WO2020143570A1 - Porous silica microspheres, manufacturing method and uses thereof - Google Patents

Porous silica microspheres, manufacturing method and uses thereof Download PDF

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WO2020143570A1
WO2020143570A1 PCT/CN2020/070444 CN2020070444W WO2020143570A1 WO 2020143570 A1 WO2020143570 A1 WO 2020143570A1 CN 2020070444 W CN2020070444 W CN 2020070444W WO 2020143570 A1 WO2020143570 A1 WO 2020143570A1
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microspheres
liquid crystal
porous silica
porous
polymer microspheres
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French (fr)
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Ang Li
Jiawei Lu
Nicholas L. Abbott
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Smart Liquid Crystal Technologies Co., Ltd.
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    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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    • C01B33/00—Silicon; Compounds thereof
    • C01B33/113—Silicon oxides; Hydrates thereof
    • C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28004—Sorbent size or size distribution, e.g. particle size
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28016—Particle form
    • B01J20/28019—Spherical, ellipsoidal or cylindrical
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28078—Pore diameter
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/281—Sorbents specially adapted for preparative, analytical or investigative chromatography
    • B01J20/282—Porous sorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/281—Sorbents specially adapted for preparative, analytical or investigative chromatography
    • B01J20/282—Porous sorbents
    • B01J20/283—Porous sorbents based on silica
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • C—CHEMISTRY; METALLURGY
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    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/02—Particle morphology depicted by an image obtained by optical microscopy
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    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
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    • C—CHEMISTRY; METALLURGY
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    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
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    • C01P2006/12—Surface area
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/16—Pore diameter

Definitions

  • the present invention relates to inorganic porous materials. More particularly, the invention relates to porous silica microspheres, their manufacturing method and their uses.
  • High performance liquid chromatography is a new high-performance and rapid analytical separation technology developed in the 1970s, which is the most commonly used analytical separation method and mainly used in chemical industry, food hygiene, drug detection, environmental monitoring and many other fields.
  • the chromatographic filler is the crucial foundation for the establishment and development of HPLC. Due to excellent mechanical strength, controllable pore structure and specific surface area, good stability and easily chemical bonding or modification, silica has become one of the most ideal filler materials for liquid chromatography, having a broad market application prospect.
  • silica gel which mainly are porous spherical silica gel (porous silica microspheres) . Since the shape, particle size and pore structure of porous silica microspheres can directly affect the column efficiency, selectivity and separation effect of a chromatographic column, how to precisely control these factors has become a key point to determine the separation ability of a chromatographic column, where the control of the internal pore structure of microspheres is more difficult. Silica microspheres with an ideal particle size can be prepared by some existing technologies.
  • Chinese patent CN102070152B discloses a method for preparing functional porous silica microspheres with a homogeneous size, but the preparation process is complicated and the arrangement of internal channels of the microspheres cannot be further controlled.
  • the traditional sol-gel method can prepare silica microspheres with an ordered internal pore structure.
  • Chinese patent CN105236427B discloses an ordered mesoporous silica nanospheres and its preparation method.
  • the size of microspheres used in a chromatographic column is generally required to be 3-10 ⁇ m, while the traditional sol-gel method is difficult to obtain silica spheres of such a large diameter.
  • one objective of the present invention is to provide porous silica microspheres having an internal structure and pore array of a radial configuration, wherein the average particle size of the porous silica microspheres is 3-300 ⁇ m.
  • the specific surface area of the porous silica microspheres is 100-1000 m 2 /g. In another embodiment, the average pore diameter of the porous silica microspheres is 1-100 nm.
  • Another objective of the present invention is to provide a method for preparing the porous silica microspheres, comprising:
  • the silica precursor is an orthosilicate ester compound or a silane compound.
  • an organic alcohol is added during the hydrolysis reaction.
  • the step of preparing porous amino-functionalized polymer microspheres comprises:
  • the amination agent used in the step (2) is ethylenediamine or ammonia.
  • the step of preparing porous functional polymer microspheres further comprises:
  • liquid crystal mixture comprises at least one reactive liquid crystal, at least one comonomer, at least one non-reactive liquid crystal and at least one polymerization initiator;
  • the comonomer contains function groups, the function groups are selected from the group of epoxy groups, hydroxyl groups, carboxyl groups, carboxylic ester groups and halogen groups.
  • the reactive liquid crystal is 5%-40%by weight of the liquid crystal mixture. In some embodiments, the molar ratio of the comonomer to the reactive liquid crystal is 1: 3-3: 1.
  • Another objective of the present invention is providing an application of the porous silica microspheres as the stationary phase in chromatograph separation.
  • the present invention discloses a method for preparing porous silica microspheres with an ordered internal structure and pore array by using the porous polymer microsphere with an ordered internal structure and pore array as the template.
  • the preparing method has the advantages of simple process, easy operation, good reproducibility and realizing large-scale production.
  • the prepared porous silica microspheres have a controllable particle size, an ordered internal structure and an ordered pore array, which make them widely used in chromatographic separation, catalytic carrier, drug release and other fields.
  • FIG. 1 is a cross polar microscope image of a porous silica microsphere prepared according to an embodiment of the present invention
  • FIG. 2 is a schematic, illustrative view of a membrane emulsifier technology for preparing liquid crystal droplets
  • FIG. 3 is (a) parallel polar and (b) cross polar microscope images of functional polymer microspheres prepared according to an embodiment of the present invention (same scale bar for all images) ;
  • FIG. 4 is IR spectra of functional polymer microspheres prepared according to embodiments of the present invention.
  • FIG. 5 is IR spectra of amino-functionalized polymer microspheres prepared according to embodiments of the present invention.
  • FIG. 6 is parallel polars (upper) and cross polars (lower) microscope images of porous silica microspheres prepared according to embodiments of the present invention, where the molar ratio of the comonomer to the reactive liquid crystal is (a) 1: 2, (b) 1: 1 and (c) 2: 1 (same scale bar for all images) ;
  • FIG. 7 is SEM images of internal structures of porous silica microspheres prepared according to an embodiment of the present invention.
  • FIG. 8 is parallel polar (upper) and cross polar (lower) microscope images of porous silica microspheres prepared according to embodiments of the present invention, where the mass percentage of the reactive liquid crystal is (a) 9.7%and (b) 19% (same scale bar for all images) ;
  • FIG. 9 is parallel polar (upper) and cross polar (lower) microscope images of porous silica microspheres prepared according to an embodiment of the present invention.
  • the invention discloses a porous silica microsphere with an internal structure and a pore array of a radial configuration, which means the internal structure and pore channels are arranged along the radial direction, resulting in the radial optical anisotropy (showing Maltese Black cross) .
  • the particle size of porous silica microspheres is uniform and controllable, and the average particle size can vary from 3 ⁇ m to 300 ⁇ m. More preferably, the average particle size can vary from 5 ⁇ m to 80 ⁇ m.
  • the specific surface area of porous silica microspheres can be adjusted between 100-1000 m 2 /g. More preferably, it can be adjusted between 100-500 m 2 /g.
  • the average pore diameter of the porous silica microspheres is 1-100 nm. More preferably, the average pore diameter of the channel is 10-50 nm.
  • the porous silica microspheres can be prepared by using functional polymer microspheres as the template. The detailed steps are described below.
  • porous amino-functionalized polymer microspheres are prepared. These polymer microspheres have an internal structure and a pore array of the radial configuration, showing the radial optical anisotropy. Meanwhile, there are many amino groups attaching to the surface and inner of the amino-functionalized polymer microspheres, which can further react with silica precursors to form silica.
  • the step also include: preparing porous functional polymer microspheres, where the functional polymer microspheres have an internal structure and a pore array of a radial configuration; functionalizing the functional polymer microspheres with amino groups.
  • the amination agent used in the reaction is ethylenediamine or ammonia.
  • the functional polymer microspheres have functional groups which can react with the amination agent and be replaced by amino groups, thus further forming porous amino-functionalized polymer microspheres.
  • silica precursor is added, which can hydrolyze on the surface and inside the pores of the amino-functionalized polymer microspheres to form silica, and then silica/polymer composite microspheres are developed.
  • the reaction can be carried out in water or a water-mixed solution, such as a mixed solution of water/ethanol or a mixed solution of water/isopropanol.
  • Some organic alcohols such as methanol, ethanol, isopropanol or glycol, can be added into the reaction to further control the hydrolysis rate, which is more favorable for the formation of silica inside the pores of polymer microspheres.
  • silica precursor can be conventional silicon sources, such as orthosilicate ester compounds (methyl orthosilicate, ethyl orthosilicate, etc. ) or silane compounds (dodecyltrimethoxysilane, etc. ) .
  • orthosilicate ester compounds methyl orthosilicate, ethyl orthosilicate, etc.
  • silane compounds dodecyltrimethoxysilane, etc.
  • TEOS ethyl orthosilicate
  • silica/polymer composite microspheres are calcined to decompose and remove the polymer, obtaining the porous silica microspheres.
  • the resulting silica microspheres retain the internal characteristics of the original functional polymer microspheres, that is to say, the prepared porous silica microspheres also have the internal structure and the pore array of a radial configuration.
  • the prepared porous silica microspheres can be applied for chromatograph separation.
  • they can be used as stationary phases of chromatographic columns. Due to the ordered internal structure and pore array of porous silica microspheres, the interaction between separated substances and stationary phase is regular, which can shorten the separation time, save mobile phase and improve the separation efficiency.
  • Step 1 at least one reactive liquid crystal, at least one non-reactive liquid crystal, at least one comonomer and at least one polymerization initiator are mixed in a certain ratio to form a uniform liquid crystal mixture.
  • the reactive liquid crystal contains polymerizable groups and can be further polymerized in the presence of polymerization initiators, such as acrylate type liquid crystals (RM257) , methacrylate type liquid crystals (HCM062) , allyl type liquid crystals (HCM126) and so on.
  • the mass percentage of the reactive liquid crystal to the liquid crystal mixture is 5%-40%. More preferably, the mass percentage is 1%-25%.
  • the non-reactive liquid crystal does not have polymerizable groups to further polymerize.
  • the non-reactive liquid crystal may contain at least one nematic liquid crystal, such as a nematic liquid crystal 5CB or a nematic liquid crystals mixture E7.
  • the comonomer contains unsaturated bonds which can react with polymerizable groups of reactive liquid crystals to form copolymers. Meanwhile, the comonomer has functional groups which can react with amination agent.
  • the functional groups include epoxy groups, hydroxyl groups, carboxyl groups, ester groups and halogen groups, but not limited to this, other functional groups which meet the conditions can also be included. In the following examples, glycidyl methacrylate containing epoxy groups is used as the comonomer.
  • the molar ratio of the comonomer to the reactive liquid crystal is 1: 3-3: 1.
  • Step 2 the liquid crystal mixture is dispersed into a continuous phase to form liquid crystal droplets through an emulsification process, where the liquid crystal droplets include the liquid crystal mixture.
  • the continuous phase can be water or a water miscible solution.
  • the method of the emulsification process includes stirring, shaking, ultrasonic and membrane emulsification.
  • the membrane emulsification is used, where the liquid crystal mixture is pushing into a continuous phase to form monodispersed liquid crystal droplets through a membrane emulsifier device.
  • the principle of the membrane emulsifier device is shown in FIG. 2, which mainly uses a membrane-based dispersion technique to achieve the preparation of monodisperse liquid crystal droplets.
  • the liquid crystal mixture as a dispersed phase is slowly passed through a micro porous inorganic membrane, and the liquid crystal mixture is extruded from the micropores of the inorganic membrane to form liquid crystal droplets dispersed into the continuous phase, thereby forming a dispersing system with the liquid crystal droplets as the disperse phase.
  • the size of the liquid crystal droplets can be controlled by the pore size of the inorganic membrane to finally control the particle size of the chiral polymer microspheres.
  • the continuous phase contains a liquid-crystal-configuration-adjusting agent, aligning the liquid crystal molecules (including the reactive liquid crystals 11 and the non-reactive liquid crystals) in the liquid crystal droplets in a regular configuration.
  • the liquid-crystal-configuration-adjusting agent aligns the liquid crystal molecules along the radial direction to form a radial configuration.
  • the liquid-crystal-configuration-adjusting agent can be an ionic surfactant, such as SDS; or inorganic salt, such as NaI and NaClO 4 . In the following examples, SDS is preferably.
  • Step 3 the reactive liquid crystals and the comonomers in the liquid crystal droplets are copolymerized to form intermediate microspheres containing the unreacted non-reactive liquid crystals.
  • liquid crystal molecules in the liquid crystal droplets are aligned in a regular configuration due to the presence of the liquid-crystal-configuration-adjusting agent.
  • the intermediate microspheres will maintain the structure in the same regular configuration.
  • the polymerization method may be photo polymerization, thermal polymerization or radiation polymerization. In the following examples, photo polymerization is preferably.
  • Step 4 functional polymer microparticles with a regular internal structure and pore array are further formed by removing the non-reactive liquid crystal. Since the non-reactive liquid crystals do not participate in the polymerization reaction, removing of the non-reactive liquid crystals forms micropores inside the functional polymer microspheres, whose distribution is influenced by the alignment of the liquid crystal molecules and tends to have a regular configuration. Meanwhile, the polymer microspheres retain the functional groups in the comonomer, which is evenly distributed on the surface and inside the pores of the polymer microspheres.
  • the structure, optical activity and preparing method of the porous silica microspheres is described in detail.
  • the specific surface area and internal pore diameter of the prepared silica microspheres can be measured by the common BET method.
  • the instrument used for BET test is Beckman Coulter specific surface analyzer SA3100.
  • the steps of preparing the liquid crystal mixture include: mixing the reactive liquid crystal, the non-reactive liquid crystal, the comonomer and the polymerization initiator according to a certain ratio, heating the mixture above the clearing point of the liquid crystals to form a uniform liquid, mixing the liquid well and then slowly cooling it to room temperature to form a homogeneous liquid crystal mixture. If photo polymerization is adopted, since the photo polymerization initiator is sensitive to light, the liquid must be kept in dark during the cooling process.
  • the steps of preparing functional polymer microspheres includes: slowly and smoothly passing the homogeneous liquid crystal mixture through a SPG membrane emulsifier device and dispersing it into a continuous phase containing a liquid-crystal-configuration-adjusting agent where the stirring speed is 300 r/min, to finally form a emulsion of monodispersed liquid crystal droplets; placing the emulsion under a UV light source (the center wavelength is 365nm) to process polymerization with continuous stirring, where the radiation intensity was 2.5 mW/cm 2 and the reaction time was 30 minutes; after polymerization, washing the reaction solution with ethanol 3 times, centrifuging it and removing the supernatant to obtain chiral polymer microspheres without the unreacted chemicals.
  • a UV light source the center wavelength is 365nm
  • a liquid crystal mixture containing 1.5 g of a reactive liquid crystal RM257, 8.5 g of a nonreactive liquid crystal 5CB, 0.1 g of a photo polymerization initiator DMPAP and 0.332 g of a comonomer glycidyl methacrylate (the mass percentage of the reactive liquid crystal is 14.4%, and the molar ratio of the comonomer to the reactive liquid crystal is 1: 1) were prepared and then polymer microspheres were prepared according to above steps, where the pore diameter of the SPG membrane is 10 ⁇ m, the continuous phase is water and the concentration of SDS in water is 2 mM. As shown in FIG.
  • the prepared polymer microspheres have an average size of 27 ⁇ m when dispersed in ethanol and show a radial optical anisotropy (Maltese Black Cross) .
  • a radial optical anisotropy Maltese Black Cross
  • the IR spectra of polymer microspheres shows that the characteristic peaks of epoxy groups at 902 cm -1 and 812 cm -1 (pointed by arrows in the figure) become more and more obvious with the increase amount of the comonomer.
  • silica/polymer composite microspheres were obtained after filtering, washing three times alternately with ethanol and distilled water and drying.
  • the porous silica microspheres were obtained by calcining the dried silica/polymer composite microspheres at 800°C for 6 hours.
  • the structures of prepared porous silica microspheres are slightly different, where the main parameters are shown in Table 1. Further, as shown in FIG. 6, the prepared porous silica microspheres all have the radial optical anisotropy (Maltese Black cross) , which indicates that the prepared porous silica microspheres all have a internal structure and pores array of a radial configuration. As shown in FIG. 7, SEM images further prove the internal structure along the radial direction.
  • 0.5 g amino-functionalized polymer microspheres were dispersed in 100 mL water/ethanol mixture solution (the volume ratio of ethanol and water is 4: 1) and 2 mL ammonia water was added slowly. Then the mixture of 3 g TEOS and 27 mL ethanol was added and the mixture solution was stirred for 24 hours.
  • the silica/polymer composite microspheres were obtained after filtering, washing three times alternately with ethanol and distilled water and drying.
  • the porous silica microspheres were obtained by calcining the dried silica/polymer composite microspheres at 800°C for 6 hours. With the different amount of the reactive liquid crystal, the structures of prepared porous silica microspheres are slightly different, where the main parameters are shown in Table 2.
  • the prepared porous silica microspheres all have the radial optical anisotropy (Maltese Black cross) , which indicates that the prepared porous silica microspheres all have a internal structure and pores array of a radial configuration.
  • a liquid crystal mixture containing 1.5 g of a reactive liquid crystal RM257, 8.5 g of a nonreactive liquid crystal 5CB, 0.1 g of a photo polymerization initiator DMPAP and 0.332 g of a comonomer glycidyl methacrylate (the mass percentage of the reactive liquid crystal is 14.4%, and the molar ratio of the comonomer to the reactive liquid crystal is 1: 1) were prepared separately and then polymer microspheres were prepared according to above steps, where the pore diameter of the SPG membrane is 2.8 ⁇ m, the continuous phase is water and the concentration of SDS in water is 2 mM.
  • 0.5 g amino-functionalized polymer microspheres were dispersed in 240 mL water/isopropanol mixture solution (the volume ratio of isopropanol and water is 5: 1) and 1 mL ammonia water was added slowly. Then the mixture of 0.5 g TEOS and 4.5 mL isopropanol was added and the mixture solution was stirred for 24 hours.
  • the silica/polymer composite microspheres were obtained after filtering, washing three times alternately with ethanol and distilled water and drying.
  • the porous silica microspheres with an average size of 10 ⁇ m were obtained by calcining the dried silica/polymer composite microspheres at 800°C for 6 hours.
  • the specific surface area is 123 m 2 /g and the average pore diameter is 25 nm.
  • the prepared porous silica microspheres all have the radial optical anisotropy (Maltese Black cross) , which indicates that the prepared porous silica microspheres all have a internal structure and pores array of a radial configuration.
  • the preparing method of the present invention can form porous silica microspheres with an ordered internal structure and pore array by using the porous polymer microsphere with an ordered internal structure and pore array as the template.
  • the preparing method has the advantages of simple process, easy operation, good reproducibility and realizing large-scale production.
  • the prepared porous silica microspheres have a controllable particle size, an ordered internal structure and an ordered pore array, which make them widely used in chromatographic separation, catalytic carrier, drug release and other fields.
  • porous silica microspheres and its manufacturing method of the present invention can be applied to the field of inorganic materials.

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CN114031087A (zh) * 2021-12-03 2022-02-11 晋江精纯科技有限公司 一种基于电位差引导组装的二氧化硅微球制备方法
CN115744925A (zh) * 2022-12-29 2023-03-07 厦门色谱分析仪器有限公司 一种采用双模板法制备单分散二氧化硅核壳微球的方法

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