powder, calcium carbonate, silicon whisker, magnesium oxide, aluminium hydroxide or magnesium hydroxide, and order number is 1000-10000 order.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
For the ease of the insulation of contrast mulch film and moisture retention, we are with PE mulch film for reference, and PE mulch film and Biodegradable mulch blowing thickness of the present invention are 0.01mm, carry out the experiment of same field, the temperature that after test plastic film mulch 24h, soil 10cm is dark, and the water vapor transmittance of film.The water vapor transmittance of PE mulch film is 10.5g/m
2* the temperature that after d, PE mulch film plastic film mulch 24h, soil 10cm is dark is 14.1 DEG C.In embodiment, melting means unit is g/10min, test condition: 190 DEG C, 2.16kg.
Embodiment 1
By 40%PBST(fusing point 110-120 DEG C, melting means: 3.8), 55%PLA(fusing point 160-170 DEG C, melting means: 4.0), 0.5%2, 2 '-bis-(2-oxazoline), 1% hydrotalcite (3000 order), 1% sodium cellulose glycolate, 1.5% antiager [0.5% compound antioxidant (1010 and 168), 0.5% UV light absorber UV-328, 0.5% photostabilizer 622], 0.5% slipping agent (0.3%N, N-ethylene bis stearamide, 0.2% amine hydroxybenzene), 0.5% silicon-dioxide (10000 order), join successively in high-speed mixer, after mixing, join further plasticizing extruding pelletization in length-to-diameter ratio 48 equidirectional parallel double-screw extruder and obtain complete biodegradable film material, further blown film again, thickness 0.01mm, water vapor transmittance is 13.2g/m
2* d, the temperature that after plastic film mulch 24h, soil 10cm is dark is 14.9 DEG C.
Embodiment 2
By 80%PBS(fusing point: 110-120 DEG C, melting means: 5.0), 10%PGA(fusing point 170-180 DEG C, melting means: 4.5), 1.5%2, 2'-(1, 3-phenylene)-bisoxazoline, 2% mica powder (5000 order), 2% Vltra tears sodium, 0.5% antiager [0.2% compound antioxidant (1024 and 626), 0.2% Ultraviolet Absorber UV-P, 0.1% photostabilizer 770], 1% slipping agent (0.5% erucicamide and 0.5% oxidation PE wax), 3% talcum powder (1000 order), join successively in high-speed mixer, after mixing, join further plasticizing extruding pelletization in length-to-diameter ratio 48 equidirectional parallel double-screw extruder and obtain complete biodegradable film material, further blown film again, thickness 0.01mm, water vapor transmittance is 9.8g/m
2* d, the temperature that after plastic film mulch 24h, soil 10cm is dark is 17.4 DEG C.
Embodiment 3
By 70%PBSA(fusing point: 100-110 DEG C, melting means: 2.8), 22%PHBV(fusing point 165-175 DEG C, melting means: 5.3), 1%4, 4-dimethyl oxazoline quinoline, 1.5% polynite (10000 order), 1.5% Xylo-Mucine, 1% antiager [0.4% compound antioxidant (1076 and 168), 0.3% UV light absorber UV-9, 0.3% photostabilizer 944], 0.8% slipping agent (0.3% Zinic stearas and 0.5%PE wax), 2.2% calcium carbonate (5000 order), join successively in high-speed mixer, after mixing, join further plasticizing extruding pelletization in length-to-diameter ratio 48 equidirectional parallel double-screw extruder and obtain complete biodegradable film material, further blown film again, thickness 0.01mm, water vapor transmittance is 11.9g/m
2* d, the temperature that after plastic film mulch 24h, soil 10cm is dark is 15.4 DEG C.
Embodiment 4
By 62%PBST(fusing point 120-130 DEG C, melting means: 4.4), 30%PHBV(fusing point 155-165 DEG C, melting means: 3.1), 1.2%2, 2-(1, 4-phenylene) bisoxazoline, 1.3% mica powder (3000 order), 1.3% Vltra tears sodium, 1.2% antiager [0.4% compound antioxidant (1098 and 168), 0.4% ultraviolet absorbent UV-531, 0.4% photostabilizer 622], 0.5% slipping agent (0.5% Zinic stearas), 2.5% silicon whisker (6000 order), join successively in high-speed mixer, after mixing, join further plasticizing extruding pelletization in length-to-diameter ratio 48 equidirectional parallel double-screw extruder and obtain complete biodegradable film material, further blown film again, thickness 0.01mm, water vapor transmittance is 10.7g/m
2* d, the temperature that after plastic film mulch 24h, soil 10cm is dark is 16.1 DEG C.
Embodiment 5
By 55%PBSA(fusing point 80-90 DEG C, melting means: 3.9), 38%PLA(fusing point 150-160 DEG C, melting means: 4.2), 1%2, 2'-isopropyl subunit two (4-phenyl-2-oxazoline), 1% hydrotalcite (5000 order), 1% sodium starch glycolate, 1% antiager [0.7% compound antioxidant (1010 and 626), 0.7% ultraviolet absorbent uv-326, 0.8% photostabilizer 770], 1% lubricant (0.5% Magnesium Stearate, 0.5%N, N-ethylene bis stearamide), 2% silicon-dioxide (5000 order), join successively in high-speed mixer, after mixing, join further plasticizing extruding pelletization in length-to-diameter ratio 48 equidirectional parallel double-screw extruder and obtain complete biodegradable film material, further blown film again, thickness 0.01mm, water vapor transmittance is 10.2g/m
2* d, the temperature that after plastic film mulch 24h, soil 10cm is dark is 14.5 DEG C.
Claims (7)
1. a Polyester full-biodegradable mulch film, is characterized in that being made up of the raw material of following mass percent:
40-80% flexibility degraded polyester, the degraded of 10-55% rigidity polyester, 0.5-1.5% reactive compatibilizer, 1-2% heat preserving agent, 1-2% wetting Agent for Printing Inks, 0.5-1.5% antiager, 0.5-1% slipping agent and 0.5-3% opening agent;
Elongation at break >=100% of described flexibility degraded polyester is one or more in poly terephthalic acid-succinic acid-butanediol ester, poly-succinic-butanediol ester or poly-succinic-hexanodioic acid-butanediol ester;
The elongation at break < 100% of described rigidity degraded polyester is one or more in poly(lactic acid), polyglycolic acid or polyhydroxybutyrate-valeric acid copolyesters;
Described reactive compatibilizer is oxazoline compounds.
2. Polyester full-biodegradable mulch film according to claim 1, it is characterized in that: Suo Shu oxazoline compounds is 2-methyl-2-oxazoline, 2-ethyl-2-oxazoline, 2,2'-(1,3-phenylene)-bisoxazolines, 4,4-bis-Jia oxazolin, 2-ethyl-4,4-dimethyl-2-oxazoline, 2-phenyl-4,4-dimethyl-2-oxazoline, 2,2 '-bis-(2-oxazoline), 2,2'-isopropyl subunit two (4-phenyl-2-oxazoline), 2,2-(Isosorbide-5-Nitrae-phenylene) bisoxazolines or 2,4,5-trimethylammonium-3-oxazoline.
3. Polyester full-biodegradable mulch film according to claim 1, is characterized in that: described heat preserving agent is layered inorganic compound, and be one or more in hydrotalcite, polynite or mica powder, order number is 3000-10000 order.
4. Polyester full-biodegradable mulch film according to claim 1, is characterized in that: described wetting Agent for Printing Inks is sodium cellulose glycolate, Xylo-Mucine, Vltra tears sodium or sodium starch glycolate.
5. Polyester full-biodegradable mulch film according to claim 1, is characterized in that: described antiager is the mixture of oxidation inhibitor, UV light absorber and photostabilizer, and the mass ratio of three is 0.5-2:0.5-2:1.
6. Polyester full-biodegradable mulch film according to claim 5, is characterized in that:
(1) oxidation inhibitor described in is that Hinered phenols antioxidant and phosphite ester kind antioxidant are according to mass ratio 1:1 mixture;
Hinered phenols antioxidant is: 1010,1076,1024,1098,245,3114,1135,1330,1520;
Phosphite ester kind antioxidant is: trimethyl phosphite 99, triethyl phosphate, tributyl phosphate, triphenylphosphate, trimethyl phosphite, triethyl-phosphite, triisopropyl phosphite, triphenyl phosphite, three [2.4-di-tert-butyl-phenyl] phosphorous acid ester, two (2,4-DTBP) pentaerythritol diphosphites;
(2) UV light absorber described in is benzophenone or phenylpropyl alcohol triazole class;
Benzophenone is: UV-O, UV-9, UV-531;
Phenylpropyl alcohol triazole class is: UV-P, UV-326, UV-327, UV-328, UV-329, UV-360, UV-234;
(3) photostabilizer described in is 622,770,944.
7. Polyester full-biodegradable mulch film according to claim 1, is characterized in that:
Described slipping agent is one or more in stearates, organic carboxyl acid amides or wax class;
Stearates is: calcium stearate, Magnesium Stearate, Zinic stearas, barium stearate;
Organic carboxyl acid amides is: erucicamide, amine hydroxybenzene, N, N-ethylene bis stearamide;
Wax class is: polyethylene wax, oxidized polyethlene wax, paraffin;
Described opening agent is: the one in silicon-dioxide, talcum powder, calcium carbonate, silicon whisker, magnesium oxide, aluminium hydroxide or magnesium hydroxide, and order number is 1000-10000 order.
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