CN101948597A - Method for preparing bacterial cellulose/polyvinyl alcohol composite membrane by wet process - Google Patents
Method for preparing bacterial cellulose/polyvinyl alcohol composite membrane by wet process Download PDFInfo
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- CN101948597A CN101948597A CN 201010272386 CN201010272386A CN101948597A CN 101948597 A CN101948597 A CN 101948597A CN 201010272386 CN201010272386 CN 201010272386 CN 201010272386 A CN201010272386 A CN 201010272386A CN 101948597 A CN101948597 A CN 101948597A
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Abstract
The invention relates to a method for preparing a bacterial cellulose/polyvinyl alcohol composite membrane by a wet process, which comprises the following steps: mechanically crushing bacterial celluloses to obtain a bacterial cellulose homogenate, and then determining the water content; preparing polyvinyl alcohol into a solution with a mass concentration of 5-15%; and uniformly mixing the bacterial cellulose homogenate and the polyvinyl alcohol solution, spreading in a mold, deaerating, standing at room temperature for 12-36 hours, and crosslinking with an aldehyde solution in a supersaturated salt solution to obtain the bacterial cellulose/polyvinyl alcohol composite membrane. By preparing the bacterial cellulose and water-soluble high molecular composite membrane by chemical crosslink in a coagulation bath, the preparation method has the characteristics of simple film-forming process, low cost, environmental friendliness and the like, and has favorable application prospects in industrial production.
Description
Technical field
The invention belongs to the preparation field of bacteria cellulose composite membrane, particularly relate to the method that a kind of wet method prepares the bacteria cellulose/polyvinyl alcohol composite membrane.
Background technology
Bacteria cellulose is that Brown at first finds, its diameter only is 1/10 of artificial synthon, is 10nm～100nm, is a kind of novel nano grade biological material.The key distinction of bacteria cellulose and plant cellulose is its other polysaccharide that undope, as hemicellulose etc., plant cellulose then contains hemicellulose and xylogen, thereby bacterial fibers have the character of many uniquenesses, for example high chemical purity and high-crystallinity, high-tensile and Young's modulus, and very strong water associativity is arranged, splendid shape maintains ability and anti-tear power, simultaneously, bacteria cellulose also is a kind of biodegradable, and the nano biological fiber of in human body, not degrading.
Bacteria cellulose can be used as the fortifying fibre in water-soluble polymer (as the polyvinyl alcohol) composite membrane, and this composite membrane is widely used, and especially aspect medical science, therefore the correlative study of this new bio nano material is subjected to various countries investigator's attention day by day.At present, the film of bacteria cellulose and water-soluble polymer composite membrane mainly contains freeze-thaw cycle method and lyophilization.The freeze-thaw cycle method is through freezing heating cycle, make bacteria cellulose and water-soluble polymer by the film forming method of physical crosslinking, the freeze-thaw cycle method makes that original crystal increases in the polyvinyl alcohol, form new crystal, improve its degree of crystallinity, but by physical action take place crosslinked a little less than, thereby the tensile strength of composite membrane and Young's modulus are all less; Lyophilization (lyophilization) is the water sublimed that makes at low temperatures in bacteria cellulose and the water-soluble polymer mixing solutions, thereby removes the film forming method of moisture, lyophilization can prevent to be dried composition heated denaturalization or deterioration by oxidation in drying process.We had once applied for a patent of invention for preparing bacteria cellulose and polyvinyl alcohol (PVA) composite membrane with lyophilization, yet bacteria cellulose and PVA composite membrane are in freeze-drying process, can ftracture in the film surface, make that its tensile strength and Young's modulus are less, thereby influence the mechanical property and the use range of composite membrane.And this patent is in the precipitation bath of supersaturated salt solution, under acidic conditions, make bacteria cellulose and PVA by the chemically crosslinked film forming with aldehyde solution, the tensile strength of the composite membrane that obtains and Young's modulus are compared obvious raising with the composite membrane that lyophilization during we once applied for a patent makes, thereby have improved its mechanical property and use range.In addition, freeze-thaw cycle method and lyophilization are had relatively high expectations to instrument, cost is also bigger, therefore, explore the novel film of bacteria cellulose and water-soluble polymer auxiliary agent composite membrane, make the performance of composite membrane further improve, and the lower desirable film of preparation cost is very necessary and urgent.Yet, at present in the research about bacteria cellulose and water-soluble polymer composite membrane, as precipitation bath, prepare the research and the methods involving thereof of composite membrane by the chemically crosslinked wet method with supersaturated salt solution, yet there are no report by retrieval.
Summary of the invention
Technical problem to be solved by this invention provides the method that a kind of wet method prepares the bacteria cellulose/polyvinyl alcohol composite membrane, this preparation method is by preparing bacteria cellulose and water-soluble polymer composite membrane by chemically crosslinked in precipitation bath, it is simple to have film-forming process, cost is low, characteristics such as environmentally friendly have a good application prospect in suitability for industrialized production.
A kind of wet method of the present invention prepares the method for bacteria cellulose/polyvinyl alcohol composite membrane, comprising:
(1) bacteria cellulose is placed the container that fills water, adopt the mechanical system fragmentation, get bacteria cellulose homogenate;
(2) water ratio of mensuration bacteria cellulose homogenate;
(3) PVAC polyvinylalcohol being mixed with mass percentage concentration with distilled water is 5%～20% the aqueous solution;
(4) with the water ratio be the bacteria cellulose homogenate of 93v/v%～99v/v% and polyvinyl alcohol water solution that concentration is 5wt%～20wt% uniform mixing by mass ratio 1: 1～15;
(5) be layered on mixture solution in the mould uniformly, at room temperature placed after the deaeration 12～36 hours, be between 1.0～5.0 at pH then, temperature is in 65 ℃～95 ℃ the supersaturated salt solution, adding concentration is the aldehyde solution of 20wt%～40wt%, carry out crosslinked 10～60min, make the bacteria cellulose/polyvinyl alcohol composite membrane, extremely neutral with the deionized water rinsing composite membrane.
The mulser fragmentation is adopted in fragmentation described in the step (1), and treatment condition are 7000～28000 rev/mins, 5～60min.
Polyvinyl alcohol described in the step (3) comprises low polymerization degree and superelevation polymerization degree polyvinyl alcohol, and molecular weight was 2～300,000 (polymerization degree is about 500～7000), and alcoholysis degree is 78%～99%.
Bacteria cellulose homogenate described in the step (4) and concentration are that the polyvinyl alcohol water solution blended ratio of 5wt%～15wt% is 1: 4～10.
Supersaturated salt solution described in the step (5) is (NH
4)
2SO
4, K
2SO
4, Na
2SO
4, NH
4Cl, KCl, NaCl, NH
4NO
3, KNO
3, NaNO
3Supersaturated aqueous solution in inorganic salt; Supersaturated salt solution is to be 1.5～4.5 with organic acid for adjusting pH value such as mineral acids such as sulfuric acid, hydrochloric acid or acetic acid, oxalic acid, and temperature is 75 ℃～90 ℃.
Mould described in the step (5) is glass wares, synthetic glass, pottery or stainless steel.
Aldehyde solution described in the step (5) is aldehyde solution such as formaldehyde solution, acetaldehyde solution, glyoxal solution or glutaraldehyde solution, and wherein, the mass ratio of aldehyde solution and bacteria cellulose/polyvinyl alcohol composite membrane is 1～5: 1.
Described bacteria cellulose/polyvinyl alcohol composite membrane, the thickness of film are 0.100～2.000mm, and water ratio is 10～25%, and breaking tenacity is 10～25N/mm
2, elongation at break is 80～240%, tensile modulus is 8～15N/mm
2
The present invention makes biomembrane material by chemically crosslinked with bacteria cellulose homogenate and water-soluble polymer auxiliary pva in precipitation bath, bacteria cellulose is the nano biological fiber, as the strongthener of composite membrane.This in precipitation bath bacteria cellulose and the wet preparation method of composite membrane of polyvinyl alcohol and the composite membrane of making following characteristics are arranged: 1. bacteria cellulose and the composite membrane of polyvinyl alcohol wet preparation method in precipitation bath is lower to the requirement of plant and instrument, and precipitation bath solution can be recycled after concentrating in addition; 2. bacteria cellulose and polyvinyl alcohol with after the aldehyde solution crosslinking film forming, can prevent its contraction in hot water in precipitation bath, have reliable intensity and good elasticity; 3. the composite membrane of Zhi Bei bacteria cellulose and polyvinyl alcohol has good biological tissue's consistency, no foreign matter rejection.
Beneficial effect
Preparation method of the present invention is by preparing bacteria cellulose and water-soluble polymer composite membrane by chemically crosslinked in precipitation bath, it is simple to have a film-forming process, and characteristics such as cost is low, and is environmentally friendly have a good application prospect in suitability for industrialized production.
Description of drawings
Fig. 1. bacteria cellulose/PVA composite membrane SEM picture;
Fig. 2. bacteria cellulose/PVA composite membrane TG graphic representation.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
(1) bacteria cellulose is placed the container that fills water, adopt the mulser fragmentation, treatment condition are 7000～28000 rev/mins, and 5～60min obtains bacteria cellulose homogenate;
(2) water content of mensuration bacteria cellulose homogenate is: 98% (V/V);
(3) with polyethylene distilled water
Be configured to mass concentration and be 10% the aqueous solution;
(4) water ratio in bacteria cellulose homogenate is 98%, will be that 10% polyvinyl alcohol water solution is by 1: 10 uniform mixing of mass ratio with concentration after the described bacteria cellulose homogenate;
(5) mixture is layered in the mould of glass wares uniformly, and to make its thickness be 0.500～2.500mm, at room temperature place 12h after the deaeration, then at the oversaturated K of 100ml
2SO
4In the solution, be 1.5 with 37wt% formaldehyde solution 2ml at pH, temperature is the crosslinked 30min time under 80 ℃ of conditions, obtains bacteria cellulose and composite membrane of polyvinyl alcohol, and is extremely neutral with the deionized water rinsing composite membrane.
The thickness of bacteria cellulose and composite membrane of polyvinyl alcohol is 0.253mm, and water ratio is 16.85%, is cut into the 80mm*20mm small pieces, and recording its breaking tenacity is 12.367N/mm
2, elongation at break is 108.14%, calculating its tensile modulus is 11.436N/mm
2
Embodiment 2
(1) bacteria cellulose is placed the container that fills water, adopt the mulser fragmentation, treatment condition are 7000～28000 rev/mins, and 5～60min obtains bacteria cellulose homogenate;
(2) water content of mensuration bacteria cellulose homogenate is: 98% (V/V);
(3) polyvinyl alcohol being configured to mass concentration with distilled water is 15% the aqueous solution;
(4) water content in bacteria cellulose homogenate is 98%, is that 15% polyvinyl alcohol water solution is by 1: 8 uniform mixing of mass ratio with described bacteria cellulose homogenate and concentration;
(5) mixture is layered in the synthetic glass mould uniformly, and to make its thickness be 0.500～2.500mm, at room temperature place 15h after the deaeration, then at the oversaturated (NH of 100ml
4)
2SO
4Be 1.5 with 40wt% acetaldehyde solution 2.5ml at pH in the solution, temperature is the crosslinked 20min time under 85 ℃ of conditions, obtains bacteria cellulose and composite membrane of polyvinyl alcohol, with the deionized water rinsing composite membrane to neutral.
The thickness of bacteria cellulose and composite membrane of polyvinyl alcohol is 0.268mm, and water ratio is 18.83%, and recording its breaking tenacity is 11.660N/mm
2, elongation at break is 119.56%, calculating its tensile modulus is 9.752N/mm
2
Embodiment 3
(1) bacteria cellulose is placed the container that fills water, adopt the mulser fragmentation, treatment condition are 7000～28000 rev/mins, and 5～60min obtains bacteria cellulose homogenate;
(2) water ratio of mensuration bacteria cellulose homogenate is: 98% (V/V);
(3) polyvinyl alcohol being configured to mass concentration with distilled water is 5% the aqueous solution;
(4) water ratio in bacteria cellulose homogenate is 98%, is that 5% polyvinyl alcohol solution is by 1: 6 uniform mixing of mass ratio with described bacteria cellulose homogenate and concentration;
(5) mixture is layered in the ceramic die uniformly, and to make its thickness be 0.500～2.500mm that 18h is at room temperature placed in deaeration, then at the oversaturated Na of 100ml
2SO
4Be 2.5 with 30wt% glyoxal solution 3ml at pH in the solution, temperature is the crosslinked 20min time under 80 ℃ of conditions, obtains bacteria cellulose and composite membrane of polyvinyl alcohol, with the deionized water rinsing composite membrane to neutral.
The thickness of bacteria cellulose and composite membrane of polyvinyl alcohol is 0.312mm, and water ratio is 20.69%, and recording its breaking tenacity is 14.843N/mm
2, elongation at break is 131.37%, calculating its tensile modulus is 11.298N/mm
2
Embodiment 4
(1) bacteria cellulose is placed the container that fills water, adopt the mulser fragmentation, treatment condition are 7000～28000 rev/mins, and 5～60min obtains bacteria cellulose homogenate;
(2) water content of mensuration bacteria cellulose homogenate is: 98% (V/V);
(3) polyvinyl alcohol being configured to mass concentration with distilled water is 20% the aqueous solution;
(4) water ratio in bacteria cellulose homogenate is 98%, is that 20% polyvinyl alcohol solution is by 1: 4 uniform mixing of mass ratio with described bacteria cellulose homogenate and concentration;
(5) mixture is layered in the stainless steel mould uniformly, and to make its thickness be 0.500～2.500mm, at room temperature place 24h after the deaeration, then at the oversaturated Na of 100ml
2SO
4Be 2 with 25wt% glutaraldehyde solution 4ml at pH in the solution, temperature is the crosslinked 30min time under 85 ℃ of conditions, bacteria cellulose that obtains and composite membrane of polyvinyl alcohol, with the deionized water rinsing composite membrane to neutral.
The thickness of bacteria cellulose and composite membrane of polyvinyl alcohol is 0.197mm, and water ratio is 14.37%, records its breaking tenacity 21.076N/mm
2, elongation at break is 149.53%, calculating its tensile modulus is 14.095N/mm
2
Embodiment 4 makes bacteria cellulose/PVA composite membrane and sees accompanying drawing 1.
Claims (9)
1. a wet method prepares the method for bacteria cellulose/polyvinyl alcohol composite membrane, comprising:
(1) bacteria cellulose is placed the container that fills water, adopt the mechanical system fragmentation, get bacteria cellulose homogenate;
(2) water ratio of mensuration bacteria cellulose homogenate;
(3) PVAC polyvinylalcohol being mixed with mass percentage concentration with distilled water is 5%～20% the aqueous solution;
(4) with the water ratio be the bacteria cellulose homogenate of 93v/v%～99v/v% and polyvinyl alcohol water solution that concentration is 5wt%～20wt% uniform mixing by mass ratio 1: 1～15;
(5) be layered on mixture solution in the mould uniformly, at room temperature placed after the deaeration 12～36 hours, be between 1.0～5.0 at pH then, temperature is in 65 ℃～95 ℃ the supersaturated salt solution behind the solidification forming, adding concentration is the aldehyde solution of 20wt%～40wt%, carry out crosslinked 10～60min, make the bacteria cellulose/polyvinyl alcohol composite membrane, extremely neutral with the deionized water rinsing composite membrane.
2. a kind of wet method according to claim 1 prepares the method for bacteria cellulose/polyvinyl alcohol composite membrane, it is characterized in that: the mulser fragmentation is adopted in the fragmentation described in the step (1), and treatment condition are 7000～28000 rev/mins, 5～60min.
3. a kind of wet method according to claim 1 prepares the method for bacteria cellulose/polyvinyl alcohol composite membrane, it is characterized in that: the polyvinyl alcohol described in the step (3) comprises low polymerization degree and superelevation polymerization degree polyvinyl alcohol, molecular weight is 2～300,000, the polymerization degree is 500～7000, and alcoholysis degree is 78%～99%.
4. a kind of wet method according to claim 1 prepares the method for bacteria cellulose/polyvinyl alcohol composite membrane, it is characterized in that: bacteria cellulose homogenate described in the step (4) and concentration are that the polyvinyl alcohol water solution blended ratio of 5wt%～15wt% is 1: 4～10.
5. a kind of wet method according to claim 1 prepares the method for bacteria cellulose/polyvinyl alcohol composite membrane, it is characterized in that: the supersaturated salt solution described in the step (5) is (NH
4)
2SO
4, K
2SO
4, Na
2SO
4, NH
4Cl, KCl, NaCl, NH
4NO
3, KNO
3, NaNO
3Supersaturated aqueous solution.
6. a kind of wet method according to claim 5 prepares the method for bacteria cellulose/polyvinyl alcohol composite membrane, it is characterized in that: described supersaturated salt solution is to be 1.5～4.5 with acid for adjusting pH value, and temperature is 75 ℃～90 ℃.
7. a kind of wet method according to claim 1 prepares the method for bacteria cellulose/polyvinyl alcohol composite membrane, it is characterized in that: the mould described in the step (5) is glass wares, synthetic glass, pottery or stainless steel.
8. a kind of wet method according to claim 1 prepares the method for bacteria cellulose/polyvinyl alcohol composite membrane, it is characterized in that: the aldehyde solution described in the step (5) is formaldehyde solution, acetaldehyde solution, glyoxal solution or glutaraldehyde solution; Wherein, the mass ratio of aldehyde solution and bacteria cellulose/polyvinyl alcohol composite membrane is 1～5: 1.
9. a kind of wet method according to claim 1 prepares the method for bacteria cellulose/polyvinyl alcohol composite membrane, it is characterized in that: described bacteria cellulose/polyvinyl alcohol composite membrane, the thickness of film is 0.100～2.000mm, and water ratio is 10～25%, and breaking tenacity is 10～25N/mm
2, elongation at break is 80～240%, tensile modulus is 8～15N/mm
2
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104693464A (en) * | 2015-02-10 | 2015-06-10 | 北京林业大学 | Preparation method of lignin-nanocelluose reinforced polylactic acid composite film |
| CN107129587A (en) * | 2017-06-09 | 2017-09-05 | 兰州理工大学 | The method that wet method prepares biodegradable CMS/composite membrane of polyvinyl alcohol |
| CN107365421A (en) * | 2017-09-05 | 2017-11-21 | 天津科技大学 | The preparation method of the biodegradable composite plastic films of bacteria cellulose/PVA |
| CN107413316A (en) * | 2017-08-01 | 2017-12-01 | 东华大学 | A kind of efficient protein adsorbing separation bacteria cellulose nano-fiber composite film and preparation method thereof |
| CN109651738A (en) * | 2019-01-02 | 2019-04-19 | 兰州理工大学 | The compound membrane preparation method of high strength and high flexibility polyethylene terephthalate/polyethylene alcohol |
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| CN115109283A (en) * | 2021-03-23 | 2022-09-27 | 中国科学院大连化学物理研究所 | High-strength and solvent-resistant cellulose composite membrane and preparation method and application thereof |
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| US20050037082A1 (en) * | 2003-08-13 | 2005-02-17 | Wan-Kei Wan | Poly(vinyl alcohol)-bacterial cellulose nanocomposite |
| CN101053674A (en) * | 2007-05-17 | 2007-10-17 | 山东轻工业学院 | Method for preparing artificial dura meter of brain using with bacterial cellulose |
| CN101215388A (en) * | 2008-01-15 | 2008-07-09 | 东华大学 | Method for preparing bacteria cellulose composite membrane |
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Patent Citations (3)
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| US20050037082A1 (en) * | 2003-08-13 | 2005-02-17 | Wan-Kei Wan | Poly(vinyl alcohol)-bacterial cellulose nanocomposite |
| CN101053674A (en) * | 2007-05-17 | 2007-10-17 | 山东轻工业学院 | Method for preparing artificial dura meter of brain using with bacterial cellulose |
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| CN104693464A (en) * | 2015-02-10 | 2015-06-10 | 北京林业大学 | Preparation method of lignin-nanocelluose reinforced polylactic acid composite film |
| CN104693464B (en) * | 2015-02-10 | 2018-01-02 | 北京林业大学 | A kind of preparation method of lignin nano-cellulose enhancing polymeric lactic acid compound film |
| CN107129587A (en) * | 2017-06-09 | 2017-09-05 | 兰州理工大学 | The method that wet method prepares biodegradable CMS/composite membrane of polyvinyl alcohol |
| CN107413316A (en) * | 2017-08-01 | 2017-12-01 | 东华大学 | A kind of efficient protein adsorbing separation bacteria cellulose nano-fiber composite film and preparation method thereof |
| CN107413316B (en) * | 2017-08-01 | 2020-08-11 | 东华大学 | Bacterial cellulose nanofiber composite membrane for efficient protein adsorption separation and preparation method thereof |
| CN107365421A (en) * | 2017-09-05 | 2017-11-21 | 天津科技大学 | The preparation method of the biodegradable composite plastic films of bacteria cellulose/PVA |
| CN107365421B (en) * | 2017-09-05 | 2020-07-03 | 天津科技大学 | Preparation method of bacterial cellulose/PVA biodegradable composite plastic film |
| CN109651738A (en) * | 2019-01-02 | 2019-04-19 | 兰州理工大学 | The compound membrane preparation method of high strength and high flexibility polyethylene terephthalate/polyethylene alcohol |
| CN110126417A (en) * | 2019-05-24 | 2019-08-16 | 深圳昌茂粘胶新材料有限公司 | A kind of flexible mobile phone is without folding line protective film and preparation method thereof |
| CN110126417B (en) * | 2019-05-24 | 2023-10-24 | 深圳昌茂粘胶新材料有限公司 | Crease-free protective film for flexible mobile phone and preparation method thereof |
| CN115109283A (en) * | 2021-03-23 | 2022-09-27 | 中国科学院大连化学物理研究所 | High-strength and solvent-resistant cellulose composite membrane and preparation method and application thereof |
| CN116239833A (en) * | 2023-03-14 | 2023-06-09 | 四川成渝双成科技有限责任公司 | Preparation method of mildew-proof modified atmosphere preservative film for fruits |
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