RU2688154C1 - Device for producing nanocapsules of vitamins - Google Patents

Abstract

FIELD: chemistry.

SUBSTANCE: invention relates to an apparatus for producing nanocapsules of vitamins. Proposed device comprises mix crushing and mixing device composed of electrohydraulic shock disperser. Heat exchanger is arranged between electric dispersant and filter to reduce temperature of obtained product prior to filtering. Electrohydropercussion dispersant comprises housing forming working chamber, inlet branch pipes, housing includes high-voltage electrodes, wherein first high-voltage electrode is installed in mixture of liquids, and the second one - in air volume, at that high-voltage electrodes are connected by high-voltage wires to high voltage source. High-voltage electrodes are connected to energy accumulator in the form of capacitors bank. A cavitation chamber is installed inside the housing, and the first high-voltage electrode is installed inside the cavitation chamber.

EFFECT: device provides for automated process of suspension preparation, increased efficiency of process, quality of obtained product and can be used for production of nanocapsules.

10 cl, 8 dwg

Description

The invention relates to the field of nanotechnology, medicine and food industry.

Previously known methods for producing microcapsules.

In patent No. 27313140, IPC A61K 009/50, A61K 009/127, Russian Federation, published 10.09.2001, a method is proposed for producing organosilicon micro lipid microcapsules using a rotary-cavitation unit with high shear forces and powerful sonar phenomena of the sound and ultrasonic range for dispersion .

The disadvantage of this method is the use of special equipment - rotary-cavitation installation, which has an ultrasonic effect, which affects the formation of microcapsules and can cause side reactions due to the fact that ultrasound has a destructive effect on protein-type polymers, therefore, the proposed method is applicable to work with polymers of synthetic origin

In pat. 2359662, IPC A61K 009/56, A61J 003/07, B01J 013/02, A23L 001/00, published on 06/27/2009, Russian Federation, proposed a method for producing sodium chloride microcapsules using spray cooling in a Niro spray cooling tower under the following conditions: temperature air inlet 10 ° C, the air temperature at the outlet 28 ° C, the speed of rotation of the spray drum 10,000 rpm / min. The microcapsules of the invention have improved stability and provide controlled and / or prolonged release of the active ingredient.

The disadvantages of the proposed method are the duration of the process and the use of special equipment, a set of certain conditions (inlet air temperature 10 ° C, air outlet temperature 28 ° C, the speed of rotation of the spray drum 10,000 rpm).

The known method proposed in US Pat. 2134967, IPC A01N 53/00, A01N 25/28, published 08/27/1999, Russian Federation (1999). A solution of a mixture of natural lipids and a pyrethroid insecticide is dispersed in water in a 2-4: 1 weight ratio in an organic solvent, which leads to a simplification of the method of microencapsulation.

The disadvantage of the method is dispersion in an aqueous medium, which makes the proposed method not applicable to the production of microcapsules of water-soluble drugs in water-soluble polymers.

The known method and device for producing nanocaplula vitamins according to the patent of the Russian Federation for invention No. 2557900, IPC A61K 3/375, publ. 07.27.2015, the prototype of the method and device.

This method of obtaining nanocapsules of vitamins in sodium alginate is characterized by the fact that sodium alginate is used as a shell, and vitamin is used as a core, the core: shell mass ratio is 1: 3, while the vitamin is added to a suspension of sodium alginate in benzene in the presence of the drug E472 with stirring, then add hexane, the resulting suspension is filtered and dried at room temperature,

This device contains a means of crushing and mixing the initial mixture and filter.

The disadvantage of the method and device: poor process performance.

Technical task: simplify and accelerate the process of obtaining nanocapsules, reducing losses in the preparation of nanocapsules (increase in mass yield).

The solution of these problems is achieved in the method of obtaining nanocapsules of vitamins in sodium alginate, characterized in that sodium alginate is used as a shell, and vitamin is used as a core, with a core: shell mass ratio of 1: 3, while the vitamin is added to sodium alginate suspension benzene in the presence of E472c with stirring, then hexane is added, the resulting suspension is filtered and dried at room temperature, characterized in that stirring is performed in a device containing an electro-hydraulic Ary emulsifier, and before filtering the mixture is cooled.

The solution of these problems is achieved in a device for producing nanocapsules of vitamins, containing a means of crushing and mixing the initial mixture and a filter, in that the means of crushing and mixing the mixture are made in the form of an electrohydraulic impact disperser, and a heat exchanger is installed between the electrostatic disperser and filter to reduce the temperature of the resulting product. filtment

Electro-hydraulic dispersant may contain a housing that forms a working chamber, partially filled with a mixture of liquids with the formation of air volume, at least one inlet and outlet pipes, and a mixing and emulsifying device, in that the mixing and emulsifying device is designed as two installed inside the working chamber high-voltage electrodes, the first high-voltage electrode is installed in a mixture of liquids, and the second - in the air volume, while the high-voltage electrodes are connected high ovoltnymi wires to high voltage source.

Both high-voltage electrodes can be connected to a capacitor bank. The body can be made of plastic. The housing can be made of metal, and both high-voltage electrodes are isolated from the capacitor, and the housing is grounded. A cavitation chamber can be installed inside the housing, and the first high-voltage electrode can be installed inside the cavitation chamber. The cavitation chamber can be made in the form of a perforated casing. Holes can be made tapering. Holes can be made expanding. Holes can be made in the form of Laval nozzles. A capacitor bank can be connected to both high voltage electrodes. The electrohydraulic emulsifier for liquids may contain a control unit and an operating mode controller connected by electrical connections. The electrohydraulic emulsifier for liquids may contain a control unit and a temperature sensor for a mixture of liquids connected by electrical connections. The electrohydraulic emulsifier for liquids may contain a control unit and a sensor for the level of a mixture of liquids connected by electrical communication. The electrohydraulic emulsifier for liquids may contain a control unit, and the supply pipes for liquids with pumps containing actuators, which are electrically connected to the control unit, are connected to the inlet nozzles.

The device may contain an outlet temperature sensor installed in front of the heat exchanger and a coolant flow regulator mounted at the inlet to the coil while the outlet temperature sensor and the coolant flow regulator are electrically connected to the control unit.

In the pipelines of the fluid supply can be installed flowmeters connected by electrical connections with the control unit. A drain pipe containing a drain valve can be connected to the outlet nozzle. The drain valve can be made controlled and connected to the control unit. A waste heat exchanger can be connected to the drain line. A convective heat exchanger can be connected to the drain line.

A distinctive feature of the proposed method is the production of nanocapsules by the non-solvent deposition method using hexane as a precipitant, and the use of sodium alginate as a shell of particles and vitamins as a core.

The result of the proposed method is to obtain nanocapsules of vitamins A, C, D, E Q ₁₀ , as well as extracts of Eleutherococcus and Ginseng.

The invention is illustrated in the drawings of FIG. 1 ... 8, where:

- in fig. 1 shows the installation,

- in fig. 2 shows a disperser with a plastic housing,

- in fig. 3 shows a disperser with a metal body,

- in fig. 4 shows a diagram of the device with the control output.

- in fig. 5 shows a vitamin nanocapsule,

- in fig. 6 shows the statistics of the distribution of nanocapsules by diameter for D ₀ = 10 nm,

- in fig. 7 shows the statistics of the distribution of nanocapsules by diameter for nanocapsules with a calculated diameter of D ₀ = 50 nm,

- in fig. 8 shows the statistics of the distribution of nanocapsules by diameter for nanocapsules with a calculated diameter of D ₀ = 100 nm,

Conventions used in the description:

1. dipergator

2. heat exchanger

3. filter

4. housing

5. working chamber

6. mixture

7. cover 7,

8. gasket 8,

9. the inlet pipe

10. the inlet pipe

11. the exhaust pipe

12. the first high-voltage electrode

13. the second high-voltage electrode

14. high-voltage wire,

15. high-voltage wire

16. energy storage

17. wires

18. high voltage source

19. source of energy.

20. metal hoop,

21. insulator.

22. insulator

23. cavitation chamber,

24. holes.

25. grounding

26. the output pipeline

27. connecting pipe

28. drain pipe,

29. the capacity of the drain,

30. pipeline recycling,

31. recirculation pump,

32. pump drive,

33. first capacity

34. second capacity

35. pipeline feed the first mixture

36. pump,

37. drive

38. flow meter

39. valve

40. pipeline feed the second mixture,

41. pump,

42. drive

43. flow meter

44. valve

45. control unit

46. electrical communications,

47. temperature sensor mixture of liquids

48. fluid level sensor,

49. electric discharge zone

50. liquid evaporation zone,

51. Serpentine

52. filter element

53. product

54. outlet temperature sensor,

55. cooler flow regulator,

56. vitamin nanocapluse,

57. core

58. shell.

A device for producing nanocapsules of vitamins (FIG. 1) contains a diper 1, a heat exchanger 2 connected to it, to the output of which a filter 3 is attached.

Dispersant 1 includes a housing 4, forming a working chamber 5, partially filled with mixture 6, a cover 7. A cover 7 is sealed with a gasket 8. At least two inlet pipes 9 and 10 and an exhaust pipe 11 are attached to the housing 4. The dispersant 1 includes a device for mixing and preparing a suspension, which is made in the form of two high-voltage electrodes 12 and 13 installed inside the working chamber, the first high-voltage electrode 12 being installed in the mixture 6, and the second 13 in the air volume of the working chamber 5, while the high-voltage Electrode 12 and 13 are connected by high-voltage cables 14 and 15 to 16 energy accumulator (capacitor bank) which is connected by wires 17 to a high voltage source 18 connected in turn to a power source 19.

Case 4 can be made of plastic, and the cover 7 metal (Fig. 1 and 2).

Concentric to the housing 4 is installed at least one annular band 20 for its amplification. Both high-voltage electrodes 12 and 13 are isolated from the capacitor 1 by insulators 21 and 22.

Inside the housing 4 mounted cavitation chamber 23, perforated holes 24.

Case 4 may be made of metal (Fig. 3), in this case it must be grounded by grounding 25.

A cavitation chamber 23 was applied to improve the mixing. In it, grinding of solid insoluble particles of vitamin and shell to the nanomolecular level takes place.

The first high-voltage electrode 12 can be installed inside the cavitation chamber 23. The cavitation chamber 23 can be made in the form of a cylinder with holes 24.

To the outlet of the device is connected to the outlet pipe 26, to which the inlet of the heat exchanger 2 is connected, to the outlet of which is connected a connecting pipe 27, the outlet of which is connected to the inlet of the filter 3, to the outlet of the filter 3 is connected a drain pipe 28.

Under the drain pipe 27 is placed a drain capacity of 29. In which a mixture of liquids is collected that form the basis of two suspensions: vitamin suspensions and shell suspensions.

In the capacity of the drain 29 entered the input of the recirculation pipe 30, containing the recirculation pump 31 with the pump drive 32.

The device contains two tanks: the first tank 33 for the suspension of the vitamin and the second tank 34 for the suspension of the shells.

The first tank 33 pipeline supplying the first mixture 35 containing the pump 36 with the actuator 37, the flow meter 38 and the valve 39 is connected to the first inlet 9.

The second tank supply line of the second mixture 40 containing the pump 41 with the actuator 42, the flow meter 43 and the valve 44 is connected to the second inlet 10.

The recirculation pipe 30 is connected to the first and second tanks 33 and 34.

Dispersant 1 can be equipped with a control unit 45 connected by electrical connections 46 with a high voltage source 18 for switching it on, off and adjusting the mode of electrical discharge.

Dispersant 1 may contain a temperature sensor dispersion 47, connected by electrical connections 46 with the control unit 45. Disperser 1 may contain a level sensor of the mixture of liquid 48, connected by electrical connection 46 with the control unit 45.

Dispersant 1 may contain an outlet temperature sensor (FIG. 2) connected by electrical connection 46 with a control unit 45 (FIG. 4). Besides

FIG. 1 shows the zone of electrical discharge 49 and the zone of intense evaporation of the liquid 50.

FIG. 4 shows a diagram of a device with an outlet temperature sensor 54 and a cooler 55 flow controller. The outlet temperature sensor 54 is installed in front of the heat exchanger 2 and the cooler 55 flow controller installed at the inlet to the coil 51 while the outlet temperature sensor 54 and the cooler 55 flow controller are connected electrical connections 46 with the control unit.

FIG. 5 shows a nanocaplula of vitamin 56, which contains the core 57 and the shell 58.

FIG. 6 shows the statistics of the distribution of nanocapsules 56 in diameter for D ₀ = 10 nm; FIG. 7 shows the statistics of the distribution of nanocapsules 56 by diameter for D ₀ = 50 nm; in FIG. 8 - statistics of the distribution of nanocapsules 56 by diameter for D ₀ = 100 nm.

EXAMPLE 1. Preparation of vitamin A nanocapsules in sodium alginate, core: shell ratio 1: 3 in the prototype unit.

100 mg of vitamin A is added to a suspension of sodium alginate in benzene containing the specified 300 mg of polymer in the presence of 0.01 g of E472c (an ester of glycerol with one or two edible fatty acid molecules and one or two citric acid molecules, and citric acid as tribasic, can be esterified by other glycerides and as oxoacid by other fatty acids. Free acid groups can be neutralized by sodium) with stirring at 1300 rev / sec. Next, pour 2 ml of hexane. The resulting suspension is filtered and dried at room temperature.

Received 3 kg g of nanocapsules powder. The yield was 99%. Processing time is 3 hours.

EXAMPLE 2. Obtaining nanocapsules of vitamin C in sodium alginate, the ratio of core: shell 1: 3. The treatment was performed in an electrohydro-disperser, cooling was applied in a heat exchanger.

100 g of vitamin C is added to a suspension of sodium alginate in benzene, containing the indicated 300 g of polymer in the presence of 10 kg of E472 s with 1300 rev / sec. Next, pour 2 liters of hexane. The resulting suspension is filtered and dried at room temperature.

Received 4 kg of nanocapsules powder. The yield was 100%. Processing time 2 hours.

EXAMPLE 3. Preparation of vitamin D nanocapsules in sodium alginate, core: shell ratio 1: 3. The treatment was performed in an electrohydro-disperser, cooling was applied in a heat exchanger.

100 mg of vitamin D is added to a suspension of sodium alginate in benzene, containing the indicated 300 g of polymer in the presence of 0.01 g of the preparation E472 with 1300 rev / sec under agitation. Next, pour 2 liters of hexane. The resulting suspension is filtered and dried at room temperature.

Received 4 kg of nanocapsules powder. The yield was 100%. Processing time - 1 hour.

Work with the device

Before carrying out the process of preparing a dispersion, tanks 33 and 34 are filled with liquids mixed with coarsely ground components for obtaining vitamin and shell.

Then the pumps 31 and 41 are turned on and the valves 39 and 44 are opened and the working chamber 23 is partially filled. The filling is monitored with the help of the fluid mix level sensor 47. The flow ratio of the mixed liquids is monitored with the help of flow meters 38 and 43. When the set level is reached, the pumps 36 and 41 are turned off, and valves 39 and 44 are closed.

Then turn on the high voltage source 18, the wires 17 recharge the energy store 16 and the high-voltage wires 14 and 15 serves the voltage simultaneously on both high-voltage electrodes 12 and 13.

Energy storage device 16 (capacitor bank) accumulates electricity and then a discharge occurs between high-voltage electrodes 12 and 13. As a result, on the basis of Yutkin's electrohydrodynamic effect, near the first electrode 12, an electrical discharge zone 49 and an evaporation zone 59 are formed (Fig. 1). The mixture of liquids flows out of the holes 24 of the cavitation chamber 23 at a very high speed and intensifies the mixing process in the working chamber 5. The process of preparing the emulsion occurs within a few seconds regardless of the volume of the working chamber 4. A small amount of energy is expended. This is due to the influence of two physical effects: the Yutkin effect, which causes the formation of plasma in the electric discharge zone 44 and the evaporation of liquid in the evaporation zone 44 at the place of discharge and cavitation, the propagation of a hydraulic shock with a pressure pulse of hundreds of thousand atm. in all directions and the phenomenon of cavitation - in the case of the use of cavitation chamber 23.

As a result, in the cavitation chamber 23, the initial components of the solid substances forming the core of the vitamin and the shell are ground to a nanoscale level and interconnected in the form of spheres.

The resulting suspension is filtered on the filter element 52 of the filter 2. The liquid is drained into the drain container 29 to return to the cycle.

Periodically, as the accumulation of the finished product 53, the operation of the device is stopped, the filter 3 is disassembled and the finished product 53 is separated from its filtering element 52.

The finished product 53 is dried at room temperature and packaged.

The use of the invention allowed:

1. Create an installation that provides an increase in its performance by 2 ... times.

2. To ensure the stability of the quality of nanocapsules.

3. To increase the efficiency of the installation and reduce the time of manufacture of the suspension.

4. Reduce power consumption.

5. To ensure ease of operation and safety of work due to the full automation of the process of preparing the suspension.

Claims (10)

1. A device for producing nanocapsules of vitamins, containing a means of crushing and mixing the mixture, inlet and outlet pipes, characterized in that the means of crushing and mixing the mixture is made in the form of an electrohydraulic impact dispersant, comprising a housing, inside which there is a working chamber having inlet pipes to which pipelines with pumps for supplying liquids are connected, two high-voltage electrodes are installed inside the working chamber, while high-voltage electrodes are connected by high-voltage wires to a high voltage source, both high-voltage electrodes are connected to a capacitor battery, and a heat exchanger is installed between the electrostatic disperser and filter, the device contains a control unit connected by electrical connections to a high-voltage source, the drives of the pumps are connected electrically to the control unit, the device contains a temperature sensor for the mixture of liquids , the level sensor of the mixture of liquids, flow meters are installed in the liquid supply pipelines, a sensor is installed in front of the heat exchanger output temperatures, with all sensors connected to the control unit by electrical connections, a coolant flow regulator is installed at the inlet to the coil, and a coolant flow regulator is installed at the inlet to the heat exchanger, while the coolant flow regulator is electrically connected to the control unit. 2. The device according to p. 1, characterized in that the casing is made of plastic. 3. The device according to claim 1, characterized in that the housing is made of metal, and both high-voltage electrodes are isolated from the housing and the housing is grounded. 4. The device according to claim 1, characterized in that a cavitation chamber is installed inside the case, and the first high-voltage electrode is installed inside the cavitation chamber. 5. The device according to p. 4, characterized in that the cavitation chamber is made in the form of a housing, perforated holes. 6. The device according to p. 5, characterized in that the holes are made tapering. 7. The device according to p. 5, characterized in that the holes are made expanding. 8. The device according to p. 5, characterized in that the holes are made in the form of Laval nozzles. 9. The device according to p. 1, characterized in that the outlet pipe is connected to the outlet pipe, containing a drain valve. 10. The device according to p. 9, characterized in that the drain valve is made controlled and connected to the control unit.

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