10/28/2019 US4361542A - Zircon retrieval - Google Patents

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Zircon retrieval

Abstract
US4361542A
Zircon, ZrSiO4, is retrieved from zircon sand comprised of ZrSiO4 crystals and contaminants
United States
including SiO2 and iron by comminuting an aqueous slurry of the sand with iron means exposing the
contaminants, admixing the resulting comminuted sand slurry with concentrated nitric and
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hydrochloric acids producing ferric chloride in solution thereby removing its iron component,
admixing the resulting suspension with a occulating agent agglomerating the suspended particles,
admixing the resulting agglomerated mass with concentrated hydro uoric acid to dissolve its SiO2 Inventor: Ronald H. Arendt

component, recovering the resulting ZrSiO4, washing it with water and drying. Current Assignee : General Electric Co

Images (1) Worldwide applications

1981 US

Application US06/324,210 events

1981-11-23 Application led by General Electric Co

1981-11-23 Priority to US06/324,210

1981-11-23 Assigned to GENERAL ELECTRIC COMPANY, A

CORP. OF NY
Classi cations
1982-11-30 Application granted

C01B33/20 Silicates 1982-11-30 Publication of US4361542A

2001-11-23 Anticipated expiration

2019-10-27 Application status is Expired - Fee Related

Info: Patent citations (7), Cited by (6), Legal events, Similar

documents, Priority and Related Applications

External links: USPTO, USPTO Assignment, Espacenet, Global

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Claims (7) Hide Dependent

What is claimed is:

1. A process for retrieving ZrSiO4 from zircon sand, said zircon sand being comprised of ZrSiO4 and a signi cant amount of impurities including SiO2 and iron, which comprises
subjecting an aqueous slurry of said zircon sand to comminuting means comprised of iron means fracturing said zircon sand to an average particle size of less than about 5
microns, admixing the recovered fractured sand slurry with nitric acid and hydrochloric acid oxidizing its iron component to ferric ion and reacting said ferric ion with said
hydrochloric acid producing ferric chloride in solution, the concentration and amount of said nitric acid being su cient to oxidize said iron component to ferric ion leaving no
signi cant amount of said iron component, the concentration and amount of said hydrochloric acid being su cient to react with said ferric ion to form ferric chloride leaving no
signi cant amount of free ferric ion, admixing the resulting suspension with a occulating agent agglomerating the suspended particles therein, admixing the resulting

agglomerated mass with concentrated hydro uoric acid dissolving its SiO2 component, said hydro uoric acid being admixed in a concentration and amount su cient to
dissolve said SiO2 component leaving no signi cant amount of said SiO2 component, washing the resulting product with water and drying said product, said dried product
having an average particle size of less than about 5 microns and consisting essentially of ZrSiO4 and containing no signi cant amount of impurities.

2. The process according to claim 1 wherein said fractured sand has an average particle size which is less than one micron and said product has an average particle size
of less than one micron.

3. The process according to claim 1 wherein said nitric acid is admixed initially with said fractured sand and the resulting mixture is admixed with said hydrochloric acid.

Overall,
4. The process according to claim 1 wherein said nitric acid has a concentration of about 69 weight % to about 71 weight how satisfied
%, said hydrochloric acid are
has ayou with
concentration of
about 36.5 weight % to about 38 weight %, and said hydro uoric acid has a concentration of about 49 weight %. Google Patents?

5. The process according to claim 4 wherein said nitric acid and said hydrochloric acid are used in substantially equal amounts.Very satisfied

6. The process according to claim 1 wherein said occulating agent is organic and soluble in water. Somewhat satisfied

7. The process according to claim 6 wherein said occulating agent is in the form of an aqueous solution.
Neither satisfied nor dissatisfied

Description Somewhat dissatisfied

Very dissatisfied
The present invention is directed to retrieving small crystallite size zircon, ZrSiO4, from commercially available zircon sands, a naturally occurring mineral deposit.

Zircon particles are widely distributed in rocks, but commercially important concentrations are found in sands of certain areas of the world. Zircon sand, if it can be
su ciently bene ted at reasonable cost, has several potentially signi cant technological applications. Among these applications are its use as the arc tube material for
high pressure, high temperature plasma lamps, and as structural components in high temperature, highly corrosive environments.

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10/28/2019 US4361542A - Zircon retrieval - Google Patents
The chemical composition of commercial zircon sands is highly variable with the major contaminants in the form of tightly bound inclusions. Speci cally, the sands are
predominantly ZrSiO4, with as much as 10 weight % SiO2 as the major contaminant. There are smaller concentrations of various minerals, the speci c composition of
which is currently unknown, except that iron usually is a signi cant component. It is these contaminants and their potentially deleterious effect on the high temperature
chemical and mechanical properties that precludes the use of these sands directly in the cited applications.

The present invention is based in part on the observation that milling of the sand preferentially fractures grains through these impurity inclusions, which renders the
impurities susceptible to chemical agents which will not signi cantly attack the ZrSiO4. Normally, milling will introduce impurities by abrasion of the grinding medium.
However, if iron, i.e. steel, is used for the mill and grinding medium, it may be easily removed, without adverse effect on the ZrSiO4, under conditions which will also attack
the exposed second phase impurities.

Brie y stated, the present invention is a process for retrieving ZrSiO4 from zircon sand, said zircon sand being comprised of ZrSiO4 and a signi cant amount of impurities
including SiO2 and iron, which comprises subjecting an aqueous slurry of said zircon sand to comminuting iron means fracturing said zircon sand to an average particle
size of less than about 5 microns, admixing the recovered fractured sand slurry with nitric acid and hydrochloric acid oxidizing its iron component to ferric ion and
reacting said ferric ion with said hydrochloric acid producing ferric chloride in solution, the concentration and amount of said nitric acid being su cient to oxidize said
iron component to ferric ion leaving no signi cant amount of said iron component, the concentration and amount of said hydrochloric acid being su cient to react with
said ferric ion to form ferric chloride leaving no signi cant amount of free ferric ion, admixing the resulting suspension with a occulating agent agglomerating the
suspended particles therein, admixing the resulting agglomerated mass with concentrated hydro uoric acid dissolving its SiO2 component, said hydro uoric acid being
admixed in a concentration and amount su cient to dissolve said SiO2 component leaving no signi cant amount of said SiO2 component, washing the resulting ZrSiO4
product with water and drying said product, said dried product having an average particle size of less than about 5 microns and consisting essentially of ZrSiO4 and
containing no signi cant amount of impurities.

The accompanying FIGURE illustrates an embodiment of the present process.

In carrying out the present process, an aqueous slurry of the zircon sand is formed, suitable for comminuting the sand to a smaller particle size, as is customary in the
comminuting or grinding art. Preferably, the slurry is formed by admixing the zircon sand with water and the resulting slurry is comminuted at ambient temperature.

Comminuting iron means are used to comminute, i.e. grind or fracture, the zircon sand. Speci cally, the iron comminuting means do not introduce any impurities into the
sand which are not already present, or which are not removed or removable under the conditions of the present process. As a practical matter, the iron means is steel, i.e.
iron containing a hardening amount of carbon with the amount of carbon increasing to produce a steel of increased hardness. The present comminuting means can be in
a conventional form such as, for example, a steel mill containing steel milling or grinding balls.

The zirconium sand is comminuted, i.e. fractured, to an average particle size of less than about 5 microns, generally an average particle size ranging from about 0.2
micron up to about 5 microns. Since the zircon crystals are very inert chemically, fracturing of the sand to such average particle size is necessary to expose the impurities
su ciently, i.e. the tightly bound contaminating inclusions to allow their removal.

When comminution is completed, the fractured sand preferably is allowed to settle out so as to remove as much water as possible by decantation to produce a
signi cantly concentrated slurry. The resulting wet fractured zircon sand slurry is retrieved from the iron comminuting means and admixed with concentrated nitric acid
and concentrated hydrochloric acid. Although these acids can be admixed with the sand slurry simultaneously or singly, it is preferable to admix the nitric acid initially
with the sand slurry to oxidize its iron component to ferric ion. Such oxidation can be carried out at room temperature, but preferably, to shorten reaction time, it is carried
out at a temperature ranging from about 60° C. up to 100° C., and most preferably, at a temperature approaching the boiling point of water. During this reaction there is
signi cant effervescence of hydrogen and nitric oxide gases.

The nitric acid should be of a concentration and should be used in an amount su cient to oxidize the iron component to ferric ion leaving no signi cant amount of iron
remaining. Preferably, a slurry of the nitric acid and zircon sand is formed to insure intimate contact of the acid with the sand. For best results, the nitric acid is as
concentrated as is feasible to increase its action on the iron component and to cut down on reaction time. Most preferably, reagent grade, i.e. 69 weight % to 71 weight %,
nitric acid is used, and about three moles of such nitric acid would be required per iron atom.

Concentrated hydrochloric acid is added to chelate the ferric ion producing ferric chloride which is soluble in the acid medium. The hydrochloric acid is admixed in a
concentration and amount su cient to complex the ferric ion to produce ferric chloride, leaving no signi cant amount of free ferric ion. For best results, the hydrochloric
acid is as concentrated as is feasible to increase reaction rate and cut down on reaction time. Most preferably, reagent grade, i.e. 36.5 weight % to 38 weight %,
hydrochloric acid is used although hydrochloric acid ranging in concentration down to about 20 weight % is useful. Also, preferably, to shorten reaction time, the reaction
to produce ferric chloride is carried out at a temperature ranging from about 60° C. up to 100° C., and preferably, at a temperature approaching the boiling point of water.

The volume of each acid used in the present process depends on the particular contaminant which it is to remove. Speci cally, the volume of nitric acid and of
hydrochloric acid required must be determined empirically since it depends on the quantity of iron present. When these acids are of reagent grade, the volume of
hydrochloric acid generally ranges from about one part to about three parts for every one part of nitric acid. Generally, at temperatures of about 60° C. up to 100° C., the
reaction of reagent grade nitric and hydrochloric acids to accomplish the desired solution reactions usually requires a total time of about one hour. The resulting
suspension is yellow in color indicating ferric chloride in solution. Preferably, this suspension is allowed to cool to ambient temperature. This suspension does not settle
out to any signi cant extent and requires a occulating agent to agglomerate the suspended particles. Preferably, the suspension is diluted with water by a factor of
about 4 before addition of the occulating agent to promote removal of soluble impurities and reduce the acidity.

A occulating agent is admixed with the resulting suspension to agglomerate, i.e. to occulate and settle, the suspended particles. Preferably, the occulating agent is
used only in an amount necessary to settle the suspended particles. Also, preferably, the occulating agent is added as an aqueous solution, usually about 0.1 gram to
about 0.2 gram of occulating agent per 100 grams of water being satisfactory. Any occulating agent can be used which is removed under the conditions of the present
process, or which can be removed by ring the product produced by the present process at an elevated temperature, below 1000° C., preferably below 600° C. Preferably,
the occulating agent is organic and soluble in water. Preferably, the supernatant is decanted from the wet agglomerated mass. Also, preferably, the wet agglomerated
mass is washed with several comparable volumes of 0.01 M HCl, each time the product being settled with the occulant and the supernatant being decanted and
discarded. Based on simple dilution calculations, the soluble impurity levels can be conveniently reduced about 5-8 orders of magnitude.

The resulting wet agglomerated mass, preferably a resulting substantially concentrated slurry of the agglomerated mass, is washed or admixed with hydro uoric acid in a
concentration and amount su cient to dissolve its silica leaving no signi cant amount thereof remaining. The volume of hydro uoric acid required must be determined
empirically since it depends on the quantity of silica present. Preferably, a slurry of the hydro uoric acid and the wet agglomerated mass is formed to insure intimate
contact with the acid and dissolution of the silica. Preferably, reagent grade, i.e, 49 weight %, hydro uoric acid is used, although hydro uoric acid ranging in concentration
down to about 30 weight % is useful.

Upon completion of reaction with hydro uoric acid, which frequently takes about one hour at room temperature, and which can be determined empirically by standard
techniques such as wet chemical analysis, the resulting product, ZrSiO4, preferably is allowed to settle and the supernatant is decanted. The product is washed with
water, preferably distilled water, to remove hydro uoric acid therefrom.

If desired, a occulating agent may be admixed with the product slurry to occulate and settle the particles. Preferably, the occulating agent is used only in an amount
necessary to settle the suspended particles. Also, preferably, the occulating agent is added as an aqueous solution, usually about 0.1 gram to about 0.2 gram of

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occulating agent per 100 grams of water being satisfactory. Any occulating agent can be used which is removed under the conditions of the present process, or which
can be removed by ring the product produced by the present process at an elevated temperature below 1000° C., preferably below 600° C. Preferably, the occulating
agent is organic and soluble in water. Preferably, the supernatant is decanted from the agglomerated product. Also, preferably, the agglomerated product is washed with
several comparable volumes of 0.01 M HF to ush out soluble SiF6 -2 and to prevent its hydrolysis and reprecipitation as silica, each time the product being settled with
occulant and the supernatant being decanted, followed by a number of washes with distilled water to reduce residual acid contact.

The product, ZrSiO4, can be dried in a conventional manner. For example, it can be dried in air at room temperature. If necessary, it is taken to dryness and heated to 500°
to 600° C. in air to thermally decompose and remove any adsorbed organic occulant.

The dried ZrSiO4 crystals have an average particle size of less than about 5 microns, and preferably, an average particle size of less than one micron. They are white in
color, and free of impurities or do not contain any signi cant amount of impurities.

The present zircon powder has a wide variety of uses. For example, it can be hot pressed in a die at temperatures of about 1600° C. under pressures of about 4000 psi to
produce a dense polycrystalline product useful as a structural material.

This invention is further illustrated by the following examples:

EXAMPLE 1

Commercially available zircon sand having an average particle size of about 100 microns containing about 12 weight % impurities was used. Speci cally, the zircon sand
contained about 10 weight % SiO2 and about 1 weight % iron.

A one-liter steel mill containing steel milling balls was lled about 3/4 full with water. One kilogram of the sand was suspended in the water, and the resulting slurry was
milled at room temperature. After about 12 hours, the milling was stopped, the milled sand was allowed to settle, and the water was decanted therefrom.

The wet fractured sand in the form of an aqueous concentrated slurry was recovered from the mill and placed in a glass beaker. It had an average particle size of less
than one micron. About 200 cc of reagent grade nitric acid were admixed with the fractured sand slurry forming a slurry therewith which was heated, with stirring, to
about 80° C. The slurry showed considerable effervescence due to production of hydrogen and nitric acid gases indicating oxidation of iron to ferric ion. When the
effervescence substantially diminished, the slurry was cooled to about 60° C. and about 600 cc of reagent grade hydrochloric acid was admixed therewith and, with
stirring, the temperature of the mixture was raised to about 80° C. The resulting suspension turned deep yellow in color indicating production of ferric chloride in solution.
The yellow suspension was allowed to cool to room temperature.

The suspension was diluted with distilled water by a factor of about 4. An aqueous occulating solution comprised of 0.02 gram of anionic occulant (a polyamide imide
powder sold under the trademark Herco oc 821) in 20 grams of distilled water was then added to the stirred suspension. The occulating solution was used in an
amount su cient to agglomerate the suspended particles. The supernatant was decanted and the wet agglomerated mass was washed with several comparable
volumes of 0.01 M HCl, each time the product being settled with the aqueous occulating solution and the supernatant being decanted therefrom.

After the nal washing with 0.01 M HCl, the occulated mass, i.e. a substantially concentrated slurry of the occulated mass, was placed in a polyethylene beaker and
washed at room temperature with about 1000 cc of reagent grade hydro uoric acid which was su cient to solubilize the silica therein. The resulting product was allowed
to settle out, and the supernatant was decanted.

The product, ZrSiO4, was washed with several comparable volumes of 0.01 M HF. After the nal wash with 0.01 M HF, the product was washed several times with distilled
water to reduce acid content.

The product was taken to dryness and heated to 500° C.-600° C. in air for about one hour to decompose and thereby remove any adsorbed organic occulant.

The resulting product was white in color and had an average particle size of less than 1 micron.

Wet chemical analysis of a portion of the product showed that it was comprised of ZrSiO4 and that it did not contain any signi cant amount of impurities, i.e. its impurity
content was less than about 0.2% by weight of the total weight of the product.

EXAMPLE 2

A portion of the ZrSiO4 product produced in Example 1 were hot pressed in a die under a pressure of about 4000 psi at a temperature of about 1600° C. for about 30
minutes. The resulting product was a very dense polycrystalline material which could be useful as a structural component.

Patent Citations (7)

Publication number Priority date Publication date Assignee Title

GB223572A * 1923-10-17 1925-06-11 Etude Des Agglomeres Process for the commercial production of pure oxide of zirconium
Soc D

US1796170A * 1929-05-18 1931-03-10 Ward Leonard Electric Process of extracting zirconia from ores
Co

GB450053A * 1935-07-10 1936-07-09 Titanium Alloy Mfg Co An improved method of purifying zircon

GB559118A * 1942-07-03 1944-02-04 Titanium Alloy Mfg Co Improvements relating to the puri cation of crude zirconium compounds or ores

GB853301A * 1956-01-11 1960-11-02 Nat Res Dev Treatment of zircon

US3109704A * 1960-05-24 1963-11-05 Ass Lead Mfg Ltd Manufacture of zirconium oxide from zircon

US3849532A * 1969-03-06 1974-11-19 Dynamit Nobel Ag Method of preparing a zirconium oxide that is crystallized mostly or completely
in cubic form

Family To Family Citations

* Cited by examiner, † Cited by third party

Cited By (6)

https://patents.google.com/patent/US4361542A/en 3/8
10/28/2019 US4361542A - Zircon retrieval - Google Patents

Publication number Priority date Publication date Assignee Title

US5637281A * 1994-03-04 1997-06-10 Rgc Mineral Sands, Ltd. Process for the removal of from oxide coatings iron
zirconiferous material

US5958355A * 1994-12-02 1999-09-28 Atomic Energy Corporation Of South Africa Process for reacting a zirconia based material
Limited

US20030082089A1 * 2001-10-23 2003-05-01 Pavlik Robert S. Method and furnace for pure, fused oxide

WO2003097533A1 * 2002-05-22 2003-11-27 Commonwealth Scienti c And Industrial Process for removal of radioactive impurities from
Research Organisation zirconium containing materials

CN102830006A * 2011-12-18 2012-12-19 湖北兴发化工集团股份有限公司 Pretreatment method for silica through microwave
digestion

CN109205669A * 2018-11-19 2019-01-15 新特能源股份有限公司 The combined preparation process of zirconium chloride
and ocratation

Family To Family Citations

* Cited by examiner, † Cited by third party, ‡ Family to family citation

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Priority And Related Applications

Priority Applications (1)

Application Priority date Filing date Title

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US06/324,210 1981-11-23 1981-11-23 Zircon retrieval

Applications Claiming Priority (1)

Application Filing date Title

US06/324,210 1981-11-23 Zircon retrieval

Legal Events

Date Code Title Description

1981-11-23 AS Assignment Owner name: GENERAL ELECTRIC COMPANY, A CORP. OF NY

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST.;ASSIGNOR:ARENDT, RONALD

H.;REEL/FRAME:003955/0099

Effective date: 19811118

Owner name: GENERAL ELECTRIC COMPANY, A CORP. OF NY, NEW YORK

Free format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:ARENDT, RONALD

H.;REEL/FRAME:003955/0099

Effective date: 19811118

1986-07-04 REMI Maintenance fee reminder mailed

1986-11-30 LAPS Lapse for failure to pay maintenance fees

1986-11-30 STCH Information on status: patent discontinuation Free format text: PATENT EXPIRED DUE TO NONPAYMENT OF MAINTENANCE FEES UNDER 37 CFR
1.362

1987-02-17 FP Expired due to failure to pay maintenance fee Effective date: 19861130

Concepts

machine-extracted Download Filter table

Name Image Sections Count Query match

HCl claims,description 21 0

HCl

HF abstract,claims,description 14 0

HF

Iron(III) chloride abstract,claims,description 10 0

Cl-

Cl- Cl- Fe+3

Polyamide-imide description 1 0

Polyethylene (PE) description 1 0

SiF6 description 1 0

Steel description 7 0

Zirconium(IV) silicate abstract,claims,description,title 25 0

O-
O-
Si Zr+4
O-
O-

abrasion description 1 0

acid description 8 0

acids description 2 0

addition description 1 0

air description 3 0

https://patents.google.com/patent/US4361542A/en 5/8
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analytical methods description 2 0

anionic group description 1 0

aqueous solution claims,description 3 0

balls description 2 0

boiling description 2 0

carbon description 2 0

carbon description 2 0

chemical reaction description 6 0

chemical reaction reagent description 8 0

chemical substance by application description 1 0

coesite abstract,claims,description 12 0

contaminant description 2 0

cristobalite abstract,claims,description 12 0

deleterious description 1 0

diminished description 1 0

dissolution description 1 0

drying abstract,claims,description 3 0

effects description 1 0

fe3+ claims,description 16 0

Fe+3

ferric ion claims,description 16 0

ring description 2 0

occulating description 3 0

occulating agents abstract,claims,description 19 0

gases description 2 0

glass description 1 0

grinding description 4 0

hydrochloric acid abstract,description 14 0

hydrochloric acid claims,description 18 0

hydrogen description 1 0

H H

hydrogen description 1 0

hydrogen description 1 0

hydrogen chloride description 3 0

hydrogen peroxide description 1 0

HO OH

hydrolysis description 1 0

increased description 2 0

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inorganic minerals description 2 0

iron abstract,claims,description 27 0

iron abstract,claims,description 28 0

Fe

iron abstract,claims,description 28 0

materials description 3 0

media description 3 0

methods claims,description 17 0

mineral description 2 0

mixtures claims,description 4 0

moulding (composite fabrication) description 1 0

nitric acid claims,description 18 0

HO O-
N+

nitric oxide description 1 0

N O

nitric oxide description 1 0

oxidation description 2 0

oxidation reaction description 2 0

oxidative claims,description 2 0

particles abstract,claims,description 25 0

polyamide-imide description 1 0

polyethylene description 1 0

polyethylenes description 1 0

powders description 2 0

production description 2 0

products claims,description 28 0

quartz abstract,claims,description 12 0

reaction time description 4 0

reduced description 1 0

reprecipitation description 1 0

rock description 1 0

sand abstract,claims,description 36 0

silicium dioxide abstract,claims,description 12 0

O Si O

silicon dioxide abstract,claims,description 17 0

silicon dioxide abstract,claims,description 17 0

slurries abstract,claims,description 24 0

solutions claims,description 8 0

steel description 7 0

stirring description 2 0

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stishovite abstract,claims,description 12 0

substances description 5 0

supernatant description 8 0

suspension abstract,claims,description 12 0

tridymite abstract,claims,description 12 0

washing abstract,claims,description 4 0

water abstract,claims,description 22 0

zircon abstract,claims,description,title 45 0

zirconium description 1 0

Zr

zirconium description 1 0

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