CN105860111A - Preparation method of microalgae-based polymer composite thin film - Google Patents
Preparation method of microalgae-based polymer composite thin film Download PDFInfo
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- CN105860111A CN105860111A CN201610249527.7A CN201610249527A CN105860111A CN 105860111 A CN105860111 A CN 105860111A CN 201610249527 A CN201610249527 A CN 201610249527A CN 105860111 A CN105860111 A CN 105860111A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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
- C08L89/00—Compositions of proteins; Compositions of derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2389/00—Characterised by the use of proteins; Derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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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
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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Abstract
The invention relates to a preparation method of a microalgae-based polymer composite thin film. The preparation method comprises the following steps of mixing a microalgae homogeneous phase water solution, a water soluble polymer homogeneous phase water solution and a plasticizer according to the dry weight mass ratio of 1:(0.1-0.9):(0.1-0.3), so as to obtain a casting liquid; stirring for 0.8-1.2h, and defoaming the casting liquid, so as to obtain a foam-free casting liquid; casting the foam-free casting liquid to a flat plate, heating the cast flat plate according to programs, and drying, so as to obtain the microalgae-based polymer composite thin film. The microalgae-based polymer composite thin film prepared by the preparation method has the advantages that the environment-friendly effect is realized, the toxicity is low or avoided, and the degradability is realized.
Description
Technical field
The present invention relates to the preparation method of a kind of microalgae based polyalcohol laminated film, be specifically related to the preparation method of the microalgae based polyalcohol laminated film of a kind of strong mechanical performance, belong to the comprehensive utilizating research field of natural biomass.
Background technology
Microalgae be a class on land, ocean widely distributed, autophyte that availability nutritious, photosynthetic is high, it is of a great variety, it is possible to the microalgae of mass propgation or production mainly has the chlorella of the spirulina of Cyanophyta, Chlorophyta.According to the literature, in spirulina, gross protein value is more than 50%, and in chlorella, crude protein content is more than 60%, and oneself is used as one of protein main source；Additionally, algae has preferable adsorption effect and for sewage disposal to metal ion；Microalgae such as spirulina, chlorella oil content are higher, Bioresource technology,
Itself and polymer copyrolysis are improved the productivity of biodiesel by 2011,102,11018.But, the application of microalgae is mostly in fields such as food, health product, biodiesel, if prepare various functional material will widen its range of application undoubtedly by compound to microalgae and polymer.But document reports the composite of other biomass such as starch, lignin, soybean protein etc. and polymer mostly, but the only very small amount research of microalgae polymer composites is in the news.
Journal
Of polymers and the environment, 2012,20,124 using Sargassum and wood powder as function ingredients, in dry powder form with polyethylene, polypropene blended be prepared for Sargassum content spin-coated thin film within 3% and injection batten, but result of study finds that the elongation at break of this composite and mechanical property decay are obvious, and fracture strength is 19MPa, and elongation at break is only 10%；Journal of
Applied polymer science, 2013,130,3263 think that microalgae is difficult to hot melt, therefore are directly mixed with polyethylene by spirulina powder, extruded or injection moulding process be prepared for spirulina, chlorella content from 0% to 60% microalgae composite polyethylene material.Its result of study shows, spirulina is preferably and polyethylene is combined, but the problem that spirulina composite polyethylene material elongation at break is low achieves a solution (during spirulina content 50% not yet, elongation at break only has 7%), this will have a strong impact on the mechanical property of material mainly due to only spirulina powder and Material cladding through break process due to size and addition problem, and spirulina carries out function ingredients and extracts and be undoubtedly material cost that is loaded down with trivial details and expensive and that make preparation and drastically rise preparing composite.
Analyze the document report seen, when microalgae is used for preparing polymer composites, microalgae is the most untreated and directly uses, therefore contain that the polymer composites molding of microalgae uses blending extrusion method and preparation substantially is block materials, and prepared sample is mechanical property extreme difference when high microalgae content.The present invention carries out water-soluble anticipating to microalgae, then prepares thin film by compound to itself and polymer by solution casting method, has expanded the preparation method of microalgae based polymer composite, the mechanical property of laminated film when improve high microalgae content.Furthermore it is known that microalgae polymer composites all using polymer as matrix material, have no the research report using microalgae to prepare composite as matrix material.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of microalgae based polyalcohol laminated film, the microalgae based polyalcohol laminated film that the method obtains is with microalgae as matrix material, and product has fracture strength and the high feature of elongation at break.
The preparation method of a kind of microalgae based polyalcohol laminated film that the present invention provides, the method be by microalgae homogeneous phase aqueous solution, water-soluble polymer homogeneous phase aqueous solution and plasticizer in dry weight than 1:0.1～0.9:0.1～0.3 ratio mixing acquisition pour liquid, to pour liquid after stirring 0.8～1.2h to carry out deaeration process and obtain still pouring liquid, the still liquid that pours is poured on flat board, flat board after pouring is drying to obtain microalgae based polyalcohol laminated film through temperature programming, wherein:
This microalgae homogeneous phase aqueous solution uses following method to prepare:
Microalgae dry powder and the deionized water of by drying, pulverizing, cross 80 mesh sieves are configured to the aqueous solution that mass concentration is 2～15%, this aqueous solution is warming up under stirring condition 45～85 DEG C and is dissolved to homogeneous, be down to room temperature and get final product；
This microalgae homogeneous phase aqueous solution makes employing casting method prepare microalgae based polymer film to be possibly realized, when microalgae homogeneous phase aqueous solution carries out mixing with aqueous solutions of polymers and pours film forming, make microalgae component in this microalgae thin film become equally distributed continuous phase, and then make the mechanical property of microalgae based polymer film be significantly improved.
This water-soluble polymer homogeneous phase aqueous solution uses following method to prepare:
Water-soluble polymer powder or granule and deionized water are configured to the aqueous solution that mass concentration is 2～15%, under stirring condition, this aqueous solution are warming up to 50～95 DEG C and are dissolved to transparent homogeneous, be down to room temperature and get final product.
In above-mentioned, this water-soluble polymer is the one in Polyethylene Glycol, polyvinyl alcohol, polymethylacrylic acid, polyacrylamide and sodium alginate.
In above-mentioned, this microalgae is spirulina, chlorella, Dunaliella salina and the one split in kettle algae.
In above-mentioned, this plasticizer is a kind of in glycerol, ethylene glycol, epoxy soybean oil, dioctyl phthalate or the mixture of any two.
In above-mentioned, deaeration processes and uses vacuum defoamation or use defoamer to carry out deaeration.
One in above-mentioned, during wherein defoamer is emulsified silicone oil, the fatty acid ester compounded thing of higher alcohols, polyoxyethylene, n-butyl alcohol, polyoxypropylene, tetramethylolmethane ether, polypropylene glycerol aether and polyoxyethylene glycerol ether.
In above-mentioned, this flat board is the one in glass plate, polycarbonate plate, polytetrafluoroethylene and silicone rubber flat board.
In above-mentioned, the operational approach that temperature programming is dried is: initial drying temperature >=50 DEG C, and the baking temperature of the upper limit is≤120 DEG C；Heat up 10 DEG C per hour.
The present invention uses that water-soluble polymer and microalgae are compound to be prepared thin film and have no that correlational study is reported.
The present invention uses microalgae to prepare microalgae based polyalcohol laminated film as the matrix material of thin film and has no research report.
The product that the preparation method of a kind of microalgae based polyalcohol laminated film that the present invention provides obtains has fracture strength and the high clear superiority of elongation at break.
Detailed description of the invention
The following examples are to further illustrate the present invention rather than limit the scope of the present invention.Microalgae powder used in embodiment, is drying, pulverizes, crosses 80 mesh sieves and obtain.
Embodiment 1:
In the single port flask of 100ml, add 20g spirulina homogeneous phase aqueous solution, 6g polyvinyl alcohol homogeneous phase aqueous solution, the glycerol of 0.6g, i.e. dry weight ratio for 1:0.3:0.3, stir 1 hour under room temperature, it is thus achieved that pour liquid；Liquid will be poured and be placed in vacuum drying oven process until pouring liquid surface without obvious bubble, obtain still pouring liquid, the still liquid that pours is poured on polycarbonate plate after levelling temperature programming again and is dried, and drying condition is: initial drying temperature 50 DEG C, 60 DEG C/1h, 70 DEG C/1h, 80 DEG C/1h, 90 DEG C/1h, 100 DEG C/1h and 110 DEG C/1h, i.e. heat up 10 DEG C per hour by initial drying temperature 50 DEG C, until being warming up to 110 DEG C.Dried thin film takes off to be placed in exsiccator and saves backup.
Spirulina homogeneous phase aqueous solution uses following method to prepare:
In 100ml single port flask, add 90g deionized water and 10g spirulina powder is configured to the spirulina aqueous solution that mass concentration is 10%, under stirring, this aqueous solution is warming up to 60 DEG C and is dissolved to homogeneous phase aqueous solution, be down to room temperature and get final product.
Polyvinyl alcohol homogeneous phase aqueous solution uses following method to prepare:
In 100ml single port flask, add 90g deionized water and 10g granule of polyvinyl alcohol is configured to the polyvinyl alcohol water solution that mass concentration is 10%, under stirring condition, this aqueous solution is warming up to 95 DEG C and is dissolved to transparent homogeneous phase aqueous solution, be down to room temperature and get final product.
Embodiment 2:
Middle parts different from embodiment 1 are that the dry weight of spirulina homogeneous phase aqueous solution, polyvinyl alcohol homogeneous phase aqueous solution and glycerol is than for 1:0.7:0.3.
Comparing embodiment 1 and embodiment 2:
In embodiment 1 and embodiment 2, spirulina dry weight: polyvinyl alcohol dry weight: glycerol dry weight is respectively 1:0.3:0.3 and 1:0.7:0.3, the thin film hot strength that embodiment 1 obtains is 6MPa, and the thin film hot strength that embodiment 2 obtains is 26MPa, elongation at break is 15%, higher than document Journal of
Polymers and the environment, 2012,20,124(19MPa, 10%)；Journal of
Applied polymer science, 2013,130,3263(2.5MPa, 7%) thin film mechanical performance with polymer as matrix reported；The carbon left of embodiment 1 and 2 is all more than 10%, but in embodiment 2, the introducing of polyvinyl alcohol makes it be down to 16% at the carbon left of 700 DEG C by the 19% of embodiment 1.
Embodiment 3:
In the single port flask of 100ml, add 20g spirulina homogeneous phase aqueous solution, 14g polyvinyl alcohol homogeneous phase aqueous solution, the glycerol of 0.6g, i.e. dry weight ratio for 1:0.7:0.3, stir 1 hour under room temperature, it is thus achieved that pour liquid；Adding the n-butyl alcohol of 50 μ l in pouring liquid and continue stirring to pouring liquid surface without obvious bubble, obtain still pouring liquid, the still liquid that pours is poured on polycarbonate plate after levelling temperature programming again and is dried, drying condition is with embodiment 1.
Wherein, the preparation of polyvinyl alcohol homogeneous phase aqueous solution and spirulina homogeneous phase aqueous solution is with embodiment 1.
Comparing embodiment 2 and embodiment 3:
The thin film hot strength that embodiment 2 obtains is 26MPa；Embodiment 3 obtain thin film hot strength be 20MPa, i.e. use n-butyl alcohol be defoamer carry out froth breaking will reduce laminated film mechanical property.While it is true, the mechanical property of embodiment 3 remains above Journal of polymers and the environment, 2012,20,124(19MPa, 10%)；Journal of applied polymer science, 2013,130,3263(2.5MPa, 7%) data with polymer as matrix of report in document.
Embodiment 4:
In the single port flask of 100ml, add 20g chlorella homogeneous phase aqueous solution, 14g polyvinyl alcohol homogeneous phase aqueous solution, the glycerol of 0.6g, i.e. dry weight ratio for when stirring 1 is little under 1:0.7:0.3 room temperature, it is thus achieved that pour liquid；To pour liquid and be placed in vacuum drying oven process until pouring liquid surface without obvious bubble, and obtain still pouring liquid, the still liquid that pours is poured on polycarbonate plate after levelling temperature programming again and is dried, drying condition is with embodiment 1.
The preparation of polyvinyl alcohol homogeneous phase aqueous solution is with embodiment 1.
Chlorella homogeneous phase aqueous solution uses following method to prepare:
100ml single port flask adds 90g deionized water and 10g chlorella powder, is configured to the chlorella aqueous solution that mass concentration is 10%, under stirring condition, this aqueous solution is warming up to 80 DEG C and is dissolved to into homogeneous phase aqueous solution, be down to room temperature and get final product.
Comparing embodiment 3 and embodiment 4:
Embodiment 4 uses chlorella to be microalgae component, the hot strength of the polymer composite film obtained is 23MPa, and elongation at break is 14%, the laminated film using spirulina to be microalgae component higher than embodiment 3, higher than Journal of polymers and the environment
2012,20,124(19MPa, 10%)；Journal of applied polymer science, 2013,130,3263(2.5MPa, 7%) mechanical performance data with polymer as matrix of reported in literature.This is better than the compatibility of each component of spirulina and water-soluble polymer mainly due to the compatibility of each component of chlorella Yu water-soluble polymer.
Embodiment 5
In the single port flask of 100ml, add 20g sodium alginate homogeneous phase aqueous solution, 2g spirulina homogeneous phase aqueous solution, the glycerol of 0.18g, i.e. dry weight ratio for 1:0.3:0.3, stir 1 hour under room temperature, it is thus achieved that pour liquid；To pour liquid and be placed in vacuum drying oven process until pouring liquid surface without obvious bubble, and obtain still pouring liquid, the still liquid that pours is poured on polycarbonate plate after levelling temperature programming again and is dried, drying condition is with embodiment 1.
Spirulina homogeneous phase aqueous solution uses following method to prepare:
In 100ml single port flask, add 91g deionized water and 9g spirulina powder, be configured to the spirulina aqueous solution that mass concentration is 9%, under stirring condition, this aqueous solution be warming up to 60 DEG C and be dissolved to homogeneous phase aqueous solution, be down to room temperature and get final product.
Sodium alginate homogeneous phase aqueous solution uses following method to prepare:
In 100ml single port flask, add 97g deionized water and 3g sodium alginate, be configured to the sodium alginate aqueous solution that mass concentration is 3%, under stirring condition, this aqueous solution be warming up to 55 DEG C and be dissolved to transparent homogeneous phase aqueous solution, be down to room temperature and get final product.
Embodiment 6:
Middle parts different from embodiment 1 are that the dry weight of spirulina homogeneous phase aqueous solution, polyvinyl alcohol homogeneous phase aqueous solution and glycerol is than for 1:0.5:0.3.
Embodiment 7:
Middle parts different from embodiment 1 are that the dry weight of spirulina homogeneous phase aqueous solution, polyvinyl alcohol homogeneous phase aqueous solution and glycerol is than for 1:0.9:0.3.
The hot strength of the spirulina polyethylene that embodiment 7 obtains is 26.5MPa, and elongation at break is 43.5%, higher than Journal of
Polymers and the environment, 2012,20,124(19MPa, 10%)；Journal of
Applied polymer science, 2013,130,3263(2.5MPa, 7%) data of reported in literature.
Claims (8)
1. the preparation method of a microalgae based polyalcohol laminated film, it is characterized in that, the method be by microalgae homogeneous phase aqueous solution, water-soluble polymer homogeneous phase aqueous solution and plasticizer in dry weight than 1:0.1～0.9:0.1～0.3 ratio mixing acquisition pour liquid, to pour liquid after stirring 0.8～1.2h to carry out deaeration process and obtain still pouring liquid, the still liquid that pours is poured on flat board, flat board after pouring is drying to obtain microalgae based polyalcohol laminated film through temperature programming, wherein:
This microalgae homogeneous phase aqueous solution uses following method to prepare:
Microalgae dry powder and the deionized water of by drying, pulverizing, cross 80 mesh sieves are configured to the aqueous solution that mass concentration is 2～15%, this aqueous solution is warming up under stirring condition 45～85 DEG C and is dissolved to homogeneous, be down to room temperature and get final product；
This water-soluble polymer homogeneous phase aqueous solution uses following method to prepare:
Water-soluble polymer powder or granule and deionized water are configured to the aqueous solution that mass concentration is 2～15%, under stirring condition, this aqueous solution are warming up to 50～95 DEG C and are dissolved to transparent homogeneous, be down to room temperature and get final product.
The preparation method of a kind of microalgae based polyalcohol laminated film the most according to claim 1, it is characterised in that this water-soluble polymer is the one in Polyethylene Glycol, polyvinyl alcohol, polymethylacrylic acid, polyacrylamide and sodium alginate.
The preparation method of a kind of microalgae based polyalcohol laminated film the most according to claim 1, it is characterised in that this microalgae is spirulina, chlorella, Dunaliella salina and the one split in kettle algae.
The preparation method of a kind of microalgae based polyalcohol laminated film the most according to claim 1, it is characterised in that this plasticizer is a kind of in glycerol, ethylene glycol, epoxy soybean oil, dioctyl phthalate or the mixture of any two.
The preparation method of a kind of microalgae based polyalcohol laminated film the most according to claim 1, it is characterised in that deaeration processes and uses vacuum defoamation or use defoamer to carry out deaeration.
The preparation method of a kind of microalgae based polyalcohol laminated film the most according to claim 5, it is characterized in that, the one during wherein defoamer is emulsified silicone oil, the fatty acid ester compounded thing of higher alcohols, polyoxyethylene, n-butyl alcohol, polyoxypropylene, tetramethylolmethane ether, polypropylene glycerol aether and polyoxyethylene glycerol ether.
The preparation method of a kind of microalgae based polyalcohol laminated film the most according to claim 1, it is characterised in that this flat board is the one in glass plate, polycarbonate plate, polytetrafluoroethylene and silicone rubber flat board.
The preparation method of a kind of microalgae based polyalcohol laminated film the most according to claim 1, it is characterised in that the operational approach that temperature programming is dried is: initial drying temperature >=50 DEG C, and the baking temperature of the upper limit is≤120 DEG C；Heat up 10 DEG C per hour.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107057247A (en) * | 2017-01-23 | 2017-08-18 | 江苏省农业科学院 | A kind of degradable blue-green algae base biological plastics and preparation method thereof |
| CN109942870A (en) * | 2019-04-01 | 2019-06-28 | 广东石油化工学院 | A kind of preparation method of the biomass combined film of polyvinyl alcohol of branch-line polymer brush protection |
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| CN102414267A (en) * | 2009-04-28 | 2012-04-11 | 金伯利-克拉克环球有限公司 | Algae-blended compositions for thermoplastic articles |
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| CN107057247A (en) * | 2017-01-23 | 2017-08-18 | 江苏省农业科学院 | A kind of degradable blue-green algae base biological plastics and preparation method thereof |
| CN109942870A (en) * | 2019-04-01 | 2019-06-28 | 广东石油化工学院 | A kind of preparation method of the biomass combined film of polyvinyl alcohol of branch-line polymer brush protection |
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