CN105602219A - Biodegradable polylactic acid modified material - Google Patents
Biodegradable polylactic acid modified material Download PDFInfo
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- CN105602219A CN105602219A CN201610186878.8A CN201610186878A CN105602219A CN 105602219 A CN105602219 A CN 105602219A CN 201610186878 A CN201610186878 A CN 201610186878A CN 105602219 A CN105602219 A CN 105602219A
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- polylactic acid
- modified polylactic
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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
- 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
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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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- 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
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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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
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
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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
- C08L2205/24—Crystallisation aids
Abstract
The invention relates to the technical field of biodegradable materials and particularly relates to a biodegradable polylactic acid modified material which comprises the following components: 50-72% of polylactic acid, 20-40% of corn starch, 2-8% of toughening agent, 1-2% of nucleating agent, 0.5-1% of acetylation reagent, 0.5-1% of catalyst and 0.5-1% of coupling agent. On one hand, by replacing the starch in the prior art with acetylated corn starch and adding an aluminate coupling agent into the system, the compatibility between starch and polylactic acid is enhanced, and the processability of polylactic acid is improved; and on the other hand, by adding the toughening agent with an active group to perform a chemical reaction with polylactic acid, a relatively ideal toughening effect is obtained, and the physical and mechanical processability of polylactic acid is obviously improved while the heat deflection temperature is basically kept unchanged.
Description
Technical field
The present invention relates to Biodegradable material technical field, particularly a kind of biodegradable polylactic acid modified materialMaterial.
Background technology
Along with social develop rapidly and scientific and technical progress, people are increasing to the demand of oil, but oilBe non-renewable resource, petroleum resources are along with a large amount of uses of various countries will face exhaustion, and nondegradable petroleum base is moulded simultaneouslyMaterial discarded object cause as contaminated soil water source, land occupation resource, threaten the series of problems such as ecological environment constantly to worsen,Cause the very big concern of countries in the world tissue, the research of degradable recyclable materials becomes worldwide focus.
PLA is a kind of taking the renewable resource such as starch, cellulose as raw material, through hydrolysis, fermentation, purifying, be polymerizedA kind of aliphatic polyester, raw material sources are extensive, can complete biodegradable, there is processability like conventional polyolefins resin-phaseCan, be considered to substitute in one-time consumption product field the optimal selection of non-degradable plastics. PLA has good biofaciesCapacitive and degradability, prepare environmentally friendly degradation material with starch blending, not only can realize the complete biology of materialDegraded, more can reduce the dependence to non-renewable petroleum base polymer, significant to solving problem of environmental pollution.
Although PLA has huge market prospects, itself is hard and crisp, and physical mechanical processing characteristics is undesirable, and this allLimit its further application, therefore, to the polylactic acid modified research emphasis that starts to become people.
Summary of the invention
One of object of the present invention is: for the deficiencies in the prior art, and provide a kind of biodegradable PLAMaterial modified, this material is in keeping original biocompatibility and degradability, and its physical and mechanical properties is also changedKind.
To achieve these goals, the present invention adopts following solution:
A kind of biodegradable modified polylactic acid material, comprises the composition of following percentage by weight:
Wherein, described PLA is to be poly (l-lactic acid), PDLLA or the above two copolymerized blend, the equal molecule of its numberAmount is 4-60 ten thousand;
Described flexibilizer is methyl methacrylate-butadiene-styrene copolymer, acrylonitrile-butadiene-benzeneAt least one in ethylene copolymer and ethylene-vinyl acetate copolymer, flexibilizer contains active group, can send out with PLABiochemical reaction, obtains comparatively ideal toughening effect, heat distortion temperature is remained unchanged substantially, and shock resistance obviously changesKind;
Described nucleator is talcum powder, phosphate metal salt, 3,4-dimethyl benzylidene sorbierite and decanedioic acid dibenzoylAt least one in hydrazine.
Described acetylation reagent is acetic anhydride; Described catalyst is NaOH;
Described coupling agent is Aluminate, coupling agent be in plastics compounding, play improve synthetic resin and inorganic filler orA kind of plastic additive of the interface performance effect of reinforcing material, it falls the sticky of process systems in the process of PLADegree, the decentralization that improves filler to be to improve processing characteristics, and then makes goods obtain good surface quality and machinery, heat and electricPerformance.
Taking described cornstarch as raw material, described acetic anhydride is that acetylation reagent, described NaOH are catalyst, utilizesMicrowave irradiation technology makes acetylated starch. The particle size of acetylated starch is little compared with the particle size of unmodified starch, andThe hydroxyl of particle surface has reduced, and has weakened the interaction between particle, has increased the combination between itself and PLA particlePower, has improved the compatibility between cornstarch and PLA;
Described methyl methacrylate-butadiene-styrene copolymer is by 42 parts of styrene-butadiene latexes, 28 parts of benzene secondThe polymerization and obtaining in water of alkene, 30 parts of methyl methacrylates.
Described biodegradable modified polylactic acid material, also comprises 0.2～1% solubilising by weight percentageAgent, described solubilizer is at least one in di-2-ethylhexyl maleate and cumyl peroxide.
Described biodegradable modified polylactic acid material, also comprises 0.2～1% antioxygen by weight percentageAgent, described antioxidant is 4-methyl-2, in 6-DI-tert-butylphenol compounds, butylated hydroxytoluene and BHT extremelyFew a kind of.
Described biodegradable modified polylactic acid material, also comprise by weight percentage 0.2～1% thermally-stabilisedAgent, described heat stabilizer is at least one in zinc stearate, pentaerythrite, dibasic lead stearate and calcium laurate. HeatBetween stabilizing agent, have cooperative effect, not only make the heat resistance of PLA get a promotion, its weather resistance and processabilityCan also be improved accordingly.
Preferably, described biodegradable modified polylactic acid material, comprises the composition of following percentage by weight:
More preferred, described biodegradable modified polylactic acid material, is characterized in that, comprises following weight hundredThe composition of proportion by subtraction:
Another object of the present invention is, a kind of preparation of described biodegradable modified polylactic acid material is providedMethod, comprises the following steps:
The first step, PLA is dry with molecular sieve vacuum drier, and the water content of PLA is 350ppm;
Second step, drops into high mixer mixing 5min by above-mentioned weight proportion;
The 3rd step, drops into double screw extruder granulation by mixed second step raw material, and screw slenderness ratio is 1:42, screw rodRotating speed is 500rpm, and screw zones heating-up temperature is 150 DEG C, 165 DEG C, 175 DEG C, 185 DEG C, 170 DEG C, 160 DEG C;
The 4th step, the grain input injection machine that the 3rd step is made, by required product mold, injection mo(u)lding, injection machine spiral shell160 DEG C of bar heating-up temperatures, pressure 90MPa;
The 5th step is carried out post bake 2min by the 4th step injection moulding product out in temperature is the drying tunnel stove of 120 DEG C.
Beneficial effect of the present invention is: the biodegradable modified polylactic acid material of one provided by the invention, comprisesThe composition of following percentage by weight: PLA 50～72%, cornstarch 20～40%, flexibilizer 2～8%, nucleator 1～2%, acetylation reagent 0.5～1%, catalyst 0.5～1%, coupling agent 0.5～1%, on the one hand, with acetylizad corn shallow lakePowder replaces starch of the prior art, and in system, adds aluminate coupling agent, has both increased between starch and PLACompatibility, has improved again the processing characteristics of PLA; On the other hand, add the flexibilizer with active group, make itself and poly-breastThere is chemical reaction in acid, obtains comparatively ideal toughening effect, when heat distortion temperature remains unchanged substantially, obviously improves poly-The physical mechanical processing characteristics of lactic acid.
Detailed description of the invention
Below in conjunction with embodiment, the present invention and beneficial effect thereof are described in further detail, but enforcement of the present inventionExample is not limited to this.
Embodiment 1
Taking 25 parts of cornstarch as raw material, 1 part of acetic anhydride is that acetylation reagent, 1 part of NaOH are catalyst, utilizes micro-Wave radiation technology makes acetylated starch. PLA is dry with molecular sieve vacuum drier, and PLA water content is 350ppm;By weight by 65 parts of PLAs, 26 parts of acetylated starches, 3 parts of methyl methacrylate-butadiene-styrene terpolymersThing, 2 parts of decanedioic acid dibenzoyl hydrazines, 1 part of aluminate coupling agent, 1 part of di-2-ethylhexyl maleate, 0.5 part of butylated hydroxytoluene, 0.5Part dibasic lead stearate drops into high mixer mixing 5min; Mixed raw material is dropped into double screw extruder granulation, and screw rod is longFootpath is than for 1:42, and screw speed is 500rpm, screw zones heating-up temperature be 150 DEG C, 165 DEG C, 175 DEG C, 185 DEG C, 170 DEG C,160 DEG C; By the grain input injection machine of making, by required product mold, injection mo(u)lding, 160 DEG C of screw in injection molding machine heating-up temperatures,Pressure 90MPa; Injection moulding product out in being the drying tunnel stove of 120 DEG C, temperature is carried out to post bake 2min.
Embodiment 2～4
Process is identical with embodiment 1, and difference is the performance of formula and products obtained therefrom, as shown in table 1 respectively:
Table 1
Comparative example 1
PLA and starch is dry with molecular sieve vacuum drier, and the water content of PLA is 350ppm, the containing of starchThe water yield is 0.1%; By weight by 60 parts of PLAs, 30 parts of cornstarch, 3 parts of methyl methacrylate-butadiene-styreneTerpolymer, 2 parts of tributyl 2-acetylcitrates, 2 parts of decanedioic acid dibenzoyl hydrazines, 1 part of di-2-ethylhexyl maleate, 1 part of butyl hydroxylBase toluene, 1 part of dibasic lead stearate drop into high mixer mixing 5min; Mixed raw material is dropped into double screw extruder to be madeGrain, screw slenderness ratio is 1:42, and screw speed is 500rpm, and screw zones heating-up temperature is 150 DEG C, 165 DEG C, 175 DEG C, 185DEG C, 170 DEG C, 160 DEG C; By the grain input injection machine of making, by required product mold, injection mo(u)lding, screw in injection molding machine heating160 DEG C of temperature, pressure 90MPa; Injection moulding product out in being the drying tunnel stove of 120 DEG C, temperature is carried out to post bake 2min.
Comparative example 2-4
Process is identical with comparative example 1, and difference is the performance of formula and products obtained therefrom, as shown in table 2 respectively:
Table 2
Can be found out by table 1 and table 2: its hot strength of the modified polylactic acid material that embodiment 1～4 makes, extension at breakAll large than comparative example 1～4 of rate, and heat distortion temperature remains unchanged substantially, that is to say, the present invention carries out second to cornstarchAfter acidylate processing, interpolation flexibilizer and coupling agent, the biodegradable modified polylactic acid material of preparation is keeping it originalWhen heat resistance and compatibility, the processing characteristicies such as its physical mechanical have all obtained to a certain degree improving.
The announcement of book and instruction according to the above description, those skilled in the art in the invention can also be to above-mentioned enforcement sideFormula changes and revises. Therefore, the present invention is not limited to above-mentioned detailed description of the invention, and every those skilled in the art existAny apparent improvement, replacement or the modification on basis of the present invention, done all belong to protection scope of the present invention. ThisOutward, although used some specific terms in this description, these terms are for convenience of description, not to the present inventionForm any restriction.
Claims (9)
1. a biodegradable modified polylactic acid material, is characterized in that, comprises the composition of following percentage by weight:
PLA 50 ~ 72%
Cornstarch 20 ~ 40%
Flexibilizer 2 ~ 8%
Nucleator 1 ~ 2%
Acetylation reagent 0.5 ~ 1%
Catalyst 0.5 ~ 1%
Coupling agent 0.5 ~ 1%,
Wherein, described PLA is to be poly (l-lactic acid), PDLLA or the above two copolymerized blend, and its number-average molecular weight is4-60 ten thousand;
Described flexibilizer is methyl methacrylate-butadiene-styrene copolymer, acrylonitrile-butadiene-styrene (ABS)At least one in copolymer and ethylene-vinyl acetate copolymer;
Described nucleator is talcum powder, phosphate metal salt, 3, in 4-dimethyl benzylidene sorbierite and decanedioic acid dibenzoyl hydrazineAt least one;
Described acetylation reagent is acetic anhydride; Described catalyst is NaOH;
Described coupling agent is aluminate coupling agent.
2. biodegradable modified polylactic acid material according to claim 1, is characterized in that, with described cornstarchFor raw material, described acetic anhydride is that acetylation reagent, described NaOH are catalyst, utilizes microwave irradiation technology to make acetylationStarch.
3. biodegradable modified polylactic acid material according to claim 1, is characterized in that: described methacrylic acidMethyl esters-butadiene-styrene copolymer is existed by 42 parts of styrene-butadiene latexes, 28 parts of styrene, 30 parts of methyl methacrylatesPolymerization in water and obtaining.
4. biodegradable modified polylactic acid material according to claim 1, is characterized in that: also comprise by weight hundredThe solubilizer of proportion by subtraction meter 0.2 ~ 1%, described solubilizer is at least one in di-2-ethylhexyl maleate and cumyl peroxide.
5. biodegradable modified polylactic acid material according to claim 4, is characterized in that: also comprise by weight hundredThe antioxidant of proportion by subtraction meter 0.2 ~ 1%, described antioxidant is 4-methyl-2,6-DI-tert-butylphenol compounds, butylated hydroxytoluene and 2,6-bis-At least one in Butylated Hydroxytoluene.
6. biodegradable modified polylactic acid material according to claim 5, is characterized in that: also comprise by weight hundredThe heat stabilizer of proportion by subtraction meter 0.2 ~ 1%, described heat stabilizer is for being zinc stearate, pentaerythrite, dibasic lead stearate and bayAt least one in acid calcium.
7. biodegradable modified polylactic acid material according to claim 6, is characterized in that, comprises following weight hundredThe composition of proportion by subtraction:
PLA 60 ~ 65%
Cornstarch 25 ~ 30%
Flexibilizer 3 ~ 5%
Nucleator 1 ~ 2%
Acetylation reagent 0.5 ~ 1%
Catalyst 0.5 ~ 1%
Coupling agent 0.5 ~ 1%
Solubilizer 0.5 ~ 1%
Antioxidant 0.5 ~ 1%
Heat stabilizer 0.5 ~ 1%.
8. biodegradable modified polylactic acid material according to claim 7, is characterized in that, comprises following weight hundredThe composition of proportion by subtraction:
PLA 65%
Cornstarch 25%
Flexibilizer 3%
Nucleator 2%
Acetylation reagent 1%
Catalyst 1%
Coupling agent 1%
Solubilizer 1%
Antioxidant 0.5%
Heat stabilizer 0.5%.
9. the preparation method of the biodegradable modified polylactic acid material described in claim 1 ~ 8 any one, is characterized in that,Comprise the following steps:
The first step, PLA is dry with molecular sieve vacuum drier, and the water content of PLA is 350ppm;
Second step, drops into high mixer mixing 5min by above-mentioned weight proportion;
The 3rd step, drops into double screw extruder granulation by mixed second step raw material, and screw slenderness ratio is 1:42, screw speedFor 500rpm, screw zones heating-up temperature is 150 DEG C, 165 DEG C, 175 DEG C, 185 DEG C, 170 DEG C, 160 DEG C;
The 4th step, the grain input injection machine that the 3rd step is made, by required product mold, injection mo(u)lding, screw in injection molding machine adds160 DEG C of hot temperature degree, pressure 90MPa;
The 5th step is carried out post bake 2min by the 4th step injection moulding product out in temperature is the drying tunnel stove of 120 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610186878.8A CN105602219A (en) | 2016-03-28 | 2016-03-28 | Biodegradable polylactic acid modified material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107699981A (en) * | 2017-09-20 | 2018-02-16 | 安徽锦翔纺织服饰有限公司 | A kind of environment-friendly degradable fiber and preparation method thereof |
| CN109608838A (en) * | 2018-10-18 | 2019-04-12 | 金旸（厦门）新材料科技有限公司 | One kind can the degradable long-acting transparent polylactic acid of toughening and preparation method thereof |
| CN109735071A (en) * | 2018-12-12 | 2019-05-10 | 苏州聚复高分子材料有限公司 | Composite material and preparation method for material extruded type increasing material manufacturing |
| CN110697909A (en) * | 2019-11-18 | 2020-01-17 | 辽宁科技学院 | Preparation method of traditional Chinese medicine wastewater treatment agent based on microorganisms |
| CN110746675A (en) * | 2019-11-05 | 2020-02-04 | 温州丰宝客科技有限公司 | Degradable environment-friendly packaging bag material and preparation method thereof |
| CN112625409A (en) * | 2020-10-23 | 2021-04-09 | 威骏(上海)环保包装有限公司 | Biodegradable plastic bottle cap and preparation method thereof |
-
2016
- 2016-03-28 CN CN201610186878.8A patent/CN105602219A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107699981A (en) * | 2017-09-20 | 2018-02-16 | 安徽锦翔纺织服饰有限公司 | A kind of environment-friendly degradable fiber and preparation method thereof |
| CN109608838A (en) * | 2018-10-18 | 2019-04-12 | 金旸（厦门）新材料科技有限公司 | One kind can the degradable long-acting transparent polylactic acid of toughening and preparation method thereof |
| CN109735071A (en) * | 2018-12-12 | 2019-05-10 | 苏州聚复高分子材料有限公司 | Composite material and preparation method for material extruded type increasing material manufacturing |
| CN110746675A (en) * | 2019-11-05 | 2020-02-04 | 温州丰宝客科技有限公司 | Degradable environment-friendly packaging bag material and preparation method thereof |
| CN110697909A (en) * | 2019-11-18 | 2020-01-17 | 辽宁科技学院 | Preparation method of traditional Chinese medicine wastewater treatment agent based on microorganisms |
| CN112625409A (en) * | 2020-10-23 | 2021-04-09 | 威骏(上海)环保包装有限公司 | Biodegradable plastic bottle cap and preparation method thereof |
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