CN1184146C - Oxo-process of preparing nickel carbonyl from coarse ore nickel - Google Patents
Oxo-process of preparing nickel carbonyl from coarse ore nickel Download PDFInfo
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- CN1184146C CN1184146C CN 02128343 CN02128343A CN1184146C CN 1184146 C CN1184146 C CN 1184146C CN 02128343 CN02128343 CN 02128343 CN 02128343 A CN02128343 A CN 02128343A CN 1184146 C CN1184146 C CN 1184146C
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Abstract
The present invention discloses a method for synthesizing and preparing nickel carbonyl from crude ore nickel. In the method, the crude ore nickel directly used as a reactant, carbon monoxide as reaction gas and hydrogen sulfide gas as a catalyst react for 8 to 12 hours under the operating conditions of reaction temperature of 160 to 200 DEG C and reaction pressure of 3.0 to 8.5MPa to generate the nickel carbonyl with the nickel extraction rate as high as 98%. The present invention shortens reaction time, and does not need to treat reaction materials so as to simplify reaction technology.
Description
Technical field
The present invention relates to the synthetic method for preparing nickle carbonoxide of a kind of rough nickel carbonyl group.
Background technology
Nickel is as important non-ferrous metal, widespread use in every field such as chemical industry, building, military affairs, Iron And Steel Industry, electronic industry, novel material.As far back as 1883, the patent report of separating nickel is just arranged, aspect the purification of nickel, be main means originally with electrolysis, still, the purity of electrolytic nickel will be subjected to the restriction of material purity.Along with science and technology development, more and more stricter to the specification of quality of nickel, electrolytic nickel can not satisfy the requirement of science and technology in some fields.Under the demand of this science and technology, latest developments a kind of carbonylation technology of refining nickel, can prepare fine nickel raw material by the nickle carbonoxide of this explained hereafter by decomposing, therefore people's attention extremely.The method of utilizing carbonylation to extract nickel in the raw mineral materials at present is representative with Canadian mesolow technology and Muscovite pressure technique mainly.The non-pressure process efficiency ratio that INCO company is adopted is lower, the used device structure complexity of middle-pressure process that the said firm adopts, also need to solve technical problems such as dynamic seal, raw materials used also is processing by strictness, therefore can limit being extensive use of of this technology in varying degrees.Though the pressure carbonylation method that Russian northern nickel company adopts has simple operation and other advantages, reaction pressure and temperature of reaction be all than higher, and long reaction time simultaneously needs 48 hours as an oxonation cycle.As seen, no matter use which type of technology, the defective of blemish in an otherwise perfect thing is always arranged.Equally, the difference of reaction raw materials, technology also need to make creationary research work.
Summary of the invention
The objective of the invention is to overcome rough nickel in the prior art need carry out long deficiency of pre-treatment and carbonylation reaction time and provide a kind of rough nickel carbonyl group the synthetic method for preparing nickle carbonoxide.
The present invention mainly be with rough nickel directly as reactant, mainly contain metal Fe4-10wt%, Co1-7wt%, Cu8-20wt%, Ni40-70wt% and minute amount of noble metal and non-metallic element O, S, C in the rough nickel.Utilize carbon monoxide to generate nickle carbonoxide with the oxonation of the generation of the nickel in the rough nickel.The hydrogen sulfide that mixes trace in reaction of carbon monoxide gas shortens the reaction times and improves the purpose that nickel transforms thereby reach as catalyzer.
Rough nickel used in the present invention does not need to handle before oxonation as reaction raw materials, directly carries out oxonation.
The synthetic method for preparing nickle carbonoxide of a kind of rough nickel carbonyl group, it is characterized in that this method will mainly contain the rough nickel of metal Fe4-10wt%, Co1-7wt%, Cu8-20wt%, Ni40-70wt% and minute amount of noble metal and non-metallic element O, S, C directly as reactant, with carbon monoxide as reaction gas, hydrogen sulfide is as catalyzer, in temperature of reaction is 160-200 ℃, reaction pressure is under the operational condition of 3.0-8.5Mpa, reacts to generate nickle carbonoxide in 8-12 hour.
The volumetric concentration of catalyst vulcanization hydrogen of the present invention in reaction gas is 10
-4-1%.
The particle diameter of the rough nickel that the present invention adopts is the 5-90 order.
After the present invention had used hydrogen sulfide as catalyzer, selected raw material was no longer handled before oxonation, and had accelerated the oxonation speed and the transformation efficiency that has improved nickel of nickel.But hydrogen sulfide is to the obvious effect of reaction, and the content height can shorten the reaction times, but partial vulcanization hydrogen can enter into the product nickle carbonoxide and influence quality product, can influence the conversion of nickel in the time of seriously.So the concentration of hydrogen sulfide is 10
-4-1% o'clock is best.
The reaction pressure height can improve speed of response, still, the high input that can increase fixed capital of pressure, the while also can increase the danger of operation, because nickle carbonoxide is a kind of volatilizable deadly poisonous compound.Reaction of the present invention can be carried out between 160-200 ℃ preferably, when temperature of reaction is higher than 200 ℃, can suppress the carrying out of oxonation on the contrary.
Concrete preparation method of the present invention packs rough nickel in the etch-proof fixed-bed reactor into, the carbon monoxide that feeding configures and the gas mixture of hydrogen sulfide, after the air Ex-all in the reaction system, begin to heat up, reaction controls under certain temperature and the pressure and reacts, till can not be carried out.
Method of the present invention can make the extraction yield of nickel reach more than 98%.
Method of the present invention has been compared following substantive distinguishing features with prior art:
1, the oxonation technology is applied to the refinement of nickel element in the more complicated raw material of component;
2, shorten the reaction times, increase work efficiency;
3, simplify reaction process, do not need reaction raw materials is handled, reduce production costs;
4, reduce temperature of reaction, reach save energy and reduce the purpose that the nickle carbonoxide that generates decomposes again.
Embodiment
Embodiment 1
30 gram raw materials described raw materials are packed in the corrosion resistant tubular reactor into Ni (50%) wherein, Fe (7.2%), Cu (15.7%), Co (1.2%).The particle diameter of raw material is the 45-60 order.Feeding contains the carbon monoxide of 0.1% hydrogen sulfide, is 200 ℃ in temperature, and pressure is under the 7.0Mpa reaction conditions, reacts 10 hours, and the extraction yield of nickel is 99.2%.
Embodiment 2
30 gram raw materials described raw materials are packed in the corrosion resistant tubular reactor into Ni (65%) wherein, Fe (6.8%), Cu (13.5%), Co (1.1%).The particle diameter of raw material is the 5-15 order.Feeding contains the carbon monoxide of 0.5% hydrogen sulfide, is 200 ℃ in temperature, and pressure is under the 4.0Mpa reaction conditions, reacts 12 hours, and the extraction yield of nickel is 98.7%.
Embodiment 3
30 gram raw materials described raw materials are packed in the corrosion resistant tubular reactor into Ni (70%) wherein, Fe (6.4%), Cu (11.5%), Co (1.3%).The particle diameter of raw material is the 18-32 order.Feeding contains the carbon monoxide of 0.1% hydrogen sulfide, is 160 ℃ in temperature, and pressure is under the 5.0Mpa reaction conditions, reacts 12 hours, and the extraction yield of nickel is 98.5%.
Embodiment 4
30 gram raw materials described raw materials are packed in the corrosion resistant tubular reactor into Ni (50%) wherein, Fe (7.2%), Cu (15.7%), Co (1.2%).The particle diameter of raw material is the 45-60 order.Feeding contains the carbon monoxide of 0.01% hydrogen sulfide, is 170 ℃ in temperature, and pressure is under the 8.0Mpa reaction conditions, reacts 9 hours, and the extraction yield of nickel is 99.2%.
Embodiment 5
30 gram raw materials described raw materials are packed in the corrosion resistant tubular reactor into Ni (65%) wherein, Fe (6.8%), Cu (13.5%), Co (1.1%).The particle diameter of raw material is the 45-60 order.Feeding contains the carbon monoxide of 0.2% hydrogen sulfide, is 200 ℃ in temperature, and pressure is under the 8.5Mpa reaction conditions, reacts 8 hours, and the extraction yield of nickel is 99.3%.
Embodiment 6
30 gram raw materials described raw materials are packed in the corrosion resistant tubular reactor into Ni (70%) wherein, Fe (6.4%), Cu (11.5%), Co (1.3%).The particle diameter of raw material is the 18-32 order.Feeding contains the carbon monoxide of 0.1% hydrogen sulfide, is 195 ℃ in temperature, and pressure is under the 3.5Mpa reaction conditions, reacts 11 hours, and the extraction yield of nickel is 98.2%.
Embodiment 7
30 gram raw materials described raw materials are packed in the corrosion resistant tubular reactor into Ni (70%) wherein, Fe (6.4%), Cu (11.5%), Co (1.3%).The particle diameter of raw material is the 18-32 order.Feeding contains the carbon monoxide of 0.08% hydrogen sulfide, is 200 ℃ in temperature, and pressure is under the 7.0Mpa reaction conditions, reacts 10 hours, and the extraction yield of nickel is 99.2%.
Embodiment 8
30 gram raw materials described raw materials are packed in the corrosion resistant tubular reactor into Ni (70%) wherein, Fe (6.4%), Cu (11.5%), Co (1.3%).The particle diameter of raw material is the 70-90 order.Feeding contains the carbon monoxide of 0.05% hydrogen sulfide, is 175 ℃ in temperature, and pressure is under the 6.0Mpa reaction conditions, reacts 9 hours, and the extraction yield of nickel is 99.2%.
Embodiment 9
30 gram raw materials described raw materials are packed in the corrosion resistant tubular reactor into Ni (70%) wherein, Fe (6.4%), Cu (11.5%), Co (1.3%).The particle diameter of raw material is the 10-50 order.Feeding contains the carbon monoxide of 0.04% hydrogen sulfide, is 180 ℃ in temperature, and pressure is under the 7.0Mpa reaction conditions, reacts 10 hours, and the extraction yield of nickel is 99.2%.
Embodiment 10
30 gram raw materials described raw materials are packed in the corrosion resistant tubular reactor into Ni (70%) wherein, Fe (6.4%), Cu (11.5%), Co (1.3%).The particle diameter of raw material is the 18-32 order.Feeding contains the carbon monoxide of 0.2% hydrogen sulfide, is 160 ℃ in temperature, and pressure is under the 6.5Mpa reaction conditions, reacts 10 hours, and the extraction yield of nickel is 99.2%.
Embodiment 11
30 gram raw materials described raw materials are packed in the corrosion resistant tubular reactor into Ni (70%) wherein, Fe (6.4%), Cu (11.5%), Co (1.3%).The particle diameter of raw material is the 18-32 order.Feeding contains the carbon monoxide of 1% hydrogen sulfide, is 175 ℃ in temperature, and pressure is under the 5.0Mpa reaction conditions, reacts 10 hours, and the extraction yield of nickel is 99.2%.
Embodiment 12
30 gram raw materials described raw materials are packed in the corrosion resistant tubular reactor into Ni (70%) wherein, Fe (6.4%), Cu (11.5%), Co (1.3%).The particle diameter of raw material is the 18-32 order.Feeding contains the carbon monoxide of 0.9% hydrogen sulfide, is 170 ℃ in temperature, and pressure is under the 4.5Mpa reaction conditions, reacts 10 hours, and the extraction yield of nickel is 98.7%.
Claims (2)
1. a rough nickel carbonyl group synthesizes the method for preparing nickle carbonoxide, it is characterized in that this method will mainly contain the rough nickel of metal Fe4-10wt%, Co1-7wt%, Cu8-20wt%, Ni40-70wt% and minute amount of noble metal and non-metallic element O, S, C directly as reactant, with carbon monoxide as reaction gas, hydrogen sulfide is as catalyzer, the volumetric concentration of hydrogen sulfide in reaction gas is 10-4-1%, in temperature of reaction is 160-200 ℃, reaction pressure is under the operational condition of 3.0-8.5Mpa, reacts to generate nickle carbonoxide in 8-12 hour.
2. as the said method of claim 1, the particle diameter that it is characterized in that rough nickel is the 5-90 order.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02128343 CN1184146C (en) | 2002-08-01 | 2002-08-01 | Oxo-process of preparing nickel carbonyl from coarse ore nickel |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02128343 CN1184146C (en) | 2002-08-01 | 2002-08-01 | Oxo-process of preparing nickel carbonyl from coarse ore nickel |
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| CN1398792A CN1398792A (en) | 2003-02-26 |
| CN1184146C true CN1184146C (en) | 2005-01-12 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100455191C (en) * | 2003-07-18 | 2009-01-28 | 有限公司阿斯考特 | Straw disinfection equipment, method for producing straw disinfection apparatus and disinfected straw product |
| CN1305774C (en) * | 2003-09-29 | 2007-03-21 | 中国科学院兰州化学物理研究所 | Method for synthesizing nickel tetracarbonyl |
| CN100357188C (en) * | 2005-12-15 | 2007-12-26 | 钢铁研究总院 | Nickel carbonyl synthesizing method |
| CN100364898C (en) * | 2006-03-17 | 2008-01-30 | 金川集团有限公司 | Method for circulation utilizing CO gas in carbonyl nickel synthetic process |
| CN103056390A (en) * | 2012-12-21 | 2013-04-24 | 中国钢研科技集团有限公司 | Constant pressure carbonylation method of flue ash containing nickel |
| CN104556249A (en) * | 2014-12-09 | 2015-04-29 | 金川集团股份有限公司 | Method for enhancing activity of raw material for preparing nickel carbonyl |
| CN113735199B (en) * | 2021-08-25 | 2022-11-15 | 广东邦普循环科技有限公司 | Method for preparing nickel sulfate from nickel iron |
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