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Disponibilité de l'Abrégé et des Revendications

L'apparition de différences dans le texte et l'image des Revendications et de l'Abrégé dépend du moment auquel le document est publié. Les textes des Revendications et de l'Abrégé sont affichés :

  • lorsque la demande peut être examinée par le public;
  • lorsque le brevet est émis (délivrance).
(12) Brevet: (11) CA 2913682
(54) Titre français: PROCEDES POUR LA PREPARATION DE CHLORURE DE MAGNESIUM PAR LIXIVIATION PAR HCL DE DIVERS MATERIAUX
(54) Titre anglais: PROCESSES FOR PREPARING MAGNESIUM CHLORIDE BY HCI LEACHING OF VARIOUS MATERIALS
(51) Classification internationale des brevets (CIB):
  • C22B 3/10 (2006.01)
  • C01B 7/01 (2006.01)
  • C01F 5/02 (2006.01)
  • C01F 5/20 (2006.01)
  • C22B 3/46 (2006.01)
  • C22B 26/22 (2006.01)
(72) Inventeurs (Pays):
  • BOUDREAULT, RICHARD (Canada)
  • PRIMEAU, DENIS (Canada)
  • LABRECQUE-GILBERT, MARIE-MAXIME (Canada)
  • DUMONT, HUBERT (Canada)
(73) Titulaires (Pays):
  • ORBITE TECHNOLOGIES INC. (Canada)
(71) Demandeurs (Pays):
  • ORBITE TECHNOLOGIES INC. (Canada)
(74) Agent: BERESKIN & PARR LLP/S.E.N.C.R.L.,S.R.L.
(45) Délivré: 2017-06-13
(22) Date de dépôt: 2013-09-26
(41) Mise à la disponibilité du public: 2014-04-03
Requête d’examen: 2015-11-27
(30) Licence disponible: S.O.
(30) Langue des documents déposés: Anglais

(30) Données de priorité de la demande:
Numéro de la demande Pays Date
61/705,898 Etats-Unis d'Amérique 2012-09-26
61/713,795 Etats-Unis d'Amérique 2012-10-15
61/726,971 Etats-Unis d'Amérique 2012-11-15
61/837,715 Etats-Unis d'Amérique 2013-06-21

Abrégé français

Les procédés décrits peuvent être efficaces pour traiter divers matériaux comprenant plusieurs métaux différents. Ces matériaux peuvent être lessivés avec HCI pour obtenir un lixiviat et un solide. Ensuite, ils peuvent être séparés l'un de l'autre et un premier métal peut être isolé du lixiviat. Ensuite, un second métal peut encore être isolé du lixiviat. Les premier et second métaux peuvent chacun être sélectivement isolés du lixiviat. Cela peut se faire en contrôlant la température du lixiviat, en ajustant le pH, en réagissant davantage sur le lixiviat avec HCI, etc. Les métaux qui peuvent être récupérés sous forme de chlorures métalliques peuvent éventuellement être transformés en oxydes métalliques correspondants, ce qui permet de récupérer le HCI. Les différents métaux peuvent être choisis parmi l'aluminium, le fer, le zinc, le cuivre, l'or, l'argent, le molybdène, le cobalt, le magnésium, le lithium, le manganèse, le nickel, le palladium, le platine, le thorium, le phosphore, l'uranium, le titane, les terres rares et les métaux rares.


Abrégé anglais


The disclosed processes can be effective for treating various materials
comprising several
different metals. These materials can be leached with HCI for obtaining a
leachate and a
solid. Then, they can be separated from one another and a first metal can be
isolated from
the leachate. Then, a second metal can further be isolated from the leachate.
The first and
second metals can each be substantially selectively isolated from the
leachate. This can be
done by controlling the temperature of the leachate, adjusting pH, further
reacting the
leachate with HCI, etc. The metals that can be recovered in the form of metal
chlorides can
eventually be converted into the corresponding metal oxides, thereby allowing
for
recovering HCI. The various metals can be chosen from aluminum, iron, zinc,
copper, gold,
silver, molybdenum, cobalt, magnesium, lithium, manganese, nickel, palladium,
platinum,
thorium, phosphorus, uranium, titanium, rare earth element and rare metals.


Note : Les revendications sont présentées dans la langue officielle dans laquelle elles ont été soumises.

WHAT IS CLAIMED IS:
1. A process for treating a magnesium-containing material, said process
comprising :
leaching the magnesium-containing material with HCI so as to obtain a
leachate comprising magnesium ions, and a solid, and separating said solid
from said leachate;
controlling the concentration of HCI in the leachate so as to precipitate
a first metal in the form of a chloride, and removing the precipitate from the

leach ate;
controlling the concentration of HCI in the leachate so as to precipitate
a second metal in the form of a chloride, and removing the precipitate from
the leachate; and
reacting the leachate with HCI so as to precipitate the magnesium ions
in the form of MgCl2.
2. The process of claim1, further comprising heating said MgCl2.
3. The process of claim 1, further comprising heating said MgCl2 in the
presence of HCI.
4. The process of claim 1, further comprising heating said MgCl2 under
conditions effective for converting MgCl2 into MgO.
5. The process of any one of claims 1 to 4, wherein the first metal is Fe.
6. The process of any one of claims 1 to 4, wherein the second metal is Ni.
7. The process of any one of claims 1 to 6, wherein said solid is separated
from
said leachate at a temperature of at least 50 °C.
8. The process of any one of claims 1 to 6, wherein said solid is separated
from
said leachate at a temperature of at least 60 °C.
87

9. The process of any one of claims 1 to 6, wherein said solid is separated
from
said leachate at a temperature of at least 75 °C.
10. The process of any one of claims 1 to 6, wherein said solid is
separated from
said leachate at a temperature of at least 100 °C.
11. The process of any one of claims 1 to 10, wherein MgCl2 is
substantially
selectively precipitated from said leachate at a temperature of about 5 to
about 70 °C.
12. The process of any one of claims 1 to 10, wherein MgCl2 is
substantially
selectively precipitated from said leachate at a temperature of about 10 to
about 60 °C.
13. The process of any one of claims 1 to 10, wherein MgCl2 is
substantially
selectively precipitated from said leachate at a temperature of about 10 to
about 40 °C.
14. The process of any one of claims 1 to 10, wherein MgCl2 is
substantially
selectively precipitated from said leachate at a temperature of about 15 to
about 30 °C.
15. The process of any one of claims 1 to 14, comprising calcining MgCl2
into
MgO and recycling gaseous HCI so-produced by contacting it with water so
as to obtain a composition having a concentration of about 25 to about 45
weight % and using said composition for leaching said magnesium-
containing material.
16. The process of any one of claims 1 to 14, comprising calcining MgCl2
into
MgO and recycling gaseous HCI so-produced by contacting it with water so
as to obtain a composition having a concentration of about 18 to about 45
weight % and using said composition for leaching said magnesium-
containing material.
17. The process of any one of claims 1 to 16, comprising treating said
solid with
HCI, in the presence of a metal chloride, so as to separate Si from Ti that
are
contained therein.
88

18. The process of any one of claims 1 to 16, comprising treating said
solid with
HCI at a concentration of less than 20 % by weight, at a temperature of less
than 85 °C, in the presence of a metal chloride, so as to separate Si
from Ti
that are contained therein.
19. The process of claim 17 or 18, wherein said solid is treated with HCI
and
said metal chloride so as to obtain a liquid portion comprising Ti and a solid

portion containing Si and wherein said liquid portion is separated from said
solid portion.
20. The process of claim 19, wherein said solid is treated with HCI and
said
metal chloride so as to obtain a liquid portion comprising TiCI4.
21. The process of claim 20, wherein said process further comprises
converting
TiCI4 into TiO2.
22. The process of claim 20, wherein TiCI4 is converted into TiO2 by
solvent
extraction of a third liquid fraction and subsequent formation of titanium
dioxide from said solvent extraction.
23. The process of claim 22, wherein TiCI4 is reacted with water and/or a
base to
cause precipitation of TiO2.
24. The process of claim 22, wherein TiCI4 is converted into TiO2 by means
of a
pyrohydrolysis, thereby generating HCI.
25. The process of claim 22, wherein TiCI4 is converted into TiO2 by means
of a
pyrohydrolysis, thereby generating HCI that is recycled.
26. The process of any one of claims 19 to 25, wherein said metal chloride
is
MgCl2.
27. The process of any one of claims 19 to 25, wherein said metal chloride
is
ZnCl2.
28. The process of any one of claims 1 to 27, wherein said solid comprises
TiO2
and SiO2 and said solid is treated with Cl2 and carbon in order to obtain a
8 9

liquid portion and a solid portion, and wherein said solid portion and said
liquid portion are separated from one another.
29. The process of claim 28, wherein said liquid portion comprises TiCl2
and/or
30. The process of claim 28, wherein said liquid portion comprises TiCl4.
31. The process of claim 30 further comprising heating TiCI4 so as to
convert it
into TiO2.
32. The process of any one of claims 21 to 25 and 31, wherein obtained TiO2

purified by means of a plasma torch.
33. The process of any one of claims 1 to 6, wherein said process comprises

reacting said leachate with gaseous HCI so as to obtain said liquid and said
precipitate, said precipitate comprising aluminum ions and being formed by
crystallization of AICI3.cndot.6H2O.
34. The process of claim 33, wherein said process comprises reacting said
liquid
with dry gaseous HCI so as to obtain said liquid and said precipitate
comprising said aluminum ions, said precipitate being formed by
crystallization of AICI3.cndot.6H2O.
35. The process of claim 33 or 34, wherein said gaseous HCI has a HCI
concentration of at least 85 % by weight.
36. The process of claim 33 or 34, wherein said gaseous HCI has a HCI
concentration of at least 90 % by weight.
37. The process of claim 33 or 34, wherein said gaseous HCI has a HCI
concentration of about 95 % by weight.
38. The process of claim 33 or 34, wherein said gaseous HCI has a
concentration of about 90 % to about 95 % by weight.
39. The process of claim 33 or 34, wherein said gaseous HCI has a
concentration of about 90 % to about 99 % by weight.

40. The process of any one of claims 33 to 39, wherein during said
crystallization of AICI3.cndot.6H2O, said liquid is maintained at a
concentration of
HCI of about 25 to about 35 % by weight.
41. The process of any one of claims 33 to 40, wherein during said
crystallization of AICI3.cndot.6H2O, said liquid is maintained at a
concentration of
HCI of about 30 to about 32 % by weight.
42. The process of any one of claims 33 to 41, wherein said HCI is obtained

from said gaseous HCI so-produced.
43. The process of any one of claims 33 to 42, wherein said process
comprises
reacting said leachate with HCI recovered during said process and having a
concentration of at least 30 % as to obtain said liquid and said precipitate
comprising said aluminum ions, said precipitate being formed by
crystallization of AICI3.cndot.6H2O.
44. The process of any one of claims 33 to 43, wherein said crystallization
is
carried out at a temperature of about 45 to about 65 °C.
45. The process of any one of claims 33 to 43, wherein said crystallization
is
carried out at a temperature of about 50 to about 60 °C.
46. The process of any one of claims 33 to 45, wherein said crystallization
is
carried out at a temperature of about 45 to about 65 °C.
47. The process of any one of claims 33 to 45, wherein said crystallization
is
carried out at a temperature of about 50 to about 60 °C.
48. The process of any one of claims 1 to 47, wherein said process
comprises
separating said solid from said leachate and washing said solid so as to
obtain silica having a purity of at least 95 %.
49. The process of any one of claims 1 to 47, wherein said process
comprises
separating said solid from said leachate and washing said solid so as to
obtain silica having a purity of at least 98 %.
91

50. The process of any one of claims 1 to 47, wherein said process
comprises
separating said solid from said leachate and washing said solid so as to
obtain silica having a purity of at least 99 %.
51. The process of any one of claims 33 to 43, wherein said process
comprises
heating said precipitate at a temperature of at least 1200 °C for
converting
AlCl3.cndot.6H2O into Al2O3.
52. The process of any one of claims 33 to 43, wherein said process
comprises
heating said precipitate at a temperature of at least 1250 °C for
converting
AlCl3.cndot.6H2O into Al2O3.
53. The process of any one of claims 33 to 43, wherein said process
comprises
heating said precipitate at a temperature of at least 900 °C for
converting
AlCl3.cndot.6H2O into Al2O3.
54. The process of any one of claims 33 to 43, wherein said process
comprises
converting AlCl3.cndot.6H2O into alpha-Al2O3.
55. The process of any one of claims 33 to 43, wherein said process
comprises
heating said precipitate at a temperature of at least 350 °C for
converting
AlCl3.cndot.6H2O into Al2O3.
56. The process of any one of claims 33 to 43, wherein said process
comprises
heating said precipitate at a temperature of about 180 °C to about 250
°C or
of about 350 °C to about 500 °C for converting AlCl3.cndot.6H2O
into Al2O3.
57. The process of any one of claims 33 to 43, wherein said process
comprises
heating said precipitate at a temperature of about 375 °C to about 450
°C for
converting AlCl3.cndot.6H2O into Al2O3.
58. The process of any one of claims 33 to 43, wherein said process
comprises
heating said precipitate at a temperature of about 375 °C to about 425
°C for
converting AlCl3.cndot.6H2O into Al2O3.
92

59. The process of any one of claims 33 to 43, wherein said process
comprises
heating said precipitate at a temperature of about 385 °C to about 400
°C for
converting AlCl3°6H2O into Al2O3.
60. The process of any one of claims 33 to 43, wherein said process
comprises
converting AlCl3°6H2O into beta-Al2O3.
61. The process of any one of claims 33 to 43, wherein converting
AlCl3°6H2O
into Al2O3 comprises carrying out a calcination via a two-stage circulating
fluid bed reactor.
62. The process of any one of claims 33 to 43, wherein converting
AlCl3°6H2O
into Al2O3 comprises carrying out a calcination via a two-stage circulating
fluid bed reactor that comprises a preheating system.
63. The process of claim 62, wherein said preheating system comprises a
plasma torch.
64. The process of claim 63, wherein said plasma torch is effective for
preheating air entering into a calcination reactor.
65. The process of claim 63, wherein said plasma torch is effective for
generating steam that is injected into a calcination reactor.
66. The process of claim 63, wherein said plasma torch is effective for
generating steam that is as fluidization medium in a fluid bed reactor.
67. The process of process of any one of claims 33 to 43 and 51 to 66,
wherein
converting AlCl3°6H2O into Al2O3 comprises carrying out a one-step
calcination.
68. The process of process of any one of claims 33 to 43 and 51 to 66,
wherein
said process comprises converting AlCl3.cndot.6H2O into Al2O3 by carrying out
a
calcination of AlCl3°6H2O, said calcination comprising steam injection.
69. The process of claim 68, wherein steam is injected at a pressure of
about
200 to about 700 psig.
93

70. The process of claim 68, wherein steam is injected at a pressure of
about
300 to about 700 psig.
71. The process of claim 68, wherein steam is injected at a pressure of
about
400 to about 700 psig.
72. The process of claim 68, wherein steam is injected at a pressure of
about
550 to about 650 psig.
73. The process of claim 68, wherein steam is injected at a pressure of
about
575 to about 625 psig.
74. The process of claim 68, wherein steam is injected at a pressure of
about
590 to about 610 psig.
75. The process of any one of claims 68 to 74, wherein steam is injected
and a
plasma torch is used for carrying out fluidization.
76. The process of any one of claims 65 to 75, wherein overheated steam is
injected and a plasma torch is used for carrying out fluidization.
77. The process of any one of claims 65 to 75, wherein said steam is
overheated.
78. The process of any one of claims 33 to 43, wherein said process
comprises
converting AlCl3.cndot.6H2O into Al2O3 by carrying out a calcination of
AlCl3.cndot.6H2O
in which is provided by the combustion of a fossil fuel, carbon monoxide,
propane, natural gas, a Refinery Fuel Gas, coal, or chlorinated gases and/or
solvants.
79. The process of any one of claims 33 to 43, wherein said process
comprises
converting AlCl3.cndot.6H2O into Al2O3 by carrying out a calcination of
AlCl3.cndot.6H2O
that is provided by the combustion of gas mixture that is an incoming smelter
gas or a reducer offgas.
80. The process of any one of claims 33 to 43, wherein said process
comprises
converting AlCl3.cndot.6H2O into Al2O3 by carrying out a calcination of
AlCl3.cndot.6H2O
that is provided by the combustion of gas mixture that comprises :
94

CH4 : 0 to about 1% vol;
C2H6 : 0 to about 2% vol;
C3H8 : 0 to about 2% vol;
C4H10 : 0 to about 1% vol;
N2 : 0 to about 0.5% vol;
H2 : about 0.25 to about 15.1 % vol;
CO : about 70 to about 82.5 % vol; and
CO2 : about 1.0 to about 3.5% vol.
81. The process of claim 80, wherein O2 is substantially absent from said
mixture.
82. The process of any one of claims 33 to 43, wherein said process
comprises
converting AICI3.cndot.6H2O into Al2O3 by carrying out a calcination of
AICI3.cndot.6H2O
in which is provided by electric heating, gas heating, microwave heating.
83. The process of any one of claims 33 to 43, wherein converting
AICI3.cndot.6H2O
into Al2O3 comprises carrying out a calcination by means of fluid bed reactor.
84. The process of claim 83, wherein the fluid bed reactor comprises a
metal
catalyst chosen from metal chlorides.
85. The process of claim 83, wherein the fluid bed reactor comprises FeCI3,

FeCl2 or a mixture thereof.
86. The process of claim 83, wherein the fluid bed reactor comprises FeCI3.
87. The process of any one of claims 1 to 86, wherein said process is a
semi-
continuous process.
88. The process of any one of claims 1 to 86, wherein said process is a
continuous process.

89. The process of any one of claims 1 to 88, wherein said process is
effective
for providing a MgO recovery yield of at least 96 %.
90. The process of any one of claims 1 to 88, wherein said process is
effective
for providing a MgO recovery yield of about 96 to about 98 %.
91. The process of any one of claims 1 to 90, wherein said process is
effective
for providing a HCI recovery yield of at least 98 %.
92. The process of any one of claims 1 to 90, wherein said process is
effective
for providing a HCI recovery yield of at least 99 %.
93. The process of any one of claims 1 to 90, wherein said process is
effective
for providing a HCI recovery yield of about 98 to about 99.9 %.
94. The process of any one of claims 1 to 93, wherein leaching is carried
out at a
pressure of about 4 to about 10 barg.
95. The process of any one of claims 1 to 93, wherein leaching is carried
out at a
pressure of about 4 to about 8 barg.
96. The process of any one of claims 1 to 93, wherein leaching is carried
out at a
pressure of about 5 to about 6 barg.
97. The process of any one of claims 1 to 96, wherein said magnesium-
containing material is an industrial refractory material.
98. The process of any one of claims 1 to 96, wherein said magnesium-
containing material is red mud.
99. The process of any one of claims 1 to 98, wherein recovered HCI is
purified
and/or concentrated.
100. The process of claim 99, wherein the recovered HCI is purified by
means of
a membrane distillation process.
101. The process of claim 99, wherein the recovered HCI is treated with
H2SO4 so
as to reduce the amount of water present in the gaseous HCI.
96

102. The process of claim 101, wherein the recovered HCI is passed through
a
packed column so as to be in contact with a H2SO4 countercurrent flow so as
to reduce the amount of water present in the gaseous HCI.
103. The process of claim 102, wherein the column is packed with
polypropylene
or polytrimethylene terephthalate.
104. The process of any one of claims 99 and 101 to 103, wherein the
concentration of gaseous HCl is increased by at least 50 %.
105. The process of any one of claims 99 and 101 to 103, wherein the
concentration of gaseous HCI is increased by at least 60 %.
106. The process of any one of claims 99 and 101 to 103, wherein the
concentration of gaseous HCI is increased by at least 70 %.
107. The process of claim 99, wherein the recovered HCI is treated with
CaCl2 so
as to reduce the amount of water present in the gaseous HCl.
108. The process of claim 107, wherein the recovered HCI is passed through
a
column packed with CaCl2 so as to reduce the amount of water present in
the gaseous HCl.
109. The process of any one of claims 1 to 108, wherein process comprises
substantially selectively precipitating MgCl2 from said leachate under
conditions effective for controlling solubility of MgCl2 based on temperature
of said leachate.
110. The process of any one of claims 1 to 108, wherein process comprises
substantially selectively precipitating MgCl2 from said leachate under
conditions effective for controlling solubility of MgCl2 based on acid
concentration.
111. The process of any one of claims 1 to 108, wherein process comprises
substantially selectively precipitating MgCl2 from said leachate under
conditions effective for controlling solubility of MgCl2 based on HCI
concentration.
97

112. A process for preparing aluminum, said process comprising :
obtaining alumina by means of a process as defined in any one of
claims 51 to 68; and
converting said Al2O3 into aluminum.
113. The process of claim 112, wherein said conversion of Al2O3 into
aluminum is
carried out :
by means of the Hall-Héroult process;
by using a reduction environment and carbon at temperature below 200°C;

by means of the Wohler Process; or
by converting Al2O3 into Al2S3 and then converting Al2S3 into aluminum.
98


Une figure unique qui représente un dessin illustrant l’invention.

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États admin

Titre Date
(22) Dépôt 2013-09-26
(41) Mise à la disponibilité du public 2014-04-03
Requête d'examen 2015-11-27
(45) Délivré 2017-06-13

Taxes périodiques

Description Date Montant
Dernier paiement 2017-09-07 100,00 $
Prochain paiement si taxe applicable aux petites entités 2018-09-26 100,00 $
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Historique des paiements

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Enregistrement de documents 100,00 $ 2015-11-27
Dépôt 400,00 $ 2015-11-27
Taxe périodique - Demande - nouvelle loi 2 2015-09-28 100,00 $ 2015-11-27
Taxe périodique - Demande - nouvelle loi 3 2016-09-26 100,00 $ 2016-09-13
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Description du
Document
Date
(yyyy-mm-dd)
Nombre de pages Taille de l’image (Ko)
Description 2015-11-27 86 3 568
Abrégé 2015-11-27 1 23
Revendications 2015-11-27 18 633
Dessins 2015-11-27 20 425
Page couverture 2016-01-05 1 42
Abrégé 2016-04-26 1 14
Revendications 2016-04-26 19 647
Description 2016-04-26 87 3 595
Revendications 2016-09-07 12 385
Dessins représentatifs 2016-10-14 1 13
Poursuite-Amendment 2016-04-26 39 1 443
Correspondance 2015-12-08 1 151
Poursuite-Amendment 2015-12-17 1 28
Poursuite-Amendment 2016-01-26 9 624
Taxes 2016-09-13 1 33
Poursuite-Amendment 2016-06-07 4 322
Poursuite-Amendment 2016-09-07 15 512
Correspondance 2017-04-20 1 49
Abrégé 2017-05-17 1 21
Page couverture 2017-05-17 1 48