CN106366587A - Preparation method of biodegradable polylactic acid/starch composite - Google Patents
Preparation method of biodegradable polylactic acid/starch composite Download PDFInfo
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- CN106366587A CN106366587A CN201610737022.5A CN201610737022A CN106366587A CN 106366587 A CN106366587 A CN 106366587A CN 201610737022 A CN201610737022 A CN 201610737022A CN 106366587 A CN106366587 A CN 106366587A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention discloses a preparation method of a biodegradable polylactic acid/starch composite. According to the specific technical scheme, the polylactic acid/starch composite is prepared from, by weight, 10-80 parts of polylactic acid, 10-60 parts of starch, 1-20 parts of toughening agent, 1-10 parts of plasticizer, 1-10 parts of epoxy vegetable oil, 0.1-3 parts of coupling agent, 0.1-3 parts of nucleating agent, 0.1-5 parts of grafting agent, 0.1-5 parts of lubricating agent and 0.1-2 parts of antioxidant. The product has good mechanical properties and heat resistance, the vicat softening temperature can reach 120-140 DEG C, and therefore the application standard and requirement for disposable tableware can be completely met; the product price is relatively low, which provides a great advantage for safe and environment-friendly biodegradable materials to enter the disposable tableware industry.
Description
Technical field
The invention belongs to Biodegradable high-molecular field of compound material, specially a kind of Biodegradable polylactic acids/shallow lake
The preparation method of powder composite material.
Background technology
When it was recognized that the presence of environmental problem, begin to explore the ability preserved the ecological environment, for improving existence ring
Border and effort.In Biodegradable material, chemosynthesis macromolecular material is compared to natural synthesis macromolecular material and micro- life
Thing synthesis macromolecular material has the advantages that plasticity, machinability and production cost are relatively low, great market prospect.But it is poly-
Lactic acid there is also certain defect in performance, and as poor in shock resistance, heat distortion temperature is low, degradation rate is very fast etc..Blending
Modification then overcomes above-mentioned deficiency to provide simple thinking for poly-lactic acid material.
Biodegradable plasticss technology is related to multi-door subject, is restricted by many complicated factors and environmental condition, its technology
There are some problems in property, the economical, aspect such as practicality, policy, need to be researched and solved further.As biodegradable plastic
Price is higher than the price of general-purpose plastics 3-5 times, 5%-15% higher than the price of disintegration-type degradative plastics.Expensive price becomes it
The obstacle promoted；Definite concept to degradative plastics and its effect in the environment there is no unified understanding and definite commenting at present
Valency；In plastics exploitation that can not be degradable, more reasonably technical recipe, more perfect, more advanced forming technique and equipment
Etc. needing further to be improved and perfect.
In order to overcome the shortcoming of polylactic acid, reduces cost, expanded application scope, and the biological degradability using polylactic acid
With excellent improved combination properties other materials.People have done a lot of researchs to the blending and modifying of polylactic acid, and polylactic acid/starch is multiple
Condensation material combines the excellent performance of polylactic acid and the advantage of starch low cost, can take into account the mechanical property of material simultaneously,
It is not only able to substitute conventional petroleum base plastics, more expanded the non-edible purposes of starch, be a kind of dropping of great DEVELOPMENT PROSPECT
Solution plastics.
Patent cn201210062675 proposes a kind of system preparing the full Biobased degradable composite material of polylactic acid/starch
Preparation Method.This patent is extruded jointly using polylactic resin, epoxidized vegetable oil, anhydride grafting modified starch material, this invention institute
The composite providing, safety non-toxic, biodegradable and mechanical performance is excellent, but preparation process complexity needs to squeeze twice
Go out, directly resulting in cost increases.Patent cn201010594708 provides a kind of fecula polylactic acid intermingling material and its preparation side
Method.This patent polylactic acid, starch, grafting agent, the characteristic of the intermingling material prepared by plasticizer, coupling agent etc. is formerly to
Grafting agent, starch, plasticizer and coupling agent etc. are added in homogenizer and stir jointly being extruded with polylactic acid, but need through
Double screw extruder twice, cost increases.
Patent cn201110158433 provides a kind of biodegradable polylactic acid/starch heat-resisting composite and its system
Preparation Method, is mixed through raw material using native starch, polylactic acid, polyvinyl alcohol, plasticizer, water, heat-proof modifier, nucleator etc.
Close, extrude the processes such as granulating, gamma Rays.Advantage is to be processed and formed at one time, and material has biodegradability and certain
Thermostability, but production method and process is relative complex and starch is surface-treated.Heat distortion temperature at 90 DEG C about, for
Relatively low for disposable food or beverage container.
Content of the invention
It is an object of the invention to provide a kind of production technology is relatively easy, excellent in mechanical performance and meet disposable plastic
The full biodegradable heat-proof polylactic acid/starch composite material of Dining tool standard.
A kind of preparation method of Biodegradable polylactic acids/starch composite material, concrete technical scheme is as follows:
PLA/Starch Blends of the present invention include the component of following weight portion: polylactic acid 10-80 part, starch
10-60 part, toughener 1-20 part, plasticiser 1-10 part, epoxidized vegetable oil 1-10 part, coupling agent 0.1-3 part, nucleator 0.1-3
Part, grafting agent 0.1-5 part, lubricant 0.1-5 part, antioxidant 0.1-2 part.
Described polylactic acid is one of plla, pdla or pdlla, and weight average molecular weight is 1-30 ten thousand dalton.
Described native starch raw material be selected from tapioca, sweet potato starch, potato starch, arrowroot starch, glutinous rice starch,
Semen oryzae sativae starch, corn starch, pea starch, Semen vignae sinensiss starch, Bulbus Lilii starch, sago starch, sorghum starch, wheaten starch, Fructus Hordei Vulgaris
One of starch, rye starch, Indica Rice Starch, Rhizoma Dioscoreae starch, green starch, Faba bean starch, water caltrop starch, Rhizoma Nelumbinis starch or several
Kind.
Described toughener is polyolefin elastomer (poe), ethylene-vinyl acetate copolymer (eva), styrene-fourth two
Thermoplastic olefinic elastomer (sbs), ethylene propylene diene rubber (epdm), poly butylene succinate (pbs), polyadipate/to benzene two
One or more of formic acid fourth diester (pbat), acrylonitrile-butadiene-styrene copolymer (abs).
Described epoxidized vegetable oil is epoxy Oleum Arachidis hypogaeae semen, epoxy soybean oil, epoxy castor oil, epoxy coconut oil, epoxy are brown
In palmitic acid oil, epoxidized linseed oil, epoxy cottonseed oil, epoxy Semen Maydis oil, epoxy Oleum Helianthi, epoxy pine-seed oil, epoxy castor oil one
Plant or several.
Described plasticizer is water, glycerol, Polyethylene Glycol, polypropylene glycol, acetic acid tributyl, tributyl citrate, acetyl
One or more of tributyl citrate, dibutyl phthalate, mineral oil, paraffin oil, carbamide.
Described anhydride is benzoyl oxide, PFPA, n-caproic anhydride, propionic andydride, isobutyric anhydride, maleic anhydride, second
One of anhydride, glutaric anhydride, stearic anhydride, phenylsuccinic acid acid anhydride.
Described coupling agent is one or more of silane coupler or titanate coupling agent mixture.
Described antioxidant is Hinered phenols antioxidant, preferably antioxidant 1010, irgasfos 168, antioxidant 300, antioxygen
One or more of agent 330.
Described nucleator be aryl phosphate ester aluminium salt, clay, Muscovitum, silicon dioxide, Pulvis Talci, montmorillonite, Calcium Carbonate,
One or more of Plant fiber, glass, calcium sulfate crystal whiskers.
Described lubricant is one or more of monoglyceride, paraffin, calcium stearate, zinc stearate, stearyl alcohol.
Present invention also offers a kind of preparation method of above-mentioned PLA/Starch Blends, the method includes following step
Rapid:
Coupling agent and starch are added stirring mixing in high speed mixing smelting machine, temperature is 20-50 DEG C, the time is 5-30 minute.
24h post-drying is placed in the mixture sealing that step (1) is obtained.
Polylactic acid after drying, toughener, polylactic acid graft are with main spout feeding.
Nucleator, antioxidant, lubricant, be surface-treated and dry in anhydride and (2) after starch high mixer setting
At a temperature of mix homogeneously, with powder body charging aperture feeding.
Plasticizer and epoxidized vegetable oil liquid inlet opening feeding.
The draw ratio of described double screw extruder is 25:1-60:1, and from feeding section to die face, each area temperature control is 145
DEG C between 220 DEG C.
Beneficial effect:
(1) product has good mechanical performance and heat resistance, and vicat softening temperature can reach 120-140 DEG C, complete
Use standard and the requirement of disposable food or beverage container entirely can be met.
(2) product price relative moderate, this enters disposable food or beverage container industry to the Biodegradable material of safety and environmental protection
Provide very big advantage.
Specific embodiment
In conjunction with the embodiments, the present invention is described in further details.
Below by embodiment, technical scheme is described in further detail, following examples are according to mechanics
Test and thermodynamics method of testing press astm standard formulation.
Embodiment 1
(1) by pretreatment corn starch 1000g, maleic anhydride 30g, antioxidant 1010 10g, calcium stearate 5g,
Tmc-300 20g adds high-speed stirred 10min under room temperature in high mixer.
(2) by the mixture obtaining in (1) and 2060g plla, 206g pbs adds double screw extruder extruding pelletization,
Each section of temperature of extruder is set as (from charging aperture to die head): 190 DEG C, 195 DEG C, 195 DEG C, 190 DEG C, 185 DEG C, 180 DEG C, 180
DEG C, 170 DEG C, 170 DEG C, 170 DEG C, screw speed 110rpm.
(3) the fully biodegradable polylactic acid starch composite material prepared by becomes white or slightly yellow solid, by the grain of extrusion
Material is dried at 80 DEG C, detects after injection molded plaques.118 DEG C of heat distortion temperature, tensile strength 34mpa, elongation at break 11%, melts
Body flow rate is 9.6g/10min (190 DEG C, 2.16kg).
Embodiment 2
(1) by pretreatment corn starch 1000g, maleic anhydride 60g, antioxidant 1010 10g, calcium stearate 5g,
Tmc-300 20g adds high-speed stirred 10min under room temperature in high mixer.
(2) by the mixture obtaining in (1) and 2060g plla, 100g pbs adds double screw extruder extruding pelletization,
Each section of temperature of extruder is set as (from charging aperture to die head): 190 DEG C, 195 DEG C, 195 DEG C, 190 DEG C, 185 DEG C, 180 DEG C, 180
℃、170℃、170℃、170℃.Screw speed 110rpm.
(3) Biodegradable polylactic acids/starch composite material prepared by is in slightly yellow solid, by the pellet of extrusion 80
Dry at DEG C, detect after injection molded plaques.124 DEG C of heat distortion temperature, tensile strength 38mpa, elongation at break 6%, melt flows
Speed is 7.8g/10min (190 DEG C, 2.16kg).
Embodiment 3
(1) by pretreatment corn starch 1000g, maleic anhydride 30g, antioxidant 1010 10g, calcium stearate 5g,
Tmc-300 20g adds high-speed stirred 10min under room temperature in high mixer.
(2) by the mixture obtaining in (1) and 2060g plla, 206g pbat adds double screw extruder extruding pelletization,
Each section of temperature of extruder is set as (from charging aperture to die head): 190 DEG C, 195 DEG C, 195 DEG C, 190 DEG C, 185 DEG C, 180 DEG C, 180
℃、170℃、170℃、170℃.Screw speed 110rpm.
(3) the fully biodegradable polylactic acid starch composite material prepared by becomes white or slightly yellow solid, by the grain of extrusion
Material is dried at 80 DEG C, detects after injection molded plaques.120 DEG C of heat distortion temperature, tensile strength 30mpa, elongation at break 15%, melts
Body flow rate is 7.2g/10min (190 DEG C, 2.16kg).
The PLA/Starch Blends of embodiment gained disclosure satisfy that the disposable performance requirement being molded dishware, produces
Product have certain market advantage.
Above-mentioned specific embodiment is only intended to clearly illustrate example of the present invention, and not to embodiment
Limit.For those of ordinary skill in the field, other multi-forms can also be made on the basis of the above description
Change or variation, there is no need to be exhaustive to all of embodiment, and thus amplified out apparent
Change or change still in protection scope of the present invention.
Claims (10)
1. a kind of preparation method of Biodegradable polylactic acids/starch composite material it is characterised in that concrete technical scheme such as
Under:
Component including following weight portion: polylactic acid 10-80 part, starch 10-60 part, toughener 1-20 part, plasticiser 1-10 part,
Epoxidized vegetable oil 1-10 part, coupling agent 0.1-3 part, nucleator 0.1-3 part, grafting agent 0.1-5 part, lubricant 0.1-5 part, antioxygen
Agent 0.1-2 part；
Preparation method comprises the following steps:
Coupling agent and starch are added stirring mixing in high speed mixing smelting machine, temperature is 20-50 DEG C, the time is 5-30 minute；To walk
Suddenly 24h post-drying is placed in the mixture sealing that (1) obtains；Polylactic acid after drying, toughener, the main feeding of polylactic acid graft
Mouth feeding；Nucleator, antioxidant, lubricant, be surface-treated and dry in anhydride and (2) after starch high mixer setting temperature
The lower mix homogeneously of degree, with powder body charging aperture feeding；Plasticizer and epoxidized vegetable oil liquid inlet opening feeding；Described twin screw
The draw ratio of extruder is 25:1-60:1, between from feeding section to die face, each area temperature control is 145 DEG C to 220 DEG C.
2. the preparation method of a kind of Biodegradable polylactic acids/starch composite material according to claim 1, its feature exists
In described polylactic acid is one of plla, pdla or pdlla, and weight average molecular weight is 1-30 ten thousand dalton.
3. the preparation method of a kind of Biodegradable polylactic acids/starch composite material according to claim 1, its feature exists
In described native starch raw material is selected from tapioca, sweet potato starch, potato starch, arrowroot starch, glutinous rice starch, Semen oryzae sativae
Starch, corn starch, pea starch, Semen vignae sinensiss starch, Bulbus Lilii starch, sago starch, sorghum starch, wheaten starch, barley starch,
One or more of rye starch, Indica Rice Starch, Rhizoma Dioscoreae starch, green starch, Faba bean starch, water caltrop starch, Rhizoma Nelumbinis starch.
4. the preparation method of a kind of Biodegradable polylactic acids/starch composite material according to claim 1, its feature exists
In described toughener is polyolefin elastomer (poe), ethylene-vinyl acetate copolymer (eva), styrene-butadiene thermoplastic
Property elastomer (sbs), ethylene propylene diene rubber (epdm), poly butylene succinate (pbs), polyadipate/p-phthalic acid fourth
One or more of diester (pbat), acrylonitrile-butadiene-styrene copolymer (abs).
5. the preparation method of a kind of Biodegradable polylactic acids/starch composite material according to claim 1, its feature exists
In, described epoxidized vegetable oil is epoxy Oleum Arachidis hypogaeae semen, epoxy soybean oil, epoxy castor oil, epoxy coconut oil, epoxy palm oil,
One of epoxidized linseed oil, epoxy cottonseed oil, epoxy Semen Maydis oil, epoxy Oleum Helianthi, epoxy pine-seed oil, epoxy castor oil or several
Kind.
6. the preparation method of a kind of Biodegradable polylactic acids/starch composite material according to claim 1, its feature exists
In described plasticizer is water, glycerol, Polyethylene Glycol, polypropylene glycol, acetic acid tributyl, tributyl citrate, acetyl tributyl citrate
One or more of tributyl, dibutyl phthalate, mineral oil, paraffin oil, carbamide.
7. the preparation method of a kind of Biodegradable polylactic acids/starch composite material according to claim 1, its feature exists
In, described anhydride is benzoyl oxide, PFPA, n-caproic anhydride, propionic andydride, isobutyric anhydride, maleic anhydride, acetic anhydride,
One of glutaric anhydride, stearic anhydride, phenylsuccinic acid acid anhydride.
8. the preparation method of a kind of Biodegradable polylactic acids/starch composite material according to claim 1, its feature exists
In described antioxidant is one or more of antioxidant 1010, irgasfos 168, antioxidant 300, antioxidant 330.
9. the preparation method of a kind of Biodegradable polylactic acids/starch composite material according to claim 1, its feature exists
In described nucleator is aryl phosphate ester aluminium salt, clay, Muscovitum, silicon dioxide, Pulvis Talci, montmorillonite, Calcium Carbonate, plant
One or more of fiber, glass, calcium sulfate crystal whiskers.
10. the preparation method of a kind of Biodegradable polylactic acids/starch composite material according to claim 1, its feature
It is, described lubricant is one or more of monoglyceride, paraffin, calcium stearate, zinc stearate, stearyl alcohol.
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