CA2418063C - Production of active nickel powder and transformation thereof into nickel carbonyl - Google Patents
Production of active nickel powder and transformation thereof into nickel carbonyl Download PDFInfo
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- CA2418063C CA2418063C CA002418063A CA2418063A CA2418063C CA 2418063 C CA2418063 C CA 2418063C CA 002418063 A CA002418063 A CA 002418063A CA 2418063 A CA2418063 A CA 2418063A CA 2418063 C CA2418063 C CA 2418063C
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- nickel
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- 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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/06—Refining
- C22B23/065—Refining carbonyl methods
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
- B22F9/22—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds using gaseous reductors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
- B22F9/305—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis of metal carbonyls
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- General Chemical & Material Sciences (AREA)
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
Active nickel powder is produced by reducing a nickel chloride containing salt having a high surface area with hydrogen gas at a temperature above 300°C. The obtained active nickel powder can be rapidly converted into nickel carbonyl by reaction with carbon monoxide gas at atmospheric or superatmospheric pressure and in the absence of conventional carbonylation catalysts.
Description
PRODUCTION OF ACTIVE NICKEL POWDER AND
TRANSFORMATION THEREOF INTO NICKEL CARBONYL
FIELD OF THE INVENTION
This invention relates to the production of an active nickel metal powder suitable for transformation into nickel carbonyl. Moreover, it relates to the transformation of the active powder into nickel carbonyl by reaction with carbon monoxide at atmospheric or superatmospheric pressure and in the absence of conventional carbonylation catalysts.
BACKGROUND OF THE INVENTION
It is well known to use the Mond process for the extraction of nickel from ores, mattes, residues, or similar compounds containing nickel, in which such compounds are reduced to yield finally divided metallic nickel which is then treated with carbon monoxide to produce nickel carbonyl that can then be decomposed to yield nickel. Various improvements to this process have been suggested to increase the rate of nickel carbonyl production and thus render the overall process more economical.
For example, in Canadian Patent No. 322,887 it is suggested to add to the reaction chamber producing nickel carbonyl, a compound containing sulphur, selenium or tellurium in "active form", such as nickel sulphide, nickel selenide or nickel telluride and carrying out the carbonylation reaction in the absence of oxygen.
The preferred additive is nickel sulphide and it is added so that the amount of active sulphur in the reaction chamber lies between 0.2% and 5% by weight. It, therefore, acts as a catalyst to promote the carbonylation reaction.
In U.S. Patent No. 4,045,541 another improvement is disclosed according to which a metal, such as iron, copper or cobalt, which forms sulphides more easily than nickel at 200 C, is admixed with the material comprising elemental nickel, such as nickel oxide, which is then subjected to carbonylation and sulfidation.
British Patent No. 649,988 discloses a process for the manufacture of nickel carbonyl by reacting an aqueous solution of a nickel salt, such as nickel chloride or nickel sulphate, with an alkaline reacting substance, producing a nickel compound which is treated in aqueous solution or suspension with carbon monoxide under superatmospheric pressure of at least 50 atmospheres and at elevated temperatures of at least 70 C, and in the presence of a minor amount of nickel sulphide or cyanide as a catalyst.
All the above prior art processes require the presence of various additives or carbonylation catalysts and/or the use of superatmospheric pressure and elevated temperature to achieve satisfactory rates of nickel carbonyl production.
There is thus a need for a simplified production of nickel carbonyl from nickel salts.
OBJECTS AND SUMMARY OF THE INVENTION
It is an object of the present invention to produce active nickel powder from nickel chloride or nickel salt mixtures containing nickel chloride, which active powder is capable to react with carbon monoxide gas at atmospheric or superatmospheric pressure to yield nickel carbonyl.
It is a further object of the present invention to transform the active nickel powder produced from nickel chloride or nickel salt mixtures containing nickel chloride into nickel carbonyl at rapid and commercial rates without addition of
TRANSFORMATION THEREOF INTO NICKEL CARBONYL
FIELD OF THE INVENTION
This invention relates to the production of an active nickel metal powder suitable for transformation into nickel carbonyl. Moreover, it relates to the transformation of the active powder into nickel carbonyl by reaction with carbon monoxide at atmospheric or superatmospheric pressure and in the absence of conventional carbonylation catalysts.
BACKGROUND OF THE INVENTION
It is well known to use the Mond process for the extraction of nickel from ores, mattes, residues, or similar compounds containing nickel, in which such compounds are reduced to yield finally divided metallic nickel which is then treated with carbon monoxide to produce nickel carbonyl that can then be decomposed to yield nickel. Various improvements to this process have been suggested to increase the rate of nickel carbonyl production and thus render the overall process more economical.
For example, in Canadian Patent No. 322,887 it is suggested to add to the reaction chamber producing nickel carbonyl, a compound containing sulphur, selenium or tellurium in "active form", such as nickel sulphide, nickel selenide or nickel telluride and carrying out the carbonylation reaction in the absence of oxygen.
The preferred additive is nickel sulphide and it is added so that the amount of active sulphur in the reaction chamber lies between 0.2% and 5% by weight. It, therefore, acts as a catalyst to promote the carbonylation reaction.
In U.S. Patent No. 4,045,541 another improvement is disclosed according to which a metal, such as iron, copper or cobalt, which forms sulphides more easily than nickel at 200 C, is admixed with the material comprising elemental nickel, such as nickel oxide, which is then subjected to carbonylation and sulfidation.
British Patent No. 649,988 discloses a process for the manufacture of nickel carbonyl by reacting an aqueous solution of a nickel salt, such as nickel chloride or nickel sulphate, with an alkaline reacting substance, producing a nickel compound which is treated in aqueous solution or suspension with carbon monoxide under superatmospheric pressure of at least 50 atmospheres and at elevated temperatures of at least 70 C, and in the presence of a minor amount of nickel sulphide or cyanide as a catalyst.
All the above prior art processes require the presence of various additives or carbonylation catalysts and/or the use of superatmospheric pressure and elevated temperature to achieve satisfactory rates of nickel carbonyl production.
There is thus a need for a simplified production of nickel carbonyl from nickel salts.
OBJECTS AND SUMMARY OF THE INVENTION
It is an object of the present invention to produce active nickel powder from nickel chloride or nickel salt mixtures containing nickel chloride, which active powder is capable to react with carbon monoxide gas at atmospheric or superatmospheric pressure to yield nickel carbonyl.
It is a further object of the present invention to transform the active nickel powder produced from nickel chloride or nickel salt mixtures containing nickel chloride into nickel carbonyl at rapid and commercial rates without addition of
-2-carbonylation catalysts or promoters, such as used in the prior art.
The invention also provides a method of producing an active nickel powder which comprises reducing a feed material comprising a nickel salt consisting of nickel chloride said feed material containing 5% to 100% by weight of nickel chloride and having a surface area in excess of 10m2/g, with a reducing hydrogen gas, at a temperature above 300 C.
The invention also provides active nickel powder capable of being rapidly converted into nickel carbonyl by reaction with carbon monoxide gas at atmospheric or superatmospheric pressure, said powder being the result of reduction by hydrogen at a temperature above 300 C of a feed material comprising nickel chloride and other reducible nickel salts in addition to nickel chloride, said feed material having a high surface area in excess of 10mZ/g.
Other objects and advantages of the present invention will become apparent from the following description thereof.
In essence, it has been found that nickel salts containing 5% to 100% of nickel chloride and having a high surface area can be rapidly reduced to active nickel powder by reaction with a reducing hydrogen gas at a temperature above 300 C, and preferably between 300 C and 600 C. The reducing hydrogen gas should normally contain at least 20% by volume of H2, but is preferably pure hydrogen. The resulting activated nickel powder can then be reacted with CO gas at atmospheric pressure and temperatures of 20 C to 60 C, preferably about 50 C, to produce nickel carbonyl -Ni(CO)4, with a yield close to 100%. The activated nickel powder can also be reached with CO at superatmospheric pressure and elevated temperature, if desired. The carbonylation reaction with CO gas is simple and effective, requiring no catalysts or other promoters.
The invention also provides a method of producing an active nickel powder which comprises reducing a feed material comprising a nickel salt consisting of nickel chloride said feed material containing 5% to 100% by weight of nickel chloride and having a surface area in excess of 10m2/g, with a reducing hydrogen gas, at a temperature above 300 C.
The invention also provides active nickel powder capable of being rapidly converted into nickel carbonyl by reaction with carbon monoxide gas at atmospheric or superatmospheric pressure, said powder being the result of reduction by hydrogen at a temperature above 300 C of a feed material comprising nickel chloride and other reducible nickel salts in addition to nickel chloride, said feed material having a high surface area in excess of 10mZ/g.
Other objects and advantages of the present invention will become apparent from the following description thereof.
In essence, it has been found that nickel salts containing 5% to 100% of nickel chloride and having a high surface area can be rapidly reduced to active nickel powder by reaction with a reducing hydrogen gas at a temperature above 300 C, and preferably between 300 C and 600 C. The reducing hydrogen gas should normally contain at least 20% by volume of H2, but is preferably pure hydrogen. The resulting activated nickel powder can then be reacted with CO gas at atmospheric pressure and temperatures of 20 C to 60 C, preferably about 50 C, to produce nickel carbonyl -Ni(CO)4, with a yield close to 100%. The activated nickel powder can also be reached with CO at superatmospheric pressure and elevated temperature, if desired. The carbonylation reaction with CO gas is simple and effective, requiring no catalysts or other promoters.
-3-When other nickel salts, such as nickel carbonate or nickel sulfate are treated in the same manner, namely by reaction with Hz gas at 300 C - 600 C, essentially no active nickel powder is produced. However, surprisingly, when such salts are admixed with at least 5% b_y weight of NiCI,, the entire admixture produces active nickel powder. The Ni recoveries obtained with the admixture of NiCO, and NiCI2 are in the range of 95-1009'o and the recoveries obtained with the admixture of NiSO4 and NiCI2 are usually slightly fower, but still in a very appreciable range of 85-90 ro, probably due to the formation of some nickel sulphide which does not carbonylate.
When reference is made to nickel chloride, it can be either dehydrated or in the form of hydrates, such as NiC1,.6H,0. Moreover, when reference is made to 3a nickel salts, they can also be in hydrated form and/or combined with other nickel compounds, such as nickel hydroxide or the compound called zaratite -2Ni(OH)z.NiCO3.4HzO.
The starting material should have a high surface area in excess of 10m2/g, and preferably between 35 and 100 m2/g.
The active nickel powder produced in accordance with the present invention can be exposed to air for a short period of time and still remain active. It can also be maintained under inert gas, such as argon, for several days without losing its activity.
Another useful feature of this powder is that once the active nickel powder loses its activity due to storage, in the absence of oxygen, it can be re-activated by exposing it to HZ gas at about 150 C or higher temperatures. If the active nickel powder loses its activity due to storage in the presence of oxygen, it can be re-activated by exposing it to H2 gas at a temperature of 300 C to 600 C. This is an important advantage of the present invention because it enables to perform the carbonylation reaction completely separately and at a different location from the reduction reaction that produces the active nickel powder.
BRIEF DESCRIPTION OF THE DRAWINGS
Fig. 1 is a graph showing nickel extraction from active nickel powder produced by reduction of nickel chloride;
Fig. 2 is a graph showing nickel extraction from active nickel powder where treatments were made on various NiCIZ materials at different temperatures.
Fig. 3 is a graph showing nickel extraction from nickel powder produced by reduction of nickel carbonate; and Fig. 4 is a graph showing nickel extraction from active nickel powder
When reference is made to nickel chloride, it can be either dehydrated or in the form of hydrates, such as NiC1,.6H,0. Moreover, when reference is made to 3a nickel salts, they can also be in hydrated form and/or combined with other nickel compounds, such as nickel hydroxide or the compound called zaratite -2Ni(OH)z.NiCO3.4HzO.
The starting material should have a high surface area in excess of 10m2/g, and preferably between 35 and 100 m2/g.
The active nickel powder produced in accordance with the present invention can be exposed to air for a short period of time and still remain active. It can also be maintained under inert gas, such as argon, for several days without losing its activity.
Another useful feature of this powder is that once the active nickel powder loses its activity due to storage, in the absence of oxygen, it can be re-activated by exposing it to HZ gas at about 150 C or higher temperatures. If the active nickel powder loses its activity due to storage in the presence of oxygen, it can be re-activated by exposing it to H2 gas at a temperature of 300 C to 600 C. This is an important advantage of the present invention because it enables to perform the carbonylation reaction completely separately and at a different location from the reduction reaction that produces the active nickel powder.
BRIEF DESCRIPTION OF THE DRAWINGS
Fig. 1 is a graph showing nickel extraction from active nickel powder produced by reduction of nickel chloride;
Fig. 2 is a graph showing nickel extraction from active nickel powder where treatments were made on various NiCIZ materials at different temperatures.
Fig. 3 is a graph showing nickel extraction from nickel powder produced by reduction of nickel carbonate; and Fig. 4 is a graph showing nickel extraction from active nickel powder
-4-produced by reduction of an admixture of nickel carbonate and nickel chloride.
Fig. 5 is a graph showing nickel extraction at superatmospheric pressure and elevated temperature from active nickel powder of the present invention as compared to regular nickel powder of the prior art.
DETAILED DESCRIPTION OF THE INVENTION
Examples of preferred but non-limitative embodiments will now be described with reference to the appended drawings. In these examples, tests were carried out by first reducing a pre-dried small sample (25mg) of finely divided nickel chloride and of nickel carbonate alone and in admixture with nickel chloride respectively.
The reduction was carried out in hydrogen at 500 C. The obtained nickel powder was then cooled to 200 C and the reactive gas switched from hydrogen to carbon monoxide at a flow rate of lOml/min. The sample was then further cooled to 50 C. Weight loss was monitored over time using computer software. The weight loss was confirmed with TGA (thermogravimetric analysis) measurements, and the residue was dissolved in acid and analyzed for nickel to give a complete mass balance. The obtained nickel metal powder reacted with CO to form volatile nickel carbonyl gas which was removed and decomposed at high temperature into a pure nickel product as in known in the art.
In this example, NiC12. 6H2O was pre-dried at 170 C in air and treated as described above. Nickel extraction of 99.6% was obtained in 45 minutes as illustrated by the curve in the graph of Fig. 1 and by curve B in the graph of Fig. 2.
The same procedure as above was repeated with a sample of NiC12 pre-dried at 300 C in N2. Ni extraction of essentially 100% was obtained in about 30 minutes as
Fig. 5 is a graph showing nickel extraction at superatmospheric pressure and elevated temperature from active nickel powder of the present invention as compared to regular nickel powder of the prior art.
DETAILED DESCRIPTION OF THE INVENTION
Examples of preferred but non-limitative embodiments will now be described with reference to the appended drawings. In these examples, tests were carried out by first reducing a pre-dried small sample (25mg) of finely divided nickel chloride and of nickel carbonate alone and in admixture with nickel chloride respectively.
The reduction was carried out in hydrogen at 500 C. The obtained nickel powder was then cooled to 200 C and the reactive gas switched from hydrogen to carbon monoxide at a flow rate of lOml/min. The sample was then further cooled to 50 C. Weight loss was monitored over time using computer software. The weight loss was confirmed with TGA (thermogravimetric analysis) measurements, and the residue was dissolved in acid and analyzed for nickel to give a complete mass balance. The obtained nickel metal powder reacted with CO to form volatile nickel carbonyl gas which was removed and decomposed at high temperature into a pure nickel product as in known in the art.
In this example, NiC12. 6H2O was pre-dried at 170 C in air and treated as described above. Nickel extraction of 99.6% was obtained in 45 minutes as illustrated by the curve in the graph of Fig. 1 and by curve B in the graph of Fig. 2.
The same procedure as above was repeated with a sample of NiC12 pre-dried at 300 C in N2. Ni extraction of essentially 100% was obtained in about 30 minutes as
-5-illustrated by curve A in the graph of Fig. 2.
The same procedure was repeated with another sample of NiC12 pre-dried at 170 C in air. Ni extraction of essentially 100% was obtained in about 1 hr. as illustrated by curve C in the graph of Fig. 3.
The same procedure was repeated but using a temperature of 600 C - 800 C
for reduction in hydrogen. In this case, essentially full extraction was reached after about 2.5 hours, as illustrated by curve D in the graph of Fig. 2. This shows that temperatures higher than 600 C actually slow down the extraction and there is no practical reason to use them. The present invention is, however, not limited to temperatures below 600 C.
The same procedure was repeated using anhydrous NiC12 without pre-drying.
In this case, only about 90% of extraction was achieved after about 5 hrs, as illustrated by curve E in the graph of Fig. 2.
The above experiments indicate that changes in drying temperatures and hydrogen reduction temperatures and in the composition of the nickel chloride may lead to variations in extraction rates and the speed of achieving the extractions.
In this example, the procedure described above was repeated but using NiCO3 as the starting material. As shown by the curve in the graph of Fig. 3, a very poor extraction rate of less than 20% was achieved after about 6 hours. It is obvious, therefore, that NiCO3 alone did not produce an active nickel powder.
The procedure of Example 2 was repeated but with replacement of the starting material with a mixture of NiCO3 and NiClz in a proportion of 3:1. This gave an
The same procedure was repeated with another sample of NiC12 pre-dried at 170 C in air. Ni extraction of essentially 100% was obtained in about 1 hr. as illustrated by curve C in the graph of Fig. 3.
The same procedure was repeated but using a temperature of 600 C - 800 C
for reduction in hydrogen. In this case, essentially full extraction was reached after about 2.5 hours, as illustrated by curve D in the graph of Fig. 2. This shows that temperatures higher than 600 C actually slow down the extraction and there is no practical reason to use them. The present invention is, however, not limited to temperatures below 600 C.
The same procedure was repeated using anhydrous NiC12 without pre-drying.
In this case, only about 90% of extraction was achieved after about 5 hrs, as illustrated by curve E in the graph of Fig. 2.
The above experiments indicate that changes in drying temperatures and hydrogen reduction temperatures and in the composition of the nickel chloride may lead to variations in extraction rates and the speed of achieving the extractions.
In this example, the procedure described above was repeated but using NiCO3 as the starting material. As shown by the curve in the graph of Fig. 3, a very poor extraction rate of less than 20% was achieved after about 6 hours. It is obvious, therefore, that NiCO3 alone did not produce an active nickel powder.
The procedure of Example 2 was repeated but with replacement of the starting material with a mixture of NiCO3 and NiClz in a proportion of 3:1. This gave an
-6-essentially 100% recovery of Ni in less than 1 hour as shown by the curve in the graph of Fig. 4.
Other amounts of mixture blends of nickel carbonate and nickel chloride were tested and good results were. obtained starting with about 5% by weight of NiC12 in the mixture. It was found, however, that the most beneficial results are obtained when the amount of chloride in the mixture is between 20 and 25% by weight based on nickel. Moreover, it was found that the higher the surface area of the mixed solids, the faster the extraction of nickel by carbonylation, with optimum results being obtained when the surface area is 80-100 m2/g and the amount of NiC12 is such as to give 20-25 wt% Cl/Ni. Thus, the presence of NiC12 in admixture with other nickel salts, including possible other compounds that may be present with such salts, produces a satisfactory and rapid conversion of the total nickel present in such mixtures into active nickel.
Larger scale tests, using samples of up to 300g, have also been carried out and gave similar results as those described in the above examples, although with conversion times of 3 to 6 hours.
A lOg sample of active nickel powder produced in accordance with the present invention was subjected to carbonylation with CO gas in a small vertical reactor at 300 psi (20 atm) and 85 C and resulted in essentially 100% of Ni extraction in less than 10 hours, as shown by curve F in Fig. 5.
Another lOg sample of non-activated nickel powder was treated in the same manner with CO gas at 300 psi and 85 C, and resulted in a conversion to Ni in over 20 hours as shown by curve G in the Fig. 5.
Other amounts of mixture blends of nickel carbonate and nickel chloride were tested and good results were. obtained starting with about 5% by weight of NiC12 in the mixture. It was found, however, that the most beneficial results are obtained when the amount of chloride in the mixture is between 20 and 25% by weight based on nickel. Moreover, it was found that the higher the surface area of the mixed solids, the faster the extraction of nickel by carbonylation, with optimum results being obtained when the surface area is 80-100 m2/g and the amount of NiC12 is such as to give 20-25 wt% Cl/Ni. Thus, the presence of NiC12 in admixture with other nickel salts, including possible other compounds that may be present with such salts, produces a satisfactory and rapid conversion of the total nickel present in such mixtures into active nickel.
Larger scale tests, using samples of up to 300g, have also been carried out and gave similar results as those described in the above examples, although with conversion times of 3 to 6 hours.
A lOg sample of active nickel powder produced in accordance with the present invention was subjected to carbonylation with CO gas in a small vertical reactor at 300 psi (20 atm) and 85 C and resulted in essentially 100% of Ni extraction in less than 10 hours, as shown by curve F in Fig. 5.
Another lOg sample of non-activated nickel powder was treated in the same manner with CO gas at 300 psi and 85 C, and resulted in a conversion to Ni in over 20 hours as shown by curve G in the Fig. 5.
-7-As previously mentioned, it is already known in the art to carbonylate Ni powder with CO gas at superatmospheric pressures and at elevated temperatures above 70 C. The present example shows that when such known carbonylation is carried out using the active nickel powder of the present invention, a considerable reduction in the time of Ni extraction is achieved.
It should be noted that the invention is not limited to the specific embodiments and examples described above, but that various modifications obvious to those skilled in the art can be made without departing from the invention and the following claims.
It should be noted that the invention is not limited to the specific embodiments and examples described above, but that various modifications obvious to those skilled in the art can be made without departing from the invention and the following claims.
-8-
Claims (15)
1. Method of producing an active nickel powder which comprises reducing a feed material comprising a nickel salt consisting of nickel chloride said feed material containing 5% to 100% by weight of nickel chloride and having a surface area in excess of 10m2/g, with a reducing hydrogen gas, at a temperature above 300°C.
2. Method according to claim 1, wherein said feed material further comprises other reducible nickel salts in addition to said nickel chloride and said feed material contains 5% to less than 100% of nickel chloride.
3. Method according to claim 1 or 2, in which the nickel chloride is in the form of its hydrates.
4. Method according to claim 2, in which said feed material is a mixture of nickel carbonate and nickel chloride.
5. Method according to claim 4, in which the nickel carbonate is in the form of zaratite - 2Ni(OH)2.NiCO3.4H2O.
6. Method according to claims 4 or 5, in which the nickel chloride is in an amount such as to give 20-25% by weight of chloride based on nickel in the mixture.
7. Method according to any one of claims 1 to 6, in which the surface area of the nickel salt is between 35 and 100m2/g.
8. Method according to any one of claims 1 to 7, in which the hydrogen containing gas is pure hydrogen gas.
9. Method according to any one of claims 1 to 8, in which the reducing reaction is carried out at a temperature of about 500°C.
10. Method of re-activating the active nickel powder produced according to any one of claims 1 to 9 that became de-activated due to storage in the absence of oxygen, comprising exposing said nickel powder to H2 gas at a temperature of at least about 150°C.
11. Method of re-activating the active nickel powder, produced according to any one of claims 1 to 9 that became de-activated due to storage in the absence of oxygen, comprising exposing said nickel powder to H2 gas at a temperature between 300°C
and 600°C.
and 600°C.
12. Method of producing nickel carbonyl comprising reacting the active nickel powder produced according to any one of claims 1 to 9 comprising reacting said active nickel powder with CO gas at atmospheric pressure and at a temperature of 40-60°C.
13. Method of producing nickel carbonyl comprising reacting the active nickel powder produced according to any one of claims 1 to 9 comprising reacting said active nickel powder with CO gas at a superatmospheric pressure and an elevated temperature.
14. Active nickel powder capable of being rapidly converted into nickel carbonyl by reaction with carbon monoxide gas at atmospheric or superatmospheric pressure, said powder being the result of reduction by hydrogen at a temperature above 300°C
of a feed material comprising nickel chloride and other reducible nickel salts in addition to nickel chloride, said feed material having a high surface area in excess of 10m2/g.
of a feed material comprising nickel chloride and other reducible nickel salts in addition to nickel chloride, said feed material having a high surface area in excess of 10m2/g.
15. Active nickel powder according to claim 14, in which the feed material is a mixture with a quantity of nickel chloride in the mixture being such as to give 20-25%
by weight of chloride based on nickel.
by weight of chloride based on nickel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA002418063A CA2418063C (en) | 2003-01-30 | 2003-01-30 | Production of active nickel powder and transformation thereof into nickel carbonyl |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CA002418063A CA2418063C (en) | 2003-01-30 | 2003-01-30 | Production of active nickel powder and transformation thereof into nickel carbonyl |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CA2418063A1 CA2418063A1 (en) | 2004-07-30 |
| CA2418063C true CA2418063C (en) | 2009-10-06 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA002418063A Expired - Lifetime CA2418063C (en) | 2003-01-30 | 2003-01-30 | Production of active nickel powder and transformation thereof into nickel carbonyl |
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| CA (1) | CA2418063C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BRPI0418785A (en) * | 2004-04-27 | 2007-10-09 | Falconbridge Ltd | production of active nickel powder and its transformation into nickel carbonyl |
| CN1305617C (en) * | 2005-02-06 | 2007-03-21 | 金川集团有限公司 | Production method of dentritic morphology nickel powder |
| AU2005234712B1 (en) * | 2005-11-21 | 2007-05-24 | Cvmr Corporation | Re-activation of de-activated nickel for nickel carbonyl production |
| CN115954129A (en) * | 2022-12-02 | 2023-04-11 | 上海苏煜新能源有限公司 | Conductive paste and preparation method thereof |
-
2003
- 2003-01-30 CA CA002418063A patent/CA2418063C/en not_active Expired - Lifetime
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| CA2418063A1 (en) | 2004-07-30 |
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