WO2015068829A1 - Dispersion liquide de silicate d'aluminium tubulaire et procédé de production pour dispersion liquide de silicate d'aluminium tubulaire - Google Patents

Dispersion liquide de silicate d'aluminium tubulaire et procédé de production pour dispersion liquide de silicate d'aluminium tubulaire Download PDF

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WO2015068829A1
WO2015068829A1 PCT/JP2014/079670 JP2014079670W WO2015068829A1 WO 2015068829 A1 WO2015068829 A1 WO 2015068829A1 JP 2014079670 W JP2014079670 W JP 2014079670W WO 2015068829 A1 WO2015068829 A1 WO 2015068829A1
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aluminum silicate
tubular aluminum
water
mixed solution
dispersion
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PCT/JP2014/079670
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English (en)
Japanese (ja)
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禄人 田口
貴志 鷲巣
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コニカミノルタ株式会社
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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
    • C01B33/20—Silicates
    • C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y02P20/129—Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines

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  • the present invention relates to a tubular aluminum silicate dispersion and a method for producing a tubular aluminum silicate dispersion.
  • imogolite is known as a tubular aluminum silicate.
  • Imogolite is a kind of natural clay component that appears in soils based on descending volcanic ejecta such as volcanic ash and pumice, and is a nano-sized tubular amorphous aluminum silicate.
  • This tubular aluminum silicate has silicon (Si), aluminum (Al), oxygen (O) and hydrogen (H) as main constituent elements, and is composed of a number of ⁇ Si—O—Al ⁇ bonds.
  • the shape is a nanotube-like structure having an outer diameter of 2.0 to 3.0 nm, an inner diameter of 0.5 to 1.5 nm, and a length of several tens of nm to several ⁇ m.
  • This tubular aluminum silicate has a unique nano tube shape and high specific surface area, water affinity, ion exchange capacity and material adsorption capacity.
  • Various industrial uses such as a catalyst carrier, a humidity control material, and a heat pump system heat exchange agent that produces a refrigerant using a low-temperature heat source are expected.
  • the tubular aluminum silicate is prepared as a dispersion dispersed in water by the production method (for example, see Patent Documents 1 and 2).
  • such an aqueous dispersion of tubular aluminum silicate can be used as a cryogen by adjusting the pH to be weakly alkaline (see, for example, Patent Document 3).
  • tubular aluminum silicate when such an aqueous dispersion of tubular aluminum silicate is dispersed in an organic dispersion medium, the tubular aluminum silicate aggregates and a uniform dispersion cannot be obtained. Therefore, it is difficult to uniformly disperse the tubular aluminum silicate in an organic material such as a resin, and the use of the tubular aluminum silicate has been limited. In addition, it is possible to forcibly disperse by adding a large amount of organic dispersion medium to the aqueous dispersion of tubular aluminum silicate, and to disperse uniformly in organic materials such as resins. Therefore, the desired effect of the tubular aluminum silicate cannot be obtained.
  • an object of the present invention is to provide a tubular aluminum silicate dispersion that can be dispersed in an organic material and has adsorptivity and ion exchange properties, and a method for producing the same.
  • a tubular aluminum silicate dispersion characterized in that water is removed from a mixed liquid of a tubular aluminum silicate, water, and an organic dispersion medium.
  • a method for producing a tubular aluminum silicate dispersion characterized by comprising:
  • tubular aluminum silicate dispersion that can be dispersed in an organic material and has adsorptivity and ion exchange, and a method for producing the same.
  • tubular aluminum silicate It is an X-ray diffraction pattern of tubular aluminum silicate. It is a scanning electron micrograph of tubular aluminum silicate. It is a conceptual diagram for demonstrating decompression evaporation. It is a conceptual diagram for demonstrating ultrafiltration.
  • ⁇ representing a numerical range is used in a sense including numerical values described before and after the numerical value as a lower limit value and an upper limit value.
  • the tubular aluminum silicate dispersion of the present invention is characterized in that water is removed from a mixed liquid of tubular aluminum silicate, water, and an organic dispersion medium.
  • Each material constituting the tubular aluminum silicate dispersion of the present invention will be specifically described below.
  • tubular aluminum silicate ⁇ There is no restriction
  • the tubular aluminum silicate used in the present invention is b / a ⁇ 10 when the outer diameter of the tubular aluminum silicate is a and the length is b, that is, imogolite. It is preferable.
  • the method for producing tube-shaped aluminum silicate is not particularly limited, and can be produced by, for example, the method described in JP 2011-42520 A. However, the tubular aluminum silicate can be efficiently produced by using the following method.
  • an orthosilicate solution having an electric conductivity of 5 to 500 ⁇ S / cm and a pH of 3.5 to 7.5 is prepared (first step).
  • the prepared orthosilicic acid solution, inorganic aluminum compound solution and urea or ammonia are mixed, and the mixed solution is adjusted to pH 2.8 to 7.5 and then heated (second step).
  • the obtained reaction product is subjected to solid separation and desalting (third step), and the desired tubular aluminum silicate can be obtained.
  • Each material and conditions used in such a manufacturing method will be described below.
  • the silicon source constituting the inorganic silicon compound solution is not particularly limited as long as silicate ions are generated when solvated.
  • Examples of such a silicon source include sodium orthosilicate, sodium metasilicate, potassium metasilicate, and water glass.
  • a solvent that can easily be solvated with the raw material silicic acid source can be appropriately selected and used.
  • water, alcohols, etc. can be used, for example. From the viewpoint of salt solubility and ease of handling during heating, water is preferably used.
  • the silicon concentration of the inorganic silicon compound solution during ion exchange is preferably 20 mM or less.
  • Ion exchanger As the ion exchanger used for the ion exchange treatment of the inorganic silicon compound solution, an anion exchanger or a cation exchanger is used.
  • the anion exchanger include an anion exchange membrane and the like
  • examples of the cation exchanger include a cation exchange resin and a cation exchange membrane. It is preferable to use a cation exchange resin because it is high and silicon concentration control is easy.
  • any conventionally known ion exchanger can be used as long as the orthosilicate solution obtained after the treatment has an electric conductivity of 5 to 500 ⁇ S / cm and a pH of 3.5 to 7.5. May be used.
  • a strong acid cation exchange resin or a weak acid cation exchange resin may be used, or a plurality of cation exchange resins may be used in combination.
  • Examples of the strongly acidic cation exchange resin include Amberlite IR120B (manufactured by Organo), Amberlite IR124 (manufactured by Organo), Amberlite 200CT (manufactured by Organo), Amberlite 252 (manufactured by Organo), Diaion SK104.
  • Examples of the weak acid cation exchange resin include Amberlite FPC3500 (manufactured by Organo), Amberlite IRC76 (manufactured by Organo), Diaion WK10 (manufactured by Mitsubishi Chemical), Diaion WK11 (manufactured by Mitsubishi Chemical), Dia Examples include, but are not limited to, ion WK100 (manufactured by Mitsubishi Chemical Corporation) and diamond ion WK40L (manufactured by Mitsubishi Chemical Corporation).
  • an ion exchange resin for example, a batch method, a column method, or the like is used as an ion exchange treatment method for the inorganic silicon compound solution.
  • a conditioned ion exchange resin is put into a container, an inorganic silicon compound solution whose concentration is adjusted is added thereto, and the reaction is performed for about 2 hours while stirring or shaking at a strength that allows the ion exchange resin to float. Thereafter, the ion exchange resin is filtered off, and the filtrate is recovered to obtain an orthosilicate solution. If a magnetic stirrer is used, depending on the type of ion exchange resin, the ion exchange resin may be destroyed. Therefore, it is desirable to perform shaking during mixing.
  • conditioning means returning the ion exchange resin to a state where the ion exchange ability can be exhibited.
  • an ion-exchange resin that has been conditioned is packed into a column, an inorganic silicon compound solution whose concentration is adjusted is flowed into the column at a constant flow rate, and the solution that flows out of the column is recovered to obtain an orthosilicate solution. obtain.
  • the electric conductivity of the resulting orthosilicate solution can be adjusted by the degree of stirring or shaking, the reaction time, etc.
  • the flow rate of the sample flowing in the column the volume of the column ( Radius, length, etc.), the amount of ion-exchange resin filling, and the like. That is, the electrical conductivity of the orthosilicate solution can be adjusted by appropriately changing the contact time and the contact area between the inorganic silicon compound solution and the ion exchanger.
  • the pH of the resulting orthosilicate solution can be adjusted by the type of ion exchange resin used, the contact time between the ion exchange resin and the inorganic silicon compound solution, and the like.
  • the pH of the orthosilicate solution obtained becomes lower as the ion exchange proceeds. Therefore, when a strongly acidic cation exchange resin having a high ion exchange rate is used, the pH of the orthosilicate solution is increased. The pH of the orthosilicic acid solution remains high when a weakly acidic cation exchange resin with a lower ion exchange rate is used.
  • an ion exchange membrane may be used as the ion exchanger.
  • the ion exchange membrane is an ion filtration membrane formed by molding an ion exchange resin into a film shape, and has a property of blocking the passage of ions having different signs and allowing only ions having the same sign to pass.
  • an ion exchange membrane it is preferable to use an anion exchange membrane and a cation exchange membrane together, but each may be used alone by combining with other methods.
  • the anion exchange membrane is positively charged because the cation group is fixed to the membrane, and only the anion is allowed to pass through without repelling the cation.
  • anion exchange membranes are used, for example, for seawater concentration salt production, concentration / removal of metal ions, removal of radioactive ions / substances, and the like.
  • anion exchange membrane By using such an anion exchange membrane, only the anion in the inorganic silicon compound solution can be permeated to prepare a target orthosilicate solution.
  • the cation exchange membrane is negatively charged because the anion group is fixed to the membrane, and only the cation is allowed to pass without repelling the anion.
  • (1.3) pH of orthosilicate solution The treatment conditions with the ion exchanger are set so that the pH of the orthosilicic acid solution prepared by the treatment with the ion exchanger is 3.5 to 7.5.
  • the pH is 7.5 or less, it is possible to suppress the formation of polysilicic acid by polymerization of orthosilicic acid in the solution, and when the pH is 3.5 or more, the pH adjustment in the second step The amount of alkali added in can be reduced.
  • PH measurement can be performed with a pH meter using a general glass electrode.
  • MODEL F-71S
  • the pH of the orthosilicate solution is as follows: phthalate pH standard solution (pH: 4.01), neutral phosphate pH standard solution (pH: 6.86), and borate pH standard solution (pH: 9.01). 18) is used as a pH standard solution, the pH meter is calibrated at three points, the electrode of the pH meter is placed in an orthosilicic acid solution, and the value after 5 minutes has elapsed and is read. At this time, the liquid temperature of the pH standard solution and the orthosilicate solution can be set to 25 ° C., for example.
  • the treatment conditions with the ion exchanger are set so that the electrical conductivity of the orthosilicic acid solution prepared by the treatment with the ion exchanger is 5 to 500 ⁇ S / cm.
  • the electrical conductivity of the orthosilicate solution is preferably 5 to 100 ⁇ S / cm, more preferably 5 to 15 ⁇ S / cm.
  • the electrical conductivity of the orthosilicate solution is 500 ⁇ S / cm or less
  • the mixing of the salt into the mixed solution prepared in the second step is suppressed, and a tubular aluminum silicate can be produced with a high yield.
  • the treatment time by an ion exchanger can be shortened and productivity can be improved as the electrical conductivity of an orthosilicic acid solution is 5 microsiemens / cm or more.
  • the electrical conductivity of theoretical pure water is an insulator of about 0.055 ⁇ S / cm, it can be said that the electrical conductivity is an index indicating the total amount of ions in the solution, particularly when the solvent of the orthosilicate solution is water.
  • the electrical conductivity of the orthosilicic acid solution can be measured with a general electrical conductivity meter. Specifically, for example, it is measured at room temperature (25 ° C.) using ES-51 (Horiba, Ltd.).
  • the aluminum source constituting the inorganic aluminum compound solution is not particularly limited as long as aluminum ions are generated when solvated.
  • Examples of such an aluminum source include aluminum chloride, aluminum perchlorate, aluminum nitrate, aluminum sec-butoxide and the like.
  • a material that can easily be solvated with the aluminum source that is a raw material can be appropriately selected and used.
  • water, alcohols, etc. can be used, for example. From the viewpoint of salt solubility and ease of handling during heating, water is preferably used.
  • the composition ratio of the tubular aluminum silicate to be produced can be changed by adjusting the amount of the inorganic aluminum compound solution to the orthosilicate aqueous solution.
  • Urea or ammonia Either urea or ammonia may be used, and it is preferable to add as a solution adjusted to a predetermined concentration from the viewpoint of handleability.
  • the mixed solution obtained by mixing the orthosilicic acid solution, the inorganic aluminum compound solution, and urea or ammonia is adjusted to pH 2.8 to 7.5.
  • a method of adding a basic solution such as an aqueous solution of sodium hydroxide or an aqueous solution of potassium hydroxide
  • a method of adding an acidic solution such as hydrochloric acid, acetic acid, or nitric acid, etc.
  • the heating temperature at this time is not particularly limited, but is preferably 80 to 120 ° C. from the viewpoint of obtaining a higher purity tubular aluminum silicate.
  • the heating temperature is not particularly limited, but is preferably 80 to 120 ° C. from the viewpoint of obtaining a higher purity tubular aluminum silicate.
  • the heating temperature is too high, rapid thermal decomposition may occur at the beginning of heating, and the ammonia concentration in the mixed solution may rise rapidly, causing the pH to approximate the alkaline side. It is considered unsuitable for the production of tubular aluminum silicates that are formed from acidic to weakly acidic.
  • the heating temperature is 80 ° C. or higher, the thermal decomposition of urea and the subsequent synthesis rate of the tubular aluminum silicate are improved, and the productivity can be improved.
  • the heating time is not particularly limited, but is preferably 12 hours or more and 100 hours or less from the viewpoint of efficiently obtaining the tubular aluminum silicate.
  • tubular aluminum silicate produced by the method as described above can be identified by measurement by X-ray diffraction and measurement by a scanning electron microscope (SEM).
  • FIG. 2 shows a scanning electron micrograph (SEM image) of the tubular aluminum silicate.
  • SEM image scanning electron micrograph
  • Organic dispersion medium As the organic dispersion medium according to the present invention, an organic dispersion medium having compatibility with water is used, and specifically, alcohols are preferable.
  • alcohols include monohydric alcohols such as methanol, ethanol, propanol, and butanol, ethylene glycol, propylene glycol, diethylene glycol, glycerin, 1,3-butanediol, 1,4-butanediol, and the like.
  • the tubular aluminum silicate dispersion of the present invention may contain two or more alcohols as an organic dispersion medium.
  • the tubular aluminum silicate of the present invention comprises 1 part by weight of a tubular aluminum silicate, 0 to 100 parts by weight of water, and 10 to 3000 parts by weight of an organic dispersion medium. It is preferable that it is comprised so that many may be included.
  • water may be completely removed and the water content may be 0 parts by weight, but preferably it contains a small amount of water.
  • Water (content) is 0 part by weight” means that water can be analyzed within a range that can be analyzed when water is removed from a mixture of tubular aluminum silicate, water, and organic dispersion medium. Means not detected.
  • a step of preparing a mixed liquid by mixing a tubular aluminum silicate, water, and an organic dispersion medium, and from the mixed liquid Removing water In the step of preparing the mixed solution, it is preferable to prepare the mixed solution so that 10% by mass or less of the tubular aluminum silicate is contained in the mixed solution.
  • the mixed liquid is in a state where the tubular aluminum silicate is uniformly dispersed without being aggregated due to the presence of water, and the organic dispersion medium is compatible with water.
  • the dispersion medium is also uniformly mixed.
  • the dispersion liquid of the present invention is constituted by removing water from the mixed liquid, the dispersion liquid of the present invention has a state in which the tubular aluminum silicate is uniformly dispersed without being aggregated in the organic dispersion medium. It has become. For this reason, by mixing such a dispersion with an organic material such as a resin, the tubular aluminum silicate can be uniformly dispersed in the organic material.
  • a method for removing water from the mixed solution it is sufficient that water can be removed while maintaining a uniform dispersion state of the tubular aluminum silicate in the mixed solution.
  • centrifugation or a drying material For example, addition of a molecular sieve, potassium carbonate, silica gel or the like
  • the method by centrifugation is preferably used when the specific gravity of the organic dispersion medium to be used is smaller than that of water, and it is preferable because it can be performed in a short time without causing problems such as mixing of impurities.
  • the method by addition of a desiccant can be used irrespective of the physical property of an organic dispersion medium.
  • Other methods for removing water from the mixed solution include a method of evaporating the mixed solution under reduced pressure and a method of ultrafiltering the mixed solution.
  • the evaporation under reduced pressure is a method in which the mixed solution is heated under reduced pressure to promote the evaporation of the mixed solution and remove the solvent.
  • the mixed solution is heated under reduced pressure (evaporated under reduced pressure) to remove water in the mixed solution.
  • the rotary evaporator 10 can be used, and in a state where the eggplant flask 16 is depressurized via the condenser 12, the mixture liquid is evaporated by heating the eggplant flask 16 while rotating the eggplant flask 16. Then, the evaporated dispersion medium (water) is cooled by the cooling water 14 in the condenser 12 and stored in the receiving flask 20.
  • an organic solvent to be substituted is added to the mixed solution after removing water and evaporated again under reduced pressure to remove water, and the same operation is repeated by adding the organic solvent.
  • the lower limit is set to a state in which the dispersion medium remains in an amount of 10 parts by weight or more with respect to the tubular aluminum silicate. Remove water.
  • Ultrafiltration is a method in which a solvent is removed by forcibly permeating a filtration membrane by applying pressure (or absorbing pressure) while circulating a mixed solution.
  • the mixed solution is circulated through the filter 32 of the ultrafiltration device 30, and the mixed solution is pressurized (or sucked) in the middle to forcibly permeate the filtration membrane 34.
  • Remove water Thereafter, an organic solvent for substitution is added to the mixed solution after removing water, and ultrafiltration is again performed to remove water, and the same operation is repeated by adding the organic solvent.
  • the tubular aluminum silicate dispersion of the present invention can be dispersed in an organic material because water is removed from a mixture of a tubular aluminum silicate, water, and an organic dispersion medium.
  • a tubular aluminum silicate having adsorptivity and ion exchange properties can be provided. This is because an organic dispersion medium having compatibility with water coexists in an aqueous dispersion of tubular aluminum silicate that forms a uniform dispersion state in water, and water is removed from the mixture. This is because a tubular aluminum silicate dispersion liquid uniformly dispersed in an organic dispersion medium can be obtained.
  • the tubular aluminum silicate dispersion liquid of the present invention is configured as described above, the concentration of the tubular aluminum silicate in the dispersion liquid is high. The ion exchange property can be sufficiently exhibited.
  • tubular aluminum silicate when water is removed by centrifuging a mixed solution of tubular aluminum silicate, water and an organic dispersion medium, the tubular aluminum silicate can be obtained in a short time without being mixed with impurities.
  • a salt dispersion can be prepared.
  • vacuum evaporation or ultrafiltration is performed instead of centrifugation, there is no need to perform an operation that induces aggregation of the tubular aluminum silicate, such as salting out or centrifugal separation. Since the aqueous dispersion of silicate can be solvent-substituted as it is, aggregation of the tubular aluminum silicate can be prevented.
  • the organic dispersion medium contains alcohol, a dispersion in which the tubular aluminum silicate is more reliably dispersed can be obtained, and the handling becomes easy.
  • Samples 2-8 In the preparation of Sample 1, the type of organic dispersion medium was changed as shown in Table 1, and the same procedure was performed except that the amounts of water and organic dispersion medium were changed so that the composition of the sample was as shown in Table 1. Samples 2 to 8 were prepared. In Sample 8, isopropyl alcohol is used as the organic dispersion medium, and in Table 1, “IPA” is used.
  • ⁇ Preparation of Sample 9 First, an aqueous dispersion of tubular aluminum silicate was prepared in the same manner as in the preparation of Sample 1. Subsequently, 30 g of ethanol was added to 10 g of the obtained aqueous dispersion of tubular aluminum silicate, and the mixture was stirred to prepare a gel under water-ethanol mixing (treatment 3). To this was added 3 g of potassium carbonate as a desiccant, and the mixture was stirred for 24 hours to absorb water in potassium carbonate, and then the potassium carbonate was taken out (treatment 4). This treatment 4 was repeated 10 times to prepare a tubular aluminum silicate dispersion of 1 part by weight of tubular aluminum silicate, 10 parts by weight of water and 200 parts by weight of ethanol. Sample 9 was prepared by mixing 100 parts by weight of this tubular aluminum silicate dispersion with 100 parts by weight of silicone resin.
  • Samples 10 and 11 were prepared.
  • a mixed dispersion medium of isopropyl alcohol and ethylene glycol is used as the organic dispersion medium.
  • 100 parts by weight of ethanol and 100 parts of ethylene glycol are used per 1 part by weight of the tubular aluminum silicate. It is prepared to include parts by weight.
  • ⁇ Preparation of Sample 14 First, an aqueous dispersion of tubular aluminum silicate was prepared in the same manner as in the preparation of Sample 1. Subsequently, 1000 parts by weight of ethanol was mixed with an aqueous dispersion of tubular aluminum silicate composed of 1 part by weight of tubular aluminum silicate and 100 parts by weight of water to prepare a tubular aluminum silicate dispersion. . 100 parts by weight of silicone resin was mixed with 100 parts by weight of this tubular aluminum silicate dispersion to prepare Sample 14.
  • Sample 15 was prepared in the same manner as in the preparation of Sample 14, except that the amounts of water and the organic dispersion medium were changed so that the composition of the sample was as shown in Table 1.
  • Sample 18 was prepared in the same manner as Sample 17 except that the number of repetitions of Process 1 and Process 2 was changed from 10 to 7.
  • Sample 19 was prepared in the same manner as in the preparation of sample 18, except that the solvent replacement target in treatment 1 was changed from ethanol to methanol.
  • the obtained mixed solution was subjected to ultrafiltration under the conditions of a flow rate of 300 ml / min (min), a liquid pressure of 1 bar, and room temperature using a Vivaflow 50 manufactured by Sartorius stedim (effective filtration area of 50 cm 2 and a molecular weight cut off of 5000) Water in the mixture was removed. 200 ml of ethanol was added to 200 ml of the obtained mixed liquid, and ultrafiltration was performed again. When the liquid volume reached 200 ml, 200 ml of ethanol was added again to perform ultrafiltration, and the solution was concentrated to 200 ml. . This operation was performed 10 times in total, and the dispersion medium in the mixed solution was replaced with ethanol.
  • sample 23 was prepared by mixing 100 parts by weight of silicone resin with 100 parts by weight of the tubular aluminum silicate dispersion.
  • Sample 24 In the preparation of sample 23, the ultrafiltration operation was changed from 10 to 7 times, and a tubular aluminum silicate dispersion of 1 part by weight of tubular aluminum silicate, 5 parts by weight of water, and 100 parts by weight of ethanol was added. Prepared. A sample 24 was prepared by mixing 100 parts by weight of a silicone resin with 100 parts by weight of the tubular aluminum silicate dispersion.
  • Sample 26 In the preparation of Sample 24, the solvent substitution target was changed from ethanol to methanol, and a tubular aluminum silicate dispersion of 1 part by weight of tubular aluminum silicate, 5 parts by weight of water, and 100 parts by weight of methanol was prepared. Sample 26 was prepared by mixing 100 parts by weight of a silicone resin with 100 parts by weight of the tubular aluminum silicate dispersion.
  • Sample 27 In the preparation of sample 26, the ultrafiltration operation was changed from 7 times to 5 times, and the concentration was adjusted so that 1 part by weight of tubular aluminum silicate, 10 parts by weight of water, and 200 parts by weight of ethanol were obtained. A silicate dispersion was prepared. Sample 27 was prepared by mixing 100 parts by weight of a silicone resin with 200 parts by weight of the tubular aluminum silicate dispersion.
  • the reflectance ratio is 95% or more.
  • ⁇ The reflectance ratio is 90% or more and less than 95%.
  • ⁇ The reflectance ratio is 85% or more and less than 90%.
  • X The reflectance ratio is less than 85%.
  • the produced printed circuit board was energized continuously for 1000 hours (hours) in a constant temperature and humidity test tank at 85 ° C. and 85%. After this test, it was observed whether migration of the electrode portion occurred with a microscope, and the number of substrates on which migration occurred was evaluated according to the following criteria. The evaluation results are shown in Tables 1 and 2.
  • A The number of migration occurrences is 1 or 0.
  • ⁇ The number of migration occurrences is two.
  • ⁇ Number of migration occurrences is 3.
  • X The number of migration occurrences is 4 or more.
  • Samples 1 to 13 according to the present invention show good results in the sulfide gas resistance evaluation and migration evaluation. Since the results of the sulfide gas resistance evaluation are good, in samples 1 to 13, hydrogen sulfide gas is adsorbed on the tubular aluminum silicate before reaching the Ag substrate, and as a result, corrosion of the Ag substrate is suppressed. The Ag substrate is considered to maintain a high reflectance. Therefore, it can be said that Samples 1 to 13 having good evaluation results of the resistance to sulfide gas are excellent in adsorptivity. In addition, since migration evaluation results are good, in Samples 1 to 13, metal ions that cause migration are adsorbed on the tubular aluminum silicate and ion exchanged with H ions that do not cause migration. Thus, it is considered that the occurrence of migration is effectively suppressed. Therefore, it can be said that Samples 1 to 13 having good migration evaluation results have excellent ion exchange properties.
  • the tubular aluminum silicate dispersion of the present invention has a particle size approximately the same as that when the tubular aluminum silicate is dispersed in water. It is shown that the tubular aluminum silicate is uniformly dispersed.
  • tubular aluminum silicate dispersion liquid that can be dispersed in an organic material and has adsorptivity and ion exchange properties can be obtained.
  • the effect of the present invention described above is that the centrifugation conditions when using centrifugation as a method for removing water as in Samples 17 to 19 are changed, and the water in the tubular aluminum silicate dispersion is significantly reduced. Has also been shown to be obtained. It has been shown that the above-described effects of the present invention can be obtained even when the water removal method is changed from centrifugation to vacuum evaporation or ultrafiltration as in samples 20 to 22 and 23 to 27. In addition, from the results of the particle size measurement of samples 17, 21, and 24, the centrifugation conditions when using centrifugation as the water removal method are changed, or the water removal method is reduced from the centrifugation to vacuum evaporation or ultrafiltration.
  • the tubular aluminum silicate dispersion of the present invention shows a particle size almost the same as when the tubular aluminum silicate is dispersed in water, even in this case, It is shown that the tubular aluminum silicate is uniformly dispersed.
  • samples 21 and 24 have a small particle size. This is because the vacuum evaporation or ultrafiltration operation is performed in the preparation of the sample, so there is no need to perform an operation that induces aggregation of the tubular aluminum silicate such as salting out or centrifugation, This is because aggregation of the tubular aluminum silicate is prevented.
  • the present invention is suitable for providing a tubular aluminum silicate dispersion which can be dispersed in an organic material and has adsorptivity and ion exchange and a method for producing the same.

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  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

La présente invention a pour objet une dispersion liquide de silicate d'aluminium tubulaire qui peut être dispersée dans un matériau organique et qui a des propriétés d'adsorption et des propriétés d'échange d'ions. La dispersion liquide de silicate d'aluminium tubulaire est caractérisée en ce que l'eau est enlevée d'un mélange liquide de silicate d'aluminium tubulaire, d'eau et d'un milieu de dispersion organique.
PCT/JP2014/079670 2013-11-11 2014-11-10 Dispersion liquide de silicate d'aluminium tubulaire et procédé de production pour dispersion liquide de silicate d'aluminium tubulaire WO2015068829A1 (fr)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS58220820A (ja) * 1982-06-09 1983-12-22 Teijin Ltd アルミノケイ酸繊維及びその製造法
JP2002220222A (ja) * 2000-12-05 2002-08-09 Eastman Kodak Co コロイド状アルミノ珪酸塩粒子混合物の分離方法
JP2002284584A (ja) * 2001-03-28 2002-10-03 Asahi Glass Co Ltd シリケート質多孔体の製造方法
JP2014075183A (ja) * 2012-10-02 2014-04-24 Hitachi Chemical Co Ltd 非水電解質二次電池

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS58220820A (ja) * 1982-06-09 1983-12-22 Teijin Ltd アルミノケイ酸繊維及びその製造法
JP2002220222A (ja) * 2000-12-05 2002-08-09 Eastman Kodak Co コロイド状アルミノ珪酸塩粒子混合物の分離方法
JP2002284584A (ja) * 2001-03-28 2002-10-03 Asahi Glass Co Ltd シリケート質多孔体の製造方法
JP2014075183A (ja) * 2012-10-02 2014-04-24 Hitachi Chemical Co Ltd 非水電解質二次電池

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