CN102309943A - Method for preparing Pickering emulsion by using bacterial cellulose - Google Patents
Method for preparing Pickering emulsion by using bacterial cellulose Download PDFInfo
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- CN102309943A CN102309943A CN2010102161423A CN201010216142A CN102309943A CN 102309943 A CN102309943 A CN 102309943A CN 2010102161423 A CN2010102161423 A CN 2010102161423A CN 201010216142 A CN201010216142 A CN 201010216142A CN 102309943 A CN102309943 A CN 102309943A
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Abstract
The invention relates to a method for preparing Pickering emulsion by using bacterial cellulose, which belongs to the field of new materials and biotechnology. Gluconacetobacter xylinus is fermented to form a bacterial cellulose hydrogel film; and the bacterial cellulose hydrogel film is subjected to centrifugation, pulping and ultrasonic dispersion to form bacterial cellulose dispersion. Microfilament serves as a solid emulsifier and stably exists on an oil-water surface to prevent dispersed microdroplets from being condensed and stabilize the emulsion. The pH value of the bacterial cellulose dispersion used for preparing the emulsion is between 4 and 12; the volume ratio between an oil phase and the dispersion in the emulsion can be controlled to a range between 1:5 and 2:1; and the mass percentage of bacterial cellulose (relative to the mass of all the mixture) is between 0.0125 percent and 0.25 percent. An emulsion-breaking phenomenon does not appear after the emulsion is stored for 3 months at room temperature.
Description
Technical field
The invention belongs to new material and biological technical field, be specifically related to a kind of method for preparing the Pickering emulsion by the bacteria cellulose dispersion liquid.
Background technology
(bacterial cellulose is by the synthetic native cellulose of gluconate pyracetobacillus (Gluconacetobacter xylinus) BC) to the used bacteria cellulose of the present invention.The first fibre diameter in the oozy Asia of thalline is 1.5nm; The synthetic microfibril diameter 3.5～4nm of inferior first group of fibers; Microfibril further is assembled into the pencil nanofibrous structures of diameter 40-60nm; Form cellulose membrane through further twining, so bacteria cellulose possesses superfine mesh nanometer structure.Bacteria cellulose has high chemical purity, high-crystallinity, strong moisture holding capacity and excellent biocompatibility, is a kind of novel nano biological medical material.
Pickering emulsification is to replace traditional chemical emulsifier with solid particle, and solid particle forms thin film at oil-water interfaces, has stoped the gathering between the drop, makes stable oil/aqueous dispersion phase.During as emulsifying agent, the stability of emulsion depends on the interaction between the particle diameter of solid particle, surface wettability and the solid particle with solid particle, and wherein the wetability of particle surface is most important influence factor.The Pickering emulsion is compared with the stable emulsion of conventional surfactant, has the advantage of himself: (1) can reduce the consumption of emulsifying agent greatly, practices thrift cost; (2) to the toxic action of human body much smaller than surfactant; (3) environmentally friendly; (4) stability of emulsion is strong, is difficult for receiving the influence of factors such as system pH, salinity, temperature and oil phase composition.
The present invention utilizes the bacteria cellulose microfibril as solid emulsifier, preparation Pickering emulsion.The Pickering emulsion of BC preparation has the character of Nantural non-toxic, and the BC consumption is few, and application cost is low, can be applicable to food, cosmetics, medicine and other fields.
Summary of the invention
The purpose of this patent is to provide emulsion of preparing with the bacteria cellulose dispersion liquid and preparation method thereof.The present invention adopts following technical scheme to realize:
1. microbial fermentation biosynthesis bacteria cellulose aquagel film
Wooden glucose vinegar acidfast bacilli inclined-plane seed with a ring or two ring activation inserts in the HS seed culture medium, and 30 ℃ of following per minute 160 rotational oscillations swing cultivates 24h; Inoculum concentration access with 5-10% (v/v) is equipped with in the container of HS fermentation medium, leaves standstill through 30 ℃ and cultivates 4-10 days, on gas-liquid interface, forms the bacteria cellulose aquagel film.
Be to remove culture medium and thalline on the bacteria cellulose film of above-mentioned fermentation method preparation, after handling with the circulating water washing by soaking, after 0.1mol/L NaOH solution soaking was spent the night, boiled 20min, washing was soaked in the deionized water 4 ℃ of preservations to neutral again.
2. bacteria cellulose dispersion liquid preparation
1. the rotating speed centrifugal dehydration 20min that the bacteria cellulose film that microbial fermentation is obtained changes with per minute 4000.
2. the cellulose membrane after centrifugal is broken up in beater, become the bacteria cellulose dispersion liquid.
3. the dispersion liquid that step is obtained in 2. further disperses 20～30min in the ultrasonic cell disruption instrument of amplitude 75～85%; Obtain the microfibril of average length 3.9 μ m, cellulose quality percentage composition is 0.1～0.3% little blue bacteria cellulose dispersion liquid.
4. the bacteria cellulose dispersion liquid that step is obtained in 3. is in 120 ℃ of following moist heat sterilization 20min, 4 ℃ of preservations.
3. bacteria cellulose Pickering emulsion preparation
1. in the bacteria cellulose dispersion liquid that step 2 obtains, add oil-based solvent, the volume ratio scope of oil phase and bacteria cellulose dispersion liquid is controlled at 1: 5～2: 1 scopes.The pH value scope 4～12 of bacteria cellulose dispersion liquid, the cellulose quality accounts for 0.1%～0.5% of mixture quality.
2. the mixture of bacteria cellulose dispersion liquid and oil phase mixing and emulsifying in ultrasonic cell disruption instrument (amplitude 75～85%) obtains stable oil-in-water Pickering emulsion.
3. said oil phase is to be in a liquid state under the emulsion preparation temperature of living in, and water-fast oil phase substance, and for example atoleine, styrene, toluene, edible oil or methyl methacrylate are medium.
Description of drawings
Fig. 1 is the bacteria cellulose Pickering emulsion (oil-water ratio 1: 1, pH value are 7, bacteria cellulose mass percent 0.2%) that the present invention prepares
Fig. 2 is the optical microscope photograph of bacteria cellulose Pickering emulsion on blood counting chamber among Fig. 1, can find out that the emulsion droplet diameter is 10-50 μ m (amplifying 100 times, grid size 50 * 50 μ m)
The specific embodiment
Below in conjunction with specific embodiment the present invention is done further elaboration in detail.The following example is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.
Embodiment 1:
Gluconate pyracetobacillus (Gluconacetobacter xylinus) bacteria cellulose film that fermentation obtains when leaving standstill cultivation is after centrifugal, beater are broken up; In ultrasonic cell disruption instrument (amplitude 75～85%), further disperse; Obtaining average length is little blue fiber dispersion of being of 3.90 μ m, the quality percentage composition 0.1% of bacteria cellulose.With NaOH solution the pH value of fiber dispersion is adjusted to 12, the atoleine with same volume disperses in ultrasonic cell disruption instrument (amplitude 75～85%) then, is prepared into emulsion, and the electrical conductivity of stable back emulsion is 1270 μ S/cm, is emulsion oil-in-water.This emulsion property is stable, does not see obvious demulsifying phenomenon in 3 months airtight the preservation down of room temperature.
Embodiment 2:
Bacteria cellulose film that fermentation obtains and bacteria cellulose dispersion liquid are with embodiment 1.Preparation bacteria cellulose Pickering emulsion, wherein the volume ratio of atoleine and bacteria cellulose was respectively 1: 5 and 1: 1 o'clock, and oil water mixture is disperseed in ultrasonic cell disruption instrument (amplitude 75～85%), prepared stable emulsion oil-in-water.This emulsion property is stable, does not see obvious demulsifying phenomenon in 3 months airtight the preservation down of room temperature.
Embodiment 3:
Bacteria cellulose film that fermentation obtains and bacteria cellulose dispersion liquid are with embodiment 1.Preparation bacteria cellulose Pickering emulsion; Wherein the volume ratio of fiber dispersion and atoleine is 1: 1; The quality percentage composition of bacteria cellulose (with respect to whole mixture qualities) is respectively 0.0125% and at 0.25% o'clock; Oil water mixture is disperseed in ultrasonic cell disruption instrument (amplitude 75～85%), prepare stable emulsion oil-in-water.This emulsion property is stable, does not see obvious demulsifying phenomenon in 3 months airtight the preservation down of room temperature.
Embodiment 4:
Bacteria cellulose film that fermentation obtains and bacteria cellulose dispersion liquid are with embodiment 1.Preparation bacteria cellulose Pickering emulsion; Wherein the volume ratio of fiber dispersion and oil-based solvent is 1: 1; The quality percentage composition of bacteria cellulose (with respect to whole mixture qualities) is 0.05%; Oil water mixture is disperseed in ultrasonic cell disruption instrument (amplitude 75～85%), test with styrene, toluene, edible oil, methyl methacrylate respectively, all obtained good effect.
Claims (2)
1. the preparation method of a bacteria cellulose Pickering emulsion is characterized in that may further comprise the steps:
(a) microbial fermentation biosynthesis bacteria cellulose aquagel film
(b) bacteria cellulose dispersion liquid preparation
The rotating speed centrifugal dehydration 20min that the bacteria cellulose film that microbial fermentation is obtained changes with per minute 4000.Cellulose membrane after centrifugal is broken up in beater, become the bacteria cellulose dispersion liquid.Dispersion liquid is further disperseed 20～30min in the ultrasonic cell disruption instrument of amplitude 75～85%, obtain the microfibril of average length 3.9 μ m.
(c) bacteria cellulose Pickering emulsion preparation
Bacteria cellulose dispersion liquid (pH is controlled at 4～12 scopes, and cellulose quality percentage is in 0.025%～0.5% scope) and oil-based solvent are disperseed in ultrasonic cell disruption instrument (amplitude 75～85%), obtain stable oil-in-water Pickering emulsion.The volume ratio scope of oil phase and bacteria cellulose dispersion liquid can be controlled in 1: 5～2: 1 scopes.
2. according to the method for the said making bacteria cellulose of claim 1 Pickering emulsion; It is characterized in that: said oil phase is to be in a liquid state under the emulsion preparation temperature of living in; And water-fast oil phase substance, for example atoleine, styrene, toluene, edible oil or methyl methacrylate etc.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104177547A (en) * | 2014-07-29 | 2014-12-03 | 江苏大学 | Method for preparing composite cellulose porous imprinting adsorbent |
| CN104825343A (en) * | 2014-02-06 | 2015-08-12 | 奈菲儿生医股份有限公司 | Cosmetic composition containing fragments of biological cellulose membrane and method for producing same |
| CN105873673A (en) * | 2013-11-19 | 2016-08-17 | 中越纸浆工业株式会社 | Emulsion which contains nanofibrillated fibrous polysaccharide, material, and processes for manufacturing same |
| CN106065081A (en) * | 2016-06-16 | 2016-11-02 | 海南大学 | The preparation method of a kind of high-dispersion nano cellulose gum and products obtained therefrom and application |
| CN106750375A (en) * | 2017-01-23 | 2017-05-31 | 陕西科技大学 | The method that Pickering emulsions are prepared using modified nanometer cellulose |
| CN103566785B (en) * | 2012-08-01 | 2017-07-04 | 天津科技大学 | A kind of method that utilization oxidizing bacteria cellulose prepares Pickering emulsions |
| CN107365417A (en) * | 2017-07-27 | 2017-11-21 | 中国林业科学研究院林产化学工业研究所 | Stable Pickering emulsions of a kind of castor oil modified cellulose and preparation method thereof |
| CN107737365A (en) * | 2016-09-14 | 2018-02-27 | 苏州顶澜医用材料科技有限公司 | A kind of postoperative skin repair biology cellulose dressing of laser therapy and preparation method thereof |
| CN108853021A (en) * | 2018-08-08 | 2018-11-23 | 华南农业大学 | A kind of probiotics liquid formulation and preparation method thereof based on double emulsion structures |
| CN108851019A (en) * | 2018-08-08 | 2018-11-23 | 华南农业大学 | A kind of pik woods pair lotions and preparation method thereof that bacteria cellulose is stable |
| CN105944581B (en) * | 2016-05-16 | 2019-01-01 | 辽宁大学 | A kind of anion responsiveness Pickering lotion and its preparation method and application |
| CN109135303A (en) * | 2018-08-22 | 2019-01-04 | 广西大学 | A kind of preparation method of nano-cellulose enhancing soybean oil base foamed plastics |
| CN110628050A (en) * | 2019-09-25 | 2019-12-31 | 天津科技大学 | Emulsion preparation method |
| CN113368231A (en) * | 2021-05-20 | 2021-09-10 | 南华大学 | Pickering emulsion, preparation method thereof and application of pickering emulsion as vaccine immunologic adjuvant |
| CN114041607A (en) * | 2021-11-23 | 2022-02-15 | 南京农业大学 | Food-grade soybean protein pickering emulsion and preparation method thereof |
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| JPH08276126A (en) * | 1995-02-10 | 1996-10-22 | Bio Polymer Res:Kk | Emulsification stabilizer |
| US5919488A (en) * | 1997-02-20 | 1999-07-06 | Somar Corporation | Antimicrobial aqueous dispersion |
| CN1281051A (en) * | 1999-07-19 | 2001-01-24 | 天津轻工业学院 | Process for preparing bacterial cellulose by glucose oxidation and bacillus fermentation |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103566785B (en) * | 2012-08-01 | 2017-07-04 | 天津科技大学 | A kind of method that utilization oxidizing bacteria cellulose prepares Pickering emulsions |
| CN105873673A (en) * | 2013-11-19 | 2016-08-17 | 中越纸浆工业株式会社 | Emulsion which contains nanofibrillated fibrous polysaccharide, material, and processes for manufacturing same |
| CN104825343A (en) * | 2014-02-06 | 2015-08-12 | 奈菲儿生医股份有限公司 | Cosmetic composition containing fragments of biological cellulose membrane and method for producing same |
| CN104177547A (en) * | 2014-07-29 | 2014-12-03 | 江苏大学 | Method for preparing composite cellulose porous imprinting adsorbent |
| CN104177547B (en) * | 2014-07-29 | 2016-09-14 | 江苏大学 | A kind of preparation method of cellulose compound porous trace adsorbent |
| CN105944581B (en) * | 2016-05-16 | 2019-01-01 | 辽宁大学 | A kind of anion responsiveness Pickering lotion and its preparation method and application |
| CN106065081A (en) * | 2016-06-16 | 2016-11-02 | 海南大学 | The preparation method of a kind of high-dispersion nano cellulose gum and products obtained therefrom and application |
| CN107737365A (en) * | 2016-09-14 | 2018-02-27 | 苏州顶澜医用材料科技有限公司 | A kind of postoperative skin repair biology cellulose dressing of laser therapy and preparation method thereof |
| CN106750375A (en) * | 2017-01-23 | 2017-05-31 | 陕西科技大学 | The method that Pickering emulsions are prepared using modified nanometer cellulose |
| CN106750375B (en) * | 2017-01-23 | 2019-04-09 | 陕西科技大学 | The method for preparing Pickering lotion using modified nanometer cellulose |
| CN107365417A (en) * | 2017-07-27 | 2017-11-21 | 中国林业科学研究院林产化学工业研究所 | Stable Pickering emulsions of a kind of castor oil modified cellulose and preparation method thereof |
| CN107365417B (en) * | 2017-07-27 | 2020-07-14 | 中国林业科学研究院林产化学工业研究所 | Stable Pickering emulsion prepared from castor oil modified cellulose and preparation method of stable Pickering emulsion |
| CN108853021A (en) * | 2018-08-08 | 2018-11-23 | 华南农业大学 | A kind of probiotics liquid formulation and preparation method thereof based on double emulsion structures |
| CN108851019A (en) * | 2018-08-08 | 2018-11-23 | 华南农业大学 | A kind of pik woods pair lotions and preparation method thereof that bacteria cellulose is stable |
| CN109135303A (en) * | 2018-08-22 | 2019-01-04 | 广西大学 | A kind of preparation method of nano-cellulose enhancing soybean oil base foamed plastics |
| CN110628050A (en) * | 2019-09-25 | 2019-12-31 | 天津科技大学 | Emulsion preparation method |
| CN113368231A (en) * | 2021-05-20 | 2021-09-10 | 南华大学 | Pickering emulsion, preparation method thereof and application of pickering emulsion as vaccine immunologic adjuvant |
| CN113368231B (en) * | 2021-05-20 | 2022-12-27 | 南华大学 | Pickering emulsion, preparation method thereof and application of pickering emulsion as vaccine immunologic adjuvant |
| CN114041607A (en) * | 2021-11-23 | 2022-02-15 | 南京农业大学 | Food-grade soybean protein pickering emulsion and preparation method thereof |
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Application publication date: 20120111 |