CN104725805A - Polylactic acid-esterified starch-attapulgite composite material and preparation method thereof - Google Patents
Polylactic acid-esterified starch-attapulgite composite material and preparation method thereof Download PDFInfo
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- CN104725805A CN104725805A CN201510147751.0A CN201510147751A CN104725805A CN 104725805 A CN104725805 A CN 104725805A CN 201510147751 A CN201510147751 A CN 201510147751A CN 104725805 A CN104725805 A CN 104725805A
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Abstract
The invention provides a polylactic acid-esterified starch-attapulgite composite material and a preparation method thereof. The polylactic acid-esterified starch-attapulgite composite material comprises the following components in parts by weight: 48-58 parts of polylactic acid, 38-44 parts of esterified starch, 8-16 parts of attapulgite, 2-5 parts of alginate, 2-5 parts of glycerol, 1-3 parts of carboxymethyl chitosan and 1-2 parts of plasticizer. The preparation method comprises the following steps: (1) preparing a carboxymethyl chitosan acetic acid solution; (2) dissolving the attapulgite in deionized water, and carrying out ultrasonic dispersion to obtain an attapulgite suspension; and (3) adding the polylactic acid into the carboxymethyl chitosan acetic acid solution, uniformly mixing, adding the attapulgite suspension the surplus material while stirring, thoroughly mixing to form a composite sol, coating a film on glass by flow casting, and carrying out vacuum drying. Compared with the polylactic acid, the polylactic acid-esterified starch-attapulgite composite material has the advantages of higher tensile strength, higher bending strength, high heat stability and lower cost.
Description
Technical field
The present invention relates to technical field of biological material, be specifically related to a kind of poly(lactic acid)-ester starch-attapulgite matrix material and preparation method thereof.
Background technology
Poly(lactic acid) is a kind of polymkeric substance of partial crystallization, can with the composite system of many polymer formation thermodynamic compatibilities or partially compatible, poly(lactic acid) has good biocompatibility and biodegradability, but because biodegradable poly(lactic acid) holds at high price, make it be difficult to be popularized use.Poly(lactic acid) and starch is used to carry out the environmentally friendly degradable composite material of blended preparation; substitute conventional polyolefins resin; material can not only be made to realize complete biodegradable; the dependence to non-renewable fossil resources can also be reduced; based on the consideration to grain security; country has promulgated that relevant policies strengthen the amyloid protection of grain, with non-grain starch for the biomass macromolecular material that development of raw materials is novel more and more comes into one's own successively.
Starch is incompatible with poly(lactic acid) thermodynamics, directly will both blended time interface binding power very poor, there will be degradation problem under poor compatibility and material mechanical performance.Starch is after esterification modification, and the hydrophilic hydroxyl groups part on molecular chain, by hydrophobic carbonyl substituted, obviously can improve the consistency of starch and poly(lactic acid).But the poor heat stability of blended resulting materials, mechanical property is also difficult to the standard reaching bio-medical material, therefore, still needs further research to the modification of poly(lactic acid) and starch blend.
Summary of the invention
goal of the invention:the object of the present invention is to provide and a kind of there is good mechanical properties, poly(lactic acid)-ester starch-attapulgite matrix material that thermostability is high and preparation method thereof.
technical scheme of the present invention:
A kind of poly(lactic acid)-ester starch-attapulgite matrix material, by weight, comprises following component: poly(lactic acid) 48 ~ 58 parts, esterification starch 38 ~ 44 parts, attapulgite 8 ~ 16 parts, alginates 2 ~ 5 parts, glycerine 2 ~ 5 parts, cm-chitosan 1 ~ 3 part and 1 ~ 2 part, softening agent.
Preferably, by weight, following component is comprised: poly(lactic acid) 52 ~ 54 parts, esterification starch 40 ~ 42 parts, attapulgite 10 ~ 12 parts, alginates 3 ~ 4 parts, glycerine 3 ~ 4 parts, cm-chitosan 2 ~ 3 parts and 2 parts, softening agent.
More preferably, by weight, following component is comprised: poly(lactic acid) 53 parts, esterification starch 41 parts, attapulgite 11 parts, alginates 3 parts, glycerine 3 parts, cm-chitosan 2 parts and 2 parts, softening agent.
Described softening agent is one or more in oxalic acid dioctyl ester, triethyl phosphate or acetyl tributyl citrate.
Described esterification starch is maleic anhydride esterification starch.
Described alginates is sodium alginate.
A preparation method for poly(lactic acid)-ester starch-attapulgite matrix material, comprises the steps:
(1) cm-chitosan being dissolved in volume fraction is in the acetum of 2 ~ 5%, is mixed with the acetum of cm-chitosan, after stirring, and set aside for use;
(2) attapulgite is dissolved in the deionized water of 3 ~ 5 times of volumes, ultrasonic disperse 5 ~ 10min, obtains attapulgite suspension, set aside for use;
(3) poly(lactic acid) is joined in the acetum of the obtained cm-chitosan of step (1), mix, add attapulgite suspension and surplus stock while stirring, at 60 ~ 65 DEG C, electric stirring makes each composition fully mix, form complex sol, then used casting method film on glass, at 60 ~ 65 DEG C of constant-temperature vacuum drying 24 ~ 30h, namely obtained poly(lactic acid)-ester starch-attapulgite matrix material.
beneficial effect:
Poly(lactic acid)-ester starch-attapulgite matrix material prepared by the present invention has higher tensile strength and flexural strength relative to poly(lactic acid), and by macromolecular material and inorganics coupling between the two, mutual supplement with each other's advantages, synergy can be reached, the performance of further raising matrix material and thermostability, and can reduce costs.
Embodiment
Below the specific embodiment of the present invention is described in detail.
embodiment 1
A kind of poly(lactic acid)-ester starch-attapulgite matrix material, by weight, comprises following component: poly(lactic acid) 48 parts, maleic anhydride esterification starch 38 parts, attapulgite 8 parts, sodium alginate 2 parts, glycerine 2 parts, cm-chitosan 1 part and oxalic acid dioctyl ester 1 part.
Preparation method, comprises the steps:
(1) cm-chitosan being dissolved in volume fraction is in the acetum of 2%, is mixed with the acetum of cm-chitosan, after stirring, and set aside for use;
(2) attapulgite is dissolved in the deionized water of 3 times of volumes, ultrasonic disperse 5min, obtains attapulgite suspension, set aside for use;
(3) poly(lactic acid) is joined in the acetum of the obtained cm-chitosan of step (1), mix, add attapulgite suspension and surplus stock while stirring, at 60 DEG C, electric stirring makes each composition fully mix, form complex sol, then used casting method film on glass, at the dry 30h of 60 DEG C of constant-temperature vacuums, namely obtained poly(lactic acid)-ester starch-attapulgite matrix material.
embodiment 2
A kind of poly(lactic acid)-ester starch-attapulgite matrix material, by weight, comprises following component: poly(lactic acid) 52 parts, maleic anhydride esterification starch 40 parts, attapulgite 10 parts, sodium alginate 3 parts, glycerine 3 parts, cm-chitosan 2 parts and triethyl phosphate 2 parts.
Preparation method, comprises the steps:
(1) cm-chitosan being dissolved in volume fraction is in the acetum of 3%, is mixed with the acetum of cm-chitosan, after stirring, and set aside for use;
(2) attapulgite is dissolved in the deionized water of 3 times of volumes, ultrasonic disperse 6min, obtains attapulgite suspension, set aside for use;
(3) poly(lactic acid) is joined in the acetum of the obtained cm-chitosan of step (1), mix, add attapulgite suspension and surplus stock while stirring, at 62 DEG C, electric stirring makes each composition fully mix, form complex sol, then used casting method film on glass, at the dry 28h of 62 DEG C of constant-temperature vacuums, namely obtained poly(lactic acid)-ester starch-attapulgite matrix material.
embodiment 3
A kind of poly(lactic acid)-ester starch-attapulgite matrix material, by weight, comprises following component: poly(lactic acid) 53 parts, maleic anhydride esterification starch 41 parts, attapulgite 11 parts, sodium alginate 3 parts, glycerine 3 parts, cm-chitosan 2 parts and oxalic acid dioctyl ester 2 parts.
Preparation method, comprises the steps:
(1) cm-chitosan being dissolved in volume fraction is in the acetum of 4%, is mixed with the acetum of cm-chitosan, after stirring, and set aside for use;
(2) attapulgite is dissolved in the deionized water of 4 times of volumes, ultrasonic disperse 8min, obtains attapulgite suspension, set aside for use;
(3) poly(lactic acid) is joined in the acetum of the obtained cm-chitosan of step (1), mix, add attapulgite suspension and surplus stock while stirring, at 62 DEG C, electric stirring makes each composition fully mix, form complex sol, then used casting method film on glass, at the dry 28h of 62 DEG C of constant-temperature vacuums, namely obtained poly(lactic acid)-ester starch-attapulgite matrix material.
embodiment 4
A kind of poly(lactic acid)-ester starch-attapulgite matrix material, by weight, comprises following component: poly(lactic acid) 54 parts; maleic anhydride esterification starch 42 parts, attapulgite 12 parts, sodium alginate 4 parts; glycerine 4 parts, cm-chitosan 3 parts and acetyl tributyl citrate 2 parts.
Preparation method, comprises the steps:
(1) cm-chitosan being dissolved in volume fraction is in the acetum of 4.5%, is mixed with the acetum of cm-chitosan, after stirring, and set aside for use;
(2) attapulgite is dissolved in the deionized water of 5 times of volumes, ultrasonic disperse 9min, obtains attapulgite suspension, set aside for use;
(3) poly(lactic acid) is joined in the acetum of the obtained cm-chitosan of step (1), mix, add attapulgite suspension and surplus stock while stirring, at 62 DEG C, electric stirring makes each composition fully mix, form complex sol, then used casting method film on glass, at the dry 26h of 65 DEG C of constant-temperature vacuums, namely obtained poly(lactic acid)-ester starch-attapulgite matrix material.
embodiment 5
A kind of poly(lactic acid)-ester starch-attapulgite matrix material, by weight, comprises following component: poly(lactic acid) 58 parts, maleic anhydride esterification starch 44 parts, attapulgite 16 parts, sodium alginate 5 parts, glycerine 5 parts, cm-chitosan 3 parts and oxalic acid dioctyl ester 2 parts.
Preparation method, comprises the steps:
(1) cm-chitosan being dissolved in volume fraction is in the acetum of 5%, is mixed with the acetum of cm-chitosan, after stirring, and set aside for use;
(2) attapulgite is dissolved in the deionized water of 5 times of volumes, ultrasonic disperse 10min, obtains attapulgite suspension, set aside for use;
(3) poly(lactic acid) is joined in the acetum of the obtained cm-chitosan of step (1), mix, add attapulgite suspension and surplus stock while stirring, at 65 DEG C, electric stirring makes each composition fully mix, form complex sol, then used casting method film on glass, at the dry 24h of 65 DEG C of constant-temperature vacuums, namely obtained poly(lactic acid)-ester starch-attapulgite matrix material.
performance test:
The poly(lactic acid)-ester starch-attapulgite matrix material prepare embodiment 1 ~ 5 and poly(lactic acid) carry out Mechanics Performance Testing and thermogravimetric analysis, the results are shown in Table 1 and table 2.
Mechanic property test method: adopt the omnipotent mechanics machine of CMT-5504 type to test tensile property and bending property according to standard GB/T/T 1040-92 and GB/T 9341-2000.
Thermogravimetric analysis: on the TGA 209 F3 Thermo System that thermogravimetric analysis is produced in German NETZSCH company from 30 DEG C to 500 DEG C to test the argon flow amount of the temperature rise rate of 10 DEG C/min and 30mL/min, sample size is about 5mg, T
0for starting temperature during melting, T
ifor the temperature of complete melting.
Table 1 mechanical experimental results
。
As can be seen from Table 1, poly(lactic acid)-ester starch-attapulgite matrix material prepared by the present invention has higher tensile strength and flexural strength relative to poly(lactic acid), and water-intake rate also reduces, and is more suitable for processed and applied.
Table 2 thermal analyses test result
。
As can be seen from Table 2, the T of poly(lactic acid)-ester starch-attapulgite matrix material for preparing of the present invention
0and T
itemperature all high than poly(lactic acid), illustrate esterification starch and poly(lactic acid) two-phase interdependent property strengthen.
Although embodiment of the present invention are open as above, but it is not restricted to listed in specification sheets and embodiment utilization, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other amendment, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details.
Claims (7)
1. poly(lactic acid)-ester starch-attapulgite matrix material, is characterized in that, by weight, comprise following component: poly(lactic acid) 48 ~ 58 parts, esterification starch 38 ~ 44 parts, attapulgite 8 ~ 16 parts, alginates 2 ~ 5 parts, glycerine 2 ~ 5 parts, cm-chitosan 1 ~ 3 part and 1 ~ 2 part, softening agent.
2. a kind of poly(lactic acid)-ester starch-attapulgite matrix material according to claim 1, it is characterized in that, by weight, comprise following component: poly(lactic acid) 52 ~ 54 parts, esterification starch 40 ~ 42 parts, attapulgite 10 ~ 12 parts, alginates 3 ~ 4 parts, glycerine 3 ~ 4 parts, cm-chitosan 2 ~ 3 parts and 2 parts, softening agent.
3. a kind of poly(lactic acid)-ester starch-attapulgite matrix material according to claim 1, is characterized in that, by weight, comprise following component: poly(lactic acid) 53 parts, esterification starch 41 parts, attapulgite 11 parts, alginates 3 parts, glycerine 3 parts, cm-chitosan 2 parts and 2 parts, softening agent.
4. a kind of poly(lactic acid)-ester starch-attapulgite matrix material according to any one of claim 1 ~ 3, is characterized in that, described softening agent is one or more in oxalic acid dioctyl ester, triethyl phosphate or acetyl tributyl citrate.
5. a kind of poly(lactic acid)-ester starch-attapulgite matrix material according to any one of claim 1 ~ 3, it is characterized in that, described esterification starch is maleic anhydride esterification starch.
6. a kind of poly(lactic acid)-ester starch-attapulgite matrix material according to any one of claim 1 ~ 3, it is characterized in that, described alginates is sodium alginate.
7., based on the preparation method of a kind of poly(lactic acid)-ester starch-attapulgite matrix material according to claim 1, it is characterized in that, comprise the steps:
(1) cm-chitosan being dissolved in volume fraction is in the acetum of 2 ~ 5%, is mixed with the acetum of cm-chitosan, after stirring, and set aside for use;
(2) attapulgite is dissolved in the deionized water of 3 ~ 5 times of volumes, ultrasonic disperse 5 ~ 10min, obtains attapulgite suspension, set aside for use;
(3) poly(lactic acid) is joined in the acetum of the obtained cm-chitosan of step (1), mix, add attapulgite suspension and surplus stock while stirring, at 60 ~ 65 DEG C, electric stirring makes each composition fully mix, form complex sol, then used casting method film on glass, at 60 ~ 65 DEG C of constant-temperature vacuum drying 24 ~ 30h, namely obtained poly(lactic acid)-ester starch-attapulgite matrix material.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106042502A (en) * | 2016-04-30 | 2016-10-26 | 湖南工业大学 | Environmental friendly packaging film used for fruit and vegetable packaging |
| CN111568884A (en) * | 2020-06-05 | 2020-08-25 | 安徽省昊祥药业有限公司 | Method for preparing Chinese medicinal patch for external use |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103539966A (en) * | 2013-09-22 | 2014-01-29 | 苏州市湘园特种精细化工有限公司 | Biological nano plastic |
| CN103881388A (en) * | 2012-12-21 | 2014-06-25 | 信越化学工业株式会社 | Curable Silicone Resin Composition, Cured Product Thereof And Photosemiconductor Apparatus |
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2015
- 2015-03-31 CN CN201510147751.0A patent/CN104725805A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103881388A (en) * | 2012-12-21 | 2014-06-25 | 信越化学工业株式会社 | Curable Silicone Resin Composition, Cured Product Thereof And Photosemiconductor Apparatus |
| CN103539966A (en) * | 2013-09-22 | 2014-01-29 | 苏州市湘园特种精细化工有限公司 | Biological nano plastic |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106042502A (en) * | 2016-04-30 | 2016-10-26 | 湖南工业大学 | Environmental friendly packaging film used for fruit and vegetable packaging |
| CN111568884A (en) * | 2020-06-05 | 2020-08-25 | 安徽省昊祥药业有限公司 | Method for preparing Chinese medicinal patch for external use |
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Application publication date: 20150624 |