Method and apparatus for preparing high-purity crystalline silica

Patent metadata

Field	Value
Publication number	US-9624110-B2
Application number	US-201514742828-A
Country	US
Kind code	B2
Filing date	Jun 18, 2015
Priority date	Dec 18, 2012
Publication date	Apr 18, 2017
Grant date	Apr 18, 2017

Abstract

The present disclosure provides a method and apparatus for preparing high-purity crystalline silica particles by mixing colloidal silica with an organic base to form a mixed sol. The mixed sol is heated up to a reaction temperature of about 180 degrees Celsius or above, which is held for a reaction time of about 8 to about 168 hours for a hydrothermal synthesis process in the mixed sol. A gravitational setting or a centrifugation is performed on the mixed sol to provide precipitates from the mixed sol. The precipitates are washed with deionized water to remove residual organic base. The washed precipitates are dried at about 60 to about 80 degrees Celsius and are collected and packaged to obtain high-purity crystalline silica particles.

First claim

What is claimed is:

1. A method for preparing high-purity crystalline silica particles, comprising:
pre-treating colloidal silica with an ion-exchange resin to purify the colloidal silica;
mixing the colloidal silica with an organic base to obtain a mixed sol;
heating up the mixed sol to a reaction temperature of about 180 degrees Celsius or above, and holding the reaction temperature for a hydrothermal synthesis process in the mixed sol for a reaction time of about 8 to about 168 hours;
performing a gravitational settling or a centrifugation on the mixed sol to provide precipitates from the mixed sol;
washing the precipitates with deionized water to remove residual organic base;
drying the washed precipitates at about 60 to about 80 degrees Celsius; and

collecting and packaging dried precipitates to obtain high-purity crystalline silica particles.

2. The method according to claim 1 , further comprising:
preparing the colloidal silica including amorphous silica particles prior to mixing with the organic base,
wherein the amorphous silica particles have an average diameter ranging from about 5 nm to about 25 μm.

3. The method according to claim 2 , wherein:
a weight fraction of silica in the mixed sol is about 1 part to about 50 parts,

a weight fraction of the organic base in the mixed sol is about 3 parts to about 90 parts, and
the weight fraction of the silica, the weight fraction of the organic base, and a weight fraction of water in the mixed sol form 100 parts in total.

4. The method according to claim 1 , wherein a content of total metal impurities are reduced from above 700 ppm in the colloidal silica to less than about 100 ppm in the high-purity crystalline silica particles after the hydrothermal synthesis process.

5. The method according to claim 1 , wherein a content of total metal impurities are reduced from above 50 ppm in the colloidal silica to less than about 5 ppm in the high-purity crystalline silica particles after the hydrothermal synthesis.

6. The method according to claim 2 , wherein:
the amorphous silica particles have an average diameter ranging from about 10 nm to about 3000 nm,
a weight fraction of silica in the mixed sol is about 3 parts to about 30 parts,
a weight fraction of the organic base in the mixed sol is about 5 parts to about 30 parts, and
the weight fraction of the silica, the weight fraction of the organic base, and the weight fraction of water in the mixed sol form 100 parts in total.

7. The method according to claim 1 , wherein the reaction temperature ranges from about 180 to about 300 degrees Celsius and the reaction time ranges from 8 hours to about 168 hours.

8. The method according to claim 1 , wherein, when the colloidal silica includes mono-disperse particles, the high-purity crystalline silica particles are single-crystal silica particles with uniform sizes.

9. The method according to claim 1 , wherein the organic base combines with and removes metal impurities from the mixed sol to provide the high-purity crystalline silica particles.

10. The method according to claim 1 , further comprising:
after the hydrothermal synthesis process, cooling down the mixed sol before performing the gravitational settling or the centrifugation on the mixed sol.

11. The method according to claim 5 , wherein a uranium content is below 0.02 ppb.

12. A method for preparing high-purity crystalline silica particles, comprising:
selecting the organic base according to a boiling point thereof, wherein the selected organic base includes fatty amines, alcohol amines, amides, esters cyclic amines, aromatic amines, naphthalene amines, polyamines, polyethyleneimine (PEI), or a combination thereof;
mixing colloidal silica with the organic base to obtain a mixed sol;
heating up the mixed sol to a reaction temperature of about 180 degrees Celsius or above, and holding the reaction temperature for a hydrothermal synthesis process in the mixed sol for a reaction time of about 8 to about 168 hours;
performing a gravitational settling or a centrifugation on the mixed sol to provide precipitates from the mixed sol;
washing the precipitates with deionized water to remove residual organic base;
drying the washed precipitates at about 60 to about 80 degrees Celsius; and

collecting and packaging dried precipitates to obtain high-purity crystalline silica particles.

13. The method according to claim 12 , further comprising:
preparing the colloidal silica including amorphous silica particles prior to mixing with the organic base,
wherein the amorphous silica particles have an average diameter ranging from about 5 nm to about 25 μm.

14. The method according to claim 13 , further comprising:
a weight fraction of silica in the mixed sol is about 1 part to about 50 parts,

a weight fraction of the organic base in the mixed sol is about 3 parts to about 90 parts, and
the weight fraction of the silica, the weight fraction of the organic base, and a weight fraction of water in the mixed sol form 100 parts in total.

15. The method according to claim 13 , wherein:
the amorphous silica particles have an average diameter ranging from about 10 nm to about 3000 nm,
a weight fraction of silica in the mixed sol is about 3 parts to about 30 parts,
a weight fraction of the organic base in the mixed sol is about 5 parts to about 30 parts, and
the weight fraction of the silica, the weight fraction of the organic base, and the weight fraction of water in the mixed sol form 100 parts in total.

16. The method according to claim 12 , wherein a content of total metal impurities are reduced from above 700 ppm in the colloidal silica to less than about 100 ppm in the high-purity crystalline silica particles after the hydrothermal synthesis process.

17. The method according to claim 12 , wherein a content of total metal impurities are reduced from above 50 ppm in the colloidal silica to less than about 5 ppm in the high-purity crystalline silica particles after the hydrothermal synthesis.

18. The method according to claim 12 , wherein the reaction temperature ranges from about 180 to about 300 degrees Celsius and the reaction time ranges from 8 hours to about 168 hours.

19. The method according to claim 12 , wherein, when the colloidal silica includes mono-disperse particles, the high-purity crystalline silica particles are single-crystal silica particles with uniform sizes.

20. The method according to claim 12 , wherein a uranium content in the prepared high-purity crystalline silica particles is below 0.02 ppb.

Assignees

• Univ Changzhou

Inventors

• Jiang Xingmao
• Zhang Tao
• Jia Hong

Classifications

• C30B7/10 Primary

  by application of pressure, e.g. hydrothermal processes · CPC title

• C01B33/18

  Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof (preparation of aerogels by dehydrating gels C01B33/158; treatment to enhance the pigmenting or filling properties C09C) · CPC title

• C30B29/60

  characterised by shape · CPC title

• B01J19/0066

  Stirrers (mixing per se B01F) · CPC title

• C30B29/18

  Quartz · CPC title