CN109911910A - A kind of kaolin piece and its stripping means can be used for emulsion-stabilizing - Google Patents
A kind of kaolin piece and its stripping means can be used for emulsion-stabilizing Download PDFInfo
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- CN109911910A CN109911910A CN201910238979.9A CN201910238979A CN109911910A CN 109911910 A CN109911910 A CN 109911910A CN 201910238979 A CN201910238979 A CN 201910238979A CN 109911910 A CN109911910 A CN 109911910A
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Abstract
The invention discloses a kind of kaolin pieces and its stripping means that can be used for emulsion-stabilizing.Its method is to carry out surface to kaolin molecule using 3-aminopropyltriethoxysilane to be modified, reduce the active force of kaolin molecule interlayer, it recycles the cavitation of ultrasonic wave and intercalator dimethyl sulfoxide is assisted to accelerate intercalation speed, utilize microwave energy segmentally heating, intercalation can be achieved to carry out simultaneously with removing, prepare thickness in the kaolin piece of Nano grade.The medicine have the advantages that raw material is simple, it is easily operated；Obtained kaolin piece can effectively keep radial dimension while greatly reduce thickness, have high width-thickness ratio, have the function of excellent stable emulsion.
Description
Technical field
The invention belongs to field of nanometer material technology, and in particular to a kind of kaolin piece that can be used for emulsion-stabilizing and its removing
Method.
Background technique
Kaolin is a kind of important nonmetallic clay mineral, and constituent is mainly kaolinite and kaolin.It is brilliant
Body structure is formed by one layer of Si-O tetrahedron and one layer of Al (O, OH) octahedron repeated arrangement on c-axis, the O and Al in the face Si-O
The hydroxyl (OH) in the face (O, OH), which will be combined into hydrogen bond, to be connected between layers, and layered silicate structure, hydrogen bond and model are formed
The collective effect of De Huali makes connection between layers very close, and interlamellar spacing is about 0.72nm.Crystal structure is stable
Kaolin has a series of excellent physicochemical properties, in papermaking, ceramics and refractory material, coating, gum filler, enamel
Glaze etc. is with a wide range of applications.
The crude kaolin individual particle flat crystal of nature is often uncommon, most of kaolin sector-meeting weight
The particle to form laminated is stacked, partial size is generally at 10-20 μm or so.In order to obtain the thinner kaolin piece of partial size, then
It needs to use kaolinic Peeling Technology to peel away crystal stack.Currently used kaolin stripping method is mainly organic
Tool method and stripping chemical method are respectively separated kaolin piece by mechanical lapping and intercalator intercalation.Both methods is equal
In place of Shortcomings.It is easy to be mixed into impurity in the process of mechanical lapping, influences the purity of kaolin piece.And traditional intercalator
Stripping means is by the way of Convective Heating, and due to generally carrying out at room temperature, process is complicated, and the period is long, often persistently several
It, efficiency and its low.
Summary of the invention
For deficiency existing for prior art described above, the first object of the present invention is to provide a kind of be applied in lotion
In so that it is shown the kaolin piece that can be used for emulsion-stabilizing of excellent dispersion stabilization.
It is low in cost another object of the present invention is to provide a kind of process is simple, it is easily operated, can separate with a thickness of
The kaolin piece stripping means that can be used for emulsion-stabilizing of nanoscale kaolin piece.The kaolin piece has low oil absorption,
High width-thickness ratio, the characteristic of high-specific surface area can be used to improve oil/water emulsion intercalation method.
The technical solution adopted by the present invention to solve the technical problems is: a kind of kaolin piece can be used for emulsion-stabilizing,
Its thickness is at 800~1700 nanometers, applied to making it show excellent dispersion stabilization in lotion.
Preferably, it can be used for the thickness of the kaolin piece of emulsion-stabilizing at 1000~1500 nanometers.
A kind of stripping means for the kaolin piece can be used for emulsion-stabilizing comprising the step of it is as follows:
(1) kaolin, 3-aminopropyltriethoxysilane (APTES) and intercalator are pressed into 1:(5~15): (5~15)
It is stirred 5~10 minutes after mass ratio mixing, forms mixture；
(2) mixture is put into micro-wave oven, i.e., with the microwave power of 30~130W and 90~120 DEG C of temperature heating 5
It~10 hours, microwave frequency 1-5 GHz, persistently stirs in microwave heating process；
(3) reactant after heating is used into ethyl alcohol and acetone washing 3~5 times respectively；
(4) it is dried 8~16 hours in 65~75 DEG C of drying box, the kaolin piece after being removed.
Preferably, a kind of stripping means for the kaolin piece can be used for emulsion-stabilizing comprising the step of it is as follows:
(1) kaolin, 3-aminopropyltriethoxysilane (APTES) and intercalator are pressed into 1:(5~15): (5~15)
It is stirred 5~10 minutes after mass ratio mixing, forms mixture；
(2) mixture is subjected to ultrasonic treatment 5~30 minutes；
(3) mixture is put into micro-wave oven, i.e., with the microwave power of 30~130W and 90~120 DEG C of temperature heating 5
It~10 hours, microwave frequency 1-5 GHz, persistently stirs in microwave heating process；
(4) reactant after heating is used into ethyl alcohol and acetone washing 3~5 times respectively；
(5) it is dried 8~16 hours in 65~75 DEG C of drying box, the kaolin piece after being removed.
Preferably, in described (1) step, kaolin, 3-aminopropyltriethoxysilane (APTES) and intercalator
Mass ratio is 1:(8~12): (8~12).
The intercalator can be dimethyl sulfoxide (DMSO), dimethylformamide, formamide, hydrazine, acetamide, acetic acid
One or more kinds of combinations in caesium, potassium acetate or ammonium acetate.
Preferably, the intercalator can be dimethyl sulfoxide (DMSO).
The ultrasonic treatment can use frequency of sound wave for 10khz~1800khz, and power density is the sound of 1~500w/L
Wave processing, and the stirring with revolving speed not higher than 100RPM under sound wave effect of irradiation, can be promoted with not causing to interfere sound wave
3-aminopropyltriethoxysilane makes intercalator enter kaolin interlayer spacings, while ultrasound modifying kaolin effect
Wave itself, which has, promotes intercalator peeling effect.
Preferably, the ultrasonic treatment is handled using staged, is first 10khz~100khz with frequency of sound wave, power is close
Degree is sonicated 5-10 minutes of 1~10w/L；It then is 100khz~500khz with frequency of sound wave, power density is 10~
The sonicated of 100w/L 5-10 minutes；Finally with frequency of sound wave it is between 500khz~1800khz that power density is 100~
The sonicated of 500w/L 5-10 minutes.Staged ultrasonication, can be improved efficiency and yield.
In (3) step, mixture is put into micro-wave oven and carries out segmentally heating, first with 30-45W microwave power and
40-65 DEG C temperature microwave heating 10-20 minutes, with 40-60W microwave power and 60-85 DEG C temperature microwave heating 10-20 minutes,
Finally with 90-120 DEG C of temperature microwave heating 6-12h of 50-130W microwave power, frequency is 2.45 GHz, in microwave heating process
Lasting stirring.
Preferably, in described (3) step, mixture is put into micro-wave oven and carries out segmentally heating, first with 30W microwave power
With 50 DEG C temperature microwave heating 15 minutes, with 45W microwave power and 75 DEG C temperature microwave heating 15 minutes, finally with 60W microwave
100 DEG C of 7 h of temperature microwave heating of power.
The present invention carries out surface to kaolin with 3-aminopropyltriethoxysilane and is modified, 3- aminopropyl triethoxy
Silane can destroy the binding force of kaolin interlayer, reduce the active force of kaolin molecule interlayer, while the sky of auxiliary ultrasonic
Change effect, so that the intercalations agent molecule such as DMSO is easier to intercalation, under the assistance of microwave intercalation energy, while DMSO molecule intercalation
It expands, so that kaolin molecule leafing slabbing crystal, in order to realize the removing of more efficient, while preventing intercalation insufficient
When microwave power is excessive causes unwanted side reaction, the mode of segmentally heating is taken in microwave heating, i.e., first with lower microwave
Power and lower temperature heating, then the method for increasing power stage by stage and improving temperature are removed.
The beneficial effects of the present invention are: raw material is simple, and it is easily operated, it is not involved with mechanical mill stripping, heating and temperature control
Under kaolin crystal decomposition temperature, kaolinic crystal structure will not be destroyed, the complete nano material of lattice structure can be made
The kaolin piece of rank；Obtained kaolin piece can effectively keep radial dimension while greatly reduce thickness, have high wide
Thickness rate has the function of excellent stable emulsion.
Detailed description of the invention
Fig. 1 is the SEM photograph of kaolin piece after removing；
Fig. 2 is that DLS analyzes result photo；
Fig. 3 is the TEM photo of the kaolin piece after removing；
Fig. 4 is to be added to the lotion of kaolin piece sample at (a) (b) (c) and be not added with the lotion point of kaolin piece sample
Not after rocking and placed 5 days and 60 days comparison diagram (wherein mixed emulsion sample 2 be added to removing after kaolin piece sample
Product).
Specific embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
The present invention is modified to kaolin progress surface by the way that characteristic reagent is added, so that intercalator is easier to intercalation, then passes through
The mode of microwave heating improves heating efficiency, accelerates intercalator intercalation speed, by controlling microwave radiation frequencies, heating temperature and
Heating time, so that kaolin is peeling-off while intercalation, nano-grade crystal is made in a step.
Embodiment 1
A kind of stripping means for the kaolin piece can be used for emulsion-stabilizing, its step are as follows:
(1) by the kaolin of 0.5g (Acros Organics) and 5g3- aminopropyltriethoxywerene werene (APTES,
Acros Organics) and 5.5g dimethyl sulphoxide solution (DMSO, Fisher Chemical) mixing, by mixture ultrasound
Processing 5 minutes；
(2) mixture of (1) is put into micro-wave oven (Discover SP, CEM), with 30W microwave power and 50 DEG C of temperature
Degree microwave heating 15 minutes, with 45W microwave power and 75 DEG C temperature microwave heating 15 minutes, finally with 100 DEG C of 60W microwave power
Temperature microwave heating 7h, frequency are 2.45 GHz, are persistently stirred in microwave heating process；
(3) reactant after heating is used into ethyl alcohol and acetone washing 3 times respectively；
(4) night is dried in 65 DEG C of drying box, obtains sample.
Kaolin piece SEM and DLS manufactured in the present embodiment analysis as shown in Figure 1-3, its diameter range for showing 800~
1700nm, thickness can not be measured accurately, but may determine that the thickness of the kaolin piece after removing exists by tem analysis result
Tens nanometers even several nanometers.
As shown in figure 4, the kaolin piece of the method for the present invention preparation also has the function of stable emulsion.We will be after removing
Kaolin piece sample is added in the mixed emulsion of dodecane and water, is rocked and be placed 5 days and 60 days heels do not add height
The mixed emulsion of ridge soil piece sample dodecane and water compares, and discovery is added to the mixing of the dodecane and water of kaolin piece sample
The dispersion stabilization of lotion is more excellent.
Embodiment 2
A kind of stripping means for the kaolin piece can be used for emulsion-stabilizing, its step are as follows:
(1) by the kaolin of 1g (Acros Organics) and 6g3- aminopropyltriethoxywerene werene (APTES,
Acros Organics) and 6g dimethyl sulphoxide solution (DMSO, Fisher Chemical) mixing, at mixture ultrasound
Reason 9 minutes forms mixture；
It (2) with frequency of sound wave is first 50khz by mixture, power density is sonicated 8 minutes of 5w/L；Then it uses
Frequency of sound wave is 200khz, and power density is sonicated 10 minutes of 20w/L；It is finally 800khz, power with frequency of sound wave
Density is sonicated 10 minutes of 400w/L.
(3) mixture of (1) is put into micro-wave oven (Discover SP, CEM), with 35W microwave power and 55 DEG C of temperature
Degree microwave heating 15 minutes, with 50W microwave power and 80 DEG C temperature microwave heating 15 minutes, finally with 110 DEG C of 70W microwave power
Temperature microwave heating 6h, frequency are 2.45 GHz, are persistently stirred in microwave heating process；
(4) reactant after heating is used into ethyl alcohol and acetone washing 4 times respectively；
(5) night is dried in 70 DEG C of drying box, obtains sample.
Kaolin piece SEM and DLS analysis manufactured in the present embodiment is almost the same with 1 result of embodiment；It is real with embodiment 1
The excellent effect for the stable emulsion tested.
Embodiment 3
A kind of stripping means for the kaolin piece can be used for emulsion-stabilizing, its step are as follows:
(1) by the kaolin of 1g (Acros Organics) and 11g3- aminopropyltriethoxywerene werene (APTES,
Acros Organics) and 10g dimethyl sulphoxide solution (DMSO, Fisher Chemical) mixing, at mixture ultrasound
Reason 10 minutes forms mixture；
It (2) with frequency of sound wave is first 60khz by mixture, power density is sonicated 8 minutes of 8w/L；Then it uses
Frequency of sound wave is 400khz, and power density is sonicated 7 minutes of 35w/L；It is finally 1500khz, power with frequency of sound wave
Density is sonicated 5 minutes of 400w/L.
(3) mixture of (1) is put into micro-wave oven (Discover SP, CEM), with 40W microwave power and 60 DEG C of temperature
Degree microwave heating 15 minutes, with 70W microwave power and 90 DEG C temperature microwave heating 10 minutes, finally with 105 DEG C of 80W microwave power
Temperature microwave heating 6.5h, frequency are 2.45 GHz, are persistently stirred in microwave heating process；
(4) reactant after heating is used into ethyl alcohol and acetone washing 5 times respectively；
(5) night is dried in 65 DEG C of drying box, obtains sample.
The kaolin piece of the method for the present invention preparation according to SEM and DLS analysis shows diameter range in 800~1700nm,
Thickness can not be measured accurately, but may determine that the thickness of the kaolin piece after removing at tens by tem analysis result
Nanometer even several nanometers.
Kaolin piece SEM and DLS analysis manufactured in the present embodiment is almost the same with 1 result of embodiment；It is real with embodiment 1
The excellent effect for the stable emulsion tested.
Embodiment 4
A kind of stripping means for the kaolin piece can be used for emulsion-stabilizing, its step are as follows:
(1) by the kaolin of 1g (Acros Organics) and 9g3- aminopropyltriethoxywerene werene (APTES,
Acros Organics) and 9g dimethyl sulphoxide solution (DMSO, Fisher Chemical) mixing, at mixture ultrasound
Reason 8 minutes forms mixture；
It (2) with frequency of sound wave is first 20khz by mixture, power density is sonicated 5 minutes of 5w/L；Then it uses
Frequency of sound wave is 300khz, and power density is sonicated 8 minutes of 30w/L；It is finally 1000khz, power with frequency of sound wave
Density is sonicated 6 minutes of 300w/L.
(3) mixture of (1) is put into micro-wave oven (Discover SP, CEM), with 40W microwave power and 60 DEG C of temperature
Degree microwave heating 15 minutes, with 70W microwave power and 90 DEG C temperature microwave heating 10 minutes, finally with 105 DEG C of 80W microwave power
Temperature microwave heating 6.5h, frequency are 2.45 GHz, are persistently stirred in microwave heating process；
(4) reactant after heating is used into ethyl alcohol and acetone washing 5 times respectively；
(5) night is dried in 72 DEG C of drying box, obtains sample.
Kaolin piece SEM and DLS analysis manufactured in the present embodiment is almost the same with 1 result of embodiment；It is real with embodiment 1
The excellent effect for the stable emulsion tested.
Embodiment 4
A kind of stripping means for the kaolin piece can be used for emulsion-stabilizing, its step are as follows:
(1) by the kaolin of 1g (Acros Organics) and 11g3- aminopropyltriethoxywerene werene (APTES,
Acros Organics) and 10g dimethyl sulphoxide solution (DMSO, Fisher Chemical) mixing, at mixture ultrasound
Reason 7 minutes forms mixture；
It (2) with frequency of sound wave is first 80khz by mixture, power density is sonicated 6 minutes of 8w/L；Then it uses
Frequency of sound wave is 250khz, and power density is sonicated 7 minutes of 80w/L；It is finally 1400khz, power with frequency of sound wave
Density is sonicated 7 minutes of 450w/L.
(3) mixture of (1) is put into micro-wave oven (Discover SP, CEM), with 38W microwave power and 56 DEG C of temperature
Degree microwave heating 10 minutes, with 48W microwave power and 85 DEG C temperature microwave heating 13 minutes, finally with 108 DEG C of 75W microwave power
Temperature microwave heating 8h, frequency are 2.45 GHz, are persistently stirred in microwave heating process；
(4) reactant after heating is used into ethyl alcohol and acetone washing 5 times respectively；
(5) night is dried in 70 DEG C of drying box, obtains sample.
Kaolin piece SEM and DLS analysis manufactured in the present embodiment is almost the same with 1 result of embodiment；It is real with embodiment 1
The excellent effect for the stable emulsion tested.
The present invention carries out surface to kaolin with 3-aminopropyltriethoxysilane and is modified, 3- aminopropyl triethoxy
Silane can destroy the binding force of kaolin interlayer, while the cavitation of auxiliary ultrasonic, so that the intercalations agent molecule such as DMSO
It is easier to intercalation, under the assistance of microwave intercalation energy, is expanded while DMSO molecule intercalation, so that kaolin molecule leafing
Slabbing crystal causes to be not required in order to which microwave power is excessive when realizing the removing of more efficient, while preventing intercalation insufficient
The side reaction wanted, microwave heating are taken the mode of segmentally heating, i.e., are first heated with lower microwave power and lower temperature, then sublevel
Duan Jia great power and the method for improving temperature are removed.The method of the present invention raw material is simple, easily operated, is not involved with machinery
Mill stripping, heating and temperature control will not destroy kaolinic crystal structure under kaolin crystal decomposition temperature, lattice knot can be made
The kaolin piece of the complete nano material rank of structure.The method of the present invention preparation kaolin piece according to SEM and DLS analysis shows
Diameter range in 800~1700nm, thickness can not be measured accurately, but after may determine that removing by tem analysis result
Kaolin piece thickness tens nanometers even several nanometers.The kaolin piece of the method for the present invention preparation, which also has, stablizes cream
The effect of liquid.Kaolin piece sample after removing is added in the mixed emulsion of dodecane and water by we, high with no addition
The mixed emulsion of ridge soil piece sample dodecane and water compares, and discovery is added to the mixing of the dodecane and water of kaolin piece sample
The dispersion stabilization of lotion is more excellent.
As described above, only presently preferred embodiments of the present invention, when cannot be limited the scope of implementation of the present invention with this,
All still belong to this hair according to simple equivalent changes and modifications made by scope of the present invention patent and invention description content generally
In the range of bright patent covers.
Claims (9)
1. a kind of kaolin piece that can be used for emulsion-stabilizing, which is characterized in that its thickness is at 800~1700 nanometers.
2. a kind of stripping means of kaolin piece that can be used for emulsion-stabilizing according to claim 1, which is characterized in that its
The steps included are as follows:
(1) kaolin, 3-aminopropyltriethoxysilane and intercalator are pressed into 1:(5~15): after (5~15) mass ratio mixes
Stirring 5~10 minutes forms mixture；
(2) mixture is put into micro-wave oven, it is small with the microwave power of 30~130W and the heating 5~10 of 90~120 DEG C of temperature
When, microwave frequency 1-5 GHz is persistently stirred in microwave heating process；
(3) reactant after heating is used into ethyl alcohol and acetone washing 3~5 times respectively；
(4) it is dried 8~16 hours in 65~75 DEG C of drying box.
3. a kind of stripping means of kaolin piece that can be used for emulsion-stabilizing according to claim 2, which is characterized in that its
The steps included are as follows:
(1) kaolin, 3-aminopropyltriethoxysilane and intercalator are pressed into 1:(5~15): after (5~15) mass ratio mixes
Stirring 5~10 minutes forms mixture；
(2) mixture is subjected to ultrasonic treatment 5~30 minutes；
(3) mixture is put into micro-wave oven, it is small with the microwave power of 30~130W and the heating 5~10 of 90~120 DEG C of temperature
When, microwave frequency 1-5 GHz is persistently stirred in microwave heating process；
(4) reactant after heating is used into ethyl alcohol and acetone washing 3~5 times respectively；
(5) it is dried 8~16 hours in 65~75 DEG C of drying box.
4. a kind of stripping means of kaolin piece that can be used for emulsion-stabilizing according to claim 3, which is characterized in that institute
State in (1) step, the mass ratio of kaolin, 3-aminopropyltriethoxysilane and intercalator is 1:(8~12): (8~12).
5. a kind of stripping means of kaolin piece that can be used for emulsion-stabilizing according to claim 3, which is characterized in that institute
Stating intercalator is in dimethyl sulfoxide, dimethylformamide, formamide, hydrazine, acetamide, cesium acetate, potassium acetate or ammonium acetate
One or more kinds of combinations.
6. a kind of stripping means of kaolin piece that can be used for emulsion-stabilizing according to claim 3, which is characterized in that institute
Stating ultrasonic treatment uses frequency of sound wave between 10khz~1800khz, and power density is the sonicated of 1~500w/L.
7. a kind of stripping means of kaolin piece that can be used for emulsion-stabilizing according to claim 6, which is characterized in that institute
It states ultrasonic treatment to handle using staged, is first between 10khz~100khz with frequency of sound wave, power density is 1~10w/L's
Sonicated 5-10 minutes；It then is between 100khz~500khz with frequency of sound wave, power density is the sound of 10~100w/L
Wave is handled 5-10 minutes；It is finally between 500khz~1800khz with frequency of sound wave, power density is the sound of 100~500w/L
Wave is handled 5-10 minutes.
8. a kind of stripping means of kaolin piece that can be used for emulsion-stabilizing according to claim 3, which is characterized in that institute
It states in (3) step, mixture is put into micro-wave oven and carries out segmentally heating, first with 30-45W microwave power and 40-65 DEG C of temperature
Microwave heating 10-20 minutes, with 40-60W microwave power and 60-85 DEG C temperature microwave heating 10-20 minutes, finally with 50-
90-120 DEG C of temperature microwave heating 6-12h of 130W microwave power, frequency are 2.45 GHz.
9. a kind of stripping means of kaolin piece that can be used for emulsion-stabilizing according to claim 8, which is characterized in that institute
It states in (3) step, mixture is put into micro-wave oven and carries out segmentally heating, first added with 30W microwave power and 50 DEG C of temperature microwaves
Heat 15 minutes, with 45W microwave power and 75 DEG C temperature microwave heating 15 minutes, finally with 100 DEG C of temperature microwaves of 60W microwave power
Heat 7h.
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