CN118145658A - Method for efficiently preparing micron-sized silicon dioxide microspheres by using water glass through reversed-phase suspension dispersion - Google Patents
Method for efficiently preparing micron-sized silicon dioxide microspheres by using water glass through reversed-phase suspension dispersion Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 178
- 239000004005 microsphere Substances 0.000 title claims abstract description 88
- 239000006185 dispersion Substances 0.000 title claims abstract description 71
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims abstract description 56
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 52
- 235000019353 potassium silicate Nutrition 0.000 title claims abstract description 41
- 239000000725 suspension Substances 0.000 title claims abstract description 17
- 235000012239 silicon dioxide Nutrition 0.000 title claims description 50
- 238000001035 drying Methods 0.000 claims abstract description 28
- 239000002245 particle Substances 0.000 claims abstract description 24
- 239000012074 organic phase Substances 0.000 claims abstract description 19
- 239000012071 phase Substances 0.000 claims abstract description 10
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 239000010705 motor oil Substances 0.000 claims description 56
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 45
- 238000002156 mixing Methods 0.000 claims description 20
- 239000011148 porous material Substances 0.000 claims description 17
- 235000011054 acetic acid Nutrition 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 12
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 9
- 239000003921 oil Substances 0.000 claims description 9
- 235000019198 oils Nutrition 0.000 claims description 9
- 239000011591 potassium Substances 0.000 claims description 9
- 229910052700 potassium Inorganic materials 0.000 claims description 9
- 235000012424 soybean oil Nutrition 0.000 claims description 9
- 239000003549 soybean oil Substances 0.000 claims description 9
- 230000032683 aging Effects 0.000 claims description 8
- 230000002378 acidificating effect Effects 0.000 claims description 7
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 6
- 235000019483 Peanut oil Nutrition 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 239000000312 peanut oil Substances 0.000 claims description 6
- 235000020238 sunflower seed Nutrition 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 5
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 230000001376 precipitating effect Effects 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 239000003929 acidic solution Substances 0.000 claims description 3
- 238000009775 high-speed stirring Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- 241000196324 Embryophyta Species 0.000 claims description 2
- 241001465754 Metazoa Species 0.000 claims description 2
- AVMNFQHJOOYCAP-UHFFFAOYSA-N acetic acid;propanoic acid Chemical compound CC(O)=O.CCC(O)=O AVMNFQHJOOYCAP-UHFFFAOYSA-N 0.000 claims description 2
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 235000019270 ammonium chloride Nutrition 0.000 claims description 2
- 235000015165 citric acid Nutrition 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 239000003502 gasoline Substances 0.000 claims description 2
- 229930195733 hydrocarbon Natural products 0.000 claims description 2
- 150000002430 hydrocarbons Chemical class 0.000 claims description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 2
- 239000003350 kerosene Substances 0.000 claims description 2
- 239000001630 malic acid Substances 0.000 claims description 2
- 235000011090 malic acid Nutrition 0.000 claims description 2
- 239000011707 mineral Substances 0.000 claims description 2
- 239000003208 petroleum Substances 0.000 claims description 2
- 229920002545 silicone oil Polymers 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- RLQWHDODQVOVKU-UHFFFAOYSA-N tetrapotassium;silicate Chemical compound [K+].[K+].[K+].[K+].[O-][Si]([O-])([O-])[O-] RLQWHDODQVOVKU-UHFFFAOYSA-N 0.000 claims description 2
- 239000004215 Carbon black (E152) Substances 0.000 claims 1
- 239000002253 acid Substances 0.000 abstract description 24
- 238000004140 cleaning Methods 0.000 abstract description 19
- 239000002994 raw material Substances 0.000 abstract description 17
- 238000002360 preparation method Methods 0.000 abstract description 13
- 238000005265 energy consumption Methods 0.000 abstract description 6
- 238000001556 precipitation Methods 0.000 abstract description 6
- 238000004064 recycling Methods 0.000 abstract description 6
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical class O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 abstract description 6
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
- 239000002002 slurry Substances 0.000 description 50
- 239000000243 solution Substances 0.000 description 36
- 239000000047 product Substances 0.000 description 34
- 238000001914 filtration Methods 0.000 description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 17
- 238000000879 optical micrograph Methods 0.000 description 12
- 238000009826 distribution Methods 0.000 description 11
- 239000000126 substance Substances 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 7
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 5
- 238000001514 detection method Methods 0.000 description 5
- 238000000053 physical method Methods 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 229940072033 potash Drugs 0.000 description 3
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 description 3
- 235000015320 potassium carbonate Nutrition 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 230000002194 synthesizing effect Effects 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 235000019484 Rapeseed oil Nutrition 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 229940008099 dimethicone Drugs 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 1
- 238000011143 downstream manufacturing Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000003925 fat Substances 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000007867 post-reaction treatment Methods 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 239000002910 solid waste Substances 0.000 description 1
- -1 sorbitan fatty acid ester Chemical class 0.000 description 1
- 239000012798 spherical particle Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- 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
- C01B33/187—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates
- C01B33/193—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof by acidic treatment of silicates of aqueous solutions of silicates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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
- C01P2006/12—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
- C01P2006/14—Pore volume
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a method for efficiently preparing micron-sized silica microspheres by using water glass through reversed-phase suspension dispersion, which adopts the principle of preparing weak acid by using strong acid, mixes different kinds of silicic acid compounds and different organic phases according to proportion, drops different kinds/concentration of acid under the condition of high-speed dispersion for reaction, continuously disperses for a period of time after the silica microspheres are separated out, and obtains monodisperse micron-sized amorphous silica microspheres with different particle diameters through precipitation, cleaning and drying. The raw material water glass used in the invention has low cost, does not need to use an emulsifying agent, greatly simplifies the operation flow, can realize the recycling of an organic phase, and has the advantages of simple operation, low energy consumption, low cost and environmental protection in the whole preparation flow. The micron-sized silica microsphere prepared by the method contains a large number of hydroxyl groups, has a large specific surface area, can regulate and control the particle size, has high sphericity, and has great advantages and application prospects in the aspect of micron-sized silica microsphere preparation.
Description
Technical Field
The invention relates to the technical field of preparation of silica microspheres, in particular to a method for efficiently preparing micron-sized silica microspheres by using water glass through reversed-phase suspension dispersion.
Background
Silica microspheres exhibiting excellent mechanical, thermal, chemical (especially acid resistance) and biological stability, composite materials made from silica microspheres are used in many monitoring fields, including detection of biomolecules, ions and compounds. In particular, the micron-sized silica microspheres have wide application, can be used as reinforcing materials in different media to improve the strength, hardness, chemical stability, wear resistance, corrosion resistance, weather resistance and other characteristics of a matrix, such as the monodisperse silica microspheres are widely applied to display panels, and stably support a gap space in liquid crystal to serve as a framework. In addition, silica microspheres have large pore size, low toxicity and high specific surface area, are ideal adsorbents and chemical carriers, and have high hydroxyl content on the surface of amorphous silica, thus providing various possibilities for surface modification.
The current method for preparing micron-sized silica microspheres is mainly divided into a physical method and a chemical method, wherein the physical method comprises a mechanical grinding method, a spray drying method and a high-temperature spheroidization method; chemical methods include template methods, gas phase methods and precipitation methods. In the physical method, irregularly shaped silica raw materials are formed into spheres by a series of physical methods. In the chemical method, silica microspheres are obtained by a series of chemical modifications using organosilicon or water glass as a raw material. Compared with the physical method, the chemical synthesis process has the main advantages of low energy consumption and high purity. However, most chemical synthesis methods use silicones as a silicon source, such as ethyl orthosilicate, which is expensive and a byproduct of the reaction is an organic substance, which increases the post-reaction treatment cost and complicates downstream processing. Compared with the precipitation method, the evaporation method and the template method use cheap water glass as a silicon source, but the problems of complex ion exchange process, poor product quality and the like are also existed. Therefore, there is an urgent need to develop a low-cost, low-energy-consumption process for synthesizing micron-sized silica microspheres to achieve the "low-carbon energy-saving" goal.
At present, the technology for synthesizing the silicon dioxide microspheres by taking water glass as a raw material is very rare, and almost all the technology is industrially used for synthesizing the silicon dioxide microspheres from Tetraethoxysilane (TEOS), because the silicon dioxide microspheres produced by the technology have good sphericity, low compactness and easily controlled size. Although the synthesis of the silicon dioxide microspheres from the water glass has the advantages of low raw material cost, low production rate, environmental protection and the like, the silicon dioxide microspheres synthesized by the technology have high degree of polymerization, spherical particles cannot be monodisperse, all the emulsifying agent is needed, and the prepared organic phase is difficult to recycle, so that the industrial production is very difficult. Therefore, it is necessary to develop a process for preparing silica microspheres with water glass as raw material, which greatly simplifies the operation flow and realizes the recycling of the organic phase.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a method for efficiently preparing micron-sized silica microspheres by using water glass through reversed-phase suspension dispersion, the invention can obtain micron-sized silica microspheres with excellent sphericity and controllable particle size and pore volume, and can realize the recycling of an organic phase after preparation, and the whole preparation process is simple to operate, low in energy consumption, low in cost and environment-friendly, thereby solving the problems mentioned in the background art.
In order to achieve the above purpose, the present invention provides the following technical solutions: a method for efficiently preparing micron-sized silica microspheres by using water glass through reversed-phase suspension dispersion comprises the following steps:
s1, mixing liquid water glass and an organic phase according to a certain proportion, and dispersing and ageing at a high speed to form a reaction precursor;
s2: dropwise adding an acidic solution into the precursor dispersed in the high-speed stirring;
S3: continuing dispersing and aging for a period of time after the silica microspheres are separated out;
s4: and precipitating, washing and drying to obtain the monodisperse micron-sized silica microspheres.
Preferably, the liquid water glass in the step S1 includes sodium water glass Na 2O·nSiO2, potassium water glass K 2O·nSiO2 and/or potassium/sodium water glass (K/Na) 2O·nSiO2 with different moduli n, where the range of the different moduli n is 2.3-3.3.
Preferably, the organic phase in the step S1 is a mixed liquid of fats or mineral hydrocarbons contained in animals and plants, including one or a mixture of several of engine oil, silicone oil, vacuum pump oil, petroleum, gasoline, kerosene, peanut oil, soybean oil, and sunflower seed oil.
Preferably, in the step S1, the volume ratio of the liquid water glass to the organic phase is 1:1 to 200.
Preferably, in the step S1, the volume ratio of the liquid water glass to the organic phase is 1:3 to 50.
Preferably, the dispersion speed in the step S1 is 100-5000 r/min, and the aging time is 1-60 min.
Preferably, the dispersion speed in the step S1 is 500-3000 r/min, and the aging time is 5-40 min.
Preferably, the mass percentage concentration of the acidic liquid in the step S2 is 1% to the pure solvent, and the dripping rate is 0.05-100 mL min -1; the acidic liquid is acetic acid, citric acid, malic acid, formic acid, acetic acid propionic acid, carbonic acid, sulfuric acid, hydrochloric acid, phosphoric acid, ammonium chloride or ethyl acetate.
Preferably, the mass percentage concentration of the acidic liquid in the step S2 is 5% to 60%, and the dripping rate is 0.5-30 mL min -1.
Preferably, the dispersion speed in the step S3 is 100-5000 r/min, and the dispersion time is 1-60 min.
Preferably, the dispersion speed in the step S3 is 500-3000 r/min, and the dispersion time is 10-30 min.
Preferably, the drying temperature in the step S4 is 20-200 ℃ and the drying time is 20 min-72 h.
Preferably, the drying temperature in the step S4 is 80-120 ℃ and the drying time is 20 min-48 h.
Preferably, the particle size of the monodisperse micron-sized amorphous silica microspheres is 1-500 mu m, the specific surface area is 5-800 m 2/g, and the pore volume is 0.1726-0.43 cm 3/g.
Preferably, the particle size of the monodisperse micron-sized amorphous silica microspheres is 20-300 mu m, the specific surface area is 100-400 m 2/g, and the pore volume is 0.17-0.2624 cm 3/g.
Preferably, in the method for preparing the micron-sized silica microspheres, the organic phase can be recycled without using an emulsifying agent, the particle size of the monodisperse micron-sized amorphous silica microspheres prepared after recycling for 30-50 times is still kept to be 1-500 mu m, the specific surface area is 5-800 m 2/g, and the pore volume is 0.17-0.43 cm 3/g.
The beneficial effects of the invention are as follows: aiming at the problems of the existing precipitation method which takes water glass as a raw material to generate silica microspheres, the invention develops a method for efficiently preparing micron-sized silica microspheres by the water glass through a reversed-phase suspension dispersion technology, adopts the principle of preparing weak acid from strong acid, utilizes the water glass to react under the acidic condition to generate silicic acid, and the characteristic of supersaturating the silicic acid to separate out the silica, and specifically comprises the following steps: mixing different kinds of silicic acid compounds and different organic phases according to a proportion, dripping different kinds of/concentration of acid under the condition of high-speed dispersion for reaction, continuously dispersing for a period of time after precipitating the silicon dioxide microspheres, and obtaining the monodisperse micron-sized amorphous silicon dioxide microspheres with different particle diameters through precipitation, cleaning and drying. Compared with the prior preparation technology, the method for preparing the silicon dioxide has the advantages that: the whole process flow is simple, the one-time balling is low in requirement on equipment, no high-temperature condition is needed, the energy consumption in the preparation process is greatly reduced, the raw materials are cheap and ten times lower than the current commercial raw material ethyl orthosilicate, the recycling of an organic phase can be realized, and the whole preparation process is environment-friendly. The silica microsphere prepared by the invention: the method has the advantages of monodispersion, good sphericity, larger pore volume and specific surface area and high yield; controllable particle size (1-400 μm) and uniform particle size distribution; the pore volume is larger, and the pore diameter distribution is uniform; the method has the excellent characteristics of high strength, high temperature resistance, corrosion resistance, stable chemical property and the like, and has great advantages and application prospects in the aspect of preparation of the silicon dioxide microspheres.
Drawings
FIG. 1 is an optical microscope image of silica microspheres prepared by taking water glass with different moduli as raw materials in examples 1-4;
FIG. 2 is a graph showing the particle size distribution of silica microspheres prepared from water glass of different moduli in examples 1-4;
FIG. 3 is an optical microscope image of silica microspheres prepared from potassium and potassium/sodium water glass as raw materials in examples 5-6;
FIG. 4 is an optical microscopy image of silica microspheres prepared in medium of rapeseed oil, soybean oil, peanut oil and dimethicone according to examples 7-10;
FIG. 5 is an optical microscope image of silica microspheres prepared by dropwise adding carbonic acid, sulfuric acid, hydrochloric acid and hydrochloric acid/sulfuric acid mixture as raw materials in examples 11-14;
FIG. 6 is an optical microscopy image of silica microspheres prepared with the engine oil medium of examples 15-16 after the second and fifth cycles;
FIG. 7 is an X-ray diffraction pattern of silica microspheres prepared under various process parameters for examples 1,2,6 and 10;
FIG. 8 is an optical microscope image of comparative example 1 for silica microspheres prepared with the addition of an emulsifier;
FIG. 9 is a state diagram showing the final phase of the system after completion of the reaction of comparative example 1 and example 1.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1:
(1) Adding 10mL of sodium water glass slurry with the modulus of 2.3 into 500mL of engine oil, uniformly mixing, and dispersing for 40min at the dispersion speed of 500r/min to make the system become uniform slurry;
(2) Dropping 25% acetic acid solution into the slurry of the step (1) with the dispersion speed of 500r/min at the dropping speed of 2 mL/min;
(3) After the acid solution is completely dripped, the engine oil in the step (2) and the obtained product are continuously stirred and dispersed (aged) for 30min at a dispersing speed of 500 r/min;
(4) Filtering the engine oil and the obtained product in the step (3) to obtain silicon dioxide microspheres;
(5) Placing the silicon dioxide microspheres in the step (4) in water, and cleaning the residual engine oil on the surfaces of the microspheres;
(6) Drying the silica microspheres obtained in the step (5) in an oven at 85 ℃ for 48 hours;
As a result of detection, the average particle diameter of the microsphere is 91.28 μm, the specific surface area is 243.83m 2/g, and the pore volume is 0.2675cm 3/g, as shown in FIG. 1 and FIG. 2. The X-ray diffraction pattern is shown in fig. 7.
Example 2:
(1) Adding 10mL of sodium water glass slurry with the modulus of 2.3 into 30mL of engine oil, uniformly mixing, and dispersing for 5min at a dispersing speed of 3000r/min to make the system become uniform slurry;
(2) Dropping 25% acetic acid solution into the slurry of the step (1) with a dispersion speed of 3000r/min at a dropping speed of 2 mL/min;
(3) After the acid solution is completely dripped, the engine oil in the step (2) and the obtained product are continuously stirred and dispersed (aged) for 10min at a dispersing speed of 3000 r/min;
(4) Filtering the engine oil and the obtained product in the step (3) to obtain silicon dioxide microspheres;
(5) Placing the silicon dioxide microspheres in the step (4) in water, and cleaning the residual engine oil on the surfaces of the microspheres;
(6) Drying the silica microspheres obtained in the step (5) in a baking oven at 120 ℃ for 20min;
As a result of detection, the average particle diameter of the microsphere is 83.35 μm, the specific surface area is 234.83m 2/g, and the pore volume is 0.1726cm 3/g, as shown in FIG. 1.
Example 3:
(1) Adding 10mL of sodium water glass slurry with the modulus of 3.3 into 100mL of engine oil, uniformly mixing, and dispersing for 20min at a dispersion speed of 2500r/min to make the system become uniform slurry;
(2) Dripping acetic acid solution with mass fraction of 5% into the slurry of the step (1) with dispersion speed of 2500r/min at a dripping speed of 30 mL/min;
(3) After the acid solution is completely dripped, the engine oil in the step (2) and the obtained product are continuously stirred and dispersed (aged) for 15min at a dispersion speed of 2500 r/min;
(4) Filtering the engine oil and the obtained product in the step (3) to obtain silicon dioxide microspheres;
(5) Placing the silicon dioxide microspheres in the step (4) in water, and cleaning the residual engine oil on the surfaces of the microspheres;
(6) Drying the silica microspheres obtained in the step (5) in a baking oven at 100 ℃ for 50min;
As a result of detection, the average particle diameter of the microspheres is 114.51 μm, the specific surface area is 176.4867m 2/g, and the pore volume is 0.432cm 3/g, as shown in FIG. 1.
Example 4:
(1) Adding 10mL of sodium water glass slurry with the modulus of 3.3 into 100mL of engine oil, uniformly mixing, and dispersing for 20min at a dispersion speed of 2500r/min to make the system become uniform slurry;
(2) Dripping 60% acetic acid solution into the slurry of the step (1) with the dispersion speed of 2500r/min at the dripping speed of 0.5 mL/min;
(3) After the acid solution is completely dripped, the engine oil in the step (2) and the obtained product are continuously stirred and dispersed (aged) for 15min at a dispersion speed of 2500 r/min;
(4) Filtering the engine oil and the obtained product in the step (3) to obtain silicon dioxide microspheres;
(5) Placing the silicon dioxide microspheres in the step (4) in water, and cleaning the residual engine oil on the surfaces of the microspheres;
(6) Drying the silica microspheres obtained in the step (5) in a baking oven at 90 ℃ for 24 hours;
As a result of detection, the average particle diameter of the microsphere is 104.81 μm, the specific surface area is 40.57m 2/g, and the pore volume is 0.2624cm 3/g, as shown in FIG. 1.
Example 5:
(1) Adding 10mL of potash water glass slurry with the modulus of 2.3 into 100mL of engine oil, uniformly mixing, and dispersing for 20min at the dispersion speed of 2500r/min to make the system become uniform slurry;
(2) Dripping acetic acid solution with mass fraction of 5% into the slurry of the step (1) with dispersion speed of 2500r/min at a dripping speed of 2 mL/min;
(3) After the acid solution is completely dripped, the engine oil in the step (2) and the obtained product are continuously stirred and dispersed (aged) for 15min at a dispersion speed of 2500 r/min;
(4) Filtering the engine oil and the obtained product in the step (3) to obtain silicon dioxide microspheres;
(5) Placing the silicon dioxide microspheres in the step (4) in water, and cleaning the residual engine oil on the surfaces of the microspheres;
(6) Drying the silica microspheres obtained in the step (5) in an oven at 85 ℃ for 48 hours;
As shown in the photo of the microsphere optical microscope and the particle size distribution shown in figure 3, the viscosity of the potash water glass is low, the potash water glass is excessively dispersed, and the silicon dioxide agglomeration is serious.
Example 6:
(1) Adding 10mL of potassium/sodium water glass slurry with the modulus of 2.3 into 100mL of engine oil, uniformly mixing, and dispersing for 20min at the dispersion speed of 2500r/min to make the system become uniform slurry;
(2) Dripping acetic acid solution with mass fraction of 5% into the slurry of the step (1) with dispersion speed of 2500r/min at a dripping speed of 2 mL/min;
(3) After the acid solution is completely dripped, the engine oil in the step (2) and the obtained product are continuously stirred and dispersed (aged) for 15min at a dispersion speed of 2500 r/min;
(4) Filtering the engine oil and the obtained product in the step (3) to obtain silicon dioxide microspheres;
(5) Placing the silicon dioxide microspheres in the step (4) in water, and cleaning the residual engine oil on the surfaces of the microspheres;
(6) Drying the silica microspheres obtained in the step (5) in an oven at 85 ℃ for 48 hours;
The detected microsphere optical microscope image is shown in figure 3, and the X-ray diffraction pattern is shown in figure 7.
Example 7:
(1) Adding 10mL of potassium/sodium water glass slurry with the modulus of 2.3 into 100mL of soybean oil, uniformly mixing, and dispersing for 20min at a dispersion speed of 2500r/min to make the system become uniform slurry;
(2) Dripping acetic acid solution with mass fraction of 5% into the slurry of the step (1) with dispersion speed of 2500r/min at a dripping speed of 2 mL/min;
(3) After the acid solution is completely dripped, the soybean oil and the obtained product in the step (2) are continuously stirred and dispersed (aged) for 15min at a dispersion speed of 2500 r/min;
(4) Filtering the soybean oil and the obtained product in the step (3) to obtain silicon dioxide microspheres;
(5) Placing the silica microspheres in the step (4) in water, and cleaning soybean oil remained on the surfaces of the microspheres;
(6) Drying the silica microspheres obtained in the step (5) in an oven at 85 ℃ for 48 hours;
the detected microsphere optical microscopy image is shown in figure 4.
Example 8:
(1) Adding 10mL of potassium/sodium water glass slurry with the modulus of 2.3 into 100mL of peanut oil, uniformly mixing, and dispersing for 20min at a dispersion speed of 2500r/min to make the system become uniform slurry;
(2) Dripping acetic acid solution with mass fraction of 5% into the slurry of the step (1) with dispersion speed of 2500r/min at a dripping speed of 2 mL/min;
(3) After the acid solution is completely dripped, continuously stirring and dispersing (aging) the peanut oil obtained in the step (2) at a dispersing speed of 2500r/min for 15min;
(4) Filtering the soybean oil and the obtained product in the step (3) to obtain silicon dioxide microspheres;
(5) Putting the silicon dioxide microspheres in the step (4) into water, and cleaning residual peanut oil on the surfaces of the microspheres;
(6) Drying the silica microspheres obtained in the step (5) in a baking oven at 110 ℃ for 20min;
the detected microsphere optical microscopy image is shown in figure 4.
Example 9:
(1) Adding 10mL of potassium/sodium water glass slurry with the modulus of 2.3 into 100mL of sunflower seed oil, uniformly mixing, and dispersing for 20min at a dispersion speed of 2500r/min to make the system become uniform slurry;
(2) Dripping acetic acid solution with mass fraction of 5% into the slurry of the step (1) with dispersion speed of 2500r/min at a dripping speed of 2 mL/min;
(3) After the acid solution is completely dripped, the sunflower seed oil in the step (2) and the obtained product are continuously stirred and dispersed (aged) for 15min at a dispersion speed of 2500 r/min;
(4) Filtering the sunflower seed oil and the obtained product in the step (3) to obtain silicon dioxide microspheres;
(5) Putting the silicon dioxide microspheres in the step (4) into water, and cleaning sunflower seed oil remained on the surfaces of the microspheres;
(6) Drying the silica microspheres obtained in the step (5) in an oven at 85 ℃ for 48 hours;
the detected microsphere optical microscopy image is shown in figure 4.
Example 10:
(1) Adding 10mL of potassium/sodium water glass slurry with the modulus of 2.3 into 100mL of methyl silicone oil, uniformly mixing, and dispersing for 20min at the dispersion speed of 2500r/min to make the system become uniform slurry;
(2) Dripping acetic acid solution with mass fraction of 5% into the slurry of the step (1) with dispersion speed of 2500r/min at a dripping speed of 2 mL/min;
(3) After the acid solution is completely dripped, the methyl silicone oil in the step (2) and the obtained product are continuously stirred and dispersed (aged) for 15min at a dispersion speed of 2500 r/min;
(4) Filtering the soybean oil and the obtained product in the step (3) to obtain silicon dioxide microspheres;
(5) Placing the silicon dioxide microspheres in the step (4) in water, and cleaning methyl silicone oil remained on the surfaces of the microspheres;
(6) Drying the silica microspheres obtained in the step (5) in a baking oven at 105 ℃ for 2 hours;
The detected microsphere optical microscope image is shown in fig. 4, and the X-ray diffraction pattern is shown in fig. 7.
Example 11:
(1) Adding 10mL of sodium water glass slurry with the modulus of 2.3 into 30mL of engine oil, uniformly mixing, and dispersing for 5min at a dispersing speed of 3000r/min to make the system become uniform slurry;
(2) Dropping 25% by mass of carbonic acid solution into the slurry of the step (1) with a dispersion speed of 3000r/min at a dropping speed of 2 mL/min;
(3) After the acid solution is completely dripped, the engine oil in the step (2) and the obtained product are continuously stirred and dispersed (aged) for 10min at a dispersing speed of 3000 r/min;
(4) Filtering the engine oil and the obtained product in the step (3) to obtain silicon dioxide microspheres;
(5) Placing the silicon dioxide microspheres in the step (4) in water, and cleaning the residual engine oil on the surfaces of the microspheres;
(6) Drying the silica microspheres obtained in the step (5) in a baking oven at 120 ℃ for 20min;
The photo of the detected microsphere light microscope and particle size distribution is shown in FIG. 5, example 12:
(1) Adding 10mL of sodium water glass slurry with the modulus of 3.3 into 100mL of engine oil, uniformly mixing, and dispersing for 20min at a dispersion speed of 2500r/min to make the system become uniform slurry;
(2) Dropping 25% sulfuric acid solution into the slurry of the step (1) with the dispersion speed of 2500r/min at the dropping speed of 0.5 mL/min;
(3) After the acid solution is completely dripped, the engine oil in the step (2) and the obtained product are continuously stirred and dispersed (aged) for 15min at a dispersion speed of 2500 r/min;
(4) Filtering the engine oil and the obtained product in the step (3) to obtain silicon dioxide microspheres;
(5) Placing the silicon dioxide microspheres in the step (4) in water, and cleaning the residual engine oil on the surfaces of the microspheres;
(6) Drying the silica microspheres obtained in the step (5) in a baking oven at 90 ℃ for 24 hours;
the photo of the detected microsphere light microscope and particle size distribution is shown in FIG. 5, example 13:
(1) Adding 10mL of sodium water glass slurry with the modulus of 2.3 into 500mL of engine oil, uniformly mixing, and dispersing for 40min at the dispersion speed of 500r/min to make the system become uniform slurry;
(2) Dropping 5% hydrochloric acid solution into the slurry of the step (1) with the dispersion speed of 500r/min at the dropping speed of 2 mL/min;
(3) After the acid solution is completely dripped, the engine oil in the step (2) and the obtained product are continuously stirred and dispersed (aged) for 30min at a dispersing speed of 500 r/min;
(4) Filtering the engine oil and the obtained product in the step (3) to obtain silicon dioxide microspheres;
(5) Placing the silicon dioxide microspheres in the step (4) in water, and cleaning the residual engine oil on the surfaces of the microspheres;
(6) Drying the silica microspheres obtained in the step (5) in an oven at 85 ℃ for 48 hours;
The photo of the microsphere light microscope and the particle size distribution is shown in FIG. 5.
Example 14:
(1) Adding 10mL of sodium water glass slurry with the modulus of 3.3 into 100mL of engine oil, uniformly mixing, and dispersing for 20min at a dispersion speed of 2500r/min to make the system become uniform slurry;
(2) Dripping 5% hydrochloric acid/sulfuric acid mixed solution into the slurry of the step (1) with the dispersion speed of 2500r/min at the dripping speed of 2mL/min;
(3) After the acid solution is completely dripped, the engine oil in the step (2) and the obtained product are continuously stirred and dispersed (aged) for 15min at a dispersion speed of 2500 r/min;
(4) Filtering the engine oil and the obtained product in the step (3) to obtain silicon dioxide microspheres;
(5) Placing the silicon dioxide microspheres in the step (4) in water, and cleaning the residual engine oil on the surfaces of the microspheres;
(6) Drying the silica microspheres obtained in the step (5) in an oven at 85 ℃ for 48 hours;
the detected microsphere optical microscopy image is shown in figure 5.
Example 15:
(1) Adding 10mL of sodium water glass slurry with the modulus of 3.3 into 100mL of engine oil (recycled for two times), uniformly mixing, and dispersing for 20min at a dispersion speed of 2500r/min to make the system uniform;
(2) Dripping acetic acid solution with mass fraction of 5% into the slurry of the step (1) with dispersion speed of 2500r/min at a dripping speed of 30 mL/min;
(3) After the acid solution is completely dripped, the engine oil in the step (2) and the obtained product are continuously stirred and dispersed (aged) for 15min at a dispersion speed of 2500 r/min;
(4) Filtering the engine oil and the obtained product in the step (3) to obtain silicon dioxide microspheres;
(5) Placing the silicon dioxide microspheres in the step (4) in water, and cleaning the residual engine oil on the surfaces of the microspheres;
(6) Drying the silica microspheres obtained in the step (5) in a baking oven at 100 ℃ for 50min;
The optical microscope and particle size distribution photograph of the microspheres prepared by the oil medium after the second circulation are shown in fig. 6.
Example 16:
(1) Adding 10mL of sodium water glass slurry with the modulus of 3.3 into 100mL of engine oil (recycled five times), uniformly mixing, and dispersing for 20min at a dispersion speed of 2500r/min to make the system uniform;
(2) Dripping acetic acid solution with mass fraction of 5% into the slurry of the step (1) with dispersion speed of 2500r/min at a dripping speed of 30 mL/min;
(3) After the acid solution is completely dripped, the engine oil in the step (2) and the obtained product are continuously stirred and dispersed (aged) for 15min at a dispersion speed of 2500 r/min;
(4) Filtering the engine oil and the obtained product in the step (3) to obtain silicon dioxide microspheres;
(5) Placing the silicon dioxide microspheres in the step (4) in water, and cleaning the residual engine oil on the surfaces of the microspheres;
(6) Drying the silica microspheres obtained in the step (5) in a baking oven at 100 ℃ for 50min;
The photo of the microsphere optical microscope and the particle size distribution prepared by the engine oil medium after the fifth cycle is detected as shown in fig. 6.
Comparative example 1
(1) Adding 10mL of sodium water glass slurry with the modulus of 2.3 into 500mL of engine oil, uniformly mixing, and dispersing for 40min at the dispersion speed of 500r/min to make the system become uniform slurry;
(2) Adding 5g of sorbitan fatty acid ester (span-80) into the slurry in the step (1) and continuing to disperse for 10min;
(3) Dropping 25% acetic acid solution into the slurry of the step (2) with the dispersion speed of 500r/min at the dropping speed of 2 mL/min;
(4) After the acid solution is completely dripped, the engine oil in the step (3) and the obtained product are continuously stirred and dispersed (aged) for 30min at a dispersing speed of 500 r/min;
(5) Filtering the engine oil and the obtained product in the step (4) to obtain silicon dioxide microspheres;
(6) Placing the silica microspheres in the step (5) in water, and cleaning the residual engine oil on the surfaces of the microspheres;
(7) Drying the silica microspheres obtained in the step (6) in an oven at 85 ℃ for 48 hours;
Using the experimental conditions of example 1, the emulsifier (span-80) was added without changing the other variables. Comparing the two experiments, as shown in fig. 8, the emulsifier aggravates the degree of microsphere agglomeration, forming spherical clusters. In addition, the yield of silica microspheres in the w/o system was only 53%, whereas the yield in example 1 was 86%. After the addition of the emulsifier, the final phase is an emulsion as shown in comparative example 1 in fig. 9; in the case of no emulsifier, as shown in example 1 of fig. 9, the aqueous phase and the organic phase can be separated and reused, and the production of silica microspheres can be realized after repeated cycling experiments.
In summary, aiming at the problems of the existing precipitation method that water glass is used as a raw material to generate silica microspheres, the application develops a method for preparing micron-sized amorphous silica microspheres by using water glass as a raw material, and the method utilizes the characteristics that the water glass reacts under an acidic condition to generate silicic acid, and the silicic acid supersaturates to separate out the silica, and specifically comprises the following steps: firstly, water glass and an organic phase are stirred according to a certain proportion and are dispersed uniformly at a high speed to form a reaction precursor solution. Then, dropwise adding an acidic solution into the solution under high-speed stirring to react and separate out silica microspheres; and finally, precipitating, washing and drying to obtain the micron-sized silica microspheres. Compared with the prior preparation technology, the method for preparing the silicon dioxide has the advantages that: the whole process flow is simple, the one-time balling is low in requirement on equipment, no high-temperature condition is needed, the energy consumption in the preparation process is greatly reduced, the raw materials are cheaper, the raw materials are ten times lower than the current commercial raw material ethyl orthosilicate, the recycling of solid wastes (the organic phase can be recycled), and the whole preparation process is environment-friendly. In addition, silica microspheres prepared according to the present application: the method has the advantages of monodispersion, good sphericity, larger pore volume and specific surface area and high yield; controllable particle size (5-300 μm) and uniform particle size distribution; the pore volume is larger, and the pore diameter distribution is uniform; the method has the excellent characteristics of high strength, high temperature resistance, corrosion resistance, stable chemical property and the like, and has great advantages and application prospects in the aspect of preparation of the silicon dioxide microspheres.
Although the present invention has been described with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described, or equivalents may be substituted for elements thereof, and any modifications, equivalents, improvements and changes may be made without departing from the spirit and principles of the present invention.
Claims (10)
1. The method for efficiently preparing the micron-sized silicon dioxide microspheres by using water glass through reversed-phase suspension dispersion is characterized by comprising the following steps of:
s1, mixing liquid water glass and an organic phase according to a certain proportion, and dispersing and ageing at a high speed to form a reaction precursor;
s2: dropwise adding an acidic solution into the precursor dispersed in the high-speed stirring;
S3: continuing dispersing and aging for a period of time after the silica microspheres are separated out;
s4: and precipitating, washing and drying to obtain the monodisperse micron-sized silica microspheres.
2. The method for efficiently preparing micron-sized silica microspheres by inverse suspension dispersion using water glass according to claim 1, wherein the method comprises the following steps: the liquid water glass in the step S1 comprises sodium water glass Na 2O·nSiO2, potassium water glass K 2O·nSiO2 and/or potassium/sodium water glass (K/Na) 2O·nSiO2 with different moduli n, wherein the range of the different moduli n is 2.3-3.3.
3. The method for efficiently preparing micron-sized silica microspheres by inverse suspension dispersion using water glass according to claim 1, wherein the method comprises the following steps: the organic phase in the step S1 is a mixed liquid of fat or mineral hydrocarbon contained in animals and plants, and comprises one or a mixture of more of engine oil, silicone oil, vacuum pump oil, petroleum, gasoline, kerosene, peanut oil, soybean oil or sunflower seed oil.
4. The method for efficiently preparing micron-sized silica microspheres by inverse suspension dispersion using water glass according to claim 1, wherein the method comprises the following steps: in the step S1, the volume ratio of the liquid water glass to the organic phase is 1:1 to 200.
5. The method for efficiently preparing micron-sized silica microspheres by inverse suspension dispersion using water glass according to claim 1, wherein the method comprises the following steps: the dispersion speed in the step S1 is 100-5000 r/min, and the aging time is 1-60 min.
6. The method for efficiently preparing micron-sized silica microspheres by inverse suspension dispersion using water glass according to claim 1, wherein the method comprises the following steps: the mass percentage concentration of the acidic liquid in the step S2 is 1% to the pure solvent, and the dripping speed is 0.05-100 mL min -1; the acidic liquid is acetic acid, citric acid, malic acid, formic acid, acetic acid propionic acid, carbonic acid, sulfuric acid, hydrochloric acid, phosphoric acid, ammonium chloride or ethyl acetate.
7. The method for efficiently preparing micron-sized silica microspheres by inverse suspension dispersion using water glass according to claim 1, wherein the method comprises the following steps: the dispersion speed in the step S3 is 100-5000 r/min, and the dispersion time is 1-60 min.
8. The method for efficiently preparing micron-sized silica microspheres by inverse suspension dispersion using water glass according to claim 1, wherein the method comprises the following steps: the drying temperature in the step S4 is 20-200 ℃ and the drying time is 20 min-72 h.
9. The method for efficiently preparing micron-sized silica microspheres by inverse suspension dispersion using water glass according to claim 1, wherein the method comprises the following steps: the particle size of the monodisperse micron-sized amorphous silica microsphere is 1-500 mu m, the specific surface area is 5-800 m 2/g, and the pore volume is 0.17-0.43 cm 3/g.
10. The method for efficiently preparing micron-sized silica microspheres by inverse suspension dispersion using water glass according to claim 1, wherein the method comprises the following steps: in the method for preparing the micron-sized silica microspheres, the organic phase can be recycled without using an emulsifying agent, and the prepared monodisperse micron-sized amorphous silica microspheres have the particle size of 1-500 mu m, the specific surface area of 5-800 m 2/g and the pore volume of 0.17-0.43 cm 3/g after being recycled for 30-50 times.
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