CN110681309A - Method for preparing emulsion by gas-driven emulsification - Google Patents
Method for preparing emulsion by gas-driven emulsification Download PDFInfo
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- CN110681309A CN110681309A CN201910939675.5A CN201910939675A CN110681309A CN 110681309 A CN110681309 A CN 110681309A CN 201910939675 A CN201910939675 A CN 201910939675A CN 110681309 A CN110681309 A CN 110681309A
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Abstract
The invention discloses a method for preparing emulsion by gas-driven emulsification, which comprises the following steps: (1) adding the oil phase and the surfactant into water, heating and uniformly mixing; (2) after the solution system in the step (1) is cooled, feeding the solution system and gas into a gas-driven emulsifying element, and emulsifying to obtain a primary emulsified emulsion; (3) and (3) continuously introducing the emulsion subjected to the primary emulsification in the step (2) into a gas driving emulsification element, and performing circulating emulsification operation to obtain the emulsion. The emulsifying device and the emulsifying method are simple in emulsifying operation, high in emulsifying efficiency and easy to scale up; the prepared emulsion has small and controllable droplet size, uniform dispersion and wide application prospect.
Description
Technical Field
The invention relates to a method for preparing emulsion by gas-driven emulsification, belonging to the technical field of emulsion preparation.
Background
An emulsion is a dispersion of one or more liquids in the form of droplets dispersed in another immiscible liquid, typically consisting of an oil phase, an aqueous phase and a surfactant. The surfactant acts as an emulsifier covering the newly formed droplet surface and provides a stable repulsion between droplet interfaces that strongly inhibits subsequent recombination or association of emulsion droplets. Shear is a necessary condition for preparing an emulsion, and it is necessary to cause a single phase droplet to be stretched by capillary instability and broken into smaller droplets.
Currently, the preparation methods of emulsions are divided into high energy and low energy methods. The high energy method mainly comprises a high pressure homogenization method, a microfluidization method, an ultrasonic method, a jet flow method and the like, and the low energy method mainly comprises a phase inversion method, a spontaneous emulsification method, a solvent replacement method and the like. The high energy method can produce emulsion with good dispersibility and small droplet size in large scale, but usually needs higher energy consumption, has high requirements on equipment and has high cost. Low energy methods have low energy consumption, but have the disadvantage of limited oil phase and solvent throughput; has a corrosion inhibition effect on the nonionic surfactant; a large proportion of solvent and oil is required to produce dispersed phase droplets of small particle size. In chinese patent CN 105285937B, ultrasonic emulsification is used to prepare ginger oil nano emulsion. Although the prepared emulsion is uniform in distribution and good in stability, the method is high in energy consumption and cannot be scaled up, and the method is not beneficial to industrial continuous production. Chinese patent CN 106243273B discloses a method for preparing hydroxyl acrylic emulsion with a shell-core structure by spontaneous polymerization emulsification. The emulsion prepared by the method has the advantages of difficult control of droplet size and low production capacity, and is not suitable for industrial production. Chinese patent CN 108464998A discloses a high-pressure homogenization method for preparing a high-stability peppermint essential oil emulsion. Although the prepared essential oil emulsion has higher stability, the droplet size is not uniform, and the production energy consumption is high.
Disclosure of Invention
Aiming at the defects of the method, the invention provides the method for preparing the emulsion by utilizing gas-driven emulsification, the average particle size of the prepared emulsion liquid drop is 8-50 nm, the dispersibility is good, the energy consumption and the cost are low, the treatment capacity is controllable, and the method can be industrially amplified. In order to achieve the purpose, the technical scheme of the invention is as follows:
a method for preparing emulsion by gas-driven emulsification specifically comprises the following steps:
(1) adding the oil phase and the surfactant into water, heating and uniformly mixing;
(2) after the solution system in the step (1) is cooled, feeding the solution system and gas into a gas-driven emulsifying element, and emulsifying to obtain a primary emulsified emulsion;
(3) and (2) continuously introducing the emulsion subjected to primary emulsification in the step (1) into a gas-driven emulsification element, and performing circulating emulsification operation to obtain the emulsion.
Further, in the step (1), the oil phase is one of squalane, isododecane, isohexadecane, olive oil, soybean oil, palm oil, ginger oil and simethicone.
Further, in the step (1), the surfactant is composed of one or more of disodium lauryl sulfosuccinate, disodium cocomonoethanolamide sulfosuccinate, cocodiethanolamide, cocamidopropyl betaine, monolauryl phosphate, fatty alcohol polyoxyethylene ether, glyceryl monostearate, fatty acid polyoxyethylene alkyl ester, polyoxyethylene sorbitan monostearate and sorbitan stearate.
Further, in the step (1), the mass ratio of the oil phase to the surfactant is 1: 0.01-1; the mass ratio of the oil phase to the water phase is 1: 0.1-10.
Further, in the step (1), the mixture is stirred and mixed at a stirring speed of 100-1000 rpm for 20-100 min, and the heating temperature is 30-100 ℃.
Further, in the step (2), the cooling temperature of the solution system is 0-30 ℃, the flow of the solution system pumped into the gas driven emulsifying element by the pump is 1-20L/h, and the flow rate of the gas fed into the gas driven emulsifying element is 100-12000L/h.
Further, in the step (2), the emulsifying element is composed of a three-way valve and a slender pipe, the aperture of three holes of the three-way valve is 2-20 mm, the inner diameter of the slender pipe is 1-10 mm, the length of the slender pipe is 2-100 cm, one hole of the three-way valve is connected with the slender pipe, and the other two holes are respectively inlets of raw materials and gas.
Further, in the step (3), the cycle number is 2-100.
The principle of the invention is as follows: the oil-water mixed solution is pumped to the inner cavity of the three-way valve, and air is introduced into the inner cavity of the three-way valve through an air compressor. The air impacts the oil-water mixed solution to accelerate the flow of the system, and the generated turbulence plays a role in shearing, so that the oil phase and the water phase are emulsified; in the slender pipe, the oil phase and the water phase are emulsified due to the strong shearing force generated by the large velocity gradient from the pipe wall to the pipe; after the gas is introduced into the slender pipe, the generated bubbles generate an emulsifying effect similar to ultrasonic cavitation due to implosion and collapse; the large shear rate at the orifice of the elongated tube also produces strong shear forces to promote emulsification.
Compared with the prior art, the invention has the beneficial effects that: the invention adopts a gas-driven emulsification technology with high efficiency and low cost, has simple operation and low equipment requirement, is easy for large-scale industrial production and can realize large-scale production. The emulsion liquid drop prepared by the invention has the particle size of 8-50 nm and good dispersibility, can be widely applied to the fields of personal care, food production, fermentation industry and the like, and has good application prospect.
Drawings
FIG. 1 is a flow chart of an apparatus for preparing an emulsion by gas-driven emulsification according to the present invention, in which 1 is a raw material liquid storage tank, 2 is a feed pump, 3 is a first liquid flow control valve, 4 is a gas flow control valve, 5 is a compressed air storage tank, 6 is a three-way valve, 7 is an elongated tube, 8 is an emulsion storage tank, 9 is a circulation pump, and 10 is a second liquid flow control valve. Wherein 6, 7 constitute the emulsifying element;
FIG. 2 is a graph showing the particle size distribution under the conditions of example 2.
Detailed Description
The present invention is further illustrated by the following specific examples, but the scope of the invention is not limited thereto.
Example 1
A method for preparing emulsion by gas-driven emulsification comprises the following specific steps: (1) weighing 10g of squalane and 0.1g of surfactant formed by mixing fatty alcohol-polyoxyethylene ether and glycerin monostearate, wherein the mass ratio of the fatty alcohol-polyoxyethylene ether to the glycerin monostearate is 1:1, simultaneously adding the squalane and the surfactant into 100g of water, heating and stirring at the temperature of 50 ℃ and the stirring speed of 100rpm for 20min, and uniformly mixing; (2) after the solution system in the step (1) is cooled to 30 ℃, sending the solution system into a gas-driven emulsification element by a pump at a flow rate of 5L/h, and sending air into the gas-driven emulsification element at a flow rate of 100L/h by an air compressor, wherein the aperture of three holes of a tee joint in the emulsification element is 5mm, the inner diameter of a slender pipe is 2mm, the length of the slender pipe is 30cm, and emulsifying to obtain a first-emulsified squalane emulsion; (3) and (3) continuously pumping the once emulsified squalane emulsion into an emulsifying element by using a pump, repeating the emulsifying operation, and circulating for 5 times to obtain the circularly emulsified squalane emulsion. The average particle diameter of the squalane emulsion droplets was 50 nm.
Example 2
A method for preparing emulsion by a gas-driven emulsifying element comprises the following specific steps: (1) weighing 10g of dimethyl silicone oil and 4g of surfactant formed by mixing fatty acid polyoxyethylene alkyl ester and polyoxyethylene sorbitan monostearate, wherein the mass ratio of the fatty acid polyoxyethylene alkyl ester to the polyoxyethylene sorbitan monostearate is 3:1, simultaneously adding the dimethyl silicone oil and the surfactant into 90g of water, heating and stirring for 60min at the temperature of 90 ℃ and the stirring speed of 600rpm, and uniformly mixing; 2) after the solution system in the step 1) is cooled to 25 ℃, sending the solution system into a gas-driven emulsification element by a pump at a flow rate of 10L/h, and sending air into the gas-driven emulsification element by an air compressor at a flow rate of 600L/h, wherein the aperture of three holes of a tee joint in the emulsification element is 8mm, the inner diameter of a slender pipe is 1mm, the length of the slender pipe is 100cm, and a primary emulsified silicone oil emulsion is obtained after emulsification; 3) and (3) continuously pumping the once emulsified silicone oil emulsion into an air driving emulsifying element by using a pump, repeating the emulsifying operation, and circulating for 3 times to obtain the circularly emulsified silicone oil emulsion. FIG. 2 is a particle size distribution diagram of the silicone oil emulsion prepared under the conditions of this example. As can be seen from the figure, the average particle diameter of the silicone oil emulsion is 8 nm; the liquid drop with the average particle size of 4nm has the highest proportion, which reaches 14.7 percent, and the particle size distribution is narrow.
Example 3
A method for preparing emulsion by a gas-driven emulsifying element comprises the following specific steps: (1) 10g of ginger oil and 1g of sorbitan stearate are weighed. Adding ginger oil and sorbitan stearate into 10g of water at the same time, heating and stirring at 70 ℃ and the stirring speed of 1000rpm for 100min, and uniformly mixing; (2) after the solution system in the step (1) is cooled to 5 ℃, sending the solution system into a gas-driven emulsification element by a pump at a flow rate of 20L/h, and sending air into the gas-driven emulsification element by an air compressor at a flow rate of 800L/h, wherein the aperture of three holes of a tee joint in the emulsification element is 5mm, the inner diameter of a slender pipe is 2mm, the length of the slender pipe is 2cm, and a primary emulsified ginger oil emulsion is obtained after emulsification; (3) and (3) continuously pumping the once emulsified ginger oil emulsion into an air driving emulsifying element by using a pump, repeating the emulsifying operation, and circulating for 10 times to obtain the circularly emulsified ginger oil emulsion. The average particle diameter of the ginger oil emulsion liquid drop is 48 nm.
Example 4
A method for preparing emulsion by a gas-driven emulsifying element comprises the following specific steps: (1) weighing 10g of isododecane and 0.5g of surfactant formed by mixing fatty alcohol-polyoxyethylene ether, polyoxyethylene sorbitan monostearate and sorbitan stearate, wherein the mass ratio of the fatty alcohol-polyoxyethylene ether, the polyoxyethylene sorbitan monostearate and the sorbitan stearate is 1:2:2, simultaneously adding the isododecane and the surfactant into 1g of water, heating and stirring for 45min at 65 ℃ and the stirring speed of 350rpm, and uniformly mixing; (2) after the solution system in the step (1) is cooled to 0 ℃, sending the solution system into a gas-driven emulsification element by a pump at a flow rate of 15L/h, and sending air into the gas-driven emulsification element at a flow rate of 1200L/h by using an air compressor, wherein the aperture of three holes of a tee joint in the emulsification element is 6mm, the inner diameter of a slender pipe is 5mm, the length of the slender pipe is 30cm, and a once-emulsified isododecane emulsion is obtained after emulsification; (3) and (3) continuously pumping the once emulsified isododecane emulsion into a gas driving emulsifying element by using a pump, repeating the emulsifying operation, and circulating for 100 times to obtain the circularly emulsified isododecane emulsion. The average particle diameter of the isododecane emulsion droplets was 39 nm.
Example 5
A method for preparing emulsion by a gas-driven emulsifying element comprises the following specific steps: (1) weighing 10g of palm oil and 5g of surfactant formed by mixing disodium lauryl sulfosuccinate, disodium cocomonoethanolamide sulfosuccinate, disodium cocodiethanolamide and cocamidopropyl betaine, wherein the mass ratio of the disodium lauryl sulfosuccinate to the disodium cocomonoethanolamide sulfosuccinate to the cocodiethanolamide to the cocamidopropyl betaine is 1:2:1:1, simultaneously adding the palm oil and the surfactant into 30g of deionized water, heating and stirring at the temperature of 30 ℃ and the stirring speed of 800rpm for 70min, and uniformly mixing; (2) after the solution system in the step (1) is cooled to 10 ℃, sending the solution system into a gas-driven emulsification element by a pump at a flow rate of 16L/h, and sending air into the gas-driven emulsification element at a flow rate of 12000L/h by using an air compressor, wherein the aperture of three holes of a tee joint in the emulsification element is 15mm, the inner diameter of a slender pipe is 7mm, the length of the slender pipe is 60cm, and a once emulsified palm oil emulsion is obtained after emulsification; (3) and (3) continuously pumping the once emulsified palm oil emulsion into a gas driving emulsifying element by using a pump, repeating the emulsifying operation, and circulating for 50 times to obtain the circularly emulsified palm oil emulsion. The average particle size of the palm oil emulsion droplets was 29 nm.
Example 6
A method for preparing emulsion by a gas-driven emulsifying element comprises the following specific steps: (1) weighing 10g of olive oil and 6g of monolauryl phosphate, simultaneously adding the olive oil and the monolauryl phosphate into 48g of deionized water, heating and stirring for 25min at the water bath temperature of 95 ℃ and the stirring speed of 500rpm, and uniformly mixing; (2) after the solution system in the step (1) is cooled to 20 ℃, sending the solution system into a gas-driven emulsification element by a pump at the flow rate of 1L/h, and sending air into the gas-driven emulsification element at the flow rate of 1500L/h by using an air compressor, wherein the aperture of three holes of a tee joint in the emulsification element is 9mm, the inner diameter of a slender pipe is 1.8mm, the length of the slender pipe is 100cm, and emulsifying to obtain a primary emulsified olive oil emulsion; (3) and (3) continuously pumping the once emulsified olive oil emulsion into a gas driving emulsifying element by using a pump, repeating the emulsifying operation, and circulating for 10 times to obtain the circularly emulsified olive oil emulsion. The average particle size of the olive oil emulsion droplets was 23 nm.
Example 7
A method for preparing emulsion by a gas-driven emulsifying element comprises the following specific steps: (1) weighing 10g of soybean oil, 7.5g of disodium cocomonoethanolamide sulfosuccinate, cocodiethanolamide and monolauryl phosphate, wherein the mass ratio of the disodium cocomonoethanolamide sulfosuccinate to the cocodiethanolamide to the monolauryl phosphate is 1:1:1, simultaneously adding the soybean oil and a surfactant into 70g of deionized water, heating and stirring at 75 ℃ and a stirring speed of 750rpm for 60min, and uniformly mixing; (2) after the solution system in the step (1) is cooled to 15 ℃, sending the solution system into a gas-driven emulsification element by a pump at the flow rate of 12L/h, and sending air into the gas-driven emulsification element at the flow rate of 2500L/h by using an air compressor, wherein the aperture of three holes of a tee joint in the emulsification element is 20mm, the inner diameter of a slender pipe is 10mm, the length of the slender pipe is 2cm, and a once emulsified soybean oil emulsion is obtained after emulsification; (3) and (3) continuously pumping the once emulsified soybean oil emulsion into an air driving emulsifying element by using a pump, repeating the emulsifying operation, and circulating for 30 times to obtain the circularly emulsified soybean oil emulsion. The average particle size of the soybean oil emulsion droplets was 30 nm.
Example 8
A method for preparing emulsion by a gas-driven emulsifying element comprises the following specific steps: (1) weighing 10g of isohexadecane, 10g of disodium coconut monoethanolamide sulfosuccinate, coconut diethanolamide and monolauryl phosphate, wherein the mass ratio of the disodium coconut monoethanolamide sulfosuccinate, the coconut diethanolamide and the monolauryl phosphate is 1:3:1, simultaneously adding isohexadecane and a surfactant into 70g of deionized water, heating and stirring at 100 ℃ and the stirring speed of 850rpm for 90min, and uniformly mixing; (2) after the solution system in the step (1) is cooled to 10 ℃, sending the solution system into a gas-driven emulsification element by a pump at a flow rate of 12L/h, and sending air into the gas-driven emulsification element at a flow rate of 1400L/h by using an air compressor, wherein the aperture of three holes of a tee joint in the emulsification element is 2mm, the inner diameter of a slender pipe is 1mm, the length of the slender pipe is 100cm, and a once emulsified isohexadecane emulsion is obtained after emulsification; (3) and (3) continuously pumping the once emulsified isohexadecane emulsion into a gas driving emulsifying element by using a pump, repeating the emulsifying operation, and circulating for 2 times to obtain the circularly emulsified isohexadecane emulsion. The average particle diameter of the isohexadecane emulsion droplets was 42 nm.
The invention also provides a device for preparing emulsion by gas-driven emulsification, which comprises a raw material liquid storage tank 1, a feeding pump 2, a first liquid flow regulating valve 3, a gas flow regulating valve 4, a compressed air storage tank 5, a three-way valve 6, a slender pipe 7, an emulsion storage tank 8, a circulating pump 9 and a second liquid flow regulating valve 10, as shown in figure 1. The raw material liquid storage tank 1, the feed pump 2 and the left inlet of the three-way valve 6 are sequentially connected through a stainless steel conveying pipeline, and a first liquid flow regulating valve 3 is installed in the conveying pipeline connecting the feed pump 2 and the three-way valve 6; the compressed air storage tank 5 is connected with an upper inlet of the three-way valve 6 through a rubber air pipe, and the rubber air pipe is internally provided with a gas flow regulating valve 4; one end of the slender tube 7 is connected with the right outlet of the three-way valve 6; the right port of the slender tube 7 is connected with an emulsion storage tank 8; the emulsion storage tank 8 is connected with a circulating pump 9 through a stainless steel pipe; the circulating pump 9 is connected with the raw material liquid storage tank 1 through a stainless steel pipe, wherein a second liquid flow regulating valve 10 is installed in the conveying pipeline.
The work flow of the whole device is as follows: the oil phase and the water phase are premixed in a raw material liquid storage tank 1 and enter a left inlet of a three-way valve through a first liquid flow regulating valve 3 under the driving of a feed pump 2. Meanwhile, air enters an upper inlet of the three-way valve from a compressed air storage tank 5 through a gas flow regulating valve 4 and is mixed with oil-water feed liquid in the three-way valve 6. The mixing proportion of the raw materials and the air can be controlled by adjusting the first liquid flow regulating valve 3 and the gas flow regulating valve 4, so as to control the emulsification of the oil and the water; the mixed oil, water and gas phases pass through the elongated tube 7 from the right outlet of the three-way valve to complete the emulsification process. The emulsified emulsion enters an emulsion storage tank 8, and the air is discharged to the external environment. The emulsion passes through the circulating pump and gets into raw materials liquid storage tank 1 from the emulsion storage tank through second liquid flow control valve 10, and the emulsification is repeated next time, can repeat 2 ~ 100 times generally. The device has low equipment requirement, is simple to operate, can prepare the emulsion at low cost, is easy for large-scale industrial production, and can realize large-scale production.
Claims (8)
1. A method for preparing an emulsion by gas-driven emulsification, which is characterized in that: the method specifically comprises the following steps:
(1) adding the oil phase and the surfactant into water, heating and uniformly mixing;
(2) after the solution system in the step (1) is cooled, feeding the solution system and gas into a gas-driven emulsifying element, and emulsifying to obtain a primary emulsified emulsion;
(3) and (3) continuously introducing the emulsion subjected to the primary emulsification in the step (2) into a gas driving emulsification element, and performing circulating emulsification operation to obtain the emulsion.
2. The method of claim 1, wherein: in the step (1), the oil phase is one of squalane, isododecane, isohexadecane, olive oil, soybean oil, palm oil, ginger oil and simethicone.
3. The method of claim 1, wherein: in the step (1), the surfactant is composed of one or a mixture of more of disodium lauryl sulfosuccinate, disodium cocomonoethanolamide sulfosuccinate, diethanolamide cocoate, cocamidopropyl betaine, monolauryl phosphate, fatty alcohol polyoxyethylene ether, glyceryl monostearate, polyoxyethylene fatty acid alkyl ester, polyoxyethylene sorbitan monostearate and sorbitan stearate.
4. The method of claim 1, wherein: in the step (1), the mass ratio of the oil phase to the surfactant is 1: 0.01-1; the mass ratio of the oil phase to the water phase is 1: 0.1-10.
5. The method of claim 1, wherein: in the step (1), the materials are stirred and mixed, the stirring speed is 100-1000 rpm, the stirring time is 20-100 min, and the heating temperature is 30-100 ℃.
6. The method of claim 1, wherein: in the step (2), the cooling temperature of the solution system is 0-30 ℃, the flow of the solution system pumped into the gas driven emulsifying element by a pump is 1-20L/h, and the flow rate of the gas fed into the gas driven emulsifying element is 100-12000L/h.
7. The method of claim 1, wherein: in the step (2), the emulsifying element consists of a three-way valve and a slender pipe, the aperture of three holes of the three-way valve is 2-20 mm, the inner diameter of the slender pipe is 1-10 mm, the length of the slender pipe is 2-100 cm, one hole of the three-way valve is connected with the slender pipe, and the other two holes are respectively inlets of raw materials and gas.
8. The method of claim 1, wherein: in the step (3), the cycle time is 2-100 times.
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| CN114307708A (en) * | 2022-01-07 | 2022-04-12 | 苏州大学 | Method for continuously preparing drug-loaded nano-emulsion |
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