CN103566785A - Method for preparing Pickering emulsion from oxidizing bacterial cellulose - Google Patents
Method for preparing Pickering emulsion from oxidizing bacterial cellulose Download PDFInfo
- Publication number
- CN103566785A CN103566785A CN201210270166.6A CN201210270166A CN103566785A CN 103566785 A CN103566785 A CN 103566785A CN 201210270166 A CN201210270166 A CN 201210270166A CN 103566785 A CN103566785 A CN 103566785A
- Authority
- CN
- China
- Prior art keywords
- bacteria cellulose
- emulsion
- dispersion liquid
- bacterial cellulose
- oil
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Medicinal Preparation (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to a preparation method of a Pickering emulsion from oxidizing bacterial cellulose, and belongs to the technical fields of new materials and biology. Aldehyde bacterial cellulose dispersion liquid is prepare from a bacterial cellulose hydrogel membrane which is fermented from gluconacetobacter xylinus through centrifuging, pulping, high-pressure homogenization and oxidization, wherein microfiber, as a solid emulsifying agent, stably exists on an oil-water interface, so as to prevent dispersed micro-droplets from coagulating and keep the emulsion stable. The pH value of oxidizing bacterial cellulose for preparing the emulsion is 3-12, the volume ratio of an oil phase to the dispersion liquid is controlled as (1:5)-(2:1) in the emulsion, and the dosage of the oxidizing bacterial cellulose (relative to total mixture volume) is 0.25-5mg/L. The prepared emulsion can be stored for 3 months at room temperature without an obvious emulsion breaking phenomenon.
Description
Technical field
The invention belongs to new material and biological technical field, be specifically related to a kind of method of utilizing oxidizing bacteria cellulose to prepare Pickering emulsion.
Background technology
The present invention's bacteria cellulose (Bacterial Cellulose, BC) used is by the synthetic native cellulose of gluconate pyracetobacillus (Gluconacetobacter xylinus).The first fibre diameter in the oozy Asia of thalline is 1.5nm, the microfibril diameter 3.5-4nm that sub-first fiber combinations becomes, microfibril is further assembled into the pencil nanofibrous structures of diameter 40-60nm, become cellulose membrane, so bacteria cellulose possesses superfine Nanostructure Network through further winding-shaped.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 drop, makes stable oil/water decentralized photo.Using solid particle during as emulsifying agent, the interaction of the stability dependency of emulsion between particle diameter, surface wettability and the solid particle of solid particle, wherein the wetability of particle surface is most important influence factor.The emulsion that Pickering emulsion is stable with conventional surfactant is compared, and has the advantage of himself: (1) can reduce the consumption of emulsifying agent greatly, cost-saving; (2) to the toxic action of human body much smaller than surfactant; (3) environmentally friendly; (4) stability of emulsion is strong, is difficult for being subject to the impact of the factors such as system pH, salinity, temperature and oil phase composition.
The effect that solid particle is stablized Pickering emulsion depends on the wetability of particle surface strongly.Cellulosic molecule is rich in a large amount of hydroxyls, and hydrophily is stronger.It,, with after sodium periodate oxidation, is become to aldehyde radical by the hydroxyl oxidize on cellulosic 2,3, can reduce cellulosic hydrophilicrty, the effect of its stable emulsion is enhanced.
The present invention utilizes oxidizing bacteria cellulose microfibril as solid emulsifier, preparation Pickering emulsion.What oxidizing bacteria cellulose microfibre was stable is positioned on oil-water interfaces, stops the water (oil) disperseing to drip and again condenses for large drop phase-splitting, stable emulsion.Pickering emulsion prepared by BC has the character of Nantural non-toxic, and BC consumption is few, and application cost is low, can be applicable to food, cosmetics, medicine and other fields.
Publication number is that the Chinese invention patent " a kind of method of utilizing bacteria cellulose to prepare Pickering emulsion " of CN102309943A discloses a kind of method of preparing Pickering emulsion with bacteria cellulose microfibril.Cellulose is rich in a large amount of hydroxyls, is water wetted material, and contact angle is less.This patent is oxidized to aldehyde radical by part of hydroxyl, reduces its hydrophilicrty, and the stability of emulsion of preparing is improved, and emulsion droplets diameter reduces.
Summary of the invention
The object of this patent is to provide emulsion of preparing with oxidizing bacteria cellulose dispersion liquid and preparation method thereof.The present invention realizes by the following technical solutions:
1. microorganism fermenting organism synthesizes bacteria cellulose aquagel film
By the wooden glucose vinegar acidfast bacilli CGMCC No.1.1822 inclined-plane of a ring or two ring activation, in access HS seed culture medium, per minute 160 turn shaken cultivation 24h at 30 ℃; Inoculum concentration access with 5-10% (v/v) is equipped with in the container of HS fermentation medium, through 30 ℃ of standing cultivation 4-10 days, forms bacteria cellulose aquagel film on gas-liquid interface.
For removing culture medium and the thalline on bacteria cellulose film prepared by above-mentioned fermentation method, after processing with circulating water washing by soaking, then through 0.1mol/L NaOH solution soaked overnight, boil after 20min, washing, to neutral, is soaked in deionized water 4 ℃ of preservations.
2. oxidizing bacteria cellulose dispersion liquid preparation
1. bacteria cellulose film microorganism fermentation being obtained is broken up in beater, becomes bacteria cellulose dispersion liquid.
2. dispersion liquid step being obtained in 1. further disperses in high pressure homogenizer, and operating pressure 100-300bar, obtains bacteria cellulose microfibril, and wherein content of cellulose is the bacteria cellulose dispersion liquid of 3mg/L left and right.
3. bacteria cellulose dispersion liquid periodate oxidation step being obtained in 2., the two mass ratio NaIO
4: BC=1～3: 1, pH=2～4, shake up reaction 30～60min at 35-40 ℃, then add 0.1mol/L ethylene glycol or glycerine to consume excessive periodate.By distilled water flushing, centrifugal for product, after the 24h that dialyses after abandoning supernatant, obtain being oxidized BC suspension.Moist heat sterilization 20min at 120 ℃, 4 ℃ of preservations.Recording aldehyde group content in the bacteria cellulose after oxidation is 10-20%.
3. oxidizing bacteria cellulose Pickering emulsion preparation
1. in the oxidizing bacteria cellulose dispersion liquid obtaining in step 2, add oil-based solvent, the volume ratio scope control of oil phase and bacteria cellulose dispersion liquid was 1: 5～2: 1 scopes.The pH value scope of bacteria cellulose dispersion liquid is 3～12, and cellulose consumption is 0.25-5mg/L.
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. described oil phase is that emulsion is prepared at temperature of living in and is in a liquid state, and water-fast oil phase substance, for example atoleine, styrene, toluene, ethyl acetate, n-hexane, n-hexyl alcohol, edible wet goods.
Accompanying drawing explanation
Fig. 1 is the oxidizing bacteria cellulose Pickering emulsion prepared of the present invention (oil-water ratio 1: 1, the pH value of bacteria cellulose dispersion liquid is 7, oil phase is atoleine, oxidizing bacteria cellulose consumption is 1.9mg/L)
Fig. 2 is oxidizing bacteria cellulose Pickering emulsion in Fig. 1 optical microscope photograph on blood counting chamber, can find out that average emulsion droplet diameter is 8.4 μ m (grid size 50 * 50 μ m)
The specific embodiment
Below in conjunction with specific embodiment, the present invention is elaborated further.The following example is illustrative, is not determinate, can not limit protection scope of the present invention with following embodiment.In addition should be understood that those skilled in the art can make an amendment or change the present invention after having read the content that the present invention tells about, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1:
Gluconate pyracetobacillus (the Gluconacetobacter xylinus CGMCC No.1.1822) bacteria cellulose film that fermentation obtains when standing cultivation is after centrifugal, beater are broken up, in high pressure homogenizer (pressure 200bar), further disperse, obtain bacteria cellulose dispersion liquid.Bacteria cellulose is become to aldehyde radical bacteria cellulose with sodium periodate oxidation, and sodium metaperiodate consumption is 2 times of bacteria cellulose quality, at pH2,37 ℃, reacts 40min, then with 0.1mol/L glycerine, consumes excessive periodate.The aldehyde radical bacteria cellulose obtaining is clean, centrifugal, dialysis 24h obtains being oxidized BC suspension, and its aldehyde group content is 15%.Aldehyde radical bacterial cellulose suspension and the atoleine of same volume are disperseed in ultrasonic cell disruption instrument (amplitude 75～85%), be prepared into emulsion, oxidizing bacteria cellulose consumption is 1.9mg/L (with respect to entire mixture volume).This emulsion can be disperseed in water, is emulsion oil-in-water, and emulsion droplets average diameter is 8.4 μ m.This emulsion property is stable, in the airtight lower preservation of room temperature, within 3 months, has no obvious demulsifying phenomenon.
Embodiment 2:
The bacteria cellulose film that fermentation obtains and oxidizing bacteria cellulose dispersion liquid are with embodiment 1.Prepare oxidizing bacteria cellulose Pickering emulsion, wherein the volume ratio of corn oil and oxidizing bacteria cellulose is respectively 1: 4 and 1: 1 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, in the airtight lower preservation of room temperature, within 3 months, has no obvious demulsifying phenomenon.
Embodiment 3:
The bacteria cellulose film that fermentation obtains and oxidizing bacteria cellulose dispersion liquid are with embodiment 1.Prepare oxidizing bacteria cellulose Pickering emulsion, wherein the volume ratio of fiber dispersion and atoleine is 1: 1, when the consumption of oxidizing bacteria cellulose is respectively 0.5mg/L and 1mg/L, oil water mixture is disperseed in ultrasonic cell disruption instrument (amplitude 75～85%), prepare stable emulsion oil-in-water.This emulsion property is stable, in the airtight lower preservation of room temperature, within 3 months, has no obvious demulsifying phenomenon.
Embodiment 4:
The bacteria cellulose film that fermentation obtains and bacteria cellulose dispersion liquid are with embodiment 1.Prepare oxidizing bacteria cellulose Pickering emulsion, wherein the volume ratio of fiber dispersion and oil-based solvent is 1: 1, the consumption of oxidizing bacteria cellulose (with respect to entire mixture quality) is 1mg/L, oil water mixture is disperseed in ultrasonic cell disruption instrument (amplitude 75～85%), with styrene, toluene, corn oil, atoleine etc., test respectively, all obtained good effect.
Claims (5)
1. utilize a preparation method for oxidizing bacteria cellulose Pickering emulsion, it is characterized in that comprising the following steps:
(a) the synthetic bacteria cellulose aquagel film of microorganism fermenting organism, through purification process and after fully cleaning, obtains highly purified bacteria cellulose film.
(b) bacteria cellulose dispersion liquid preparation
Bacteria cellulose film is broken up in beater, become bacteria cellulose dispersion liquid.Dispersion liquid is further disperseed in high pressure homogenizer, and pressure is 100-300bar.
(c) oxidizing bacteria cellulose dispersion liquid preparation
By the periodate oxidation of bacteria cellulose dispersion liquid, the two mass ratio NaIO
4: bacteria cellulose=1～3: shake up reaction 30～60min at 1, pH=2～4,35～40 ℃, then add 0.1mol/L ethylene glycol or glycerine to consume excessive periodate.By distilled water flushing, centrifugal for product, after the 24h that dialyses after abandoning supernatant, obtain oxidizing bacteria cellulose suspension.
(d) bacteria cellulose Pickering emulsion preparation
Oxidizing bacteria cellulose dispersion liquid (pH is controlled at 3～12 scopes, and cellulose consumption is in 0.25～5mg/L 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. in accordance with the method for claim 1, it is characterized in that described bacteria cellulose take wooden glucose vinegar acidfast bacilli Gluconacetobacter xylinus CGMCC No.1.1822 as producing bacterial strain.
3. the aldehyde group content that in accordance with the method for claim 1, it is characterized in that oxidizing bacteria cellulose is 10-20%.
4. according to the method for making bacteria cellulose Pickering emulsion described in claim 1, it is characterized in that purification process adopts after 0.1M sodium hydroxide solution soaked overnight, then boil 30min in 0.1M sodium hydroxide solution, then fully clean to film and be neutral.
5. method according to claim 1, is characterized in that described oil phase is that emulsion is prepared at temperature of living in and is in a liquid state, and water-fast oil phase substance, such as atoleine, styrene, toluene, edible oil, n-hexane, n-hexyl alcohol, ethyl acetate etc.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210270166.6A CN103566785B (en) | 2012-08-01 | 2012-08-01 | A kind of method that utilization oxidizing bacteria cellulose prepares Pickering emulsions |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210270166.6A CN103566785B (en) | 2012-08-01 | 2012-08-01 | A kind of method that utilization oxidizing bacteria cellulose prepares Pickering emulsions |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103566785A true CN103566785A (en) | 2014-02-12 |
| CN103566785B CN103566785B (en) | 2017-07-04 |
Family
ID=50040014
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210270166.6A Expired - Fee Related CN103566785B (en) | 2012-08-01 | 2012-08-01 | A kind of method that utilization oxidizing bacteria cellulose prepares Pickering emulsions |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103566785B (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108727507A (en) * | 2017-04-21 | 2018-11-02 | 中国农业大学 | Oxycellulose is prepared and its in the application for washing and carrying prescription face |
| CN108783373A (en) * | 2018-04-03 | 2018-11-13 | 上海应用技术大学 | A kind of citral pickering emulsion and preparation method thereof |
| CN112314838A (en) * | 2020-10-29 | 2021-02-05 | 成都大学 | Antibacterial food fresh-keeping Pickering emulsion and preparation method thereof |
| CN113501973A (en) * | 2021-07-12 | 2021-10-15 | 江南大学 | Pickering emulsion stabilized by nano-cellulose hydrogel |
| CN113754929A (en) * | 2021-09-17 | 2021-12-07 | 天津科技大学 | Pickering emulsion |
| CN113845667A (en) * | 2021-11-01 | 2021-12-28 | 江南大学 | Preparation method and application of oxidized nano cellulose pickering emulsion |
| CN113940994A (en) * | 2021-11-09 | 2022-01-18 | 南华大学 | Preparation method and application of chitosan-Pickering emulsion interleukin 12 adjuvant system |
| CN115721007A (en) * | 2022-11-30 | 2023-03-03 | 东北林业大学 | PH change-resistant biomass-based Pickering emulsion and preparation method thereof |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101584879B (en) * | 2009-06-18 | 2012-08-15 | 天津大学 | Oxidizing bacteria cellulose micrometer-nanometer tissue engineering scaffold material and preparing method thereof |
| CN102309943A (en) * | 2010-07-02 | 2012-01-11 | 天津科技大学 | Method for preparing Pickering emulsion by using bacterial cellulose |
| CN102206689B (en) * | 2011-03-07 | 2013-04-24 | 海南椰国热带水果食品加工有限公司 | Method for modifying bacterial cellulose in the fermentation process |
| CN102352051B (en) * | 2011-09-30 | 2013-09-25 | 北京科技大学 | Method for preparing collagen-modified bacteria cellulose compound film |
-
2012
- 2012-08-01 CN CN201210270166.6A patent/CN103566785B/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108727507A (en) * | 2017-04-21 | 2018-11-02 | 中国农业大学 | Oxycellulose is prepared and its in the application for washing and carrying prescription face |
| CN108727507B (en) * | 2017-04-21 | 2022-09-30 | 中国农业大学 | Preparation of oxidized cellulose and application thereof in washing and medicine loading |
| CN108783373A (en) * | 2018-04-03 | 2018-11-13 | 上海应用技术大学 | A kind of citral pickering emulsion and preparation method thereof |
| CN112314838A (en) * | 2020-10-29 | 2021-02-05 | 成都大学 | Antibacterial food fresh-keeping Pickering emulsion and preparation method thereof |
| CN113501973A (en) * | 2021-07-12 | 2021-10-15 | 江南大学 | Pickering emulsion stabilized by nano-cellulose hydrogel |
| CN113754929A (en) * | 2021-09-17 | 2021-12-07 | 天津科技大学 | Pickering emulsion |
| CN113845667A (en) * | 2021-11-01 | 2021-12-28 | 江南大学 | Preparation method and application of oxidized nano cellulose pickering emulsion |
| CN113940994A (en) * | 2021-11-09 | 2022-01-18 | 南华大学 | Preparation method and application of chitosan-Pickering emulsion interleukin 12 adjuvant system |
| CN113940994B (en) * | 2021-11-09 | 2023-09-15 | 南华大学 | Preparation method and application of chitosan-Pickering emulsion interleukin 12 adjuvant system |
| CN115721007A (en) * | 2022-11-30 | 2023-03-03 | 东北林业大学 | PH change-resistant biomass-based Pickering emulsion and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103566785B (en) | 2017-07-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103566785A (en) | Method for preparing Pickering emulsion from oxidizing bacterial cellulose | |
| CN102309943A (en) | Method for preparing Pickering emulsion by using bacterial cellulose | |
| Rahman et al. | Recent developments of carboxymethyl cellulose | |
| El-Gendi et al. | Recent advances in bacterial cellulose: a low-cost effective production media, optimization strategies and applications | |
| CN102552965B (en) | Method for preparing nano-cellulose antibacterial composite material through on-line culture | |
| CN101921700B (en) | Device and method for preparing hollow heteromorphic bacteria cellulose material | |
| CN102888027B (en) | Bacterial cellulose/collagen-chitosan composite material and preparation method thereof | |
| CN106040026A (en) | Method for preparing Pickering emulsion from TEMPO oxidized bacterial cellulose | |
| CN103572507A (en) | Preparation method for antibiosis ultraviolet prevention silk fibroin nanofiber membrane | |
| Ho et al. | The trend of bacterial nanocellulose research published in the science citation index expanded from 2005 to 2020: a bibliometric analysis | |
| CN101264335A (en) | Bacteria cellulose membrane containing silver chloride nano particle and preparation and application thereof | |
| CN101914434B (en) | Device and method for dynamically preparing heterocavity bacterium cellulose materials | |
| Jiang et al. | Effects of sodium alginate on microstructural and properties of bacterial cellulose nanocrystal stabilized emulsions | |
| CN109180988A (en) | A kind of functionalized nano-fiber hydrogel and preparation method thereof | |
| TWI398276B (en) | Method for producing bacterial cellulose with controlled pore size and its use in wound dressing | |
| Khan et al. | Extraction processes for deriving cellulose: A comprehensive review on green approaches | |
| CN105175558A (en) | Preparation method of composite membrane | |
| Souza et al. | Kinetic study of a bacterial cellulose production by Komagataeibacter rhaeticus using coffee grounds and sugarcane molasses | |
| CN111973517A (en) | A moisture keeping facial mask containing Saviae Miltiorrhizae radix extract with high water locking effect, and its preparation method | |
| CN102764451B (en) | Preparation method and application of porous biological cellulose gel material | |
| CN107519540A (en) | A kind of implantable fibroin/bacteria cellulose/graphene composite conductive film of high tensile flexible printing opacity | |
| CN107189081A (en) | A kind of Preparation method and use of multi-functional polysaccharide hydrogel | |
| CN106727280A (en) | A kind of nano biological matter base anticancer sustained-release gel and preparation method thereof | |
| CN116459195A (en) | Janus structure nanocellulose/aloe essence mask and preparation method thereof | |
| CN100478360C (en) | Process for producing hyaluronic acid or its salt by concentration |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20170704 Termination date: 20210801 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |