CN117263501A - Preparation method and application of yttrium-containing hollow glass spheres - Google Patents
Preparation method and application of yttrium-containing hollow glass spheres Download PDFInfo
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- CN117263501A CN117263501A CN202311287543.1A CN202311287543A CN117263501A CN 117263501 A CN117263501 A CN 117263501A CN 202311287543 A CN202311287543 A CN 202311287543A CN 117263501 A CN117263501 A CN 117263501A
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- 229910052727 yttrium Inorganic materials 0.000 title claims abstract description 53
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 title claims abstract description 53
- QXJJQWWVWRCVQT-UHFFFAOYSA-K calcium;sodium;phosphate Chemical compound [Na+].[Ca+2].[O-]P([O-])([O-])=O QXJJQWWVWRCVQT-UHFFFAOYSA-K 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 239000002002 slurry Substances 0.000 claims abstract description 54
- 239000011521 glass Substances 0.000 claims abstract description 38
- 238000001354 calcination Methods 0.000 claims abstract description 34
- 239000007921 spray Substances 0.000 claims abstract description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000001694 spray drying Methods 0.000 claims abstract description 23
- 239000011259 mixed solution Substances 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000000853 adhesive Substances 0.000 claims abstract description 17
- 230000001070 adhesive effect Effects 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 15
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 11
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 11
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims description 28
- 239000007788 liquid Substances 0.000 claims description 23
- 239000002245 particle Substances 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 14
- 206010028980 Neoplasm Diseases 0.000 claims description 11
- 230000001105 regulatory effect Effects 0.000 claims description 10
- 230000002572 peristaltic effect Effects 0.000 claims description 9
- 239000011230 binding agent Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 238000005086 pumping Methods 0.000 claims description 5
- 239000003814 drug Substances 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 4
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 230000001276 controlling effect Effects 0.000 claims description 2
- 230000003993 interaction Effects 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 239000004005 microsphere Substances 0.000 description 25
- 230000008569 process Effects 0.000 description 10
- 239000000843 powder Substances 0.000 description 9
- VWQVUPCCIRVNHF-OUBTZVSYSA-N Yttrium-90 Chemical compound [90Y] VWQVUPCCIRVNHF-OUBTZVSYSA-N 0.000 description 7
- 238000001959 radiotherapy Methods 0.000 description 7
- 230000005855 radiation Effects 0.000 description 6
- 206010061902 Pancreatic neoplasm Diseases 0.000 description 5
- 208000015486 malignant pancreatic neoplasm Diseases 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 201000002528 pancreatic cancer Diseases 0.000 description 5
- 208000008443 pancreatic carcinoma Diseases 0.000 description 5
- 239000000377 silicon dioxide Substances 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 230000009471 action Effects 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 230000014509 gene expression Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000002285 radioactive effect Effects 0.000 description 3
- 239000011347 resin Substances 0.000 description 3
- 229920005989 resin Polymers 0.000 description 3
- 208000005189 Embolism Diseases 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000010109 chemoembolization Effects 0.000 description 2
- 239000000839 emulsion Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 239000004088 foaming agent Substances 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 230000006870 function Effects 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000000338 in vitro Methods 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 238000002271 resection Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- RUDFQVOCFDJEEF-UHFFFAOYSA-N yttrium(III) oxide Inorganic materials [O-2].[O-2].[O-2].[Y+3].[Y+3] RUDFQVOCFDJEEF-UHFFFAOYSA-N 0.000 description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 206010028813 Nausea Diseases 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 210000004204 blood vessel Anatomy 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000034994 death Effects 0.000 description 1
- 231100000517 death Toxicity 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 235000006694 eating habits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000007496 glass forming Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000000875 high-speed ball milling Methods 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000008693 nausea Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 210000004881 tumor cell Anatomy 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/10—Forming beads
- C03B19/107—Forming hollow beads
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K51/00—Preparations containing radioactive substances for use in therapy or testing in vivo
- A61K51/02—Preparations containing radioactive substances for use in therapy or testing in vivo characterised by the carrier, i.e. characterised by the agent or material covalently linked or complexing the radioactive nucleus
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/001—Use of materials characterised by their function or physical properties
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L24/00—Surgical adhesives or cements; Adhesives for colostomy devices
- A61L24/0047—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material
- A61L24/0052—Composite materials, i.e. containing one material dispersed in a matrix of the same or different material with an inorganic matrix
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C12/00—Powdered glass; Bead compositions
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61L—METHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
- A61L2430/00—Materials or treatment for tissue regeneration
- A61L2430/36—Materials or treatment for tissue regeneration for embolization or occlusion, e.g. vaso-occlusive compositions or devices
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Epidemiology (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Surgery (AREA)
- Organic Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Pharmacology & Pharmacy (AREA)
- Optics & Photonics (AREA)
- Medicinal Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- General Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Composite Materials (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Glass Compositions (AREA)
Abstract
The present disclosure provides a preparation method and an application of an yttrium-containing hollow glass sphere, wherein the preparation method of the yttrium-containing hollow glass sphere includes: adding a glass raw material comprising nano silicon dioxide and yttrium oxide into water, and stirring to form a mixed solution; adding an adhesive into the mixed solution to obtain slurry; introducing the slurry into a centrifugal spray dryer at a constant speed, and performing spray drying treatment to obtain a blank; and (3) sending the green body into a calciner, and performing calcination treatment to vitrify the green body to form the yttrium-containing hollow glass spheres.
Description
Technical Field
The embodiment of the disclosure relates to a preparation method of radioactive glass microspheres, in particular to a preparation method and application of yttrium-containing hollow glass spheres.
Background
According to the data issued by the international cancer research Institute (IARC) of the world health organization, it is shown that the number of new pancreatic cancer cases increases every year, the number of deaths of new cancers increases, and the incidence of pancreatic cancer increases year by year with the high side of eating habits and the prolongation of life expectancy. However, pancreatic cancer is hidden from disease and the anatomical location is complex, and only 20% of patients initially diagnosed with pancreatic cancer have an opportunity for surgical resection. Currently, there are multiple uses for arterial chemoembolization and in vitro radiotherapy for pancreatic cancer cases where surgical resection is not possible.
Compared with in-vitro radiotherapy, the arterial chemoembolization can kill tumor cells more closely and locally, avoid damaging other functions of the organism as much as possible, and reduce serious damage to the organism functions caused by radiotherapy. Currently, there are many methods for controlling the flow of liquid. As a targeted tumor radiotherapy scheme, glass microsphere radiation embolism treatment technology is also widely applied to selective in vivo radiotherapy of nausea tumors, and the radioactive glass microsphere plays a role in killing cancer cells at a focus through targeted high-dose high-energy beta radiation.
At present, resin microspheres or yttrium 90 glass microspheres are often adopted for targeted tumor radiotherapy in medical treatment, wherein the yttrium 90 glass microspheres have lower leaching rate compared with the resin microspheres, can ensure the stability of the microspheres in human bodies, but have higher density and poor following property; compared with glass microspheres, the resin microspheres have smaller density, can be more uniformly distributed in blood vessels around a focus, but have poor stability.
Disclosure of Invention
In order to solve at least one technical problem of the above or other aspects, the present disclosure provides a preparation method and an application of an yttrium-containing hollow glass ball, where the yttrium-containing hollow glass ball prepared by the method has a smaller density, a higher yttrium content, and a higher radiation active energy, so that the yttrium-containing hollow glass ball is convenient to be delivered in a human body on the basis of conforming to biotoxicity and is beneficial to be uniformly distributed at a tumor part.
As one aspect of the present disclosure, there is provided a method of preparing an yttrium-containing hollow glass sphere, comprising: adding a glass raw material comprising nano silicon dioxide and yttrium oxide into water, and stirring to form a mixed solution; adding an adhesive into the mixed solution to obtain slurry; introducing the slurry into a centrifugal spray dryer at a constant speed, and performing spray drying treatment to obtain a blank; and (3) sending the green body into a calciner, and performing calcination treatment to vitrify the green body to form the yttrium-containing hollow glass spheres.
In another aspect of the embodiments of the present disclosure, there is provided an application of the yttrium-containing hollow glass spheres prepared by the above method in preparing a medicament for treating tumor.
According to the preparation method and the application of the yttrium-containing hollow glass spheres, the glass raw materials comprising nano silicon dioxide and yttrium oxide are added into water to form a mixed solution, and the raw materials are nano-scale, so that the uniformity of particle size of the prepared spheres is ensured; adding an adhesive into the mixed solution, namely fully contacting and uniformly mixing the glass raw materials with the adhesive to form slurry; then spray drying treatment is carried out to atomize the slurry to form tiny liquid drops and evaporate water in the liquid drops to form a green body, and the slurry is controlled to enter a centrifugal spray dryer at a constant speed so as to ensure that the particle size of the green body is uniform; and further calcining in a calciner to decompose the binder thermally to increase the internal pressure of the blank, thereby forming the yttrium-containing hollow glass spheres. The method can improve the balling rate of the yttrium-containing hollow glass spheres to obtain the hollow glass spheres with low density, and the prepared yttrium-containing hollow glass spheres contain yttrium, oxygen and silicon and have simpler element composition.
Drawings
FIG. 1 is a schematic operation flow diagram of a method for preparing yttrium-containing hollow glass spheres in an embodiment of the disclosure;
FIG. 2 is a schematic diagram of a centrifugal spray dryer apparatus in an embodiment of the present disclosure;
FIG. 3 is a flow chart of the manufacture of yttrium-containing hollow glass spheres in an embodiment of the present disclosure.
The reference numerals have the following meanings:
210-a slurry barrel;
220-peristaltic pump;
230-centrifugal spray head;
240-a drying tower;
250-heater;
260-cyclone separator;
270-a collection container;
280-valve.
Detailed Description
For the purposes of promoting an understanding of the principles and advantages of the disclosure, reference will now be made to the embodiments illustrated in the drawings and specific language will be used to describe the same.
It should be understood that the description is only exemplary and is not intended to limit the scope of the present disclosure. In the following detailed description, for purposes of explanation, numerous specific details are set forth in order to provide a thorough understanding of the embodiments of the present disclosure. It may be evident, however, that one or more embodiments may be practiced without these specific details. In addition, in the following description, descriptions of well-known techniques are omitted so as not to unnecessarily obscure the concepts of the present disclosure.
The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the disclosure. The term "comprising" as used herein indicates the presence of a feature, step, operation, but does not preclude the presence or addition of one or more other features.
Where expressions like at least one of "A, B and C, etc. are used, the expressions should generally be interpreted in accordance with the meaning as commonly understood by those skilled in the art (e.g.," a system having at least one of A, B and C "shall include, but not be limited to, a system having a alone, B alone, C alone, a and B together, a and C together, B and C together, and/or A, B, C together, etc.). Where a formulation similar to at least one of "A, B or C, etc." is used, in general such a formulation should be interpreted in accordance with the ordinary understanding of one skilled in the art (e.g. "a system with at least one of A, B or C" would include but not be limited to systems with a alone, B alone, C alone, a and B together, a and C together, B and C together, and/or A, B, C together, etc.).
All terms (including technical and scientific terms) used herein have the same meaning as commonly understood by one of ordinary skill in the art unless otherwise defined. It should be noted that the terms used herein should be construed to have meanings consistent with the context of the present specification and should not be construed in an idealized or overly formal manner.
In the process of realizing the disclosure, it is found that only two types of yttrium 90 microspheres approved by the Food and Drug Administration (FDA) have been obtained, related researchers are discussing how to further improve the performance of the yttrium 90 microspheres, a droplet method is adopted to uniformly mix water glass or other glass forming materials with other additives according to a proper proportion, then the mixed solution is sprayed into a spray drying tower, and after spray drying, heat treatment is collected, glass microspheres can be obtained, and other researchers prepare glass microspheres by adopting a dry gel method and taking salts such as silicon, sodium, calcium, aluminum, boron and the like as raw materials.
In view of the above, the present disclosure provides a preparation method and application of an yttrium-containing hollow glass sphere, and provides an yttrium-containing hollow glass sphere with high radiation active energy, so as to facilitate smooth transportation in a human body on the basis of conforming to biotoxicity, and facilitate achieving uniform distribution at tumor sites to achieve treatment.
As an aspect of the present disclosure, a method for preparing an yttrium-containing hollow glass ball is provided, and fig. 1 is a schematic operation flow diagram of the method for preparing an yttrium-containing hollow glass ball according to an embodiment of the present disclosure, and as shown in fig. 1, the method for preparing an yttrium-containing hollow glass ball includes steps S101 to S104.
The step S101 includes: adding the glass raw materials comprising nano silicon dioxide and yttrium oxide into water, and stirring to form a mixed solution.
Step S102 includes: a binder is added to the mixed solution to obtain a slurry.
Step S103 includes: and (3) introducing the slurry into a centrifugal spray dryer at a constant speed, and performing spray drying treatment to obtain a blank.
Step S104 includes: and (3) sending the green body into a calciner, and performing calcination treatment to vitrify the green body to form the yttrium-containing hollow glass spheres.
According to the embodiment of the disclosure, specifically, in step S101, the raw materials selected for preparing the yttrium-containing hollow glass microspheres do not contain an organic foaming agent or other impurities, nano-scale silicon dioxide and yttrium oxide powder are added as raw materials into deionized water, and after mixing, the raw materials are subjected to high-speed ball milling and stirring for at least 3 hours by using a planetary ball mill so as to uniformly mix the raw materials, and then the mixed solution with the solid content of 5-30% is obtained through sieving, so that the uniformity of the prepared mixed solution is ensured.
In step S102, after the adhesive is added into the mixed solution, the mixed solution is fully stirred for 0.5-2 hours by using an electric stirrer, so that the adhesive is fully dissolved, the uniformity of a formed blank in the subsequent spray drying process is ensured, nano silicon dioxide and yttrium oxide are fully and uniformly mixed, contacted and bonded, a slurry with a certain viscosity is formed, layering can be avoided for a long time, uniform mixing is maintained, and a blank with uniform material and regular shape is formed after spray drying treatment.
In step S103, the slurry is fed at a uniform speed into a centrifugal spray dryer, where the slurry is atomized into fine droplets, which are then dried by heat exchange with hot air to form a green body.
In step S104, the green body is fed into a calciner, and during the calcination process in the calcination device, the binder in the green body is burned and decomposed, the internal pressure is increased, a hollow structure is formed, and the green body is vitrified by high-temperature instant heating, so that a solid yttrium-containing hollow glass ball is formed.
According to the embodiment of the disclosure, the yttrium-containing hollow glass spheres are prepared from the following materials: the preparation method comprises the steps of preparing slurry from glass raw materials, an adhesive and deionized water, wherein the selected materials do not contain an organic foaming agent or other impurities, atomizing the slurry to form tiny liquid drops through spray drying treatment, evaporating water in the liquid drops to form a green body, calcining the green body to enable the adhesive to react through thermal decomposition and the like, removing the adhesive, vitrifying the green body, and forming the solid yttrium-containing hollow glass microspheres in a powder form.
According to an embodiment of the present disclosure, performing a spray drying process includes: pumping the slurry into a centrifugal nozzle of a centrifugal spray dryer by utilizing a peristaltic pump, rotating blades in the centrifugal nozzle, and atomizing the slurry under the interaction of centrifugal force and friction force to form liquid drops; the droplets are contacted with hot air in a drying tower of a centrifugal spray dryer, heat exchange occurs, and water in the droplets volatilizes to form a blank body.
According to the embodiment of the disclosure, the slurry in a stirring state is conveyed into the centrifugal spray head by the peristaltic pump, 12 pore channels are uniformly distributed on the centrifugal spray head, the centrifugal spray head rotates at a high speed, and the slurry is atomized into fine liquid drops under the action of centrifugal force and friction force in the centrifugal spray head. At the same time, hot air enters the drying tower through a gas disperser at the top of the drying tower of the centrifugal spray dryer, the air flow direction is spiral downwards, atomized liquid drops are instantaneously heated by contacting with the hot air and undergo strong heat exchange, so that the solvent (deionized water) in the liquid drops is volatilized and depleted in a very short time, and a dried small-particle green body is formed.
According to an embodiment of the present disclosure, performing the spray drying process further includes: pumping the slurry into a centrifugal nozzle at a constant speed in a continuous state so as to regulate and control the particle size uniformity of the blank; the particle size of the green body is regulated and controlled by regulating the rotating speed of the centrifugal spray head.
According to the embodiment of the disclosure, the slurry is pumped in a pulse mode in the process of pumping the slurry by the peristaltic pump, so that the slurry is pumped to be in a continuous fluid state, the particle size difference of blanks prepared by centrifugal spraying is reduced, the uniformity of the blanks is improved, and the liquid outlet end of the peristaltic pump is connected with the flow stabilizing device, so that the liquid pumped into the centrifugal nozzle by the peristaltic pump is in a continuous flow state.
According to the embodiment of the disclosure, the rotating speed of the centrifugal nozzle can be adjusted in a large range, and the larger the rotating speed of the centrifugal nozzle is, the smaller the particle size of the thrown liquid drops is.
According to the embodiments of the present disclosure, the rotational speed of the centrifugal nozzle is 18000 rpm to 36000 rpm, for example, 18000 rpm, 20000 rpm, 25000 rpm, 28000 rpm, 30000 rpm, etc., but not limited to the recited values, and other non-recited values within the range of values are equally applicable. The adjustable range of liquid drops thrown out of the centrifugal spray head is larger.
According to the embodiments of the present disclosure, the inlet temperature of centrifugal spray drying of the centrifugal spray dryer is set to 220 to 300 ℃, for example, 220 ℃, 230 ℃, 250 ℃, 280 ℃, 300 ℃ and the like can be used, but the present invention is not limited to the recited values, and other non-recited values within the range of the values are equally applicable. If the temperature is too low, the solvent is not evaporated by a sufficient heat source, only a small part of the solvent is lost, the particles are not completely dried, and the rest part of the solvent becomes sticky due to concentration, so that the product is agglomerated; if the temperature is too high, it will cause the evaporation of water to be accelerated, leaving a large amount of heat remaining, which will allow the microspheres to form more quickly without sufficient time to shrink, resulting in a larger green body size or product deterioration.
According to the embodiments of the present disclosure, the outlet temperature of the centrifugal spray dryer is 100 to 150 ℃, for example, 100 ℃, 110 ℃, 120 ℃, 150 ℃, etc., but not limited to the recited values, and other non-recited values within the range of values are equally applicable. If the outlet temperature is too low, the pellets in the drying tower will not become sufficiently dry after treatment, which will result in sticky pellets being able to clog or plug the channels; if the outlet temperature is too high, there may be an excess capacity that is still not utilized.
According to the embodiment of the disclosure, the particle size of the green body formed after the spray drying treatment directly affects the particle size of the yttrium-containing hollow glass spheres formed after the calcination treatment, and the particle size and the quality of the green body finally collected from the centrifugal spray drying equipment can be controlled by adjusting the rotation speed of a centrifugal nozzle of a centrifugal spray dryer, the inlet temperature and the outlet temperature of the centrifugal spray drying, and the solid content and the viscosity of slurry.
Fig. 2 is a schematic diagram of a centrifugal spray drying treatment system in an embodiment of the present disclosure.
As shown in fig. 2, the centrifugal spray drying treatment system includes a slurry tank 210, a peristaltic pump 220, a centrifugal spray head 230, a drying tower 240, a heater 250, a cyclone 260, a receiving device 270, and a valve 280. The centrifugal spray drying process is briefly described below in connection with fig. 2.
According to embodiments of the present disclosure, the prepared slurry is poured into the slurry barrel 210, the valve 280 under the slurry barrel 210 is opened, and the slurry enters the peristaltic pump 220, wherein an electric stirrer may be installed in the slurry barrel 210 to perform uninterrupted stirring, so that the slurry is in a uniformly mixed state. The heater 250 is opened to introduce hot air into the drying tower 240 from below the centrifugal spray head 230, a high-temperature environment is provided for the drying tower, slurry is conveyed into the centrifugal spray head 230 of the centrifugal spray dryer by the peristaltic pump 220, the slurry is thrown out and atomized into liquid drops under the combined action of centrifugal force and friction force under the high-speed rotation action of the centrifugal spray head 230, the liquid drops enter the drying tower 240 to be contacted with the dried hot air for heat exchange, moisture in the liquid drops is quickly evaporated under the high-temperature action, the trend of the liquid drops in the drying tower 240 is the same as the airflow direction of the hot air, and the liquid drops form blanks in the drying tower 240. The bottom of the drying tower 240 is provided with a valve 280, the valve 280 can be opened to collect the green body into the collecting container 270, the cyclone separator 260 can be opened to separate hot air from the green body, and the green body is collected into the collecting container 270 below the cyclone separator 260, so that the spray drying treatment is completed.
According to the embodiment of the disclosure, when the calcination treatment is performed, the calcination time of the green body is adjusted by adjusting the feeding rate of the green body into the calciner; the calcination temperature of the green body is regulated by regulating the ratio of air to combustible gas in the calciner.
According to embodiments of the present disclosure, the green body is fed into the calciner at a feed rate of 10 to 30g/min. The feed rate may be 10g/min, 15g/min, 18g/min, 22g/min, 28g/min, etc., but is not limited to the recited values, and other non-recited values within this range are equally applicable. The overfire length of the green body in the calciner can be controlled by adjusting the feeding amount of the green body fed into the calciner, so that the prepared yttrium-containing hollow glass spheres have the advantages of small density, small particle size and higher yttrium content.
According to the embodiment of the disclosure, main components of the calciner are a feeding and distributing system, a powder calcining chamber and a powder collecting bin. In the calcining process, the green body is scattered through a feeding and distributing system and uniformly enters a powder calcining chamber, high-temperature flame is arranged in the powder combustion chamber and provides calcining temperature, the green body is rapidly heated through a high-temperature flame zone to be calcined, then enters a powder collecting bin, and finally, microspheres settled in a collecting disc at the bottom of the powder collecting bin are yttrium-containing hollow glass spheres.
According to the embodiment of the present disclosure, the calcination temperature of the calcination treatment is 700 to 900 ℃, for example, 700 ℃, 800 ℃, 850 ℃, 900 ℃, or the like, but the calcination treatment is not limited to the listed values, and other non-listed values within the range of the values are equally applicable. The calcination temperature and the calcination time of the high-temperature calcination treatment affect the quality of the product, and when the calcination temperature is too high, the performance of the product is reduced, even the overburning defect occurs, and when the calcination temperature is too low, the performance of the product is possibly reduced because the calcination is not thorough, or a hollow structure cannot be formed. The proper calcination time can promote the formation of glass microspheres, and the microstructure of the yttrium-containing hollow glass spheres can be perfected by adjusting the calcination time according to the state of a blank body obtained in the preparation process, but if the calcination time is too long, crystal grains of the yttrium-containing hollow glass spheres can grow rapidly, secondary recrystallization occurs, and the performance control of products is not facilitated.
According to the embodiment of the disclosure, the blank obtained after centrifugal spray drying treatment is sent into a calciner, the feeding rate is provided by a gas loading mode, and the binder in the blank is burnt out in the process of rapid high-temperature calcination in a calcination device, so that the formed glass microspheres only contain silicon dioxide and yttrium oxide. The original blank is vitrified by the instant heating process at 700-900 ℃ to form the firm yttrium-containing hollow glass ball.
According to an embodiment of the present disclosure, the binder comprises at least one of polyvinyl alcohol, cetyltrimethylammonium bromide; the amount of the binder to be added is 1% to 10%, and may be, for example, 1%, 3%, 5%, 8%, 10%, etc.
According to embodiments of the present disclosure, the adhesion of the slurry is improved by the addition of the binder to bond the nanoscale silica and yttria. After the adhesive is added into the mixed solution and stirred uniformly, the method further comprises the following steps: and testing the viscosity of the slurry, and adjusting the viscosity of the slurry according to the test result to ensure that the viscosity of the slurry is not higher than 200cps.
According to the embodiment of the disclosure, after the adhesive is added into the mixed solution, stirring is carried out for 0.5-2 hours, so that the emulsion slurry is fully and uniformly mixed with the adhesive to form adhesive slurry, the viscosity of the emulsion slurry is lower than 200cps, and the uniformity of a blank body formed subsequently is ensured.
According to embodiments of the present disclosure, the purity of silica and yttria is 99.99%, and the particle size is nano-scale.
According to the embodiment of the disclosure, the mass mixing ratio of the nano silicon dioxide to the yttrium oxide is 4:1 to 3:2, for example, may be 4: 1. 2: 1. 3:2, etc., siO 2 And Y is equal to 2 O 3 The ratio of (3) can be adjusted according to the difference of the subsequent use scenes, and slurries with different yttrium contents can be formed by adjusting different mixing ratios of raw materials, and the water content in the mixed solution can be 30% -70%, for example, 30%, 40%, 50%, 60% and 70%, but the water content is not limited to the listed values, and other non-listed values in the numerical range are applicable. When the water content is too large, the fluidity of the slurry is large, after the slurry is atomized into small liquid drops by a centrifugal spray dryer, the water content in the liquid drops is more, the mass of solids in the green body is less after the solvent is evaporated in the drying process, the particle size is also smaller, and the green body with uniform and regular quality is not easy to form; when the water content is too small, the viscosity of the slurry becomes high, and the slurry cannot be atomized into droplets against intermolecular friction under a fixed centrifugal force, cannot leave the spray dryer, and may form droplets having a large diameter, and cannot be dried rapidly to form a green body.
According to an embodiment of the disclosure, fig. 3 is a flowchart of a process for manufacturing an yttrium-containing hollow glass ball in the embodiment of the disclosure, as shown in fig. 3, firstly, mixing silicon dioxide, yttrium oxide and deionized water, stirring to obtain a mixed solution, adding an adhesive into the mixed solution, introducing the formed slurry into a centrifugal spray dryer, performing spray drying treatment to obtain a blank, and then, placing the blank into a high-temperature powder calciner for calcination treatment to obtain the yttrium-containing hollow glass ball.
In another aspect of the embodiments of the present disclosure, there is provided an application of the yttrium-containing hollow glass spheres prepared by the above method in preparing a medicament for treating tumor.
According to the embodiment of the disclosure, the yttrium-containing hollow glass spheres prepared by the method have the mass fraction of yttrium of 10% -50%, have lower density of 0.8-3.6 g/cc, are more beneficial to smooth transportation in a human body and can reach and be uniformly distributed at tumor sites. The irradiation of the yttrium-containing hollow glass spheres comprises the steps of placing the glass microspheres in a neutron reactor for irradiation, so that the glass microspheres produce yttrium element @, and 89 radioisotope of Y) 90 Y) with radioactivity. After irradiation, yttrium element in the yttrium-containing hollow glass spheres is provided with radioactivity by generating radioisotope of the yttrium element, so that the glass microspheres can be used for radiotherapy. Yttrium 90% 90 The Y) microsphere can emit pure beta rays in the treatment of radioactive embolism, the highest energy reaches 2.27 megaelectron volts (MeV), the average is 0.9367MeV, the half life is 64.2h, the radiation range is small, the maximum penetration in tissues is 11mm, and the average is 2.5mm; the energy is released to 87% in 8 days, 95% in 2 weeks, and the effective radiation lasts for 7 half-lives, namely about 18 days. 90 The mode of Y decay is: 39 Y 90 → 40 Zr 90 +β - zirconium 90 which decays from yttrium 90 to stable and nontoxic 90 Zr)。
The preparation method provided by the disclosure has the advantages of simple raw material proportion, simple and available equipment, short time consumption in the preparation process and suitability for miniaturized production. And the obtained yttrium-containing hollow glass microspheres have high yttrium content, smaller density and particle size and wide application prospect.
Thus, embodiments of the present disclosure have been described in detail with reference to the accompanying drawings.
It should be noted that, in the drawings or the text of the specification, implementations not shown or described are all forms known to those of ordinary skill in the art, and not described in detail. Furthermore, the above definitions of the components are not limited to the specific structures, shapes or modes mentioned in the embodiments, and may be simply modified or replaced by those of ordinary skill in the art.
It should also be noted that, in the specific embodiments of the disclosure, unless otherwise noted, the numerical parameters set forth in the specification and attached claims are approximations that may vary depending upon the desired properties sought to be obtained by the present disclosure. In particular, all numbers expressing dimensions, range conditions, and so forth, used in the specification and claims are to be understood as being modified in all instances by the term "about". In general, the meaning of expression is meant to include a variation of + -10% in some embodiments, a variation of + -5% in some embodiments, a variation of + -1% in some embodiments, and a variation of + -0.5% in some embodiments by a particular amount.
Those skilled in the art will appreciate that the features recited in the various embodiments of the disclosure and/or in the claims may be provided in a variety of combinations and/or combinations, even if such combinations or combinations are not explicitly recited in the disclosure. In particular, the features recited in the various embodiments of the present disclosure and/or the claims may be variously combined and/or combined without departing from the spirit and teachings of the present disclosure. All such combinations and/or combinations fall within the scope of the present disclosure.
The foregoing embodiments have been provided for the purpose of illustrating the general principles of the present disclosure, and are not meant to limit the disclosure to the particular embodiments disclosed, but to limit the scope of the disclosure to the particular embodiments disclosed.
Claims (10)
1. A method for preparing yttrium-containing hollow glass spheres, comprising the following steps:
adding a glass raw material comprising nano silicon dioxide and yttrium oxide into water, and stirring to form a mixed solution;
adding an adhesive into the mixed solution to obtain slurry;
introducing the slurry into a centrifugal spray dryer at a constant speed, and performing spray drying treatment to obtain a blank;
and (3) sending the green body into a calciner, and calcining to vitrify the green body to form the yttrium-containing hollow glass spheres.
2. The preparation method according to claim 1, wherein,
the spray drying treatment comprises:
pumping the slurry into a centrifugal nozzle of the centrifugal spray dryer by utilizing a peristaltic pump, rotating blades in the centrifugal nozzle, and atomizing the slurry under the interaction of centrifugal force and friction force to form liquid drops;
and the liquid drops are contacted with hot air in a drying tower of the centrifugal spray dryer, heat exchange is carried out, and water in the liquid drops is volatilized to form the blank body.
3. The preparation method according to claim 2, wherein,
pumping the slurry into a centrifugal nozzle at a constant speed in a continuous state so as to regulate and control the particle size uniformity of the blank;
and regulating and controlling the particle size of the green body by regulating the rotating speed of the centrifugal spray head.
4. The preparation method according to claim 3, wherein,
the rotating speed of the centrifugal nozzle is 18000-36000 r/min;
the inlet temperature of the centrifugal spray dryer is 220-300 ℃;
the outlet temperature of the centrifugal spray dryer is 100-150 ℃.
5. The preparation method according to claim 1, wherein,
when the calcination treatment is carried out, the calcination time of the green body is regulated by regulating the feeding rate of the green body into the calciner;
the calcination temperature of the green body is regulated by regulating the ratio of air to combustible gas in the calciner.
6. The preparation method according to claim 1, wherein,
after the adhesive is added into the mixed solution and stirred uniformly, the method further comprises the following steps:
and testing the viscosity of the slurry, and adjusting the viscosity of the slurry according to the test result so that the viscosity of the slurry is not higher than 200cps.
7. The preparation method according to claim 1, wherein,
the mass mixing ratio of the nano silicon dioxide to the yttrium oxide is 4:1 to 3:2;
the water content in the mixed solution is 30-70%.
8. The preparation method according to claim 1, wherein,
the binder comprises at least one of polyvinyl alcohol and cetyltrimethylammonium bromide;
the addition amount of the adhesive is 1-10%.
9. The preparation method according to claim 5, wherein,
the feeding rate of the green body into the calciner is 10-30 g/min;
the calcination temperature of the calcination treatment is 700-900 ℃.
10. Use of yttrium-containing hollow glass spheres prepared by the method of any one of claims 1 to 9 in the manufacture of a medicament for the treatment of tumors.
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