CN106853982A - A kind of preparation method of high-purity zinc oxide - Google Patents
A kind of preparation method of high-purity zinc oxide Download PDFInfo
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- CN106853982A CN106853982A CN201710051747.3A CN201710051747A CN106853982A CN 106853982 A CN106853982 A CN 106853982A CN 201710051747 A CN201710051747 A CN 201710051747A CN 106853982 A CN106853982 A CN 106853982A
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- zinc
- leaching
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- iron
- liquid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention provides a kind of preparation method of high-purity zinc oxide, the slurry of zinc-containing raw materials is provided first；The raw material includes zinc and iron, and limiting the content of zinc, to be not less than 5wt% and the particle diameter of raw material be 100~150 mesh；Neutral leaching is carried out to the slurry using acid solution, neutral leachate is obtained after separation of solid and liquid, neutral leachate is carried out except separation of solid and liquid after iron, heavy zinc reaction is carried out after obtaining treatment fluid, calcining obtains zinc-containing precipitated, obtains high-purity zinc oxide.The present invention provides the raw material that particle diameter is 100~150 mesh, by the mixing of acid solution, realizes the separation of leachate and filter residue, only needs in raw material, and the weight/mass percentage composition of zinc is not less than 5%；With reference to iron removal, it is ensured that with the abundant removal of impurity in the precipitation that this is obtained, and then avoid the influence that iron during heavy zinc precipitates to zinc；Realize the abundant removal of iron by abovementioned steps, the precipitation of precalcining treatment need not crush ball milling and directly carry out calcination process and can obtain high-purity zinc oxide.
Description
Technical field
The invention belongs to MOS Technology field, more particularly to a kind of preparation method of high-purity zinc oxide.
Background technology
Zinc oxide (ZnO), is commonly called as zinc white, is a kind of oxide of zinc, is insoluble in water, dissolves in acid and highly basic.Zinc oxide
Pottery is widely used in its relatively low coefficient of expansion, the advantage that specific surface area is big, covering power is strong and iron content is few
Porcelain products preparation field, the ceramic prepared with high pure zinc oxide, aberration is small, highly polished and with good
Thermal vibration high and mechanical oscillation effect.
The preparation method of zinc oxide conventional at present has a wet method, by immersion by the impurity in raw material and other gold more than wet method
Press filtration obtains the zinc ingot metal of more than Zn content 95wt% after category raw material is leached, then produces zinc oxide by blast-furnace roasting, is forged in zinc ingot metal
Crushing ball mill is first carried out to zinc ingot metal during firing standby zinc oxide, then be calcined, not only technique is cumbersome can also consume big
Energy.
The content of the invention
In view of this, it is an object of the invention to provide a kind of preparation method of high-purity zinc oxide, the system that the present invention is provided
Preparation Method process is simple, need not carry out crushing the process of ball milling before zinc ingot metal calcining.
In order to realize foregoing invention purpose, the present invention provides following technical scheme：
The invention provides a kind of preparation method of high-purity zinc oxide, comprise the following steps：
(1) slurry of zinc-containing raw materials is provided；The raw material includes zinc and iron, the weight/mass percentage composition of zinc in the raw material
It is not less than 5wt%；The particle diameter of the raw material is 100~150 mesh；
(2) neutral leaching is carried out to the slurry of the step (1) using acid solution, neutral leaching is obtained after separation of solid and liquid
Liquid；
(3) the neutral leachate that the step (2) is obtained is carried out, except separation of solid and liquid after iron, obtaining except iron charge liquid；
(4) reacted what the step (3) was obtained except iron charge liquid carries out heavy zinc, obtain zinc-containing precipitated；
(5) what the calcining step (4) obtained is zinc-containing precipitated, obtains high-purity zinc oxide.
Preferably, the quality of zinc-containing raw materials and the volume ratio of initial acid solution are (3.5 in the slurry of the step (2)
~4.5) g：1L；The initial concentration of the acid solution is 90~110g/L；
The neutral temperature for leaching is 65~70 DEG C；Neutral leaching end when the pH value of mixed liquor is 4.8~5.4
Only.
Preferably, neutral leaching filter residue is also obtained after the separation of solid and liquid of the step (2), is also included：Using acid solution
Acidic leaching is carried out to the neutral filter residue that leaches, acid leaching solution is obtained after separation of solid and liquid；
The acid leaching solution is carried out into heavy zinc reaction, the precipitation calcining that will be obtained obtains high-purity zinc oxide.
Preferably, the initial concentration of the acidic leaching acid solution is 150~200g/L, and the acidic leaching is in acid
Property solution concentration be 80g/L when terminate；
The volume ratio of the neutral quality for leaching filter residue and the acidic leaching acid solution is (3~4) g：1L；
The temperature of the acidic leaching is 80~90 DEG C.
Preferably, also include before the heavy zinc reaction：Using zinc raw material to described except iron charge liquid or acid leaching solution are carried out
Displacement reaction.
Preferably, the moisture content of slurry is 20~30wt% in the step (1).
Preferably, except iron includes in the step (3)：By the neutral leachate and H2O2It is 4.5 that pH value is adjusted after mixing
~5.5；Iron ion and H in the neutral leachate2O2Material amount ratio be (1.5~2)：1.
Preferably, the temperature of the calcining stands alone as 600~850 DEG C.
Preferably, the heavy zinc reaction includes：Sunk described except iron charge liquid or acid leaching solution mix with carbonate
Zinc reacts；The consumption of the carbonate by described except being counted on the basis of the content of zinc in iron charge liquid or acid leaching solution, the carbonic acid
The ratio between salt and amount of material of the zinc are 1：(1.5~1.7).
Preferably, the temperature of the heavy zinc reaction is 40~70 DEG C, and the time of the heavy zinc reaction is 1~1.5h.
The invention provides a kind of preparation method of high-purity zinc oxide, the slurry of zinc-containing raw materials is provided first；The raw material
Including zinc and iron, limiting the weight/mass percentage composition of zinc in the raw material, to be not less than 5wt% and the particle diameter of raw material be 100~150 mesh；
Neutral leaching is then carried out to the slurry using acid solution, neutral leachate is obtained after separation of solid and liquid, the neutrality that will be obtained
Leachate carries out, except separation of solid and liquid after iron, obtaining treatment fluid；Heavy zinc reaction is carried out to treatment fluid, obtains zinc-containing precipitated, calcine institute
State zinc-containing precipitated, obtain high-purity zinc oxide.The present invention provide particle diameter be 100~150 mesh zinc-containing raw materials, by with acid solution
Mixing, realize the separation of leachate and filter residue, the content requirement to zinc in raw material is low, only needs the quality percentage of zinc in raw material to contain
Amount is not less than 5%；Further combined with iron removal, it is ensured that with the abundant removal of impurity in the precipitation that this is obtained, and then keep away
Exempt from the influence that iron during heavy zinc is precipitated to zinc；The abundant removal of iron, the precipitation nothing of precalcining treatment are realized by abovementioned steps
Ball milling need to be crushed directly carry out calcination process and can obtain high-purity zinc oxide.The result of the embodiment of the present invention shows, according to this hair
The purity zinc oxide that bright preparation method is obtained is up to 99.9%.
Specific embodiment
The invention provides a kind of preparation method of high-purity zinc oxide, the slurry of zinc-containing raw materials is provided first；The raw material
Including zinc and iron, limiting the weight/mass percentage composition of zinc in the raw material, to be not less than 5wt% and the particle diameter of raw material be 100~150 mesh；
Neutral leaching is then carried out to the slurry using acid solution, neutral leachate is obtained after separation of solid and liquid, the neutrality that will be obtained
Leachate carries out, except separation of solid and liquid after iron, obtaining treatment fluid；Heavy zinc reaction is carried out to treatment fluid, obtains zinc-containing precipitated, calcine institute
State zinc-containing precipitated, obtain high-purity zinc oxide..
The present invention provides the raw material that particle diameter is 100~150 mesh, by the mixing of acid solution, realizes leachate and filter residue
Separation, the content requirement to zinc in raw material is low, only needs in raw material, and the weight/mass percentage composition of zinc is not less than 5%, is capable of achieving
The recycling of waste material；Further combined with iron removal, it is ensured that with the abundant removal of impurity in the precipitation that this is obtained, and then keep away
Exempt from the influence that iron during heavy zinc is precipitated to zinc；The abundant removal of iron, the precipitation nothing of precalcining treatment are realized by abovementioned steps
Ball milling need to be crushed directly carry out calcination process and can obtain high-purity zinc oxide.The result of the embodiment of the present invention shows, according to this hair
The zinc oxide mass fraction that bright preparation method is obtained reaches 95~98.5%.
The present invention provides the slurry of zinc-containing raw materials.In the present invention, the zinc-containing raw materials include zinc and iron.In this hair
In bright, zinc and the preferred independent presence in the form of simple substance of iron in the zinc-containing raw materials.In the present invention, in the raw material zinc matter
Amount percentage composition is not less than 5wt%, more preferably preferably 6~70wt%, 10~15wt%；In the present invention, the raw material
Particle diameter be 100~150 mesh, preferably 120~140 mesh, more preferably 125~130 mesh.
In the present invention, the slurry is preferably obtained by the way of pulp；Concrete form of the present invention to the pulp
There is no particular/special requirement, using pulp form well-known to those skilled in the art.In an embodiment of the present invention, the slurry
Change and be specially wet ball-milling, the present invention does not have particular/special requirement to the ratio of grinding media to material of the wet ball-milling, Ball-milling Time, can obtain institute
State slurry.
In the present invention, the raw material is preferably blast furnace gas mud or blast furnace gas ash.The present invention is with described
Blast furnace gas mud, blast furnace gas ash or blast furnace pipeline ash realize the recycling to waste material for raw material.This
Invention is adopted to the no particular/special requirement in source of the blast furnace gas mud, blast furnace gas ash or blast furnace pipeline ash
With well-known to those skilled in the art.
In the present invention, the moisture content of the slurry is preferably 20~30wt%, more preferably 25~28wt%.
In the present invention, the zinc-containing raw materials are provided in a form of slurry, are easy to be fully contacted with acid solution, are improved and neutral are leached effect
Rate.
The present invention carries out neutral leaching using acid solution to the slurry, and neutral leachate is obtained after separation of solid and liquid.
In the present invention, the acid solution is preferably sulfuric acid solution, hydrochloric acid solution or salpeter solution；The present invention is to the acid solution
Originate no particular/special requirement, using acid solution well-known to those skilled in the art.
In the present invention, the consumption of the acid solution is on the basis of the gross mass of zinc-containing raw materials in the slurry to count, institute
State the quality of zinc-containing raw materials in slurry and ratio preferably (3.5~4.5) g of initial acid liquor capacity：1L, more preferably
(3.2~4.2) g:1L, more preferably 4g:1L.In the present invention, the initial concentration of the acid solution is preferably 90~110g/
L, more preferably 95~105g/L, more preferably 100g/L.In the present invention, the neutral temperature for leaching is preferably 65
~70 DEG C, more preferably 66~69 DEG C.In the present invention, the neutral leaching is when the pH value of mixed liquor is 4.8~5.4
Terminate, preferably 5.0~5.2.
In the present invention, the time that the neutrality is leached is preferably 4~6h, more preferably 4.5~5.5h, more preferably
It is 5h.In the neutral leaching process, the form that zinc and iron simple substance in zinc-containing raw materials are converted to ion is present in the present invention
In neutral leachate, specially：In neutral leaching process, the oxide of zinc and ferrous oxide can effectively dissolve,
And calcium oxide and lead oxide then generate the salt precipitation of indissoluble, when in the neutral leaching process, using sulfuric acid as acid leaching solution
When, the mechanism of calcium oxide and lead oxide forming salt precipitation is CaO+H2SO4=CaSO4↓+H2O, PbO+H2SO4=PbSO4↓+H2O；
In the neutral leaching process, the concentration and the neutral scope for leaching pH value when terminating of strict control acid solution, it is to avoid
The zinc ion that neutral leaching process is obtained forms zinc hydroxide precipitation, reduces the leaching rate of zinc.
The present invention does not have particular/special requirement to the neutral specific implementation process for leaching, ripe using those skilled in the art institute
The raw material leaching process known；In an embodiment of the present invention, the neutral leaching is specifically carried out in neutral leaching tanks.
After the neutral leaching, the present invention carries out separation of solid and liquid to the slurry after the neutral leaching, obtains neutral leaching
Liquid, contains zinc ion and iron ion in the neutral leachate.The present invention does not have particular/special requirement to the mode of the separation of solid and liquid,
Using solid-liquid separation method well-known to those skilled in the art.In the present invention, the separation of solid and liquid is preferably press filtration
Separate；In an embodiment of the present invention, the separation of solid and liquid specifically carries out the separation of solid and liquid using closed delivery filter press.
After obtaining neutral leachate, the present invention carries out the neutral leachate, except separation of solid and liquid after iron, to obtain treatment fluid.
In the present invention, it is described except iron preferably includes following steps：By the neutral leachate and H2O2PH value to 4.5 is adjusted after mixing
Carried out after~5.5 except iron.In the present invention, the temperature except iron is preferably 70~80 DEG C, more preferably 72~75 DEG C.
In the present invention, the H2O2So that the iron in neutral leachate forms scum in the form of precipitating, and in the present invention, neutrality leaching
The divalent iron and H gone out in liquid2O2Reaction generation trivalent iron, FeOOH precipitations is formed under pH value condition and is removed, reaction mechanism tool
Body is：When also manganese ion is contained in the neutral leachate, the H2O2So that in
Manganese in property leachate forms scum in the lump in the form of precipitating with foregoing iron.
In the present invention, iron ion and H in the neutral leachate2O2Material amount than be preferably (1.5~2)：1, enter
One step is preferably (1.6~1.8)：1.In the present invention, the H2O2It is preferred that provided in the form of hydrogen peroxide, the hydrogen peroxide
Mass concentration is preferably 22~27wt%, more preferably 24~25%；The present invention does not have special wanting to the source of the hydrogen peroxide
Ask, using hydrogen peroxide well-known to those skilled in the art.After the mixing, the pH value of the preferred regulation mixed liquor of the present invention
It is 4.5~5.5, more preferably 4.8~5.0.In the present invention, the regulation of the pH value is preferably adjusted using refined lime；
In the present invention, the addition of the refined lime is defined by that can obtain the pH value.
It is described except iron after, the present invention carries out heavy zinc reaction to the treatment fluid, obtains zinc-containing precipitated.
In the present invention, the heavy zinc reaction is preferably included：The treatment fluid is mixed with carbonate carries out heavy zinc reaction.
In the present invention, the consumption of the carbonate is on the basis of the content of zinc in the treatment fluid preferably to count, the carbonate and institute
State the ratio between amount of material of zinc and be preferably 1：(1.5~1.7), more preferably 1：(1.55~1.65), more preferably 1:
1.6；In the present invention, the carbonate is provided preferably in the form of carbonate solution.Concentration of the present invention to the carbonate
There is no particular/special requirement, in the present invention, the concentration of the carbonate solution is preferably 30~50wt%, more preferably
40wt%.In the present invention, the carbonate is preferably sodium carbonate or ammonium hydrogen carbonate.
In the present invention, the mixed process carries out the heavy zinc reaction simultaneously.In the present invention, the heavy zinc reacts
Temperature is preferably 40~70 DEG C, more preferably 50~60 DEG C.In the present invention, the zinc sinks reaction preferably in reaction solution
PH value be 6.8~7 and reaction solution in free alkali mass concentration be 0.3~0.5% when terminate.Heavy zinc described in preferred pair of the present invention
Mixed liquor in course of reaction carries out the real-time monitoring of the mass concentration of free alkali in pH value and the mixed liquor, and the present invention is to institute
The mode for stating real-time monitoring does not have particular/special requirement, using pH value well-known to those skilled in the art and the mass concentration of free alkali
Monitoring method.In the present invention, the time of the heavy zinc reaction be preferably 1~1.5h, more preferably 1.2~
1.4h。
In the present invention, it is described to be carried out preferably under conditions of heating stirring except iron charge liquid mixes with carbonate；In this hair
In bright, the temperature of the heating stirring is the temperature of the heavy zinc reaction, and the time of the heating stirring is the heavy zinc
The time of reaction；The rotating speed of the heating stirring preferably 100~200rpm.
After completing the heavy zinc reaction, the product that preferred pair of the present invention is obtained carries out separation of solid and liquid, obtains heavy containing zinc
Form sediment.In the present invention, the zinc-containing precipitated specially basic zinc carbonate filter cake.
In the present invention, the separation of solid and liquid is preferably press filtration, the concrete operation method that the present invention to the press filtration separate
There is no particular/special requirement, so that filtrate and zinc-containing precipitated separation can be realized.
When also copper is included in the raw material, preferably also include before the heavy zinc reaction：Using zinc raw material to the treatment
Liquid enters line replacement reaction.In the present invention, the temperature of the displacement reaction is preferably 50~60 DEG C, more preferably 55~58
℃.Present invention preferably employs zinc raw material the treatment fluid is entered line replacement reaction, complete zinc raw material to copper in the treatment fluid from
The displacement of son, obtains zinc solution.In the present invention, the addition of the zinc raw material is preferably with the quality of copper in the treatment fluid
On the basis of count, in the present invention, the quality of the zinc raw material is 3~5 times of copper mass in the treatment fluid.The present invention preferably with
The product of the copper ion concentration and the treatment fluid volume is the quality of copper in the treatment fluid to be replaced.Preferred survey of the invention
Try the concentration of copper ion in the treatment fluid and the volume for the treatment of fluid to be replaced；The present invention is to the copper ion concentration and treatment fluid
The mensuration mode of volume does not have particular/special requirement, is determined using copper ion concentration well-known to those skilled in the art and liquor capacity
Method.The no particular/special requirement in source to the zinc raw material of the invention, it is former using zinc well-known to those skilled in the art
Material；In the present invention, the purity of the zinc raw material is preferably 95~99%.In the present invention, the zinc raw material preferably with
The form of zinc powder is provided；The present invention does not have particular/special requirement, preferably 100~150 mesh to the particle diameter of the zinc powder.
When the present invention enters line replacement reaction to the mixed liquor using zinc raw material, preferably zinc raw material is added described to be replaced
In treatment fluid；In the present invention, the zinc raw material add the time according on the basis of the gross mass of the zinc raw material count, preferably
(90~100) min/ (4~5) Kg；In the present invention, preferably by controlling the addition time when zinc raw material is added, to ensure
Being uniformly added into for zinc raw material, is easy to the uniform contact of zinc raw material and mixed liquor.In the present invention, the mixing is preferably and stirs mixed
Close, the speed of the stirring mixing is preferably 0.5~1m/s, more preferably 0.6~0.8m/s；In the present invention, it is described
Stir mixing time be it is described displacement reaction time, in the present invention it is described stirring mixing preferably in mixed liquor copper from
The mass concentration of son terminates when being not higher than 0.5g/L.Mode present invention preferably employs real-time monitoring determines copper in the mixed liquor
The concentration of ion；The present invention does not have particular/special requirement to the mode of the real-time monitoring, in an embodiment of the present invention, described real-time
Monitoring is completed especially by real-time watch device.In the present invention, the time that the stirring mixes is preferably 30~60min.
In the present invention, the displacement reaction obtains also obtaining copper ashes while zinc solution, realizes the recovery to copper.
After the displacement reaction obtains zinc solution, the present invention carries out solid-liquid point after the heavy reaction of zinc to the zinc solution
From obtaining zinc-containing precipitated.In the present invention, the heavy zinc reaction is consistent with the heavy zinc reaction described in above-mentioned technical proposal, herein
Repeat no more.
Filtrate is also obtained while obtaining zinc-containing precipitated to heavy zinc product separation of solid and liquid, the present invention is excellent to the filtrate
Choosing is evaporated treatment, realizes the recovery of solute in the filtrate, and in the present invention, the solute in the filtrate preferably includes sulphur
Sour sodium, sodium chloride, sodium nitrate, ammonium sulfate, ammonium chloride or ammonium nitrate；In the present invention, the evaporation process is preferably steamed in triple effect
Carried out in hair device.
Obtain it is described it is zinc-containing precipitated after, the present invention to it is described it is zinc-containing precipitated calcine, obtain high-purity zinc oxide.In this hair
In bright, before the calcining, preferably by obtain it is zinc-containing precipitated washed successively and dried, remove it is described it is zinc-containing precipitated on it is residual
Remaining reagent.The present invention does not have particular/special requirement to the mode of the washing, using mode of washing well-known to those skilled in the art
；In embodiments of the present invention, the washing is specially and zinc-containing precipitated is rinsed to described using deionized water.In this hair
In bright, the dry temperature is preferably 80~150 DEG C, and the dry time is preferably 10~20min；The present invention is to described
Dry specific embodiment does not have particular/special requirement, using drying mode well-known to those skilled in the art.In this hair
In bright, the drying is carried out preferably in drying machine；The present invention does not have particular/special requirement to the type of the drying machine, using ability
Drying machine known to field technique personnel；In an embodiment of the present invention, the drying machine is preferably flash dryer.
In the present invention, the temperature of the calcining is preferably 600~850 DEG C, more preferably 650~700 DEG C.At this
In invention, the time of the calcining is preferably 20~60min, more preferably 30~40min.In the present invention, it is described to forge
The atmosphere of burning is preferably natural gas atmosphere, for the calcining provides calcination atmosphere.In the present invention, the calcining is preferably in revolution
Carried out in stove, the present invention does not have particular/special requirement to the type of the rotary furnace, using revolution well-known to those skilled in the art
Stove.In an embodiment of the present invention, the rotary furnace is preferably internal-heated rotary furnace.
It is described it is neutral leach after separation of solid and liquid also obtain it is neutral leach filter residue, when the raw material also include copper, indium, gold,
During one or more in silver, zinc and lead, acid leaching is carried out to the neutral filter residue that leaches present invention preferably employs acid solution
Go out, acid leaching solution is obtained after separation of solid and liquid.In the present invention, the acidic leaching realizes that centering leaches zinc in filter residue
Reclaim.The present invention is not required the existence form of copper, indium, gold, silver, zinc or lead in the raw material.In the present invention, the acid
Property leach temperature be preferably 80~90 DEG C, more preferably 85~88 DEG C.In the present invention, the consumption of the acid solution
It is preferred that being counted on the basis of the neutral quality for leaching filter residue, the volume ratio of the neutral quality and acid solution for leaching filter residue
It is (3~4) g：1L, more preferably 3.5g：1L.In the present invention, the initial concentration of the acid solution of the acidic leaching
Preferably 150~200g/L, more preferably 160~180g/L；In the present invention, the acid solution of the acidic leaching
Terminate concentration and be preferably 80g/L.
In the present invention, the kind of the acid solution during the acidic leaching and acid solution described in above-mentioned technical proposal
Class is consistent, will not be repeated here.
The present invention realizes the recovery of filter residue to also obtaining acidic leaching filter residue after the acid leaching solution separation of solid and liquid.
In the present invention, one or more in compound of the acidic leaching filter residue comprising copper, indium, gold, silver, zinc and lead, in this hair
In bright, the compound of the copper, indium, gold, silver, zinc or lead preferably exists with existence form initial in raw material.
After obtaining the acid leaching solution, the acid leaching solution is preferably carried out heavy zinc reaction by the present invention, by what is obtained
Precipitation calcining, obtains high-purity zinc oxide.In the present invention, the heavy zinc reaction is preferably included：By the acid leaching solution and carbon
Hydrochlorate mixing carries out heavy zinc reaction；The consumption of the carbonate is described to be counted on the basis of the content of zinc in the acid leaching solution
The ratio between carbonate and amount of material of the zinc are 1：(1.5~1.7), more preferably 1：(1.55~1.65), more preferably
It is 1:1.6.
In the present invention, the heavy zinc reaction for being carried out to the acid leaching solution is consistent with heavy zinc reaction mentioned above, then
It is secondary to repeat no more.
When the present invention carries out heavy zinc reaction to the acid leaching solution, preferably by the acid leaching solution and above-mentioned technical side
Mentioned by case except carrying out heavy zinc reaction after iron liquid mixing.When to the acid leaching solution and except the mixed liquor of iron charge liquid sinks
When zinc reacts, the consumption of the heavy zinc reaction carbonate is preferably counted on the basis of the content of the zinc in the mixed liquor；This hair
The carbonate consumption that requirement and the above-mentioned technical proposal of the bright consumption to the carbonate are limited is consistent, will not be repeated here.
After completing the heavy zinc reaction, preferred pair mixed liquor of the present invention carries out separation of solid and liquid, obtains zinc-containing precipitated.In this hair
In bright, the separation of solid and liquid is preferably press filtration separation, and the present invention does not have special wanting to the concrete operation method that the press filtration is separate
Ask, so that filtrate and zinc-containing precipitated separation can be realized.
In the present invention, obtain it is zinc-containing precipitated after, the present invention contain to the zinc-containing precipitated calcining for carrying out and to described
Washing and drying that zinc precipitation is preferably carried out, it is consistent with the above-mentioned corresponding technical scheme for referring to respectively, will not be repeated here.
When also copper is included in the raw material, preferably also include before heavy zinc reaction is carried out to the acid leaching solution：Using
Zinc raw material enters line replacement reaction to the acid solution.Line replacement is entered to the acid leaching solution present invention preferably employs zinc raw material
Reaction, completes displacement of the zinc raw material to copper ion in the acid leaching solution, obtains zinc solution.In the present invention, the zinc
The addition of raw material preferably to be counted on the basis of the quality of copper in the acid leaching solution, in the present invention, the matter of the zinc raw material
Measure is 3~5 times of copper mass in the acid leaching solution.In the present invention, the displacement reaction for being carried out to the acid leaching solution
It is consistent with the displacement reaction mentioned by above-mentioned technical proposal, will not be repeated here.
Completing the displacement reacted acid leaching solution also filtered while separation of solid and liquid obtains zinc-containing precipitated
Liquid, the present invention is preferably evaporated treatment to the filtrate, realizes the recovery of solute in the filtrate, in the present invention, described
Solute in filtrate preferably includes sodium sulphate, sodium chloride, sodium nitrate, ammonium sulfate, ammonium chloride or ammonium nitrate；In the present invention, institute
State evaporation process is carried out preferably in triple effect evaporator.
The invention provides a kind of preparation method of high-purity zinc oxide, the slurry of zinc-containing raw materials is provided first；The raw material
Including zinc and iron, limiting the weight/mass percentage composition of zinc in the raw material, to be not less than 5wt% and the particle diameter of raw material be 100~150 mesh；
Neutral leaching is then carried out to the slurry using acid solution, neutral leachate is obtained after separation of solid and liquid, the neutrality that will be obtained
Leachate carries out, except separation of solid and liquid after iron, obtaining treatment fluid；Heavy zinc reaction is carried out to treatment fluid, obtains zinc-containing precipitated, calcine institute
State zinc-containing precipitated, obtain high-purity zinc oxide..
The present invention provides the raw material that particle diameter is 100~150 mesh, by the mixing of acid solution, realizes leachate and filter residue
Separation, the content requirement to zinc in raw material is low, only needs in raw material, and the weight/mass percentage composition of zinc is not less than 5%；Further
With reference to iron removal, it is ensured that with the abundant removal of impurity in the precipitation that this is obtained, and then during avoiding heavy zinc, iron is precipitated to zinc
Influence；The abundant removal of iron is realized by abovementioned steps, the precipitation of precalcining treatment need not crush ball milling and directly be calcined
Process is that can obtain high-purity zinc oxide.
A kind of preparation method of the high-purity zinc oxide provided the present invention with reference to embodiment is described in detail, but
It is that they can not be interpreted as limiting the scope of the present invention.
Embodiment 1
(1) with blast furnace gas mud that zinc weight/mass percentage composition is 5% as raw material, gas mud is passed through into wet ball mill
Ball milling is carried out, moisture content is obtained for 25wt%, particle diameter is the slurry of 200 mesh.
(2) will be according to gas mud in slurry and solution 3.5:The slurry that 1 solid-to-liquid ratio will be obtained is 110g/ with initial concentration
The sulfuric acid solution mixing of L, controls temperature for 70 DEG C, carries out neutral leaching；After continuous leaching 4h, it is 5.4 to determine pH value, in terminating
Property leach, separated using the press filtration of closed delivery filter press, obtain neutral leachate and it is neutral leach filter residue, in determining neutral leachate
Zn content is 250g/L.
(3) neutrality is leached into liquid pump to iron removal trough, the concentration of iron ion in leachate is determined, according to iron in neutral leachate
Ion and H2O2The amount of material compare 1.7：1, add mass concentration to be 27% hydrogen peroxide, while adding refined lime regulation and control pH value
It is 5.5, controls temperature for 80 DEG C, the iron in filtrate, manganese is formed precipitation and enter scum；Scum after being separated through press filtration is returned back
Converter is recycled.
(4) content of zinc in filtrate is determined, is 1 according to the mol ratio of Zn content and sodium carbonate:1.5 ratio, in sulfuric acid
Sodium carbonate liquor is added in zinc filtrate, the wherein mass concentration of sodium carbonate liquor is 40%, temperature is controlled for 70 DEG C, to mixed liquor
The real-time monitoring of the mass concentration of pH value and the free alkali is carried out, it is 7.0, the quality of free alkali that pH value is measured after reaction 1.5h
Concentration is 0.3%, terminates heavy zinc process.
Press filtration separation is carried out to sinking the mixed liquor after zinc, filtrate is metabisulfite solution, using using triple effect evaporation
Device evaporation process, obtains byproduct sal glauberi；Filter cake discloses interior washing washing, wash water through the bipolar film processing system of counter-infiltration at
After reason, part returns to washing procedure recycling, and remainder returns to heavy zinc process as fresh Water circulation.
(5) to the filter cake that obtains according to《GB/T 3185---1992 zinc oxide indirect methods》With《HG/T2572--2006 works
Industry activated zinc oxide》Requirement, filter cake is dried using flash dryer, then directly using natural gas participate in burn
Mode, in interior hot auger type rotary furnace calcining 30min, control furnace temperature between 600-850 DEG C, zinc oxide product.
Zinc oxide to preparing carries out performance detection, and the weight/mass percentage composition of zinc oxide is in zinc oxide product
98.5wt%, moisture is 0.65wt%, and water solubles content is 0.45wt%, and the content of lead oxide is 0.01wt%, oxidation
The content of manganese is 0.001wt%, and the content of cupric oxide is 0.001wt%, and specific surface area is 45m2/ g, contour structures are line style
, bulk density：0.35g/cm3, fineness (45 μm of testing sieves) is 0.1%, meets the requirement of industrial ceramics zinc oxide.
Embodiment 2
(1) with blast furnace gas mud that zinc weight/mass percentage composition is 5% as raw material, gas mud is passed through into wet ball mill
Ball milling is carried out, moisture content is obtained for 20wt%, particle diameter is the slurry of 150 mesh.
(2) will be according to gas mud in slurry and solution 4:The slurry that 1 solid-to-liquid ratio will be obtained is 90g/L's with initial concentration
Sulfuric acid solution mixes, and controls temperature for 65 DEG C, carries out neutral leaching；After continuous leaching 4h, it is 4.8 to determine pH value, terminates neutral
Leach, separated using the press filtration of closed delivery filter press, obtain neutral leachate and neutral leaching filter residue, determine zinc in neutral leachate
Content is 200g/L.
(3) neutrality is leached into liquid pump to iron removal trough, the concentration of iron ion in leachate is determined, according to iron in neutral leachate
Ion and H2O2The amount of material compare 1.5：1, add mass concentration to be 22% hydrogen peroxide, while adding refined lime regulation and control pH value
It is 4.5, controls temperature for 70 DEG C, the iron in filtrate, manganese is formed precipitation and enter scum；Scum after being separated through press filtration is returned back
Converter is recycled；Filtrate send zincification to replace operation copper removal.
(4) content of copper ion in filtrate is determined, is 3 times of copper mass of benchmark addition zinc powder, grain according to zinc powder quality
Footpath is that the zinc powder of 150 mesh is added in the filtrate that step (3) is obtained in 90min, and zinc powder adding procedure is complete under agitation
Into stir speed (S.S.) is 1m/s, the carrying out of subsequent real-time monitoring filtrate displacement reaction, and reaction terminating is monitored after 30min, terminates to stir
Mix；Reacted mixed liquor is replaced described in separation of solid and liquid, the filtrate containing zinc sulfate is obtained.
(5) content of zinc in filtrate is determined, is 1 according to the mol ratio of Zn content and sodium carbonate:1.5 ratio, in sulfuric acid
Sodium carbonate liquor is added in zinc filtrate, the wherein mass concentration of sodium carbonate liquor is 40%, temperature is controlled for 40 DEG C, to mixed liquor
The real-time monitoring of the mass concentration of pH value and the free alkali is carried out, it is 6.8, the quality of free alkali that pH value is measured after reaction 1.5h
Concentration is 0.3%, terminates heavy zinc process.
Press filtration separation is carried out to sinking the mixed liquor after zinc, filtrate is metabisulfite solution, using using triple effect evaporation
Device evaporation process, obtains byproduct sal glauberi；Filter cake discloses interior washing washing, wash water through the bipolar film processing system of counter-infiltration at
After reason, part returns to washing procedure recycling, and remainder returns to heavy zinc process as fresh Water circulation.
(6) to the filter cake that obtains according to《GB/T 3185---1992 zinc oxide indirect methods》With《HG/T2572--2006 works
Industry activated zinc oxide》Requirement, filter cake is dried using flash dryer, then directly using natural gas participate in burn
Mode, in interior hot auger type rotary furnace calcining 30min, control furnace temperature between 600-850 DEG C, zinc oxide product.
Zinc oxide to preparing carries out performance detection, and the weight/mass percentage composition of zinc oxide is in zinc oxide product
99.9wt%, moisture is 0.5wt%, and water solubles content is 0.40wt%, and the content of lead oxide is 0.005wt%, oxidation
The content of manganese is 0.001wt%, and the content of cupric oxide is 0.001wt%, and specific surface area is 40m2/ g, contour structures are line style
, bulk density：0.37g/cm3, fineness (45 μm of testing sieves) is 0.08%, meets the requirement of industrial ceramics zinc oxide.
Embodiment 3
(1) with blast furnace gas mud that zinc weight/mass percentage composition is 5% as raw material, gas mud is passed through into wet ball mill
Ball milling is carried out, moisture content is obtained for 20wt%, particle diameter is the slurry of 150 mesh.
(2) will be according to gas mud in slurry and solution 4.5:The slurry that 1 solid-to-liquid ratio will be obtained is 100g/ with initial concentration
The sulfuric acid solution mixing of L, controls temperature for 65 DEG C, carries out neutral leaching；After continuous leaching 4h, it is 5.2 to determine pH value, in terminating
Property leach, separated using the press filtration of closed delivery filter press, obtain neutral leachate and it is neutral leach filter residue, in determining neutral leachate
Zn content is 150g/L.
(3) neutrality is leached into liquid pump to iron removal trough, the concentration of iron ion in leachate is determined, according to iron in neutral leachate
Ion and H2O2The amount of material compare 1.5：1, add mass concentration to be 27% hydrogen peroxide, while adding refined lime regulation and control pH value
It is 5, controls temperature for 70 DEG C, the iron in filtrate, manganese is formed precipitation and enter scum；Scum after being separated through press filtration returns to revolution
Stove is recycled；Filtrate send zincification to replace operation copper removal；
Filter residue and solution 4 are leached according to neutrality:The filter residue that 1 solid-to-liquid ratio will be obtained is the sulfuric acid of 150g/L with initial concentration
Solution mixes, wherein the volume ratio for limiting the neutral quality for leaching filter residue and sulfuric acid solution is 3g：1L, controls temperature for 90 DEG C,
Carry out acidic leaching；After continuous leaching 12h, it is 80g/L to determine sulfuric acid solution concentration, terminates neutral leaching, using closed delivery pressure
Filter press filtration is separated, and obtains neutral leachate and neutral leaching filter residue, and Zn content is 45g/L in determining neutral leachate.
Slurries after acidic leaching are separated using the press filtration of closed delivery filter press, and filter residue is used to return after plant area stores up temporarily
Rotary furnace is recycled.
(4) the neutral leaching filtrate and acidic leaching filtrate after iron removal by oxidation are mixed, determines copper ion in mixing filtrate
Content, be 5 times of copper mass of benchmark addition zinc powder according to zinc powder quality, particle diameter is that the zinc powder of 200 mesh is added in 90min
In the filtrate obtained to step (3), zinc powder adding procedure is completed under agitation, and stir speed (S.S.) is 1m/s, is then supervised in real time
The carrying out of filtrate displacement reaction is surveyed, reaction terminating is monitored after 30min, terminate stirring；Replaced described in separation of solid and liquid reacted mixed
Liquid is closed, the filtrate containing zinc sulfate is obtained.
(5) content of zinc in filtrate is determined, is 1 according to the mol ratio of Zn content and sodium carbonate:1.7 ratio, in sulfuric acid
Sodium carbonate liquor is added in zinc filtrate, the wherein mass concentration of sodium carbonate liquor is 50%, temperature is controlled for 70 DEG C, to mixed liquor
The real-time monitoring of the mass concentration of pH value and the free alkali is carried out, it is 6.8, the quality of free alkali that pH value is measured after reaction 1.0h
Concentration is 0.3%, terminates heavy zinc process.
Press filtration separation is carried out to sinking the mixed liquor after zinc, filtrate is metabisulfite solution, using using triple effect evaporation
Device evaporation process, obtains byproduct sal glauberi；Filter cake discloses interior washing washing, wash water through the bipolar film processing system of counter-infiltration at
After reason, part returns to washing procedure recycling, and remainder returns to heavy zinc process as fresh Water circulation.
To the filter cake that obtains according to《GB/T 3185---1992 zinc oxide indirect methods》With《HG/T2572--2006 industry is living
Property zinc oxide》Requirement, filter cake is dried using flash dryer, then directly using natural gas participate in burn side
Formula, in interior hot auger type rotary furnace calcining 30min, control furnace temperature between 600-850 DEG C, zinc oxide product.
Zinc oxide to preparing carries out performance detection, and the weight/mass percentage composition of zinc oxide is in zinc oxide product
99.9wt%, moisture is 0.45wt%, and water solubles content is 0.40wt%, and the content of lead oxide is 0.01wt%, oxidation
The content of manganese is 0.001wt%, and the content of cupric oxide is 0.001wt%, and specific surface area is 35m2/ g, contour structures are line style
, bulk density：0.45g/cm3, fineness (45 μm of testing sieves) is 0.1%, meets the requirement of industrial ceramics zinc oxide.
Embodiment 4
(1) with blast furnace gas mud that zinc weight/mass percentage composition is 5% as raw material, gas mud is passed through into wet ball mill
Ball milling is carried out, moisture content is obtained for 20wt%, particle diameter is the slurry of 150 mesh.
(2) will be according to gas mud in slurry and solution 4.5:The slurry that 1 solid-to-liquid ratio will be obtained is 100g/ with initial concentration
The sulfuric acid solution mixing of L, controls temperature for 65 DEG C, carries out neutral leaching；After continuous leaching 4h, it is 5.2 to determine pH value, in terminating
Property leach, separated using the press filtration of closed delivery filter press, obtain neutral leachate and it is neutral leach filter residue, in determining neutral leachate
Zn content is 150g/L.
(3) neutrality is leached into liquid pump to iron removal trough, the concentration of iron ion in leachate is determined, according to iron in neutral leachate
Ion and H2O2The amount of material compare 1.5：1, add mass concentration to be 27% hydrogen peroxide, while adding refined lime regulation and control pH value
It is 5, controls temperature for 70 DEG C, the iron in filtrate, manganese is formed precipitation and enter scum；Scum after being separated through press filtration returns to revolution
Stove is recycled；Filtrate send zincification to replace operation copper removal；
Filter residue and solution 4 are leached according to neutrality:The filter residue that 1 solid-to-liquid ratio will be obtained is the sulfuric acid of 150g/L with initial concentration
Solution mixes, wherein the volume ratio for limiting the neutral quality for leaching filter residue and sulfuric acid solution is 3g：1L, controls temperature for 90 DEG C,
Carry out acidic leaching；After continuous leaching 12h, it is 80g/L to determine sulfuric acid solution concentration, terminates neutral leaching, using closed delivery pressure
Filter press filtration is separated, and obtains neutral leachate and neutral leaching filter residue, and Zn content is 45g/L in determining neutral leachate.
Slurries after acidic leaching are separated using the press filtration of closed delivery filter press, and filter residue is used to return after plant area stores up temporarily
Rotary furnace is recycled.
(4) the neutral leaching filtrate and acidic leaching filtrate after iron removal by oxidation are mixed, zinc contains in measure mixing filtrate
Amount, is 1 according to the mol ratio of Zn content and sodium carbonate:1.7 ratio, sodium carbonate liquor is added in zinc sulfate filtrate, wherein
The mass concentration of sodium carbonate liquor is 50%, controls temperature for 70 DEG C, and the quality of pH value and the free alkali is carried out to mixed liquor
The real-time monitoring of concentration, it is 6.8 that pH value is measured after reaction 1.0h, and the mass concentration of free alkali is 0.3%, terminates heavy zinc process.
Press filtration separation is carried out to sinking the mixed liquor after zinc, filtrate is metabisulfite solution, using using triple effect evaporation
Device evaporation process, obtains byproduct sal glauberi；Filter cake discloses interior washing washing, wash water through the bipolar film processing system of counter-infiltration at
After reason, part returns to washing procedure recycling, and remainder returns to heavy zinc process as fresh Water circulation.
To the filter cake that obtains according to《GB/T 3185---1992 zinc oxide indirect methods》With《HG/T2572--2006 industry is living
Property zinc oxide》Requirement, filter cake is dried using flash dryer, then directly using natural gas participate in burn side
Formula, in interior hot auger type rotary furnace calcining 30min, control furnace temperature between 600-850 DEG C, zinc oxide product.
Zinc oxide to preparing carries out performance detection, and the weight/mass percentage composition of zinc oxide is in zinc oxide product
98.5wt%, moisture is 0.70wt%, and water solubles content is 0.50wt%, and the content of lead oxide is 0.01wt%, oxidation
The content of manganese is 0.001wt%, and the content of cupric oxide is 0.001wt%, and specific surface area is 45m2/ g, contour structures are line style
, bulk density：0.40g/cm3, fineness (45 μm of testing sieves) is 0.1%, meets the requirement of industrial ceramics zinc oxide.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of high-purity zinc oxide, comprises the following steps：
(1) slurry of zinc-containing raw materials is provided；The raw material includes zinc and iron, and the weight/mass percentage composition of zinc is not low in the raw material
In 5wt%；The particle diameter of the raw material is 100~150 mesh；
(2) neutral leaching is carried out to the slurry of the step (1) using acid solution, neutral leachate is obtained after separation of solid and liquid；
(3) the neutral leachate that the step (2) is obtained is carried out, except separation of solid and liquid after iron, obtaining except iron charge liquid；
(4) reacted what the step (3) was obtained except iron charge liquid carries out heavy zinc, obtain zinc-containing precipitated；
(5) what the calcining step (4) obtained is zinc-containing precipitated, obtains high-purity zinc oxide.
2. preparation method according to claim 1, it is characterised in that the matter of zinc-containing raw materials in the slurry of the step (2)
It is (3.5~4.5) g to measure with the volume ratio of initial acid solution：1L；The initial concentration of the acid solution is 90~110g/L；
The neutral temperature for leaching is 65~70 DEG C；The neutral leaching terminates when the pH value of mixed liquor is 4.8~5.4.
3. preparation method according to claim 1, it is characterised in that in also being obtained after the separation of solid and liquid of the step (2)
Property leach filter residue, also include：Acidic leaching is carried out to the neutral filter residue that leaches using acid solution, is obtained after separation of solid and liquid
Acid leaching solution；
The acid leaching solution is carried out into heavy zinc reaction, the precipitation calcining that will be obtained obtains high-purity zinc oxide.
4. preparation method according to claim 3, it is characterised in that the initial concentration of the acidic leaching acid solution
It is 150~200g/L, the acidic leaching terminates when the concentration of acid solution is 80g/L；
The volume ratio of the neutral quality for leaching filter residue and the acidic leaching acid solution is (3~4) g：1L；
The temperature of the acidic leaching is 80~90 DEG C.
5. the preparation method according to claim 1 or 3, it is characterised in that also include before the heavy zinc reaction：It is former using zinc
Material is to described except iron charge liquid or acid leaching solution enter line replacement reaction.
6. preparation method according to claim 1, it is characterised in that in the step (1) moisture content of slurry be 20~
30wt%.
7. preparation method according to claim 1, it is characterised in that except iron includes in the step (3)：By the neutrality
Leachate and H2O2It is 4.5~5.5 that pH value is adjusted after mixing；Iron ion and H in the neutral leachate2O2Material amount ratio
It is (1.5~2)：1.
8. the preparation method according to claim 1 or 3, it is characterised in that the temperature of the calcining stands alone as 600~850
℃。
9. the preparation method according to claim 1 or 3, it is characterised in that the heavy zinc reaction includes：Described will remove iron charge
Liquid or acid leaching solution mix with carbonate carries out heavy zinc reaction；The consumption of the carbonate is with described except iron charge liquid or acidity are soaked
Go out in liquid on the basis of the content of zinc and count, the ratio between the carbonate and amount of material of the zinc are 1：(1.5~1.7).
10. preparation method according to claim 9, it is characterised in that the temperature of the heavy zinc reaction is 40~70 DEG C, institute
The time for stating heavy zinc reaction is 1~1.5h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107500341A (en) * | 2017-09-29 | 2017-12-22 | 河北长力环保科技有限公司 | Method for preparing nano zinc oxide from zinc-containing waste |
| CN108046307A (en) * | 2017-12-18 | 2018-05-18 | 东北大学 | A kind of waste water extraction zinc of iron content containing zinc and the method for preparing zinc oxide |
| CN110357145A (en) * | 2019-08-15 | 2019-10-22 | 昆明理工大学 | A method of zinc oxalate is prepared using zinc oxide fumes and prepares nano zine oxide |
| CN112028113A (en) * | 2020-09-17 | 2020-12-04 | 常宁市华兴冶化实业有限责任公司 | Method for recovering zinc oxide powder in zinc hydrometallurgy process |
| CN112176199A (en) * | 2020-09-27 | 2021-01-05 | 衡阳市大宇锌业有限公司 | Process for efficiently purifying zinc oxide from zinc smelting waste residues |
| CN112593074A (en) * | 2020-11-16 | 2021-04-02 | 安徽铜冠有色金属（池州）有限责任公司 | Cyclic iron-removing process for low-temperature roasting and leaching of jarosite |
| CN113511669A (en) * | 2021-07-13 | 2021-10-19 | 常州市武进康佳化工有限公司 | Recovery and purification process of blast furnace zinc ash for preparing zinc carbonate |
| CN114314638A (en) * | 2021-12-29 | 2022-04-12 | 阜新成泰环保科技有限公司 | Process for producing glaze-grade zinc oxide by using blast furnace gas ash |
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| CN110357145A (en) * | 2019-08-15 | 2019-10-22 | 昆明理工大学 | A method of zinc oxalate is prepared using zinc oxide fumes and prepares nano zine oxide |
| CN112028113A (en) * | 2020-09-17 | 2020-12-04 | 常宁市华兴冶化实业有限责任公司 | Method for recovering zinc oxide powder in zinc hydrometallurgy process |
| CN112176199A (en) * | 2020-09-27 | 2021-01-05 | 衡阳市大宇锌业有限公司 | Process for efficiently purifying zinc oxide from zinc smelting waste residues |
| CN112593074A (en) * | 2020-11-16 | 2021-04-02 | 安徽铜冠有色金属（池州）有限责任公司 | Cyclic iron-removing process for low-temperature roasting and leaching of jarosite |
| CN113511669A (en) * | 2021-07-13 | 2021-10-19 | 常州市武进康佳化工有限公司 | Recovery and purification process of blast furnace zinc ash for preparing zinc carbonate |
| CN114314638A (en) * | 2021-12-29 | 2022-04-12 | 阜新成泰环保科技有限公司 | Process for producing glaze-grade zinc oxide by using blast furnace gas ash |
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