CN101665263B - Method for processing zinc oxide ore or zinc oxide secondary resource to prepare superfine active zinc oxide - Google Patents
Method for processing zinc oxide ore or zinc oxide secondary resource to prepare superfine active zinc oxide Download PDFInfo
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- CN101665263B CN101665263B CN 200910186123 CN200910186123A CN101665263B CN 101665263 B CN101665263 B CN 101665263B CN 200910186123 CN200910186123 CN 200910186123 CN 200910186123 A CN200910186123 A CN 200910186123A CN 101665263 B CN101665263 B CN 101665263B
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- zinc oxide
- leaching
- zinc
- filtrate
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Abstract
The invention relates to a method for processing zinc oxide ore or zinc oxide secondary resource to prepare superfine active zinc oxide. The method comprises the following steps: ammonium leaching: using zinc oxide ore containing 2-60% of zinc or complex zinc oxide secondary resource as raw material, extracting in an ammonium system coordinately, filtering to remove the residue, wherein the filtrate is applied to the next process; replacement and purification: replacing and purifying the extracted filtrate with zinc powder to eliminate impure elements, and then filtering and removing the residue, wherein the filtrate is applied to the next process; pulverization and drying: decomposing the purified filtrate through high-temperature pulverization to prepare powder A, condensing, spraying and absorbing the tail gas which is then returned to the leaching process to prepare the extracting agent; and toasting: toasting the powder A to obtain superfine active zinc oxide. The purified liquid can be used for directly preparing even powder through efficient pulverization and drying. The technological process of the method has a circular loop so that a small amount of waste gas and waste water is discharged. The method has a rational tail gas heat exchanger. Ammonia gas is recycled in a condensing manner to prepare the leaching liquid. The rest of the ammonia gas is absorbed through spraying, thereby reducing the discharge pressure of three wastes, namely, waste gas, waste water and industrial residue.
Description
Affiliated technical field
The present invention relates to a kind of preparation method of zinc oxide, especially process the method for zinc oxide ore or zinc oxide secondary resource to prepare superfine active zinc oxide.
Background technology
Active zinc flower is a kind of broad-spectrum industrial chemicals, and existing preparation method mainly contains direct precipitation method, homogeneous precipitation method, sol-gel method, microemulsion method, hydrothermal method, alkoxide hydrolysis, solvent evaporation method etc.Simultaneously there is extremely abundant zinc oxide ore resource in China, but it is few to contain the ratio that accounts for than the higher-grade zinc oxide ore of Zn 〉=20%.Can't effectively process with traditional metallurgy and beneficiation method at present for low-grade zinc oxide ore.
Summary of the invention
For overcoming above-mentioned deficiency, the invention provides a kind of method of processing zinc oxide ore or zinc oxide secondary resource to prepare superfine active zinc oxide.
The technical solution adopted for the present invention to solve the technical problems is: the technological process of described method is sequentially:
The ammonia leaching: take the zinc oxide ore that contains zinc 2-60% or complicated zinc oxide secondary resource as raw material, in ammonia gonosome system, cooperate leaching, filter cleaner, filtrate enters subsequent processing;
Displacement purge: with zinc powder the filtrate of leaching is carried out displacement purge and remove impurity element, refilter slagging-off, filtrate enters subsequent processing;
Atomization drying: the filtrate of purification is carried out the high-temperature spray decomposition and is produced powders A, and tail gas returns leaching process configuration leaching agent through condensation, spray-absorption;
Roasting: powders A becomes superfine active zinc oxide through roasting.
The technology condition of each operation is as follows:
Ammonia leaching operation: the leach liquor composition is [NH
4 +]=0.5-5 (mol/L), [NH
3]=0.5-10 (mol/L); Liquid-solid mass ratio is 2-10: 1; Extraction temperature is 10-50 ℃; Extraction time is 0.3-4h;
The displacement purge operation: the zinc powder consumption is 1.5-30 times of theoretical consumption; Purification temperature 10-50 ℃; Time 0.5-5h;
Atomization drying operation: inlet temperature=100-800 ℃, temperature out is 80-700 ℃; Input speed=10-100mL/min; Charging zinc concentration=5-200g/L;
Calcining process: maturing temperature=200-800 ℃; Roasting time=5-180min.
In ammonia leaching operation, low-grade zinc oxide ore or the zinc oxide secondary resource that contains zinc 2-5% adopted dump leaching or circulating leaching method.
The atomization drying operation is finished in Efficent sprayer, and atomizer is rotational pressure formula spraying gun, centrifugal pressure formula spraying gun, combination pressure formula spraying gun, pneumatic atomizer, centrifugal spray-dryer.
Calcining process is finished in flash dryer, fluidizing furnace or retort furnace.
The invention has the beneficial effects as follows: spray atomization decompose and drying process as a kind of emerging ultrafine particle technology of preparing, have that rate of drying is fast, product purity is high, granularity and composition is even, process simple continuous, have much the advantage such as industrialization potentiality.After the feed liquid spraying, surface-area increases greatly, and in high temperature gas flow, moment just can be evaporated the moisture content of 95%-98%, finishes and only needs 5-20s time of drying.Because drying process finishes in moment, the particle of final product can keep approximate spherical of drop basically, and product has good dispersiveness, flowability and solvability.Production process is simplified, convenient operation and control.Spraying drying is generally used for the solution of solid content below 60%, after the drying, does not need precipitation, filtration, drying, pulverizes and screening, has reduced production process, has simplified production technique.For particle diameter, loose density, the moisture content of product, within the specific limits, can change operational condition adjustment, control, manage all very convenient.The method technical process is short, and operation is manually few.Scavenging solution is produced powder through the high-efficient atomizing drying, does not need the operations such as precipitation, filtration, drying, fragmentation, powder process.Under high-temperature spray, the powder of producing is zinc oxide, no longer needs to carry out roasting.The closed cycle of the method flow process, the waste gas discharge of wastewater is few.High-temperature tail gas rationally utilizes through over-heat-exchanger after the atomizing, and ammonia adopts condensation to reclaim and disposes leach liquor again, and remaining ammonia alleviates three waste discharge pressure through spray-absorption.
Description of drawings
The present invention is further described below in conjunction with drawings and Examples.
Fig. 1 is process flow sheet of the present invention.
Technological process of the present invention and reaction principle are as follows:
One, leaching process
First ammonium salt and/or ammoniacal liquor are made into the satisfactory leaching agent aqueous solution, will cooperate leaching in zinc oxide ore or the zinc oxide secondary resource adding leaching agent again.Zinc is with Zn (NH
3)
i 2+Or Zn (OH)
m 2-mCooperate the form of ion to enter in the leach liquor, Cu, Cd, Co, Ni are also with Me (NH
3)
j 2+(Me represents Cu, Cd, Co, Ni) ammonia cooperates the form of ion to enter in the leach liquor, and Fe, In, Mn, Cr, Sn and most of Pb, Sb and Bi are not leached, and stays in the residue, removes after filtration.When containing the lower zinc oxide ore of Zn or zinc oxide secondary resource as raw material, in order to improve the Zn in the leach liquor
2+Concentration will be carried out 1-5 time circulating leaching to more than the 50g/L, be about to previous leach liquor as after the leaching agent that once leaches, by that analogy, by increasing cycle index, improve Zn in the leach liquor
2+Concentration with relative minimizing evaporation of water amount in spray-drying process, reduces consuming, and improves production capacity.
Leaching reaction is as follows:
ZnO+2NH
4 ++(i-2)NH
3＝Zn(NH
3)
i 2++H
2O
Zn(OH)
2+2NH
4 ++(i-2)NH
3＝Zn(NH
3)
i 2++2H
2O
ZnCO
3+iNH
3＝Zn(NH
3)
i 2++CO
3 2-
ZnSO
4+iNH
3＝Zn(NH
3)
i 2++SO
4 2-
ZnO+H
2O+(i-2)OH
-＝Zn(OH)
i 2-i
Zn(OH)
2+(i-2)OH
-＝Zn(OH)
i 2-i
ZnCO
3+iOH
-＝Zn(OH)
i 2-i+CO
3 2-
ZnSO
4+iOH
-＝Zn(OH)
i 2-i+SO
4 2-
Two, scavenging process
The cooperation ion Me (NH that contains Cu, Cd, Co, Ni in the leach liquor
3)
j 2+, adding zinc dust precipitation and remove, its chemical equation is as follows:
Zn+Me(NH
3)
j 2+＝Zn(NH
3)
i 2++Me+(j-i)NH
3
The zinc powder add-on is 1.5-30 times of theoretical amount, and zinc powder particle size is generally 0.175-0.104mm.Adopt two sections adverse currents to purify, filter after first paragraph purifies, the scavenging solution of removing copper cadmium (lead) slag enters second segment and purifies with fresh zinc powder, and the filter residue that second segment purifies returns first paragraph and purifies, to utilize as much as possible and to save zinc powder.Purify the rear impurity constituent content and mostly be down to below the 1mg/L, after the filtration, liquid send spraying drying to decompose after will purifying.
Three, spray atomization decomposes and drying process
When the scavenging solution spray atomization decomposes with drying, in high temperature efficient spray moisture eliminator, finish.Mainly finish volatilization, the evaporation of water of ammonia, the dry decomposition course of powder, scavenging solution pumps in the spraying gun, be atomized into little droplet, each little droplet is as a reactor, ammonia is highly volatile at high temperature, along with the volatilization of ammonia, overbalance is stablized in the Zn cooperation in the droplet, thereby separates out zinc subcarbonate.Simultaneously, because the steam partial pressure of particle surface is much larger than airborne steam partial pressure, drying process is carried out fast, and partial pressure difference is the impellent of drying process.When the steam partial pressure of particle surface equals even less than airborne steam partial pressure, partial pressure difference between the two equals zero even is tending towards negative value, and at this moment, material no longer carries out drying, but decomposes rapidly, and obtains powders A.
Principal reaction is as follows:
3Zn(NH
3)
4CO
3+3H
2O＝ZnCO
3·2Zn(OH)
2·H
2O↓+12NH
3↑+2CO
2↑
ZnCO
3·2Zn(OH)
2·H
2O＝3ZnO+3H
2O↑+CO
2↑
Four, roasting process
Be subjected to temperature effect in the sedimentator, powders A is zinc oxide entirely not necessarily, wherein may also have zinc subcarbonate, need to carry out further Roasting Decomposition, and its reaction is as follows:
ZnCO3·2Zn(OH)2·H2O＝3ZnO+3H2O↑+CO2↑
Embodiment:
The embodiment of the inventive method is as follows:
Embodiment 1: zinc oxide ore composition (%): Zn 19.51, and Fe 13.51, and Pb 2.30, and Cu 0.022, and Cd 0.23, and S 2.10, As0.098, and Sb 0.20, SiO
213.78, Al
2O
30.46 CaO 9.31, MgO 0.33, and MnO 0.93.
Prepare first [NH
4Cl]=5mol/L, [NH
3The leaching agent 1L of]=5mol/L takes by weighing zinc oxide ore 250g, and liquid-solid volume mass under 25 ℃, leached 1h than 4: 1, used the solution washing leached mud identical with the leaching agent composition during filtration, and the leach liquor volume is identical with leaching agent to be as the criterion the washing lotion amount to keep.Zinc leaching rate 83.67% contains the Zn amount and is 40.81g/L.Leach liquor as leaching agent, is leached zinc oxide ore 250g, filtration washing under the same conditions again, incorporate washing lotion into, obtain for the second time leach liquor, leach liquor contains the Zn amount and is 81.25g/L, and leaching yield reaches 82.93%, leach liquor composition (g/L): Zn 81.25, Pb 0.8, and Cu 0.008, Cd4.3, As 0.036, and Sb 0.0073.Amount by 3ml/L and 3g/L adds respectively H
2O
2And FeCl
2, to remove antimony, 40 ℃ of purification temperatures, churning time 1h; Filter rear filtrate by 2 times of adding zinc powders of displacement Cu, Cd, the required zinc powder theoretical amount of Pb, churning time 1h, 40 ℃ of displacement temperature.Liquid reacts in atomizing drier after purifying, and reaction conditions is: inlet temperature is 250 ℃, and temperature out is 150 ℃, and input speed is 60mL/min, and the charging zinc concentration is 85g/L.After spray-dried, obtain the basic carbonate zinc powder, powder is roasting in retort furnace, and temperature is 400 ℃, time 1h.Zinc oxide purity reaches 99.7%, and iodine sorption value reaches more than the 40mg/g.
Embodiment 2: zinc oxide ore composition (%): Zn 4.94, and Pb 1.74, and Cu 0.01, and Fe 13.53, and Cd 0.29, and Co 0.038.
Prepare first [(NH
4)
2CO
3]=2.5mol/L, [NH
3The leaching agent 1L of]=5mol/L takes by weighing zinc oxide ore 500g, and liquid-solid volume mass is than 2: 1, under 35 ℃, leaches 1h, incorporate washing lotion into after the leach liquor volume identical with leaching agent, leach liquor contains zinc 21.33g/L; This leach liquor as leaching agent, is leached zinc oxide ore 500g under the same conditions again, and zinc content is brought up to 42.41g/L in the leach liquor for the second time; Leach liquor is as leaching agent for the second time, carry out under the same conditions for the third time circulating leaching, filter, washing, incorporate washing lotion into, obtain for the third time leach liquor 1000ml, zinc concentration is increased to 63.47g/L, zinc leaching rate 85.21%, leach liquor composition (g/L): Zn 63.47, Pb 0.06, and Cu 0.12, and Cd 0.71.3 times by displacement Cu, Cd, the required zinc powder theoretical amount of Pb add zinc powder, churning time 1h, 30 ℃ of temperature.Liquid reacts in the efficient spray moisture eliminator and directly generates Zinc oxide powder after purifying, and reaction conditions is: inlet temperature is 600 ℃, and temperature out is 420 ℃, and input speed is 40mL/min, and the charging zinc concentration is 70g/L.Zinc oxide purity reaches more than 99.8%, and iodine sorption value reaches more than the 45mg/g.
Embodiment 3: raw material is the zinc oxide secondary resource, i.e. secondary zinc oxide cigarette ash, and composition (%): Zn 45.76, and Pb 7.45, Cd0.47, Fe4.09, In0.044, Mn0.40, Cu0.072, Ag0.0044, Cl0.04, F0.84, Sb0.34, As1.28.Prepare first [NH
4HCO
3]=2mol/L, [NH
3The leaching agent 1L of]=6mol/L takes by weighing zinc oxide fume dust 250g, and liquid-solid volume mass was than 4: 1, under 20 ℃, leach 1h, incorporate washing lotion into after the leach liquor volume identical with leaching agent, zinc leaching rate 93.26%, leach liquor composition (g/L): Zn 106.69, Pb 0.45, and Cu 0.06, and Cd 0.82, As 0.046, and Sb 0.0058.4 times by displacement Cu, Cd, the required zinc powder theoretical amount of Pb add zinc powder, churning time 0.5h, temperature 50 C.Liquid reacts in the efficient spray moisture eliminator and generates powders A after purifying, and reaction conditions is: inlet temperature is 450 ℃, and temperature out is 280 ℃, and input speed is 50mL/min, and the charging zinc concentration is 100g/L.Have part zinc subcarbonate unreacted complete, powders A is the mixture of zinc subcarbonate and zinc oxide.Powders A is at boiling kiln roasting, 400 ℃ of temperature, time 10min.Zinc oxide purity reaches more than 99.8%, and iodine sorption value reaches more than the 45mg/g.
Embodiment 4: zinc oxide ore composition (%): Zn 4.94, and Pb 1.74, and Cu 0.01, and Fe 13.53, and Cd 0.29, and Co 0.038.
Prepare first [NH
4Cl]=0.5mol/L, [NH
3The leaching agent 2L of]=10mol/L takes by weighing zinc oxide ore 2500g, under 25 ℃, circulating column soaks, and leaches and uses the solution washing leaching post identical with the leach liquor composition 2 times after finishing, and then washes with water 2 times, incorporate that the leach liquor volume is 2.5L after the washing lotion into, leach liquor contains zinc 48.41g/L; Zinc leaching rate 98.01%, leach liquor composition (g/L): Zn48.41, Pb 0.07, and Cu 0.13, and Cd 0.68.3 times by displacement Cu, Cd, the required zinc powder theoretical amount of Pb add zinc powder, churning time 1h, 30 ℃ of temperature.Liquid reacts in the efficient spray moisture eliminator and directly generates Zinc oxide powder after purifying, and reaction conditions is: inlet temperature is 350 ℃, and temperature out is 180 ℃, and input speed is 30mL/min, and the charging zinc concentration is 45g/L.Zinc oxide purity reaches more than 99.8%, and iodine sorption value reaches more than the 45mg/g.
Claims (3)
1. method of processing zinc oxide ore or zinc oxide secondary resource to prepare superfine active zinc oxide comprises following operation:
The ammonia leaching: take the zinc oxide ore that contains zinc 2-60% or complicated zinc oxide secondary resource as raw material, in ammonia gonosome system, cooperate leaching, filter cleaner, filtrate enters subsequent processing;
Displacement purge: with zinc powder the filtrate of leaching is carried out displacement purge and remove impurity element, refilter slagging-off, filtrate enters subsequent processing;
Decompose: produce powders A the decomposition of the filtrate of purification,
Roasting: powders A becomes superfine active zinc oxide through roasting;
It is characterized in that: decomposition process is atomization drying, and the filtrate that is about to purify is carried out the high-temperature spray decomposition and produced powders A, and tail gas returns leaching process configuration leaching agent through condensation, spray-absorption.
2. method according to claim 1 is characterized in that the technology condition of each operation is as follows:
Ammonia leaching operation: the leach liquor composition is [NH
4 +]=0.5-5 (mol/L), [NH
3]=0.5-10 (mol/L);
Liquid-solid mass ratio is 2-10: 1; Extraction temperature is 10-50 ℃; Extraction time is 0.3-4h;
The displacement purge operation: the zinc powder consumption is 1.5-30 times of theoretical consumption; Purification temperature 10-50 ℃; Time 0.5-5h;
Atomization drying operation: inlet temperature=100-800 ℃, temperature out is 80-700 ℃; Input speed=10-100mL/min; Charging zinc concentration=5-200g/L;
Calcining process: maturing temperature=200-800 ℃; Roasting time=5-180min.
3. method according to claim 1, it is characterized in that: the atomization drying operation is finished in Efficent sprayer, and atomizer is rotational pressure formula spraying gun, centrifugal pressure formula spraying gun, combination pressure formula spraying gun, pneumatic atomizer, centrifugal spray-dryer.
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Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101818248A (en) * | 2010-05-28 | 2010-09-01 | 中南大学 | Method for deeply purifying zinc-ammonia leaching solution |
| CN102583503B (en) * | 2011-01-18 | 2013-07-17 | 郴州市金贵银业股份有限公司 | Method for preparing activated zinc oxide by utilizing high-arsenic secondary zinc oxide resource ammonia-ammonium process |
| CN102660681A (en) * | 2011-12-31 | 2012-09-12 | 成都易态科技有限公司 | Liquid zinc purification process and zinc powder displacement method in liquid zinc purification |
| WO2014047761A1 (en) * | 2012-09-25 | 2014-04-03 | 陈尚全 | Method for producing high-purity nanometer zinc oxide from low-grade zinc oxide ore by ammonia process |
| WO2014047765A1 (en) * | 2012-09-25 | 2014-04-03 | 四川巨宏科技有限公司 | Method for producing nanometer lithopone from low-grade zinc oxide ore compound waste gypsum |
| WO2014047762A1 (en) * | 2012-09-25 | 2014-04-03 | 四川巨宏科技有限公司 | Method for producing high-purity nanometer zinc oxide from low-grade zinc oxide ore by ammonia decarburization |
| US9346934B2 (en) * | 2012-09-25 | 2016-05-24 | Sichuan Xinhong Technology Co., Ltd | Method for producing nanometer lithopone from electrolytic zinc acid leaching residue |
| CN112578077B (en) * | 2020-11-11 | 2022-08-12 | 韶关凯鸿纳米材料有限公司 | Zinc recovery method for silicon dioxide detection |
| CN112408460B (en) * | 2020-12-10 | 2022-09-13 | 平江县吉成科技有限责任公司 | Preparation method of nano zinc oxide |
| CN113264549A (en) * | 2021-06-04 | 2021-08-17 | 江永县潇湘化工有限公司 | New preparation process of active zinc oxide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1413911A (en) * | 2002-09-30 | 2003-04-30 | 吴晓东 | Process for preparing high-purity Nano-class zinc oxide |
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| CN1413911A (en) * | 2002-09-30 | 2003-04-30 | 吴晓东 | Process for preparing high-purity Nano-class zinc oxide |
Non-Patent Citations (1)
| Title |
|---|
| 刘亚川等."低品位氧化锌矿的氨—铵盐浸出研究".《矿产综合利用》.2008,(第2期),3-6. |
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