WO2021165884A1 - Procédé de production de nano-silice - Google Patents

Procédé de production de nano-silice Download PDF

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Publication number
WO2021165884A1
WO2021165884A1 PCT/IB2021/051401 IB2021051401W WO2021165884A1 WO 2021165884 A1 WO2021165884 A1 WO 2021165884A1 IB 2021051401 W IB2021051401 W IB 2021051401W WO 2021165884 A1 WO2021165884 A1 WO 2021165884A1
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WO
WIPO (PCT)
Prior art keywords
solution
range
cake
silica
nano
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PCT/IB2021/051401
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English (en)
Inventor
Karim ONIY AGHMIUNI
Taher RAHIMI AGHDAM
Omid KARBALAEE
Original Assignee
Oniy Aghmiuni Karim
Rahimi Aghdam Taher
Karbalaee Omid
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Application filed by Oniy Aghmiuni Karim, Rahimi Aghdam Taher, Karbalaee Omid filed Critical Oniy Aghmiuni Karim
Publication of WO2021165884A1 publication Critical patent/WO2021165884A1/fr

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    • 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
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/34—Silicon-containing compounds
    • C08K3/36—Silica
    • 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
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/002—Physical properties
    • C08K2201/006—Additives being defined by their surface area
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives

Definitions

  • the present subject matter is, in general, related to production of chemical materials, and more particularly, but not exclusively, to a method for producing of a participated nano-silica with a particle size less than 100 nm.
  • Precipitated nano-silica is one of the most used nanoparticles in many industries such as tire and rubber industries, toothpaste, paints and coatings, cement and concrete, cosmetics, plastics, papers, food industries, and construction.
  • industries such as tire and rubber industries, toothpaste, paints and coatings, cement and concrete, cosmetics, plastics, papers, food industries, and construction.
  • the most rapidly growing usage of the participated silica is for the plastic market, especially the tire industry due to the decrease in the application of carbon black and the development of green tires in the automobile industries of the world.
  • silica-filled compounds are used widely
  • Precipitated silica has been used for a long time as a reinforcing filler in different elastomers.
  • the reinforcing filler needs to be distributed well throughout the polymer matrix to achieve the properties suitable for the elastomeric matrix.
  • one of the fundamental problems associated with this kind of fillers is the ability to distribute favorably in elastomeric matrices.
  • Another problem associated with producing a nanostructure of this kind of fillers is obtaining an utterly uniform structure with a particle size less than 100 nm as well as mesoporous pores.
  • the present disclosure is directed to an exemplary method for producing of a participated nano-silica.
  • the exemplary method may comprise preparing a first solution comprising at least one precursor of silicon and water, preparing a second solution comprising at least one acid and water, mixing the first solution and the second solution in at least three steps such that a slurry may obtain, filtering the slurry to remove a salt residual and obtain a cake of silicone, drying the cake of silicon to obtain a dried silicate cake, and disintegrating the dried silicate cake to obtain the participated nano-silica.
  • the precursor of silicon may comprise any type of silicate salt.
  • the precursor of silicon may comprise a mixture of at least two silicate salts.
  • the acid may comprise at least one organic acid, at least one inorganic acid, or a mixture thereof.
  • the three steps of mixing may comprise mixing the first solution and the second solution in any order such that a pH value of a mixed solution may be adjusted in a range of 9 to 12, adding the first solution and the second solution in any order such that the pH value of the mixed solution may be adjusted in a range of 7 to 10, and adding the second solution such that the pH value may be adjusted in a range of 4 to 6. In an exemplary implementation.
  • the three steps of the mixing may be performed in a temperature in a range of 40-90 °C.
  • drying the cake may be performed utilizing a spin flash drier, a rotary drum drier, an atomizer, or a fluid bed drier.
  • mixing of the first and the second solution may be performed in a continuous condition, a semi- continuous condition, or a discontinuous condition.
  • the participated nano-silica may comprise a plurality of specific properties.
  • the specific properties may include BET specific surface area in a range of 50-350 m 2 .g -1 , CTAB specific surface area in a range of 50-300 m 2 .g -1 , a particle size in a range of 10-100 nm, an agglomerate size in a range of 1-100 ⁇ m, a minimum pore size of 15 nm, and a minimum pore volume of 1.2 cm 3 .g -1 .
  • disintegrating the dried silicate cake may be performed utilizing a grinding device, a granulation device, or a combination thereof.
  • the present disclosure is directed to an exemplary method for producing of a participated nano-silica.
  • the exemplary method may comprise preparing a first solution comprising at least one precursor of silicon and water, preparing a second solution comprising at least one acid and water, mixing the first solution and the second solution in at least three steps to obtain a slurry, such that the three steps may comprise mixing the first solution and the second solution in any order such that a pH value of a mixed solution may be adjusted in a range of 9 to 12, adding the first solution and the second solution in any order such that the pH value of the mixed solution may be adjusted in a range of 7 to 10, and adding the second solution such that the pH value may be adjusted in a range of 4 to 6, and the three steps may be performed in a temperature in a range of 40 to 90 °C, obtaining a cake of silicon utilizing a filtering step of the slurry.
  • the exemplary method may further comprise drying the cake of silicon to obtain a dried silicate cake, and disintegrating the dried silicate cake to obtain the participated nano-
  • the precursor of silicon may comprise at least one silicate salt, a mixture thereof, or any type of silicate salt.
  • the acid may comprise at least one organic acid, at least one inorganic acid, or a mixture thereof.
  • drying the cake may be performed utilizing a spin flash drier, a rotary drum drier, an atomizer, or a fluid bed drier.
  • mixing of the first and the second solutions may be performed in a continuous condition, a semi- continuous condition, or a discontinuous condition.
  • the participated nano-silica may comprise a plurality of specific properties.
  • the specific properties may include BET specific surface area in a range of 50-350 m 2 .g -1 , CTAB specific surface area in a range of 50-300 m 2 .g -1 , a particle size in a range of 10-100 nm, an agglomerate size in a range of 1-100 ⁇ m, a minimum pore size of 15 nm, and a minimum pore volume of 1.2 cm 3 .g -1 .
  • disintegrating the dried silicate cake may be performed utilizing a grinding device, a granulation device, or a combination thereof.
  • FIG. 1 illustrates a flowchart of an exemplary method for producing of a participated nano-silica, consistent with one or more exemplary embodiments of the present disclosure.
  • FIG. 1 illustrates a flowchart of an exemplary three steps of mixing, consistent with one or more exemplary embodiments of the present disclosure.
  • FIG. 1 illustrates an X-ray pattern of a participated nano-silica, consistent with one or more exemplary embodiments of the present disclosure.
  • FIG. 1 illustrates FESEM images of a participated nano-silica in two different magnifications, consistent with one or more exemplary embodiments of the present disclosure.
  • the exemplary method 100 may comprise preparation of a first solution that may comprise at least one precursor of silicon 102, preparation of a second solution that may comprise at least on acid 104.
  • the exemplary method 100 may further comprise mixing the first aquas solution and the second aquas solution in at least three steps to obtain a slurry 106.
  • the exemplary method may comprise filtering the slurry such that may remove a salt residual and obtain a cake of silicon 108.
  • the exemplary method 100 may further comprise drying the cake of silicon to obtain a dried silicate cake 110 and disintegrating the dried silicate cake to obtain the participated nano-silica 112.
  • the first solution may comprise any type of silicate salt, for example, but not limited to, sodium silicate, potassium silicate.
  • the first solution may comprise a mixture of at least two precursors of silicon.
  • the precursor of silicon may comprise at least one silicate salt.
  • the precursor of silicon may comprise any kinds of silicon compound that are well known for those skilled in the art.
  • a concentration of the precursor in the first solution may be in a range of 2% to 10% by weight. In an exemplary embodiment, the concentration of the precursor in the first solution may be at least 4% by weigh.
  • the acid of the second solution may comprise at least one organic acid, for example, but not limited to, acetic acid, citric acid, oxalic acid and other inorganic acids that are well known for those skilled in the art.
  • the acid may comprise at least one inorganic acid, for example, but not limited to sulfuric acid, hydrochloric acid, nitric acid, and other inorganic acids that are well known for those skilled in the art.
  • the second solution may comprise a mixture of at least two acids.
  • the at least two acids may comprise at least two organic acids, at least two inorganic acids, and/or a combination thereof.
  • the second solution may comprise a mixture of at least one organic acid and at least one inorganic acid.
  • a concentration of the acid in the second solution may be in a range of 2% to 30% by mass. In an exemplary embodiment, the concentration of the acid in the second solution may be at least 2% by mass.
  • the three steps 200 may comprise mixing the first solution and the second solution in any order such that a pH value of a mixed solution may be adjusted in a range of 9 to 12 (202), adding the first solution and the second solution in any order such that the pH value of the mixed solution may be adjusted in a range of 7 to 10 (204), and adding the second solution such that the pH value may be adjusted in a range of 4 to 6 (206).
  • the three steps 200 of mixing the first and the second solution 106 may be performed utilizing at least one reactor.
  • the 202 , 204 and 206 steps may be done in a semi-continuous condition and/or a discontinuous condition.
  • the three steps 200 of mixing the first and the second solution 106 may be performed utilizing at least three reactors such that the reactors may be provided a continuous condition to progress mixing the first and second solutions 106 .
  • the reactors may operate in the semi-continuous condition and/or the discontinuous condition.
  • the first solution and the second solution may be added into the reactors in any order or simultaneously in both steps 202 and 204 .
  • the reactors may comprise at least one agitator such that the agitator may be configured to stirrer the first and the second solution to obtain the mixed solution, introduce the mixed solution as well as creating a backflow.
  • the agitator may comprise an axial agitator and/or a radial agitator.
  • the agitator may comprise a jet rotary agitator.
  • the reactor may comprise at least one axial or radial agitator and the rotary jet agitator.
  • the reactor may comprise a turbine agitator, an anchor agitator, a propeller agitator, a blade agitator, a universal agitator, and/or other agitators that are well known for those skilled in the art.
  • the slurry resulted from step 10 8 may comprise at least 2% by weigh of dispersed silica in water.
  • the slurry may be filtered utilizing a separation process such as, but not limited to, filter press, rotary vacuum, drum filter, and other processes that are well known for those skilled in the art, to remove at least one impurity and obtain the cake of silicone.
  • the impurity may comprise any residual precursors of silicon such as any unreacted silicate salts, any formed salts during the mixing and reaction of the first and the second solutions.
  • the step 108 may be performed at least two times.
  • the obtained cake of silicon may be dispersed again into water and a pH value of a prepared suspension may be adjusted in a range of 6 to 7 utilizing a third solution and the prepared suspension may be filtered.
  • the third solution may comprise at least one alkali and water.
  • a concentration of the silicon in the cake of silicon may be in a range of 15% to 22% by weight. In an exemplary embodiment, the concentration of the silicon in the cake of silicon may be at least 15% by weight.
  • the cake of silicon may be dried to obtain the dried silicate cake (step 110 ) utilizing a drier apparatus.
  • the drier apparatus may comprise a spin flash drier, a rotary drum drier, an atomizer, a fluid bed drier, and/or other drier apparatuses that are well known for those skilled in the art.
  • the step 110 may be performed in a temperature in a range of 150 to 450 °C.
  • the dried silicate cake may contain a concentration of moisture less than 10% by weight.
  • the dried silicate cake may be disintegrated (step 112 ) utilizing a grinding device, a granulation device, or a combination thereof such that the participated nano-silica may be obtained.
  • the participated nano-silica may comprise a plurality of specific properties.
  • the specific properties may comprise BET specific surface area in a range of 50-350 m 2 .g -1 , CTAB specific surface area in a range of 50-300 m 2 .g -1 , a particle size in a range of 10-100 nm, an agglomerate size in a range of 1-100 ⁇ m, a minimum pore size of 15 nm, and a minimum pore volume of 1.2 cm 3 .g -1 .
  • a silicate compound that contain a silicate concentration about 5% by weigh and 50-liters water was mixed to prepared a first solution (step 102).
  • a second solution was prepared such that the second solution contain a concentration of an acid about 2% by mass (step 104).
  • first step of adding the solutions to the reactor step 202
  • 80 liters of the first solution and 20 liters of the second solution were added into the reactor at a temperature of 60 °C and a first mixed solution was obtained.
  • a pH value of the first mixed solution was adjusted in a range of 10-11.
  • step 204 the first solution and the second solution were added to the first mixed solution to obtain a second mixed solution such that the pH value of the second mixed solution was adjusted in a range of 8-9.
  • the pH value of the second mixed solution was adjusted around 5 by adding the second solution to the reactor in the third step of adding (step 206) such that a slurry was obtained (step 106).
  • the slurry that contain a plurality of silicate particles was filtered and washed to remove existing impurities such as residual silicate salts or silicates compound, and/or unreacted acid and a cake of silicon was obtained (step108).
  • step 110 the dried silicate cake was grinded utilizing a mill and characterization tests was caried out.
  • a surface morphology of the produced participated nano-silica was investigated utilizing FESEM. illustrates two FESEM images of the participated nano-silica in two different magnifications. As illustrated in , the participated nano silica particles have a particle size less than 100 nm.
  • EDS Energy-dispersive X-ray spectroscopy
  • EDS and element mapping were applied to investigate composition elements and distribution pattern of the elements, respectively.
  • the results of the EDS and element mapping are illustrated in and , respectively.
  • the results show that the produced participated nano-silica was mainly composed of silicon, oxygen, and the elements such as aluminum, sodium, and sulfur are existing weight percent less than 2% weight.

Abstract

L'invention concerne un procédé de production d'une nano-silice participante. Le procédé comprend au moins six étapes comprenant la préparation d'une première solution, la préparation d'une deuxième solution de sorte que la première solution comprend au moins un précurseur de silicium et la deuxième solution comprend au moins un acide, le mélange de la première et de la deuxième solution dans au moins un réacteur en au moins trois étapes afin d'obtenir une suspension, la filtration de la suspension pour obtenir un gâteau, le séchage du gâteau pour obtenir un gâteau de silicate séché, et la désintégration du gâteau séché pour obtenir la nano-silice participante. La nano-silice participante produite a une taille de particule inférieure à 100 nm.
PCT/IB2021/051401 2020-02-19 2021-02-18 Procédé de production de nano-silice WO2021165884A1 (fr)

Applications Claiming Priority (2)

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IR13983010820 2020-02-19
IR139850140003010810 2020-02-19

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150299501A1 (en) * 2013-08-08 2015-10-22 Boe Technology Group Co., Ltd. Modified nano-silica and method for preparing the same, pigment dispersion and photosensitive resin composition
US20170294647A1 (en) * 2013-07-26 2017-10-12 Nanotek Instruments, Inc. Methods for Mass-Producing Silicon Nano Powder and Graphene-Doped Silicon Nano Powder

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20170294647A1 (en) * 2013-07-26 2017-10-12 Nanotek Instruments, Inc. Methods for Mass-Producing Silicon Nano Powder and Graphene-Doped Silicon Nano Powder
US20150299501A1 (en) * 2013-08-08 2015-10-22 Boe Technology Group Co., Ltd. Modified nano-silica and method for preparing the same, pigment dispersion and photosensitive resin composition

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