Hydrotalcite compound particles, and anion scavenger and resin composition containing said particles

Abstract

The present disclosure relates to hydrotalcite compound particles and an anion scavenger containing the particles. Specifically, the present disclosure relates to: hydrotalcite compound particles which exhibit an excellent effect of capturing a trace amount of anions, particularly chlorine ions, contained in various resins; and an anion scavenger containing the particles.　The hydrotalcite compound particles include primary particles and aggregated particles formed from the primary particles, and have a specific surface area of 18 m2 / g or more. In a pore distribution obtained by a mercury press-in method, the ratio (μ2 / μ1) of the second peak diameter μ2 to the first peak diameter μ1 is 100 or less. The primary particles have an average major axis diameter of 0.01-0.30 μm.

Description

Hydrotalcite compound particles, and anion scavengers and resin compositions containing said particles

[0001] This disclosure relates to hydrotalcite compound particles, and anion scavengers and resin compositions containing such particles.

[0002] It is known that encapsulants are used to protect semiconductors and other elements used in electronic and electrical equipment from light, heat, moisture, dust, and shock. Resin materials are known as encapsulants. On the other hand, there are concerns about corrosion, destruction, and degradation of the conductive parts of the elements due to anions remaining in the resin material.

[0003] Therefore, it is known to include adsorbents such as hydrotalcite in the sealing material.

[0004] On the other hand, there is a demand for a reduction in the long-term failure rate and further improvement in the performance of anion adsorbents. Specifically, there is a demand for improved chlorine adsorption performance.

[0005] Japanese Patent Publication No. 2018-184306 (Patent Document 1) discloses hydrotalcite compounds, resin compositions prepared by blending these compounds, and molded articles thereof. However, the BET specific surface area of ​​the hydrotalcite compounds is 15 m². ２ Because the concentration is low ( / g), its ability to adsorb chlorine is insufficient.

[0006] Japanese Patent Publication No. 2018-184306

[0007] For sealing materials to be used in practical applications, high chlorine adsorption capacity is required.

[0008] This embodiment addresses the above-mentioned problems. Specifically, the object of this disclosure is to provide hydrotalcite compound particles that exhibit excellent effects in capturing trace amounts of anions, particularly chloride ions, contained in various resins, and to provide an anion scavenger containing said particles.

[0009] The aforementioned technical problems can be solved by the present invention as follows.

[0010] That is, the hydrotalcite compound particles according to this embodiment include primary particles and aggregated particles formed by the primary particles, and 18m ２／ Having a specific surface area of ​​g or more, and in the pore distribution obtained by the mercury intrusion method, the first peak diameter μ １ The second peak diameter μ for ２ Ratio (μ ２ / μ １ The ratio is 100 or less, and the average major axis diameter of the primary particles is 0.01 to 0.30 μm. (Embodiment 1)

[0011] Alternatively, the hydrotalcite compound particles according to Embodiment 1 may have a 50% average particle size (D50) in the particle size distribution of the hydrotalcite compound particles according to this embodiment being 0.1 to 30.0 μm. (Embodiment 2)

[0012] Furthermore, the hydrotalcite compound particles according to this embodiment may also be hydrotalcite compound particles according to Embodiment 1 or 2, wherein the shape of the primary particles is plate-shaped or spherical. (Embodiment 3)

[0013] Furthermore, the anion scavenger according to this embodiment is an anion scavenger containing hydrotalcite compound particles according to Embodiment 1 or 2. (Embodiment 4)

[0014] Furthermore, the resin composition according to this embodiment is a resin composition containing a hydrotalcite compound according to Embodiment 1 or 2. (Embodiment 5)

[0015] According to this embodiment, the specific surface area, pore diameter ratio, and average major axis diameter of the primary particles are controlled to specific values. This improves the performance of adsorbing or capturing anions in the resin. The hydrotalcite compound particles according to this embodiment are expected to be used as anion scavenger suitable for electronic materials such as semiconductor encapsulants.

[0016] The following describes the embodiments. The following description of preferred embodiments is essentially illustrative. The embodiments described below are not intended to limit any of these embodiments, their application methods, or their uses.

[0017] First, the hydrotalcite-type compound particles according to the present embodiment will be described.

[0018] The specific surface area of the hydrotalcite-type compound particles according to the present embodiment is 18 m ２ ／ / g or more. When the specific surface area is 18 m ２ / g or more, the chloride ion adsorption capacity is excellent. The specific surface area is preferably 20 m ２ / g or more, more preferably 22 m ２ / g or more. The upper limit of the specific surface area is not particularly limited. However, in consideration of the possibility of magnesium or aluminum being dissolved, the specific surface area is preferably 150 m ２ / g or less, more preferably 130 m ２ / g or less.

[0019] The pore size distribution of the hydrotalcite-type compound particles according to the present embodiment is obtained by a mercury intrusion porosimetry method. In the present embodiment, the ratio of the second peak diameter μ １ to the first peak diameter μ ２ (μ ２ / μ １ ) is 100 or less. Here, the first peak diameter μ １ is the pore diameter corresponding to the first peak observed within the pore diameter range of 0.01 to 0.5 μm in the pore size distribution. The first peak is the peak corresponding to the maximum pore volume value within the aforementioned pore diameter range. The second peak diameter μ ２ is the pore diameter corresponding to the second peak observed within the pore diameter range of 0.5 to 100 μm. The second peak is the peak corresponding to the maximum pore volume value within the aforementioned pore diameter range.

[0020] When the aforementioned ratio (μ ２ / μ １ ) is 100 or less, the chloride ion adsorption capacity is excellent. The aforementioned ratio (μ ２ / μ １ ) is preferably 98 or less, more preferably 95 or less. The lower limit of the aforementioned ratio (μ ２ / μ １ ) is not particularly limited. A preferred ratio (μ ２ / μ １) is 5 or more. A more preferred ratio (μ ２ / μ １ ) is 10 or more.

[0021] In the pore distribution obtained by the mercury intrusion porosimetry of the hydrotalcite-type compound particles according to the present embodiment, among the peaks observed in the respective pore diameter ranges of 0.01 to 0.5 μm or 0.5 to 100 μm, the peak showing the maximum pore volume (ml / g) is defined as the peak corresponding to the maximum pore volume value within the pore diameter range.

[0022] The average major axis diameter of the primary particles contained in the hydrotalcite-type compound particles according to the present embodiment is 0.01 to 0.30 μm. When the average major axis diameter of the primary particles is outside the above range, sufficient dispersibility in a resin may not be obtained, or the chlorine ion scavenging ability may not be sufficiently exhibited. The average major axis diameter of the primary particles is preferably 0.03 to 0.25 μm, more preferably 0.04 to 0.20 μm.

[0023] The average minor axis diameter of the primary particles contained in the hydrotalcite-type compound particles according to the present embodiment is not particularly limited. From the viewpoint of dispersibility, the preferred average minor axis diameter of the primary particles is in the range of 0.002 to 0.08 μm.

[0024] The particle shape of the primary particles contained in the hydrotalcite-type compound particles according to the present embodiment is preferably plate-like or spherical. With the above shape, aggregated particles having high dispersibility in a resin can be formed.

[0025] In the particle size distribution of the hydrotalcite-type compound particles according to the present embodiment, D50 which is the 50% average particle diameter is preferably 0.1 to 30.0 μm, more preferably 0.2 to 25.0 μm, still more preferably 0.5 to 20 μm. When the D50 is outside the above range, the dispersibility of the hydrotalcite-type compound particles in the resin may decrease, or the chlorine ion scavenging ability may not be sufficiently exhibited.

[0026] The total pore volume obtained by the mercury intrusion method for hydrotalcite compound particles according to this embodiment is preferably 0.5 to 3.0 ml / g, more preferably 1.0 to 2.9 ml / g, and even more preferably 1.6 to 2.8 ml / g. If the total pore volume is outside the above range, the chloride ion scavenging ability may not be fully exhibited.

[0027] The composition of the hydrotalcite compound particles according to this embodiment is not particularly limited. For example, the hydrotalcite compound particles contain magnesium (Mg), aluminum (Al), and zinc (Zn). This composition is generally referred to as the Mg-Al system. A more specific example of the composition of the hydrotalcite compound particles according to this embodiment is a hydrotalcite-type particle represented by the following composition formula.

[0028] (Mg １－ｙ Zn ｙ ) １－ｘ Al ｘ ・(OH) ２ An ｎ－ ｐ mH ２ O 0.2 ≤ x ≤ 0.5, 0 ≤ y ≤ 0.6, 0 < m ≤ 1, p = x / n, An: n-valence anion

[0029] The Mg / Al molar ratio of the hydrotalcite compound particles according to this embodiment is not particularly limited. Preferably, the molar ratio is in the range of 1.0 to 4.0. If the molar ratio is within this range, hydrotalcite can be synthesized in a single phase. Furthermore, sufficient chloride ion scavenging ability can be achieved.

[0030] The particle shape of the hydrotalcite compound particles according to this embodiment is not particularly limited. A preferred example of the particle shape is spherical. This shape enhances the dispersibility of the hydrotalcite compound particles in the resin.

[0031] Next, a method for producing hydrotalcite compound particles according to the present embodiment will be described.

[0032] Hydrotalcite compound particles according to this embodiment can be obtained by mixing an alkaline aqueous solution containing anions, an aqueous magnesium solution, and an aqueous aluminum salt solution, aging the resulting mixture, adding a pH adjuster to the aged mixture, and drying it.

[0033] A preferred example of the alkaline aqueous solution containing anion in this embodiment is a mixed alkaline aqueous solution comprising an aqueous solution containing anion and an alkaline hydroxide aqueous solution.

[0034] Preferred examples of aqueous solutions containing anions include aqueous solutions containing one or more of the following: sodium carbonate, potassium carbonate, sodium phosphate, sodium silicate, sodium sulfate, organic carboxylates, organic sulfonates, and organic phosphates.

[0035] Preferred examples of alkali hydroxide aqueous solutions include sodium hydroxide aqueous solution, potassium hydroxide aqueous solution, ammonia aqueous solution, and urea aqueous solution.

[0036] Examples of magnesium aqueous solutions that can be used in this embodiment include magnesium sulfate aqueous solution, magnesium chloride aqueous solution, and magnesium nitrate aqueous solution. Alternatively, a slurry containing well-dispersed magnesium oxide powder or magnesium hydroxide powder may be used as a substitute.

[0037] Examples of aluminum salt aqueous solutions in this embodiment include aluminum sulfate aqueous solution, aluminum chloride aqueous solution, and aluminum nitrate aqueous solution. Preferred examples are aluminum sulfate aqueous solution and aluminum chloride aqueous solution. Alternatively, a slurry containing well-dispersed aluminum oxide powder or aluminum hydroxide powder may be used.

[0038] The mixing order of the anion-containing alkaline aqueous solution, magnesium aqueous solution, and aluminum aqueous solution is not particularly limited. Alternatively, each aqueous solution or slurry may be mixed simultaneously. Preferably, an aqueous solution or slurry containing pre-mixed magnesium and aluminum is added to the anion-containing alkaline aqueous solution.

[0039] Furthermore, the method of adding each aqueous solution may be either by adding the aqueous solution all at once, or by continuously adding the aqueous solution dropwise.

[0040] The temperature of the aqueous solution or slurry obtained by mixing the magnesium aqueous solution and the aluminum aqueous solution is preferably 30 to 80°C, more preferably 40 to 70°C. When the temperature of the aqueous solution or slurry is within this range, the reaction proceeds uniformly. As a result, particle growth is promoted. Therefore, hydrotalcite compound particles with a low BET value can be obtained.

[0041] The temperature during the maturation reaction is preferably 40 to 105°C, more preferably 45 to 100°C. Hydrotalcite compounds will be formed even at temperatures below 40°C. However, considering the effects of the season and the heat of neutralization, additional equipment such as cooling devices will be required. Therefore, temperatures below 40°C are not economical. If the temperature exceeds 105°C, growth in the direction of the plate surface is accelerated. As a result, BET may decrease.

[0042] The reaction time for the maturation reaction is preferably 1 to 16 hours. If the reaction time for the maturation reaction is less than 1 hour, it is difficult to obtain the desired particles. A reaction time for the maturation reaction exceeding 16 hours is not economical.

[0043] Preferably, a cake is obtained by suction filtration of the matured slurry. Alternatively, a washed cake is obtained by washing the obtained cake with pure water.

[0044] Next, preferably, a pH adjusting agent is added to the matured slurry, cake, or washed cake. The pH adjusting agent increases dispersibility. As a result, it is expected that the desired particles can be obtained. The pH adjusting agent used in this embodiment is not particularly limited. Examples of pH adjusting agents to be added include additives such as citric acid, acetic acid, malic acid, benzoic acid, sulfuric acid, sodium acetate, ascorbic acid, and lactic acid. One of the exemplified pH adjusting agents can be used alone. Alternatively, two or more of the exemplified pH adjusting agents may be used in combination. Furthermore, pH adjusting agents dispersed in a solvent such as water may also be used.

[0045] The amount of pH adjuster added is not particularly limited. The pH after adding the pH adjuster is preferably 11 or lower.

[0046] Afterward, it can be washed, dried, and crushed using conventional methods.

[0047] The drying method is not particularly limited. Examples of drying methods include natural drying, hot air drying, vacuum drying, static drying, and spray drying.

[0048] Next, the anion scavenger according to this embodiment will be described.

[0049] By including the hydrotalcite compound particles according to this embodiment in electronic materials such as semiconductor encapsulants, the hydrotalcite compound particles can be used as an anion scavenger.

[0050] Examples of the aforementioned anions include chloride ions, sulfate ions, and nitrate ions.

[0051] For the preparation of the anion scavenger according to this embodiment, the hydrotalcite compound particles according to this embodiment may be used alone. Alternatively, the hydrotalcite compound particles may be used in combination with other compounds. Furthermore, pre-processed hydrotalcite compound particles may be used.

[0052] Next, the resin composition according to this embodiment will be described.

[0053] The resin composition according to this embodiment contains hydrotalcite compound particles and / or anion scavengers according to Embodiments 1 to 4. That is, the hydrotalcite compound particles and / or anion scavengers according to this embodiment can be added to a resin composition containing anions and used in the preparation of the resin composition.

[0054] The resin composition according to this embodiment preferably contains 0.01 to 10 parts by weight of the hydrotalcite compound particles and / or anion scavenger per 100 parts by weight of resin. If the content is less than 0.01 parts by weight, the effect as a scavenger decreases. If the content exceeds 10 parts by weight, the effect becomes saturated, so there is no point in adding more than necessary. Furthermore, if an excessive amount of hydrotalcite compound particles is added, foaming is likely to occur. In addition, the resin composition may be affected by adverse effects such as poor appearance or initial discoloration.

[0055] The resin used in the resin composition according to this embodiment is not particularly limited. Examples of the resin include vinyl chloride resin, polyolefin resin, polyamide resin, vinyl acetate resin, polyimide resin, polystyrene, and polypropylene resin. One of these exemplified resins can be used alone. Alternatively, a mixed resin containing two or more mixed resins may be used.

[0056] Furthermore, the resin may contain plasticizers, other stabilizers, and other additives as needed.

[0057] Examples of preferred plasticizers include trimetate ester plasticizers containing trioctyl trimellitate (TOTM) and tri-n-octyl-n-decyl trimellitate, phthalate ester plasticizers containing diirodecyl phthalate (DIDP), diisononyl phthalate (DINP), and di-2-ethylhexyl phthalate (DOP), and polyester plasticizers containing polypropylene adipate and polypropylene sebacate.

[0058] Examples of other preferred stabilizers include zinc compounds, including zinc stearate, zinc laurate, and zinc ricinoleate; β-diketones, including dibenzoylmethane, stearoylbenzoylmethane, and dehydroacetic acid; phosphites, including alkylallyl phosphates and trialkyl phosphates; polyhydric alcohol compounds, including dipentaerythritol, pentaerythritol, glycerin, diglycerin, and trimethylolpropane; higher fatty acids, including stearic acid, lauric acid, and oleic acid; and phenylalanine compounds, including epoxidized linseed oil and epoxidized soybean oil.

[0059] Other additives that can be used include antioxidants including phenolic compounds, amine compounds, and phosphate compounds; gelation accelerators including polyesters having OH-substituted ends, acrylonitrile-styrene copolymers, and methylstyrene methacrylate copolymers; bulking agents including calcium carbonate, silica, glass beads, mica, and glass fibers; inorganic flame retardants including antimony trioxide, aluminum hydroxide, and zinc borate; brominated organic flame retardants and halogenated phosphate ester flame retardants; lubricants including stearic acid, polyethylene wax, calcium stearate, magnesium stearate, and barium stearate; and antifungal agents including triclosan, orthocide, San-Isol 100, and San-Isol 300.

[0060] When the hydrotalcite compound particles according to this embodiment are used as an anion-containing resin composition, the hydrotalcite compound particles may be subjected to surface treatment. For surface treatment, at least one surface treatment agent selected from higher fatty acids, anionic surfactants, higher fatty acid phosphate esters, coupling agents, and polyhydric alcohol esters can be used. By applying surface treatment, the hydrotalcite compound particles can be given even greater stability to the resin composition.

[0061] Examples of higher fatty acids include lauric acid, stearic acid, palmitic acid, oleic acid, and linoleic acid. Examples of higher fatty acid phosphate esters include stearyl ether phosphate, oleyl ether phosphate, and lauryl ether phosphate. Examples of polyhydric alcohol esters include sorbitan monooleate, sorbitan monolaurate, and stearate monoglyceride.

[0062] Examples of anionic surfactants include salts such as sodium lauryl sulfate, sodium dodecylbenzenesulfonate, sodium stearate, potassium oleate, and potassium castor oil.

[0063] Examples of coupling agents that can be used include silane-based, aluminum-based, titanium-based, and zirconium-based coupling agents.

[0064] The treatment method using the surface treatment agent is not particularly limited. For example, the surface treatment can be carried out by a wet reaction on the surface of the hydrotalcite compound particles. Alternatively, the surface of the hydrotalcite compound particles may be dry-surface-treated, for example, by a Henschel mixer. Or, the hydrotalcite compound particles and the surface treatment agent may simply be mixed together.

[0065] <Effect> The specific surface area, pore diameter ratio, and average major axis diameter of the primary particles of the hydrotalcite compound particles according to this embodiment can be controlled to specific values. This increases the ability to adsorb anions contained in the resin.

[0066] The reason is still unclear, but it can be considered as follows. The hydrotalcite compound particles according to this embodiment include primary particles and aggregated particles formed by the primary particles. Of these, the first peak diameter μ is presumed to be the pore diameter originating from the primary particles. １ The second peak diameter μ is presumed to be due to pores originating from aggregated particles. ２ Ratio (μ ２ / μ １The ) is small. In other words, the dispersed primary particles are densely packed, forming aggregated particles. Therefore, the primary particles can be easily dispersed with a small share. As a result, the contact efficiency between the anions and the primary particles is increased. Consequently, the hydrotalcite compound particles are thought to have excellent anion scavenging ability. In fact, the hydrotalcite compound particles according to this embodiment have excellent performance in adsorbing or capturing anions in resin.

[0067] Examples of this embodiment are shown below. However, this embodiment is not limited to these examples.

[0068] The BET specific surface area value was measured by the BET method using nitrogen.

[0069] To determine the average major axis diameter of the primary particles contained in hydrotalcite compound particles, the hydrotalcite compound particles were observed using a Hitachi High-Tech S-4800 microscope (magnification 20,000x). The major axis diameters of 100 primary particles shown in the micrographs obtained from the observation were evaluated. The average of the evaluated major axis diameters was defined as the average major axis diameter of the primary particles.

[0070] To determine the average minor axis diameter of the primary particles contained in hydrotalcite compound particles, the hydrotalcite compound particles were observed using a Hitachi High-Tech S-4800 microscope (magnification 20,000x). The minor axis diameters of 100 primary particles shown in the micrographs obtained from the observation were evaluated. The average of the evaluated minor axis diameters was defined as the average minor axis diameter of the primary particles. In the micrographs, the longest straight-line distance observed within the particle projection was defined as the major axis diameter of the primary particles of the hydrotalcite compound. In the same micrographs, the shortest straight-line distance (including the distance in the thickness direction) observed within the particle projection was defined as the minor axis diameter of the primary particles of the hydrotalcite compound.

[0071] The 50% average particle size D50 of hydrotalcite compound particles was evaluated using a particle size distribution measurement method compliant with JIS R1622. A particle size distribution analyzer (LMS-3000, manufactured by Seishin Corporation) was used for the measurement.

[0072] The pore distribution and total pore volume of hydrotalcite compound particles were obtained by measurement using an automated mercury porosimeter pore distribution analyzer, Autopore V9620 (manufactured by micromeritics). In the obtained pore distribution, the pore diameter corresponding to the maximum pore volume in the pore diameter range of 0.01 to 0.5 μm was the first peak diameter μ １ It was defined as follows. Similarly, the pore diameter corresponding to the maximum pore volume in the pore diameter range of 0.5 to 100 μm is the second peak diameter μ ２ It was defined as follows.

[0073] The Mg / Al (molar ratio) was measured using an ICP emission spectrometer iCAPPRO (manufactured by ThermoFisher Scientific). As a pretreatment, weighed hydrotalcite particles were mixed with hydrochloric acid. Subsequently, the resulting mixture was heated and dissolved to obtain the sample solution. The obtained sample solution was then diluted to a predetermined concentration using deionized water. Using the diluted sample solution, the target measurement value was obtained by the calibration curve method.

[0074] When observed using a Hitachi High-Tech S-4800 (10,000x magnification) instrument, the primary particles contained in hydrotalcite compound particles were considered spherical when no clear corners were observed. Conversely, when corners were observed, the primary particles were considered plate-like.

[0075] Anion adsorption capacity and anion capture capacity were evaluated as chlorine extraction rates. The chlorine extraction rate was determined by a chlorine adsorption performance evaluation test. Specifically, 2.0 parts by weight of hydrotalcite compound particles were added to 100 parts by weight of epoxy resin. This prepared a cured resin product. Subsequently, 5.0 g of the cured resin product and 50 mL of deionized water were placed in a sealed container and subjected to a heat extraction treatment at 120°C for 24 hours. The concentration of chlorine in the extract obtained after the heat extraction treatment was measured using ion chromatography (DIONEXINTEGRION, ThermoFisher Scientific). From the obtained chlorine concentration, the amount of chlorine extracted was determined. By considering the amount of chlorine extracted from epoxy resin without hydrotalcite compound particles (blank) as 100%, the chlorine extraction rate was calculated using the following formula (Equation 1). A chlorine extraction rate of 40% to 100% was rated as C (low effectiveness). A chlorine extraction rate of 20% to less than 40% was rated as B (good). A chlorine extraction rate of less than 20% was rated as A (particularly good). Chlorine extraction rate = (Amount of chlorine extracted when hydrotalcite compound particles obtained in the example or comparative example are included / Amount of chlorine extracted in the blank) × 100 (Equation 1)

[0076] (Example 1) Magnesium oxide (Wako Pure Chemical Industries) (33.8 g) and aluminum sulfate hexahydrate (Wako Pure Chemical Industries) (178.4 g) were dissolved in pure water (321.6 mL) so that the molar ratio of magnesium to aluminum was 3.0. A magnesium-aluminum mixture was prepared.

[0077] Next, a mixed alkaline aqueous solution was prepared by mixing sodium carbonate (Wako Pure Chemical Industries) (35.7 g), an 18 mol / L sodium hydroxide aqueous solution (141.3 g), and pure water (406 ml). The mixed alkaline aqueous solution was then added to the magnesium-aluminum mixture while maintaining its temperature at 60°C to prepare a reaction mixture solution. The reaction mixture solution was then aged at 95°C for 6 hours.

[0078] After maturation, the slurry was filtered by suction to prepare the cake. This cake was then washed with pure water to obtain a washed cake.

[0079] A dispersion was prepared by dispersing this washing cake in pure water (1000 mL) and acetic acid (9.5 g). The pH of the dispersion was 8. Subsequently, the prepared cake was obtained by suction filtration of the dispersion.

[0080] Next, the prepared cake, which had been dried at 120°C for 6 hours, was pulverized to obtain hydrotalcite compound particles according to this embodiment. The average short axis diameter of the obtained hydrotalcite compound particles was 0.040 μm. Furthermore, the hydrotalcite compound particles were spherical.

[0081] (Example 2) In Example 2, the manufacturing conditions were changed in various ways, as shown in Table 1. Under these conditions, hydrotalcite compound particles according to the present embodiment were obtained using the same procedure as in Example 1.

[0082] (Examples 3-5) In Examples 3-5, the manufacturing conditions were changed in various ways, as shown in Table 1. Under these conditions, a washed cake was obtained using the same procedure as in Example 1.

[0083] A dispersion was obtained by dispersing this washing cake in pure water (1000 mL) and acetic acid (3.3 g in Example 3, 7.5 g in Example 4, and 2.1 g in Example 5). The pH of the dispersion obtained in the previous step was 10 in Example 3.

[0084] The concentration of hydrotalcite compound particles in the dispersion (dispersion concentration) was 10% by weight in Example 3. In Example 4, the dispersion concentration was 10% by weight. In Example 5, the dispersion concentration was 5% by weight. The drying conditions for the dispersions in Examples 3 to 5 using a spray dryer were a drying temperature of 220°C, a nozzle air pressure of 0.44 MPa, and a spray speed of approximately 600 mL / min. Under these conditions, hydrotalcite compound particles according to this embodiment were obtained. The total pore volume of the hydrotalcite compound particles obtained in Example 3 was 2.58 ml / g. The total pore volume of the hydrotalcite compound particles obtained in Example 4 was 1.76 ml / g.

[0085] (Comparative Example 1) In Comparative Example 1, the manufacturing conditions were changed in various ways, as shown in Table 1. Under these conditions, hydrotalcite compound particles were obtained using the same procedure as in Example 1, except that acetic acid was not added.

[0086] (Comparative Examples 2 and 3) In Comparative Examples 2 and 3, the manufacturing conditions were changed in various ways, as shown in Table 1. Under these conditions, the same procedure as in Example 1 was used to obtain the washed cake.

[0087] After drying this washed cake at 120°C for 6 hours, hydrotalcite compound particles were obtained by pulverizing it.

[0088] (Comparative Examples 4 and 6) In Comparative Examples 4 and 6, the manufacturing conditions were changed in various ways, as shown in Table 1. Under these conditions, the same procedure as in Example 1 was followed until maturation.

[0089] After maturation, the slurry was treated in an autoclave at 110°C for 3 hours.

[0090] After processing, a cake was prepared by suction filtration of the slurry. A washed cake was obtained by washing this cake with pure water. This washed cake was dried at 120°C for 6 hours and then ground to obtain hydrotalcite compound particles.

[0091] (Comparative Example 5) In Comparative Example 5, the manufacturing conditions were changed in various ways, as shown in Table 1. Under these conditions, the operation was carried out in the same procedure as in Example 1 until maturation.

[0092] After maturation, the slurry was treated in an autoclave at 110°C for 3 hours.

[0093] After processing, a cake was prepared by suction filtration of the slurry. A washed cake was obtained by washing this cake with pure water. A 4% by weight slurry was obtained by dispersing this washed cake in pure water (1000 mL) using a homomixer.

[0094] The drying conditions for this slurry using a spray dryer were a drying temperature of 220°C, a nozzle air pressure of 0.44 MPa, and a spray rate of approximately 600 mL / min. Under these conditions, hydrotalcite compound particles were obtained. The total pore volume of the hydrotalcite compound particles obtained in Comparative Example 5 was 2.72 ml / g.

[0095] Table 1 shows the manufacturing conditions (Mg / Al, magnesium-aluminum mixture, mixed alkaline aqueous solution, aging temperature, and aging time) for each example and comparative example.

[0096]

[0097] The first peak diameter μ of the hydrotalcite compound particles obtained in each example and comparative example １ , the ２ Peak diameter μ ２ , μ ２ / μ １ Table 2 shows the BET, Mg / Al, D50, average major axis diameter of primary particles, particle shape, and chlorine extraction rate (compared to blank).

[0098]

[0099] The hydrotalcite compound particles according to this embodiment include primary particles and aggregated particles formed by the primary particles, and 18m ２ Having a specific surface area of ​​1 / g or more, and in the pore distribution obtained by the mercury intrusion method, the first peak diameter μ １ The second peak diameter μ for ２ Ratio (μ ２ / μ １ The ratio is 100 or less, and the average major axis diameter of the primary particles is 0.01 to 0.30 μm.

[0100] The hydrotalcite compound particles according to this embodiment have anion adsorption and anion scavenging capabilities. In particular, the hydrotalcite compound particles according to this embodiment have been shown to have excellent adsorption and scavenging properties for chloride ions.

[0101] The hydrotalcite compound particles according to this embodiment exhibit excellent anion-capturing properties, particularly for capturing chloride ions. Therefore, these hydrotalcite compound particles are expected to be used as an anion adsorbent for semiconductor encapsulating materials.

Claims

1. A material comprising primary particles and aggregated particles formed by the primary particles, 18m ２ Having a specific surface area of ​​1 / g or more, and in the pore distribution obtained by the mercury intrusion method, the first peak diameter μ １ The μ of the second peak diameter relative to ２ Ratio (μ ２ / μ １ Hydrotalcite compound particles wherein the ratio is 100 or less, and the average major axis diameter of the primary particles is 0.01 to 0.30 μm.

2. Hydrotalcite compound particles according to claim 1, wherein the 50% average particle size (D50) in the particle size distribution is 0.1 to 30.0 μm.

3. Hydrotalcite compound particles according to claim 1 or 2, wherein the shape of the primary particles is plate-like or spherical.

4. An anion scavenger comprising hydrotalcite compound particles according to claim 1 or 2.

5. A resin composition comprising the hydrotalcite compound described in claim 1 or 2.

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