CN102746627B - Polylactic acid and diatomite composite and preparation method thereof - Google Patents
Polylactic acid and diatomite composite and preparation method thereof Download PDFInfo
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- CN102746627B CN102746627B CN201210246773.9A CN201210246773A CN102746627B CN 102746627 B CN102746627 B CN 102746627B CN 201210246773 A CN201210246773 A CN 201210246773A CN 102746627 B CN102746627 B CN 102746627B
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- diatomite
- poly
- lactic acid
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- composite material
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
Abstract
The invention discloses polylactic acid and diatomite composite and a preparation method thereof. The polylactic acid and diatomite composite is obtained by mixing and extruding the following raw materials including, by weight, 60-80 parts of polylactic acid, 20-40 parts of diatomite, 1.2-1.9 parts of plasticizer, 0.2-0.7 part of activator, 1-2 parts of coupling reagent and 0.2-0.3 part of antioxidant. The polylactic acid and diatomite composite obtained can be formed in brown naturally without addition of chemical pigment, is excellent in performance indexes, the tensile breaking strength is 45-70MPa, the tensile modulus ranges from 3500MPa to 4500MPa, the bending strength is 85-110MPa, the bending modulus ranges from 5000MPa to 7000MPa, and heat-resistant temperature can be up to 95 DEG C or above. The polylactic acid and diatomite composite containing diatomite can improve water and fertilizer retention capability of soil after being subjected to biodegradation.
Description
Background technology
The waste that Plastic Packaging Materials produces has caused the concern of the whole society day by day to the negative impact that environment brings, therefore, research and develop all kinds of novel ecological environment-friendly materials and achieve larger progress, some material starts suitability for industrialized production.Such as starch plastics, poly(lactic acid) etc.
Poly(lactic acid) is Poly Lactic Acid(PLA by name entirely), having another name called W-Gum resin, is a kind of polylactide.Poly(lactic acid) is a multiduty high molecular polymer, forms by extracting starch → by fermentation → process manufacture such as anhydrate → be polymerized in plant completely, nontoxicity.Be a kind of reproducible resource, effectively can substitute non-renewable fossil resources.
Degradable plastics is prepared by mineral filler and additive modification poly(lactic acid), it is the problem that scientific research circle in recent years and manufacturing enterprise are researching and solving always, such as number of patent application is 201010169771.5 to disclose " a kind of modified polylactic acid material and preparation method thereof ", wherein mineral filler is starch, talcum powder, mica, calcium carbonate, polynite, one in clay or its mixture, for another example the patent No. is 20109050016.2 to disclose " a kind of polylactic acid degradable material and preparation method thereof ", what wherein mineral filler adopted is talcum powder, mica, calcium carbonate, polynite, clay, due to talcum powder, mica, calcium carbonate, polynite, Clay Density is large, Heavy Weight, generally be only suitable for making membrane-based article.
Diatomite molecular formula SiO
2, by unbodied SiO
2composition, diatomite is generally formed by the dead later silicate remains of the unicellular algae being referred to as diatom, it has the performance of some uniquenesses, as: porousness, lower density, larger surface-area, relative incompressibility and chemical stability, pH value is neutral, nontoxic, suspension property is good, absorption property is strong.
summary of the invention:
Technical problem to be solved by this invention is: for current poly(lactic acid) poor processability, thermotolerance is inadequate, the problem of widespread use can not be met, the limitation of membrane-based article can only be made for current polylactic acid modified product simultaneously, with poly(lactic acid) and diatomite for main raw material through modification, mix, extrude and obtain a kind of matrix material, this matrix material is suitable for the fields such as Industrial products packaging, food product pack, electronic product Neto, gift and toy.Due to the dark brown that diatomite has a kind of pure natural stable, therefore, goods are without the need to carrying out any dyeing or desolventing technology can use, safety, environmental protection.
The present invention is achieved through the following technical solutions:
Poly(lactic acid), diatomite composite material, obtained via mixing, extruding by following raw materials in part by weight;
Poly(lactic acid) 60-80 part diatomite 20-40 part softening agent 1.2-1.9 part promoting agent 0.2-0.7 part coupling agent 1-2 part oxidation inhibitor 0.2-0.3 part.
The further improvement project of the present invention is, described poly(lactic acid) molecular-weight average is 100,000-20 ten thousand.
The present invention further improvement project is, described softening agent is one or more mixing in glycerine, mono-glycerides, sorbyl alcohol.
The present invention further improvement project is, described promoting agent is stearic acid.
The present invention further improvement project is, described coupling agent is one or more mixing in titanic acid ester, Aluminate, aluminium titanium mixture.
The present invention further improvement project is, described oxidation inhibitor is 168 models i.e. three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid esters or is 1010 models i.e. four (β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid).
Prepare the method for above-mentioned poly(lactic acid), diatomite composite material, comprise the steps:
(1) diatomite is passed through sunlight seasoning to water content lower than 10%;
(2) calcine: diatomite is put into incinerator, and calcining temperature controls below 500 DEG C, and the diatomite water content after burning is lower than 1%;
(3) superfine grinding: the diatomite obtaining more than 1000 orders;
(4) by proportioning according to claim 1, poly(lactic acid), diatomite, softening agent, promoting agent, coupling agent, oxidation inhibitor are added in (SRL type) high-speed mixer, mix under 120-130 DEG C of condition, be then cooled to less than 80 DEG C;
(5) mixture step (4) obtained sends into twin screw extruder melt blending, and extrusion temperature 180-230 DEG C, with mould face air cooling butt formula granulating.
The present invention compared with prior art, has following obvious advantage:
One, poly(lactic acid) diatomite composite material of the present invention does not need to add chemical pigment, naturally can become coffee-like.Polymkeric substance of the present invention, due to containing diatomite, can improve soil water-reataining fertilizer-keeping ability after biological degradation.
Two, performance index of the present invention are excellent: tensile break strength (MPa) is 45-70, and tensile modulus (MPa) is 3500-4500, and flexural strength (MPa) is 85-110, and modulus in flexure (MPa) is 5000-7000, and heat resisting temperature reaches more than 95 DEG C.
Embodiment
In the examples below, poly(lactic acid) used is polylactide (PLA), and molecular-weight average is 10-20 ten thousand; Diatomite originates from Shengzhou, Zhejiang Province.
embodiment 1
Get 0.2 part, poly(lactic acid) 60 parts of diatomite 20 parts of softening agent 1.2 portions of promoting agents 0.2 part of coupling agent 1 part of oxidation inhibitor.
Described softening agent is mono stearate glyceryl ester, and described promoting agent is stearic acid, and described coupling agent is titanic acid ester, and described oxidation inhibitor is three ［ 2.4-di-tert-butyl-phenyl ］ phosphorous acid ester.
Its preparation comprises the steps:
(1) diatomite is passed through sunlight seasoning to water content lower than 10%;
(2) calcine: diatomite is put into incinerator, and calcining temperature controls below 500 DEG C, and the diatomite water content after burning is lower than 1%;
(3) superfine grinding: obtain 1200 order diatomite;
(4) by above-mentioned proportioning, poly(lactic acid), diatomite, softening agent, promoting agent, coupling agent, oxidation inhibitor are added in (SRL type) high-speed mixer, mix under 120-130 DEG C of condition, be then cooled to less than 80 DEG C;
(5) mixture step (4) obtained sends into twin screw extruder melt blending, and extrusion temperature 180-230 DEG C, with mould face air cooling butt formula granulating.
By the poly(lactic acid) of the present embodiment, diatomite composite material made into particulate form, and then become goods (such as: cutter, fork etc.) with the injection moulding of this particle.
Through JISK7127 determination of experimental method: tensile break strength (MPa) is 65, tensile modulus (MPa) is 4500, and flexural strength (MPa) is 105, and modulus in flexure (MPa) is 6000, heat resisting temperature 90 DEG C.
embodiment 2
Get 0.3 part, poly(lactic acid) 70 parts of diatomite 30 parts of softening agent 1.5 portions of promoting agents 0.5 part of coupling agent 1.5 parts of oxidation inhibitor.
Described softening agent is glycerine and mono-glycerides mixture, can mix in any proportion, presses 1:1 mixing in the present embodiment; Described promoting agent is stearic acid; Described coupling agent is Aluminate, and described oxidation inhibitor is four (β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid).
All the other are implemented as embodiment 1.
By the poly(lactic acid) of the present embodiment, diatomite composite material made into particulate form, and then become goods (such as: cutter, fork, cup, bowl etc.) with the injection moulding of this particle.
Through JISK7127 determination of experimental method: tensile break strength (MPa) is 70, tensile modulus (MPa) is 4500, and flexural strength (MPa) is 110, and modulus in flexure (MPa) is 6000, heat resisting temperature 95 DEG C.
The poly(lactic acid) that embodiment 1 obtains, diatomite composite material, with talcum powder, lactic acid composite material (with the diatomite in talcum powder alternate embodiment 1, all the other conditions are constant), Testing index contrast is under the same conditions as follows:
| Talcum powder poly(lactic acid) | Diatomite poly(lactic acid) | |
| Tensile break strength (MPa) | 48 | 65 |
| Tensile modulus (MPa) | 3000 | 4500 |
| Flexural strength (MPa | 83 | 105 |
| Modulus in flexure (MPa) | 3828 | 6000 |
| Heat resisting temperature | 65 | 90 |
| Finished color | White | Natural coffee look |
The data provided from above-mentioned table are known, and indices of the present invention is all better than talcum powder, lactic acid composite material, are applicable to making disposable tableware, or make the storage bag mounted box etc. of some materials.As " due to containing diatomite, improving soil water-reataining fertilizer-keeping ability after biological degradation " described in advantage above, simultaneously with poly(lactic acid), diatomite composite material that diatomite is prepared as additive, raw material is easy to get, with low cost.
Claims (2)
1. the preparation method of poly(lactic acid), diatomite composite material, is characterized in that: following raw materials in part by weight obtains via mixing, extruding;
Poly(lactic acid) 60-80 part diatomite 20-40 part softening agent 1.2-1.9 part promoting agent 0.2-0.7 part coupling agent 1-2 part oxidation inhibitor 0.2-0.3 part;
Described matrix material obtains through following preparation process:
(1) diatomite is passed through sunlight seasoning to water content lower than 10%;
(2) calcine: diatomite is put into incinerator, and calcining temperature controls below 500 DEG C, and the diatomite water content after calcining is lower than 1%;
(3) superfine grinding: the diatomite obtaining more than 1000 orders;
(4) by described proportioning, poly(lactic acid), diatomite, softening agent, promoting agent, coupling agent, oxidation inhibitor are added in high-speed mixer, mixes under 120-130 DEG C of condition, be then cooled to less than 80 DEG C;
(5) mixture step (4) obtained sends into twin screw extruder melt blending, and extrusion temperature 180-230 DEG C, with mould face air cooling butt formula granulating.
2. the preparation method of poly(lactic acid) as claimed in claim 1, diatomite composite material, is characterized in that: described poly(lactic acid) molecular-weight average is 100,000-20 ten thousand.
3. the preparation method of poly(lactic acid) as claimed in claim 1, diatomite composite material, is characterized in that: described softening agent is one or more mixing in glycerine, mono-glycerides, sorbyl alcohol.
4. the preparation method of poly(lactic acid) as claimed in claim 1, diatomite composite material, is characterized in that: described promoting agent is stearic acid.
5. the preparation method of poly(lactic acid) as claimed in claim 1, diatomite composite material, is characterized in that: described coupling agent is one or more mixing in titanic acid ester, Aluminate, aluminium titanium mixture.
6. the preparation method of poly(lactic acid) as claimed in claim 1, diatomite composite material, is characterized in that: described oxidation inhibitor is 168 models or is 1010 models.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210246773.9A CN102746627B (en) | 2012-07-17 | 2012-07-17 | Polylactic acid and diatomite composite and preparation method thereof |
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| CN201210246773.9A CN102746627B (en) | 2012-07-17 | 2012-07-17 | Polylactic acid and diatomite composite and preparation method thereof |
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| CN106189146A (en) * | 2016-08-29 | 2016-12-07 | 佛山市高明区尚润盈科技有限公司 | A kind of preparation method of polylactic acid antibacterial matrices |
| CN106519619A (en) * | 2016-11-24 | 2017-03-22 | 安徽省天乐塑业有限公司 | Food packaging film and preparation method thereof |
| CN111548617B (en) * | 2020-06-24 | 2022-11-04 | 南方科技大学 | Biodegradable polylactic acid material and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100999587A (en) * | 2006-12-25 | 2007-07-18 | 刘津平 | Biological whole degrading film and mfg. process of its material |
| CN102453320A (en) * | 2010-10-25 | 2012-05-16 | 中国石油化工股份有限公司 | Polylactic acid composition for environmentally-friendly synthetic paper and preparation method thereof |
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| US6583189B1 (en) * | 2002-05-07 | 2003-06-24 | Nien Made Enterprise Co., Ltd. | Strengthened thermoplastic |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100999587A (en) * | 2006-12-25 | 2007-07-18 | 刘津平 | Biological whole degrading film and mfg. process of its material |
| CN102453320A (en) * | 2010-10-25 | 2012-05-16 | 中国石油化工股份有限公司 | Polylactic acid composition for environmentally-friendly synthetic paper and preparation method thereof |
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