CN108794775A - A method of preparing Pickering lotions using the nano cellulose crystal of mercerization - Google Patents
A method of preparing Pickering lotions using the nano cellulose crystal of mercerization 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
- 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
- C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
- C08J3/091—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids characterised by the chemical constitution of the organic liquid
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- 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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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
- C08J3/091—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids characterised by the chemical constitution of the organic liquid
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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 invention discloses a kind of methods that the nano cellulose crystal using mercerization prepares Pickering lotions.Cellulosic raw material through mercerization, the nano cellulose crystal of mercerization is obtained after freeze-drying by this method using sulphuric acid hydrolysis through centrifuge washing after dialysis.The nano cellulose crystal of mercerization is as Solid particle emulsifying agents, after being mixed with oil phase, through emulsifying up to Pickering lotions.Nano cellulose crystal is present in oil-water interfaces particle stabilizedly, forms interfacial film, prevents the wadding of liquid poly-, keeps the stabilization of lotion.Oil-water ratio is 1 in lotion:10-4:6, the dosage of nano cellulose crystal is 0.001%-2.0%.The grain size D of prepared lotion（4,3）For 5-60um, centrifugal stability is preferable, under 4000g centrifugal force, creaming of emulsion but is not demulsified；It is not demulsified in addition, the sample without centrifugal treating stores June at room temperature.
Description
Technical field
The present invention relates to Pickering lotions and biomass technical field, and in particular to a kind of nanometer using mercerization
The method that cellulose crystals prepare Pickering lotions.
Background technology
Traditional lotion is the interfacial tension by reduction two-phase using amphiphilic surfactant, is reached a kind of liquid
Body is uniformly scattered in the dispersion formed in another and incompatible liquid.Pickering lotions refer to using glue
Body particle replaces the lotion that traditional emulsifier is stablized.Compared with conventional emulsifier, it is irreversible by colloidal solid
It is adsorbed on two-phase interface, forms interfacial film at interface, or the three-dimensional network knot that colloidal solid is formed in dispersed phase simultaneously
Structure achievees the effect that stable emulsion to prevent the wadding of dispersed phase drop poly-.Compared to traditional lotion, Pickering lotions
Few with stabilizing agent dosage, small to human toxicity effect, ambient pollution burden is low, and lotion has many advantages, such as good stability.
Therefore it has been widely used in fields such as cosmetics, medicine, heterogeneous catalysis and food.
Currently, more with respect to research still prepares Pickering lotions using inorganic particle.Due to biological material
Derive from a wealth of sources, it is renewable, while there is good biocompatibility, therefore utilize the particle stabilized of biomass source in recent years
Pickering lotions gradually start the interest for causing researcher.
Cellulose is as a kind of abundant natural reproducible resource, and using very extensive, while surface is contained largely
Hydroxyl reactive group can be chemically modified its surface, therefore, gradually cause the interest of researcher.Nano-cellulose is
There is a kind of novel high polymer material huge potential using value, ultra-fine nanostructure to make the property of nano-cellulose
There is very big difference with general fibre element in matter.Nanofiber is known as that density is low, and large specific surface area, adsorption capacity is strong, chemical reaction
The advantages that active height, biocompatibility is strong.The unique structure of nano-cellulose and excellent performance, make its preparation and application always
All it is the hot spot studied both at home and abroad.
Nano cellulose crystal is depended on as the particle stabilizers for stablizing Pickering lotions, emulsifiability
The pattern and surface wettability of nano cellulose crystal.The crystal structure for changing nanofiber crystal by mercerization, from
And change the pattern and particle wetting characteristics of nano cellulose crystal.To enhance its emulsifiability.
Invention content
The purpose of the present invention is to provide a kind of sides preparing Pickering lotions using the nanometer cellulose crystal of mercerization
Method.
The present invention is realized using following technical scheme.
A method of Pickering lotions being prepared using the nano cellulose crystal of mercerization, are included the following steps：
By cellulosic raw material through mercerization, sulphuric acid hydrolysis is used after freeze-drying, through centrifuge washing, after dialysis
To the nano cellulose crystal of mercerization；Then using the nano cellulose crystal of mercerization as Solid particle emulsifying agents, with oil
After mixing, through emulsifying up to Pickering lotions.
Preferably, the cellulosic raw material is absorbent cotton, cotton linter, dissolving pulp, commodity MCC and from biological material
It is one or more in multi cellulose raw material of middle extraction etc..
Preferably, the technique of the mercerization is：Cellulosic raw material is immersed in NaOH solution and is reacted, then
With water centrifuge washing to neutrality；A concentration of 16-19wt% of the NaOH solution, the temperature of reaction are 25-26 DEG C, reaction when
Between be 1.5h-1d.
It is further preferred that a concentration of 18.5wt% of the NaOH solution, the temperature of reaction is 25 DEG C, the time of reaction
For 1.5h.
Preferably, the technique of the sulphuric acid hydrolysis cellulose is：Sulphuric acid hydrolysis will be added in cellulose after freeze-drying,
Then water is added and terminates hydrolysis, then staticly settles, centrifuge washing is repeated in lower liquid, cleaning solution is water, until
There is blue gel to get the nanofiber Crystal suspensions of mercerization in centrifugation upper layer.
It is further preferred that the ratio between the cellulosic raw material quality and sulfuric acid volume are 1g:8mL-1g:12mL, sulfuric acid
Mass concentration be 63-65%, the temperature of hydrolysis is 40-45 DEG C, the time 25-40min of hydrolysis.
Preferably, the oil phase is to be in liquid, and oil phase substance not soluble in water at room temperature.Including polar oil, non-
One kind or several in polar oil etc., such as dichloromethane, trichloro ethylene, toluene, hexadecane, atoleine slab oil etc.
Kind.
Preferably, during preparing Pickering lotions, oil-water ratio 1:10-4:6, the dosage of nano cellulose crystal
For 0.001wt%-2.0wt%.
Preferably, the mode of the emulsification is to handle, be ultrasonically treated or both the method being combined using homogenizer.
It is further preferred that in the homogenizer processing procedure, the rotating speed of homogenizer is 3000-7000rpm, homogeneous when
Between be 0.5-5min.
It is further preferred that the temperature of the supersound process is controlled at 15-30 DEG C, ultrasonic time 9-5min, ultrasound interval
It is 2s/3s, ultrasonic power 10-30kw/ml with the working time.
Compared with prior art, the invention has the advantages that：
1, the present invention prepares Pickering breasts using the nano cellulose crystal of mercerization as Solid particle emulsifying agents
Liquid.Nano cellulose crystal is irreversible to be adsorbed on oil-water interfaces, and interfacial film is formed, and prevents the wadding of dispersion particle poly-.
2, the present invention prepares Pickering breasts using the nano cellulose crystal of mercerization as Solid particle emulsifying agents
Liquid.A kind of particle emulsifying agents of new biomass source are provided for the emulsification of Pickering lotions.
3, the grain size D [4.3] of the prepared lotion of this hair is 5-60um, and centrifugal stability is preferable, under 4000g centrifugal force,
It creaming of emulsion but is not demulsified；Storage is not demulsified June at room temperature.
4, Pickering lotions prepared by the present invention have the property of Nantural non-toxic, and nano cellulose crystal is as stabilization
The advantages that agent has dosage few, does not generate foam, and environmental pollution is small, biodegradable and good biocompatibility, can be applied to
Food, drug, cosmetics, medicine and other fields.
Description of the drawings
Fig. 1 a are the AFM figures of the nano cellulose crystal of mercerization prepared by embodiment 5.
Fig. 1 b are the TEM figures of the nano cellulose crystal of mercerization prepared by embodiment 5.
Fig. 2 is that embodiment 5 uses the Pickering lotions that the nano cellulose crystal of mercerization is stablized in microscope
Under emulsion particle figure.
Specific implementation mode
The specific implementation of the present invention is elaborated further with reference to specific embodiment, but the embodiment party of the present invention
Formula is without being limited thereto.
Embodiment 1：
Commodity MCC is immersed in the NaOH solution of a concentration of 16wt%, reaction temperature is 25 DEG C, and the reaction time is
1.5h.Washing is centrifuged repeatedly to neutrality using distilled water after processing, and 63wt% sulphuric acid hydrolysis is used after freeze-drying.Cellulosic material
The ratio between quality and sulfuric acid volume are 1g:8mL, temperature are 40 DEG C, reaction time 25min, to add the distillation of ten times of sulfuric acid dosages
Water terminates hydrolysis.Gained system staticly settles, and centrifuge washing is repeated using distilled water in lower liquid, until centrifugation
Upper liquid shows blue, collects upper layer blue liquid, is placed in the bag filter that molecular cut off is 14000 and dialyses, thoroughly
It is distilled water to analyse the medium used, until for neutrality.Then by hexadecane with oil phase:Water phase volume ratio is 1:9 ratio adds
It is added in the suspension of the nano cellulose crystal after thickening, the dosage of nano-cellulose is 0.001wt%, uses the side of ultrasound
Formula is emulsified, ultrasonic time 30s, 15 DEG C of temperature, and ultrasound works and intermittent time are 2s/3s, amplitude 40%, and ultrasonic power is
10kw/ml.Gained lotion is the Pickering lotions of oil-in-water type, and the processing of 4000g centrifugal intensities is not in demulsifying phenomenon.
In addition, the sample without centrifugal treating is stored 6 months at room temperature does not occur demulsifying phenomenon.
Embodiment 2：
Commodity dissolving pulp is immersed in the NaOH solution of a concentration of 19wt%, reaction temperature is 26 DEG C, and the reaction time is
1d.Washing is centrifuged repeatedly to neutrality using distilled water after processing, and 65wt% sulphuric acid hydrolysis is used after freeze-drying.Cellulosic material matter
The ratio between amount and sulfuric acid volume are 1g:12mL, temperature are 45 DEG C, reaction time 40min, to add the distilled water of ten times of sulfuric acid dosages
Terminate hydrolysis.Gained system staticly settles, and centrifuge washing is repeated using distilled water in lower liquid, until in centrifugation
Layer liquid, which is presented, there is blue, collects upper layer blue liquid, is placed in the bag filter that molecular cut off is 14000 and dialyses, thoroughly
It is distilled water to analyse the medium used, until for neutrality.Then by liquid paraffin with oil phase：Water phase volume ratio 4:6 ratio addition
In the suspension of nano cellulose crystal to after thickening, the dosage of nano-cellulose is 2.0wt%, using ultrasound mode into
Row emulsification, ultrasonic time 3.5min, 30 DEG C of temperature, ultrasound works and intermittent time are 2s/3s, amplitude 40%, and ultrasonic power is
30kw/ml.Gained lotion is the Pickering lotions of oil-in, and the processing of 4000g centrifugal intensities is not in demulsifying phenomenon；This
Outside, the sample without centrifugal treating is stored 6 months at room temperature does not occur demulsifying phenomenon.
Embodiment 3：
Degreasing cotton linter is immersed in the NaOH solution of a concentration of 17.5wt%, reaction temperature is 25.5 DEG C, when reaction
Between be 11.5h.Washing is centrifuged repeatedly to neutrality using distilled water after processing, and 64wt% sulphuric acid hydrolysis is used after freeze-drying.Fiber
The ratio between cellulosic material quality and sulfuric acid volume are 1g:9.6mL, temperature is 42.5 DEG C, reaction time 32.5min, to add ten times of sulphur
The distilled water of sour dosage terminates hydrolysis.Gained system staticly settles, and centrifugation is repeated using distilled water in lower liquid
Washing collects upper layer blue liquid until centrifugation upper liquid presents and blue occurs, is placed in the dialysis that molecular cut off is 14000
It dialyses in bag, the medium used of dialysing is distilled water, until for neutrality.Then by soybean oil with oil phase：Water phase volume ratio
It is 2:5 ratio is added in the suspension of the nano cellulose crystal after thickening, and the dosage of nano-cellulose is 0.1wt%,
It is ultrasonically treated, ultrasonic time 2min, 22.5 DEG C of temperature, ultrasound works are 2s/3s, amplitude 40%, ultrasonic power with the intermittent time
For 20kw/ml.Gained lotion is the Pickering lotions of oil-in-water type, and the processing of 4000g centrifugal intensities is not in that demulsification is existing
As；In addition, the sample without centrifugal treating is stored 6 months at room temperature does not occur demulsifying phenomenon.
Embodiment 4：
Degreasing cotton linter is immersed in the NaOH solution of a concentration of 18.5wt%, reaction temperature is 25 DEG C, the reaction time
For 2h.Washing is centrifuged repeatedly to neutrality using distilled water after processing, and 64wt% sulphuric acid hydrolysis is used after freeze-drying.Cellulosic material
The ratio between quality and sulfuric acid volume are 1g:10mL, temperature are 45 DEG C, reaction time 35min, to add the distillation of ten times of sulfuric acid dosages
Water terminates hydrolysis.Gained system staticly settles, and centrifuge washing is repeated using distilled water in lower liquid, until centrifugation
Upper liquid, which is presented, there is blue, collects upper layer blue liquid, is placed in the bag filter that molecular cut off is 14000 and dialyses,
The medium used of dialysing is distilled water, until for neutrality.Then by soybean oil with oil phase：Water phase volume ratio is 1:10 ratio adds
It is added in the suspension of the nano cellulose crystal after thickening, the dosage of nano-cellulose is 0.6wt%, uses high speed shear
Mode carries out pre-emulsification, the rotating speed 3000rpm of homogenizer, homogenizing time 2.25min.Gained lotion is oil-in-water type
Pickering lotions, the processing of 4000g centrifugal intensities is not in demulsifying phenomenon；In addition, the sample without centrifugal treating is at room temperature
Storage does not occur demulsifying phenomenon in 6 months.
Embodiment 5：
Commodity MCC is immersed in the NaOH solution of a concentration of 18.5wt%, reaction temperature is 25 DEG C, and the reaction time is
1.5h.Washing is centrifuged repeatedly to neutrality using distilled water after processing, and 64wt% sulphuric acid hydrolysis is used after freeze-drying.Cellulosic material
The ratio between quality and sulfuric acid volume are 1g:10mL, temperature are 45 DEG C, reaction time 30min, to add the distilled water of ten gallic acid dosages
Terminate hydrolysis.Gained system staticly settles, and centrifuge washing is repeated using distilled water in lower liquid, until in centrifugation
Layer liquid shows blue, collects upper layer blue liquid, is placed in the bag filter that molecular cut off is 14000 and dialyses, dialyses
The medium used is distilled water, until for neutrality.Then by hexadecane with oil phase：Water phase volume ratio is 2:8 ratio addition
In the suspension of nano cellulose crystal to after thickening, the dosage of nano-cellulose is 1.0wt%, using ultrasound mode into
Row emulsification, ultrasonic time 30s, 25 DEG C of temperature, ultrasound works and intermittent time are 2s/3s, amplitude 40%, and ultrasonic power is
20kw/ml。
The pattern of nano cellulose crystal manufactured in the present embodiment is in approximate ellipsoid, as shown in Figure 1 a, 1 b, it is seen that long
Degree is 15-25nm, width 10-12nm, thickness 5-7nm, draw ratio 1.5-2.5；The crystal form of cellulose shows as fiber
The crystal form of plain II types；Surface charge density is 0.100-0.110e/nm2。
The Pickering lotions obtained after the present embodiment emulsification are the lotion of O/W types, and emulsion particle diameter D (4,3) is 5-
60um has good stability of emulsion, under 4000g centrifugal force, creaming of emulsion but is not demulsified；In addition, without centrifugal treating
Sample store at room temperature 6 months and do not occur demulsifying phenomenon.As shown in Figure 2.The nano-cellulose of the mercerization in the lotion is brilliant
Body is used as Solid particle emulsifying agents, stablize be present on oil-water interfaces, form interfacial film, prevent the wadding of oil phase particulate poly-,
Keep the stabilization of lotion.
Claims (10)
1. a kind of method that nano cellulose crystal using mercerization prepares Pickering lotions, which is characterized in that including with
Lower step：
By cellulosic raw material through mercerization, silk is obtained after dialysis using sulphuric acid hydrolysis after freeze-drying through centrifuge washing
Photochemical nano cellulose crystal；Then mixed with oil phase using the nano cellulose crystal of mercerization as Solid particle emulsifying agents
After conjunction, through emulsifying up to Pickering lotions.
2. according to the method described in claim 1, it is characterized in that, the cellulosic raw material is absorbent cotton, cotton linter, dissolving
Slurry, commodity MCC and from one or more in the multi cellulose raw material extracted in biological material.
3. according to the method described in claim 1, it is characterized in that, the technique of the mercerization is：By cellulose former material
Material, which is immersed in NaOH solution, to react, and then uses water centrifuge washing to neutrality；A concentration of 18-19wt% of the NaOH solution,
The temperature of reaction is 24-26 DEG C, and the time of reaction is 1.5h-1d.
4. according to the method described in claim 1, it is characterized in that, the technique of the sulphuric acid hydrolysis cellulose is：It is dry to freezing
Sulphuric acid hydrolysis is added in cellulose after dry, water is then added and terminates hydrolysis, then staticly settles, by lower liquid repeatedly into
Row centrifuge washing, cleaning solution are water, until centrifugation upper layer blue gel occurs to get the nanofiber crystal suspension of mercerization
Liquid.
5. according to the method described in claim 4, it is characterized in that, the cellulose quality after the freeze-drying and sulfuric acid volume
The ratio between be 1g:8mL-1g:The mass concentration of 12mL, sulfuric acid are 63-65%, and the temperature of hydrolysis is 40-45 DEG C, hydrolysis
Time be 25-40min.
6. according to the method described in claim 1, it is characterized in that, the oil phase is dichloromethane, trichloro ethylene, toluene, just
One or more of hexadecane and atoleine slab oil.
7. according to the method described in claim 1, it is characterized in that：Oil-water ratio is 1 in the Pickering lotions:10-4:6,
The dosage of nano cellulose crystal is 0.001wt%-2.0wt%.
8. according to the method described in claim 1, it is characterized in that, the mode of the emulsification is handled using homogenizer, at ultrasound
The method that reason or both is combined.
9. according to the method described in claim 8, it is characterized in that, in the homogenizer processing procedure, the rotating speed of homogenizer is
The time of 3000-7000rpm, homogeneous are 0.5-5min.
10. according to the method described in claim 8, it is characterized in that, the temperature control of the supersound process surpasses at 15-30 DEG C
The time of sound is 0.5-3.5min, and ultrasound interval is 2s/3s, ultrasonic power 10-30kw/ml with the working time.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111074675A (en) * | 2019-12-04 | 2020-04-28 | 中国科学院理化技术研究所 | Hydrophobic slurry and preparation method and application thereof |
| CN111961349A (en) * | 2020-08-26 | 2020-11-20 | 南京林业大学 | High-strength photoluminescent soybean protein film and preparation method thereof |
| CN113136194A (en) * | 2021-04-26 | 2021-07-20 | 中国石油大学(华东) | Emulsion based on nanocellulose and preparation method and application thereof |
| CN113185709A (en) * | 2021-04-22 | 2021-07-30 | 华南理工大学 | Pickering emulsion based on pineapple peel residue nanocellulose and preparation method thereof |
| CN113647608A (en) * | 2021-09-08 | 2021-11-16 | 河北农业大学 | Oil-in-water gel Pickering emulsion and preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111074675A (en) * | 2019-12-04 | 2020-04-28 | 中国科学院理化技术研究所 | Hydrophobic slurry and preparation method and application thereof |
| CN111961349A (en) * | 2020-08-26 | 2020-11-20 | 南京林业大学 | High-strength photoluminescent soybean protein film and preparation method thereof |
| CN111961349B (en) * | 2020-08-26 | 2022-02-08 | 南京林业大学 | High-strength photoluminescent soybean protein film and preparation method thereof |
| CN113185709A (en) * | 2021-04-22 | 2021-07-30 | 华南理工大学 | Pickering emulsion based on pineapple peel residue nanocellulose and preparation method thereof |
| CN113136194A (en) * | 2021-04-26 | 2021-07-20 | 中国石油大学(华东) | Emulsion based on nanocellulose and preparation method and application thereof |
| CN113647608A (en) * | 2021-09-08 | 2021-11-16 | 河北农业大学 | Oil-in-water gel Pickering emulsion and preparation method and application thereof |
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Application publication date: 20181113 |