CN102604164A - Master batch capable of fully and biologically degrading plastic film and preparation method thereof - Google Patents
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Abstract
The invention discloses a master batch capable of fully and biologically degrading a plastic film and a preparation method thereof, and belongs to the field of high molecular films. The formula of the master batch comprises the following materials in parts by weight: 100 parts of starch, 2-9 parts of coupling agent, 8-18 parts of dispersing agent, 8-25 parts of polycyclolactone, 1-50 parts of polylactic acid, 8-15 parts of poly (hydroxybutyrate-hydroxyvalerate) (PHBV), 10-25 parts of plasticizer, 0.15-1.0 part of anti-tackiness agent, 0.15-1.2 parts of pro-oxidant and 1-15 parts of chemical precipitation promoter. The preparation method of the master batch comprises the three steps of: thinning the starch; mixing; and forming. The product provided by the invention has the advantages of high starch content, being a fast-growing and renewable resource, rich resource, low unit cost, high substitutability, obvious economic benefit and ecological benefit and capabilities of reducing the content of polycyclolactone, increasing polylactic acid and poly (hydroxybutyrate-hydroxyvalerate) (PHBV), improving product performance and meanwhile reducing cost.
Description
Technical field
The invention belongs to the polymeric membrane technical field, particularly relate to masterbatch prescription of a kind of fully biodegradable plastic film and preparation method thereof.
Background technology
Known degradable plastics material, because of containing polyolefine compositions such as Vilaterm, Vestolen PP 7052, the degraded of consequently discarded back is not thorough, and " white pollution " problem is solved fully, and plastic garbages a large amount of in the life have caused very big pressure to environment.
In recent years; Documents and materials such as " characteristic introduction of pla-pcl and application prospect thereof ", " production technology research of bio-based degradable plastics POLYACTIC ACID ", " collection of thesis of the 3rd special commission of degradative plastics of association is moulded by China ", " mikrobe synthesizing polyhydroxyalkanoateby polymer masterbatch ", " biolysis plastics and bio-based plastics " disclose: what have ester group gathers the cyclic lactone plastic matrix as gathering NSC 403079, pla-pcl, polyhydroxyalkanoate etc.; Can be degraded rapidly by the enzyme of microorganism secretion, ester group-O on its main chain-C-can rupture rapidly generates carbonic acid gas and water reaches complete biodegradable.But the unit cost of production high (5-6 dollars/kilograms) and right and wrong speed production-goods source because of this type masterbatch are difficult to promote on market.And containing the influence that the plastics that gather cyclic lactone are filled a prescription because of the controllability of degradative plastics, mechanical strength is different with characteristics such as chemical oil-proofness, weather resistance, thermotolerances.
Summary of the invention
The object of the invention aims to provide plastic film masterbatch of the lower fully biodegradable of a kind of unit cost of production and preparation method thereof.
Technical scheme of the present invention: a kind of masterbatch of fully biodegradable plastic film, its prescription (by weight) is: 100 parts of starch, coupling agent 2-9 part; Dispersion agent 8-18 part is gathered cyclic lactone 8-25 part, POLYACTIC ACID 1-50 part; Polyhydroxybutyrate valeric acid copolyesters (PHBV) 8-15 part, softening agent 10-25 part, anticaking agent 0.15-1.0 part; Pro-oxidant 0.15-1.2 part, chemical degradation accelerating agent 1-15 part.
Said coupling agent is aluminic acid ester or vulcabond;
Said dispersion agent is glycerine, Semen Maydis oil or white oil;
The said cyclic lactone that gathers is the cyclic lactone that gathers that the repeating unit chain link is short in the molecular structure, rigidity is big, hardness is high when preparing the engineering plastics masterbatch of fully biodegradable, is preferably and gathers NSC 403079 or polylactide.
The said cyclic lactone that gathers is the cyclic lactone that gathers that the repeating unit chain link is long, flexible greatly in the molecular structure, toughness is strong when preparing the plastic film masterbatch of fully biodegradable, is preferably polycaprolactone or poly-hydroxy fatty acid, is preferably and gathers β-hydroxyl butyl ester.
Said softening agent is silane-modified low-molecular-weight wax (CH-PA) or ethene-vinyl acetate between to for plastic copolymerization (EVA) low-molecular-weight wax;
Said pro-oxidant is low thermal oxidation agent or unsaturated fatty acids;
The hydroxy acid salt that said chemical degradation accelerating agent is a transition metal;
Said anticaking agent is sodium silicoaluminate or silicon-dioxide etc.
With starch is main raw, and with POLYACTIC ACID (PLA), polyhydroxybutyrate valeric acid copolyesters biodegradable resins such as (PHBV) is the formula system of auxiliary material, good, the bio-based full degradable membrane cheaply of preparation use properties.
With starch is main raw, is the biolysis goods of auxiliary material with polyhydroxybutyrate valeric acid copolyesters (PHBV), POLYACTIC ACID biodegradable resins such as (PLA).Starch is a kind of renewable resources, and easy processing makes, and low price also is one of main carbon source of mikrobe utilization, because starch has good film-forming properties, therefore, has selected the main raw material of starch as full degradable membrane in the bio-based full degradable membrane production process again.The plastics that the characteristic of POLYACTIC ACID has determined to add POLYACTIC ACID (PLA) have the intensity more superior than general plastics, transparency reaches the resistivity to climate change.Polyhydroxybutyrate valeric acid copolyesters (PHBV) then has excellent biological compatibility, biological degradation and Bioabsorbable performance, and PHBV resin physicals and PP are close, and consistency is good, and fusing point is low, is unusual ideal thermoplastic material.In order to make the film series products that use properties and lower production cost preferably arranged, we have carried out composite use.PHBV etc. are hydrophobic resins, and filler auxiliary agents such as starch are hydroaropic substances, in order to improve mixed effect, add relevant coupling agent etc. and technologic innovation through the prescription innovation, solve the compatibility problem of various materials.Only adopt the obtained material of above-mentioned prescription, also exist the product tensile property poor, be prone to characteristics such as crisp; POLYACTIC ACID and a kind of biodegradable softening agent of a small amount of interpolation; Can effectively improve materials processed and request for utilization, and select suitable crosslinking agent for use, to improve the water resistance of film.
Polyhydroxybutyrate valeric acid copolyesters (PHBV), POLYACTIC ACID (PLA) obtain through raw material biological fermentations such as starch in the bio-based degradative membrane raw materials for production; Compare raw material PP, PE, PS, the PVC of other Plastic Packaging Materials; Can reduce the dependence that the petroleum by-product resource is used, meet the construction trend of current conservation-minded society.Simultaneously, can cross biolysis during product abandonment and can be decomposed into carbonic acid gas and water fully, realize circular form production.
In the above-mentioned composition of fully biodegradable plastic matrix of the present invention, adding softening agent, dispersion agent are the plasticization temperatures that gathers cyclic lactone in order to reduce, and make it and the mixing preferably combination of starch.
In the above-mentioned composition of fully biodegradable plastic matrix of the present invention; Because it is hydrophilic radical that three hydroxyls are arranged on the starch molecule chain link; Just only such group is arranged and gather cyclic lactone,, carries out modification so also need add coupling agent for the two can be good at combining at last-of-chain.
The preparation method of fully biodegradable plastic matrix of the present invention may further comprise the steps:
(1) starch refinement; Dehydration: 1. starch, water, anticaking agent are mixed, stir pulping; Pour that refinement 20-30min is 1-10 μ m to the starch granules particle diameter in the sand milling dispersion machine into, refining temperature is controlled at 40-60 ℃, and the farinaceous size of preliminary refinement is dewatered through the ultra-filtration membrane unit; 2. the starch after will dewatering is for the first time mixing, is stirring pulping with glycerine or Semen Maydis oil; Pour in the sand milling dispersion machine refinement 40-50min once more into to starch granules particle diameter＜1 μ m; Refining temperature is controlled at 50-70 ℃, and the farinaceous size of secondary refinement is dewatered to starch water cut＜0.5% through the ultrafiltration unit; Starch behind the second dehydration placed make oil-bound distemper in the whizzer and separate in right amount; 3. with step 2. gained starch and coupling agent pour into and mediate modification 20-30min in the high speed kneader, make modified starch 1;
(2) mixing: as once to add in the modified starch 1 that in step 1, makes: gather cyclic lactone, POLYACTIC ACID, polyhydroxybutyrate valeric acid copolyesters (PHBV), softening agent, dispersion agent, pro-oxidant, chemistry short fall to mediate plasticate, the kneading time is 20-30min;
(3) moulding: the obtained material of step 2 is placed the granulation of the double gas extruding pelletization of twin screw unit, obtain required plastic matrix.
In the preparing method's of above-mentioned fully biodegradable plastic matrix forming step (3), can also after granulation, increase to vacuumize and pack step, to guarantee product stock, unlikely the becoming damp and rotten of transportation, guarantee that the finished product handling ease of ultimate product is carried out.
When preparing the film class plastic matrix of fully biodegradable, above-mentioned steps (3) mold temperature is controlled at 80-120 ℃, and (unit is 80 ℃ for 1 group, and 2 groups is 88 ℃, and 3 groups is 93 ℃; 4 groups is 98 ℃, and 5 groups is 105 ℃, and 6 groups is 112 ℃; 7 groups is 118 ℃, and 8 groups is 120 ℃, and head is 115 ℃).
The said extruding pelletization unit of step (3) is the double gas extruding pelletization of a twin screw unit.Select for use twin screw exhaust extruding pelletization unit mainly to be because: gather on the molecular structure of cyclic lactone and starch and all contain great amount of hydroxy group; Adsorbed water molecule very easily, and extrude through twin-screw mixer, then can make the two fusion well, combine; Form inierpeneirating network structure; Then can water molecules be removed totally effectively through double depressed structure again,, help the processing of ultimate product so that obtain dry article.
Above-mentioned all the other processes are generally necessary process, have no special requirements.
In the preparation method of fully biodegradable plastic matrix of the present invention; The starch refinement is because the particle diameter of starch commonly used big (20-150 μ m); Be unfavorable for that starch combines with gathering cyclic lactone; So below refinement starch to the 1 μ m, reaching increases it with the purpose of gathering cyclic lactone bonded surface-area, so that it combines with gathering cyclic lactone better.
In the preparation method of fully biodegradable plastic matrix of the present invention, because of starch contains a large amount of hydrophilic radicals, water cut is higher, is unfavorable for product molding, and for this reason, the dehydration of starch is most important.
Adopt the advantage of the fully biodegradable plastic matrix that preparation method of the present invention makes to be: use discarded after; Because of absolutely being degraded rapidly at short notice by the enzyme of microorganism secretion; All change into water and carbonic acid gas, thereby real the realization eliminated " white pollution ", assimilates with environment; Play ecological protection effect preferably, ensured agricultural sustainable development; Because of the component content height of starch at goods according to the invention; And starch is cheap, makes the unit cost of goods according to the invention low, and the existing cyclic lactone plastic matrix cost that gathers reduces more than 3-4 times; Again because starch is that speed is given birth to, renewable resources; Aboundresources makes the substitutability of goods according to the invention good, has remarkable economic efficiency and ecological benefits; Reduce the content, increase POLYACTIC ACID and the polyhydroxybutyrate valeric acid copolyesters (PHBV) that gather cyclic lactone and can improve performance of products, reduced cost simultaneously.
Embodiment
Below will describe implementation process of the present invention in detail with the mode of embodiment.In following each embodiment, like no special declaration, the mark of said component is weight part, and every weight part is 1kg.
Embodiment 1: in SK80-2A sand milling dispersion machine refinement is poured 100 parts of starch, 150 parts in water, 0.25 part of mixing of anticaking agent, stirring pulping in (1), and the refinement time is that 20-30min is 1-10 μ m to the starch granules particle diameter, and refining temperature is controlled at 40-60 ℃; (2) farinaceous size with preliminary refinement dewaters through HDZC-006-1 ultra-filtration membrane unit; (3) starch after will dewatering for the first time and glycerine or 100 parts of remix of Semen Maydis oil, stir pulping, pour refinement in the aforementioned sand milling dispersion machine once more into, the refinement time be 40-50min to starch granules particle diameter＜1 μ m, refining temperature is controlled at 50-79 ℃; (4) farinaceous size with the secondary refinement dewaters to starch water cut＜0.5% through aforementioned ultra-filtration membrane unit; (5) starch behind the second dehydration is placed make oil-bound distemper in the GKH1250-N whizzer and separate in right amount; (6) pour starch that makes in the step (5) and coupling agent in GL500/1600 high speed kneader kneading modification 20-30min for 4 parts; (7) add successively again and gather 25 parts of NSC 403079s, 25 parts of POLYACTIC ACIDs, 8 parts of polyhydroxybutyrate valeric acid copolyesters, 11 parts in softening agent, 8 parts of dispersion agents, 0.15 part of pro-oxidant, 5 parts of chemical degradation accelerating agents, kneading is plasticated, and the time is 20-30min; (8) the obtained material of step (7) is placed the granulation of the double gas extruding pelletization of twin screw unit, extrusion temperature is controlled at 130-160 ℃, and (unit is 125 ℃ for 1 group, and 2 groups is 130 ℃; 3 groups is 140 ℃, and 4 groups is 145 ℃, and 5 groups is 150 ℃; 6 groups is 155 ℃, and 7 groups is 160 ℃, and head is 165 ℃); The gained pellet vacuumizes sealing, and this pellet can be used for preparing fully biodegradable mulch film plastics.
Embodiment 2: in SK80-2A sand milling dispersion machine refinement is poured 100 parts of starch, 150 parts in water, 0.5 part of mixing of anticaking agent, stirring pulping in (1), and the refinement time is that 20-30min is 1-10 μ m to the starch granules particle diameter, and refining temperature is controlled at 40-60 ℃; (2) farinaceous size with preliminary refinement dewaters through HDZC-006-1 ultra-filtration membrane unit; (3) starch after will dewatering for the first time and glycerine or 100 parts of remix of Semen Maydis oil, stir pulping, pour refinement in the aforementioned sand milling dispersion machine once more into, the refinement time be 40-50min to starch granules particle diameter＜1 μ m, refining temperature is controlled at 50-79 ℃; (4) farinaceous size with the secondary refinement dewaters to starch water cut＜0.5% through aforementioned ultra-filtration membrane unit; (5) starch behind the second dehydration is placed make oil-bound distemper in the GKH1250-N whizzer and separate in right amount; (6) pour starch that makes in the step (5) and coupling agent in GL500/1600 high speed kneader kneading modification 20-30min for 4 parts; (7) add 18 parts of polylactides more successively, 28 parts of POLYACTIC ACIDs, 8 parts of polyhydroxybutyrate valeric acid copolyesters, 10 parts in softening agent, 8 parts of dispersion agents, 0.5 part of pro-oxidant, 8 parts of chemical degradation accelerating agents, kneading is plasticated, and the time is 20-30min; (8) the obtained material of step (7) is placed the granulation of the double gas extruding pelletization of twin screw unit, extrusion temperature is controlled at 130-160 ℃, and (unit is 125 ℃ for 1 group, and 2 groups is 130 ℃; 3 groups is 140 ℃, and 4 groups is 145 ℃, and 5 groups is 150 ℃; 6 groups is 155 ℃, and 7 groups is 160 ℃, and head is 165 ℃); The gained pellet vacuumizes sealing, and this pellet can be used for preparing fully biodegradable mulch film plastics.
Embodiment 3: in SK80-2A sand milling dispersion machine refinement is poured 100 parts of starch, 180 parts in water, 1 part of mixing of anticaking agent, stirring pulping in (1), and the refinement time is that 20-30min is 1-10 μ m to the starch granules particle diameter, and refining temperature is controlled at 40-60 ℃; (2) farinaceous size with preliminary refinement dewaters through HDZC-006-1 ultra-filtration membrane unit; (3) starch after will dewatering for the first time and glycerine or 100 parts of remix of Semen Maydis oil, stir pulping, pour refinement in the aforementioned sand milling dispersion machine once more into, the refinement time be 40-50min to starch granules particle diameter＜1 μ m, refining temperature is controlled at 50-79 ℃; (4) farinaceous size with the secondary refinement dewaters to starch water cut＜0.5% through aforementioned ultra-filtration membrane unit; (5) starch behind the second dehydration is placed make oil-bound distemper in the GKH1250-N whizzer and separate in right amount; ⑹ pour starch that makes among the step ⑸ and coupling agent in GL500/1600 high speed kneader kneading modification 20-30min for 8 parts; ⑺ pour 15 parts of pla-pcls, 50 parts of POLYACTIC ACIDs, 12 parts of polyhydroxybutyrate valeric acid copolyesters, 13 parts in softening agent, 10 parts of dispersion agents, 0.25 part of pro-oxidant more successively into, 10 parts of chemical degradation accelerating agents, and kneading is plasticated, and the time is 20-30min; ⑻ place the granulation of extruding pelletization unit with the obtained material of step ⑺, and extrusion temperature is controlled at 105-120 ℃, and (unit is 105 ℃ for 1 group, and 2 groups is 110 ℃; 3 groups is 110 ℃, and 4 groups is 115 ℃, and 5 groups is 115 ℃; 6 groups is 105 ℃, and 7 groups is 105 ℃, and 8 groups is 120 ℃; Head is 120 ℃), the gained pellet vacuumizes sealing, and this pellet can be used for preparing the fully-biodegradable film plastics.
Embodiment 4: with 100 parts of starch, 200 parts in water, 0.8 part of mixing of anticaking agent, stirring pulping, pour refinement in the SK80-2A sand milling dispersion machine into, the refinement time is that 20-30min is 1-10 μ m to the starch granules particle diameter, and refining temperature is controlled at 40-60 ℃; ⑵ dewater the farinaceous size of preliminary refinement through HDZC-006-1 ultra-filtration membrane unit; ⑶ starch after will dewater for the first time and glycerine or 100 parts of remix of Semen Maydis oil, stir pulping, pour refinement in the aforementioned sand milling dispersion machine once more into, the refinement time be 40-50min to starch granules particle diameter＜1 μ m, refining temperature is controlled at 50-70 ℃; ⑷ dewater the farinaceous size of secondary refinement to starch water cut＜0.5% through aforementioned ultra-filtration membrane unit; (5) starch behind the second dehydration is placed make oil-bound distemper in the GKH1250-N whizzer and separate in right amount; ⑹ pour starch that makes among the step ⑸ and coupling agent in GL500/1600 high speed kneader kneading modification 20-30min for 9 parts; ⑺ pour into successively and gather 10 parts of beta-hydroxy butyl esters, 45 parts of POLYACTIC ACIDs, 15 parts of polyhydroxybutyrate valeric acid copolyesters, 25 parts in softening agent, 18 parts of dispersion agents, 1.2 parts of pro-oxidants, 15 parts of chemical degradation accelerating agents, and kneading is plasticated, and the time is 20-30min; ⑻ place the granulation of extruding pelletization unit with the obtained material of step ⑺, and extrusion temperature is controlled at 105-120 ℃, and (unit is 105 ℃ for 1 group, and 2 groups is 105 ℃; 3 groups is 110 ℃, and 4 groups is 110 ℃, and 5 groups is 115 ℃; 6 groups is 115 ℃, and 7 groups is 105 ℃, and 8 groups is 115 ℃; Head is 120 ℃), the gained pellet vacuumizes sealing, and this pellet can be used for preparing the fully-biodegradable film plastics.
Resulting product degradation property detected result sees the following form.
| Embodiment | Degree of degradation |
| 1 | 85.1 |
| 2 | 86.3 |
| 3 | 89.6 |
| 4 | 91.3 |
Degree of degradation adopts the detection method of ISO14855 to measure: measure the crumble method of experimental technique-Analysis for CO 2 generations of performance of aerobic biological degradation performance and the structure of plastic material under controlled composting conditions.Stipulate among the ISO14855: use the reference material of the Mierocrystalline cellulose of ability complete biodegradable as test plastic material degradation rate, its test experiments is after 85 days, and the biological degradation rate of reference material is degraded fully greater than 80%.
The degradation rate of existing starch-type biodegradable plastic material is lower; National sector standard QB/T2461-1999 (packaging degrading polyethylene film) regulation degradation rate is not less than 20%, and environmental labelling product technical requirements HJBI12-2000 (packing articles) regulation degradation rate is not less than 15%.So the data from above form can find out that plastic matrix of the present invention can be degraded fully.
Claims (7)
1. the masterbatch of a fully biodegradable plastic film, its prescription (by weight) is: 100 parts of starch, coupling agent 2-9 part; Dispersion agent 8-18 part is gathered cyclic lactone 8-25 part, POLYACTIC ACID 1-50 part; Polyhydroxybutyrate valeric acid copolyesters (PHBV) 8-15 part, softening agent 10-25 part, anticaking agent 0.15-1.0 part; Pro-oxidant 0.15-1.2 part, chemical degradation accelerating agent 1-15 part.
2. the masterbatch of a kind of fully biodegradable plastic film according to claim 1 is characterized in that: described coupling agent is aluminic acid ester or vulcabond.
3. the masterbatch of a kind of fully biodegradable plastic film according to claim 1 is characterized in that: described dispersion agent is glycerine, Semen Maydis oil or white oil.
4. the masterbatch of a kind of fully biodegradable plastic film according to claim 1 is characterized in that: described masterbatch is the engineering plastics masterbatch of fully biodegradable, and the described cyclic lactone that gathers is to gather NSC 403079 or polylactide.
5. the masterbatch of a kind of fully biodegradable plastic film according to claim 1 is characterized in that: described masterbatch is the plastic film masterbatch of fully biodegradable, and the described cyclic lactone that gathers is polycaprolactone or poly-hydroxy fatty acid.
6. the masterbatch of a kind of fully biodegradable plastic film according to claim 5 is characterized in that: described poly-hydroxy fatty acid is to gather β-hydroxyl butyl ester.
7. the preparation method of the masterbatch of an a kind of fully biodegradable plastic film as claimed in claim 1 may further comprise the steps:
(1) starch refinement; Dehydration: 1. starch, water, anticaking agent are mixed, stir pulping; Pour that refinement 20-30min is 1-10 μ m to the starch granules particle diameter in the sand milling dispersion machine into, refining temperature is controlled at 40-60 ℃, and the farinaceous size of preliminary refinement is dewatered through the ultra-filtration membrane unit; 2. the starch after will dewatering is for the first time mixing, is stirring pulping with glycerine or Semen Maydis oil; Pour in the sand milling dispersion machine refinement 40-50min once more into to starch granules particle diameter＜1 μ m; Refining temperature is controlled at 50-70 ℃, and the farinaceous size of secondary refinement is dewatered to starch water cut＜0.5% through the ultrafiltration unit; Starch behind the second dehydration placed make oil-bound distemper in the whizzer and separate in right amount; 3. with step 2. gained starch and coupling agent pour into and mediate modification 20-30min in the high speed kneader, make modified starch;
(2) mixing: as once to add in the modified starch that in step (1), makes: gather cyclic lactone, POLYACTIC ACID, polyhydroxybutyrate valeric acid copolyesters (PHBV), softening agent, dispersion agent, pro-oxidant, chemistry short fall to mediate plasticate, the kneading time is 20-30min;
(3) moulding: the obtained material of step (2) is placed the granulation of the double gas extruding pelletization of twin screw unit, obtain required plastic matrix.
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| CN103059146A (en) * | 2013-02-05 | 2013-04-24 | 湘潭大学 | Starch surface treatment process |
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| CN109096713B (en) * | 2018-08-15 | 2020-12-29 | 南京溧水高新创业投资管理有限公司 | Starch compound for agricultural mulching film and preparation method of mulching film for pear in germination period |
| CN110564122A (en) * | 2019-10-23 | 2019-12-13 | 天津科技大学 | novel degradable antibacterial film and preparation thereof |
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Application publication date: 20120725 |