WO2023163169A1 - Méthode de concentration de sol de silice par ultrafiltration - Google Patents

Méthode de concentration de sol de silice par ultrafiltration Download PDF

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Publication number
WO2023163169A1
WO2023163169A1 PCT/JP2023/007039 JP2023007039W WO2023163169A1 WO 2023163169 A1 WO2023163169 A1 WO 2023163169A1 JP 2023007039 W JP2023007039 W JP 2023007039W WO 2023163169 A1 WO2023163169 A1 WO 2023163169A1
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silica sol
concentration
silica
requirement
sol
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PCT/JP2023/007039
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English (en)
Japanese (ja)
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透 西村
滋 三井
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日産化学株式会社
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Publication of WO2023163169A1 publication Critical patent/WO2023163169A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14—Ultrafiltration; Microfiltration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14—Ultrafiltration; Microfiltration
    • B01D61/16—Feed pretreatment
    • 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
    • C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
    • C01B33/141—Preparation of hydrosols or aqueous dispersions
    • 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

Definitions

  • the present invention relates to a silica sol concentration method using an ultrafiltration method.
  • a sol in which colloidal silica particles are dispersed in an aqueous medium can be obtained by heating an aqueous silicic acid solution obtained by removing sodium ions from an aqueous sodium silicate solution as a raw material, or by hydrolyzing an alkoxysilane.
  • Silica sol immediately after production is generally a liquid with a low concentration of silica components, but it is commercialized by concentrating it.
  • concentration is performed by ultrafiltration or an evaporation method. In the method of concentrating the silica component in the silica sol by ultrafiltration, the concentration of the silica component in the silica sol is increased by removing water out of the system through an ultrafiltration membrane.
  • a concentration method by ultrafiltration for example, after heating a zirconium salt aqueous solution in the presence of urea to obtain a transparent zirconia sol, a chelating agent and a metal compound other than zirconium are blended, and the temperature is 80 ° C. or less.
  • a method of concentrating with an ultrafiltration membrane is disclosed (see Patent Document 1). Also, when producing a colloidal silica concentrate from a geothermal fluid containing silica, silica colloidal growth is initiated by cooling from the initial temperature to the nucleation temperature, and the fluid containing silica particles is subjected to ultrafiltration to obtain a silica concentrate.
  • a method is disclosed.
  • Ultrafiltration can be used to concentrate the silica particles in the silica sol, but when the filtrate is removed from the system, the ultrafiltration membrane has a high-concentration silica layer called a cake layer on the inner surface of the ultrafiltration membrane. Deposits of particles may form.
  • the coarse silica particles contained in the cake layer drop out into the silica sol when the silica sol is circulated in the ultrafiltration device to increase the concentration of silica particles, and are mixed into the final product (concentrated silica sol product).
  • concentration silica sol product Concentrated silica sol product
  • An object of the present invention is to provide a method for concentrating silica sol that can prevent
  • the present inventors found that the following requirement A and requirement B are satisfied in the concentration step of increasing the concentration of silica particles contained in the silica sol using an ultrafiltration device.
  • the flow velocity of the silica sol liquid near the ultrafiltration membrane By increasing the flow velocity of the silica sol liquid near the ultrafiltration membrane and creating a situation in which silica particles are less likely to aggregate, it is possible to prevent the formation of aggregated silica particles in the concentrated silica sol.
  • a method for concentrating silica sol was discovered, and the present invention was completed.
  • a first aspect of the present invention is a method for concentrating a sol (silica sol) in which silica particles are dispersed as dispersoid particles in a dispersion medium, wherein the concentration of silica particles contained in the silica sol is increased by an ultrafiltration device. It relates to a method for concentrating a silica sol, characterized in that the following requirements A and B are satisfied in the concentration process.
  • Requirement A The liquid temperature of the silica sol immediately before being injected into the ultrafiltration device must be in the range of 0 to 45°C.
  • Requirement B By circulating the silica sol through the ultrafiltration device, the concentration of silica particles contained in the silica sol after the concentration step should be higher than before the concentration step.
  • Requirement B includes further injecting silica sol into the ultrafiltration device during or after the concentration step of circulating silica sol in the ultrafiltration device, and the injected silica sol is concentrated It relates to the method for concentrating silica sol according to the first aspect, wherein the concentration is 0.1 to 30 times the concentration of silica particles contained in the silica sol before the step.
  • the liquid temperature of the silica sol immediately before being injected into the ultrafiltration device is adjusted to a range of 0 to 30 ° C. It relates to a method for concentrating the described silica sol.
  • the ultrafiltration device is further injected with silica sol having the same concentration as the silica sol before the concentration step, or the silica sol with a higher concentration than the silica sol before the concentration step is circulated through the ultrafiltration device.
  • the silica sol concentration method according to the second aspect is characterized in that the concentration of silica particles contained in the silica sol after the concentration step is higher than that before the concentration step.
  • the concentrated silica sol is directly passed through a pipe from the ultrafiltration device after the concentration step, and filled into a concentrated silica sol filling container under conditions where the concentration of silica particles decreases within 5% by mass.
  • the method for concentrating silica sol according to any one of the first to fourth aspects characterized by:
  • the concentration step is performed in a concentration ratio range of 2 to 30 in which the concentration of the silica particles after the concentration step is in the range of 2 to 30 with respect to the concentration of the silica particles before the concentration step. It relates to the silica sol concentration method according to any one of the 1st to 5th aspects.
  • the silica sol before being injected into the ultrafiltration device is a silica sol containing silica particles obtained by heating an aqueous silicic acid solution obtained by removing alkali metal ions from an aqueous alkali silicate solution. It relates to the method for concentrating silica sol according to any one of the first to sixth aspects, characterized by:
  • the method of the present invention prevents the formation of agglomerated silica particles in the concentrated silica sol in performing concentration for increasing the concentration of the silica component in the silica sol by ultrafiltration, while removing the silica sol.
  • concentration for increasing the concentration of the silica component in the silica sol by ultrafiltration, while removing the silica sol.
  • the effect of being able to concentrate is exhibited.
  • the present invention is a method for concentrating a sol (silica sol) dispersed in water using silica particles as dispersoid particles as a dispersion medium, comprising a concentration step of increasing the concentration of silica particles contained in the silica sol using an ultrafiltration device.
  • a silica sol concentration method characterized in that the following requirements A and B are satisfied in the concentration step.
  • Requirement A The liquid temperature of the silica sol immediately before injection into the ultrafiltration device should be in the range of 0 to 45°C, preferably 0 to 40°C, more preferably 0 to 35°C, and most preferably 0 to 30°C.
  • Requirement B By circulating the silica sol through the ultrafiltration device, the concentration of silica particles contained in the silica sol after the concentration step should be higher than before the concentration step.
  • the present invention will be described in detail below.
  • an ultrafiltration membrane for example, an ultrafiltration membrane (UF membrane) is formed into a tube, silica sol to be concentrated circulates inside the tube, and an aqueous medium is discharged outside the tube.
  • a silica sol having a structure in which the silica component of the silica sol is concentrated can be used.
  • the main component of the aqueous medium is water, cations and anions contained in the silica sol may be discharged at the same time.
  • a cross-flow system is preferable for the ultrafiltration membrane, and by forming a flow parallel to the surface of the ultrafiltration membrane, the phenomenon of suspended solids and colloidal silica particles in the silica sol being deposited on the surface of the ultrafiltration membrane is suppressed. while increasing the silica component concentration in the silica sol.
  • ultrafiltration membranes examples include polyethylene, polyethylene fluoride, polyvinylidene fluoride, polypropylene, cellulose acetate, polyacrylonitrile, polyimide, polysulfone, and polyethersulfone. Also, aluminum oxide, zirconium oxide, titanium oxide, stainless steel, glass, or the like can be used alone or in combination with the above materials for the film material.
  • the ultrafiltration membrane module for example, it is possible to use a casing housing method, in which a membrane element formed by integrating members such as an ultrafiltration membrane, its support, and a channel material is housed in a casing. Then, silica sol is forced into the casing by a pump to filter the aqueous medium and concentrate the colloidal silica component to obtain a concentrated silica sol product.
  • the molecular weight cutoff of the ultrafiltration membrane is, for example, the nominal pore diameter of the membrane is about 5 nm to 100 nm, the suitable particle diameter is, for example, 5 nm to 500 nm, and the molecular weight cut off is, for example, 50 k (5 10,000), 100k (100,000), 300k (300,000), and 500k (500,000) can be used.
  • the molecular weight cutoff is 50,000
  • the nominal pore size of the membrane is 5 nm and the suitable particle size is 15 to 30 nm.
  • the nominal pore size of the membrane is 10 nm and the suitable particle size is 30 to 90 nm.
  • the nominal pore size of the membrane is 35 nm and the suitable particle size is 90 to 200 nm.
  • the molecular weight cutoff is 1 million, the nominal pore size of the membrane is 100 nm and the suitable particle size is 300-600 nm.
  • Delivery of the silica sol to the UF device is, for example, 0.01 to 10 MPa, or 0.05 to 5.0 MPa, or 0.1 to 1.0 MPa. It can be performed at a pressure of 0 MPa, or 0.3 to 1.0 MPa.
  • the time required to concentrate the silica sol to obtain the desired silica concentration is about 0.1 to 50 hours.
  • Requirement A is based on the condition that the liquid temperature of the silica sol immediately before being injected into the ultrafiltration device is in the range of 0 to 45°C.
  • the liquid temperature of the silica sol is, for example, 0 to 45°C, 0 to 40°C, 0 to 35°C, or 0 to 30°C.
  • Requirement A is based on the condition that the liquid temperature of the silica sol immediately before being injected into the ultrafiltration device is in the range of 0 to 45 ° C. If the liquid temperature of the silica sol is higher than this temperature, it is cooled. Therefore, it is preferable to adjust the liquid temperature within this range.
  • For cooling it is preferable to deposit the ultrafiltration membrane module in a tank in which cooling water is circulated and cool the silica sol to a predetermined temperature.
  • the temperature immediately before injection into the ultrafiltration membrane module is 0 to 45°C, or 0 to 40°C, or 0 to 35°C. , or 0 to 30 ° C., or 0 to 25 ° C., or 0 to 15 ° C., and is again injected from the ultrafiltration membrane module through temperature adjustment (for example, cooling) to the above temperature range. preferably.
  • Requirement B is a condition that the concentration of silica particles contained in the silica sol after the concentration process is higher than before the concentration process by circulating the silica sol in the ultrafiltration device.
  • circulation means, for example, once recovering silica sol that has been injected into an ultrafiltration device and has undergone a concentration step, and then injecting it into the ultrafiltration device again.
  • concentration step means, for example, once recovering silica sol that has been injected into an ultrafiltration device and has undergone a concentration step, and then injecting it into the ultrafiltration device again.
  • forming is meant repeating the concentration step without recovering the silica sol, and is also meant to include combinations thereof.
  • circulating the silica sol in the ultrafiltration device can prevent the cake layer from falling off. That is, by circulating the silica sol having a low silica concentration, it is possible to prevent the cake layer from being dissolved in the low-concentration portion. Then, it is preferable to circulate a silica sol having a higher concentration than the silica sol before concentration.
  • silica sol can be further injected into the silica sol circulating in the ultrafiltration membrane module during or after the concentration process.
  • the injected silica sol preferably has a concentration of 0.1 to 30 times the concentration of silica particles contained in the silica sol before the concentration step.
  • silica sol is more concentrated than before the concentration step, but further injection of silica sol is preferably performed with silica sol having the same concentration as the silica sol before the concentration step. It is preferably carried out at a higher concentration than the silica sol before concentration.
  • the concentrated silica sol When the concentrated silica sol is taken out from the ultrafiltration device as a final product, if low-concentration silica sol or water is used as the carrying-out solvent, the concentration of the concentrated silica sol is temporarily lowered due to the carrying-out solvent, resulting in a cake layer. is dropped into the silica sol product by the transported solvent, which causes coarse particles. Therefore, the concentrated silica sol is packed (filled into a container filled with concentrated silica sol) as a concentrated silica sol product under the condition that the silica concentration decreases by 5% by mass or less upon completion of concentration through a direct pipe from the ultrafiltration device. preferably.
  • these operations are carried out through a pipe directly from the ultrafiltration device when the final product of silica sol is obtained, under the condition that the silica concentration decreases within 5% by mass when the concentration is completed, for example in the range of 0 to 5% by mass. It is desirable that the concentrated silica sol product be packed (filled in a container filled with concentrated silica sol) under the above conditions, preferably without causing a decrease in silica concentration.
  • the silica sol concentration step is preferably carried out in a concentration ratio range of 2 to 30 for the concentration of the silica particles after the concentration step to the concentration of the silica particles before the concentration step.
  • the silica sol concentration method of the present invention is characterized by little change in concentration of ionic components (cations and anions) contained in the silica sol before and after the concentration process.
  • cations e.g., cations containing potassium ions, typically potassium ions
  • anions e.g., anions containing sulfate ions, typically is a sulfate ion.
  • the ionic component imparts an electric charge to the surface of the silica particles in the silica sol and forms an appropriate repulsive force of the silica particles to prevent aggregation of the silica particles. can be done.
  • the presence of a large amount of ionic components also leads to agglomeration of silica particles.
  • the concentrations of cations and anions in these silica sols change little by ultrafiltration. For example, it is preferable to suppress changes in the concentration of cations and anions within 10 times the concentration (mass % concentration) in the silica sol before the concentration step. Formation of a cake layer can be suppressed by setting the concentrations of these ion components within the above range.
  • the process (requirement B) by injecting or circulating silica sol in the concentration process. That is, by further injecting silica sol into the silica sol during the circulating concentration step or after the concentration step (the concentration of silica particles contained in the silica sol to be further injected is the same as that of the silica particles contained in the silica sol before the concentration step
  • the concentration is 0.1 to 30 times the concentration of ), and the above range can be set by adjusting the circulation time of the silica sol.
  • Examples of the above cations include monovalent cations, and potassium ions or sodium ions are particularly preferable from the viewpoint of suppressing coarse particles.
  • Examples of the above anions include anions containing sulfate ions, and sulfate ions are particularly preferable from the viewpoint of suppressing coarse particles.
  • silica sol produced by the alkoxide method can also be used as the silica sol to be concentrated by the ultrafiltration device.
  • a silica sol containing can be preferably used.
  • JIS No. 3 sodium water glass was prepared as a raw water-soluble alkali metal silicate.
  • the main components of this water glass other than water were SiO 2 : 28.8% by weight and Na 2 O: 9.47% by weight.
  • 833 kg of the above water glass was diluted with 5167 kg of pure water to prepare 6000 kg of sodium silicate aqueous solution (a).
  • the sodium silicate aqueous solution (a) was passed through a column filled with a hydrogen-type strongly acidic cation exchange resin Amberlite IR-120B at a space velocity of 4.5 per hour to recover 5500 kg of an aqueous solution of active silicic acid. did.
  • Example 1 (Concentration of silica sol thin liquid)
  • the obtained silica sol thin liquid 1 was circulated through a polysulfone tubular ultrafiltration membrane (also referred to as a UF tube, inner diameter: 1/2 inch) having a molecular weight cutoff of 100,000, under a pressure of 0.25 MPa and a flow rate of 6.0.
  • a polysulfone tubular ultrafiltration membrane also referred to as a UF tube, inner diameter: 1/2 inch
  • the solution was concentrated to a silica concentration of about 40% by mass.
  • the silica concentration of the sample is diluted with pure water to 15.0% by mass, and the LPC value is measured using AccuSizer FX-nano manufactured by PSS Japan Co., Ltd. (trade name AccuSizer A9000, manufactured by Nihon Entegris LLC). It was measured. When the silica concentration of the sample was less than 15.0% by mass, it was measured as it was, and the measured value was converted to 15.0% by mass. About 1 g of a sample was precisely weighed, dried on a hot plate at 140° C., fired at 1000° C. for 0.5 hours, and the silica concentration was calculated from the fired residue.
  • Example 2 The silica sol obtained by the same operation as in Example 1 was circulated through a polysulfone tubular ultrafiltration membrane (inner diameter of 1/2 inch) having a molecular weight cut off of 100,000, and the pressure was 0.10 MPa and the flow rate was 8.8 L/ The mixture was concentrated at 30° C. for a minute to a silica concentration of about 40% by mass.
  • Example 3 The silica sol obtained by the same operation as in Example 1 was circulated through a polysulfone tubular ultrafiltration membrane (inner diameter of 1/2 inch) having a molecular weight cut off of 100,000, and the pressure was 0.05 MPa and the flow rate was 9.5 L/ The mixture was concentrated at 30° C. for a minute to a silica concentration of about 40% by mass.
  • Example 4 The silica sol obtained by the same operation as in Example 1 was circulated through a polysulfone tubular ultrafiltration membrane (inner diameter of 1/2 inch) having a molecular weight cut off of 500,000, and the pressure was 0.25 MPa and the flow rate was 6.9 L/ The mixture was concentrated at 30° C. for a minute to a silica concentration of about 40% by mass.
  • Example 5 The silica sol obtained by the same operation as in Example 1 was circulated through a polysulfone tubular ultrafiltration membrane (inner diameter of 1/2 inch) having a molecular weight cut off of 500,000, and the pressure was 0.10 MPa and the flow rate was 8.8 L/ The mixture was concentrated at 30° C. for a minute to a silica concentration of about 40% by mass.
  • Example 6 The silica sol obtained by the same operation as in Example 1 was circulated through a polysulfone tubular ultrafiltration membrane (inside diameter of 1/2 inch) having a cutoff molecular weight of 500,000, and the pressure was 0.05 MPa and the flow rate was 9.5 L/ The mixture was concentrated at 30° C. for a minute to a silica concentration of about 40% by mass.
  • Example 7 The silica sol obtained by the same operation as in Example 1 was circulated through a polysulfone tubular ultrafiltration membrane (inner diameter of 1/2 inch) having a molecular weight cut off of 100,000, and the pressure was 0.05 MPa and the flow rate was 9.5 L/ The mixture was concentrated at 15° C. to a silica concentration of about 40% by mass.
  • Table 1 shows the concentration of silica sol using a UF tube with an inner diameter of 1/2 inch, and the presence or absence of contamination of washing water after UF concentration (so-called operation of removing silica sol from the pipe by pushing water). Those that did not use washing water after UF concentration were indicated as (none), and those that used washing water after UF concentration were indicated as (yes).
  • Thin liquid 1 is a silica sol having a silica concentration of 3.2% by mass before UF concentration, and is a raw material for the following silica concentrates 1 to 13 obtained in Examples 1 to 8 and Comparative Examples 1 to 5.
  • Concentrated liquid 1 is a silica sol having a silica concentration of 36.0% by mass by UF concentration obtained in Example 1 (Example 1).
  • Concentrated liquid 2 is a silica sol having a silica concentration of 35.7% by mass obtained by UF concentration obtained in Example 2 (Example 2).
  • Concentrated liquid 3 is a silica sol having a silica concentration of 35.2% by mass by UF concentration obtained in Example 3 (Example 3).
  • Concentrated liquid 4 is the silica sol having a silica concentration of 38.4% by mass by UF concentration obtained in Example 4 (Example 4).
  • Concentrated liquid 5 is a silica sol having a silica concentration of 35.1% by mass by UF concentration obtained in Example 5 (Example 5).
  • Concentrated liquid 6 is the silica sol having a silica concentration of 36.9 mass % obtained by UF concentration obtained in Example 6 (Example 6).
  • Concentrated liquid 7 is the silica sol having a silica concentration of 38.6% by mass by UF concentration obtained in Example 7 (Example 7). (--) in Table 1 indicates that it was not implemented.
  • Table 2 shows the physical properties of the concentrated silica sol. SiO2 concentration (mass %), cation content (mass percent), anion content (mass percent) are indicated.
  • LPC in Table 2 indicates the number of coarse particles having a particle diameter of 0.48 ⁇ m or more.
  • (--) in Table 2 indicates unmeasured.
  • Example 3 and Example 7 When comparing Example 3 and Example 7 at the same cutoff molecular weight and the same pressure, the concentrated solution 7 of Example 7 with a UF treatment temperature of 15 ° C. was higher than the concentrated solution 3 of Example 3 with a UF treatment temperature of 30 ° C. It was confirmed that the numerical value of LPC decreased in . When comparing Examples 1 to 3 and Examples 4 to 6 at the same temperature and the same molecular weight cutoff, it was confirmed that the value of LPC increases as the UF treatment pressure increases.
  • Example 8 Silica sol obtained by the same operation as in Example 1 was filtered using a commercially available ultrafiltration device equipped with a polyvinylidene fluoride tubular ultrafiltration membrane (inner diameter of 1 inch) having a cutoff molecular weight of 100,000. It was concentrated to a SiO 2 concentration of about 40% by weight at 30° C. at 3 MPa and a flow rate of 420 L/min. There was no contamination of washing water after UF concentration (so-called operation of removing silica sol from pipes by pushing water).
  • Example 5 Silica sol obtained by the same operation as in Example 1 was filtered using a commercially available ultrafiltration device equipped with a polyvinylidene fluoride tubular ultrafiltration membrane (inner diameter of 1 inch) having a cutoff molecular weight of 100,000. Concentration was carried out at 50 to 70° C. to a SiO 2 concentration of about 40 mass % at 3 MPa and a flow rate of 420 L/min. The case where the washing water after UF concentration was mixed (the so-called operation of taking out the silica sol from the pipe by pushing water) and the case where it was not were also shown. The case where the washing water after UF concentration is mixed is the case where pure water is flowed into the UF tube and the concentrated solution is collected.
  • a commercially available ultrafiltration device equipped with a polyvinylidene fluoride tubular ultrafiltration membrane (inner diameter of 1 inch) having a cutoff molecular weight of 100,000. Concentration was carried out at 50 to 70° C. to a SiO 2 concentration of about 40 mass
  • Concentrated liquid 8 is the silica sol having a silica concentration of 39.0% by mass by UF concentration obtained in Example 8 (Example 8).
  • Concentrated liquid 9 is the silica sol having a silica concentration of 36.6 mass % obtained by UF concentration obtained in Comparative Example 1 (Comparative Example 1).
  • Concentrated liquid 10 is the silica sol having a silica concentration of 43.4% by mass by UF concentration obtained in Comparative Example 2 (Comparative Example 2).
  • Concentrated liquid 11 is the silica sol having a silica concentration of 40.0% by mass by UF concentration obtained in Comparative Example 3 (Comparative Example 3).
  • Concentrated liquid 12 is silica sol having a silica concentration of 40.6% by mass obtained by UF concentration obtained in Comparative Example 4 (Comparative Example 4).
  • Concentrated liquid 13 is the silica sol having a silica concentration of 44.3% by mass by UF concentration obtained in Comparative Example 5 (Comparative Example 5). (--) in Table 3 indicates that it was not implemented.
  • Table 4 shows the physical properties of the concentrated silica sol. SiO2 concentration (mass %), cation content (mass percent), anion content (mass percent) are indicated. LPC in Table 4 indicates the number of coarse particles having a particle diameter of 0.48 ⁇ m or more.
  • Example 8 and Comparative Examples 1 and 3 In comparison with the same cutoff molecular weight, the same pressure, and no mixing of washing water after UF, by comparison of Example 8 and Comparative Examples 1 and 3, the value of LPC increases as the UF treatment temperature rises. was confirmed. In comparison with the same cutoff molecular weight, the same pressure, and the same UF treatment temperature, Example 8 and Comparative Example 5 were compared in the case where washing water was not mixed after UF and when washing water was mixed after UF. Also, from the comparison between Comparative Examples 1 and 2 and the comparison between Comparative Examples 3 and 4, the LPC increased significantly due to the mixing of washing water after UF. Mixing of washing water after UF means an operation of pouring pure water into the UF tube and recovering the concentrate, but the concentration of silica in the concentrate is greatly reduced locally.
  • Circulating the silica sol in the device or injecting silica sol further into the ultrafiltration device is related to the fact that the concentration of silica particles contained in the silica sol after the concentration step is higher than before the concentration step.) Suppresses the contamination of LPC (coarse particles) generated in the silica sol concentration step. We were able to.
  • the silica sol concentration method of the present invention it is possible to prevent the formation of agglomerated silica particles in the concentrated silica sol when concentration is performed to increase the concentration of silica components in the silica sol by ultrafiltration. Therefore, the method is useful for producing silica sol used for polishing silicon wafers for semiconductors and devices, for example, because it can suppress inclusion of LPC (coarse particles) into the silica sol.

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  • Engineering & Computer Science (AREA)
  • Water Supply & Treatment (AREA)
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Abstract

Le problème décrit par la présente invention est de fournir une méthode de concentration de sol de silice avec laquelle il est possible, lors de la réalisation d'une concentration au moyen d'une ultrafiltration afin d'augmenter la concentration d'un composant de silice dans un sol de silice, d'empêcher la formation de particules de silice agrégées dans le sol de silice concentré. À cet effet, l'invention concerne une méthode de concentration pour un sol (sol de silice) dans lequel des particules de silice sont dispersées dans un milieu de dispersion en tant que particules dispersoïdes, ladite méthode de concentration de sol de silice étant caractérisée en ce qu'elle comprend une étape de concentration pour augmenter la concentration des particules de silice contenues dans le sol de silice à l'aide d'un dispositif d'ultrafiltration, et l'exigence A et l'exigence B étant satisfaites pendant l'étape de concentration. Exigence A : La température de solution du sol de silice immédiatement avant d'être versé dans le dispositif d'ultrafiltration étant dans la plage de 0 à 45 °C. Exigence B : La concentration des particules de silice contenues dans le sol de silice après l'étape de concentration étant augmentée par rapport à avant l'étape de concentration suite à la circulation du sol de silice dans le dispositif d'ultrafiltration.
PCT/JP2023/007039 2022-02-28 2023-02-27 Méthode de concentration de sol de silice par ultrafiltration WO2023163169A1 (fr)

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