CA1210592A - Production of copper sulphate solution from a bed of metallic copper particles containing insoluble material - Google Patents
Production of copper sulphate solution from a bed of metallic copper particles containing insoluble materialInfo
- Publication number
- CA1210592A CA1210592A CA000439206A CA439206A CA1210592A CA 1210592 A CA1210592 A CA 1210592A CA 000439206 A CA000439206 A CA 000439206A CA 439206 A CA439206 A CA 439206A CA 1210592 A CA1210592 A CA 1210592A
- Authority
- CA
- Canada
- Prior art keywords
- reactor
- insoluble material
- inlet portion
- copper
- copper particles
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/02—Apparatus therefor
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/10—Sulfates
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
ABSTRACT OF THE DISCLOSURE
A process and an apparatus for leaching of a bed of metallic copper particles containing insoluble material is disclosed. The apparatus comprises a vertical reactor having an inlet portion at the bottom of smaller cross-sectional area than the reactor itself. The process comprises flowing a copper sulphate solution upwardly through the inlet portion of said reactor at a velocity such as to cause fluidization of the copper particles and the insoluble material contained in the inlet portion of the reactor only, and withdrawing the insoluble material and some copper particles together with some solution, from the inlet portion of the reactor to prevent the accu-mulation of insoluble material in the reactor.
A process and an apparatus for leaching of a bed of metallic copper particles containing insoluble material is disclosed. The apparatus comprises a vertical reactor having an inlet portion at the bottom of smaller cross-sectional area than the reactor itself. The process comprises flowing a copper sulphate solution upwardly through the inlet portion of said reactor at a velocity such as to cause fluidization of the copper particles and the insoluble material contained in the inlet portion of the reactor only, and withdrawing the insoluble material and some copper particles together with some solution, from the inlet portion of the reactor to prevent the accu-mulation of insoluble material in the reactor.
Description
~Z~ ~S92 - PRODUCTION OF COPPER SULPHATE SO.LUTION FROM
A BED OF METALLIC COPPER PARTICLES CONTAINING
INSOLUBLE MATERIAL
This invention relates to a process and apparatus for leaching of a bed of metallic copper particles con-taining insoluble material with an upwardly flowing copper sulphate solution, thereby producing copper sulphate solu-tion of sufficient strength for crystallization.
Copper sulphate is conventionally produced byreacting metallic copper, for instance, copper-bearing scrap, with hot aerated sulphuric acid solution in accord-ance with the equation:
Cu + H2S04 + ~o2 ~ CuS04 + H20 (l) . The resulting copper sulphate solution is subsequently cooled to crystallize CuS04-5H20.
In another method described in U.S. Patent 4,251,489, a hot copper sulphate solution is passed through a bed of particulate metallic copper, such as chopped wire scrap, whereby copper dissolves to form a small amount of cuprous sulphate in accordance with the equation:
Cu + CuSO4 ~ Cu2SO4 (2) The cuprous sulphate is oxidized to cupric sulphate in a separate vessel in accordance with the equation:
Cu2SO4 + ~02 + H2SO4 2CuSO4 + H20 (3) The solution depleted in monovalent copper is re-cycled to the bed where additional copper dissolves.
The overa~l reaction is identical to that in the , ~. J
i2~0sgz conventional process, equation (1). The process of U.S.
Patent 4,251,489 is potentially easier and more economical to operate than the conventional process because of the sepa-ration into two steps. However, scrap contains insoluble material, such as residual plastic insulation, which will accumulate in the bed and eventually require a shut-down of the system in order to remove it. This considerably detracts from the benefits of using the process on an industrial scale. For instance, if the scrap contains 3% by weight of insoluble material and one bed volume is treated every 24 hours, about 20% of the bed would consist of insoluble material after one week. The above mentioned patent does not describe any means of overcoming this problem.
It is, therefore, the object of the present invention to provide a process for the production of copper sulphate from a bed of metallic copper particles which allows the removal of the insoluble material contained in the bed with-out interrupting the operation of the process.
The process, in accordance with the present invention, comprises the steps of providing a vertical reactor having an inl~t portion at the bottom of smaller cross-sectional area than the reactor itself, flowing a copper sulphate solu-tion upwardly through the inlet portion of the reactor at a velocity such as to cause fluidization of the copper par-ticles and the insoluble material contained in the inletportion of the reactor only, and withdrawing the insoluble ~terial and some copper particles from the inlet portion of ~2~0sg2 the reactor to prevent the accumulation of insoluble material in the reactor. Obviously, some solution also escapes during such witharawal.
The reactor inlet portion can be of any desired shape, although a conical shape with an opening for introduction of the copper sulphate solution at the apex of the cone is preferred. The cone angle at the apex should preferably be between 45 and 90, although 60 is the most practical angle.
The means for withdrawing the insoluble material and some copper particles,together with some solution,from the inlet portion of the reactor preferably consists of an out-let provided with a suitable valve.
A grid is preferably positioned within the inlet portion of the reactor to hold the initial bed of copper particles and prevent the copper particles from flowing out of the reactor if circulation of the copper sulphate solution is stopped.
The invention will now be disclosed, by way of example, with reference to the accompanying drawing in which:
FLgure 1 is a flow diagram of the copper sulphate production circuit; and Figure 2 is an enlarged view of the bottom inlet portion of the reactor.
Referring to Figure 1, there is shown a closed circuit consisting of a vertical reactor 10 and an oxidation . ~
12i0592 tank 12 through which a copper sulphate solution is circulated to carry out the process in accordance-with the present invention. The copper sulphate solution is cir-culated by a pump 14 from the oxida~ion tank up through a bed of metallic copper particles 16 in the reactor and back into the oxidation tank 12. The metallic copper in the reactor dissolves to form a small amount of cuprous sulphate and such small amount of cuprous sulphate is oxidized in the oxidation tank to form cupric sulphat~.
The solution in the oxidation tank is agitated by a stirrer 18 beneath which air or oxygen is introduced via a conduit 20. The solution depleted in monovalent copper is re-cyc,led several times to the bed of copper particles where additional copper dissolves each time. The solution is cir-culated at a rate such that the contact time with themetallic copper particles is less than 5 minutes, preferably less than 60 seconds. ~hen the soluticn has achieved sufficient copper concentration, it can be continuously or periodically withdrawn from the system and replaced by a fresh, weak solution or by sulphuric acid.
As shown in Figure 2, the bot~om portion of the reactor has a copper sulphate solution inlet portion 22 which is of a smaller cross-sectional area than the reactor itself. It is shown here as being of conical ~: 25 shape but it could, of course, take other shapes. The conical bottom portion of the reactor has a dimension as compared to the reactor such that when the solution is introduced through the apex of the cone, the solid ;:~ B
lZ~OSg2 particles in the reactor are set in motion locally in the botto~ portion of the reactor and a fluidized bed is formed in that bottom portion only but not in the reactor.
In operation, it has been found that the insolubles slowly migrate to the bottom of the reactor where they are fluidized, together with some of the copper which is in the process of dissolution. Removal of the insolubles from the cone is effected by discharge of the fluidized material through a side outlet 24, located at an appro-priate level and fitted with a suitable valve 26, thedriving force being the slight pressure in the reactor due to the hydrostatic and velocity heads of the flowi~g solu-tion. ~ischarge can be intermittent, at such intervals of time as will prevent the accumulation of insolubles in the reactor.
It should be noted that the solution velocity required to achieve fluidization is determined by the size of the individual metallic copper particles. For choppings of fine copper wire of 24 gauge, it has been found that a solution velocity of at least 0.15 ft/sec.(4.5 cm/sec.), preferably 0.2 ft/sec. (6 cm/sec.) is satisfactory.
No supporting devices,such as grids or screens, are needed to hold the column of metallic copper particles ; above the fluidized bed. The cohesive forces between the metallic copper particles are sufficiently strong to allow the material to span the cone at a height where the solution velocity is no longer high enough to fluidize the particles. Nevertheless, a B
~2~0~a2 perforated plate or grid 28 is provided at the apex to hold the initial metallic copper charge and to prevent solids from dropping out into the pump if circulation is stopped.
The reactor can be of any desired cross-sectional shape although a circular shape is preferred for convenience in construction. Similarly, the inlet portion of the reactor can be of any desired cross-sectional shape of smaller cross-sectional area, although a conical shape is preferred.
The cone angle at the apex should preferably be between 45 and 90 , although 60 is the most practical angle.
Example A reactor was assembled consisting of a 6 in. (15 cm) diam. x 6 ft (180 cm)column fitted with a 60 bottom cone ending in a 1.5 in. (3.75 cm) solution inlet and having a 3/4 in. (1.8 cm) outlet pipe located about 1~ in. (3.75 cm) above the cone apex. The outlet pipe was fitted with an air-operated pinch valv~. A perforated plate (25 holes of ~ în. (0.6 cm) diameter) was also installed at the cone apex (Figure 2). A pump and oxidation tank completed the closed circuit required to operate the reactor which was loaded to a height of about 5.5 ft (165 cm) with about 200 lbs (90 kg) of chopped fine wire scrap containing insol-ubles. An acid-~earing copper sulphate solution at 91 DC was circulated upward through the bed at a rate of 8.5 U.S.
gal./min (0.5 L/sec.) returning to the pump through the oxidation tank ~y gravity. From time to time, solution was ~ `' bled from the system and acid was added so as to maintain a constant solution composition. Scrap was also added to the top of the reactor to maintain the bed height. After about 70 hours of continuous operation, when sufficient insolubles had accumulated in the cone following the dis-solution of about 140 lbs (63 kg) of copper, the discharge valve on the side outlet of the cone was opened momentar-ily. The discharged material contained a high proportion of insolubles consisting of pieces of plastic insulation, coarse copper parti~les too large to dissolve to a signif-icant degree in the time allowed and other metallic insolubles.
It should be understood that the invention is not limited to the specific embodiment described herein or illus-trated in the,drawing. For example, instead of the cone atthe bottom of the reactor, it is possible to provide a frustum or some other arrangement in which there may be one or more partitions or the like that would produce adequate fluidization of the material within the inlet portion of the reactor. Also, the smaller cross-sectional area at the bottom of the reactor may be formed by internal restrictions rather than external shape. Moreover, the removal of the fluidized material need not be done through a side outlet, as shown in the drawing, but could be carried out through a bottom outlet or the like.
~ .
A BED OF METALLIC COPPER PARTICLES CONTAINING
INSOLUBLE MATERIAL
This invention relates to a process and apparatus for leaching of a bed of metallic copper particles con-taining insoluble material with an upwardly flowing copper sulphate solution, thereby producing copper sulphate solu-tion of sufficient strength for crystallization.
Copper sulphate is conventionally produced byreacting metallic copper, for instance, copper-bearing scrap, with hot aerated sulphuric acid solution in accord-ance with the equation:
Cu + H2S04 + ~o2 ~ CuS04 + H20 (l) . The resulting copper sulphate solution is subsequently cooled to crystallize CuS04-5H20.
In another method described in U.S. Patent 4,251,489, a hot copper sulphate solution is passed through a bed of particulate metallic copper, such as chopped wire scrap, whereby copper dissolves to form a small amount of cuprous sulphate in accordance with the equation:
Cu + CuSO4 ~ Cu2SO4 (2) The cuprous sulphate is oxidized to cupric sulphate in a separate vessel in accordance with the equation:
Cu2SO4 + ~02 + H2SO4 2CuSO4 + H20 (3) The solution depleted in monovalent copper is re-cycled to the bed where additional copper dissolves.
The overa~l reaction is identical to that in the , ~. J
i2~0sgz conventional process, equation (1). The process of U.S.
Patent 4,251,489 is potentially easier and more economical to operate than the conventional process because of the sepa-ration into two steps. However, scrap contains insoluble material, such as residual plastic insulation, which will accumulate in the bed and eventually require a shut-down of the system in order to remove it. This considerably detracts from the benefits of using the process on an industrial scale. For instance, if the scrap contains 3% by weight of insoluble material and one bed volume is treated every 24 hours, about 20% of the bed would consist of insoluble material after one week. The above mentioned patent does not describe any means of overcoming this problem.
It is, therefore, the object of the present invention to provide a process for the production of copper sulphate from a bed of metallic copper particles which allows the removal of the insoluble material contained in the bed with-out interrupting the operation of the process.
The process, in accordance with the present invention, comprises the steps of providing a vertical reactor having an inl~t portion at the bottom of smaller cross-sectional area than the reactor itself, flowing a copper sulphate solu-tion upwardly through the inlet portion of the reactor at a velocity such as to cause fluidization of the copper par-ticles and the insoluble material contained in the inletportion of the reactor only, and withdrawing the insoluble ~terial and some copper particles from the inlet portion of ~2~0sg2 the reactor to prevent the accumulation of insoluble material in the reactor. Obviously, some solution also escapes during such witharawal.
The reactor inlet portion can be of any desired shape, although a conical shape with an opening for introduction of the copper sulphate solution at the apex of the cone is preferred. The cone angle at the apex should preferably be between 45 and 90, although 60 is the most practical angle.
The means for withdrawing the insoluble material and some copper particles,together with some solution,from the inlet portion of the reactor preferably consists of an out-let provided with a suitable valve.
A grid is preferably positioned within the inlet portion of the reactor to hold the initial bed of copper particles and prevent the copper particles from flowing out of the reactor if circulation of the copper sulphate solution is stopped.
The invention will now be disclosed, by way of example, with reference to the accompanying drawing in which:
FLgure 1 is a flow diagram of the copper sulphate production circuit; and Figure 2 is an enlarged view of the bottom inlet portion of the reactor.
Referring to Figure 1, there is shown a closed circuit consisting of a vertical reactor 10 and an oxidation . ~
12i0592 tank 12 through which a copper sulphate solution is circulated to carry out the process in accordance-with the present invention. The copper sulphate solution is cir-culated by a pump 14 from the oxida~ion tank up through a bed of metallic copper particles 16 in the reactor and back into the oxidation tank 12. The metallic copper in the reactor dissolves to form a small amount of cuprous sulphate and such small amount of cuprous sulphate is oxidized in the oxidation tank to form cupric sulphat~.
The solution in the oxidation tank is agitated by a stirrer 18 beneath which air or oxygen is introduced via a conduit 20. The solution depleted in monovalent copper is re-cyc,led several times to the bed of copper particles where additional copper dissolves each time. The solution is cir-culated at a rate such that the contact time with themetallic copper particles is less than 5 minutes, preferably less than 60 seconds. ~hen the soluticn has achieved sufficient copper concentration, it can be continuously or periodically withdrawn from the system and replaced by a fresh, weak solution or by sulphuric acid.
As shown in Figure 2, the bot~om portion of the reactor has a copper sulphate solution inlet portion 22 which is of a smaller cross-sectional area than the reactor itself. It is shown here as being of conical ~: 25 shape but it could, of course, take other shapes. The conical bottom portion of the reactor has a dimension as compared to the reactor such that when the solution is introduced through the apex of the cone, the solid ;:~ B
lZ~OSg2 particles in the reactor are set in motion locally in the botto~ portion of the reactor and a fluidized bed is formed in that bottom portion only but not in the reactor.
In operation, it has been found that the insolubles slowly migrate to the bottom of the reactor where they are fluidized, together with some of the copper which is in the process of dissolution. Removal of the insolubles from the cone is effected by discharge of the fluidized material through a side outlet 24, located at an appro-priate level and fitted with a suitable valve 26, thedriving force being the slight pressure in the reactor due to the hydrostatic and velocity heads of the flowi~g solu-tion. ~ischarge can be intermittent, at such intervals of time as will prevent the accumulation of insolubles in the reactor.
It should be noted that the solution velocity required to achieve fluidization is determined by the size of the individual metallic copper particles. For choppings of fine copper wire of 24 gauge, it has been found that a solution velocity of at least 0.15 ft/sec.(4.5 cm/sec.), preferably 0.2 ft/sec. (6 cm/sec.) is satisfactory.
No supporting devices,such as grids or screens, are needed to hold the column of metallic copper particles ; above the fluidized bed. The cohesive forces between the metallic copper particles are sufficiently strong to allow the material to span the cone at a height where the solution velocity is no longer high enough to fluidize the particles. Nevertheless, a B
~2~0~a2 perforated plate or grid 28 is provided at the apex to hold the initial metallic copper charge and to prevent solids from dropping out into the pump if circulation is stopped.
The reactor can be of any desired cross-sectional shape although a circular shape is preferred for convenience in construction. Similarly, the inlet portion of the reactor can be of any desired cross-sectional shape of smaller cross-sectional area, although a conical shape is preferred.
The cone angle at the apex should preferably be between 45 and 90 , although 60 is the most practical angle.
Example A reactor was assembled consisting of a 6 in. (15 cm) diam. x 6 ft (180 cm)column fitted with a 60 bottom cone ending in a 1.5 in. (3.75 cm) solution inlet and having a 3/4 in. (1.8 cm) outlet pipe located about 1~ in. (3.75 cm) above the cone apex. The outlet pipe was fitted with an air-operated pinch valv~. A perforated plate (25 holes of ~ în. (0.6 cm) diameter) was also installed at the cone apex (Figure 2). A pump and oxidation tank completed the closed circuit required to operate the reactor which was loaded to a height of about 5.5 ft (165 cm) with about 200 lbs (90 kg) of chopped fine wire scrap containing insol-ubles. An acid-~earing copper sulphate solution at 91 DC was circulated upward through the bed at a rate of 8.5 U.S.
gal./min (0.5 L/sec.) returning to the pump through the oxidation tank ~y gravity. From time to time, solution was ~ `' bled from the system and acid was added so as to maintain a constant solution composition. Scrap was also added to the top of the reactor to maintain the bed height. After about 70 hours of continuous operation, when sufficient insolubles had accumulated in the cone following the dis-solution of about 140 lbs (63 kg) of copper, the discharge valve on the side outlet of the cone was opened momentar-ily. The discharged material contained a high proportion of insolubles consisting of pieces of plastic insulation, coarse copper parti~les too large to dissolve to a signif-icant degree in the time allowed and other metallic insolubles.
It should be understood that the invention is not limited to the specific embodiment described herein or illus-trated in the,drawing. For example, instead of the cone atthe bottom of the reactor, it is possible to provide a frustum or some other arrangement in which there may be one or more partitions or the like that would produce adequate fluidization of the material within the inlet portion of the reactor. Also, the smaller cross-sectional area at the bottom of the reactor may be formed by internal restrictions rather than external shape. Moreover, the removal of the fluidized material need not be done through a side outlet, as shown in the drawing, but could be carried out through a bottom outlet or the like.
~ .
Claims (5)
1. A process for leaching of a bed of metallic copper particles containing insoluble material comprising the steps of:
a) providing a vertical reactor having an inlet portion at the bottom of smaller cross-sectional area than the reactor itself;
b) flowing a copper sulphate solution upwardly through the inlet portion of said reactor at a velocity such as to causefluidization of the copper particles and the insoluble material contained in the inlet portion of the reactor only; and c) withdrawing the insoluble material and some copper particles from the inlet portion of the reactor to prevent the accumulation of insoluble material in the reactor.
a) providing a vertical reactor having an inlet portion at the bottom of smaller cross-sectional area than the reactor itself;
b) flowing a copper sulphate solution upwardly through the inlet portion of said reactor at a velocity such as to causefluidization of the copper particles and the insoluble material contained in the inlet portion of the reactor only; and c) withdrawing the insoluble material and some copper particles from the inlet portion of the reactor to prevent the accumulation of insoluble material in the reactor.
2. An apparatus for leaching of a bed of metallic copper particles containing insoluble material comprising:
a) a vertical reactor having an inlet portion at the bottom of smaller cross-sectional area than .
the reactor itself;
b) means for flowing a copper sulphate solution upwardly through the inlet portion of said reactor at a velocity such as to cause fluidization of the copper particles and the insoluble material contained in the inlet portion of the reactor only; and c) means for withdrawing the insoluble material and some copper particles from the inlet portion of the reactor to prevent the accumulation of insoluble material in the reactor.
a) a vertical reactor having an inlet portion at the bottom of smaller cross-sectional area than .
the reactor itself;
b) means for flowing a copper sulphate solution upwardly through the inlet portion of said reactor at a velocity such as to cause fluidization of the copper particles and the insoluble material contained in the inlet portion of the reactor only; and c) means for withdrawing the insoluble material and some copper particles from the inlet portion of the reactor to prevent the accumulation of insoluble material in the reactor.
3. An apparatus as defined in claim 2, wherein the reactor has a conical inlet portion with an opening for introduction of the copper sulphate solution.
4. An apparatus as defined in claim 2, wherein said means for withdrawing the insoluble material and some copper particles from the inlet portion of the reactor is an outlet provided with a suitable valve.
5. An apparatus as defined in claim 2, further comprising a grid within the inlet portion of the reactor to hold the initial bed of copper particles and prevent the copper particles from flowing out of the reactor if circulation of the copper sulphate solution is stopped.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA000439206A CA1210592A (en) | 1983-10-18 | 1983-10-18 | Production of copper sulphate solution from a bed of metallic copper particles containing insoluble material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA000439206A CA1210592A (en) | 1983-10-18 | 1983-10-18 | Production of copper sulphate solution from a bed of metallic copper particles containing insoluble material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1210592A true CA1210592A (en) | 1986-09-02 |
Family
ID=4126307
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000439206A Expired CA1210592A (en) | 1983-10-18 | 1983-10-18 | Production of copper sulphate solution from a bed of metallic copper particles containing insoluble material |
Country Status (1)
| Country | Link |
|---|---|
| CA (1) | CA1210592A (en) |
-
1983
- 1983-10-18 CA CA000439206A patent/CA1210592A/en not_active Expired
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