# US 11,111,179 B2 · Non-fired monoliths

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- Number: US 11,111,179 B2
- Document ID: US11111179B2
- Status: Granted
- Kind: B2
- Application number: 16/754,290
- Filed: 2018-10-11
- Published: 2021-07-01
- Granted: 2021-09-07
- Earliest claimed: 2017-10-11
- Assignees: Katholieke Universiteit Leuven
- Applicants: Katholieke Universiteit Leuven
- Inventors: Tobias Hertel; Yiannis Pontikes
- Web page: https://patentgrep.com/patent/US11111179B2

## CPC

- C04B 28/008: {Mineral polymers other than those of the Davidovits type, e.g. from a reaction mixture containing waterglass}
- C04B 12/005: {Geopolymer cements, e.g. reaction products of aluminosilicates with alkali metal hydroxides or silicates}
- C04B 14/10: Clay {(sepiolite C04B14/042; grog C04B18/025)}
- C04B 18/0409: {Waste from the purification of bauxite, e.g. red mud}
- C04B 20/0048: {Fibrous materials}
- C04B 28/005: {containing gelatineous or gel forming binders, e.g. gelatineous Al(OH)3, sol-gel binders}
- C04B 40/024: {Steam hardening, e.g. in an autoclave}
- Y02P 40/10: Production of cement, e.g. improving or optimising the production methods; Cement grinding
- C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE
- Y02P: CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS

## Abstract

The invention relates to methods for manufacturing an inorganic polymer object from a precursor wherein the precursor consists of one or more or comprises one or more selected from the group consisting of gibbsite-containing bauxite, gibbsite containing residue of the Bayer process, thermally processed gibbsite-containing bauxite, and thermally processed gibbsite-containing residue of the Bayer process, the method comprising the steps of alkaline-activating said precursor, mixing the precursor, shaping the mixed precursor and hydrothermally curing the shaped precursor at a temperature between 70° C. and 350° C.

## Claims

### Claim 1

A method for manufacturing an inorganic polymer object from a precursor that comprises a gibbsite-containing residue or a thermally processed gibbsite-containing residue of the Bayer process, the precursor comprising less than 0.01 wt % silica fume, the method comprising:
alkaline-activating the precursor;
mixing the precursor;
shaping the precursor after the mixing; and
hydrothermally curing the precursor, after the shaping, at a temperature from 70° C. to 350° C. and under a pressure greater than 1 bar and less than 500 bar.

### Claim 2 (depends on 1)

The method according to claim 1, wherein the gibbsite containing residue comprises gibbsite in an amount greater than 2 wt %.

### Claim 3 (depends on 1)

The method according to claim 1, wherein the precursor further comprises a gibbsite containing bauxite or a thermally processed gibbsite containing bauxite.

### Claim 4 (depends on 1)

The method according to claim 1, wherein said precursor comprises up to 40 wt % one or more of a component selected from the group consisting of quartz sand, precipitated silica, natural clay, calcareous sand, thermally-activated clay, chemically-activated clay, mechanically-activated clay, fly ash from bituminous coal, subbituminous coal or lignite, gibbsite-containing electrostatic precipitation dust (ESP dust), aluminium salt cake, processed aluminium dross, CaCO3, CaO, Ca(OH)2, monocalcium silicate, dicalcium silicate, tricalcium silicate, metallurgical slag, EN 197-1 blended cement, cement kiln dust, soda-lime-silica glass or other glass compositions, thermally processed bauxite residue, and vitreous slag.

### Claim 5 (depends on 1)

The method according to claim 1, wherein the hydrothermal curing is performed under a pressure from 1 bar to 90 bar.

### Claim 6 (depends on 1)

The method according to claim 1, wherein the precursor consists of a naturally occurring mineral, of a rock, or of a residue from an ore subjected to the Bayer process.

### Claim 7 (depends on 1)

The method according to claim 1, wherein the precursor contains less than 15 wt % diaspore [(α-AlO(OH)] and less than 15 wt % boehmite [γ-AlO(OH)].

### Claim 8 (depends on 1)

The method according to claim 1, wherein the precursor has a normalized chemical composition, as deduced by X-Ray fluorescence analysis, comprising the following elements, expressed as oxides:
from 1 wt % to 60 wt % Fe2O3;
from 5 wt % to 80 wt % Al2O3;
from 0 wt % to 50 wt % SiO2;
from 0 wt % to 25 wt % TiO2;
from 0 wt % to 20 wt % Na2O; and
from 0 wt % to 20 wt % CaO.

### Claim 9 (depends on 1)

The method according to claim 1, wherein the precursor has, as determined by a thermogravimetric analysis carried out at a temperature between 25° C. to 1000° C., a loss on ignition or volatile substances from 1 wt % to 40 wt %.

### Claim 10 (depends on 1)

The method according to claim 1, wherein the alkaline-activating the precursor comprises contacting the precursor with an alkaline solution selected from one or more of the group consisting of hydroxides, silicates, sulfates, sulfides, sulfites, carbonates of Na- and/or K- and/or Ca, spent Bayer liquor, Na-aluminate solution, and a liquid component of bauxite residue slurry.

### Claim 11 (depends on 1)

The method according to claim 1, wherein the alkaline-activating the precursor comprises contacting the precursor with an alkaline solution having a 0.5 mol/L to 28 mol/L equivalent concentration for NaOH and a 0.5 mol/L to 22 mol/L equivalent concentration for KOH.

### Claim 12 (depends on 1)

The method according to claim 1, wherein the alkaline-activating the precursor comprises contacting the precursor with a solution that has a total molar ratio of SiO2/(Na2O+K2O) from 0 to 4 and a total molar ratio of H2O/(Na2O+K2O) from 5 to 200.

### Claim 13 (depends on 1)

The method according to claim 1, wherein shaping the precursor comprises casting the precursor into a mold, optionally followed by vibration, with a shaping pressure not exceeding 5 MPa.

### Claim 14 (depends on 1)

The method according to claim 1, wherein shaping the precursor comprises press-shaping the precursor at a pressure from 5 MPa to 80 MPa.

### Claim 15 (depends on 1)

The method according to claim 1, wherein the shaping of the precursor is performed for a time from 1 sec to 10 min.

### Claim 16 (depends on 1)

The method according to claim 1, wherein the hydrothermal curing is performed at a temperature from 90° C. to 350° C.

### Claim 17 (depends on 1)

The method according to claim 1, wherein the precursor comprises from 0 wt % to less than 0.01 wt % water-soluble silicate in the form of sodium silicate or potassium silicate.

### Claim 18 (depends on 1)

The method according to claim 1, wherein the precursor comprises from 0 wt % to less than 0.1 wt % fluoride.

### Claim 19 (depends on 1)

The method according to claim 1, wherein the precursor comprises a total from 0 wt % to less than 0.01 wt %, based on the total weight of the precursor, of ground granulated blast furnace slag, basic oxygen furnace slag, kaolin tailings, and coal gangue.

### Claim 20 (depends on 1)

The method according to claim 1, wherein the precursor further comprises from 0.05 wt % to 0.3 wt % fibers, based on the total weight of the precursor.