US20120285880A1 - Powder, method of producing powder and adsorption apparatus - Google Patents

Powder, method of producing powder and adsorption apparatus Download PDF

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US20120285880A1
US20120285880A1 US13/497,635 US201013497635A US2012285880A1 US 20120285880 A1 US20120285880 A1 US 20120285880A1 US 201013497635 A US201013497635 A US 201013497635A US 2012285880 A1 US2012285880 A1 US 2012285880A1
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powder
particles
aggregates
sintered
slurry
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Shintaro Kobayashi
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Hoya Corp
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Hoya Corp
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    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/048—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing phosphorus, e.g. phosphates, apatites, hydroxyapatites
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    • B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
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    • B02C19/00—Other disintegrating devices or methods
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Definitions

  • the present invention relates to powder, a method of producing powder, and an adsorption apparatus.
  • Hydroxyapatite has high biocompatibility, high safety and the like. For these reasons, in recent years, the hydroxyapatite has been used generally as a material for stationary phase of a chromatography which is used when a bio medicine such as an antibody and a vaccine is purified and isolated.
  • the hydroxyapatite is used as the material for stationary phase of the chromatography, which can be produced as follows.
  • a first liquid containing calcium hydroxide is mixed with a second liquid containing phosphoric acid to obtain a mixture.
  • the calcium hydroxide is reacted with the phosphoric acid with stirring the mixture to obtain a slurry containing primary particles of hydroxyapatite and aggregates thereof.
  • the slurry containing the primary particles and the aggregates thereof is dried.
  • the dried primary particles and aggregates are granulated to thereby obtain secondary particles (powder) of the hydroxyapatite.
  • sintered powder The powder and the sintered powder are filled in a column (absorption apparatus) as a material for stationary phase (adsorbent) (see Patent Document 1).
  • the calcium hydroxide has low solubility to the first liquid. Due to the fact, the reaction of the calcium hydroxide and phosphoric acid becomes a solid-liquid reaction. Therefore, the aggregates of the primary particles formed in the slurry are non-uniform in an agglomeration degree thereof.
  • a particle in this specification means each of particles (secondary particles) and powder in this specification means that a plurality of particles gathered together.
  • Patent document 1 is JP-A 03-218460.
  • Powder including hydroxyapatite wherein the hydroxyapatite includes primary particles and secondary particles obtained by drying a slurry containing the primary particles and aggregates thereof and granulating the primary particles and the aggregates, and the powder comprising: mainly the secondary particles of the hydroxyapatite, wherein a bulk density of the powder is 0.65 g/mL or more and a specific surface area of the secondary particles is 70 m 2 /g or more.
  • the powder which has the bulk density within such a range and the particles having the specific surface area within such a range, has high strength and are capable of exhibiting excellent adsorption capability when it is used for an adsorbent used in an adsorption apparatus.
  • a sphericity of each of the secondary particles of the powder is in the range of 0.95 to 1.00.
  • the powder including the particles having high sphericity is used as an adsorbent used in an adsorption apparatus, it is possible to improve a filling ratio of the powder into an adsorbent filling space of the adsorption apparatus.
  • the secondary particles consisting the powder are classified so as to have an average particle size of 40 ⁇ 4 ⁇ m, wherein when a repose angle of the powder constituted of the classified secondary particles is measured, the repose angle is 27° or lower.
  • the powder having a low repose angle has a high flowability. Therefore, when the powder is used as an adsorbent used in an adsorption apparatus, it is possible to improve a filling efficiency of filling the powder into an adsorbent filling space of the adsorption apparatus.
  • the powder is sintered at a temperature of 700° C. to obtain sintered powder having particles, and then the particles of the sintered powder are classified so as to have an average particle size of 40+4 ⁇ m, wherein when a compressive particle strength of the classified particles is measured, the compressive particle strength is over 9.0 MPa.
  • the powder comprised of the particles having the compressive particle strength within such a range can have sufficiently strength when it is used as an adsorbent used in an adsorption apparatus.
  • the powder is sintered at a temperature of 700° C. to obtain sintered powder including particles each having a surface and micropores formed on the surface, wherein an average pore size of the micropores is 0.07 ⁇ m or less.
  • an average particle size of the secondary particles of the powder is in the range of 2 to 100 ⁇ m.
  • the powder of the particles having such an average particle size is preferably used to the present invention.
  • the powder When the powder is used for an adsorbent used in an adsorption apparatus, the powder exhibits high strength and excellent adsorption capability.
  • a method of producing the powder described in the above-mentioned items (1) comprises: mixing a first liquid containing a calcium raw material with a second liquid containing a phosphoric raw material to obtain a mixture; reacting the calcium raw material with the phosphoric raw material with stirring the mixture to obtain the slurry containing the primary particles of the hydroxyapatite and the aggregates thereof; crushing the aggregates contained in the slurry physically to disperse crushed aggregates in the slurry; and drying the slurry and granulating the crushed aggregates to obtain the powder mainly constituted from the secondary particles of the hydroxyapatite.
  • the bulk density of the powder is 0.65 g/mL or more and the specific surface area of the particles of the powder is 70 m 2 /g or more.
  • the crushing the aggregates physically is performed by a wet-type jet mill method in which the slurry is sprayed under a high pressure to obtain droplets of the slurry and the droplets are crashed to each other.
  • the method it is possible to reliably crush the aggregates of the primary particles of the hydroxyapatite. Therefore, it is possible to reliably obtain powder which has a bulk density of 0.65 g/mL or more and particles having a specific surface area of 70 m 2 /g or more.
  • an average particle size of the crushed aggregates is 1 ⁇ m or less.
  • the present invention it is possible to produce powder which is mainly constituted of hydroxyapatite by drying a slurry containing primary particles of the hydroxyapatite and then granulating the primary particles.
  • the bulk density of the powder is 0.65 g/mL or more and the specific surface area of the particles is 70 m 2 /g or more. Therefore, the powder has high strength and is capable of exhibiting excellent adsorption capability when it is used for an adsorbent used in an adsorption apparatus.
  • the method of producing powder of the present invention it is possible to reliably and easily produce the powder which has a bulk density of 0.65 g/mL or more and particles having a specific surface area of 70 m 2 /g or more.
  • FIG. 1 is a sectional view which shows one example of an adsorption apparatus to be used in the present invention.
  • FIG. 2 shows particle size distribution curves of aggregates contained in a slurry.
  • FIG. 2( a ) shows a particle size distribution curve of the aggregates before crushing.
  • FIG. 2( b ) shows a particle size distribution curve of the aggregates after crushing.
  • FIG. 3 shows electron microscope photographs of dried powders obtained in Example 1 and Comparative Example 1.
  • FIG. 4 shows electron microscope photographs in the vicinities of surfaces of particles of dried powders obtained in Example 1 and Comparative Example 1.
  • FIG. 5 shows micropore distribution curves in surfaces of particles of sintered powders obtained in Example 1 and Comparative Example 1.
  • FIG. 6 shows electron microscope photographs of dried powders obtained in Example 2 and Comparative Example 2.
  • FIG. 7 shows a particle size distribution curve of particles of dried powder obtained in Example 2.
  • FIG. 1 is a sectional view which shows one example of an adsorption apparatus to be used in the present invention. It is to be noted that in the following description, the upper side and the lower side in FIG. 1 will be referred to as “inflow side” and “outflow side”, respectively.
  • the inflow side means a side from which liquids such as a sample solution (i.e., a liquid containing a sample) and an eluate are supplied into the adsorption apparatus to separate (purify) a target material to isolate
  • the outflow side means a side located on the opposite side from the inflow side, that is, a side through which the liquids described above discharge out of the adsorption apparatus as a discharge liquid.
  • the adsorption apparatus 1 shown in FIG. 1 which is used for separating (isolating) the target material to isolate from the sample solution, includes a column 2 , a granular adsorbent (filler) 3 , and two filter members 4 and 5 .
  • the column 2 is constituted from a column main body 21 and caps 22 and 23 to be attached to the inflow-side end and outflow-side end of the column main body 21 , respectively.
  • the column main body 21 is formed from, for example, a cylindrical member.
  • Examples of a constituent material of each of the parts (members) constituting the column 2 including the column main body 21 include various glass materials, various resin materials, various metal materials, and various ceramic materials and the like.
  • An opening of the column main body 21 provided on its inflow side is covered with the filter member 4 , and in this state, the cap 22 is threadedly mounted on the inflow-side end of the column main body 21 .
  • an opening of the column main body 21 provided on its outflow side is covered with the filter member 5 , and in this state, the cap 23 is threadedly mounted on the outflow-side end of the column main body 21 .
  • the column 2 having such a structure as described above has an adsorbent filling space 20 which is defined by the column main body 21 and the filter members 4 and 5 , and at least a part of the adsorbent filling space 20 is filled with the adsorbent 3 (in this embodiment, almost the entire of the adsorbent filling space 20 is filled with the adsorbent 3 ).
  • a volumetric capacity of the adsorbent filling space 20 is appropriately set depending on the volume of a sample solution to be used.
  • a volumetric capacity is not particularly limited, but is preferably in the range of about 0.1 to 100 mL, and more preferably in the range of about 1 to 50 mL per 1 mL of the sample solution.
  • a size of the adsorbent filling space 20 By setting a size of the adsorbent filling space 20 to a value within the above range and by setting a size of the adsorbent 3 (which will be described later) to a value within a range as will be described later, it is possible to selectively isolate (purify) the target material to isolate (isolation material) from the sample solution. In other words, it is possible to reliably separate the isolation material such as a protein, an antibody and a vaccine from contaminating substances (foreign substances) other than the isolation material contained in the sample solution.
  • liquid-tightness between the column main body 21 and the caps 22 and 23 is ensured by attaching the caps 22 and 23 to the openings of the column main body 21 .
  • An inlet pipe 24 is liquid-tightly fixed to the cap 22 at substantially the center thereof, and an outlet pipe 25 is also liquid-tightly fixed to the cap 23 at substantially the center thereof.
  • the liquids described above are supplied to the adsorbent filling space 20 through the inlet pipe 24 and the filter member 4 .
  • the liquids supplied to the adsorbent filling space 20 pass through gaps between particles of the adsorbent 3 and then discharge out of the column 2 through the filter member 5 and the outlet pipe 25 .
  • the isolation material and the contaminating substances other than the isolation material contained in the sample solution (sample) are separated from each other based on a difference in degree of adsorption of each of the isolation material and the contaminating substances with respect to the adsorbent 3 and a difference in degree of affinity of each of the isolation material and the contaminating substances with respect to an eluate.
  • Each of the filter members 4 and 5 has a function of preventing the adsorbent 3 from discharging out of the adsorbent filling space 20 .
  • each of the filter members 4 and 5 is formed of a nonwoven fabric, a foam (a sponge-like porous body having communicating pores), a woven fabric, a mesh or the like, which is made of a synthetic resin such as polyurethane, polyvinyl alcohol, polypropylene, polyetherpolyamide, polyethylene terephthalate, or polybutylene terephthalate.
  • the adsorbent 3 used to the adsorption apparatus 1 is constituted of the powder of the present invention (secondary particles of hydroxyapatite) or sintered powder thereof.
  • the powder of present invention is obtained by drying a slurry containing primary particles of hydroxyapatite (Ca 10 (PO 4 ) 6 (OH) 2 ) and aggregates thereof, and granulating them.
  • the particles of the powder are mainly constituted of the hydroxyapatite. It is characterized in that a bulk density of the powder is 0.65 g/mL or more and a specific surface area of the particles of the powder is 70 m 2 /g or more.
  • the hydroxyapatite is constituted from a chemically stable apatite structure.
  • the hydroxyapatite is reliably used for the adsorbent which is provided with the adsorption apparatus.
  • a Ca/P ratio of the hydroxyapatite is in the range of about 1.64 to 1.70.
  • the separation material contained in the sample solution is specifically adsorbed to the adsorbent 3 with inherent adsorbability (carrying power) of the separation material. Then, the separation material is separated from the contaminating substances other than the separation material contained in the sample solution according to a difference between the adsorbalilities of the separation material and contaminating substances with respect to the adsorbent 3 , and thus is purified.
  • the bulk density of secondary particles (powder) of the hydroxyapatite may be 0.65 g/mL or more, and more preferably is in the range of about 0.70 to 0.95 g/mL or more. It is considered that the secondary particles having the bulk density within such a range have a heavyweight and gaps in the particle are lowered. In other words, the secondary particles can exhibit high strength because the secondary particles have a high filling density. Therefore, when the secondary particles are used as the adsorbent 3 , it is possible to assist a long life of the adsorbent 3 .
  • the specific surface area of the particles of the powder may be 70 m 2 /g or more, and more preferably is in the range of about 75 to 100 m 2 /g.
  • the powder which is constituted of the particles having a high specific surface area within such a range makes it possible to increase an opportunity to make the isolation material contact with the adsorbent 3 , thereby improving interaction between the isolation material and adsorbent 3 , when the powder is used as the adsorbent 3 . Therefore, the adsorbent 3 exhibits excellent adsorption capability with respect to the isolation material.
  • particles of powder having a high bulk density generally, have a low specific surface area.
  • the bulk density is 0.65 g/mL or more and the specific surface area of the particles is 70 m 2 /g or more.
  • the primary particles of the hydroxyapatite have a fine columnar shape, and the primary particles having the fine columnar shape complicatedly intervene with each other.
  • gaps between the primary particles tend to be too large in primary particles having an indefinite shape, a plate shape and a spherical shape, so that it is difficult to maintain both the high bulk density and the large specific surface area.
  • a form (shape) of the secondary particles namely the adsorbent 3 is preferably a granulated shape (granular shape) as shown in FIG. 1 .
  • a sphericity of each of the secondary particles is preferably in the range of about 0.95 to 1.00 and more preferably in the range of about 0.97 to 1.00.
  • a repose angle of such powder is preferably 27° or lower and more preferably in the range of about 25 to 22° when such a repose angle is measured by using the secondary particles classified to an average particle size in the range of 40 ⁇ 4 ⁇ m.
  • the secondary particles of the powder having such a low repose angle have high flowability and can assist the improvement of the operability (filling efficiency) when the secondary particles are filled into the adsorbent filling space 20 as the adsorbent 3 .
  • an average pore size of micropores formed on the surface thereof is preferably 0.07 ⁇ m or less, and more preferably in the range of about 0.04 to 0.06 ⁇ m.
  • the average pore size of the micropores is preferably 0.05 ⁇ m or less, and more preferably in the range of about 0.02 to 0.04 ⁇ m.
  • Such secondary particles are classified to the average particle size in the range of 40 ⁇ 4 ⁇ m.
  • a compressive particle strength (breaking strength) of the classified secondary particles (powder) is preferably 2.0 MPa or larger, and more preferably in the range of about 2.4 to 3.0 MPa.
  • a compressive particle strength (breaking strength) of the classified particles of the sintered powder is preferably 9 MPa or larger, and more preferably in the range of about 9.4 to 10 MPa.
  • a compressive particle strength of the particles is preferably 7.0 MPa or larger, and more preferably in the range of about 7.3 to 8.0 MPa.
  • the powder and the sintered powder each having the compressive particle strength within such a range have enough strength to be used for the adsorbent 3 .
  • an average particle size of the secondary particles is not particularly limited, but is preferably in the range of about 2 to 100 ⁇ m, more preferably in the range of about 2 to 80 ⁇ m, and even more preferably in the range of about 3 to 10 ⁇ m.
  • the secondary particles having such an average particle size are reliably used for the present invention.
  • the secondary particles can exhibit high strength and superior adsorption capability.
  • the adsorbent filling space 20 of the adsorption apparatus of the present invention may be partially filled with the adsorbent 3 (e.g., a part of the adsorbent filling space 20 located on its one side where the inlet pipe 24 is provided may be filled with the adsorbent 3 ). In this case, the remaining part of the adsorbent filling space 20 may be filled with another adsorbent.
  • the powder of the present invention as described above can be produced by the method of producing the powder of the present invention as follows.
  • a first liquid containing a calcium raw material such as calcium hydroxide as a calcium source is mixed with a second liquid containing a phosphate raw material such as phosphoric acid as a phosphoric source to obtain a mixture.
  • the calcium raw material is reacted with the phosphate raw material with stirring the mixture to obtain a slurry containing primary particles of hydroxyapatite and aggregates thereof.
  • These operations are referred to as a first step [S 1 ].
  • the aggregates contained in the slurry are crushed physically, so that the crushed aggregates are dispersed in the slurry. This operation is referred to as a second step [S 2 ].
  • the slurry is dried, and then the crushed aggregates are granulated to obtain powder which is mainly constituted from secondary particles of the hydroxyapaite. This operation is referred to as a third step [S 3 ].
  • a calcium hydroxide dispersion liquid containing calcium hydroxide (first liquid) is mixed with a phosphoric acid aqueous solution containing phosphoric acid (second liquid) to obtain the mixture.
  • the calcium hydroxide is reacted with the phosphoric acid with stirring the mixture to obtain the slurry containing the aggregates of the primary particles of hydroxyapatite.
  • the phosphoric acid aqueous solution (second liquid) is dropped into the calcium hydroxide dispersion liquid (first liquid) in a vessel (not shown) while the calcium hydroxide dispersion liquid is stirred.
  • the mixture of the calcium hydroxide dispersion liquid and the phosphoric acid aqueous solution are prepared.
  • the calcium hydroxide is reacted with the phosphoric acid in the mixture to obtain the slurry containing the aggregates of the hydroxyapatite.
  • power for stirring the mixture containing the phosphoric acid aqueous solution and the calcium hydroxide dispersion liquid is not particularly limited to a specific power, but preferably in the range of about 0.75 to 2.0 W and more preferably in the range of about 0.925 to 1.85 W per 1 L of the mixture (slurry).
  • the stirring power By setting the stirring power to a value within the above range, it is possible to further improve the efficiency of the reaction between the calcium hydroxide and the phosphoric acid.
  • a content of the calcium hydroxide in the calcium hydroxide dispersion liquid is preferably in the range of about 5 to 15 wt % and more preferably in the range of about 10 to 12 Wt %.
  • a content of the phosphoric acid in the phosphoric acid aqueous solution is preferably in the range of about 10 to 25 wt % and more preferably in the range of about 15 to 20 Wt %.
  • a rate of dropping the phosphoric acid aqueous solution into the calcium hydroxide dispersion liquid is preferably in the range of about 1 to 40 L/hr and more preferably in the range of about 3 to 30 L/hr.
  • the phosphoric acid aqueous solution is preferably dropped (added) into (to) the calcium hydroxide dispersion liquid for a length of time from about 5 to 32 hours, and more preferably for a length of time from about 6 to 30 hours.
  • the phosphoric acid aqueous solution is dropped into the calcium hydroxide dispersion liquid in such a period of time to react the calcium hydroxide with the phosphoric acid, it is possible to sufficiently synthesize hydroxyapatite. It is to be noted that even if the time for dropping the phosphoric acid aqueous solution into the calcium hydroxide dispersion liquid is prolonged to exceed the above upper limit value, it cannot be expected that the reaction between the calcium hydroxide and the phosphoric acid will further proceed.
  • fine particles of hydroxyapatite synthetic material
  • a chemical structure of such fine particles includes positively-charged parts and negatively-charged parts. Therefore, Van der Waals' forces (intermolecular force) are made between the positively-charged parts in the chemical structure of one fine particle of the fine particles and the negatively-charged parts in the chemical structure of the other fine particle of the fine particles. By this Van der Waals' forces, the one fine particle and the other fine particle adhere to each other to obtain a pre-aggregate.
  • aggregates hydroxyapatite (synthetic material) (hereinafter, simply referred to as “aggregates”).
  • the aggregates make a viscosity of the slurry increase gradually.
  • the aggregates of the primary particles of hydroxyapatite contained in the slurry obtained in the above step [S 1 ] are physically crushed. Then, the crushed aggregates are dispersed in the slurry.
  • a method of physically crushing the aggregates of the primary particles of hydroxyapatite is not particularly limited, but examples thereof include a wet-type jet mill method, a ball mill method and the like.
  • the wet-type jet mill method includes steps of spraying a slurry under high pressure to obtain droplets of the slurry and crashing the droplets to each other.
  • the ball mill method includes steps of placing the slurry into a closed vessel with spherical objects constituted of ceramics such as zirconia and rotating the closed vessel. Among them, it is preferred that the wet-type jet mill method is used.
  • the wet-type jet mill method is a method as follows: First, high pressure is added to the slurry in which the aggregates of the primary particles of hydroxyapatite are dispersed. Next, by spraying the slurry, the slurry is introduced into an opposing crash chamber, a ball crash chamber or a single nozzle chamber in a state of droplets of the slurry. By doing so, the droplets of the slurry are crashed to each other to crush the aggregates.
  • the aggregates of the primary particles of hydroxyapatite are crushed reliably. Therefore, it is possible to reliably obtain powder (secondary particles) of hydroxyapatite which will be obtained in a later step [S 3 ] so that the bulk density of the powder is 0.65 g/mL or more and the specific surface area of the secondary particles is 70 m 2 /g or more.
  • An average particle size of the crushed aggregates is preferably 1 ⁇ m or less and more preferably in the range of about 0.1 to 0.6 ⁇ m.
  • a method of adding a surfactant or a dispersant to disperse the primary particles into the slurry may be used as the method of dispersing the primary particles into the slurry other than the method of physically crushing the aggregates of the primary particles as this embodiment.
  • the added surfactant or dispersant remains in the powder of hydroxyapatite during a step of drying the slurry in the later step [S 3 ]. Therefore, in order to remove them, it is needed that the powder of hydroxyapatite is sintered at a temperature of 800° C. or higher. When the powder is sintered at such a temperature, a specific surface area of the particles of the powder is lowered. Therefore, it is substantially impossible for the former method to set the specific surface area of the particles to 70 m 2 /g or more as the powder of the present invention.
  • the slurry containing the aggregates crushed and obtained in the above step [S 2 ] is dried and then the crushed aggregates is granulated, so that powder (dried powder) mainly constituted from the secondary particles of hydroxyapatite is obtained.
  • the aggregates in which the primary particles of hydroxyapatite are aggregated are crushed to obtain aggregates of a small size in the above step [S 2 ]. Therefore, in the powder of hydroxyapatite obtained in the present step [S 3 ], a bulk density thereof becomes 0.65 g/mL or more and a specific surface area of the particles becomes 70 m 2 /g or more.
  • a method of drying the slurry is not particularly limited to a specific method, but a spray drying method is preferably used. According to such a method, it is possible to reliably obtain powder including particles having a predetermined particle size for a short period of time by granulating the crushed aggregates.
  • a drying temperature of the slurry is preferably in the range of about 75 to 250° C. and more preferably in the range of about 95 to 220° C. By setting the drying temperature to a value within the above range, it is possible to obtain powder which has a high bulk density and the secondary particles having a large specific surface area.
  • the method of producing the powder according to the present embodiment is suitable to produce powder containing particles having an intended particle size in the range of about 2 to 100 ⁇ m (in particular, about 3 to 10 ⁇ m).
  • such powder can be sintered to obtain sintered powder. This makes it possible to improve compressive particle strength (breaking strength) of the particles of the powder (sintered powder).
  • a sintering temperature of the powder is preferably in the range of about 200 to 900° C. and more preferably in the range of about 400 to 700° C.
  • the present invention is not limited thereto.
  • the method of producing the powder according to the present invention may further include a pre-step before the step [S 1 ], an intermediate step between the step [S 1 ] and the step [S 2 ] or between the step [S 2 ] and the step [S 3 ], and a post-step after the step [S 3 ] for any purpose.
  • an ambient temperature during the dropping process was set to normal temperature (25° C.)
  • a stirring power of the slurry in which the phosphoric acid aqueous solution was dropped into the calcium hydroxide dispersion liquid was set to 1.7 W with respect to 1 L of the slurry.
  • a particle size distribution curve of each of the aggregates contained in the slurry before crushing and the aggregates contained in the slurry after crushing was measured by using a particle size distribution analyzer (“MT 3300 ” produced by Microtrac).
  • the aggregates contained in the slurry could be crushed by using the wet-type jet mill apparatus. Concretely, it found that the aggregates could be crushed by an average particle size of 0.74 ⁇ m.
  • the slurry containing the crushed aggregates was spray-dried at a temperature of 210° C. using a spray drier (“MAD-6737R” manufactured by MATSUBO Corporation) to thereby granulate hydroxyapatite contained in the slurry. In this way, particulate secondary particles (dried powder) were obtained. Thereafter, the thus obtained secondary particles (dried powder) (hydroxyapatite powder) were classified by using a cyclone classifier (“TC-15” produced by NISSHIN ENGINEERING INC.) to obtain particles having a median particle size of about 40 ⁇ m.
  • TC-15 produced by NISSHIN ENGINEERING INC.
  • the thus obtained powder (secondary particles) was confirmed to be hydroxyapatite by a powder X-ray diffractometry.
  • the bulk densities of the dried powder and the sintered powders obtained in the Example 1 were improved by about 10% as compared with the bulk densities of the dried powder and the sintered powders obtained in the Comparative Example 1. From these results, it is considered that not only gaps in the particle of the formed dried powder but also gaps in the particle of the formed sintered powders became small by crushing the aggregates of their primary particles contained in the slurry, so that a filling density in the tube became high.
  • the sphericities of the particles of the dried powder and the sintered powders obtained in the Example 1 were improved as compared with the sphericities of the particles of the dried powder and the sintered powders obtained in the Comparative Example 1. Further, as clearly seen from the electron microscope photographs in FIG. 3 , the sphericity of each particle of the dried powder obtained in the Example 1 was higher than the sphericity of each particle of the dried powder obtained in the Comparative Example 1. In addition to that, each surface of the particles of the dried powder obtained in the Example 1 was smooth.
  • Electron microscope photographs in the vicinities of the surfaces of the particles of the dried powders obtained in the Example 1 and the Comparative Example 1 are shown in FIG. 4 .
  • Example 1 Each of the sintered powders sintered at the sintering temperatures of 400° C. and 700° C. and obtained in the Example 1 and the Comparative Example 1 was subjected to a pore size analyzer (“Micromeritics AutoPore 9200 ” produced by Shimadzu Corporation). Then, micropore distribution curves in the surfaces of the particles of each of the sintered powders were measured by using a mercury intrusion technique.
  • a pore size analyzer (“Micromeritics AutoPore 9200 ” produced by Shimadzu Corporation).
  • MT-1001 produced by SEISHIN ENTERPRISE CO., LTD.
  • Example 1 Each of the dried powders (secondary particles) and the sintered powders sintered at the sintering temperatures of 400° C. and 700° C., which were obtained in the Example 1 and the Comparative Example 1, were subjected to a compression testing machine (“MCT-W200-J” manufactured by Shimadzu Corporation) to obtain compressive particle strengths of the particles thereof.
  • a compression testing machine (“MCT-W200-J” manufactured by Shimadzu Corporation) to obtain compressive particle strengths of the particles thereof.
  • the sphericities of the particles of the dried powder and the sintered powders obtained in the Example 1 were higher than those of the particles of the dried powder and the sintered powders obtained in the Comparative Example 1.
  • the surfaces of the particles of the dried powder and the sintered powders obtained in the Example 1 were smooth. Due to the results, the repose angles of the dried powder and the sintered powders obtained in the Example 1 became low. From these results, it is considered that it is possible to improve operability in filling each of the dried powder and the sintered powders obtained in the Example 1 into a filling space of a column.
  • the slurry containing the crushed aggregates was spray-dried at a temperature of 110° C. by using a small spray drier (“Mobile Minor Spray Dryer” manufactured by Niro Inc., a spray system is a twin-fluid atomizing system, a tip flow path is 300 ⁇ m). Then, hydroxyapatite contained in the slurry was granulated to obtain particulate secondary particles (dried powder).
  • a small spray drier (“Mobile Minor Spray Dryer” manufactured by Niro Inc., a spray system is a twin-fluid atomizing system, a tip flow path is 300 ⁇ m).
  • the dried powder obtained in the Example 2 had particles having a high sphericity and had a particle size distribution curve as shown in FIG. 7 . In addition to that, it was not confirmed that particles having a large particle size of 30 ⁇ m or larger were mixed in the dried powder obtained in the Example 2.
  • the sphericity of the particles of the dried powder obtained in the Comparative Example 2 was clearly lower than that of the particles of the dried powder obtained in the Example 2. Furthermore, many particles having the particle size of 30 ⁇ m or larger were mixed in the dried powder obtained in the Comparative Example 2. That is, it was difficult to obtain particles having the particle size of 10 ⁇ m or less because the aggregates in themselves were aggregated in a particle size of a few dozen ⁇ m.
  • the powder according to the present invention is mainly constituted from the secondary particles of the hydroxyapatite obtained by drying slurry containing the primary particles of the hydroxyapatite and the aggregates thereof, and then granulating the primary particles and the aggregates.
  • the bulk density of the powder is 0.65 g/mL or more and the specific surface area of the secondary particles is 70 m 2 /g or more. Therefore, the powder according to the present invention has the high strength and is capable of exhibiting the excellent adsorption capability when it is used for the adsorbent the adsorption apparatus has. Accordingly, the powder according to the present invention has industrial applicability.

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