CN102851490A - Method for preparing high-quality calcine by fluidized reduction roasting of nickel oxide ore - Google Patents
Method for preparing high-quality calcine by fluidized reduction roasting of nickel oxide ore Download PDFInfo
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Abstract
The invention discloses a method for preparing high-quality calcine by fluidized reduction roasting of nickel oxide ore, which comprises the steps of firstly crushing and grinding nickel ore, wherein the proportion of the particle size of the crushed and ground nickel ore smaller than 74 mu m is more than 70%, and then drying and dehydrating the crushed and ground nickel ore, wherein the water content of the dehydrated ore is not more than 10%; then heating the obtained dry ore in a first-stage fluidized bed furnace, wherein the heating temperature is more than 750 ℃; then carrying out fluidized circulating roasting on the heated ore in a reducing atmosphere (more than 80 percent of materials are forcibly circulated and returned to the furnace); and finally, performing rapid water quenching on the obtained selectively reduced ore, and performing liquid-solid separation after water quenching to obtain high-quality calcine, thereby laying a foundation for the subsequent efficient leaching and separation of valuable metals of nickel, cobalt and iron, and providing a new reduction roasting process idea for the reduction roasting-normal pressure ammonia leaching process of nickel oxide ore with abundant reserves and without realizing the comprehensive economic value of the nickel oxide ore.
Description
Technical field
The present invention relates to the method that a kind of nickel oxide ore prepares calcining, relate in particular to the method that a kind of fluidized reduction roasting oxidation nickel minerals prepares the high-quality calcining.
Background technology
Nickel is a kind of important strategy metal, is widely used in the industries such as stainless steel, superalloy, plating and chemical industry.The nickel resources of occurring in nature about 70% exists with the oxidized ore form, only has 30% to exist with the sulphide ores form, but in the at present nickel industry nearly 60% nickel from nickel sulfide ore.
The treatment process of red soil nickel ore can be divided into two kinds of pyrogenic process and wet methods.Pure wet processing mainly is acid leaching process, comprise normal pressure acidleach and pressurized acid leaching, the acid consumption is high, metal leaches poor selectivity and the low shortcoming of the rate of recovery and the normal pressure acid leaching process exists, pressurized acid leaching technique, though metal leaches selectivity and the rate of recovery increases, and has the drawback that cost of investment is high, the construction period is long, technology maturity is inadequate.Pure thermal process mainly is the nickel metallurgy iron process, be divided into blast furnace (or blast furnace) melting technology and rotary kiln-electric furnace reduction melting technology, the former environmental pollution is serious, energy consumption is high, to be subject to the restriction of national environmental protection policy and Energy policy, though and the latter be fit to process various types of red soil nickel ores, but its energy consumption is large, only power consumption just accounts for 50% of cost, requires simultaneously ore that higher nickel grade is arranged.
Patent CN1858274 discloses a kind of New Method for Processing of nickel oxide ore, although this method adopts normal pressure to leach, reduce energy consumption and reduced Technology difficulty and running cost, but nickel oxide ore can't be converted into the nickel product, and two step of magnetic separation and flotation waste can cause the corresponding loss of valuable metal in the technique.
Patent CN101020957 discloses a kind of new technology of rotary hearth furnace rapid reduction of carbonaceous nickel oxide ore pelletizing enriching nickel, though this method technical process is short, adaptability to raw material is strong, nickel recovery is high, but this method does not relate to iron and recovery of Co utilization in the ore deposit, and only nickel has been carried out enrichment, the enrichment nickel minerals that obtains also needs to select further refining technique.
Patent CN1718787 discloses a kind of method of low-grade nickel oxide ore bulk infusion extracting nickel cobalt, though this method has been avoided the with high investment and high running cost of pressure leaching, but the acid consumption is large and iron is leached in a large number, for follow-up nickeliferous purification brings difficulty, this technique raffinate amount is large simultaneously, work period is longer, and efficient is lower.
Patent CN1827799A discloses and has a kind ofly reclaimed the method for nickel cobalt from nickel oxide ore silicic acid nickel minerals, and this method is allocated pelletizing behind coke powder, chlorizating agent and the auxiliary agent after being ground to into raw ore is broken, adopts chlorination segregation-magnetic separation that material is processed.This method is simple and environmental protection is better, but nickel, the cobalt rate of recovery of this method processing red soil nickel ore are lower, only have respectively 80% and 70%, and iron are not fully utilized.
Patent CN1995414 discloses the vitriol intensified leach extraction method of nickel oxide ore, although this method is lower than conventional pressure leaching process equipment requirements, technology is grasped easily, and metal leaching selectivity is bad, and foreign matter content is higher in the leach liquor, and subsequent purification is difficult.
By contrast, the reduction roasting-ammonia leaching process quilt that is proposed by professor Caron is thought comparatively successful Proress Technolgies of Laterite-nickel Ore.The operation of in succession building up and go into operation in Cuba Nicaro, Australian Townsville, Philippines Marinduque, Albania and Chinese first tor smeltery of this technique.The purpose of this technique reducing roasting is that the nickel in the ore deposit and cobalt mineralss are reduced into metal to greatest extent, and the reduction-state of control iron is Fe
3O
4, then the gained calcining is leached in ammonia solution, and then continues next step nickel product preparation section.Reducing roasting is the key of whole technique, how can control the reduction degree of nickel/cobalt and iron well, namely nickel/cobalt metallize as far as possible and iron do not metallize as far as possible will be most important to the comprehensive utilization of nickel and cobalt recovery rate and iron.Reducing roasting can adopt multiple hearth furnace, rotary kiln and fluidized bed furnace to realize in general, Nicaro adopts the smeltery many thoraxes reverberatory furnace, Townsville and Marinduque smeltery adopt laminar Herreschoff reduction roaster, what unit tor smeltery adopted is rotary kiln, and the nickel cobalt purification factory that is second to the cooperative development seventies in last century by China and Albany then adopts two sections fluidizing furnaces.The processing power that multiple hearth furnace and rotary kiln and fluidized bed furnace compare the ore deposit is lower, energy consumption is slightly high, and because of the long effective control that does not utilize nickel and iron selective reduction of the residence time, two sections fluidizing furnaces generally are fit to process the laterite of particle diameter 0～3mm, for ore particle footpath less than 74 μ m account for more than 70% breeze then and be not suitable for, reason is that fluidizing furnace can not guarantee the residence time enough than mineral fine, causes the metallization of nickel cobalt insufficient, affects nickel and cobalt recovery.
To sum up, how can control well nickel and iron in the ore deposit the efficient selective reduction and obtain the high-quality calcining, improve simultaneously the processing power of FU time, reducing energy consumption is the key that realizes the efficient high value processing nickel oxide ore of reducing roasting-normal pressure ammonia soaking technology.
Summary of the invention
The purpose of this invention is to provide the method that a kind of fluidized reduction roasting oxidation nickel minerals prepares the high-quality calcining, this method adopts the method for one section fluidizing furnace heating and one section circulating fluidized bed reduction to realize well controlling the selective reduction of nickel, cobalt and iron in the ore deposit within a short period of time, and then obtains the high-quality calcining.
The objective of the invention is to be achieved through the following technical solutions:
Fluidized reduction roasting oxidation nickel minerals of the present invention prepares the method for high-quality calcining, comprises step:
Broken mill/the drying of A, nickel minerals: nickel minerals break mill, require the rear particle diameter of broken mill less than the ratio of 74 μ m greater than 70%, then carry out drying and dehydrating, dewater that rear the ore deposit is moisture is no more than 10%, dried ore deposit enters step B;
B, the heating of first paragraph fluidizing furnace: the dried ore deposit that steps A obtains is heated in the first paragraph fluidizing furnace, and Heating temperature is more than 750 ℃, is heated rear ore deposit and enters step C;
The reduction of C, second segment circulating fluidized bed: circulating fluid-bed is sent in the ore deposit after the heating that step B is obtained, and carries out fluidization circulation roasting under reducing atmosphere, and the ore deposit after being reduced by selectivity enters step D;
D, shrend/liquid-solid separation: with step C obtain reduced by selectivity after the ore deposit carry out quick shrend, liquid-solid separation after the shrend obtains the high-quality calcining and is sent to follow-up leaching operation, liquid then returns the recycle of shrend operation.
As seen from the above technical solution provided by the invention, the fluidized reduction roasting oxidation nickel minerals that the embodiment of the invention provides prepares the method for high-quality calcining, because wherein the first paragraph fluidizing furnace is used for heating, the second segment circulating fluidized bed is used for reducing, obtain the high-quality calcining, can well control nickel in the ore deposit within a short period of time, the selective reduction of cobalt and iron, and then obtain the high-quality calcining, be follow-up efficient leaching separating valuable metals nickel, cobalt and iron lay the foundation, for reserves are abundant but the always nickel oxide ore reducing roasting that is worth of unrealized its mixed economy-normal pressure ammonia soaking technology provides a kind of new reducing roasting technique thinking.
Description of drawings
The fluidized reduction roasting oxidation nickel minerals that Fig. 1 provides for the embodiment of the invention prepares the schematic flow sheet of the method for high-quality calcining.
Embodiment
The below will be described in further detail the embodiment of the invention.
Fluidized reduction roasting oxidation nickel minerals of the present invention prepares the method for high-quality calcining, and its better embodiment comprises step as shown in Figure 1:
Broken mill/the drying of A, nickel minerals: nickel minerals break mill, require the rear particle diameter of broken mill less than the ratio of 74 μ m greater than 70%, then carry out drying and dehydrating, dewater that rear the ore deposit is moisture is no more than 10%, dried ore deposit enters step B;
B, the heating of first paragraph fluidizing furnace: the dried ore deposit that steps A obtains is heated in the first paragraph fluidizing furnace, and Heating temperature is more than 750 ℃, is heated rear ore deposit and enters step C;
The reduction of C, second segment circulating fluidized bed: circulating fluid-bed is sent in the ore deposit after the heating that step B is obtained, and carries out fluidization circulation roasting under reducing atmosphere, and the ore deposit after being reduced by selectivity enters step D;
D, shrend/liquid-solid separation: with step C obtain reduced by selectivity after the ore deposit carry out quick shrend, liquid-solid separation after the shrend obtains the high-quality calcining and is sent to follow-up leaching operation, liquid then returns the recycle of shrend operation.
Broken mill in the described steps A is wet-milling or dry grinding.
Drying in the described steps A adopts rotary kiln drying, and drying temperature is 200～350 ℃.
Carrier gas when the first paragraph fluidizing furnace among the described step B heats is air or oxygen-rich air.
First paragraph fluidizing furnace heat source among the described step B is provided as the heating of electrically heated or fuel, and Heating temperature is 750～900 ℃, and fuel used is one or more of heavy oil, coal, Sweet natural gas and liquefied gas.
The residence time in ore deposit was 10～30min when the first paragraph fluidizing furnace among the described step B heated.
Carrier gas among the described step C during two sections circulating fluidized beds reduction of the is the mixture of reducing gas and rare gas element, and blending ratio is that reducing gas and rare gas element volume ratio are 1: 1～1: 10.
The reducing gas of second segment circulating fluidized bed among described step C reduction be carbon monoxide and hydrogen one or both, rare gas element is one or both of nitrogen and carbonic acid gas, the add-on of reducing gas is for adding 5～20% of ore deposit amount.
The internal circulating load in ore deposit was more than 80% of total ore deposit amount when the second segment circulating fluidized bed among the described step C reduced, and the residence time in ore deposit is 10～30min during reduction.
Dense separation or band filter filtering separation are adopted in liquid-solid separation among the described step D.
Described nickel oxide ore comprises brown swage laterite and/or garnirite.
The present invention adopts the method for two sections fluidized reduction roasting oxidation nickel minerals, wherein the first paragraph fluidizing furnace is used for heating, the second segment circulating fluidized bed is used for reducing, obtain the high-quality calcining, for follow-up efficient leaching separating valuable metals nickel, cobalt and iron lay the foundation, for reserves are abundant but the always nickel oxide ore reducing roasting that is worth of unrealized its mixed economy-normal pressure ammonia soaking technology provides a kind of new reducing roasting technique thinking.With the present invention and the contrast of existing nickel oxide ore reducing roasting technique, can find following advantage:
(1) introducing of fluidizing furnace and circulating fluidized bed has realized the fluosolids roasting of nickel oxide ore, the employing of second segment circulating fluidized bed technique is melted down the breeze pump circulation more than 80%, guaranteed that breeze has sufficient reaction time in stove, thereby made the reduction of metal target efficient selective.
The employing of (2) two sections fluosolids roastings, reduction section is separated with heating zone, guaranteed the reducing atmosphere of reduction section nickel minerals, and atmosphere is convenient to control, be conducive to realize the selective reduction of metal, also guarantee simultaneously abundant burning and the calorific value utilization of heating zone fuel, improved the processing power of equipment, reduced energy consumption and production cost.
(3) gained calcining nickel, cobalt degree of metalization height, and the degree of metalization of iron is very low, realized the selective reduction of three kinds of object elements, lay a good foundation the comprehensive high-value-use of associated element iron when being conducive to realize valuable element nickel in the nickel oxide ore/cobalt high-recovery for follow-up leaching and iron recovery process.
Embodiment 1:
Referring to accompanying drawing, raw ore gets particle diameter and accounts for 80% nickel oxide ore less than 74 μ m after broken wet-milling, then in rotary kiln through 200 ℃ of dryings, get moisture 8% breeze, send into one section fluidizing furnace, 800 ℃ of lower heating, the heating heat is provided by heavy oil, the ore deposit residence time is 15min, and breeze enters two sections circulating fluidized beds after the heating, passes into carbon monoxide and nitrogen, wherein the volume ratio of carbon monoxide and nitrogen is 1: 10, the carbon monoxide add-on is for adding 5% of ore deposit amount, and the ore deposit residence time is 15min, and quick shrend is sent in the ore deposit after being reduced, carry out liquid-solid separation after the shrend, the nickel reduction degree reaches 83 ± 5% in the gained high-quality calcining, and the cobalt reduction degree reaches 80 ± 5%, and the iron reduction degree reaches 85 ± 5%, ferrous metal rate 4%, calcining is sent into follow-up leaching operation, and one section fluidizing furnace is returned in the thin ore deposit of dust collecting system gained, and gas is lighted rear emptying.
Embodiment 2:
Raw ore gets particle diameter and accounts for 70% nickel oxide ore less than 74 μ m after broken wet-milling, then in rotary kiln through 250 ℃ of dryings, get moisture 6% breeze, send into one section fluidizing furnace, 780 ℃ of lower heating, the heating heat is provided by coal dust, and the ore deposit residence time is 25min, breeze enters two sections circulating fluidized beds after the heating, pass into carbon monoxide and nitrogen, wherein the volume ratio of carbon monoxide and nitrogen is 1: 5, and the carbon monoxide add-on is for adding 10% of ore deposit amount, the ore deposit residence time is 25min, quick shrend is sent in ore deposit after being reduced, carries out liquid-solid separation after the shrend, and the nickel reduction degree reaches 85 ± 3% in the gained high-quality calcining, the cobalt reduction degree reaches 80 ± 3%, the iron reduction degree reaches 87 ± 3%, ferrous metal rate 5%, and calcining is admitted to follow-up leaching operation, one section fluidizing furnace is returned in the thin ore deposit of dust collecting system gained, and gas is lighted rear emptying.
Embodiment 3:
Raw ore gets particle diameter and accounts for 85% nickel oxide ore less than 74 μ m after broken wet-milling, then in rotary kiln through 300 ℃ of dryings, get moisture 5% breeze, send into one section fluidizing furnace, 820 ℃ of lower heating, the heating heat is provided by electrically heated, and the ore deposit residence time is 20min, breeze enters two sections circulating fluidized beds after the heating, pass into carbon monoxide and carbonic acid gas, wherein the volume ratio of carbon monoxide and nitrogen is 1: 7, and the carbon monoxide add-on is for adding 15% of ore deposit amount, the ore deposit residence time is 20min, quick shrend is sent in ore deposit after being reduced, carries out liquid-solid separation after the shrend, and the nickel reduction degree reaches 83 ± 3% in the gained high-quality calcining, the cobalt reduction degree reaches 80 ± 3%, the iron reduction degree reaches 85 ± 3%, ferrous metal rate 4%, and calcining is admitted to follow-up leaching operation, one section fluidizing furnace is returned in the thin ore deposit of dust collecting system gained, and gas is lighted rear emptying.
Embodiment 4:
Raw ore gets particle diameter and accounts for 90% nickel oxide ore less than 74 μ m after broken wet-milling, then in rotary kiln through 350 ℃ of dryings, get moisture 3% breeze, send into one section fluidizing furnace, 750 ℃ of lower heating, the heating heat is provided by coal dust, and the ore deposit residence time is 30min, breeze enters two sections circulating fluidized beds after the heating, pass into carbon monoxide and nitrogen, wherein the volume ratio of carbon monoxide and nitrogen is 1: 3, and the carbon monoxide add-on is for adding 20% of ore deposit amount, the ore deposit residence time is 30min, quick shrend is sent in ore deposit after being reduced, carries out liquid-solid separation after the shrend, and the nickel reduction degree reaches 81 ± 3% in the gained high-quality calcining, the cobalt reduction degree reaches 79 ± 3%, the iron reduction degree reaches 84 ± 3%, ferrous metal rate 3%, and calcining is admitted to follow-up leaching operation, one section fluidizing furnace is returned in the thin ore deposit of dust collecting system gained, and gas is lighted rear emptying.
Embodiment 5:
Raw ore gets particle diameter and accounts for 100% nickel oxide ore less than 74 μ m after broken wet-milling, then in rotary kiln through 280 ℃ of dryings, get moisture 5% breeze, send into one section fluidizing furnace, 900 ℃ of lower heating, the heating heat is provided by coal dust, and the ore deposit residence time is 10min, breeze enters two sections circulating fluidized beds after the heating, pass into carbon monoxide and carbonic acid gas, wherein the volume ratio of carbon monoxide and nitrogen is 1: 1, and the carbon monoxide add-on is for adding 5% of ore deposit amount, the ore deposit residence time is 10min, quick shrend is sent in ore deposit after being reduced, carries out liquid-solid separation after the shrend, and the nickel reduction degree reaches 85 ± 3% in the gained high-quality calcining, the cobalt reduction degree reaches 82 ± 3%, the iron reduction degree reaches 85 ± 3%, ferrous metal rate 4%, and calcining is admitted to follow-up leaching operation, one section fluidizing furnace is returned in the thin ore deposit of dust collecting system gained, and gas is lighted rear emptying.
The above; only for the better embodiment of the present invention, but protection scope of the present invention is not limited to this, anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (10)
1. a fluidized reduction roasting oxidation nickel minerals prepares the method for high-quality calcining, it is characterized in that, comprises step:
Broken mill/the drying of A, nickel minerals: nickel minerals break mill, require the rear particle diameter of broken mill less than the ratio of 74 μ m greater than 70%, then carry out drying and dehydrating, dewater that rear the ore deposit is moisture is no more than 10%, dried ore deposit enters step B;
B, the heating of first paragraph fluidizing furnace: the dried ore deposit that steps A obtains is heated in the first paragraph fluidizing furnace, and Heating temperature is more than 750 ℃, is heated rear ore deposit and enters step C;
The reduction of C, second segment circulating fluidized bed: circulating fluid-bed is sent in the ore deposit after the heating that step B is obtained, and carries out fluidization circulation roasting under reducing atmosphere, and the ore deposit after being reduced by selectivity enters step D;
D, shrend/liquid-solid separation: with step C obtain reduced by selectivity after the ore deposit carry out quick shrend, liquid-solid separation after the shrend obtains the high-quality calcining and is sent to follow-up leaching operation, liquid then returns the recycle of shrend operation.
2. fluidized reduction roasting oxidation nickel minerals according to claim 1 prepares the method for high-quality calcining, it is characterized in that, the broken mill in the described steps A is wet-milling or dry grinding.
3. fluidized reduction roasting oxidation nickel minerals according to claim 1 prepares the method for high-quality calcining, it is characterized in that, the drying in the described steps A adopts rotary kiln drying, and drying temperature is 200～350 ℃.
4. fluidized reduction roasting oxidation nickel minerals according to claim 1 prepares the method for high-quality calcining, it is characterized in that, the carrier gas when the first paragraph fluidizing furnace among the described step B heats is air or oxygen-rich air.
5. fluidized reduction roasting oxidation nickel minerals according to claim 4 prepares the method for high-quality calcining, it is characterized in that, first paragraph fluidizing furnace heat source among the described step B is provided as electrically heated or fuel heating, Heating temperature is 750～900 ℃, and fuel used is one or more of heavy oil, coal, Sweet natural gas and liquefied gas.
6. fluidized reduction roasting oxidation nickel minerals according to claim 5 prepares the method for high-quality calcining, it is characterized in that, the residence time in ore deposit was 10～30min when the first paragraph fluidizing furnace among the described step B heated.
7. fluidized reduction roasting oxidation nickel minerals according to claim 1 prepares the method for high-quality calcining, it is characterized in that, carrier gas among the described step C during two sections circulating fluidized beds reduction of the is the mixture of reducing gas and rare gas element, and blending ratio is that reducing gas and rare gas element volume ratio are 1: 1～1: 10.
8. fluidized reduction roasting oxidation nickel minerals according to claim 7 prepares the method for high-quality calcining, it is characterized in that, the reducing gas of second segment circulating fluidized bed among described step C reduction be carbon monoxide and hydrogen one or both, rare gas element is one or both of nitrogen and carbonic acid gas, the add-on of reducing gas is for adding 5～20% of ore deposit amount;
The internal circulating load in ore deposit was more than 80% of total ore deposit amount when the second segment circulating fluidized bed among the described step C reduced, and the residence time in ore deposit is 10～30min during reduction.
9. fluidized reduction roasting oxidation nickel minerals according to claim 1 prepares the method for high-quality calcining, it is characterized in that, dense separation or band filter filtering separation are adopted in the liquid-solid separation among the described step D.
10. prepare according to claim 1 the method for high-quality calcining to 9 each described fluidized reduction roasting oxidation nickel minerals, it is characterized in that described nickel oxide ore comprises brown swage laterite and/or garnirite.
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Cited By (6)
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| CN103421924A (en) * | 2013-07-10 | 2013-12-04 | 中国恩菲工程技术有限公司 | Fluidization laterite ore reducing method |
| CN103740927A (en) * | 2014-01-02 | 2014-04-23 | 上海大学 | Method for recovering ferronickel refined ore powder and ferrous powder from laterite nickel ores by two-step reduction method |
| CN106086468A (en) * | 2016-08-09 | 2016-11-09 | 江苏省冶金设计院有限公司 | A kind of method and system utilizing ferronickel powder to extract nickel oxide |
| CN106086469A (en) * | 2016-08-09 | 2016-11-09 | 江苏省冶金设计院有限公司 | A kind of method and system utilizing lateritic nickel ore to extract nickel oxide |
| CN106086467A (en) * | 2016-08-09 | 2016-11-09 | 江苏省冶金设计院有限公司 | A kind of method and system utilizing lateritic nickel ore to extract nickel oxide |
| CN116426768A (en) * | 2023-05-16 | 2023-07-14 | 东北大学 | Method for synchronously reducing and cooperatively recycling cobalt and iron in cobalt oxide ore by dry method |
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| CN106086468A (en) * | 2016-08-09 | 2016-11-09 | 江苏省冶金设计院有限公司 | A kind of method and system utilizing ferronickel powder to extract nickel oxide |
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| CN106086467A (en) * | 2016-08-09 | 2016-11-09 | 江苏省冶金设计院有限公司 | A kind of method and system utilizing lateritic nickel ore to extract nickel oxide |
| CN106086469B (en) * | 2016-08-09 | 2018-08-28 | 江苏省冶金设计院有限公司 | A kind of method and system for extracting nickel oxide using lateritic nickel ore |
| CN116426768A (en) * | 2023-05-16 | 2023-07-14 | 东北大学 | Method for synchronously reducing and cooperatively recycling cobalt and iron in cobalt oxide ore by dry method |
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