CN114409963A - Method for preparing submicron-grade aqueous antioxidant emulsion based on membrane emulsification technology - Google Patents
Method for preparing submicron-grade aqueous antioxidant emulsion based on membrane emulsification technology Download PDFInfo
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Abstract
The invention discloses a method for preparing submicron-grade aqueous antioxidant emulsion based on a membrane emulsification technology, belonging to the field of fine chemical engineering. The invention utilizes the membrane emulsification technology to control the actual size of the antioxidant in a molten state by utilizing the aperture of the glass fiber membrane with different apertures, then utilizes the emulsifier to carry out emulsification, and finally prepares the water-based antioxidant emulsion by reduced pressure distillation. The antioxidant emulsion prepared by the method has controllable particle size, uniform distribution and good stability, and can be stored for a long time.
Description
Technical Field
The invention relates to the technical field of fine chemical engineering, in particular to a method for preparing submicron-order aqueous antioxidant emulsion based on a membrane emulsification technology.
Background
The aqueous antioxidant emulsion has the characteristics of good dispersibility, convenient use, environmental protection and the like, is popular in the wide consumption market, and is widely applied to the fields of aqueous paint, adhesive, synthetic rubber and synthetic resin. The essence of the aqueous antioxidant emulsion is the dispersion of the antioxidant, the continuous phase is submicron-grade antioxidant particles, the continuous phase is water, and the antioxidant is dispersed in the water by virtue of the action of a surfactant to form a special system which is thermodynamically unstable but kinetically stable.
Generally, the particle size of the aqueous antioxidant emulsion is required to be less than 0.5um and the aqueous antioxidant emulsion is required to be uniformly dispersed in order to maintain good stability. The preparation method of the water-based antioxidant emulsion commonly used in the industry at present mainly comprises the following modes, for example, the phase transition technology used in patent CN 201210429339.4 is that the antioxidant is melted and heated, then the emulsifier and a small amount of water are mixed, an antioxidant homogeneous system in a water-in-oil state is formed under the action line of high-speed shearing, then the antioxidant homogeneous body is transited from a water-in-oil structure to an oil-in-water structure by adding water, namely, the phase inversion process under the condition of antioxidant molten state is realized, and the antioxidant emulsion is finally prepared, the technology has higher requirement on the antioxidant, the technology is suitable for preparing high molecular weight antioxidant emulsion, such as hydroquinone dicyclopentadiene polymer (trade mark antioxidant 616, CPL, Wingstay-L), which is not suitable for preparing antioxidant emulsion with high melting point and low molecular weight, is the most mature technology for preparing antioxidant emulsion in industrialization at present; for the high melting point water-based antioxidant, a normal temperature method or a solvent method can be used, such as the method disclosed in patent CN201711134723.0 and patent CN201711134722.6, the method is to dissolve the antioxidant by using a water-soluble solvent, such as ethanol, acetone and the like, water is added in the process of homogenizing and emulsifying in the dissolved antioxidant solution, the antioxidant is precipitated into tiny particles from a continuous phase due to the change of the solubility, an antioxidant emulsion is formed under the action of an emulsifier, and finally the solvent in the system is removed by a reduced pressure distillation mode, the method is characterized in that the water-based antioxidant emulsion can be prepared under the condition of not increasing the temperature, and the method has a small amount of application in the industry at present, but has the limitation that the polarity of the emulsified antioxidant needs to be matched with the used solvent, and the prepared antioxidant emulsion has a long period and is not suitable for large-scale continuous production; for the technology of preparing antioxidant emulsion by a continuous method, there are also reports at present, for example, in the patent of CN 201611209163.6, a rotor pump is used instead of or in line with an emulsifier to perform emulsification phase inversion, and finally, an aqueous antioxidant emulsion is prepared. The particle size of the aqueous antioxidant emulsion prepared by the technology can reach a micron level, and the aqueous antioxidant emulsion is suitable for industrial practical application, but the preparation method has the defects that the prepared antioxidant emulsion has general stability and is easy to separate after being stored for a long time, and a large amount of emulsifier and thickener are required to be added for maintaining the stability of the antioxidant emulsion. The use of a large amount of emulsifiers and thickeners can cause certain influence on the practical application of the subsequent antioxidant, and a method for preparing antioxidant emulsion in the industry is called as a grinding method, wherein the antioxidant is physically ground by using equipment such as a colloid mill, and the longer the grinding time is, the smaller the particle size of the prepared antioxidant emulsion is, but the method has higher energy consumption.
In view of the above-mentioned drawbacks and the actual needs of the current industrial development, how to provide an antioxidant emulsion with excellent stability is a problem to be solved by those skilled in the art.
Disclosure of Invention
In view of the above, the invention provides a method for preparing a submicron-grade aqueous antioxidant emulsion based on a membrane emulsification technology, wherein the pore size of a membrane in the membrane emulsification process is controllable, membranes with different pore sizes can be selected according to the requirement of actual particle size, and further the aqueous antioxidant emulsion with controllable particle size and narrow distribution can be prepared.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing submicron-order aqueous antioxidant emulsion based on a membrane emulsification technology comprises the following steps:
(1) placing the antioxidant part in a reaction kettle, heating to melt, and then placing in a membrane emulsifying machine for membrane emulsification, wherein the continuous phase at the outer side of the membrane is an emulsifier aqueous solution and the temperature is higher than the melting point of the antioxidant;
(2) increasing the pressure of a melt cavity of the membrane emulsifying machine to enable the antioxidant in a molten state to enter a continuous phase part on the outer side of the membrane through a glass fiber membrane, and obtaining antioxidant emulsion;
(3) and (3) carrying out reduced pressure concentration treatment on the antioxidant emulsion obtained in the step (2) to obtain high-concentration antioxidant emulsion.
Preferably, the mass ratio of the antioxidant to the emulsifier aqueous solution is (5-40): (60-95).
Preferably, the mass ratio of the emulsifier to the water in the emulsifier aqueous solution is (0.01-0.1): 1.
preferably, the melting point of the antioxidant is less than or equal to 100 ℃.
Preferably, the antioxidant is one or a mixture of more of an antioxidant 245, an antioxidant 1076, an antioxidant DSTP and an antioxidant DLTP.
Preferably, the emulsifier is one or more of polyvinyl alcohol, polyvinylpyrrolidone, hydroxymethyl cellulose, polyethylene glycol, potassium stearate, potassium fatty acid and potassium oleate.
Preferably, the glass fiber membrane has a pore diameter of 50-800nm and no surface charge.
Preferably, the reduced pressure concentration temperature is 40-60 ℃, the pressure is-0.1 MPa, and the solid content of the prepared high-concentration antioxidant emulsion is 40-50%.
According to the technical scheme, compared with the prior art, the invention discloses a method for preparing the submicron-scale aqueous antioxidant emulsion based on the membrane emulsification technology, which has the following beneficial effects:
the whole process of preparing the aqueous antioxidant emulsion by using the membrane emulsification technology has no chemical reaction change, and is safe and environment-friendly. The prepared aqueous antioxidant emulsion has controllable particle size, uniform particle size distribution, good storage stability and long storage time.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a graph of the dynamic flash back-flash curve over time for the sample of example 1;
FIG. 2 is a graph of the dynamic flash back flash curve over time for the sample of example 2;
FIG. 3 is a graph of the dynamic flash back-flash curve over time for the sample of example 3;
FIG. 4 is a graph of the dynamic flash back-flash curve over time for the sample of example 4;
FIG. 5 is a graph of the dynamic flash back-flash curve over time for the samples of example 5;
fig. 6 is a graph of the dynamic light flash back-flash curve over time for the comparative example.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
(1) Putting 50g of the antioxidant 245 into a reaction kettle, heating to 95 ℃ to completely melt the antioxidant, and putting the melted antioxidant into a film emulsifying machine for film emulsification; the continuous phase part at the outer side of the membrane in the membrane emulsification process is 950g of aqueous solution of polyvinyl alcohol, wherein the polyvinyl alcohol accounts for 5 wt% of the used water, and the temperature is controlled at 95 ℃;
(2) the pressure of the melt cavity of the membrane emulsifying machine is increased, so that the antioxidant 245 in a molten state enters the outer continuous phase part through the gaps (the aperture is 100nm) of the glass fiber membrane of the membrane emulsifying machine, and the antioxidant emulsion can be obtained.
(3) And (3) carrying out reduced pressure concentration on the obtained antioxidant emulsion at 60 ℃ and under the condition of-0.1 Mpa, testing the solid content of the concentrated antioxidant emulsion in the concentration process, and stopping concentration when the solid content reaches 40% so as to obtain the high-concentration antioxidant emulsion.
Example 2
(1) Placing 100g of antioxidant 1076 in a reaction kettle, heating to 65 ℃ to completely melt the antioxidant, and placing the melted antioxidant in a film emulsifying machine for film emulsification; the outer continuous phase part of the membrane during membrane emulsification was 900g of an aqueous solution of potassium oleate, the potassium oleate amounting to 2 wt% of the water used and the temperature was controlled at 65 ℃;
(2) the pressure of the melt cavity of the membrane emulsifying machine is increased, so that the antioxidant 1076 in a molten state enters the outer continuous phase part through the gaps (with the aperture of 500nm) of the glass fiber membrane of the membrane emulsifying machine, and the antioxidant emulsion can be obtained.
(3) And (3) carrying out reduced pressure concentration on the obtained antioxidant emulsion at 40 ℃ and under the condition of-0.1 Mpa, testing the solid content of the concentrated antioxidant emulsion in the concentration process, and stopping concentration when the solid content reaches 50% so as to obtain the high-concentration antioxidant emulsion.
Example 3
(1) Putting 100g of antioxidant 1076 and 100g of antioxidant DLTP into a reaction kettle, heating to 65 ℃ to completely melt the antioxidant, and putting the melted antioxidant into a membrane emulsifying machine for membrane emulsification; in the membrane emulsification process, the continuous phase part at the outer side of the membrane is 800g of aqueous solution of potassium stearate and potassium fatty acid, wherein the potassium stearate and the potassium fatty acid are in any proportion and account for 1 wt% of the used water, and the temperature is controlled at 65 ℃;
(2) and (3) increasing the pressure of a melt cavity of the film emulsifying machine to ensure that the antioxidant 1076 and the antioxidant DLTP in a molten state enter the outer continuous phase part through a gap (the aperture is 250nm) of a glass fiber film of the film emulsifying machine, thus obtaining the antioxidant emulsion.
(3) And (3) carrying out reduced pressure concentration on the obtained antioxidant emulsion at 40 ℃ and under the condition of-0.1 Mpa, testing the solid content of the concentrated antioxidant emulsion in the concentration process, and stopping concentration when the solid content reaches 50% so as to obtain the high-concentration antioxidant emulsion.
Example 4
(1) Putting 50g of the antioxidant 245 and 150g of the antioxidant DSTP into a reaction kettle, heating to 90 ℃ to completely melt the antioxidant, and putting the melted antioxidant into a film emulsifying machine for film emulsification; in the membrane emulsification process, the continuous phase part at the outer side of the membrane is 800g of aqueous solution of potassium oleate and polyethylene glycol, wherein the potassium oleate and the polyethylene glycol are in any proportion and account for 1 wt% of the used water, and the temperature is controlled at 90 ℃;
(2) and (3) increasing the pressure of a melt cavity of the membrane emulsifying machine to ensure that the antioxidant 245 and the antioxidant DLTP in a molten state enter the outer continuous phase part through a gap (the aperture is 300nm) of a glass fiber membrane of the membrane emulsifying machine, thus obtaining the antioxidant emulsion.
(3) And (3) carrying out reduced pressure concentration on the obtained antioxidant emulsion at 60 ℃ and under the condition of-0.1 Mpa, testing the solid content of the concentrated antioxidant emulsion in the concentration process, and stopping concentration when the solid content reaches 50% so as to obtain the high-concentration antioxidant emulsion.
Example 5
(1) 50g of antioxidant DSTP is placed in a reaction kettle, the reaction kettle is heated to 90 ℃ to completely melt the antioxidant, and the melted antioxidant is placed in a membrane emulsifying machine for membrane emulsification; the continuous phase part at the outer side of the membrane in the membrane emulsification process is 400g of aqueous solution of hydroxymethyl cellulose, wherein the hydroxymethyl cellulose accounts for 1 wt% of the used water, and the temperature is controlled at 90 ℃;
(2) and (3) increasing the pressure of a melt cavity of the membrane emulsifying machine to enable the antioxidant DLTP in a molten state to enter an outer continuous phase part through a gap (the aperture is 400nm) of a glass fiber membrane of the membrane emulsifying machine, so as to obtain the antioxidant emulsion.
(3) And (3) carrying out reduced pressure concentration on the obtained antioxidant emulsion at 60 ℃ and under the condition of-0.1 Mpa, testing the solid content of the concentrated antioxidant emulsion in the concentration process, and stopping concentration when the solid content reaches 50% so as to obtain the high-concentration antioxidant emulsion.
Comparative example
The antioxidant 245 was physically milled using a colloid mill using an aqueous solution of polyvinyl alcohol as the dispersion, wherein the polyvinyl alcohol accounted for 5 wt% of the water used, for 12 hours to obtain a dispersion of the antioxidant 245.
And (3) testing and conclusion:
the aqueous antioxidants obtained in examples 1 to 5 and comparative example were tested for their average particle diameter (Dz) and particle size distribution index (PDI) using a dynamic light scattering particle sizer (ZS-90, Markov. England) and for their stability using a dynamic light scattering stabilizer (Turbiscan, Formulation, France) according to the following table:
| solid content (%) | Average particle diameter (nm) | PDI | |
| Example 1 | 40 | 100.8 | 0.029 |
| Example 2 | 50 | 503.1 | 0.083 |
| Example 3 | 50 | 247.2 | 0.035 |
| Example 4 | 50 | 303.2 | 0.039 |
| Example 5 | 50 | 397.4 | 0.041 |
| Comparative example | 40 | 1850 | 0.386 |
As can be seen from the table, the particle size of the antioxidant emulsion prepared by the membrane emulsification technology is equivalent to the size of the used glass fiber membrane, and the particle size distribution index PDI value of the prepared antioxidant emulsion is less than 0.1, which is narrow particle size distribution. In the comparative example, the grain size of the antioxidant emulsion prepared by using the grinding technology is micron-sized, and the grain size distribution index is particularly wide and is far larger than 0.1.
FIGS. 1 to 5, which are shown in the description of the drawings, are dynamic light scattering stability curves (back flash mode) of the antioxidant emulsions prepared in examples 1 to 5, and it can be seen from the measurement of 24 hours that the intensity of the back flash light of the samples in examples 1 to 5 hardly changes with the lapse of time, whereas in the comparative example, it can be seen that the intensity of the light at the bottom of the sample cell containing the antioxidant emulsion prepared in the comparative example becomes significantly weaker with the lapse of the test time, the light scattering curve is shifted to the right, and the light intensity signal at the upper part of the sample increases, which indicates that the sample has been delaminated, the lower part of the sample cell becomes clear, and the sample becomes unstable.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. A method for preparing submicron-order aqueous antioxidant emulsion based on a membrane emulsification technology is characterized by comprising the following steps:
(1) placing the antioxidant part in a reaction kettle, heating to melt, and then placing in a membrane emulsifying machine for membrane emulsification, wherein the continuous phase at the outer side of the membrane is an emulsifier aqueous solution and the temperature is higher than the melting point of the antioxidant;
(2) increasing the pressure of a melt cavity of the membrane emulsifying machine to enable the antioxidant in a molten state to enter a continuous phase part on the outer side of the membrane through a glass fiber membrane, and obtaining antioxidant emulsion;
(3) and (3) carrying out reduced pressure concentration treatment on the antioxidant emulsion obtained in the step (2) to obtain high-concentration antioxidant emulsion.
2. The method for preparing the submicron-sized aqueous antioxidant emulsion based on the membrane emulsification technology as claimed in claim 1, wherein the mass ratio of the antioxidant to the emulsifier aqueous solution is (5-40): (60-95).
3. The method for preparing the submicron-sized aqueous antioxidant emulsion based on the membrane emulsification technology as claimed in claim 1 or 2, wherein the mass ratio of the emulsifier to water in the emulsifier aqueous solution is (0.01-0.1): 1.
4. the method for preparing submicron-sized aqueous antioxidant emulsion based on membrane emulsification technology as claimed in claim 1, wherein the melting point of the antioxidant is less than or equal to 100 ℃.
5. The method for preparing submicron-sized aqueous antioxidant emulsion based on membrane emulsification technology as claimed in claim 4, wherein the antioxidant is one or more of antioxidant 245, antioxidant 1076, antioxidant DSTP, antioxidant DLTP.
6. The method for preparing submicron-sized aqueous antioxidant emulsion based on membrane emulsification technology as claimed in claim 1, wherein the emulsifier is one or more of polyvinyl alcohol, polyvinylpyrrolidone, hydroxymethyl cellulose, polyethylene glycol, potassium stearate, potassium fatty acid, and potassium oleate.
7. The method for preparing submicron-sized aqueous antioxidant emulsion based on membrane emulsification technology as claimed in claim 1, wherein the glass fiber membrane has a pore size of 50-800nm and no surface charge.
8. The method for preparing submicron-sized aqueous antioxidant emulsion based on membrane emulsification technology as claimed in claim 1, wherein the concentration under reduced pressure is at 40-60 deg.C and-0.1 MPa, and the solid content of the prepared high-concentration antioxidant emulsion is 40-50%.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005028254A (en) * | 2003-07-10 | 2005-02-03 | Taisho Pharmaceut Co Ltd | Emulsion production device |
| JP2009178698A (en) * | 2008-02-01 | 2009-08-13 | Kanagawa Acad Of Sci & Technol | Monodisperse emulsion produced by membrane emulsification method, method for producing the same and method for producing polymer fine particle and composite particle by using the method |
| CN110151695A (en) * | 2019-06-05 | 2019-08-23 | 山东大学 | A kind of method that low-energy emulsification prepares anti-oxidant nano oil-in-water emulsion |
| CN110627929A (en) * | 2019-10-25 | 2019-12-31 | 长春工业大学 | Preparation method of micro-nano polymer water-based antioxidant emulsion |
| CN113875968A (en) * | 2020-07-03 | 2022-01-04 | 广州中国科学院先进技术研究所 | Preparation method of oil-soluble plant extract emulsion |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005028254A (en) * | 2003-07-10 | 2005-02-03 | Taisho Pharmaceut Co Ltd | Emulsion production device |
| JP2009178698A (en) * | 2008-02-01 | 2009-08-13 | Kanagawa Acad Of Sci & Technol | Monodisperse emulsion produced by membrane emulsification method, method for producing the same and method for producing polymer fine particle and composite particle by using the method |
| CN110151695A (en) * | 2019-06-05 | 2019-08-23 | 山东大学 | A kind of method that low-energy emulsification prepares anti-oxidant nano oil-in-water emulsion |
| CN110627929A (en) * | 2019-10-25 | 2019-12-31 | 长春工业大学 | Preparation method of micro-nano polymer water-based antioxidant emulsion |
| CN113875968A (en) * | 2020-07-03 | 2022-01-04 | 广州中国科学院先进技术研究所 | Preparation method of oil-soluble plant extract emulsion |
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