CN104109756B - High-purity iron oxide red wet fire one subtraction unit and high-purity iron oxide red preparation method - Google Patents
High-purity iron oxide red wet fire one subtraction unit and high-purity iron oxide red preparation method Download PDFInfo
- Publication number
- CN104109756B CN104109756B CN201410319562.2A CN201410319562A CN104109756B CN 104109756 B CN104109756 B CN 104109756B CN 201410319562 A CN201410319562 A CN 201410319562A CN 104109756 B CN104109756 B CN 104109756B
- Authority
- CN
- China
- Prior art keywords
- pipeline
- iron oxide
- oxide red
- absorption tower
- purity iron
- 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.)
- Active
Links
Classifications
-
- 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
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention relates to high-purity iron oxide red technical field, be a kind of high-purity iron oxide red wet fire one subtraction unit and high-purity iron oxide red preparation method；This high-purity iron oxide red wet fire one subtraction unit, including ball mill by wet process, acidleach tank, single filter machine, removing calcium and magnesium tank, cascade filtration machine, preconcentrator, slurry absorption tower, hydrolysis calcining furnace and rotary calciner；The discharge end of ball mill by wet process and the feed end of acidleach tank are fixed together by the first pipeline.It is high-purity iron oxide red that the present invention utilizes pyro metallurgical plant rotary calciner to produce, and the chloride high-temperature flue gas of generation both provided heat for hydrolysis calcining kiln, achieved again wet dedusting, the HCl being stripped of in flue gas and dust；Utilizing the acidleach technology of hydrometallurgy, complete the removing of impurity in siderite, the hydrochloric acid in the present invention can recycle, do not introduce other media, produce without byproduct, there is no secondary pollution, thus reduce production cost, it is achieved that the comprehensive utilization of low-grade siderite.
Description
Technical field
The present invention relates to high-purity iron oxide red technical field, be a kind of high-purity iron oxide red wet fire one subtraction unit and high-purity iron oxide red preparation method.
Background technology
Hydrometallurgy is exactly that metalliferous mineral raw material carries out chemical treatment or organic solvent extraction in the aqueous solution of acid medium or alkaline medium, separates impurity, extraction metal and the process of compound thereof.The advantage of hydrometallurgy is that in raw material, valuable metal synthetical recovery degree is high, and production process is easier to realize serialization and automation.Pyrometallurgy fuel, electric energy or other energy produce high temperature, at high temperature, extract and refined metals or its compound from ore.Pyrometallurgy typically divides ore to prepare, smelt, refine and the step such as fume treatment.The main chemical reactions of pyrometallurgy is reduction-oxidation reaction.Pyrometallurgy has technical maturity, easy large-scale production, has dominant position at metallurgy industry.But pyrogenic process there is also and the grade of ore requires high, energy consumption height, and high-temperature flue gas is difficult to the problem thoroughly processed, thus adds production cost.
And wet method has applicability, has applicability and valuable metal comprehensive utilization yield height to similar metals mineral difficulty separation mineral poor value, process and pollute feature thoroughly, be strong supplementing to pyrometallurgy.But acid medium, alkaline medium or other media used in hydrometallurgy cannot circular regeneration, will form accessory substance cannot process, and mostly forms solid, liquid debris is discharged, and can work the mischief environment.
China's siderite resource is the abundantest, but average iron content 30% to 35%, and ore is adopted, selected, smelting is the most difficult, so utilization rate is the highest.Industry technology personnel's research emphasis is technique of preparing at present, specifically includes that the combined process flows such as the single flow process such as flotation, high intensity magnetic separation and calcining magnetic separation.But through practice have shown that for many years, it is high that prior art all also exists running cost, produces secondary pollution problems, most siderite is caused to be in idle state.
Summary of the invention
The invention provides a kind of high-purity iron oxide red wet fire one subtraction unit and high-purity iron oxide red preparation method, overcome the deficiency of above-mentioned prior art, it can effectively solve prior art and all there is running cost height, produces secondary pollution, causes the problem that siderite is in idle state.
One of technical scheme is realized by following measures: a kind of high-purity iron oxide red wet fire one subtraction unit, including ball mill by wet process, acidleach tank, single filter machine, removing calcium and magnesium tank, cascade filtration machine, preconcentrator, slurry absorption tower, hydrolysis calcining furnace and rotary calciner；nullThe discharge end of ball mill by wet process and the feed end of acidleach tank are fixed together by the first pipeline，The discharge end of acidleach tank and the liquid feeding end of single filter machine are fixed together by the second pipeline，The outlet end of single filter machine and the feed end of removing calcium and magnesium tank are fixed together by the 3rd pipeline，It is installed with cleaner pipe on the top of removing calcium and magnesium tank，The discharge end of removing calcium and magnesium tank and the liquid feeding end of cascade filtration machine are fixed together by the 4th pipeline，The outlet end of cascade filtration machine and the feed end of preconcentrator are fixed together by the 5th pipeline，The feed end of the discharge end of preconcentrator and hydrolysis calcining furnace is fixed together by the 6th pipeline，It is installed with conveying worm by support in the lower section of hydrolysis calcining furnace，The discharge end of hydrolysis calcining furnace is corresponding with the feed end of conveying worm，The discharge end of conveying worm and the feed end of rotary calciner are fixed together by the 7th pipeline；It is fixedly connected with the 8th pipeline between liquid feeding end and the second pipeline on slurry absorption tower, it is fixedly connected with the 9th pipeline between outlet end and the top of acidleach tank on slurry absorption tower, the outlet side of preconcentrator and the inlet end on slurry absorption tower are fixed together by the tenth pipeline, are installed with pump respectively on the second pipeline, the 4th pipeline and the 6th pipeline.
Further optimization and/or improvements to foregoing invention technical scheme one of are presented herein below:
The above-mentioned outside at preconcentrator has hydrochloric acid absorption tower and tail gas washing tower respectively；The outlet side on slurry absorption tower and the inlet end of hydrochloric acid absorption tower are fixed together by the 11st pipeline, the outlet side of hydrochloric acid absorption tower and the inlet end of tail gas washing tower are fixed together by the 12nd pipeline, are installed with blower fan on the 12nd pipeline；It is fixedly connected with the 13rd pipeline between the top of acidleach tank and the 11st pipeline；The outlet side of tail gas washing tower is fixedly connected with escape pipe, the liquid feeding end of tail gas washing tower is fixedly connected with water inlet pipe, the outlet end of tail gas washing tower and the liquid feeding end of hydrochloric acid absorption tower are fixed together by the 14th pipeline, it is fixedly connected with the 15th pipeline between the outlet end and the 9th pipeline of hydrochloric acid absorption tower, 14th pipeline and the 15th pipeline are installed with pump respectively, the second pipeline and the 8th pipeline are installed with valve respectively.
The above-mentioned outside at hydrolysis calcining furnace has gas generator and cyclone separator respectively；The inlet end of gas generator outlet side and hydrolysis calcining furnace is fixed together by the 16th pipeline, the outlet side of hydrolysis calcining furnace and the feed end of cyclone separator are fixed together by the 17th pipeline, the outlet side of cyclone separator and the inlet end of preconcentrator are fixed together by the 18th pipeline, being fixedly connected with tremie pipe on the discharge end of cyclone separator, the discharge end of tremie pipe is positioned at the top of conveying worm corresponding；Between the inlet end and the 16th pipeline of rotary calciner, it is fixedly connected with the 19th pipeline, between the bottom of the outlet side of rotary calciner and hydrolysis calcining furnace, is fixedly connected with the 20th pipeline；16th pipeline and the 19th pipeline are installed with valve respectively.
Above-mentioned on the discharge end of rotary calciner, it is fixedly connected with discharge nozzle, discharge nozzle is installed with valve.
Above-mentioned on acidleach tank, it is installed with agitator；Removing calcium and magnesium tank is installed with agitator.
The two of technical scheme are realized by following measures: a kind of high-purity iron oxide red preparation method, carry out in the steps below: the first step, siderite is added ball mill by wet process carries out ball milling, entered in the pickle liquor in acidleach tank by the first pipeline after ball milling and carry out acidleach, pickle liquor is aqueous hydrochloric acid solution, the temperature of pickle liquor is 85 DEG C to 95 DEG C, and the pH value of pickle liquor is 4 to 5, obtains a slurry after acidleach；Second step, one time slurry enters in single filter machine and slurry absorption tower by the second pipeline and the 8th pipeline respectively, return in acidleach tank by the 9th pipeline after a slurry in slurry absorption tower and smoke reaction, one-level filtrate is obtained after entering a slurries filtration in single filter machine, one-level filtrate carries out reaction by the 3rd pipeline in removing calcium and magnesium tank with the ammonium fluoride aqueous solution in cleaner pipe and obtains secondary slurry, the reaction temperature of one-level filtrate and ammonium fluoride aqueous solution is 78 DEG C to 82 DEG C, during in ammonium fluoride aqueous solution, the amount of the material of ammonium fluoride is one-level filtrate 1.2 times of the amount of the total material of calcium ions and magnesium ions to 1.3 times；3rd step, secondary slurry is entered in cascade filtration machine by the 4th pipeline and filters, obtaining two grades of filtrates after filtration, two grades of filtrates are entered in preconcentrator by the 5th pipeline and carry out being concentrated to give concentrate, and the volume of concentrate is the 70% to 85% of two grades of filtrate volumes；4th step, concentrate enters, by the 6th pipeline, the reaction that is hydrolyzed in hydrolysis calcining furnace, solid phase after hydrolysis is entered in rotary calciner by conveying worm and the 7th pipeline and calcines, obtain after calcining weight/mass percentage composition be 99.4% to 99.9% high-purity iron oxide red.
Be presented herein below to foregoing invention technical scheme two further optimization and/or improvements:
nullThe coal gas that above-mentioned gas generator produces is entered in hydrolysis calcining furnace and rotary calciner by the 16th pipeline and the 19th pipeline respectively and burns，Flue gas in rotary calciner is entered in hydrolysis calcining furnace by the 20th pipeline，Flue gas in hydrolysis calcining furnace is entered in cyclone separator by the 17th pipeline and separates，Solid phase after separation is entered in conveying worm by tremie pipe，Flue gas after separation is entered in preconcentrator by the 18th pipeline and reacts with two grades of filtrates，In preconcentrator, reacted flue gas is entered in slurry absorption tower by the tenth pipeline and reacts with a slurry，In slurry absorption tower, reacted flue gas is entered in hydrochloric acid absorption tower by the 11st pipeline and reacts with the liquid phase in hydrochloric acid absorption tower，In hydrochloric acid absorption tower, reacted flue gas is discharged from escape pipe after being entered by the 12nd pipeline and reacting with the water in water inlet pipe in tail gas washing tower，In the reacted flue gas of tail gas washing tower, HCl concentration is less than 5PPm，In tail gas washing tower, reacted liquid phase is entered in hydrochloric acid absorption tower by the 14th pipeline，In hydrochloric acid absorption tower, reacted liquid phase is entered in acidleach tank by the 15th pipeline，Gas in acidleach tank is entered in hydrochloric acid absorption tower by the 13rd pipeline.
The mass percent concentration of above-mentioned ammonium fluoride aqueous solution is 20% to 40%；Or/and, in the first step, the particle diameter after siderite ball milling is that 60 mesh are to 100 mesh.
The calcining heat of above-mentioned rotary calciner 800 DEG C to 900 DEG C；Or/and, the bottom temp 600 DEG C to 700 DEG C of hydrolysis calcining furnace, the top of hydrolysis calcining furnace is 350 DEG C to 450 DEG C, and going out to hydrolyze the weight/mass percentage composition of iron oxide in the solid phase of calcining furnace is 94.5% to 96.5%.
In above-mentioned siderite, the weight/mass percentage composition of iron is 30% to 45%, and the weight/mass percentage composition of magnesia is less than 1%, and the weight/mass percentage composition of calcium oxide is less than 2%, and the weight/mass percentage composition of aluminum oxide is less than 1%.
It is high-purity iron oxide red that the present invention utilizes pyro metallurgical plant rotary calciner to produce, and the chloride high-temperature flue gas of generation both provided heat for hydrolysis calcining kiln, achieved again wet dedusting, the HCl being stripped of in flue gas and dust；Utilizing the acidleach technology of hydrometallurgy, complete the removing of impurity in siderite, the hydrochloric acid in the present invention can recycle, do not introduce other media, produce without byproduct, there is no secondary pollution, thus reduce production cost, it is achieved that the comprehensive utilization of low-grade siderite.
Accompanying drawing explanation
Accompanying drawing 1 is the process flow diagram of the present invention.
nullCoding in accompanying drawing is respectively as follows: 1 for ball mill by wet process，2 is acidleach tank，3 is single filter machine，4 is removing calcium and magnesium tank，5 is cascade filtration machine，6 is preconcentrator，7 is slurry absorption tower，8 is hydrolysis calcining furnace，9 is rotary calciner，10 is the first pipeline，11 is the second pipeline，12 is the 3rd pipeline，13 is cleaner pipe，14 is the 4th pipeline，15 is the 5th pipeline，16 is the 6th pipeline，17 is conveying worm，18 is the 7th pipeline，19 is the 8th pipeline，20 is the 9th pipeline，21 is the tenth pipeline，22 is pump，23 is hydrochloric acid absorption tower，24 is tail gas washing tower，25 is the 11st pipeline，26 is the 12nd pipeline，27 is blower fan，28 is the 13rd pipeline，29 is escape pipe，30 is water inlet pipe，31 is the 14th pipeline，32 is the 15th pipeline，33 is gas generator，34 is cyclone separator，35 is the 16th pipeline，36 is the 17th pipeline，37 is the 18th pipeline，38 is tremie pipe，39 is the 19th pipeline，40 is the 20th pipeline，41 is discharge nozzle，42 is agitator.
Detailed description of the invention
The present invention is not limited by following embodiment, can determine specific embodiment according to technical scheme and actual conditions.
In the present invention, for the ease of describing, the description of the relative position relation of each parts is all that the Butut mode according to Figure of description 1 is described, such as: the position relationship of forward and backward, upper and lower, left and right etc. is based on the Butut direction of Figure of description 1 and determines.
Below in conjunction with embodiment and accompanying drawing, the invention will be further described:
Embodiment 1, as shown in Figure 1, this high-purity iron oxide red wet fire one subtraction unit includes ball mill by wet process 1, acidleach tank 2, single filter machine 3, removing calcium and magnesium tank 4, cascade filtration machine 5, preconcentrator 6, slurry absorption tower 7, hydrolysis calcining furnace 8 and rotary calciner 9；nullThe discharge end of ball mill by wet process 1 and the feed end of acidleach tank 2 are fixed together by the first pipeline 10，The discharge end of acidleach tank 2 and the liquid feeding end of single filter machine 3 are fixed together by the second pipeline 11，The outlet end of single filter machine 3 and the feed end of removing calcium and magnesium tank 4 are fixed together by the 3rd pipeline 12，It is installed with cleaner pipe 13 on the top of removing calcium and magnesium tank 4，The discharge end of removing calcium and magnesium tank 4 and the liquid feeding end of cascade filtration machine 5 are fixed together by the 4th pipeline 14，The outlet end of cascade filtration machine 5 and the feed end of preconcentrator 6 are fixed together by the 5th pipeline 15，The feed end of the discharge end of preconcentrator 6 and hydrolysis calcining furnace 8 is fixed together by the 6th pipeline 16，It is installed with conveying worm 17 by support in the lower section of hydrolysis calcining furnace 8，The discharge end of hydrolysis calcining furnace 8 is corresponding with the feed end of conveying worm 17，The discharge end of conveying worm 17 and the feed end of rotary calciner 9 are fixed together by the 7th pipeline 18；It is fixedly connected with the 8th pipeline 19 between liquid feeding end and the second pipeline 11 on slurry absorption tower 7, it is fixedly connected with the 9th pipeline 20 between outlet end and the top of acidleach tank 2 on slurry absorption tower 7, the outlet side of preconcentrator 6 and the inlet end on slurry absorption tower 7 are fixed together by the tenth pipeline 21, are installed with pump 22 respectively on the second pipeline the 11, the 4th pipeline 14 and the 6th pipeline 16.Ball mill by wet process 1, acidleach tank 2, single filter machine 3, removing calcium and magnesium tank 4, cascade filtration machine 5, preconcentrator 6, slurry absorption tower 7, hydrolysis calcining furnace 8 and rotary calciner 9 are existing public equipment.
According to actual needs above-described embodiment 1 can be made further optimization and/or improvements:
As shown in Figure 1, there are hydrochloric acid absorption tower 23 and tail gas washing tower 24 respectively in the outside of preconcentrator 6；The outlet side on slurry absorption tower 7 and the inlet end of hydrochloric acid absorption tower 23 are fixed together by the 11st pipeline 25, the outlet side of hydrochloric acid absorption tower 23 and the inlet end of tail gas washing tower 24 are fixed together by the 12nd pipeline 26, are installed with blower fan 27 on the 12nd pipeline 26；It is fixedly connected with the 13rd pipeline 28 between the top of acidleach tank 2 and the 11st pipeline 25；The outlet side of tail gas washing tower 24 is fixedly connected with escape pipe 29, the liquid feeding end of tail gas washing tower 24 is fixedly connected with water inlet pipe 30, the outlet end of tail gas washing tower 24 and the liquid feeding end of hydrochloric acid absorption tower 23 are fixed together by the 14th pipeline 31, it is fixedly connected with the 15th pipeline 32 between the outlet end and the 9th pipeline 20 of hydrochloric acid absorption tower 23,14th pipeline the 31 and the 15th pipeline 32 is installed with pump 22 respectively, the second pipeline 11 and the 8th pipeline 19 are installed with valve respectively.Blower fan 27 ensure that the high-purity iron oxide red wet fire one subtraction unit of the present invention is in micro-vacuum state.
As shown in Figure 1, the outside at hydrolysis calcining furnace 8 has gas generator 33 and cyclone separator 34 respectively；The inlet end of gas generator 33 outlet side and hydrolysis calcining furnace 8 is fixed together by the 16th pipeline 35, the outlet side of hydrolysis calcining furnace 8 and the feed end of cyclone separator 34 are fixed together by the 17th pipeline 36, the outlet side of cyclone separator 34 and the inlet end of preconcentrator 6 are fixed together by the 18th pipeline 37, being fixedly connected with tremie pipe 38 on the discharge end of cyclone separator 34, the discharge end of tremie pipe 38 is positioned at the top of conveying worm 17 corresponding；Between the inlet end and the 16th pipeline 35 of rotary calciner 9, it is fixedly connected with the 19th pipeline 39, between the bottom of the outlet side of rotary calciner 9 and hydrolysis calcining furnace 8, is fixedly connected with the 20th pipeline 40；16th pipeline the 35 and the 19th pipeline 39 is installed with valve respectively.
As shown in Figure 1, the discharge end of rotary calciner 9 is fixedly connected with discharge nozzle 41, discharge nozzle 41 is installed with valve.
As shown in Figure 1, acidleach tank 2 is installed with agitator 42；Removing calcium and magnesium tank 4 is installed with agitator 42.
Embodiment 2, as shown in Figure 1, this high-purity iron oxide red preparation method, carry out in the steps below: the first step, siderite is added ball mill by wet process 1 carries out ball milling, entered by the first pipeline 10 after ball milling and the pickle liquor in acidleach tank 2 carries out acidleach, pickle liquor is aqueous hydrochloric acid solution, the temperature of pickle liquor is 85 DEG C to 95 DEG C, and the pH value of pickle liquor is 4 to 5, obtains a slurry after acidleach；Second step, one time slurry enters in single filter machine 3 and slurry absorption tower 7 by the second pipeline 11 and the 8th pipeline 19 respectively, return in acidleach tank 2 by the 9th pipeline 20 after a slurry in slurry absorption tower 7 and smoke reaction, one-level filtrate is obtained after entering a slurries filtration in single filter machine 3, one-level filtrate carries out reaction by the 3rd pipeline 12 in removing calcium and magnesium tank 4 with the ammonium fluoride aqueous solution in cleaner pipe 13 and obtains secondary slurry, the reaction temperature of one-level filtrate and ammonium fluoride aqueous solution is 78 DEG C to 82 DEG C, during in ammonium fluoride aqueous solution, the amount of the material of ammonium fluoride is one-level filtrate 1.2 times of the amount of the total material of calcium ions and magnesium ions to 1.3 times；3rd step, secondary slurry is entered in cascade filtration machine 5 by the 4th pipeline 14 and filters, obtaining two grades of filtrates after filtration, two grades of filtrates are entered by the 5th pipeline 15 and carry out being concentrated to give concentrate in preconcentrator 6, and the volume of concentrate is the 70% to 85% of two grades of filtrate volumes；4th step, concentrate enters, by the 6th pipeline 16, the reaction that is hydrolyzed in hydrolysis calcining furnace 8, solid phase after hydrolysis is entered in rotary calciner 9 calcined by conveying worm 17 and the 7th pipeline 18, obtain after calcining weight/mass percentage composition be 99.4% to 99.9% high-purity iron oxide red.Control the pH value of acidleach, it is ensured that the Al of a slurry is qualified.In secondary slurry, the average content of Ca ion is 5PPm, and the average content of magnesium ion is 9PPM.During in acidleach tank 2, the amount of the material of hydrochloric acid is siderite the 75% to 85% of the amount of the total material of iron, magnesium, calcium and aluminium, in acidleach tank 2, the reaction time is 1.0h to 2.0h.
According to actual needs above-described embodiment 2 can be made further optimization and/or improvements:
nullAs shown in Figure 1，The coal gas that gas generator 33 produces is entered in hydrolysis calcining furnace 8 and rotary calciner 9 by the 16th pipeline the 35 and the 19th pipeline 39 respectively and burns，Flue gas in rotary calciner 9 is entered in hydrolysis calcining furnace 8 by the 20th pipeline 40，Flue gas in hydrolysis calcining furnace 8 is entered in cyclone separator 34 by the 17th pipeline 36 and separates，Solid phase after separation is entered in conveying worm 17 by tremie pipe 38，Flue gas after separation is entered in preconcentrator 6 by the 18th pipeline 37 and reacts with two grades of filtrates，In preconcentrator 6, reacted flue gas is entered in slurry absorption tower 7 by the tenth pipeline 21 and reacts with a slurry，In slurry absorption tower 7, reacted flue gas is entered in hydrochloric acid absorption tower 23 by the 11st pipeline 25 and reacts with the liquid phase in hydrochloric acid absorption tower 23，In hydrochloric acid absorption tower 23, reacted flue gas is discharged from escape pipe 29 after being entered by the 12nd pipeline 26 and reacting with the water in water inlet pipe 30 in tail gas washing tower 24，In the reacted flue gas of tail gas washing tower 24, HCl concentration is less than 5PPm，In tail gas washing tower 24, reacted liquid phase is entered in hydrochloric acid absorption tower 23 by the 14th pipeline 31，In hydrochloric acid absorption tower 23, reacted liquid phase is entered in acidleach tank 2 by the 15th pipeline 32，Gas in acidleach tank 2 is entered in hydrochloric acid absorption tower 23 by the 13rd pipeline 28.The mean temperature of flue gas discharged by hydrolysis calcining furnace 8 is 400 DEG C, and its flue gas content (volume fraction %) is, HCl:8.15%, H2O:42.18%, N2: 39.52%, CO2: 7.49%；After the smoke contacts discharged in two grades of filtrates and cyclone separator 34, the volume of concentrate is the 70% to 85% of two grades of filtrate volumes, go out 1.28 times that average flue gas concentration is the flue gas concentration discharged in cyclone separator 34 of preconcentrator 6, the flue gas average content (mass fraction %) going out preconcentrator 6 is, HCl:5.77%, H2O:53.26%, N2: 32%；Gas generator 33 is existing known two sections of gas generators, by coal gas desulfurization, the average clean gas producing 30 DEG C.The inflow of water inlet pipe 30 is the 50% to 80% of hydrochloric acid absorption tower 23 liquid outlet quantity quality, and the average salt acid concentration of the liquid phase entering hydrochloric acid absorption tower 23 by the 14th pipeline 31 is 0.1% to 0.5%, and the average salt acid concentration of the liquid phase going out hydrochloric acid absorption tower 23 is 5% to 6%.
As required, the mass percent concentration of ammonium fluoride aqueous solution is 20% to 40%；Or/and, in the first step, the particle diameter after siderite ball milling is that 60 mesh are to 100 mesh.
As required, the calcining heat of rotary calciner 9 800 DEG C to 900 DEG C；Or/and, the bottom temp 600 DEG C to 700 DEG C of hydrolysis calcining furnace 8, the top of hydrolysis calcining furnace 8 is 350 DEG C to 450 DEG C, and going out to hydrolyze the weight/mass percentage composition of iron oxide in the solid phase of calcining furnace 8 is 94.5% to 96.5%.
As required, in siderite, the weight/mass percentage composition of iron is 30% to 45%, and the weight/mass percentage composition of magnesia is less than 1%, and the weight/mass percentage composition of calcium oxide is less than 2%, and the weight/mass percentage composition of aluminum oxide is less than 1%.The loss on ignition average out to 30% of siderite.
In the present invention, the average leaching rate of a slurry is as shown in table 1；Average solid phase composition after hydrolysis is as shown in table 2；The most high-purity iron oxide red composition obtained after calcining is as shown in table 3；Baosteel one-level Ferric Oxide Used for Soft Ferrite index is as shown in table 4；What the present invention obtained as can be seen from Table 3 high-purity iron oxide red can reach soft magnetic bodies iron oxide product index.
Acidleach and hydrolysis that the present invention is carried out in acidleach tank 2 and hydrolysis calcining furnace 8 are as follows:
The present invention utilizes the inherent advantage of the low-grade mineral of hydrometallurgical process, it is possible to obtain high-grade intermediate product, as the high-quality raw material of pyrometallurgy, by the technique that pyrometallurgy is ripe, is finally obtained in that the product of high-quality；And the unserviceable high-temperature flue gas that pyrogenic process produces, can be as wet method thermal source while, rely on wet method to carry out the regeneration cycle of acid and the process of dedusting etc., form a series of efficient utilization to low-grade mineral, soil boy structure is friendly, the new technology that energy efficient utilizes.The present invention chemical mineral processing by low-grade mineral, the regeneration cycle of acid medium and the cascade utilization of heat；By wet fire one method, utilize hydrochloric acid that siderite is carried out acidleach, then the silicon in removing siderite, aluminium, calcium, magnesium, obtain pure frerrous chloride and ferric chloride solution, then pyrohydrolysis is carried out, while obtaining chloride iron oxide, siderite slurry is utilized to absorb the HCl in flue gas, it is achieved that high temperature acidleach and the circular regeneration of hydrochloric acid；And chloride iron oxide enters and carries out high-temperature calcination in rotary calciner 9, it is thus achieved that while high purity ferric oxide product, chloride high-temperature dust-containing flue gas enters pyrohydrolysis system, as the thermal source of pyrohydrolysis.And the high-temperature flue gas chloride, dust-laden in rotary calciner 9 carries out dedusting by cyclone separator 34, slurry absorption tower 7, hydrochloric acid absorption tower 23 and tail gas washing tower 24, it is achieved dust and the qualified discharge of HCl；Hydrochloric acid in the present invention can recycle, and does not introduce other media, produces without byproduct, does not has secondary pollution, thus reduce production cost, it is achieved that the comprehensive utilization of low-grade siderite.
The high-purity iron oxide red wet fire one subtraction unit of the present invention is equally applicable to low-grade magnesite and lateritic nickel ore etc..
Above technical characteristic constitutes embodiments of the invention, and it has stronger adaptability and implementation result, can increase and decrease non-essential technical characteristic according to actual needs, meet the demand of different situations.
Table 1
| Element | Fe | Al | Ca | Mg | Si |
| Leaching rate/% | 75 to 85 | 3 to 5 | 20 to 25 | 25 to 35 | 0 to 0.05 |
Table 2
| Material | Fe2O3 | Al2O3 | CaO | MgO | Cl |
| Content (%) | 94.5 to 96.5 | 0 to 0.007 | 0 to 0.015 | 0 to 0.009 | 1.0 to 5.0 |
Table 3
| Material | Fe2O3 | Al2O3 | CaO | MgO | Cl |
| Content (%) | 99.4 to 99.9 | 0 to 0.009 | 0 to 0.018 | 0 to 0.009 | 0 to 0.13 |
Table 4
| Material | Fe2O3 | Al2O3 | CaO | MgO | SiO2 | Cl |
| Content (%) | >99.30 | <0.01 | <0.02 | <0.01 | <0.012 | <0.15 |
Claims (17)
1. a high-purity iron oxide red wet fire one subtraction unit, it is characterised in that include ball mill by wet process, acidleach tank, single filter machine, removing calcium and magnesium tank, cascade filtration machine, preconcentrator, slurry absorption tower, hydrolysis calcining furnace and rotary calciner；nullThe discharge end of ball mill by wet process and the feed end of acidleach tank are fixed together by the first pipeline，The discharge end of acidleach tank and the liquid feeding end of single filter machine are fixed together by the second pipeline，The outlet end of single filter machine and the feed end of removing calcium and magnesium tank are fixed together by the 3rd pipeline，It is installed with cleaner pipe on the top of removing calcium and magnesium tank，The discharge end of removing calcium and magnesium tank and the liquid feeding end of cascade filtration machine are fixed together by the 4th pipeline，The outlet end of cascade filtration machine and the feed end of preconcentrator are fixed together by the 5th pipeline，The feed end of the discharge end of preconcentrator and hydrolysis calcining furnace is fixed together by the 6th pipeline，It is installed with conveying worm by support in the lower section of hydrolysis calcining furnace，The discharge end of hydrolysis calcining furnace is corresponding with the feed end of conveying worm，The discharge end of conveying worm and the feed end of rotary calciner are fixed together by the 7th pipeline；It is fixedly connected with the 8th pipeline between liquid feeding end and the second pipeline on slurry absorption tower, it is fixedly connected with the 9th pipeline between outlet end and the top of acidleach tank on slurry absorption tower, the outlet side of preconcentrator and the inlet end on slurry absorption tower are fixed together by the tenth pipeline, are installed with pump respectively on the second pipeline, the 4th pipeline and the 6th pipeline.
High-purity iron oxide red wet fire one subtraction unit the most according to claim 1, it is characterised in that the outside of preconcentrator has hydrochloric acid absorption tower and tail gas washing tower respectively；The outlet side on slurry absorption tower and the inlet end of hydrochloric acid absorption tower are fixed together by the 11st pipeline, the outlet side of hydrochloric acid absorption tower and the inlet end of tail gas washing tower are fixed together by the 12nd pipeline, are installed with blower fan on the 12nd pipeline；It is fixedly connected with the 13rd pipeline between the top of acidleach tank and the 11st pipeline；The outlet side of tail gas washing tower is fixedly connected with escape pipe, the liquid feeding end of tail gas washing tower is fixedly connected with water inlet pipe, the outlet end of tail gas washing tower and the liquid feeding end of hydrochloric acid absorption tower are fixed together by the 14th pipeline, it is fixedly connected with the 15th pipeline between the outlet end and the 9th pipeline of hydrochloric acid absorption tower, 14th pipeline and the 15th pipeline are installed with pump respectively, the second pipeline and the 8th pipeline are installed with valve respectively.
High-purity iron oxide red wet fire one subtraction unit the most according to claim 1 and 2, it is characterised in that the outside of hydrolysis calcining furnace has gas generator and cyclone separator respectively；The inlet end of gas generator outlet side and hydrolysis calcining furnace is fixed together by the 16th pipeline, the outlet side of hydrolysis calcining furnace and the feed end of cyclone separator are fixed together by the 17th pipeline, the outlet side of cyclone separator and the inlet end of preconcentrator are fixed together by the 18th pipeline, being fixedly connected with tremie pipe on the discharge end of cyclone separator, the discharge end of tremie pipe is positioned at the top of conveying worm corresponding；Between the inlet end and the 16th pipeline of rotary calciner, it is fixedly connected with the 19th pipeline, between the bottom of the outlet side of rotary calciner and hydrolysis calcining furnace, is fixedly connected with the 20th pipeline；16th pipeline and the 19th pipeline are installed with valve respectively.
High-purity iron oxide red wet fire one subtraction unit the most according to claim 1 and 2, it is characterised in that be fixedly connected with discharge nozzle on the discharge end of rotary calciner, be installed with valve on discharge nozzle.
High-purity iron oxide red wet fire one subtraction unit the most according to claim 3, it is characterised in that be fixedly connected with discharge nozzle on the discharge end of rotary calciner, be installed with valve on discharge nozzle.
High-purity iron oxide red wet fire one subtraction unit the most according to claim 1 and 2, it is characterised in that be installed with agitator on acidleach tank；Removing calcium and magnesium tank is installed with agitator.
High-purity iron oxide red wet fire one subtraction unit the most according to claim 3, it is characterised in that be installed with agitator on acidleach tank；Removing calcium and magnesium tank is installed with agitator.
High-purity iron oxide red wet fire one subtraction unit the most according to claim 4, it is characterised in that be installed with agitator on acidleach tank；Removing calcium and magnesium tank is installed with agitator.
9. the high-purity iron oxide red preparation method of the high-purity iron oxide red wet fire one subtraction unit used described in claim 3, it is characterized in that carrying out in the steps below: the first step, siderite is added ball mill by wet process carries out ball milling, entered in the pickle liquor in acidleach tank by the first pipeline after ball milling and carry out acidleach, pickle liquor is aqueous hydrochloric acid solution, the temperature of pickle liquor is 85 DEG C to 95 DEG C, and the pH value of pickle liquor is 4 to 5, obtains a slurry after acidleach；Second step, one time slurry enters in single filter machine and slurry absorption tower by the second pipeline and the 8th pipeline respectively, return in acidleach tank by the 9th pipeline after a slurry in slurry absorption tower and smoke reaction, one-level filtrate is obtained after entering a slurries filtration in single filter machine, one-level filtrate carries out reaction by the 3rd pipeline in removing calcium and magnesium tank with the ammonium fluoride aqueous solution in cleaner pipe and obtains secondary slurry, the reaction temperature of one-level filtrate and ammonium fluoride aqueous solution is 78 DEG C to 82 DEG C, during in ammonium fluoride aqueous solution, the amount of the material of ammonium fluoride is one-level filtrate 1.2 times of the amount of the total material of calcium ions and magnesium ions to 1.3 times；3rd step, secondary slurry is entered in cascade filtration machine by the 4th pipeline and filters, obtaining two grades of filtrates after filtration, two grades of filtrates are entered in preconcentrator by the 5th pipeline and carry out being concentrated to give concentrate, and the volume of concentrate is the 70% to 85% of two grades of filtrate volumes；4th step, concentrate enters, by the 6th pipeline, the reaction that is hydrolyzed in hydrolysis calcining furnace, solid phase after hydrolysis is entered in rotary calciner by conveying worm and the 7th pipeline and calcines, obtain after calcining weight/mass percentage composition be 99.4% to 99.9% high-purity iron oxide red.
nullHigh-purity iron oxide red preparation method the most according to claim 9，It is characterized in that the coal gas that gas generator produces is entered in hydrolysis calcining furnace and rotary calciner by the 16th pipeline and the 19th pipeline respectively to burn，Flue gas in rotary calciner is entered in hydrolysis calcining furnace by the 20th pipeline，Flue gas in hydrolysis calcining furnace is entered in cyclone separator by the 17th pipeline and separates，Solid phase after separation is entered in conveying worm by tremie pipe，Flue gas after separation is entered in preconcentrator by the 18th pipeline and reacts with two grades of filtrates，In preconcentrator, reacted flue gas is entered in slurry absorption tower by the tenth pipeline and reacts with a slurry，In slurry absorption tower, reacted flue gas is entered in hydrochloric acid absorption tower by the 11st pipeline and reacts with the liquid phase in hydrochloric acid absorption tower，In hydrochloric acid absorption tower, reacted flue gas is discharged from escape pipe after being entered by the 12nd pipeline and reacting with the water in water inlet pipe in tail gas washing tower，In the reacted flue gas of tail gas washing tower, HCl concentration is less than 5ppm，In tail gas washing tower, reacted liquid phase is entered in hydrochloric acid absorption tower by the 14th pipeline，In hydrochloric acid absorption tower, reacted liquid phase is entered in acidleach tank by the 15th pipeline，Gas in acidleach tank is entered in hydrochloric acid absorption tower by the 13rd pipeline.
11. according to the high-purity iron oxide red preparation method described in claim 9 or 10, it is characterised in that the mass percent concentration of ammonium fluoride aqueous solution is 20% to 40%；Or/and, in the first step, the particle diameter after siderite ball milling is that 60 mesh are to 100 mesh.
12. according to the high-purity iron oxide red preparation method described in claim 9 or 10, it is characterised in that the calcining heat of rotary calciner 800 DEG C to 900 DEG C；Or/and, the bottom temp 600 DEG C to 700 DEG C of hydrolysis calcining furnace, the top of hydrolysis calcining furnace is 350 DEG C to 450 DEG C, and going out to hydrolyze the weight/mass percentage composition of iron oxide in the solid phase of calcining furnace is 94.5% to 96.5%.
13. high-purity iron oxide red preparation methods according to claim 11, it is characterised in that the calcining heat of rotary calciner 800 DEG C to 900 DEG C；Or/and, the bottom temp 600 DEG C to 700 DEG C of hydrolysis calcining furnace, the top of hydrolysis calcining furnace is 350 DEG C to 450 DEG C, and going out to hydrolyze the weight/mass percentage composition of iron oxide in the solid phase of calcining furnace is 94.5% to 96.5%.
14. according to the high-purity iron oxide red preparation method described in claim 9 or 10, it is characterized in that in siderite, the weight/mass percentage composition of iron is 30% to 45%, the weight/mass percentage composition of magnesia is less than 1%, and the weight/mass percentage composition of calcium oxide is less than 2%, and the weight/mass percentage composition of aluminum oxide is less than 1%.
15. high-purity iron oxide red preparation methods according to claim 11, it is characterized in that in siderite, the weight/mass percentage composition of iron is 30% to 45%, the weight/mass percentage composition of magnesia is less than 1%, and the weight/mass percentage composition of calcium oxide is less than 2%, and the weight/mass percentage composition of aluminum oxide is less than 1%.
16. high-purity iron oxide red preparation methods according to claim 12, it is characterized in that in siderite, the weight/mass percentage composition of iron is 30% to 45%, the weight/mass percentage composition of magnesia is less than 1%, and the weight/mass percentage composition of calcium oxide is less than 2%, and the weight/mass percentage composition of aluminum oxide is less than 1%.
17. high-purity iron oxide red preparation method according to claim 13, it is characterized in that in siderite, the weight/mass percentage composition of iron is 30% to 45%, the weight/mass percentage composition of magnesia is less than 1%, and the weight/mass percentage composition of calcium oxide is less than 2%, and the weight/mass percentage composition of aluminum oxide is less than 1%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410319562.2A CN104109756B (en) | 2014-07-07 | 2014-07-07 | High-purity iron oxide red wet fire one subtraction unit and high-purity iron oxide red preparation method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410319562.2A CN104109756B (en) | 2014-07-07 | 2014-07-07 | High-purity iron oxide red wet fire one subtraction unit and high-purity iron oxide red preparation method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104109756A CN104109756A (en) | 2014-10-22 |
| CN104109756B true CN104109756B (en) | 2016-08-24 |
Family
ID=51706742
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410319562.2A Active CN104109756B (en) | 2014-07-07 | 2014-07-07 | High-purity iron oxide red wet fire one subtraction unit and high-purity iron oxide red preparation method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104109756B (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1900831A1 (en) * | 2003-05-16 | 2008-03-19 | Jaguar Nickel Inc. | A process for the recovery of value metals from material containing base metal oxides |
| CN101338376A (en) * | 2008-08-15 | 2009-01-07 | 中南大学 | Method for Comprehensive Development and Utilization of Nickel-Cobalt, Iron and Magnesium in Laterite Nickel Ore |
| CN103451411A (en) * | 2013-09-09 | 2013-12-18 | 新疆蓝天镁业股份有限公司 | Technique and system for preparing fine iron powder from siderite |
-
2014
- 2014-07-07 CN CN201410319562.2A patent/CN104109756B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1900831A1 (en) * | 2003-05-16 | 2008-03-19 | Jaguar Nickel Inc. | A process for the recovery of value metals from material containing base metal oxides |
| CN101338376A (en) * | 2008-08-15 | 2009-01-07 | 中南大学 | Method for Comprehensive Development and Utilization of Nickel-Cobalt, Iron and Magnesium in Laterite Nickel Ore |
| CN103451411A (en) * | 2013-09-09 | 2013-12-18 | 新疆蓝天镁业股份有限公司 | Technique and system for preparing fine iron powder from siderite |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104109756A (en) | 2014-10-22 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103130279B (en) | A kind of method of chlorination production high purity vanadic anhydride | |
| CN107523702B (en) | A kind of method that the pressure oxidation of sodium salt system prepares sodium pyroantimonate | |
| CN104694760B (en) | It is a kind of to handle the method and system that red mud reclaims Iron concentrate | |
| CN102978381B (en) | Technology for producing tungsten trioxide by prilling and roasting of tungsten slag | |
| CN104480328B (en) | The method of germanium in the low-grade brown coal germanium concentrate of vacuum enriching and recovering | |
| CN104773751B (en) | A kind of method of fluorine, chlorine and valuable metal in removing secondary zinc oxide | |
| CN109160744A (en) | Red mud magnetizing roast utilization system and technique | |
| CN107619946A (en) | Comprehensive utilization method of blast furnace flue gas dedusting ash | |
| CN111286630B (en) | A kind of method for suspension roasting, impurity removal and purification of titanium concentrate | |
| CN102020299A (en) | Method for producing industrial activated aluminum oxide from pulverized fuel ash | |
| CN110172595A (en) | A kind of device and method that vanadium slag suspended state oxidizing roasting-is acid-leaching vanadium-extracted | |
| CN109402380B (en) | Method for extracting vanadium from vanadium slag | |
| CN102503190B (en) | Method and device for preparing high-purity high-density magnesia by utilizing magnesite | |
| CN101475219B (en) | A kind of powdery manganese dioxide ore fluidized reduction method | |
| CN115637340B (en) | Mixed rare earth concentrate suspension state ore phase conversion-clean leaching system and use method thereof | |
| CN114934196B (en) | A method for extracting lithium from low-aluminum and lithium-rich clay | |
| CN105692684A (en) | High-purity zinc oxide production technology | |
| CN105755298B (en) | The method that tungsten copper bismuth iron is extracted from tungstenic limonite | |
| CN103539182A (en) | Method for preparing aluminum chloride hexahydrate by using pulverized fuel ash as raw material through ferrous chloride induced crystallization | |
| CN103451411B (en) | Technique and system for preparing fine iron powder from siderite | |
| CN104109756B (en) | High-purity iron oxide red wet fire one subtraction unit and high-purity iron oxide red preparation method | |
| CN104108733B (en) | Highly-purity magnesite wets fire one subtraction unit and prepare the method for highly-purity magnesite | |
| CN103215446A (en) | Serpentine type laterite nickel ore hydrochloric acid normal pressure leaching cleaning production method | |
| CN103194767A (en) | Method for preparing manganese sulfate electrolyte by using high-iron and high-phosphor manganese ores | |
| CN107541607A (en) | A method for two-stage roasting-conversion treatment-cyanidation gold leaching of high-arsenic gold ore |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20181224 Address after: 835000 No. 16 Workshop of Block A4, First Opening Area, Border Cooperation Center of Holguos Port, Yili Kazakh Autonomous Prefecture, Xinjiang Uygur Autonomous Region Patentee after: Xinjiang Zhaofeng Biotechnology Co., Ltd. Address before: Room 303, Venture Building, 682 Tianjin South Road High-tech Venture Service Center, Urumqi High-tech Industrial Development Zone, Xinjiang Uygur Autonomous Region, 830011 Patentee before: XINJIANG DAZHENG ENVIRONMENTAL PROTECTION TECHNOLOGY CO., LTD. |
|
| TR01 | Transfer of patent right |