CN115779135A - Method and reaction device for preparing high-purity polyvinyl alcohol embolization microspheres with controllable particle size - Google Patents

Abstract

The invention relates to the technical field of medical materials, in particular to a method and a reaction device for preparing high-purity polyvinyl alcohol embolic microspheres with controllable particle size; the advantage of using microwave technology to prepare polyvinyl alcohol embolic microspheres in this application is that it is conducive to the preparation and formation of microspheres. Uniform suspension or emulsion, so that the particle size and particle size distribution of the microspheres can be effectively controlled; at the same time, the efficiency of the crosslinking reaction is improved; in addition, the phase stabilizer and other additives used in the preparation of the microspheres will be adsorbed on the microspheres In the pore size, the adsorption residue can be efficiently cleaned by microwave, so as to improve the purity of the product and ensure its safety.

Description

Method and reaction device for preparing high-purity polyvinyl alcohol embolization microspheres with controllable particle size

technical field

The invention relates to the technical field of medical materials, in particular to a method and a reaction device for preparing high-purity polyvinyl alcohol embolic microspheres with controllable particle size.

Background technique

Rising incidence of cancer has resulted in growing demand for various interventional oncology products and procedures. According to GLOBOCAN2018, there were 609,596 new liver cancer cases in Asia in 2018, and this number is expected to increase by 142,982 by 2025. Due to the advantages of minimally invasive surgery compared with traditional treatment procedures, such as less surgical complications, shorter hospital stay, less pain, smaller and more beautiful incisions, lower risk of infection, and faster recovery, the demand for minimally invasive surgery for tumor treatment has increased significantly. Embolic agents have also been rapidly developed, and various calibrated microspheres and bioglues made of natural and synthetic polymers have been developed as flow-directing embolic agents. Currently available commercial embolic materials, including different polymer-based particles and hydrogels, were developed for endovascular embolization therapy. Embolization microspheres have been widely used as a new type of particle embolization agent. The existing microspheres can be divided into polyvinyl alcohol microspheres, starch microspheres, albumin microspheres, gelatin microspheres, polylactic acid microspheres, Sodium alginate microspheres, chitosan microspheres and ethyl cellulose microspheres, etc. Polyvinyl alcohol embolic microspheres occupy a major position in the embolic agent market because of their safety, uniform particle size, strong compressibility and non-degradability.

At present, polyvinyl alcohol embolization microspheres are generally prepared by reverse-phase suspension polymerization process. The specific steps are: use linear polyvinyl alcohol or functionalized polyvinyl alcohol as the main chain molecule to dissolve in the water phase, and disperse in the non-polar polyvinyl alcohol. The solvent is used as the oil phase to form a uniformly mixed suspension or emulsion, and the polyvinyl alcohol hydrogel microspheres are obtained after cross-linking polymerization and solidification by the cross-linking agent (see Figure 1 for the preparation chemical reaction formula). This method has the following disadvantages: (1) the preparation process of the suspension or emulsion is complicated, and the process stability is poor; (2) the efficiency of cross-linking polymerization is low, which reduces the application efficiency of polyvinyl alcohol microspheres; (3) the preparation process requires The addition of phase stabilizers and other additives is not easy to be washed completely, and thus remains in the polyvinyl alcohol microspheres, resulting in a decrease in the purity of the product and a safety risk.

The heating principle of dielectric microwave heating is: when polar molecular dielectrics and nonpolar molecular dielectrics are placed in a microwave electromagnetic field, dipoles or existing dipoles will be rearranged in the dielectric material, and with the high-frequency alternating electromagnetic field Swinging at a speed of up to hundreds of millions of times per second, the molecules must overcome the interference and obstacles of the original thermal motion of the molecules and the interaction between the molecules if they want to rearrange with the direction of the changing high-frequency electric field, and produce friction similar to friction. The effect is to realize the "stirring" at the molecular level, thereby generating a large amount of heat. Thus it can be seen that conventional heating and microwave heating are two completely different heating methods; Series of unique advantages that traditional heating does not have. Compared with the contact heating method, the three-dimensional heating method using microwave can ensure the homogeneity and stability of the two-phase system. At the same time, microwave can accelerate the thermal movement of molecules, thereby improving the efficiency of olefin polymerization. Patent CN100381363C discloses a kind of iron salt and ferrous salt as raw materials, adopts microwave reactor in alkaline solution, and prepares iron ferric oxide nanocrystal by temperature control and air pressure. Patent CN101337695B discloses a method for rapidly preparing magnetic nano-microspheres in a non-aqueous solvent using iron salt as a raw material by using micro-powder technology. The microspheres prepared by this method have uniform particle size distribution and controllable particle size.

Most of the hydrogel microspheres are prepared by cross-linking and solidifying into balls by suspension polymerization process. In view of the insufficient degree of cross-linking of branched chains, hydrogel microspheres contain a small part of small molecular impurities that cannot form a three-dimensional cross-linked network structure; and the cleaning process of microspheres generally uses purified water or sodium chloride solution to boil for more than 30 minutes, repeated many times The process is extremely cumbersome and the cleaning effect is not ideal, resulting in the problem that the residue of starting materials will cause the purity of the product to decrease, so this solution is formulated.

Contents of the invention

The purpose of the present invention is to provide a method and a reaction device for preparing high-purity polyvinyl alcohol embolic microspheres with controllable particle size, more target products of three-dimensional cross-linked network structure of macromolecules, and use microwave technology to remove the target products wrapped in hydrogel Impurities in the microspheres are removed to obtain polymer hydrogel microspheres with a high-purity three-dimensional cross-linked network structure.

In order to solve the problems of the technologies described above, the present invention adopts the following technical solutions:

The invention provides a method and a reaction device for preparing high-purity polyvinyl alcohol embolic microspheres with controllable particle size, comprising the following steps:

S1: Dissolving polyvinyl alcohol: Add polyvinyl alcohol into the water phase kettle filled with purified water, turn on the stirring device of the water phase kettle, heat to 90-98°C and stir the solution to dissolve completely, and circulate the refrigerant into the interlayer of the kettle body to Cool the solution in the kettle to 20-30°C;

S2: Functionalization reaction: add N-acrylamide acetaldehyde dimethyl acetal to the water phase tank equipped with the solution of step S1, then add hydrochloric acid to adjust the pH value to 1-2, and stir for 1-6 hours. Add sodium hydroxide solution to the reaction kettle to adjust the pH value of the solution to neutrality;

S3: Preparation of aqueous phase solution: adding sodium 2-acrylamide-2-methylpropanesulfonate and potassium persulfate into the aqueous phase kettle containing the solution of step S2 in sequence, and stirring until completely dissolved;

S4: Oil phase solution preparation: Add butyl acetate and cellulose acetate butyrate into the oil phase kettle, stir until cellulose acetate butyrate is completely dissolved in butyl acetate, and heat to 50-70°C;

S5: Cross-linking balling reaction: transfer the water phase solution prepared in the water phase tank equipped with the solution of step S3 to the oil phase solution equipped with the prepared oil phase solution through a pneumatic device, and use the strong shear force of the stirring paddle to dissolve the water phase solution It forms a stable suspension with the oil phase solution. Add tetramethylethylenediamine to make the water phase undergo free radical polymerization, and at the same time start the intermittent microwave to maintain the temperature at 50-70°C, stir the reaction for 1-6 hours to make the water phase droplets solidify quickly, then turn off the microwave, and naturally cure for 1 ~6 hours, the curing reaction is complete. The reaction solution is discharged from the kettle body, and the microspheres in the kettle body are collected to obtain the crude product of polyvinyl alcohol hydrogel microspheres;

S6: Cleaning of the hydrogel microspheres: adding butyl acetate 1 to 5 times the volume of the microspheres, stirring and heating with microwave radiation, draining the liquid, and repeating the washing for 1 to 5 times. Add purified water 1 to 5 times the volume of the microspheres, stir and heat with microwave radiation, then drain the liquid, and then repeat the washing for 1 to 5 times. Finally, the water for injection was repeatedly washed for 1 to 5 times, and the obtained polyvinyl alcohol embolization microspheres were stored in normal saline. The high-purity polyvinyl alcohol embolic microspheres obtained by this process can be used not only as embolization agents but also as drug-carrying carriers of cationic drugs to obtain drug-machine-combined drug-loading embolic microspheres.

Preferably, the polyvinyl alcohol preferably has a 1,3-diol structure on the main chain of the embolization microspheres.

Preferably, the degree of polymerization of polyvinyl alcohol ranges from 1700 to 2400, and the degree of alcoholysis ranges from 50 to 99; preferably, the degree of polymerization is 1700 and the degree of hydrolysis is 88.

Preferably, the weight ratio of N-acrylamide acetaldehyde dimethyl acetal to polyvinyl alcohol is preferably 0.1-2:1;

The weight ratio of the sodium 2-acrylamide-2-methylpropanesulfonate to polyvinyl alcohol is preferably 0.1-2:1;

The weight ratio of potassium persulfate to polyvinyl alcohol is preferably 0.1-2:1.

Preferably, the weight ratio of cellulose acetate butyrate to butyl acetate is preferably 0.01-0.1:1.

Preferably, the weight ratio of tetramethylethylenediamine to polyvinyl alcohol is preferably 0.1-2:1.

Preferably, the microwave radiation frequency of the cross-linking curing reaction is 2000-3000 Hz, and the temperature is controlled at 50-90°C.

The present invention also provides a reaction device for preparing high-purity polyvinyl alcohol embolism microspheres, which includes a frame, a water phase kettle, an oil phase kettle, a semi-automatic control system, a controllable frequency conversion microwave device, a driving motor, a stirring component, a Drain line components;

The oil phase kettle is on the frame, including a kettle cover provided with a feed inlet, a kettle body, and a lower kettle cover provided with a filter screen;

The water phase kettle and the oil phase kettle are connected by pipelines, and the water phase kettle is transported to the oil phase solution through the power device;

The semi-automatic control system includes liquid inlet control, liquid discharge control, motor stirring control, microwave wavelength and start control.

Wherein the liquid inlet and outlet pipeline assembly includes a power delivery device. The power transmission device is non-electric power, including pneumatic power device or negative pressure power device and electromagnetic control switch.

Compared with the prior art, the beneficial technical effects of the present invention: the advantages of using microwave technology to prepare polyvinyl alcohol embolism microspheres in this application are: (1) it is beneficial to prepare and form a uniform suspension or emulsion, thereby effectively controlling microspheres. The particle size and particle size distribution of the ball; (2) Improve the efficiency of the crosslinking reaction; (3) The phase stabilizer and other additives used in the preparation of the microsphere will be adsorbed in the pore size of the microsphere, and the microwave energy can be efficiently Cleaning of the adsorption residue, thereby improving the purity of the product and ensuring its safety.

Description of drawings

The present invention will be further described below in conjunction with the accompanying drawings.

Fig. 1 is a schematic diagram of a reaction device for preparing high-purity polyvinyl alcohol embolic microspheres according to the present invention.

Detailed ways

This example discloses a method for preparing high-purity polyvinyl alcohol embolic microspheres with controllable particle size, which is characterized in that it includes the following steps:

S1: Dissolving polyvinyl alcohol

Add polyvinyl alcohol into the water phase kettle filled with purified water; turn on the built-in stirring mechanism of the water phase kettle, and heat the solution in the water phase kettle to 90-98°C at the same time, and stir the solution to dissolve; wait in the water phase kettle After the polyvinyl alcohol is completely dissolved, cool down the solution in the kettle to 20-30°C;

S2: Functionalization reaction

Add N-acrylamide acetaldehyde dimethyl acetal to the water phase tank equipped with the solution of step S1, then add hydrochloric acid to adjust the pH value of the solution in the tank to 1-2; then carry out stirring reaction for 1-6 hours, then Add sodium hydroxide solution to the water phase kettle to adjust its pH value to neutral;

S3: Preparation of aqueous phase solution

Add sodium 2-acrylamide-2-methylpropanesulfonate and potassium persulfate into the water phase kettle in step S2 in sequence, and stir until completely dissolved;

S4: Preparation of oil phase solution

Add butyl acetate and cellulose acetate butyrate to the oil phase kettle, and stir until the cellulose acetate butyrate is completely dissolved in butyl acetate, while heating to 50-70°C;

S5: Cross-linking sphere reaction

Transfer the prepared water phase solution in the water phase tank containing the solution of step S3 to the prepared oil phase solution through the conveying device, and use the strong shear force of the stirring paddle to form the water phase solution and the oil phase solution into a stable suspension . Add tetramethylethylenediamine to make the water phase undergo free radical polymerization, and start the intermittent microwave at the same time to maintain the temperature at 50-70°C, wait for 1-6 hours to make the water phase droplets solidify quickly, and then turn off the microwave generating device. Natural curing takes 1-6 hours to complete the curing reaction. The reaction solution is discharged from the kettle body, and the microspheres in the kettle body are collected to obtain the crude product of polyvinyl alcohol hydrogel microspheres;

S6: Washing of hydrogel microspheres

Add butyl acetate 1 to 5 times the volume of polyvinyl alcohol hydrogel microspheres, drain the liquid after stirring and heating with microwave radiation, and repeat the above cleaning for 1 to 5 times;

Add purified water of 1 to 5 times the volume of the microspheres, stir and heat with microwave radiation, drain the liquid, and repeat the above cleaning for 1 to 5 times;

Finally, the water for injection was repeatedly washed for 1 to 5 times, and the obtained polyvinyl alcohol embolization microspheres were stored in normal saline.

Wherein the polyvinyl alcohol includes 1,2-diol structure or 1,3-diol structure on the main chain of embolization microspheres.

The degree of polymerization of the polyvinyl alcohol ranges from 1700 to 2400, and the degree of alcoholysis ranges from 50 to 99.

The weight ratio of N-acrylamide acetaldehyde dimethyl acetal to polyvinyl alcohol is preferably 0.1-2:1; the weight ratio of 2-acrylamide-2-methylpropanesulfonate sodium to polyvinyl alcohol The ratio is preferably selected to be 0.1-2:1; the weight ratio of the potassium persulfate to polyvinyl alcohol is preferably selected to be 0.1-2:1.

In this embodiment, the weight ratio of the cellulose acetate butyrate to butyl acetate is preferably selected to be 0.01˜0.1:1.

The weight ratio of tetramethylethylenediamine to polyvinyl alcohol is preferably 0.1-2:1.

The microwave radiation frequency of the cross-linking curing reaction is 2000-3000 Hz, and the temperature is controlled at 50-90°C.

As shown in Figure 1, the present invention also discloses a reaction device for preparing high-purity polyvinyl alcohol embolism microspheres, which includes a water phase kettle and an oil phase kettle;

Wherein said water phase kettle is communicated with said oil phase kettle through a delivery pipeline, and a delivery pump is installed on the delivery pipeline, and the water phase kettle transports the water phase solution to the oil phase kettle through a power device; wherein in said Stirring components are respectively arranged in the water phase kettle and the oil phase kettle;

The water phase kettle transports raw materials through the liquid inlet pipeline assembly and the power unit, and a solenoid valve is installed on the liquid inlet pipeline; the oil phase kettle is installed in the microwave device through the frame, and most of the oil phase kettle is in the In the cavity of the microwave generator, raw materials are conveyed through the liquid inlet pipeline assembly and the power unit, and a solenoid valve is installed on the liquid inlet pipeline;

The above-mentioned electromagnetic valve, power unit, delivery pump, microwave unit, and stirring assembly are all regulated and controlled by the control system.

Specifically, the oil phase kettle is on the frame, which includes a kettle cover with a feed inlet, a kettle body, and a lower kettle cover with a filter screen.

Specifically, the power transmission device is non-electric power, which includes a pneumatic power device or a negative pressure power device and an electromagnetic control switch.

Implementation example 1

Polyvinyl alcohol dissolution: Add polyvinyl alcohol into the water phase kettle filled with purified water, start the stirring of the water phase kettle, heat up to 95°C, keep the temperature at 95°C and stir the solution to be completely transparent without visible solid particles.

Functionalization reaction: Cool the solution in the kettle to 25°C by introducing circulating refrigerant, add N-acrylamide acetaldehyde dimethyl acetal to the reaction device, then add hydrochloric acid to adjust the pH value to 1-2, and stir for 6 hours. Add sodium hydroxide solution to the reaction kettle to adjust the pH value of the solution to 6-8 to terminate the reaction.

Preparation of aqueous phase solution: Add sodium 2-acrylamide-2-methylpropanesulfonate and potassium persulfate into the aqueous phase kettle in sequence, and stir until completely dissolved.

Oil phase solution preparation: Add butyl acetate and cellulose acetate butyrate into the oil phase kettle, stir until the cellulose acetate butyrate is completely dissolved in butyl acetate, and heat to 55°C.

Cross-linking ball reaction: the water phase solution prepared in the water phase tank is transferred to the prepared oil phase solution through a pneumatic device, and the water phase solution and the oil phase solution are formed into a stable suspension by the strong shear force of the stirring paddle , reduce the stirring speed, the water phase has no coagulation and stratification. Add tetramethylethylenediamine to the oil phase kettle to make the water phase undergo free radical polymerization, and start the intermittent microwave at the same time to maintain the temperature at 55°C, stir the reaction for 6 hours to make the water phase droplets solidify quickly, then turn off the microwave, and naturally solidify After 1 hour, the curing reaction is complete. The reaction solution is discharged from the kettle body, and the microspheres in the kettle body are collected to obtain the crude polyvinyl alcohol hydrogel microspheres.

Cleaning of hydrogel microspheres: Add butyl acetate twice the volume of the microspheres, turn on the oil phase kettle to stir, start the microwave to radiate and heat the oil phase kettle solution for 3 minutes, then drain the liquid, and repeat the cleaning twice. Add purified water 5 times the volume of the microspheres, turn on the oil phase kettle to stir, start the microwave to radiate and heat the oil phase kettle solution for 3 minutes, then drain the liquid, and repeat the cleaning 2 times. Finally, the water for injection was repeatedly washed twice, and the obtained polyvinyl alcohol embolization microspheres were stored in normal saline.

Other examples of embolization microspheres

Implementation example 2

Water phase solution preparation: add gelatin to the water phase kettle filled with purified water, start the stirring of the water phase kettle, heat up to 70°C, keep the temperature at 70°C and stir the solution to be completely transparent without visible solid particles, and then pass in a refrigerant to cool down to 15°C ℃.

Preparation of oil phase solution: Add liquid paraffin and Span 80 into the oil phase kettle and stir evenly.

Cross-linking ball reaction: the water phase solution prepared in the water phase tank is transferred to the prepared oil phase solution through a pneumatic device, and the water phase solution and the oil phase solution are formed into a stable suspension by the strong shear force of the stirring paddle , reduce the stirring speed, the water phase has no coagulation and stratification. Add formaldehyde to the oil phase kettle to make the gelatin undergo cross-linking polymerization reaction. At the same time, start the intermittent microwave to maintain the temperature at 30 ° C. Stir the reaction for 1 hour to make the water phase droplets solidify quickly, then turn off the microwave and let it naturally cure for 1 hour. The curing reaction is complete. . The reaction solution is discharged from the kettle body, and the microspheres in the kettle body are collected to obtain the crude product of gelatin sponge hydrogel microspheres.

Hydrogel microsphere cleaning: add 2% Span 80 aqueous solution 5 times the volume of the microspheres, turn on the oil phase kettle to stir, start the microwave to radiate and heat the oil phase kettle solution for 3 minutes, then drain the liquid, and repeat the cleaning twice. Add purified water 5 times the volume of the microspheres, turn on the oil phase kettle to stir, start the microwave to radiate and heat the oil phase kettle solution for 3 minutes, then drain the liquid, and wash twice. Finally, the gelatin sponge embolization microspheres were obtained after repeated washing twice with water for injection and drying.

Chemical Reaction Formula for Preparation of Polyvinyl Alcohol Microspheres

In describing the present invention, it is to be understood that the terms "vertical", "transverse", "upper", "lower", "front", "rear", "left", "right", "vertical" , "horizontal", "top", "bottom", "inner", "outer" and other indicated orientations or positional relationships are based on the orientations or positional relationships shown in the drawings, and are only for the convenience of describing the present invention, rather than indicating Or imply that the device or element referred to must have a specific orientation, be constructed and operate in a specific orientation, and therefore should not be construed as limiting the invention.

The above embodiments are only descriptions of the preferred modes of the present invention, and are not intended to limit the scope of the present invention. Without departing from the design spirit of the present invention, those skilled in the art may make various modifications and changes to the technical solutions of the present invention. Improvements should all fall within the scope of protection determined by the claims of the present invention.

Claims (10)

1. The method for preparing the particle size controllable high-purity polyvinyl alcohol embolism microsphere is characterized by comprising the following steps: the method comprises the following steps:

s1: dissolving polyvinyl alcohol

Adding polyvinyl alcohol into a water phase kettle containing purified water; starting a built-in stirring device of the water phase kettle, heating the solution in the water phase kettle to 90-98 ℃, and stirring the solution to dissolve; after polyvinyl alcohol in the water phase kettle is completely dissolved, cooling the solution in the kettle to 20-30 ℃;

s2: functionalization reactions

Adding N-acrylamide acetaldehyde dimethyl acetal into the water phase kettle filled with the solution in the step S1, and then adding hydrochloric acid to adjust the pH value of the solution in the kettle to 1-2; then stirring and reacting for 1-6 hours, and then adding a sodium hydroxide solution into the water phase kettle to adjust the pH value of the water phase kettle to be neutral;

s3: preparation of aqueous solution

Sequentially adding 2-acrylamide-2-methylpropanesulfonic acid sodium salt and potassium persulfate into the water phase kettle filled with the solution obtained in the step S2, and stirring until the sodium 2-acrylamide-2-methylpropanesulfonate and the potassium persulfate are completely dissolved;

s4: preparation of oil phase solution

Adding butyl acetate and cellulose acetate butyrate into an oil phase kettle, stirring until the cellulose acetate butyrate is completely dissolved in the butyl acetate, and simultaneously heating to 50-70 ℃;

s5: crosslinking into balls

And (4) transferring the water phase solution prepared in the water phase kettle in the step (S3) into the oil phase solution with the prepared oil phase solution through a conveying device, and forming stable suspension by using the strong shearing force of a stirring paddle. Adding tetramethylethylenediamine to enable the water phase to generate free radical polymerization reaction, starting intermittent microwave to maintain the temperature at 50-90 ℃, enabling the water phase droplets to be rapidly crosslinked and cured after stirring for 1-6 hours, then closing a microwave generating device, and naturally curing for 1-6 hours to complete the curing reaction. Discharging the reaction liquid out of the kettle body, and collecting microspheres in the kettle body to obtain a crude product of the polyvinyl alcohol hydrogel microspheres; s6: hydrogel microsphere cleaning

Adding 1-5 times of butyl acetate in the volume of the polyvinyl alcohol hydrogel microspheres, stirring, heating by microwave radiation, discharging liquid, and repeating the cleaning for 1-5 times;

adding purified water with the volume of 1-5 times that of the microspheres, stirring, heating by microwave radiation, draining the liquid, and repeatedly cleaning for 1-5 times;

and finally, repeatedly washing the mixture for 1 to 5 times by using water for injection to obtain the polyvinyl alcohol embolism microsphere and storing the polyvinyl alcohol embolism microsphere in physiological saline.

2. The method for preparing high-purity polyvinyl alcohol embolization microspheres with controllable particle size according to claim 1, wherein: the polyvinyl alcohol comprises a plug microsphere backbone with 1,2-diol structure or 1,3-diol structure.

3. The method for preparing high-purity polyvinyl alcohol embolization microspheres with controllable particle size according to claim 1, wherein: the polymerization degree of the polyvinyl alcohol is 1700-2400, and the alcoholysis degree is 50-99.

4. The method for preparing high-purity polyvinyl alcohol embolization microspheres with controllable particle size according to claim 1, wherein: the weight ratio of the N-acrylamide acetaldehyde dimethyl acetal to the polyvinyl alcohol is preferably 0.1-2: 1;

the weight ratio of the 2-acrylamide-2-methyl sodium propane sulfonate to the polyvinyl alcohol is preferably 0.1-2: 1;

the weight ratio of the potassium persulfate to the polyvinyl alcohol is preferably 0.1-2: 1.

5. the method for preparing high-purity polyvinyl alcohol embolization microspheres with controllable particle size according to claim 1, wherein: the weight ratio of the cellulose acetate butyrate to the butyl acetate is preferably 0.01-0.1: 1.

6. the method for preparing high-purity polyvinyl alcohol embolization microspheres with controllable particle size according to claim 1, wherein: the weight ratio of the tetramethylethylenediamine to the polyvinyl alcohol is preferably 0.1-2: 1.

7. the method and the reaction device for preparing the particle size controllable high-purity polyvinyl alcohol embolism microsphere according to claim 1 are characterized in that: the microwave radiation frequency of the crosslinking curing reaction is 2000-3000 Hz, wherein the temperature is controlled at 50-70 ℃.

8. A reaction device for preparing high-purity polyvinyl alcohol embolism microsphere according to any one of claims 1-7, which is characterized in that: comprises a water phase kettle and an oil phase kettle;

the water phase kettle is communicated with the oil phase kettle through a conveying pipeline, a conveying pump is arranged on the conveying pipeline, and the water phase kettle conveys water phase solution to the oil phase kettle through a power device; wherein stirring components are respectively arranged in the water phase kettle and the oil phase kettle;

the water phase kettle conveys raw materials through a liquid inlet pipeline assembly and a power device, and an electromagnetic valve is arranged on the liquid inlet pipeline;

the oil phase kettle is arranged in the microwave device through the rack, and conveys raw materials through the liquid inlet pipeline assembly and the power device, and the liquid inlet pipeline is provided with an electromagnetic valve;

the electromagnetic valve, the power device, the delivery pump, the microwave device and the stirring assembly are all regulated and controlled by the control system.

9. The reaction device for preparing the high-purity polyvinyl alcohol embolism microsphere according to claim 8, wherein: the oil phase kettle is arranged on the rack and comprises a kettle cover provided with a feed inlet, a kettle body and a lower kettle cover provided with a filter screen.

10. The reaction device for preparing the high-purity polyvinyl alcohol embolic microspheres according to claim 8, wherein: the power transmission device is non-electric power and comprises a pneumatic power device or a negative pressure power device and an electromagnetic control switch.

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