CN109821470A - A kind of preparation method of density switch type compound emulsifying agent - Google Patents
A kind of preparation method of density switch type compound emulsifying agent Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of density switch type compound emulsifying agent, compound emulsifying agent hydroxyapatite solution and nor-leucine solution are mixed first, adjust the pH of water phase, then a certain proportion of oily phase is added, obtained solution is emulsified under high-speed mixer, obtains stable Pickering lotion.After a certain amount of deionized water is added in the stable lotion, quick and complete demulsification may be implemented.Raw material of the present invention is nontoxic green, biological safety is splendid, abundance is easy to get, low in cost, synthesis technology is simple, easy to implement, product quality stabilization and good process repeatability, especially Pickering lotion has switch property to emulsifier concentration, the amount that need to only control the deionized water of addition can realize the complete demulsification for preparing stable lotion and lotion, lotion prepared by the present invention has higher stability, the nontoxic green of the emulsifier being related to, Switching Condition is very simple and easy, has good practical value.
Description
Technical field
The invention belongs to Colloid and interface chemistry fields, and in particular to a kind of preparation side of density switch type compound emulsifying agent
Method.
Background technique
Pickering lotion is always that preparation is steady due to its unique membrana granulosa stable mechanism and continuous phase rheological behavior
The indispensable method for determining lotion has important application value in food, cosmetics and medicine and other fields.But in reality
During production and living, people generally require to regulate and control emulsion intercalation method according to the needs of itself, such as in the specific time
It needs to destroy its stability of emulsion under the conditions of or, so environmental response type lotion was concerned in recent years.
Such as CN108440770A disclose a kind of pH value and the dual regulation of temperature switching mode Pickering emulsion and its
Preparation method, by the Pickering lotion for the oil-in-water type that emulsifier, oil phase and water phase form, emulsifier includes nano-silica
Silicon carbide particle and the block polyether copolymer for containing oxyethylene chain (EO chain) and oxypropylene chain (PO chain).CN106582431A is disclosed
A kind of room temperature carbon dioxide switching mode compound emulsifying agent, by commodity nanometer silicon dioxide particle and CO2/ without any modification
N2 surfactant is formed, and belongs to Pickering emulsion by the stable emulsion of the emulsifier, into emulsion
Lead to emulsifier inactivation and emulsion breakdown after being passed through N2 or air, is passed through CO into the system2, then emulsifier can be made to restore to live
Property, stable Pickering emulsion can be retrieved.CN106943949B, which is disclosed, a kind of prepares temperature sensitive type Pickering
Poly(N-isopropylacrylamide) and cellulose acetate are dissolved in acetone by the method for emulsifier respectively;By poly- (N- isopropyl third
Acrylamide) shell solution of the acetone soln as coaxial EFI, using the acetone soln of cellulose acetate as coaxial EFI
Stratum nucleare solution carries out EFI and prepares microballoon;Ultraviolet irradiation needle point exports solidified microsphere, collects microballoon;To containing the water-soluble of microballoon
Liquid carries out frozen dried to get temperature sensitive type Pickering emulsifier is arrived.
Though the above method develops certain methods to realize the preparation of switching mode lotion, there are still need biocompatibility
Bad surfactant compounds, and needs harsh device requirement, the triggering agent higher cost of addition or the triggering of realization
The deficiencies of condition higher cost.
Summary of the invention
It is rich and easy to get, low in cost that the purpose of the present invention is to provide a kind of raw material sources, and synthesis technology is simple and technique
Reproducible, easy to implement, biological safety is splendid, and product quality is stablized, and stability of emulsion is higher, and to emulsifier concentration
The preparation method of sensitive density switch type compound emulsifying agent.
The implementation of the object of the invention is that a kind of preparation method of density switch type compound emulsifying agent, specific steps are such as
Under:
1) 0.01mol calcium nitrate is dissolved in 10g deionized water, forms solution A;
2) 0.01mol sodium citrate is dissolved in 10g deionized water, forms solution B;
3) 0.006mol sodium phosphate is dissolved in 10g deionized water, forms solution C;
4) step 2) acquired solution B is added dropwise in step 1) acquired solution A at room temperature, 5min, shape is sufficiently stirred
At mixed liquor one;
5) step 3) acquired solution C is added dropwise in mixed liquor one obtained by step 4) at room temperature, during being added dropwise not
Disconnected stirring continues to stir 10min after completion of dropwise addition, forms mixed liquor two;
6) mixed liquor two obtained by step 5) is transferred in closed hydrothermal reactor, after being reacted 6 hours at 180 DEG C, from
It is so cooled to room temperature, obtains reaction solution;
7) it is centrifuged reaction solution obtained by step 6) to obtain sediment using supercentrifuge, utilizes deionized water and anhydrous second
Three times, excessive electrolyte, is then scattered in deionized water alcohol alternating centrifugal washing precipitate again in removal system, utilizes
0.1M sodium hydroxide solution tune pH to 9.5 obtains solution D, i.e. hydroxyapatite dispersion liquid;
8) nor-leucine is dissolved in deionized water, forms solution E;
9) it is compounded step 7) acquired solution D and step 8) acquired solution E to obtain the water phase of 10mL, be sufficiently stirred
10min, wherein the mass fraction of hydroxyapatite is 0.5%-5%, and the concentration of nor-leucine is 5-50mmol/L;Then it utilizes
PH is adjusted to 4.0-10.0 by 0.1M sodium hydroxide solution or 0.1M hydrochloric acid solution, and 25-30mL oil phase is added, 10min is sufficiently stirred,
Form mixed liquor three;
The oil is mutually paraffin oil or biodiesel;
10) mixed liquor three obtained by step 9) is formed into stable lotion in the emulsified 2min of high-speed mixer;
11) 15-120mL deionized water is added into lotion stable obtained by step 10), originally stable lotion can be quick
Demulsification, obtains density switch type compound emulsifying agent.
The invention has the advantages that the biocompatibility and bioactivity of drug used are preferable, meet wanting for the chemistry of green
It asks, and at low cost.Furthermore a certain amount of by being added by the preparation-obtained lotion of hydroxyapatite to the concentration sensitive of emulsifier
Deionized water can realize demulsification, good process repeatability.
The present invention provides the systems of the switching mode compound emulsifying agent compounded based on hydroxyapatite nanoparticle with leucine
Preparation Method.The present invention is not related to any toxic additive, and addition water can realize quickly in simple original emulsion system
Complete demulsification.The present invention can be widely applied to food, cosmetics, medicine and other fields.
Detailed description of the invention
Fig. 1 is the X-ray diffractogram of water soluble hydroxy phosphorite nanocrystalline prepared by embodiment 1.
Fig. 2 is the transmission electron microscope photo of water soluble hydroxy phosphorite nanocrystalline prepared by embodiment 1.
Fig. 3 is lotion photo (standing 24 hours) prepared by embodiment 1.
Specific embodiment
The present invention first mixes compound emulsifying agent hydroxyapatite solution and nor-leucine solution, adjusts the pH of water phase,
Then a certain proportion of oily phase is added, obtained solution is emulsified under high-speed mixer, obtains stable Pickering
Lotion.After a certain amount of deionized water is added in the stable lotion, quick and complete demulsification may be implemented.Pass through the concentration to emulsifier
Adjusting control emulsion intercalation method.
The present invention is described in detail with specific embodiment below.
Experimental method used in following embodiments is conventional method unless otherwise specified.
The materials, reagents and the like used in the following examples is commercially available unless otherwise specified.
Embodiment 1:
1) 0.01mol calcium nitrate is dissolved in 10g deionized water, forms solution A;
2) 0.01mol sodium citrate is dissolved in 10g deionized water, forms solution B;
3) 0.006mol sodium phosphate is dissolved in 10g deionized water, forms solution C;
4) step 2) acquired solution B is added dropwise in step 1) acquired solution A at room temperature, 5min, shape is sufficiently stirred
At mixed liquor one;
5) step 3) acquired solution C is added dropwise in mixed liquor one obtained by step 4) at room temperature, during being added dropwise not
Disconnected stirring continues to stir 10min after completion of dropwise addition, forms mixed liquor two;
6) mixed liquor two obtained by step 5) is transferred in closed hydrothermal reactor, after being reacted 6 hours at 180 DEG C, from
It is so cooled to room temperature, obtains reaction solution;
7) it is centrifuged reaction solution obtained by step 6) to obtain sediment using supercentrifuge, utilizes deionized water and anhydrous second
Three times, excessive electrolyte, is then scattered in deionized water alcohol alternating centrifugal washing precipitate again in removal system, utilizes
0.1M sodium hydroxide solution tune pH to 9.5 obtains solution D, i.e. hydroxyapatite solution.
8) nor-leucine is dissolved in deionized water, forms solution E;
9) it is compounded hydroxyapatite solution obtained by step 7) and step 8) acquired solution E to obtain the water phase of 10mL,
10min is sufficiently stirred, wherein the mass fraction of hydroxyapatite is 1%, and the concentration of nor-leucine is 5mmol/L, is then utilized
PH is adjusted to 4.5 by 0.1M hydrochloric acid solution, and 5mL paraffin oil is added, and 10min is sufficiently stirred, and forms mixed liquor three;
10) mixed liquor three obtained by step 9) is formed into stable lotion in the emulsified 2min of high-speed mixer;
11) 15mL deionized water is added into lotion stable obtained by step 10), originally stable lotion can quickly be broken
Cream obtains density switch type compound emulsifying agent.
The X-ray of water soluble hydroxy phosphorite nanocrystalline in the density switch type compound emulsifying agent of Ordering-the embodiment preparation is spread out
It penetrates figure and sees Fig. 1, illustrate that product is pure ha and crystallinity is good.The transmission electron microscope of water soluble hydroxy phosphorite nanocrystalline
Photo is shown in Fig. 2, illustrates that product is nano-scale Rod-like shape, and particle size is very uniform.
The form that the density switch type compound emulsifying agent of Ordering-the embodiment preparation stands 24 hours is shown in Fig. 3, and explanation prepares
Density switch type compound emulsifying agent it is highly stable.
Embodiment 2: with embodiment 1, the difference is that,
9) it is compounded hydroxyapatite solution obtained by step 7) and step 8) acquired solution E to obtain the water phase of 10mL,
10min is sufficiently stirred, wherein the mass fraction of hydroxyapatite is 0.5%, and the concentration of nor-leucine is 10mmol/L, then sharp
PH is adjusted to 4.0 with 0.1M hydrochloric acid solution, 5mL paraffin oil is added, 10min is sufficiently stirred, forms mixed liquor three;
11) 40mL deionized water is added into lotion stable obtained by step 10), originally stable lotion can quickly be broken
Cream obtains density switch type compound emulsifying agent.
Embodiment 3: with embodiment 1, the difference is that,
9) it is compounded hydroxyapatite solution obtained by step 7) and step 8) acquired solution E to obtain the water phase of 10mL,
10min is sufficiently stirred, wherein the mass fraction of hydroxyapatite is 1.5%, and the concentration of nor-leucine is 15mmol/L, then sharp
PH is adjusted to 5.0 with 0.1M hydrochloric acid solution, 5mL biodiesel is added, 10min is sufficiently stirred, forms mixed liquor three;
11) 50mL deionized water is added into lotion stable obtained by step 10), originally stable lotion can quickly be broken
Cream obtains density switch type compound emulsifying agent.
Embodiment 4: with embodiment 1, the difference is that,
9) it is compounded hydroxyapatite solution obtained by step 7) and step 8) acquired solution E to obtain the water phase of 10mL,
10min is sufficiently stirred, wherein the mass fraction of hydroxyapatite is 2%, and the concentration of nor-leucine is 20mmol/L, is then utilized
PH is adjusted to 5.5 by 0.1M hydrochloric acid solution, and 5mL biodiesel is added, and 10min is sufficiently stirred, and forms mixed liquor three;
11) 45mL deionized water is added into lotion stable obtained by step 10), originally stable lotion can quickly be broken
Cream obtains density switch type compound emulsifying agent.
Embodiment 5: with embodiment 1, the difference is that,
9) it is compounded hydroxyapatite solution obtained by step 7) and step 8) acquired solution E to obtain the water phase of 10mL,
10min is sufficiently stirred, wherein the mass fraction of hydroxyapatite is 2.5%, and the concentration of nor-leucine is 25mmol/L, then sharp
PH is adjusted to 10.0 with 0.1M sodium hydroxide solution, 5mL paraffin oil is added, 10min is sufficiently stirred, forms mixed liquor three;
11) 90mL deionized water is added into lotion stable obtained by step 10), originally stable lotion can quickly be broken
Cream obtains density switch type compound emulsifying agent.
Embodiment 6: with embodiment 1, the difference is that,
9) it is compounded hydroxyapatite solution obtained by step 7) and step 8) acquired solution E to obtain the water phase of 10mL,
10min is sufficiently stirred, wherein the mass fraction of hydroxyapatite is 3%, and the concentration of nor-leucine is 30mmol/L, is then utilized
PH is adjusted to 9.0 by 0.1M sodium hydroxide solution, and 5mL paraffin oil is added, and 10min is sufficiently stirred, and forms mixed liquor three;
11) 100mL deionized water is added into lotion stable obtained by step 10), originally stable lotion can quickly be broken
Cream obtains density switch type compound emulsifying agent.
Embodiment 7: with embodiment 1, the difference is that,
9) it is compounded hydroxyapatite solution obtained by step 7) and step 8) acquired solution E to obtain the water phase of 10mL,
10min is sufficiently stirred, wherein the mass fraction of hydroxyapatite is 4%, and the concentration of nor-leucine is 20mmol/L, is then utilized
PH is adjusted to 7.0 by 0.1M sodium hydroxide solution, and 5mL biodiesel is added, and 10min is sufficiently stirred, and forms mixed liquor three;
11) 95mL deionized water is added into lotion stable obtained by step 10), originally stable lotion can quickly be broken
Cream obtains density switch type compound emulsifying agent.
Embodiment 8: with embodiment 1, the difference is that,
9) it is compounded hydroxyapatite solution obtained by step 7) and step 8) acquired solution E to obtain the water phase of 10mL,
10min is sufficiently stirred, wherein the mass fraction of hydroxyapatite is 5%, and the concentration of nor-leucine is 50mmol/L, is then utilized
PH is adjusted to 6.0 by 0.1M hydrochloric acid solution, and 12mL biodiesel is added, and 10min is sufficiently stirred, and forms mixed liquor three;
11) 120mL deionized water is added into lotion stable obtained by step 10), originally stable lotion can quickly be broken
Cream obtains density switch type compound emulsifying agent.
Comparative example 1:
1) 0.01mol calcium nitrate is dissolved in 10g deionized water, forms solution A;
2) 0.01mol sodium citrate is dissolved in 10g deionized water, forms solution B;
3) 0.006mol sodium phosphate is dissolved in 10g deionized water, forms solution C;
4) step 2) acquired solution B is added dropwise in step 1) acquired solution A at room temperature, 5min, shape is sufficiently stirred
At mixed liquor one;
5) step 3) acquired solution C is added dropwise in mixed liquor one obtained by step 4) at room temperature, during being added dropwise not
Disconnected stirring continues to stir 10min after completion of dropwise addition, forms mixed liquor two;
6) mixed liquor two obtained by step 5) is transferred in closed hydrothermal reactor, after being reacted 6 hours at 180 DEG C, from
It is so cooled to room temperature, obtains reaction solution;
7) it is centrifuged reaction solution obtained by step 6) to obtain sediment using supercentrifuge, utilizes deionized water and anhydrous second
Three times, excessive electrolyte, is then scattered in deionized water alcohol alternating centrifugal washing precipitate again in removal system, utilizes
0.1M sodium hydroxide solution tune pH to 9.5, obtains solution D;
9) it is compounded hydroxyapatite solution obtained by step 7) and step 8) acquired solution E to obtain the water phase of 10mL,
10min is sufficiently stirred, wherein the mass fraction of hydroxyapatite is 1%, and the concentration of nor-leucine is 0mmol/L, is then utilized
PH is adjusted to 7.5 by 0.1M sodium hydroxide solution, and 15mL biodiesel is added, and 10min is sufficiently stirred, and forms mixed liquor three;
10) mixed liquor three obtained by step 9) cannot be formed into stable lotion in the emulsified 2min of high-speed mixer,
Also without switching mode.Mainly because of the proper amount of nor-leucine of addition without step 8), the lemon for causing particle surface to adsorb
Carboxyl on acid group molecule cannot be combined with the amino on nor-leucine, be promoted lipophilic.
Claims (2)
1. a kind of preparation method of density switch type compound emulsifying agent, it is characterised in that: specific step is as follows:
1) 0.01mol calcium nitrate is dissolved in 10g deionized water, forms solution A;
2) 0.01mol sodium citrate is dissolved in 10g deionized water, forms solution B;
3) 0.006mol sodium phosphate is dissolved in 10g deionized water, forms solution C;
4) step 2) acquired solution B is added dropwise in step 1) acquired solution A at room temperature, 5min is sufficiently stirred, formed mixed
Close liquid one;
5) step 3) acquired solution C is added dropwise in mixed liquor one obtained by step 4) at room temperature, is constantly stirred during being added dropwise
It mixes, continues to stir 10min after completion of dropwise addition, form mixed liquor two;
6) mixed liquor two obtained by step 5) is transferred in closed hydrothermal reactor, it is naturally cold after being reacted 6 hours at 180 DEG C
But to room temperature, reaction solution is obtained;
7) it is centrifuged reaction solution obtained by step 6) to obtain sediment using supercentrifuge, be handed over using deionized water and dehydrated alcohol
Three times for centrifuge washing sediment, electrolyte excessive in removal system, is then scattered in deionized water again, utilizes 0.1M hydrogen
Sodium hydroxide solution tune pH to 9.5 obtains solution D, i.e. hydroxyapatite dispersion liquid;
8) nor-leucine is dissolved in deionized water, forms solution E;
9) it is compounded step 7) acquired solution D and step 8) acquired solution E to obtain the water phase of 10mL, 10min is sufficiently stirred,
Wherein the mass fraction of hydroxyapatite is 0.5%-5%, and the concentration of nor-leucine is 5-50mmol/L;Then 0.1M hydrogen is utilized
PH is adjusted to 4.0-10.0 by sodium hydroxide solution or 0.1M hydrochloric acid solution, and 25-30mL oil phase is added, and 10min is sufficiently stirred, and is formed mixed
Close liquid three;
The oil is mutually paraffin oil or biodiesel;
10) mixed liquor three obtained by step 9) is formed into stable lotion in the emulsified 2min of high-speed mixer;
11) 15-120mL deionized water is added into lotion stable obtained by step 10), originally stable lotion can quickly be broken
Cream obtains density switch type compound emulsifying agent.
2. a kind of preparation method of density switch type compound emulsifying agent according to claim 1, it is characterised in that: by right
The adjusting of the concentration of emulsifier controls emulsion intercalation method.
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