CN108219208A - A kind of thermoplastic starch powder composite material and preparation method thereof - Google Patents
A kind of thermoplastic starch powder composite material and preparation method thereof Download PDFInfo
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- CN108219208A CN108219208A CN201711263595.XA CN201711263595A CN108219208A CN 108219208 A CN108219208 A CN 108219208A CN 201711263595 A CN201711263595 A CN 201711263595A CN 108219208 A CN108219208 A CN 108219208A
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- lactic acid
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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
- C08L3/00—Compositions of starch, amylose or amylopectin or of their derivatives or degradation products
- C08L3/02—Starch; Degradation products thereof, e.g. dextrin
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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
- 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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Abstract
The invention discloses a kind of thermoplastic starch powder composite materials and preparation method thereof.By weight, raw material and composition are thermoplastic starch powder composite material：00 parts by weight of thermoplastic starch copolymer 1,10 40 parts by weight of stereocomplex PLA, wherein, in stereocomplex PLA, 30 70 parts by weight of Poly L-lactic acid, poly- 30 70 parts by weight of L-lactic acid.Stereocomplex type polylactic acid and thermoplastic starch are blended, enhance the mechanical property of pure thermoplastic starch resin.Raw material in the present invention is easy to get, it is simple for process, using the method for two step melt blendings, it avoids introducing the nondegradable materials such as chain extender, without introducing other non-degradable substances while the mechanical property for enhancing pure thermoplastic starch resin, therefore the thermoplastic starch powder composite material formed has excellent biodegradability.
Description
Technical field
The invention belongs to biodegradated polymer materal technical fields.It is related to the preparation side of thermoplastic starch powder composite material
Method.
Background technology
It is mutually associated with hydrogen bond between native starch molecule, there is microstructure and granular texture, the melting temperature of crystallite
Degree is allowed to do not have thermoplastic processability, but if it is micro- that starch structure disordering can be made to destroy its higher than starch heat decomposition temperature
Crystalline substance, with regard to that can make starch that there is thermoplastic processability.Thermoplastic starch（TPS）Production principle：In thermal field, external force field and plasticising
Under the action of agent, it is plasticized stronger hydrogen bond action between agent and starch with intramolecular hydrogen bond between starch molecule and is replaced, starch
Molecule activity ability is improved.It adds in plasticizer and destroys the original crystalline texture of starch, make molecular structure disordering, realize
From crystalline state to amorphous conversion, so as to which it be made first to be realized before decomposition, melting forms thermoplastic starch.Thermoplastic starch was both
Property with plastics, and can rapidly degrade in the environment, it is complete biodegradable plastics truly, with original
Starch plastics are compared, it is advantageous that：All has complete biodegradability in various environment, the starch in product point
Son forms CO after degradation2, soil or air are not polluted；Appropriate technique is taken, is reached after starch thermoplastic can be made
The mechanical property identical with plastics.
Polylactic acid（PLA）It is by that can become lactic acid with the amylofermentation that regenerated plant resources extract, further be polymerized
Aliphatic polyester, be that one of more active kind is studied in aliphatic polyester.Polylactic acid glass transition temperature and fusing point
Respectively 60 DEG C and 175 DEG C or so, be a kind of hard macromolecule in glassy state, hot property and polystyrene at room temperature
It is similar.Polylactic acid has thermoplasticity, can be carried out on general process equipment as the synthesis macromolecule such as PP, PS and PET
Processing and forming.Polylactic acid can complete biodegradable, various poly-lactic acid products are using burying in the soil later, by certain time
Meeting natural decomposition is water and carbon dioxide later, will not cause environmental pollution.Polylactic acid synthesizes high molecular material not with general
Together, there are biodegradable and plant origin two major features.Around this two big characteristic, polylactic acid can reduce environment dirt
Dye, the application saved petroleum resources and be unfolded much to have much meaning in terms of mitigating global greenhouse effect.There are three types of vertical for polylactic acid
Body isomers：Poly L-lactic acid（PLLA）, poly- L-lactic acid（PDLA）And ploy DL lactic caid.Wherein, Poly L-lactic acid and the poly- right side
Stereocomplex can occur between rotation lactic acid and obtain the stereoscopic composite of polylactic acid, referred to as Stereocomplex type polylactic acid.
1987, [the Macromolecules 1987,20 such as Ikada:904-906] Stereocomplex type polylactic acid is reported for the first time, it
Afterwards, the attention of researchers is gradually caused.In recent years, exploitation heat-proof polylactic acid is become using Stereocomplex technology
A new direction.Research shows that the fusing point of Stereocomplex type polylactic acid is up to 230oC, than pure Poly L-lactic acid or the poly- right side
The fusing point for revolving lactic acid is high by 50oC or so, thermal stability, mechanical property and anti-hydrolytic performance than pure Poly L-lactic acid or gather
L-lactic acid will be got well.
Patent CN106883564A discloses a kind of starch plastic enhancing composite material and preparation method thereof excessively to containing barium phosphate
Basalt fibre be modified processing, be finally coupled under the action of coupling agent with starch plastic, be compound, so as to obtain
Basalt fibre and the better starch plastic composite material of starch plastic material compatibility, it is good to starch plastic humidification, but
It is process complexity, using pollution surrounding material.How simple and effective and complete biodegradable method enhances thermoplastic starch
Properties are a challenging problems.The present invention enhances thermoplastic starch by the way that stereocomplex PLA is prepared in situ
Powder solves more than problem.
Invention content
The purpose of the present invention is being directed to existing thermoplastic starch powder composite material and preparation method thereof above-mentioned deficiency, and provide
A kind of thermoplastic starch powder composite material and preparation method thereof.Preparation method is watery fusion processing method, i.e. melt processing temperature
Higher than Poly L-lactic acid and the fusing point of poly- L-lactic acid, less than the fusing point of Stereocomplex type polylactic acid.In such processing temperature
Section, thermoplastic starch resin, Poly L-lactic acid and poly- L-lactic acid can melt completely, only Stereocomplex type polylactic acid
Crystal can be grown, once being formed Stereocomplex type polylactic acid crystal, will be dispersed in the form of solid phase thermoplastic starch-based
In matter resin, the Stereocomplex type polylactic acid being formed in situ not only can effectively enhance the mechanical property of pure thermoplastic starch resin
Can, and within the scope of very wide temperature（Less than the fusing point of Stereocomplex type polylactic acid）Regulate and control the drawing of pure thermoplastic starch resin
Stretch mechanical behavior and melt index.
The present invention is made of thermoplastic starch and stereocomplex PLA, and weight is：
100 stereocomplex PLA 10-40 of thermoplastic starch；
The stereocomplex PLA is obtained for Poly L-lactic acid and poly- L-lactic acid by melt blending, weight
For：
The poly- L-lactic acid 30-70 parts by weight of Poly L-lactic acid 30-70.
The starch that thermoplastic starch uses is cornstarch, potato starch and tapioca, and wherein glycerol content is 20 weight
Part.
The weight average molecular weight of Poly L-lactic acid is 1 ~ 200,000, and the weight average molecular weight of poly- L-lactic acid is 1 ~ 200,000.
Preparation method is：It is 1 ~ 200,000 poly- left-handed breasts by thermoplastic starch and weight average molecular weight that weight average molecular weight is 5-20 ten thousand
Acid is added in mixer, is mixed 5-15 minutes under conditions of 165-185 DEG C, 80 revs/min, later in same condition
Lower addition weight average molecular weight is 1 ~ 200,000 poly- L-lactic acid mixing 5-20 minutes, and postcooling is blended to room temperature, as thermoplastic starch
Powder composite material.
The thermoplastic starch powder, preparation method thereof that the present invention uses is as follows：
By 100 parts by weight of starch, after the mixing completely of 20 parts by weight of glycerine, later under the conditions of 120 DEG C, 80 turns/min, it is added to
Mixer is kneaded 10 minutes, obtains thermoplastic starch.
Invention effect：
Thermoplastic starch powder composite material raw material of the present invention is easy to get, simple for process.Using two step melt-mixing methods, avoid
The nondegradable raw material such as other chain extenders are introduced, Poly L-lactic acid and poly- L-lactic acid melt blending are being prepared into thermoplasticity
It is in situ during starch composite material to obtain stereocomplex PLA, improve the mechanical property of thermoplastic starch, rheological behaviour and
Hydrophobicity.Stereocomplex PLA for enhancing is a kind of reinforcing agent of complete biology base, is enhancing pure thermoplastic starch tree
Without introducing other non-degradable substances while the physical property of fat, therefore the thermoplastic starch powder composite material formed is with excellent
Mechanical property, rheological behavior, hydrophobicity and completely biodegradable energy.
Specific embodiment
The raw material Poly L-lactic acid and poly- L-lactic acid used in the present invention is placed on vacuum drying chamber 80oIt is dried, does in C
Dry 3h.
Comparative example 1
Thermoplastic starch is made in cornstarch, 30min is mixed under conditions of 165 DEG C, 80 revs/min, obtains being not added with pure
Thermoplastic starch carries out stretching mechanical, melt index and contact angle determination.It the results are shown in Table 1.
Comparative example 2
Thermoplasticity potato starch is made in potato starch, 10min is mixed under conditions of 175 DEG C, 80 revs/min, obtains
It is not added with pure thermoplastic starch and carries out stretching mechanical, melt index and contact angle determination.It the results are shown in Table 1.
Comparative example 3
Thermoplastic starch is made in tapioca, 35min is mixed under conditions of 185 DEG C, 80 revs/min, obtains being not added with pure
Thermoplastic starch carries out stretching mechanical, melt index and contact angle determination.It the results are shown in Table 1.
Embodiment 1
It is 100,000 Poly L-lactic acid, 3 parts by weight by 100 parts by weight of thermoplastic starch made of cornstarch and weight average molecular weight, adds
Enter into mixer, mixed 10 minutes under conditions of 165 DEG C, 80 revs/min, add in divide equally again under identical condition later
Son amount mixes 20 minutes for 100,000 poly- 7 parts by weight of L-lactic acid, blending postcooling to room temperature, as thermoplastic starch composite wood
Material.Composite material is subjected to stretching mechanical, melt index and contact angle determination.It the results are shown in Table 1.
Embodiment 2
It is 20,000 Poly L-lactic acid, 14 parts by weight by 100 parts by weight of thermoplastic starch made of cornstarch and weight average molecular weight, adds
Enter into mixer, mixed 15 minutes under conditions of 165 DEG C, 80 revs/min, add in divide equally again under identical condition later
Son amount mixes 15 minutes for 20,000 poly- 6 parts by weight of L-lactic acid, blending postcooling to room temperature, as thermoplastic starch powder composite material.
Composite material is subjected to stretching mechanical, melt index and contact angle determination.It the results are shown in Table 1.
Embodiment 3
It is 200,000 Poly L-lactic acid, 24 parts by weight by 100 parts by weight of thermoplastic starch made of cornstarch and weight average molecular weight,
It is added in mixer, is mixed under conditions of 165 DEG C, 80 revs/min 12 minutes, it is equal to add in weight under identical condition later
Molecular weight mixes 18 minutes for 50,000 poly- 16 parts by weight of L-lactic acid, blending postcooling to room temperature, as thermoplastic starch composite wood
Material.Composite material is subjected to stretching mechanical, melt index and contact angle determination.It the results are shown in Table 1.
Embodiment 4
It is 50,000 Poly L-lactic acid, 8 parts by weight by 100 parts by weight of thermoplastic starch made of potato starch and weight average molecular weight,
It is added in mixer, is mixed under conditions of 175 DEG C, 80 revs/min 5 minutes, it is equal to add in weight under identical condition later
Molecular weight mixes 5 minutes for 50,000 poly- 8 parts by weight of L-lactic acid, blending postcooling to room temperature, as thermoplastic starch composite wood
Material.Composite material is subjected to stretching mechanical, melt index and contact angle determination.It the results are shown in Table 1.
Embodiment 5
It is 150,000 Poly L-lactic acid, 12 weight by 100 parts by weight of thermoplastic starch made of potato starch and weight average molecular weight
Part, it is added in mixer, is mixed under conditions of 175 DEG C, 80 revs/min 5 minutes, add in weight under identical condition later
Average molecular weight mixes 5 minutes for 150,000 poly- 18 parts by weight of L-lactic acid, blending postcooling to room temperature, and as thermoplastic starch is compound
Material.Composite material is subjected to stretching mechanical, melt index and contact angle determination.It the results are shown in Table 1.
Embodiment 6
It is 10,000 Poly L-lactic acid, 20 parts by weight by 100 parts by weight of thermoplastic starch made of potato starch and weight average molecular weight,
It is added in mixer, is mixed under conditions of 175 DEG C, 80 revs/min 5 minutes, it is equal to add in weight under identical condition later
Molecular weight mixes 5 minutes for 10,000 poly- 20 parts by weight of L-lactic acid, blending postcooling to room temperature, as thermoplastic starch composite wood
Material.Composite material is subjected to stretching mechanical, melt index and contact angle determination.It the results are shown in Table 1.
Embodiment 7
It is 180,000 Poly L-lactic acid, 3.6 parts by weight by 100 parts by weight of thermoplastic starch made of tapioca and weight average molecular weight,
It is added in mixer, is mixed under conditions of 185 DEG C, 80 revs/min 15 minutes, it is equal to add in weight under identical condition later
Molecular weight mixes 20 minutes for 180,000 poly- 8.4 parts by weight of L-lactic acid, blending postcooling to room temperature, and as thermoplastic starch is compound
Material.Composite material is subjected to stretching mechanical, melt index and contact angle determination.It the results are shown in Table 1.
Embodiment 8
It is 120,000 Poly L-lactic acid, 9 parts by weight by 100 parts by weight of thermoplastic starch made of tapioca and weight average molecular weight, adds
Enter into mixer, mixed 15 minutes under conditions of 185 DEG C, 80 revs/min, add in divide equally again under identical condition later
Son amount mixes 20 minutes for 120,000 poly- 27 parts by weight of L-lactic acid, blending postcooling to room temperature, as thermoplastic starch composite wood
Material.Composite material is subjected to stretching mechanical, melt index and contact angle determination.It the results are shown in Table 1.
Embodiment 9
It is 10,000 Poly L-lactic acid, 16 parts by weight by 100 parts by weight of thermoplastic starch made of tapioca and weight average molecular weight, adds
Enter into mixer, mixed 15 minutes under conditions of 185 DEG C, 80 revs/min, add in divide equally again under identical condition later
Son amount mixes 20 minutes for 10,000 poly- 24 parts by weight of L-lactic acid, blending postcooling to room temperature, as thermoplastic starch composite wood
Material.Composite material is subjected to stretching mechanical, melt index and contact angle determination.It the results are shown in Table 1.
The present invention is first melted thermoplastic starch with Poly L-lactic acid using two step melt-mixing methods at a certain temperature
Blending is allowed to after being mixed thoroughly that poly- L-lactic acid is added in melt blending under identical condition again, obtains vertical structure in situ
The composite material of the thermoplastic starch of compound polylactic acid enhancing.Avoiding during melt blending introducing other chain extenders etc. can not
The raw material of degradation obtain composite material complete biodegradable.
Tensile mechanical properties measure：Using stretching experiment test is carried out on 1211 type electronic tensile machines of Instron, sample takes
From the thin slice being directly molded, at room temperature, 10 mm/min of rate of extension.The live part size of tensile bars for 20mm long,
4mm wide, thickness about 1mm.Final result takes the average value of five batten institute measured data.
Melt index determination：Using melt indexer, capillary diameter is 2.095 mm, and pipe range is 8 mm.It is heated to 190
After DEG C, upper end applies 2.16 kg counterweights by piston and extrudes downwards, measures its weight being extruded in 10 minutes, as should
The melt index of sample.
Contact angle determination：Using contact angle measurement, sample to be tested molding flakiness measures contact angle of the water to sample.
Static stretch mechanical property and melt index table 1
Claims (5)
1. a kind of thermoplastic starch powder composite material, it is characterised in that it is made of thermoplastic starch and stereocomplex PLA,
Weight is：
100 stereocomplex PLA 10-40 of thermoplastic starch；
The stereocomplex PLA is obtained for Poly L-lactic acid and poly- L-lactic acid by melt blending, weight
For：
The poly- L-lactic acid 30-70 parts by weight of Poly L-lactic acid 30-70.
2. thermoplastic starch powder composite material according to claim 1, it is characterised in that the starch that thermoplastic starch uses is
Cornstarch, potato starch and tapioca, wherein glycerol content are 20 parts by weight.
3. thermoplastic starch powder composite material according to claim 1 or 2, it is characterised in that the Weight-average molecular of Poly L-lactic acid
It is 1 ~ 200,000 to measure, and the weight average molecular weight of poly- L-lactic acid is 1 ~ 200,000.
4. thermoplastic starch powder composite material according to claim 1 or 2, it is characterised in that preparation method is：It will divide equally again
The thermoplastic starch and weight average molecular weight that son amount is 5-20 ten thousand are 1 ~ 200,000 Poly L-lactic acid, are added in mixer, in 165-
It is mixed under conditions of 185 DEG C, 80 revs/min 5-15 minutes, it is 1 ~ 200,000 to add in weight average molecular weight under identical condition later
Poly- L-lactic acid mixing 5-20 minutes, blending postcooling to room temperature, as thermoplastic starch powder composite material.
5. thermoplastic starch powder composite material according to claim 1 or 2, it is characterised in that preparation method is：：
By 100 parts by weight of starch, after the mixing completely of 20 parts by weight of glycerine, later under the conditions of 120 DEG C, 80 turns/min, it is added to
Mixer is kneaded 10 minutes, obtains thermoplastic starch.
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| CN201711263595.XA CN108219208A (en) | 2017-12-05 | 2017-12-05 | A kind of thermoplastic starch powder composite material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110016215A (en) * | 2019-04-12 | 2019-07-16 | 南昌航空大学 | A kind of method of starch/polylactic acid composite material preparation |
| CN112239566A (en) * | 2020-10-22 | 2021-01-19 | 青岛周氏塑料包装有限公司 | Thermoplastic starch and preparation method thereof |
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| CN101157792A (en) * | 2007-09-20 | 2008-04-09 | 浙江海正生物材料股份有限公司 | Fully biodegradable polylactic acid composite material and preparation method thereof |
| CN102597106A (en) * | 2009-08-28 | 2012-07-18 | 东丽株式会社 | Polylactic acid stereocomplex, process for production thereof, and nucleating agent for polylactic acid resin |
| CN103265797A (en) * | 2013-05-27 | 2013-08-28 | 四川大学 | Completely-degradable polylactic acid composite material with high crystallinity and preparation method thereof |
| CN105885368A (en) * | 2014-12-12 | 2016-08-24 | 允友成(宿迁)复合新材料有限公司 | Highly heat-resistant polylactic acid/thermoplastic starch composite material and preparation method thereof |
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2017
- 2017-12-05 CN CN201711263595.XA patent/CN108219208A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101157792A (en) * | 2007-09-20 | 2008-04-09 | 浙江海正生物材料股份有限公司 | Fully biodegradable polylactic acid composite material and preparation method thereof |
| CN102597106A (en) * | 2009-08-28 | 2012-07-18 | 东丽株式会社 | Polylactic acid stereocomplex, process for production thereof, and nucleating agent for polylactic acid resin |
| CN103265797A (en) * | 2013-05-27 | 2013-08-28 | 四川大学 | Completely-degradable polylactic acid composite material with high crystallinity and preparation method thereof |
| CN105885368A (en) * | 2014-12-12 | 2016-08-24 | 允友成(宿迁)复合新材料有限公司 | Highly heat-resistant polylactic acid/thermoplastic starch composite material and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110016215A (en) * | 2019-04-12 | 2019-07-16 | 南昌航空大学 | A kind of method of starch/polylactic acid composite material preparation |
| CN112239566A (en) * | 2020-10-22 | 2021-01-19 | 青岛周氏塑料包装有限公司 | Thermoplastic starch and preparation method thereof |
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Application publication date: 20180629 |