CN113088104B - Process for preparing high-dispersion homogeneous nano silicon dioxide spheres - Google Patents
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Abstract
The invention discloses a process for preparing high-dispersion homogeneous nano silicon dioxide spheres, which comprises the following steps: adding a silica sol aqueous solution, a silane coupling agent and toluene as initial raw materials into a reaction furnace, stirring and reacting at 90-110 ℃ to obtain a silica particle intermediate solution, and performing high-frequency resonance on the silica particle intermediate solution by using an ultrasonic oscillation device to form micron-sized fog drops. And introducing the fog drops into a reaction furnace through a conveying pipeline, and reacting in the reaction furnace to obtain the high-dispersion homogeneous nano silicon dioxide ball solution. And (3) allowing the nanometer-scale fog drops formed by high-frequency resonance of the silicon dioxide sphere solution by adopting a nanometer-scale ultrasonic generator to enter a centrifugal machine through a nanometer-scale filter membrane, and separating and dehydrating by using the centrifugal machine at the temperature of 50-95 ℃ to obtain the high-dispersion homogeneous nano silicon dioxide spheres. The silicon dioxide spheres are used as the silicon-based nano material, so that the advantages of controllable gradual release of the medicine, long effective period and good uniformity can be better utilized.
Description
Technical Field
The invention relates to the technical field of silicon dioxide ball preparation, in particular to a process for preparing high-dispersion homogeneous nano silicon dioxide balls.
Background
Two kinds of crystalline silica and amorphous silica exist in nature, and the crystalline silica is divided into quartz, tridymite and cristobalite due to different crystal structures. Pure quartz is colorless crystal, and large and transparent prism-shaped quartz is called crystal. If the crystal containing a small amount of impurities has different colors, purple crystal, tea crystal and the like exist. Common sand is fine quartz crystal, diatomite existing in nature is amorphous silicon dioxide, remains of diatom of lower aquatic plants are white solid or powder, and is porous, light, soft and solid, and strong in adsorbability.
At present, interventional therapy is minimally invasive therapy carried out by utilizing modern high-tech means, and the specific method is to introduce special catheters, guide wires and other precise instruments into a human body under the guidance of medical imaging equipment to diagnose and locally treat internal diseases. Has the characteristics of no operation, small wound, quick recovery and good effect, and is a development trend of medical science. In the tube intervention operation, an embolizing agent is needed to embolize abnormal tumor blood vessels, rupture bleeding arteries or excessively enlarge abnormal organs so as to achieve the treatment purposes of killing tumors, saving lives or recovering the normal functions of the organs. The tumor interventional minimally invasive therapy is also named as minimally invasive interventional therapy, the therapy has small wound, and the skin incision is only about 2 mm; the targeting property is strong, can be directly acted on the tumor with targeting, and has small damage to normal tissues; the recovery is fast, the normal activity can be realized within 12 hours after the operation, and the patient can be discharged after 5 to 7 days; the repeatability is strong, and the medicine can be repeatedly implemented in stages and for multiple times according to the condition of illness and the treatment requirement; the method can be applied in combination with various technologies, for example, for primary liver cancer, hepatic artery embolism is firstly adopted to close tumor vessels to the maximum extent, then the argon-helium ultralow temperature freezing technology is adopted to reduce the tumor volume and reduce the tumor load in a short time, and finally the immunobiotherapy is applied in order, so that the ideal effects of fusion of modern medicine and high and new technology, synergy and superposition of therapy and complementary advantages are achieved.
Embolization, also known as embolization, is the controlled injection of an embolization material into the supply vessel of a diseased organ via an arterial or intravenous catheter to occlude the vessel and interrupt the blood supply in order to control bleeding, treat tumors and vascular lesions and eliminate the function of the diseased organ. Embolization is an important technique in interventional therapy and is one of the three main techniques in interventional radiology, and microspheres are the main type of embolization particles. At present, the embolization particles mainly have four types, including microspheres, particles, DEB and radioactive embolization microspheres, but the drug-loaded microspheres in the prior art have uncontrollable drug release process and poor material uniformity, and the products mainly come from imports and are high in price and difficult to achieve expected effects.
Disclosure of Invention
The invention overcomes the defects of the prior art and provides a process for preparing high-dispersion homogeneous nano silicon dioxide spheres.
In order to achieve the purpose, the invention adopts the technical scheme that: a process for preparing high-dispersion homogeneous nano silicon dioxide spheres comprises the following steps:
step S1: adding a silica sol aqueous solution, a silane coupling agent and toluene as initial raw materials into a reaction furnace, stirring and reacting at 90-110 ℃ to obtain a silica particle intermediate solution, and performing high-frequency resonance on the silica particle intermediate solution by using an ultrasonic oscillation device to form micron-sized fog drops.
Step S2: and introducing the fog drops into a reaction furnace through a conveying pipeline, introducing inert gas containing nitrogen into the reaction furnace, simultaneously adding a dimethylformamide mixed solvent into the reaction furnace, and reacting the fog drops containing silicon dioxide particles in the dimethylformamide solvent to obtain a silicon dioxide ball solution.
And step S3: and (3) allowing the nanometer-scale fog drops formed by high-frequency resonance of the silicon dioxide sphere solution by adopting a nanometer-scale ultrasonic generator to enter a centrifugal machine through a nanometer-scale filter membrane, and separating and dehydrating by using the centrifugal machine at the temperature of 50-95 ℃ to obtain the high-dispersion homogeneous nano silicon dioxide spheres.
In a preferred embodiment of the present invention, the initial raw materials in step S1 include: 55-80 parts of silica sol aqueous solution, 60-95 parts of silane coupling agent and 15-30 parts of toluene.
In a preferred embodiment of the present invention, the nano-scale filtration membrane has nano-pores with a diameter in the range of 50-80 nm uniformly distributed thereon.
In a preferred embodiment of the present invention, the mixed solvent of dimethylformamide in step S2 includes: copolymers with alkynyl groups at non-terminal ends of the molecular chain.
In a preferred embodiment of the present invention, the copolymer with alkynyl on the non-terminal group of the molecular chain is prepared by reacting maleic anhydride, toluene solvent, nitrogen, propiolic alcohol, tetrahydrofuran and initiator at 80 ℃.
In a preferred embodiment of the present invention, the initiator is selected from one or more of benzoyl peroxide tert-butyl ester, azobisisobutyronitrile and benzoyl peroxide.
In a preferred embodiment of the present invention, the inert gas comprises: helium, krypton, and argon.
In a preferred embodiment of the present invention, the concentration of the nitrogen in the inert gas is controlled to be between 60% and 80%.
In a preferred embodiment of the invention, in the step S3, the temperature is increased in a stepwise manner from 50-55 ℃ to 90-95 ℃ during the separation and dehydration process of the centrifuge; when the nano-scale droplets are completely dehydrated, slowly cooling the nano-scale droplets to 15-20 ℃ in a stepwise manner from 90-95 ℃.
In a preferred embodiment of the present invention, the nanofiltration membrane has a certain ductility, and is made of seaweed gel.
The invention solves the defects in the background technology, and has the following beneficial effects:
(1) The nanometer fog drops enter the centrifuge for separation and dehydration through the nanometer filtering membrane, the diameter of the silicon dioxide spherulites in the nanometer fog drops can be effectively controlled, the nanometer fog drops are dehydrated in the centrifuge to form high-dispersion homogeneous silicon dioxide spherulites, and on the other hand, the diameter of the silicon dioxide spherulites can be further controlled by uniformly arranging nanometer micropores with the diameter within the range of 50-80 nanometers on the filtering membrane, so that the high-dispersion homogeneous effect of the preparation process is improved.
(2) According to the invention, the dimethyl formamide mixed solvent is added into the reaction furnace, and the copolymer containing a molecular chain with alkynyl on a non-terminal group is used for coating the surface of the silicon dioxide spherulites, so that the silicon dioxide spherulites can be prevented from forming agglomeration in liquid drops, the dispersion effect of the silicon dioxide spherulites is further effectively improved, and meanwhile, the efficiency of preparing the silicon dioxide spherulites is improved.
(3) According to the invention, the silica sphere solution is vibrated to form micron-scale liquid drops and nanometer-scale fog drops through two processes, and the preparation of the silica spheres can form stepped treatment, so that the preparation method is suitable for reaction conditions of different stages, and the homogeneity degree of the silica spheres is improved.
(4) In the process of separation and dehydration of the centrifugal machine, the temperature is increased to 90-95 ℃ in a stepped manner from 50-55 ℃; after the nano-scale fog drops are completely dehydrated, slowly cooling the nanometer-scale fog drops to 15-20 ℃ in a stepped manner from 90-95 ℃, further controlling reaction conditions, and avoiding the distance change of the silicon dioxide spherulites due to the reaction conditions, thereby improving the homogeneity degree of the silicon dioxide spherulites.
(5) The nano-scale filtering membrane has certain ductility, and can be stretched and extruded according to different requirements, so that micropores on the filtering membrane are changed in a certain range, and further silicon dioxide particles with different particle size requirements are obtained.
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In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a line graph showing the reaction time and the distribution of the silica pellet particle diameter in accordance with the preferred embodiment of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described herein, and therefore the scope of the present invention is not limited by the specific embodiments disclosed below.
In the description of the present invention, it is to be understood that the terms "first", "second", and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicit indication of the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the invention, the meaning of "a plurality" is two or more unless otherwise specified.
As shown in fig. 1, a process for preparing high-dispersion homogeneous nano-silica spheres comprises the following steps:
step S1: adding a silica sol aqueous solution, a silane coupling agent and toluene as initial raw materials into a reaction furnace, stirring and reacting at 90-110 ℃ to obtain a silica particle intermediate solution, and performing high-frequency resonance on the silica particle intermediate solution by using an ultrasonic oscillation device to form micron-sized fog drops.
Step S2: and (3) introducing the fog drops into the reaction furnace through a conveying pipeline, introducing inert gas containing nitrogen into the reaction furnace, adding a dimethylformamide mixed solvent into the reaction furnace, and reacting the fog drops containing silicon dioxide particles in the dimethylformamide solvent to obtain a silicon dioxide ball solution.
And step S3: and (3) allowing the nano-scale fog drops formed by high-frequency resonance of the silicon dioxide sphere solution by adopting a nano-scale ultrasonic generator to enter a centrifugal machine through a nano-scale filter membrane, and separating and dehydrating by using the centrifugal machine at the temperature of 50-95 ℃ to obtain the high-dispersion homogeneous nano-silicon dioxide spheres.
In a preferred embodiment of the invention, the nanometer-scale droplets pass through the nanometer-scale filter membrane and enter the centrifuge for separation and dehydration, so that the diameter of the silica spheres in the nanometer-scale droplets can be effectively controlled, and the nanometer-scale droplets are dehydrated in the centrifuge to form high-dispersion homogeneous silica spheres. And the silicon dioxide spheres are used as the silicon-based nano material, so that the advantages of controllable gradual release of the medicine, long validity period and good uniformity can be better utilized.
In a preferred embodiment of the present invention, the nano-scale filtration membrane is uniformly distributed with nano-micropores with a diameter in the range of 50-80 nm; the diameter of the silicon dioxide spherulites can be further controlled by uniformly arranging the nanometer micropores with the diameter within the range of 50-80 nanometers on the filtering membrane, and the high-dispersion and homogeneous effect of the preparation process is improved.
In a preferred embodiment of the present invention, the inert gas comprises: any one or more of helium, krypton and argon prevents the silicon dioxide in the reaction furnace from generating side reaction with other gases in the air through inert gas, the molecular purity of the silicon dioxide spheres is influenced, and meanwhile, the concentration of nitrogen in the inert gas is controlled to be between 60 and 80 percent, so that the nitrogen can be better used for promoting the generation of the copolymer with alkynyl on the non-terminal group of the molecular chain.
In a preferred embodiment of the present invention, the mixed solvent of dimethylformamide in step S2 includes: the copolymer with alkynyl on the molecular chain non-terminal group is prepared by reacting maleic anhydride, a toluene solvent, nitrogen, propiolic alcohol, tetrahydrofuran and an initiator at 80 ℃. The initiator is selected from one or more of benzoyl peroxide tert-butyl ester, azobisisobutyronitrile and benzoyl peroxide; by adding the dimethyl formamide mixed solvent into the reaction furnace and coating the surface of the silicon dioxide spherulites by using the copolymer containing the alkynyl on the non-terminal group of the molecular chain, the silicon dioxide spherulites can be prevented from forming agglomeration in liquid drops, the dispersion effect of the silicon dioxide spherulites is further effectively improved, and meanwhile, the efficiency of preparing the silicon dioxide spherulites is improved, and compared with the existing silicon dioxide sphere preparation technology, the preparation method has greater application advantages.
In a preferred embodiment of the invention, the silica sphere solution is vibrated to form micro-scale droplets and nano-scale droplets through two processes, so that the preparation of the silica spheres can form step-type treatment, thereby adapting to reaction conditions of different stages and improving the homogeneity degree of the silica spheres.
In a preferred embodiment of the invention, the temperature is increased to 90-95 ℃ in a step-like manner from 50-55 ℃ in the separation and dehydration process of the centrifugal machine; after the nano-scale fog drops are completely dehydrated, slowly cooling the nanometer-scale fog drops to 15-20 ℃ in a stepped manner from 90-95 ℃, further controlling reaction conditions, and avoiding the distance change of the silicon dioxide spherulites due to the reaction conditions, thereby improving the homogeneity degree of the silicon dioxide spherulites.
In a preferred embodiment of the present invention, the nano-scale filtration membrane has a certain ductility, and can be stretched and extruded according to different requirements, such that the micropores of the filtration membrane are changed within a certain range, thereby obtaining silica particles with different particle size requirements, and on the other hand, the nano-scale filtration membrane made of seaweed gel has a degradable property, and can obtain high-purity high-dispersion homogeneous nano-silica spheres by degrading the nano-scale filtration membrane.
Example one
Adding 55 parts of silica sol aqueous solution, 60 parts of silane coupling agent and 15 parts of toluene as initial raw materials into a reaction furnace, stirring and reacting at 90 ℃ to obtain silica particle intermediate solution, and performing high-frequency resonance on the silica particle intermediate solution by using an ultrasonic oscillation device to form micron-sized fog drops. And (3) introducing the fog drops into the reaction furnace through a conveying pipeline, introducing inert gas containing nitrogen into the reaction furnace, adding a dimethyl formamide mixed solvent into the reaction furnace, and reacting the fog drops containing silicon dioxide particles in the dimethyl formamide solvent to obtain a silicon dioxide ball solution. Enabling nanometer fog drops formed by high-frequency resonance of a silicon dioxide ball solution by adopting a nanometer ultrasonic generator to enter a centrifugal machine through a nanometer filtering membrane, and raising the temperature from 50 ℃ to 90 ℃ in a stepped manner; and after the nano-scale fog drops are completely dehydrated, slowly cooling the nano-scale fog drops from 90 ℃ to 15 ℃ in a stepped mode to obtain the high-dispersion homogeneous nano-silica spherical particles.
Example two
Adding 80 parts of silica sol aqueous solution, 95 parts of silane coupling agent and 30 parts of toluene as initial raw materials into a reaction furnace, stirring and reacting at 110 ℃ to obtain silica particle intermediate solution, and performing high-frequency resonance on the silica particle intermediate solution by using an ultrasonic oscillation device to form micron-sized fog drops. And (3) introducing the fog drops into the reaction furnace through a conveying pipeline, introducing inert gas containing nitrogen into the reaction furnace, adding a dimethylformamide mixed solvent into the reaction furnace, and reacting the fog drops containing silicon dioxide particles in the dimethylformamide solvent to obtain a silicon dioxide ball solution. Enabling nanometer fog drops formed by high-frequency resonance of a silicon dioxide ball solution by adopting a nanometer ultrasonic generator to enter a centrifugal machine through a nanometer filtering membrane, and raising the temperature from 55 ℃ to 95 ℃ in a stepped manner; and after the nano-scale fog drops are completely dehydrated, slowly cooling the nano-scale fog drops to 20 ℃ in a stepped manner from 95 ℃ to obtain the high-dispersion homogeneous nano-silica spherical particles.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.
Claims (7)
1. A process for preparing high-dispersion homogeneous nano silicon dioxide spheres is characterized by comprising the following steps:
step S1: adding a silica sol aqueous solution, a silane coupling agent and toluene serving as initial raw materials into a reaction furnace, stirring and reacting at 90-110 ℃ to obtain a silicon dioxide particle intermediate solution, and performing high-frequency resonance on the silicon dioxide particle intermediate solution by using an ultrasonic oscillation device to form micron-sized fog drops;
step S2: introducing the fog drops into a reaction furnace through a conveying pipeline, introducing inert gas containing nitrogen into the reaction furnace, simultaneously adding a dimethylformamide mixed solvent into the reaction furnace, and reacting the fog drops containing silicon dioxide particles in the dimethylformamide solvent to obtain a silicon dioxide ball solution;
and step S3: enabling nanometer-scale droplets formed by high-frequency resonance of a silicon dioxide ball solution by adopting a nanometer-scale ultrasonic generator to pass through a nanometer-scale filtering membrane to enter a centrifugal machine, wherein the nanometer-scale filtering membrane has certain ductility and is made of seaweed gel;
separating and dehydrating at 50-95 deg.C with a centrifuge, wherein the temperature is increased from 50-55 deg.C to 90-95 deg.C in stepwise manner during the separation and dehydration process; after the nano-scale fog drops are completely dehydrated, slowly cooling the nano-scale fog drops to 15-20 ℃ in a stepwise manner from 90-95 ℃ to obtain high-dispersion homogeneous nano-silica spherical particles;
the nanometer filtering membrane is uniformly distributed with nanometer micropores with the diameter ranging from 50 to 80 nanometers, and the high dispersion and homogenization effect of the silicon dioxide spherulites can be improved.
2. The process for preparing high-dispersion homogeneous nano silica spheres of claim 1, wherein the process comprises the following steps: the initial raw materials in the step S1 comprise: 55-80 parts of silica sol aqueous solution, 60-95 parts of silane coupling agent and 15-30 parts of toluene.
3. The process for preparing high-dispersion homogeneous nano silica spheres of claim 1, wherein the process comprises the following steps: the mixed solvent of dimethylformamide in the step S2 comprises: copolymers with alkynyl groups at non-terminal ends of the molecular chain.
4. The process for preparing high-dispersion homogeneous nano-silica spheres as claimed in claim 3, wherein the process comprises the following steps: the copolymer with alkynyl on the non-terminal group of the molecular chain is generated by the reaction of maleic anhydride, a toluene solvent, nitrogen, propiolic alcohol, tetrahydrofuran and an initiator at the temperature of 80 ℃.
5. The process for preparing high-dispersion homogeneous nano-silica spheres as claimed in claim 4, wherein the process comprises the following steps: the initiator is selected from one or more of benzoyl peroxide tert-butyl ester, azobisisobutyronitrile and benzoyl peroxide.
6. The process for preparing high-dispersion homogeneous nano silica spheres of claim 1, wherein the process comprises the following steps: the inert gas includes: helium, krypton, and argon.
7. The process for preparing high-dispersion homogeneous nano silica spheres of claim 6, wherein the process comprises the following steps: the concentration of the nitrogen in the inert gas is controlled between 60 and 80 percent.
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