Method of producing fluoroapatite powder, fluoroapatite powder, and adsorption apparatus

Patent metadata

Field	Value
Publication number	US-10407306-B2
Application number	US-56875309-A
Country	US
Kind code	B2
Filing date	Sep 29, 2009
Priority date	Sep 30, 2008
Publication date	Sep 10, 2019
Grant date	Sep 10, 2019

Abstract

A method of producing fluoroapatite powder by using a calcium compound, a phosphate compound, and a fluorine compound as a raw material is provided. The method comprises: preparing a slurry containing fluoroapatite produced from the raw material by using a wet process; applying an ultrasonic wave to the slurry; and drying the slurry to obtain the fluoroapatite powder mainly constituted of the fluoroapatite. The method provides fluoroapatite powder having improved particle strength. Further, an adsorption apparatus including the fluoroapatite powder is also provided.

First claim

What is claimed is:

1. A method of producing fluoroapatite powder from raw materials consisting of a calcium compound, a phosphate compound, a fluorine compound, and water, the method comprising:
preparing a slurry containing fluoroapatite primary particles mainly constituted of fluoroapatite from the raw materials at a pH of 2.5 to 4.5;
applying an ultrasonic wave to the slurry; and
drying the slurry to which the ultrasonic wave is applied to granulate the fluoroapatite primary particles contained in the slurry to obtain the fluoroapatite powder mainly constituted of the fluoroapatite,
wherein applying the ultrasonic wave to the slurry is carried out by using an ultrasonic washing machine having an ultrasonic tank containing water, wherein the slurry is put in a container and then the container containing the slurry is put in the ultrasonic tank, and wherein in such a state, when a total amount of the slurry and the water is 180 L, a power of the ultrasonic wave to be applied to the slurry is in the range of 500 to 2500 W, and
wherein the fluoroapatite powder has a compressive particle strength of 5.4 MPa or more, and the compressive particle strength is measured for fluoroapatite powder particles having an average particle size is 40±5 μm.

2. The method as claimed in claim 1 , wherein the step of applying the ultrasonic wave to the slurry is carried out after the fluoroapatite is produced.

3. The method as claimed in claim 1 , wherein a time of applying the ultrasonic wave to the slurry is in the range of 10 minutes to 10 hours.

4. The method as claimed in claim 1 , wherein an amount of the fluoroapatite primary particles contained in the slurry is 20 wt % or less.

5. The method as claimed in claim 1 , wherein the calcium compound is calcium hydroxide.

6. The method as claimed in claim 1 , wherein the phosphate compound is phosphoric acid.

7. The method as claimed in claim 1 , wherein the fluorine compound is hydrogen fluoride.

8. The method as claimed in claim 1 , wherein the slurry containing the fluoroapatite primary particles is obtained by reacting the calcium compound and the phosphate compound in water to obtain a slurry containing hydroxyapatite having hydroxyl groups and the water, and then reacting the hydroxyapatite and the fluorine compound having fluorine atoms in the hydroxyapatite slurry so that at least a part of the hydroxyl groups of the hydroxyapatite is substituted by the fluorine atoms of the fluorine compound to thereby obtain the fluoroapatite primary particles.

9. The method as claimed in claim 1 , wherein the slurry containing the fluoroapatite primary particles is obtained by preparing a first mixture consisting of the calcium compound and water, and a second mixture consisting of the phosphate compound and the fluorine compound having fluorine atoms and water, dropping the second mixture into the first mixture so that hydroxyapatite having hydroxyl groups is prepared, and then at least a part of the hydroxyl groups of the hydroxyapatite is substituted by the fluorine atoms of the fluorine compound to thereby obtain the fluoroapatite primary particles.

10. The method as claimed in claim 1 , wherein the pH of the slurry during its preparation is 2.5 to 3.4.

11. The method as claimed in claim 1 , wherein the pH of the slurry during its preparation is 2.5 to 3.00.

12. The method of claim 1 , wherein the fluoroapatite is adapted to be formed by substituting hydroxyl groups of hydroxyapatite present on a surface and an inside thereof by fluorine atoms of the fluorine compound, and
wherein a rate of substitution of the hydroxyl groups by the fluorine atoms is 75% or more.

13. A method of producing fluoroapatite powder from raw materials consisting of a calcium compound, a phosphate compound, a fluorine compound, and water, the method comprising:
preparing a slurry containing fluoroapatite primary particles mainly constituted of fluoroapatite from the raw materials at a pH of 2.5 to 4.5;
applying an ultrasonic wave to the fluoroapatite primary particles in the slurry without collecting the fluoroapatite primary particles from the slurry; and
drying the slurry to which the ultrasonic wave is applied to granulate the fluoroapatite primary particles contained in the slurry to obtain the fluoroapatite powder mainly constituted of the fluoroapatite,
wherein applying the ultrasonic wave to the slurry is carried out by using an ultrasonic washing machine having an ultrasonic tank containing water, wherein the slurry is put in a container and then the container containing the slurry is put in the ultrasonic tank, and wherein in such a state, when a total amount of the slurry and the water is 180 L, a power of the ultrasonic wave to be applied to the slurry is in the range of 500 to 2500 W, and
wherein the fluoroapatite powder has a compressive particle strength of 5.4 MPa or more, and the compressive particle strength is measured for fluoroapatite powder particles having an average particle size is 40±5 μm.

14. The method as claimed in claim 13 , wherein the pH of the slurry during its preparation is 2.5 to 3.4.

15. The method as claimed in claim 13 , wherein the pH of the slurry during its preparation is 2.5 to 3.00.

Assignees

• Ishikawa Tsuyoshi
• Ogawara Yoshiyuki
• Yoshitake Tomohiko
• Murakami Yukiko
• Hoya Corp

Inventors

• Ishikawa Tsuyoshi
• Ogawara Yoshiyuki
• Yoshitake Tomohiko
• Murakami Yukiko

Classifications

• C01B25/32 Primary

  Phosphates of magnesium, calcium, strontium, or barium · CPC title

• B01J2220/56

  Use in the form of a bed · CPC title

• B01J2220/52

  Sorbents specially adapted for preparative chromatography · CPC title

• B01J20/282

  Porous sorbents (ion exchange B01J39/00 - B01J41/00) · CPC title

• B01J20/048

  containing phosphorus, e.g. phosphates, apatites, hydroxyapatites · CPC title