CN108774342A - A kind of orange oil pickering emulsion and preparation method thereof stablized using nano-cellulose - Google Patents
A kind of orange oil pickering emulsion and preparation method thereof stablized using nano-cellulose Download PDFInfo
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- CN108774342A CN108774342A CN201810372513.3A CN201810372513A CN108774342A CN 108774342 A CN108774342 A CN 108774342A CN 201810372513 A CN201810372513 A CN 201810372513A CN 108774342 A CN108774342 A CN 108774342A
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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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/02—Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose
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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
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/04—Oxycellulose; Hydrocellulose
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Abstract
The present invention provides a kind of orange oil pickering emulsion stablized using nano-cellulose, the lotion is using nano-cellulose as Solid particle emulsifying agents, and orange oil is oil phase, and the embedding rate of orange oil is 79.60 ~ 88.36%.It is that after ammonium persulfate oxidation modification, nano-cellulose suspension is obtained by washing using microcrystalline cellulose as raw material the present invention also provides above-mentioned orange oil pickering emulsion and preparation method thereof；This suspension is freeze-dried, nano-cellulose powder is obtained；Nano-cellulose powder is scattered in deionized water, nano-cellulose suspension is formed and, by high speed homogenization, obtains stable orange oil pickering emulsion then to orange oil is added in above-mentioned suspension.Orange oil pickering emulsion prepared by the present invention has the characteristics that nano-cellulose dosage is few, preparation process is simple and application cost is low.The present invention can effectively reduce the volatilization of aroma substance in orange oil, increase its stability.
Description
Technical field
The invention belongs to field of food chemical industry, are related to a kind of orange oil pickering emulsion, and specifically a kind of utilize is received
The orange oil pickering emulsion and preparation method thereof that rice cellulose is stablized.
Background technology
Orange oil is produced by cold-press, cold grinding method or steam distillation by the full fruit of orange or skin, is one
Kind flavor oil has unique fragranced, favored by consumers, has been widely used in food, tobacco, cosmetics and medicine
In equal fields.It can be used for allocating a variety of different savory essences of orange, while can also arrange in pairs or groups with other essence, be existed with increasing essence
Pure and fresh elegant sense on sense organ.In addition, terpenes, limonene equal size are higher in orange oil, bacterial growth in food can be inhibited,
It is commonly used in food service industry as antiseptic to improve foodsafety.
However, orange oil is made of limonene and the very strong flavor substance of some other volatility, and highly volatile, indissoluble
Yu Shui, and fragrance remaining time is short, " head perfume (or spice) fragrance " can only be used as to use.And to light, heat and O2It is very sensitive, storage and it is processed
Loss and denaturalization phenomenon are extremely serious in journey, especially lose bigger under the processing environment of high temperature.Therefore, in food processing and production
In the process, it needs to protect orange oil, to reduce its volatility, prevents fragrance from escaping, avoid oxidation deterioration.It is more at present
Orange oil is embedded using microencapsulation technology.
In food processing technology, the carrier systems based on lotion are widely used, can effectively deliver, protect and
Release lipotropic component improves the quality of product, extends its shelf life to make it be not easy to be aoxidized during preservation.Using breast
Change technology, orange oil is emulsified, and can increase its dissolubility, protects aromatic substance from the influence of external environment, thus
The volatility for reducing orange oil aroma substance, expands its application range in the food industry.
Pickering emulsion is a kind of New Emulsion stablized using solid particle, the breast stablized with Small molecular surfactant
There is resistant to aggregation, deflocculation, anti-Ovshinsky to be melted into the advantages such as ripe and stability is good for liquid phase ratio, the system.In recent years, researcher
With a series of edible solid particles such as polysaccharide, protein, it is prepared for stable food-grade pickering emulsion, there is bio-compatible
The advantages that property and environment friendly, the carrier of conveying bioactivator can be used as, it may also be used for coat unstable chemical combination
Object.Using nano-cellulose as Solid particle emulsifying agents, by high speed homogenization, orange oil pickering emulsion is prepared so that orange oil
Water solubility improves its stability well while raising, this method has many advantages, such as that preparation process is simply and at low cost, and
Stability of emulsion is strong, is not easy to be influenced by factors such as system pH, salinity and temperature.At present using nano-cellulose as solid
Particle emulsifying agents, the correlative study for preparing orange oil pickering emulsion have not been reported.
Invention content
For above-mentioned technical problem in the prior art, the present invention provides a kind of orange oil pickering emulsion and its preparations
Method, described this orange oil pickering emulsion and preparation method thereof will solve in the prior art that orange oil aroma quality is not
It is good, oxidizable rotten technical problem.
The present invention provides a kind of orange oil pickering emulsions stablized using nano-cellulose, and the lotion is with nanometer
Cellulose is Solid particle emulsifying agents, and orange oil is oil phase, and the embedding rate of orange oil is 79.60 ~ 88.36%.
The present invention also provides a kind of preparation sides of above-mentioned orange oil pickering emulsion stablized using nano-cellulose
Method includes the following steps：
1）One the step of preparing ammonium persulfate aqueous solution；
It dissolves ammonium persulfate into deionized water, stirring forms ammonium persulfate aqueous solution, in the over cure until fully dissolving
In sour aqueous ammonium, a concentration of 0.5 ~ 2mol/L of the ammonium persulfate；
2）One the step of preparing nano-cellulose suspension；
It weighs microcrystalline cellulose and is added to step 1）In obtained ammonium persulfate aqueous solution, in rotating speed 1000r/min magnetic agitations
Under, it is put into 60 DEG C of water-bath constant temperature and stirs 4 ~ 16h, fully after reaction, stopping agitating and heating obtaining nano-cellulose suspension；
The material ratio of microcrystalline cellulose and ammonium persulfate aqueous solution is 1 ~ 2.5 gram：1L,
3）One the step of preparing nano-cellulose powder；
By step 2）Obtained nano-cellulose suspension is centrifuged at 10000rpm, removes the complete ammonium persulfate of unreacted, from
The heart at least twice, until suspension pH be 7；Precooling 4h, then exists under the conditions of suspension after having centrifuged is placed in -70 DEG C
Condenser temperature is -70 DEG C, vacuum degree is freeze-dried for 24 hours under the conditions of being 5Pa, obtains nano-cellulose powder；
4）One the step of preparing orange oil pickering emulsion；
By step 3）Obtained nano-cellulose powder is dissolved in deionized water, after being sufficiently stirred, obtains nano-cellulose suspension
Liquid, in the nano-cellulose suspension, a concentration of 5 ~ 20g/L of nano-cellulose.In 10000 ~ 19000rpm high
Under fast homogeneous, the orange oil of 2 ~ 8% amounts, high speed homogenization time is added dropwise by percent by volume in nano-cellulose suspension
For 2 ~ 5min, orange oil pickering emulsion is obtained.
A kind of orange oil pickering emulsion of the present invention, is to aoxidize the nano-cellulose to be formed through ammonium persulfate as solid
Then particle emulsifying agents are added orange oil and are formed by lotion.
A kind of preparation method using the orange oil pickering emulsion stablized using nano-cellulose of the present invention is with city
It is raw material to sell microcrystalline cellulose, and after ammonium persulfate oxidation modification, nano-cellulose suspension is obtained by washing；This is hanged
Supernatant liquid is freeze-dried, and obtains nano-cellulose powder；Nano-cellulose powder is scattered in deionized water, nanofiber is formed
Plain suspension, by high speed homogenization, obtains stable orange oil pik woods breast then to orange oil is added in above-mentioned suspension
Liquid.
Cellulose is that nature contains abundant renewable resource, cheap and easy to get, environmentally safe, and having can be again
Raw advantage has the properties such as low-density, Environmental Sustainability, adjustability and low cost.Microcrystalline cellulose is the one of cellulose
Kind important derivatives, are obtained through acidolysis or mechanical treatment by native cellulose, have large specific surface area, high-hydroscopicity and pole
The characteristics such as good mobility can be used as emulsifier and anti-agglomerating agent in view of its unique structure and property.But microcrystalline cellulose
With stronger intermolecular and intramolecular active force, causes it to be insoluble in water, greatly limit its emulsifiability.Through ammonium persulfate
Modified obtained nano-cellulose has the advantageous properties such as higher surface-active, higher length-width ratio and high intensity, is stable
The ideal emulsified material of pickering emulsion.
The present invention is compared with prior art, and technological progress is significant.Orange oil pickering emulsion prepared by the present invention,
Grain size is small and particle diameter distribution is uniform, and nano-cellulose is arranged closely in oil-water interfaces, and Irreversible Adsorption shape occurs in oil-water interfaces
At stable emulsion, it is effectively prevent emulsion polymerization and Ostwald ripening, and the embedding rate of orange oil is up to 79.60 ~ 88.36%, to have
Effect prevents orange oil fragrance from escaping, and increases its stability.Moreover, orange oil pickering emulsion prepared by the present invention has Nanowire
The features such as plain dosage of dimension is few, preparation process is simple and application cost is low.
Description of the drawings
Fig. 1 is the orange oil pickering emulsion outside drawing prepared by the embodiment of the present invention 2.
Specific implementation mode
The invention will now be described in further detail by way of examples and with reference to the accompanying drawings, but is not intended to limit the present invention.
Embodiment 1
（1）The preparation of ammonium persulfate aqueous solution
Ammonium persulfate is dissolved in 1L deionized waters, stirring forms ammonium persulfate aqueous solution, described until fully dissolving
In ammonium persulfate aqueous solution, a concentration of 0.5mol/L of the ammonium persulfate；
（2）The preparation of nano-cellulose suspension
1.5 grams of commercially available microcrystalline celluloses are added to step（1）In obtained 1L ammonium persulfate aqueous solutions, in rotating speed 1000r/
Under min magnetic agitations, it is put into 60 DEG C of water-bath constant temperature stirring 4h and stops agitating and heating fully after reaction, obtain nano-cellulose
Suspension；
（3）The preparation of nano-cellulose powder
By step（2）Obtained nano-cellulose suspension is centrifuged at 10000rpm, removes the complete ammonium persulfate of unreacted, from
Calculation, until the pH of suspension is 7；Precooling 4h under the conditions of suspension after having centrifuged is placed in -70 DEG C, then in cold-trap
Temperature is -70 DEG C, vacuum degree is freeze-dried for 24 hours under the conditions of being 5Pa, obtains nano-cellulose powder；
（4）The preparation of orange oil pickering emulsion
By 1g steps（3）Obtained nano-cellulose powder is dissolved in 100mL deionized waters, after being sufficiently stirred, obtains Nanowire
The plain suspension of dimension.In the nano-cellulose suspension, a concentration of 10g/L of nano-cellulose.In 13000rpm high
Under fast homogeneous, 8mL orange oils are added dropwise in nano-cellulose suspension, the high speed homogenization time is 3min, is formed and is stablized
Orange oil pickering emulsion.
Through determined by ultraviolet spectrophotometry, orange oil embedding rate is 79.60% in the orange oil pickering emulsion of gained.
The assay method of embedding rate is as follows：It takes 2mL lotions to be added in 5mL absolute ethyl alcohols, after whirlpool shakes 3min, stands
3h takes upper layer alcohol layer, is diluted 40 times, its absorbance is surveyed in maximum absorption wave strong point, according to standard curve determination ethyl alcohol
The concentration of orange oil in layer calculates embedding rate according to following equation：
E（Embedding rate）=（m-m1）/m×100%
m：The addition of orange oil, g in emulsion preparation process；
m1：The amount for the orange oil not embedded, g.
Embodiment 2
（1）The preparation of ammonium persulfate aqueous solution
Ammonium persulfate is dissolved in 1L deionized waters, stirring forms ammonium persulfate aqueous solution, described until fully dissolving
In ammonium persulfate aqueous solution, a concentration of 2mol/L of the ammonium persulfate；
（2）The preparation of nano-cellulose suspension
1 gram of microcrystalline cellulose is added to step（1）In obtained 1L ammonium persulfate aqueous solutions, in rotating speed 1000r/min magnetic force
Under stirring, it is put into 60 DEG C of water-bath constant temperature stirring 16h and stops agitating and heating fully after reaction, obtain nano-cellulose suspension
Liquid；
（3）The preparation of nano-cellulose powder
By step（2）Obtained nano-cellulose suspension is centrifuged at 10000rpm, removes the complete ammonium persulfate of unreacted, from
Calculation, until the pH of suspension is 7；Precooling 4h under the conditions of suspension after having centrifuged is placed in -70 DEG C, then in cold-trap
Temperature is -70 DEG C, vacuum degree is freeze-dried for 24 hours under the conditions of being 5Pa, obtains nano-cellulose powder；
（4）The preparation of orange oil pickering emulsion
By 0.5g steps（3）Obtained nano-cellulose powder is dissolved in 100mL deionized waters, after being sufficiently stirred, obtains nanometer
Cellulose suspension.In the nano-cellulose suspension, a concentration of 5g/L of nano-cellulose.In 10000rpm high
Under fast homogeneous, 4mL orange oils are added dropwise in nano-cellulose suspension, the high speed homogenization time is 5min, is formed and is stablized
Orange oil pickering emulsion.
Through determined by ultraviolet spectrophotometry, orange oil embedding rate is 88.36% in the orange oil pickering emulsion of gained.
Embodiment 3
（1）The preparation of ammonium persulfate aqueous solution
Ammonium persulfate is dissolved in 1L deionized waters, stirring forms ammonium persulfate aqueous solution, described until fully dissolving
In ammonium persulfate aqueous solution, a concentration of 1.5mol/L of the ammonium persulfate；
（2）The preparation of nano-cellulose suspension
2 grams of microcrystalline celluloses are added to step（1）In obtained 1L ammonium persulfate aqueous solutions, in rotating speed 1000r/min magnetic force
Under stirring, it is put into 60 DEG C of water-bath constant temperature stirring 12h and stops agitating and heating fully after reaction, obtain nano-cellulose suspension
Liquid；
（3）The preparation of nano-cellulose powder
By step（2）Obtained nano-cellulose suspension is centrifuged at 10000rpm, removes the complete ammonium persulfate of unreacted, from
Calculation, until the pH of suspension is 7；Precooling 4h under the conditions of suspension after having centrifuged is placed in -70 DEG C, then in cold-trap
Temperature is -70 DEG C, vacuum degree is freeze-dried for 24 hours under the conditions of being 5Pa, obtains nano-cellulose powder；
（4）The preparation of orange oil pickering emulsion
By 2g steps（3）Obtained nano-cellulose powder is dissolved in 100mL deionized waters, after being sufficiently stirred, obtains Nanowire
The plain suspension of dimension.In the nano-cellulose suspension, a concentration of 20g/L of nano-cellulose.In 19000rpm high
Under fast homogeneous, 6mL orange oils are added dropwise in nano-cellulose suspension, the high speed homogenization time is 2min, is formed and is stablized
Orange oil pickering emulsion.
Through determined by ultraviolet spectrophotometry, orange oil embedding rate is 84.93% in the orange oil pickering emulsion of gained.
Embodiment 4
（1）The preparation of ammonium persulfate aqueous solution
Ammonium persulfate is dissolved in 1L deionized waters, stirring forms ammonium persulfate aqueous solution, described until fully dissolving
In ammonium persulfate aqueous solution, a concentration of 1mol/L of the ammonium persulfate；
（2）The preparation of nano-cellulose suspension
2.5 grams of microcrystalline celluloses are added to step（1）In obtained 1L ammonium persulfate aqueous solutions, in rotating speed 1000r/min magnetic
Under power stirring, it is put into 60 DEG C of water-bath constant temperature stirring 8h and stops agitating and heating fully after reaction, obtain nano-cellulose suspension
Liquid；
（3）The preparation of nano-cellulose powder
By step（2）Obtained nano-cellulose suspension is centrifuged at 10000rpm, removes the complete ammonium persulfate of unreacted, from
Calculation, until the pH of suspension is 7；Precooling 4h under the conditions of suspension after having centrifuged is placed in -70 DEG C, then in cold-trap
Temperature is -70 DEG C, vacuum degree is freeze-dried for 24 hours under the conditions of being 5Pa, obtains nano-cellulose powder；
（4）The preparation of orange oil pickering emulsion
By 1.5g steps（3）Obtained nano-cellulose powder is dissolved in 100mL water, after being sufficiently stirred, obtains nano-cellulose
Suspension.In the nano-cellulose suspension, a concentration of 15g/L of nano-cellulose.It is equal in 16000rpm high speeds
Under matter, 2mL orange oils are added dropwise in nano-cellulose suspension, the high speed homogenization time is 4min, forms stable sweet tea
Orange oil pickering emulsion.
Through determined by ultraviolet spectrophotometry, orange oil embedding rate is 80.68% in the orange oil pickering emulsion of gained.
Claims (2)
1. a kind of orange oil pickering emulsion stablized using nano-cellulose, it is characterised in that：The lotion is with Nanowire
Dimension element is Solid particle emulsifying agents, and orange oil is oil phase, and the embedding rate of orange oil is 79.60 ~ 88.36%.
2. a kind of preparation method of orange oil pickering emulsion stablized using nano-cellulose described in claim 1, special
Sign is：Include the following steps：
1）One the step of preparing ammonium persulfate aqueous solution；
It dissolves ammonium persulfate into deionized water, stirring forms ammonium persulfate aqueous solution, in the over cure until fully dissolving
In sour aqueous ammonium, a concentration of 0.5 ~ 2mol/L of the ammonium persulfate；
2）One the step of preparing nano-cellulose suspension；
It weighs microcrystalline cellulose and is added to step 1）In obtained ammonium persulfate aqueous solution, in rotating speed 1000r/min magnetic agitations
Under, it is put into 60 DEG C of water-bath constant temperature and stirs 4 ~ 16h, fully after reaction, stopping agitating and heating obtaining nano-cellulose suspension；
The material ratio of microcrystalline cellulose and ammonium persulfate aqueous solution is 1 ~ 2.5 gram：1L；
3）One the step of preparing nano-cellulose powder；
By step 2）Obtained nano-cellulose suspension is centrifuged at 10000rpm, removes the complete ammonium persulfate of unreacted, from
The heart at least twice, until suspension pH be 7；Precooling 4h, then exists under the conditions of suspension after having centrifuged is placed in -70 DEG C
Condenser temperature is -70 DEG C, vacuum degree is freeze-dried for 24 hours under the conditions of being 5Pa, obtains nano-cellulose powder；
4）One the step of preparing orange oil pickering emulsion；
By step 3）Obtained nano-cellulose powder is dissolved in deionized water, after being sufficiently stirred, obtains nano-cellulose suspension
Liquid, in the nano-cellulose suspension, a concentration of 5 ~ 20g/L of nano-cellulose；
Under 10000 ~ 19000rpm high speed homogenizations, 2 ~ 8% amounts are added dropwise by percent by volume in nano-cellulose suspension
Orange oil, the high speed homogenization time be 2 ~ 5min, obtain orange oil pickering emulsion.
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Cited By (2)
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| CN110982091A (en) * | 2019-11-17 | 2020-04-10 | 江南大学 | High-stability cyclodextrin emulsion based on interfacial regularity strategy and preparation method thereof |
| CN111171343A (en) * | 2018-11-12 | 2020-05-19 | 中国科学院过程工程研究所 | Emulsion preparation method based on steam-exploded lignin |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111171343A (en) * | 2018-11-12 | 2020-05-19 | 中国科学院过程工程研究所 | Emulsion preparation method based on steam-exploded lignin |
| CN110982091A (en) * | 2019-11-17 | 2020-04-10 | 江南大学 | High-stability cyclodextrin emulsion based on interfacial regularity strategy and preparation method thereof |
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Application publication date: 20181109 |