CN110975677A

CN110975677A - Polylactic acid microsphere emulsifying machine with uniform dispersion

Info

Publication number: CN110975677A
Application number: CN201911092297.8A
Authority: CN
Inventors: 李倩倩; 吴景梅; 葛晓蝶; 赵勇; 杜明肖; 陈叶生
Original assignee: Bengbu College
Current assignee: Bengbu College
Priority date: 2019-11-11
Filing date: 2019-11-11
Publication date: 2020-04-10

Abstract

The invention discloses a polylactic acid microsphere emulsifying machine with uniform dispersion degree, and mainly relates to the field of microsphere emulsifying machines. The shell comprises an upper shell and a lower shell which are arranged up and down, wherein the upper shell is a cylindrical shell, and the lower shell is an inverted conical shell; a coaxial high-speed rotating shaft is arranged in the upper shell, and the rotating speed of the high-speed rotating shaft is 600-1200 r/min; the lower shell is internally provided with a coaxial uniform-speed rotating shaft, and the rotating speed of the uniform-speed rotating shaft is 400-800 r/min. The invention has the beneficial effects that: it is easy to form flocculation flow, and obtain different shearing force, avoid dispersed phase adhesion, and is favorable to obtain smaller microsphere grain size.

Description

Polylactic acid microsphere emulsifying machine with uniform dispersion

Technical Field

The invention relates to a microsphere emulsifying machine, in particular to a polylactic acid microsphere emulsifying machine with uniform dispersity.

Background

Polylactic acid microspheres, which means that polylactic acid exists in the form of microspheres. Is generally used as a drug carrier. The biodegradable polymer microsphere is used as a novel drug carrier and has wide research and application in the field of drug controlled release. The microsphere carrier can overcome some defects of the existing medicinal preparation, and has the advantages of controlling the release speed of the medicament to achieve long-acting slow release, increasing the targeting property of the medicament, reducing toxic and side effects, improving curative effect and the like.

The current definition of microspheres in pharmaceutics refers to micro-spherical entities, spherical or sphere-like, formed by dissolving or dispersing drugs in high molecular materials, which are generally prepared into suspensions for injection or oral administration. The particle size range of the microspheres is generally 1-500 um, the small particle can be several nanometers, the large particle can reach 800um, the particle size is smaller than 500nm, the microspheres are also commonly called nanospheres or nanoparticles, and the microspheres belong to the category of colloids.

Micronized formulations of drugs can be prepared by different methods depending on the nature of the drug and the requirements of the formulation. Mainly includes emulsion solvent evaporation method, spray drying method, phase separation method and melting method. The present invention is designed based mainly on the first main method of the emulsion solvent evaporation method.

The method is that two phases which are not miscible are made into emulsion by mechanical stirring or ultrasonic emulsification, the inner phase solvent is volatilized and removed, the balling material is separated out and solidified into microspheres. The solvent of the inner dispersed phase must have some solubility and volatility in the outer continuous phase. Under slow stirring, the inner dispersed phase solvent continuously diffuses to the outer phase, transports to the liquid surface and volatilizes into the air. The extraction-volatilization-extraction process is repeated, so that the carrier material in the inner dispersed phase is separated out to form a capsule membrane, and the drug is wrapped in the capsule membrane until the microspheres are completely solidified. The preparation method can be divided into oil-in-water type O/W, oil-in-oil type O/O, and water/oil/water double emulsion type W/O/W according to the type of emulsion. The O/W type is designed by dissolving polylactic acid in organic phase, adding into water phase containing emulsifier to form O/W type emulsion, and making into medicine. The W/O/W type is prepared through dissolving medicine in inner water phase, adding organic phase to emulsify to form W/O colostrum, adding colostrum to outer water phase to form W/O/W emulsion and volatilizing organic solvent in the middle layer to form cured microsphere.

The device for emulsifying is an emulsifying machine which is mainly used for producing microemulsion and superfine suspension. The materials move at high speed in the narrow gaps of the reactor and the stirring blades and are sheared by stronger hydraulic force, so that the effects of emulsification, emulsification and crushing are achieved. The distribution range of the grain diameter of the material, the homogenizing and refining effects and the yield are determined by the material to be processed, the physical properties, the number of the working cavities and the residence time of the material in the working cavities.

The requirement on the shearing force in the emulsification is complex, so that the stirring time is generally longer, and the strength is higher. The requirement on the motor and equipment is high due to long-time operation at high rotating speed. Meanwhile, the same shearing force is not beneficial to dispersion and emulsification, so the emulsification effect of the prior common emulsifying machine is not ideal.

Disclosure of Invention

The invention aims to provide a polylactic acid microsphere emulsifying machine with uniform dispersion, which is easy to form flocculation flow, obtains different shearing force, avoids dispersed phase adhesion and is beneficial to obtaining smaller microsphere particle size.

In order to achieve the purpose, the invention is realized by the following technical scheme:

a polylactic acid microsphere emulsifying machine with uniform dispersion degree comprises a machine shell, wherein the machine shell comprises an upper shell and a lower shell which are arranged up and down, the upper shell is a cylindrical shell, and the lower shell is an inverted conical shell;

a coaxial high-speed rotating shaft is arranged in the upper shell, and the rotating speed of the high-speed rotating shaft is 600-1200 r/min;

the lower shell is internally provided with a coaxial uniform-speed rotating shaft, and the rotating speed of the uniform-speed rotating shaft is 400-800 r/min.

Preferably, the bottom of the uniform-speed rotating shaft is provided with a stirring rod, the stirring rod extends horizontally, the number of the stirring rods is 2-4, the stirring rods surround the uniform-speed rotating shaft in an annular array, the upper portion of each stirring rod is provided with vertically extending upper comb teeth, and the lower portion of each stirring rod is provided with 2-4 rows of lower comb teeth.

Preferably, the top end of the high-speed rotating shaft is provided with a high-speed stirring part, and the high-speed stirring part is of a paddle type stirring structure.

Preferably, the high-speed stirring part comprises 3 stirring blades which are annularly arrayed at the top end of the high-speed rotating shaft, and the stirring blades are blades with inclined surfaces.

Preferably, the specific application is as follows:

the high-speed rotating shaft and the uniform-speed rotating shaft are alternately started;

or

And the high-speed rotating shaft and the uniform-speed rotating shaft are alternatively started.

Preferably, the inner walls of the upper shell and the lower shell are made of 316L or 316Ti stainless steel.

Preferably, an installation plate is arranged in the middle of the end face of the top end of the upper shell, an upper bearing seat is arranged on the installation plate, the uniform-speed rotating shaft is installed in the upper bearing seat through a sealing bearing, and windows for feeding are arranged on two sides of the installation plate;

the bottom end face of the lower shell is of a closed structure and is provided with a lower bearing seat, and the high-speed rotating shaft is installed in the lower bearing seat through a sealing bearing.

Compared with the prior art, the invention has the beneficial effects that:

the continuous shearing machine can continuously run for a long time, has large treatment capacity, more stable operation and more convenient disassembly and assembly, is suitable for industrial online continuous production, has narrow particle size distribution range and good dispersion effect, has no dead angle, and cuts 100 percent of materials through dispersion.

The upper stirring component and the lower stirring component work alternately, so that the flocculation flow is easy to form, different shearing forces are obtained, the adhesion of dispersed phases is avoided, the liquid drops are finer, the particle size distribution is narrower, and the stability of the generated mixed liquid is better. The rotating speed is adjustable, the upper stirring structure and the lower stirring structure can be used together or independently, and the device is suitable for different processes.

Drawings

FIG. 1 is a schematic diagram of the present invention.

Fig. 2 is a schematic view of the internal structure of the present invention.

FIG. 3 is a schematic diagram of the stirring structure of the present invention.

Figure 4 is a schematic of the present invention.

Figure 5 is a schematic of the present invention.

Reference numerals shown in the drawings:

1. an upper housing; 2. a lower housing; 3. a high-speed rotating shaft; 4. stirring blades; 5. mounting a plate; 6. a uniform speed rotating shaft; 7. a stirring rod; 8. comb teeth are arranged; 9. and (4) lower comb teeth.

Detailed Description

The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and these equivalents also fall within the scope of the present application.

The instruments, reagents, materials and the like used in the following examples are conventional instruments, reagents, materials and the like in the prior art and are commercially available in a normal manner unless otherwise specified. Unless otherwise specified, the experimental methods, detection methods, and the like described in the following examples are conventional experimental methods, detection methods, and the like in the prior art.

Example (b): polylactic acid microsphere emulsifying machine with uniform dispersion

In the process of emulsification balling, the two phases at the initial stage need to be sheared at a high speed to ensure that the organic phase is dispersed into small balls to form emulsion. The shear force required is high. When a time axis is fixed, the improvement of the stirring speed can increase the shearing force of an emulsion system only by a certain emulsification node, so that the dispersion effect of a dispersion phase in a continuous phase is improved. The oil phase has small emulsion drop, good balling and small particle size.

After the time factor is taken into consideration, as the time required for stirring is very long, generally speaking, the longer the stirring time is, the better the microsphere is formed (certainly, after the time is longer than a certain time, generally 3.5 hours, the effect is not obviously increased), but under the same shearing force, the dispersion speed of the microsphere in the dispersant is reduced, the larger the microsphere particle size is, the less dispersion is caused under the same shearing force, and the adhesion occurs, so that the microsphere is not easily formed.

Therefore, the control of the shearing force under mechanical stirring can not meet the requirements of long-time operation and interval adjustment of the shearing force in the conventional emulsifying machine, thereby causing the common problems of poor emulsifying effect and unsatisfactory balling.

The product is an emulsifying machine, is mainly used for an emulsifying process in the preparation of polylactic acid microspheres in a multi-stirring mode, and has the following specific structure:

the machine shell comprises an upper cylindrical shell 1 in the upper half part and a lower conical shell 2 in the lower half part, wherein the bottom end of the lower shell 2 is tightened.

The bottom of the lower shell 2 is of a sealed and closed structure, a bearing seat is installed on the end face of the bottom end of the lower shell 2, a high-speed rotating shaft 3 is installed in the bearing seat through a sealed bearing, the high-speed rotating shaft 3 is driven by a motor, the rotating speed is 600-flour-plus-oil-plus-1200 r/min, and the rotating speed of the motor can be set according to reflected materials. The high-speed rotating shaft 3 is coaxial with the lower shell 2. The top of high-speed pivot 3 is equipped with the high-speed stirring portion, the high-speed stirring portion is constituteed through stirring leaf 4 of three annular array, stirring leaf 4 is the platelike structure that the slope set up, and the lower casing 2 shape of cooperation back taper is favorable to forming stronger vortex and shearing force in the high-speed stirring, makes the material receive comprehensive action such as stronger hydraulic shear, centrifugal extrusion, high-speed cutting, striking and grinding to reach emulsification, broken effect.

The top of the upper shell 1 is provided with a mounting plate 5, the mounting plate 5 is centered on the axis of the upper shell 1, the mounting plate 5 is provided with a uniform-speed rotating shaft 6 which is coaxial with the upper shell 1, the uniform-speed rotating shaft 6 is driven by a motor, the rotating speed is 400 plus materials at 800r/min, and the rotating speed of the motor can be set according to the reflected materials. And feeding windows are arranged on two sides of the mounting plate 5.

Be equipped with puddler 7 on the pivot of samming 6, the bottom symmetry setting of the relative pivot of samming 6 of puddler 7, the top side of puddler 7 is equipped with one row of broach 8 of going up, the downside of puddler 7 is equipped with symmetry downwardly extending's lower broach 9, and two lower broach 9 and last broach 8 form the triangle-shaped and distribute in the side. When the uniform-speed rotating shaft 6 rotates, because the upper shell 1 is cylindrical and the stirring component is in the structure as shown in the above and the attached drawings, a soft shearing force is easily formed, and the structure of the stirring part expands to most of the chambers of the upper shell 1, so that the effect of integrally dispersing and stirring the solution is better. Wherein, go up broach 8 and be the rotation of one row of cooperation puddler 7 to the stirring efficiency of solution, compare that broach 9 is the rotation of two rows of cooperation puddlers 7 is different to the stirring efficiency of solution, easily obtain the difference to solution upper portion lower part shearing force, easily form the turbulent flow, increase balling-up effect.

This emulsion machine establishes the great puddler 7 that has the broach extension of structure in through columniform last casing 1 to the even speed stirring of relative low establishes compact structure small and exquisite in conical casing 2 down, and the high-speed stirring portion of relative stirring speed obtains two kinds of stirring effects that are distinct respectively: the effect 1) the stirring of high-speed stirring portion easily obtains vortex and high shear force, strengthens comprehensive actions such as hydraulic shearing, centrifugal extrusion, high-speed cutting, striking and grinding of material, and the effect 2) the comprehensive stirring effect of puddler 7 combination broach. When the stirring device is applied, the high-speed rotating shaft 3 and the uniform-speed rotating shaft 6 are alternately started to obtain the alternate action of two stirring effects, so that the flocculation flow is particularly easy to form, different shearing forces are obtained, the dispersed phase is prevented from being adhered, and the smaller particle size of the microspheres is favorably obtained.

Meanwhile, the high-speed stirring part is small and compact in structure, is beneficial to long-time high-speed rotation, is combined with the alternative up-and-down stirring, is more beneficial to realizing long-time continuous operation, and solves the defect that the common emulsifying machine is short in operation time.

The advantages of the present device are specifically set out below:

1) the continuous shearing machine can continuously run for a long time, has large treatment capacity, more stable operation and more convenient disassembly and assembly, is suitable for industrial online continuous production, has narrow particle size distribution range and good dispersion effect, has no dead angle, and cuts 100 percent of materials through dispersion.

2) The upper stirring component and the lower stirring component work alternately, so that the liquid drops are finer and finer, the particle size distribution is narrower, and the stability of the generated mixed liquid is better.

3) The rotating speed is adjustable, the upper stirring structure and the lower stirring structure can be used together or independently, and the device is suitable for different processes.

Claims

1. The polylactic acid microsphere emulsifying machine with uniform dispersity is characterized by comprising a machine shell, wherein the machine shell comprises an upper shell and a lower shell which are arranged up and down, the upper shell is a cylindrical shell, and the lower shell is an inverted conical shell;

2. The polylactic acid microsphere emulsifying machine with uniform dispersion degree according to claim 1, wherein the bottom end of the uniform speed rotating shaft is provided with a stirring rod, the stirring rod extends horizontally, the number of the stirring rods is 2-4, the stirring rods surround the uniform speed rotating shaft in an annular array, the upper part of the stirring rod is provided with vertically extending upper comb teeth, and the lower part of the stirring rod is provided with 2-4 rows of lower comb teeth.

3. The polylactic acid microsphere emulsifying machine with uniform dispersion degree according to claim 1, wherein the top end of the high-speed rotating shaft is provided with a high-speed stirring part, and the high-speed stirring part is of a paddle type stirring structure.

4. The emulsification machine of claim 3, wherein the high-speed stirring part comprises 3 stirring blades annularly arrayed at the top end of the high-speed rotating shaft, and the stirring blades are blades with inclined surfaces.

5. The polylactic acid microsphere emulsifying machine with uniform dispersion degree according to claim 1, which is characterized in that when in specific application:

or

6. The polylactic acid microsphere emulsifying machine with uniform dispersion degree according to claim 1, wherein the inner walls of the upper shell and the lower shell are made of 316L or 316Ti stainless steel.

7. The polylactic acid microsphere emulsifying machine with uniform dispersion degree according to claim 1, wherein a mounting plate is arranged in the middle of the top end surface of the upper shell, an upper bearing seat is arranged on the mounting plate, the uniform-speed rotating shaft is arranged in the upper bearing seat through a sealing bearing, and windows for feeding materials are arranged on two sides of the mounting plate;