CN1603240A - Method for synthesizing nickel tetracarbonyl - Google Patents
Method for synthesizing nickel tetracarbonyl Download PDFInfo
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- CN1603240A CN1603240A CN 03135044 CN03135044A CN1603240A CN 1603240 A CN1603240 A CN 1603240A CN 03135044 CN03135044 CN 03135044 CN 03135044 A CN03135044 A CN 03135044A CN 1603240 A CN1603240 A CN 1603240A
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- nickel
- carbon monoxide
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Abstract
The invention relates to a compound method for nickel carbonoxide. It sets thermalloy or ambrose first alloy onto fixed bed reactor and is continuously pumped into carbon monoxide with catalyst. The reaction pressure is controlled from 5.0Mpa to 15.0Mpa, and temperature is controlled from 150 degree centigrade to 250 degree centigrade. Thus, the carbonylation ratio of nickel in raw material is very high. And experiment safety factor is sharply increased.
Description
Technical field
The present invention relates to a kind of synthetic method of nickle carbonoxide.
Background technology
Carbonylation is carried the metallurgical technology that nickel technology is RECENT DEVELOPMENTS, and its technological process is with nickel-bearing raw materials such as pure nickel, cupronickel or nickel oxide, by obtaining carbonyl nickel (CO) with reaction of carbon monoxide
4From 1902 since Ke Laidaqi refinery of moral nickel company set up to be covered by Britain, carbonyl process is through the development of last 100 years, and now having formed with the Ke Laidaqi of International nickel Co. Ltd. Inco. Ltd. (INCO) nickel refining factory is that the normal pressure of representative, middle pressure that copper precipice nickel refining factory of International nickel Co. Ltd. Inco. Ltd. (INCO) is representative, Man Qiegeersike factory of Russian northern nickel company are three kinds of technologies of the pressure carbonylation method of representative.The Britain Ke Laidaqi of International nickel Co. Ltd. Inco. Ltd. (INCO) nickel refining factory non-pressure process synthetic operation is a continous way, normal pressure carbonyl process equipment and technology process is simple, but efficient is low, reinforced, discharge, synthetic and CO circulation are carried out continuously with the operation of total systems such as replenishing, a certain link is obstructed all can influence the carrying out of whole process, so the thermal equilibrium of production control management, system and the balance of CO require all very strict, are difficult for grasping.And because of no rectification working process, to the bad adaptability of raw material.Russia northern nickel company adopts the pressure carbonylation method to have simple to operate, equipment easily solves, the advantage that construction costs is low, but owing to pressure, temperature drift, its synthesis device wall thickness, heat radiation discharge difficulty to the poor selectivity of contained multiple metallic element in the raw material, requires the raw material iron content can not be too high in the CARBONYLATION PROCESSES.And can cause precious metal to run off, be difficult to bring into play the fireballing advantage of reaction under high pressure.
During adopting, Canadian copper precipice nickel refining factory of International nickel Co. Ltd. Inco. Ltd. (INCO) and New Caledonia Bu Wazi factory press carbonyl process to have moderate pressure, synthesis device efficient height, the advantage stronger to the adaptability of raw material, but its device structure complexity, dynamic rotary seal under the press strip spare during synthesis reactor need be implemented, technical requirements difficulty height involves great expense.But, from the carbonylation state of the art and the development trend of nickel consider that middle pressure carbonylation technology is the most competitive in the world.
Summary of the invention
In the objective of the invention is to obtain under the press strip spare selectivity efficient carbonylation put forward the nickel technology.The objective of the invention is to be achieved through the following technical solutions.
A kind of synthetic method of nickle carbonoxide is characterized in that corronel or nickel copper alloy are placed fixed-bed reactor, feeds the CO (carbon monoxide converter) gas that contains catalyzer continuously, and control reaction pressure 5.0-15.0MPa, temperature 150-250 ℃ is reacted; Wherein catalyzer is ammonia, methylamine, ethamine, quadrol or triethylamine.
The volumn concentration that contains catalyzer in the CO (carbon monoxide converter) gas of catalyzer is 0.5%-10%.
Reaction raw materials cupronickel or nickel copper alloy that we adopt, the weight percentage of nickel is 25-75%.
Outstanding feature of the present invention is: lacked with this method synthesizing carbonyl nickel yield height, the reaction times (1), reaction pressure moderate (5.0-15.0MPa); (2) this method synthesizing carbonyl nickel reactant temperature is low and temperature applicable range is wide in range, all can obtain more satisfactory result under 150-250 ℃; (3) this method is less demanding to reaction raw materials, wide adaptability.(4) this method reaction process is simple and raw material is cheap and easy to get, can carry out scale operation.
The present invention puies forward the nickel synthetic technology for cupronickel or nickel copper alloy carbonylation under middle press strip spare.Because pressure and temp is more moderate, to the too late Muscovite high-pressure process strictness of the requirement of equipment and raw material; Simultaneously, by the activation treatment to the raw material uniqueness, can realize the selectivity efficient carbonylation of nickel again at reactor, cross over the technical difficulty requirement of pressing the dynamic revolving reaction still of carbonylation in the INCO company, construction costs will greatly reduce.
Embodiment
Provide following examples for further setting forth spy of the present invention, obviously embodiments of the present invention are not limited to subordinate embodiment.
Embodiment 1
In reactor, add 30g nickel copper alloy particle, reactor is through vacuumizing and with after the carbon monoxide displaced air, feed the carbon monoxide that contains ammonia continuously, wherein under pressure 7.0MPa, 180 ℃ of conditions of temperature, reacted 48 hours, the reaction mixture gas body that contains nickle carbonoxide imports the condensing air liquid/gas separator, collect nickle carbonoxide, the tail gas recycle.
Embodiment 2-4
According to the method and the step of example 1, but the pressure of system is in the change oxonation:
(2)5.0MPa
(3)12.0MPa
(4)15.0MPa
Embodiment 5-8
According to the method and the step of example 1, the system temperature of reaction of example 1-4 is set to 150 ℃, 210 ℃, 250 ℃ respectively.
Embodiment 9-12
In reactor, add the 30g nickel copper alloy, reactor is through vacuumizing and with after the carbon monoxide displaced air, feed continuously the CO (carbon monoxide converter) gas that contains an amount of methylamine (or one of ethamine, quadrol, triethylamine), at pressure 7.0MPa, temperature was reacted 48 hours for 180 ℃, the reaction mixture gas body that contains nickle carbonoxide imports the condensing air liquid/gas separator, collects nickle carbonoxide, the tail gas recycle.
Embodiment 13
In reactor, add the 30g corronel, reactor is through vacuumizing and with after the carbon monoxide displaced air, feed the CO (carbon monoxide converter) gas that contains an amount of ammonia continuously, under pressure 10MPa, 200 ℃ of conditions of temperature, reacted 48 hours, the reaction mixture gas body that contains nickle carbonoxide imports the condensing air liquid/gas separator, collect nickle carbonoxide, the tail gas recycle.
Table 1: the carbonylation yield of embodiment 1-14 nickel
| Yield (%) | Yield (%) | ||
| Embodiment one | ??98.73 | Embodiment eight | ????96.45 |
| Embodiment two embodiment three embodiment four embodiment five embodiment six embodiment seven | ??95.37 ??96.13 ??98.66 ??95.63 ??97.72 ??98.23 | Embodiment nine embodiment ten embodiment 11 embodiment 12 embodiment 13 | ????93.46 ????91.34 ????94.10 ????95.78 ????98.83 |
Claims (3)
1, a kind of synthetic method of nickle carbonoxide is characterized in that corronel or nickel copper alloy are placed fixed-bed reactor, feeds the CO (carbon monoxide converter) gas that contains catalyzer continuously, and control reaction pressure 5.0-15.0MPa, temperature 150-250 ℃ is reacted; Wherein catalyzer is ammonia, methylamine, ethamine, quadrol or triethylamine.
2, the method for claim 1, the volumn concentration that it is characterized in that containing catalyzer in the CO (carbon monoxide converter) gas of catalyzer is 0.5%-10%.
3, the method for claim 1 is characterized in that reaction raw materials cupronickel or nickel copper alloy, and the weight percentage of nickel is 25-75%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031350445A CN1305774C (en) | 2003-09-29 | 2003-09-29 | Method for synthesizing nickel tetracarbonyl |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB031350445A CN1305774C (en) | 2003-09-29 | 2003-09-29 | Method for synthesizing nickel tetracarbonyl |
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| Publication Number | Publication Date |
|---|---|
| CN1603240A true CN1603240A (en) | 2005-04-06 |
| CN1305774C CN1305774C (en) | 2007-03-21 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB031350445A Expired - Fee Related CN1305774C (en) | 2003-09-29 | 2003-09-29 | Method for synthesizing nickel tetracarbonyl |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100357188C (en) * | 2005-12-15 | 2007-12-26 | 钢铁研究总院 | Nickel carbonyl synthesizing method |
| CN101985366A (en) * | 2010-11-23 | 2011-03-16 | 金川集团有限公司 | Equipment and method for preparing carbonyl nickel spheres |
| CN102719801A (en) * | 2012-06-05 | 2012-10-10 | 金川集团股份有限公司 | Method for preparing nickel foil |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6153167A (en) * | 1998-05-12 | 2000-11-28 | American Air Liquide | Generation of metal-carbonyl standards for the calibration of spectroscopic systems |
| CN1184146C (en) * | 2002-08-01 | 2005-01-12 | 中国科学院兰州化学物理研究所 | Oxo-process of preparing nickel carbonyl from coarse ore nickel |
-
2003
- 2003-09-29 CN CNB031350445A patent/CN1305774C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100357188C (en) * | 2005-12-15 | 2007-12-26 | 钢铁研究总院 | Nickel carbonyl synthesizing method |
| CN101985366A (en) * | 2010-11-23 | 2011-03-16 | 金川集团有限公司 | Equipment and method for preparing carbonyl nickel spheres |
| CN101985366B (en) * | 2010-11-23 | 2013-02-13 | 金川集团有限公司 | Equipment and method for preparing carbonyl nickel spheres |
| CN102719801A (en) * | 2012-06-05 | 2012-10-10 | 金川集团股份有限公司 | Method for preparing nickel foil |
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| Publication number | Publication date |
|---|---|
| CN1305774C (en) | 2007-03-21 |
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Granted publication date: 20070321 Termination date: 20120929 |