CN107365421A - The preparation method of the biodegradable composite plastic films of bacteria cellulose/PVA - Google Patents
The preparation method of the biodegradable composite plastic films of bacteria cellulose/PVA Download PDFInfo
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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
- C08L29/00—Compositions 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; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
- C08L29/02—Homopolymers or copolymers of unsaturated alcohols
- C08L29/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2329/00—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
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—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
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/02—Cellulose; Modified cellulose
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2201/00—Properties
- C08L2201/06—Biodegradable
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/16—Applications used for films
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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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Abstract
The invention discloses a kind of preparation method of the biodegradable composite plastic films of bacteria cellulose/PVA, bacteria cellulose is fully broken, BC slurries are obtained after adding a small amount of distilled water diluting stirring, a period of time is blended under 90 DEG C of water-baths with the PVA aqueous solution prepared in advance；Take a certain amount of starch and a small amount of distilled water to be placed in three-necked flask, be gelatinized under similarity condition, after 30min is blended with above-mentioned PVA systems, adds certain content plasticizer and continue after reacting 45 60min vacuum defoamations, the casting film-forming on flat board.Bacteria cellulose/PVA composite plastic films prepared by this method have excellent mechanical property, and its tensile strength reaches 55.47MPa, improves 47.61% compared to pure PVA film, film elongation at break rate reaches 241.29%, and angle tear strength reaches 127.87MPa.
Description
Technical field
The invention belongs to new material technology field, is related to PVA plastic sheetings, and it is high-strength to be prepared by a kind of solution casting method by it
Spend the biodegradable composite plastic films of bacteria cellulose/PVA.
Background technology
With a large amount of uses of plastic sheeting in people's daily life, increasing high molecule plastic is produced shaping
To meet the market demand, the thing followed is exactly that plastic refuse brings " white pollution " of people and is on the rise.PVA conducts
Can degradable high polymer material have also been used to prepare biodegradable plastic film, because it has good film forming
Property and degradability, can be with degradable for H in biotic environment2O and CO2, gradually weighed in packaging and new material technology field
Depending on.But pure PVA film quality is excessively soft, and mechanical strength is not high, yielding in the production and use process, to a certain degree
On greatly limit the scope of application of PVA film, so it is new material technology in recent years that the enhancing for PVA plastic sheetings, which is modified,
The important topic of research.
Because bacteria cellulose (BC) is a kind of biosynthesis raw material, there is high-crystallinity, high-tensile, high resiliency mould
Amount and good biocompatibility, are obtained for extensively in biological medicine, food industry and papermaking material etc. at present
General application.And BC has excellent three dimensions reticular fiber structure, its fiber surface with the presence of great amount of hydroxy group, can break BC again
Obtained slurries and PVA aqueous solution homogeneous blends after broken, and the alcoholic extract hydroxyl group phase interaction contained using BC this architectural characteristic with PVA
With the two forms intermolecular hydrogen bond, can lift the mechanical strength of PVA film, and and can is enough greatly cut to a certain extent
Water solubility after weak PVA film forming.Therefore, the biodegradable composite plastic of high intensity is prepared using bacteria cellulose enhancing PVA
Expect film, both expanded the application of PVA film, meet the Research Prospects of current environmentally friendly high polymer material again, it is right
There is highly important directive significance in the research of field of material technology.
By retrieval, following Patents are found：
CN101948597B discloses a kind of method that wet method prepares bacteria cellulose/polyvinyl alcohol composite membrane, including：
(1) bacteria cellulose is placed in the container for filling water, crushed using mechanical system, obtain bacteria cellulose homogenate；(2) measure is thin
The moisture content of fungin homogenate；(3) it is 5%~20% PVAC polyvinylalcohol to be configured into mass percentage concentration with distilled water
The aqueous solution；(4) the bacteria cellulose homogenate using moisture content as 93v/v%~99v/v% and concentration are the poly- of 5wt%~20wt%
The uniform mixing of vinyl alcohol aqueous solution in mass ratio 1: 1~15；(5) mixture solution is uniformly spread in a mold, after deaeration
Place at room temperature 12~36 hours, then between pH is 1.0~5.0, temperature is 65 DEG C~95 DEG C of supersaturated salt solution
After middle solidification forming, the aldehyde solution that concentration is 20wt%~40wt% is added, carries out 10~60min of crosslinking, bacterial fibers are made
Element/composite membrane of polyvinyl alcohol, with deionized water rinsing composite membrane to neutrality.
CN102961784B discloses a kind of bacteria cellulose/polyvinyl alcohol composite and its preparation method and application,
Comprise the following steps：(1) preparation of medical bacterial cellulose wet-coating block；(2) preparation of Polymer Solution：In high temperature 95~130
DEG C, under conditions of 0.05~0.15MPa of high pressure, prepare the polyvinyl alcohol water solution of mass concentration 20~40%, as macromolecule
Solution；(3) bacterial cellulose wet-coating block dipping Polymer Solution：(4) freeze thawing is crosslinked, and forms composite.Prepared by the present invention
PVA/BC composite series materials, when PVA concentration reaches 20%, modulus of compressibility reaches more than 30MPa, and especially PVA concentration reaches
During to 28%, modulus of compressibility reaches more than 50MPa, available for preparing the alternative of meniscus or cartilaginous tissue, or prepares first quarter moon
The reparation product of plate or cartilaginous tissue, the mechanical strength needs of the bearing type tissue such as cartilage, meniscus can be met.
CN101570616A discloses a kind of bacteria cellulose/polyvinyl alcohol plural gel material and preparation method thereof, step
Suddenly it is：(1) polyvinyl alcohol is put into deionized water and stirred, after solution into after transparent, poly-vinyl alcohol solution is made；(2) poly-
Bacterial cellulose wet-coating is added in glycohol solution, the poly-vinyl alcohol solution containing bacterial cellulose wet-coating is put into rotary evaporation
In device, using rotating pressure-decreasing distillating method, the water in bacterial cellulose wet-coating is interpenetrated with poly-vinyl alcohol solution and reach flat
Weighing apparatus；(3) polyvinyl alcohol bacterial cellulose wet-coating is taken out to be put into household freezer and slowly freezed, then taken out, place into incubator
In slowly heating thaw, the speed of freeze-thaw is 0.1~1 DEG C/min；(4) by step (3) repetitive cycling 3-6 times, that is, it is made
Bacteria cellulose/polyvinyl alcohol plural gel material finished product.
The PVA composites that above-mentioned three patents obtain in spite of certain excellent performance but can not all be reprocessed with
Post forming, it can only be molded in composite preparation process；The PVA that the inventive method obtains fully is plasticized, and can be carried out
It is processed further, end article is obtained by way of extruding or being molded, the scope of application is wider.
The content of the invention
It is biodegradable multiple that high-intensity fine fungin/PVA is prepared it is an object of the invention to provide a kind of solution casting method
Close plastic sheeting.
To achieve these goals, the technical solution adopted by the present invention is：
A kind of preparation method of the biodegradable composite plastic films of bacteria cellulose/PVA, comprises the following steps：
(1) bacteria cellulose is prepared；
(2) bacteria cellulose for preparing step (1) is fully broken, and BC slurries are obtained after adding distilled water diluting stirring；
A period of time is blended with the PVA aqueous solution prepared in advance in BC slurries after dilution under 90 DEG C of water-baths；
(3) take a certain amount of starch and a small amount of distilled water to be placed in three-necked flask, be gelatinized under 80-90 DEG C of water-bath, it is and above-mentioned
After PVA systems blending 30-90min, add plasticizer and continue vacuum defoamation after reaction 45-60min, the casting film-forming on flat board.
80-90 DEG C of temperature range is the more satisfactory temperature that PVA dissolves in water, to the shadow of film in this temperature range
Ring less, can be adjusted using time temperature equivalence passage time；Time minimum 30min is blended, otherwise starch can not be gelatinized
Completely, plasticizer can not also play plastication completely, but also unsuitable long.
Moreover, the mass ratio of PVA and starch is 6 in casting solution：4-9：1.
Moreover, the addition of bacteria cellulose is the 0.1-2wt% of PVA total amounts.
Moreover, plasticizer is glycerine, caprolactam, polyethylene glycol, one or more of mixtures of Tween 80.
Moreover, the content of plasticizer is the 10-50wt% of PVA total amounts in PVA casting solutions.
Moreover, the preparation method of bacteria cellulose is：With glucose, peptone, dusty yeast, disodium hydrogen phosphate, acetic acid etc.
Prepare bacterial liquid culture medium according to a certain percentage for raw material, be inoculated with acetobacter in the medium after high-temperature sterilization, by liquid
Body culture medium 30 DEG C of temperature, humidity 50% biochemical cultivation case in stand 10-15 days, obtain bacteria cellulose.
The beneficial effects of the invention are as follows：
(1) present invention cooperates with starch with bacteria cellulose by a certain percentage is added in casting solution, and the bacterium of preparation is fine
Dimension element/PVA composite plastic films have excellent mechanical property, and its tensile strength reaches 55.47MPa, is carried compared to pure PVA film
47.61% is risen, elongation at break reaches 241.29%, and angle tear strength reaches 127.87MPa.
(2) present invention by being blended obtained casting solution in the solution by BC and PVA, so as to be obtained using solution casting method
The method of PVA composite plastic films, there is the advantages that experiment condition is easy, easy to implement the method, system is simple.
(3) the PVA composite membranes that the present invention obtains can be by carrying out secondary operation after melting.
Brief description of the drawings
Fig. 1 is that the DSC of laminated film of the present invention schemes；
Fig. 2 is that starch, influence figure of its content to film tensile strength is used alone；
Fig. 3 is that BC, influence figure of its content to film tensile strength is used alone；
Fig. 4 is that fixed content of starch is 10%, influence figure of the different BC additions to film tensile strength.
Embodiment
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention
Content is not limited solely to the following examples.
Prepare bacteria cellulose：
Specific formula is following (mass fraction)：Distilled water 1000ml, glucose 25g (2.5%), peptone 10g (1%),
Dusty yeast 7.5g (0.75%), disodium hydrogen phosphate 10g (1%), acetic acid 10ml (1%) prepares bacterial liquid culture medium, through high temperature
Acetobacter is inoculated with after sterilizing in the medium, by fluid nutrient medium 30 DEG C of temperature, humidity 50% biochemical cultivation case in it is quiet
Put 10-15 days, obtain homemade bacteria cellulose.
Embodiment 1：
Bacteria cellulose is fully beaten, obtains BC slurries after adding the stirring of 10g distilled water dilutings, wherein BC contents are
The 0.8% of PVA total amounts, the common 65g of the aqueous solution for being 9g with the PVA contents being pre-configured with are blended 30min under 90 DEG C of water-baths, take 1g
Starch and 15g distilled water are placed in three-necked flask, after being gelatinized under 80 DEG C of -90 DEG C of water-baths, 100g blendings common with above-mentioned PVA systems
After 30min, add 3g glycerine and continue after reacting 45-60min vacuum defoamations, the casting film-forming on flat board.The tensile strength of the film
It is 55.47MPa；Elongation at break 241.29%, angle tear strength 127.87MPa.
Embodiment 2：
Bacteria cellulose is fully beaten, obtains BC slurries after adding the stirring of 10g distilled water dilutings, wherein BC contents are
The 1% of PVA total amounts, the common 60g of the aqueous solution for being 7g with the PVA contents being pre-configured with are blended 30min under 90 DEG C of water-baths, take 3g to form sediment
Powder and 20g distilled water are placed in three-necked flask, after being gelatinized under 80 DEG C of -90 DEG C of water-baths, 100g blendings common with above-mentioned PVA systems
After 30min, add 2g polyethylene glycol and continue after reacting 45-60min vacuum defoamations, the casting film-forming on flat board.The stretching of the film
Intensity is 21.32MPa；Elongation at break 192.36%, angle tear strength 106.27MPa.
Embodiment 3：
Bacteria cellulose is fully beaten, obtains BC slurries after adding the stirring of 10g distilled water dilutings, wherein BC contents are
The 1% of PVA total amounts, the common 60g of the aqueous solution for being 8g with the PVA contents being pre-configured with are blended 30min under 90 DEG C of water-baths, take 2g to form sediment
Powder and 20g distilled water are placed in three-necked flask, after being gelatinized under 80 DEG C of -90 DEG C of water-baths, 100g blendings common with above-mentioned PVA systems
After 30min, add 3g glycerine and 1g caprolactams continue after reacting 45-60min vacuum defoamations, the casting film-forming on flat board.Should
The tensile strength of film is 30.82MPa；Elongation at break 328.15%, angle tear strength 113.39MPa.
Fig. 1 is that the DSC of laminated film of the present invention schemes, and terrace part is more obvious, illustrates that plasticizing effect protrudes.
Bacteria cellulose and starch cis-trans isomerism each other, both are different in space arrangement, determine both hydroxyls in sky
Between distribution it is different.Both are added in PVA simultaneously, PVA intramolecular hydrogen bonds can be effectively reduced.Stretching with regard to composite membrane is strong
For degree, the tensile strength of pure PVA film increases, the tensile strength of composite membrane after 37.5Mpa, addition starch with content of starch
Can decline successively, during content of starch 10%, tensile strength 30MPa, when increasing to 40%, tensile strength can as little as 15MPa, such as
Shown in Fig. 2.When being individually added into bacteria cellulose, bacterial fibers cellulose content from 0.2% increase to 1% when, the stretching of composite membrane is strong
Degree is basically unchanged, and purer film has increased slightly, and is reached maximum when 0.8%, is 42.7MPa, as shown in figure 3, but working as starch and bacterium
Cellulose adds simultaneously when, the two can produce cooperative effect, 10% starch, the addition of 0.4% bacteria cellulose, can make
The tensile strength of PVA composite membranes brings up to 51.5MPa, and when bacterial fibers cellulose content is 0.8%, tensile strength can be brought up to
55MPa, as shown in Figure 4.
Claims (6)
- A kind of 1. preparation method of the biodegradable composite plastic films of bacteria cellulose/PVA, it is characterised in that：Including following Step：(1) bacteria cellulose is prepared；(2) bacteria cellulose for preparing step (1) is fully broken, and BC slurries are obtained after adding distilled water diluting stirring；Will be dilute A period of time is blended with the PVA aqueous solution prepared in advance under 90 DEG C of water-baths for BC slurries after releasing；(3) take a certain amount of starch and a small amount of distilled water to be placed in three-necked flask, be gelatinized under 80-90 DEG C of water-bath, with above-mentioned PVA bodies After system blending 30-90min, add plasticizer and continue vacuum defoamation after reaction 45-60min, the casting film-forming on flat board.
- 2. preparation method according to claim 1, it is characterised in that：The mass ratio of PVA and starch is 6 in casting solution： 4-9：1.
- 3. preparation method according to claim 1, it is characterised in that：The addition of bacteria cellulose is PVA total amounts 0.1-2wt%.
- 4. preparation method according to claim 1, it is characterised in that：Plasticizer be glycerine, caprolactam, polyethylene glycol, One or more of mixtures of Tween 80.
- 5. preparation method according to claim 1, it is characterised in that：The content of plasticizer is PVA total amounts in PVA casting solutions 10-50wt%.
- 6. preparation method according to claim 1, it is characterised in that：The preparation method of bacteria cellulose is：With glucose, Peptone, dusty yeast, disodium hydrogen phosphate, acetic acid etc. are that raw material prepares bacterial liquid culture medium according to a certain percentage, are gone out through high temperature Acetobacter is inoculated with after bacterium in the medium, by fluid nutrient medium 30 DEG C of temperature, humidity 50% biochemical cultivation case in stand 10-15 days, obtain bacteria cellulose.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108570156A (en) * | 2018-03-28 | 2018-09-25 | 华南理工大学 | Vegetables taste bacteria cellulose-base edible condiment packaging film and its preparation method and application |
| CN109251450A (en) * | 2018-07-17 | 2019-01-22 | 王晚秀 | A kind of high barrier PVA group compound film and preparation method thereof |
| CN109337149A (en) * | 2018-09-21 | 2019-02-15 | 南京理工大学 | A kind of Multifunctional rubber composite material and preparation method containing bacteria cellulose |
| CN111471199A (en) * | 2020-04-20 | 2020-07-31 | 上海交通大学 | Preparation method of food packaging film based on bacterial nano-cellulose |
| CN111995800A (en) * | 2020-09-03 | 2020-11-27 | 蔡营龙 | Preparation method of cellulose-based antibacterial food packaging film |
| CN115368694A (en) * | 2022-09-30 | 2022-11-22 | 河北百展科技发展有限公司 | Biomass-based reinforced polyvinyl alcohol composite material and preparation method thereof |
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|---|---|---|---|---|
| US20010034383A1 (en) * | 1998-02-26 | 2001-10-25 | Masaru Uryu | Polymeric composite material and method of manufacturing the same |
| CN101948597A (en) * | 2010-09-03 | 2011-01-19 | 东华大学 | Method for preparing bacterial cellulose/polyvinyl alcohol composite membrane by wet process |
| CN104974381A (en) * | 2014-04-08 | 2015-10-14 | 上海耐特复合材料制品有限公司 | Starch-based biodegradable composite material and preparation method thereof |
-
2017
- 2017-09-05 CN CN201710789965.7A patent/CN107365421B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20010034383A1 (en) * | 1998-02-26 | 2001-10-25 | Masaru Uryu | Polymeric composite material and method of manufacturing the same |
| CN101948597A (en) * | 2010-09-03 | 2011-01-19 | 东华大学 | Method for preparing bacterial cellulose/polyvinyl alcohol composite membrane by wet process |
| CN104974381A (en) * | 2014-04-08 | 2015-10-14 | 上海耐特复合材料制品有限公司 | Starch-based biodegradable composite material and preparation method thereof |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108570156A (en) * | 2018-03-28 | 2018-09-25 | 华南理工大学 | Vegetables taste bacteria cellulose-base edible condiment packaging film and its preparation method and application |
| CN108570156B (en) * | 2018-03-28 | 2020-11-24 | 华南理工大学 | Vegetable-flavor bacterial cellulose-based edible seasoning packaging film and preparation method and application thereof |
| CN109251450A (en) * | 2018-07-17 | 2019-01-22 | 王晚秀 | A kind of high barrier PVA group compound film and preparation method thereof |
| CN109337149A (en) * | 2018-09-21 | 2019-02-15 | 南京理工大学 | A kind of Multifunctional rubber composite material and preparation method containing bacteria cellulose |
| CN111471199A (en) * | 2020-04-20 | 2020-07-31 | 上海交通大学 | Preparation method of food packaging film based on bacterial nano-cellulose |
| CN111995800A (en) * | 2020-09-03 | 2020-11-27 | 蔡营龙 | Preparation method of cellulose-based antibacterial food packaging film |
| CN115368694A (en) * | 2022-09-30 | 2022-11-22 | 河北百展科技发展有限公司 | Biomass-based reinforced polyvinyl alcohol composite material and preparation method thereof |
| CN115368694B (en) * | 2022-09-30 | 2023-10-13 | 河北百展科技发展有限公司 | Biomass-based reinforced polyvinyl alcohol composite material and preparation method thereof |
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