CN109052452A - A kind of zinc oxide of production method and this method production of activated zinc oxide - Google Patents
A kind of zinc oxide of production method and this method production of activated zinc oxide Download PDFInfo
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- CN109052452A CN109052452A CN201811035767.2A CN201811035767A CN109052452A CN 109052452 A CN109052452 A CN 109052452A CN 201811035767 A CN201811035767 A CN 201811035767A CN 109052452 A CN109052452 A CN 109052452A
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Abstract
The present invention provides a kind of production methods of activated zinc oxide, comprising the following steps: (1) zinc oxide is added in sulfuric acid solution, reaction obtains solution A；(2) potassium permanganate is added into the solution A, is filtered after being stirred to react, obtains solution B；(3) zinc powder is added into the solution B, is filtered after being stirred to react, obtains solution C；(4) carbonate solution is added into the solution C, liquid phase A is obtained after being stirred to react；(5) after being successively filtered the liquid phase A, wash, dry, calcining obtains the activated zinc oxide.This method converts the substandard products zinc oxide containing plurality of impurities to the activated zinc oxide of high-purity according to kinetics principle under equilibrium condition and the heat transfer technology of reinforcing, belongs to typical green chemical industry technique, environmentally friendly.
Description
Technical field
The present invention relates to Inorganic synthese technical fields, and in particular to a kind of production method of activated zinc oxide and the party
The activated zinc oxide of method production.
Background technique
Zinc oxide is the oxide of zinc, is insoluble in water, dissolves in acid and highly basic.Zinc oxide is a kind of common chemistry addition
Agent is widely used in plastics, silicate product, synthetic rubber, lubricating oil, paint, ointment, adhesive, food, electricity
In the production of the products such as pond, fire retardant.The band gap and exciton bind energy of zinc oxide are larger, and transparency is high, there is excellent room temperature
Luminescent properties have application in the products such as the liquid crystal display, thin film transistor (TFT), light emitting diode of semiconductor field.In addition,
The zinc oxide of microparticle also starts to play a role in related fields as a kind of nano material.
Zinc oxide manufacturer is concentrated mainly on Liaoning, Shandong, Hebei, Jiangsu, zhejiang and other places, the zinc oxide of production with
Based on 99.7% content, it is commonly called as 997 zinc oxide.In recent years, activated zinc oxide is answered with its excellent nano-meter characteristic, rapid development
It is also more and more extensive with field.
The partial size of activated zinc oxide is a kind of high-end high function fine inorganic product, shows between 1-100nm
Many special properties, such as non-migratory, fluorescence, piezoelectricity, absorption and scatters ultraviolet ability.Using its light, electricity,
The property of magnetic, sensitivity etc. can manufacture gas sensor, fluorophor, rheostat, UV shielding material, image note
Record material, piezoelectric material, varistor, effective catalyst, magnetic material and plastic film etc..Pass through practice, present active oxygen
Change zinc to be widely used in every field such as rubber with its excellent characteristic.
The production method of usual zinc oxide is divided into three classes: i.e. direct method (also known as U.S. law), indirect method (also known as method national law)
And wet chemistry method.Current many commercially available zinc oxide are mostly direct method or indirect method product, and granularity is micron order, specific surface area compared with
Small, these properties constrain their application field and its performance in product significantly.
In consideration of it, the present invention is specifically proposed.
Summary of the invention
The first object of the present invention is to provide a kind of production method of activated zinc oxide.
The second object of the present invention is to provide the activated zinc oxide that this method produces.
To achieve the above object, technical scheme is as follows:
The present invention relates to a kind of production methods of activated zinc oxide, comprising the following steps:
(1) zinc oxide is added in sulfuric acid solution, reaction obtains solution A；
(2) potassium permanganate is added into the solution A, is filtered after being stirred to react, obtains solution B；
(3) zinc powder is added into the solution B, is filtered after being stirred to react, obtains solution C；
(4) carbonate solution is added into the solution C, liquid phase A is obtained after being stirred to react；
(5) after being successively filtered the liquid phase A, wash, dry, calcining obtains the activated zinc oxide.
Preferably, in step (1), the zinc oxide is substandard products zinc oxide, wherein containing the oxide of other metallic elements.
Preferably, other metallic elements are selected from at least one of Pb, Fe, Cu, Cd, Mn.
Preferably, in step (1), the molar ratio of the substandard products zinc oxide and sulfuric acid is 1:(1~1.5).
Preferably, in step (1), reaction temperature is 60~80 DEG C.
Preferably, the dosage of potassium permanganate, step are determined in step (2) according to Fe the and Mn content in substandard products zinc oxide
(3) dosage of zinc powder is determined according to Cu and Cd content in substandard products zinc oxide.
Preferably, in step (2) and (3), reaction temperature is 40~60 DEG C.
Preferably, in step (4), the carbonate is Na2CO3Or K2CO3, the substandard products zinc oxide and the carbonate
Molar ratio be 1:(1~1.5).
Preferably, in step (5), obtained filter cake is dried using Rotatingandflashstreamingdrier, using cyclone collection
Device is collected desciccate, and calcination temperature is 550~650 DEG C, obtains activated zinc oxide.
The invention further relates to the activated zinc oxide that the above method produces, the partial size of the activated zinc oxide is 30~
80nm, specific surface area are 50~80m2/g。
Beneficial effects of the present invention:
The present invention produces nano level superfine activated zinc oxide using wet chemistry method.This method can be used containing various metals member
The substandard products zinc oxide of plain oxide converts zinc ion for zinc oxide using acidleach first as raw material, and then purification removes former
Impurity in material, then precipitating obtains basic zinc carbonate, and after rotary drying and cyclone collection, it is forged at high temperature
It burns, obtains activated zinc oxide.This method will contain according to kinetics principle under equilibrium condition and the heat transfer technology of reinforcing
The substandard products zinc oxide of plurality of impurities is converted into the activated zinc oxide of high-purity, belongs to typical green chemical industry technique, to environment friend
It is good.This method has been able to carry out large-scale continuous production.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical solution of the present invention will be carried out below
Detailed description.Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Base
Embodiment in the present invention, those of ordinary skill in the art are obtained all without making creative work
Other embodiment belongs to the range that the present invention is protected.
The present embodiments relate to a kind of production methods of activated zinc oxide, comprising the following steps:
(1) zinc oxide is added in sulfuric acid solution, reaction obtains solution A.
In one embodiment of the invention, which is substandard products zinc oxide, wherein containing the oxygen of other metallic elements
Compound.Substandard products zinc oxide is also referred to as secondary zinc oxide, is the rim charge in zinc oxide sintering procedure.The wherein mass content one of zinc oxide
As be 40%~70%, it is also possible to reach 80%.The ground such as Guangxi, Guizhou, Yunnan, Hunan yield is larger, purposes mainly into
One step processes electrolytic zinc or zinc oxide, and some is also used for displacement and uses.
Further, in above-mentioned substandard products zinc oxide, in addition to Zn-ef ficiency, other metallic elements are selected from Pb, Fe, Cu, Cd, Mn
At least one.Therefore it needs to purify it during subsequent.
In one embodiment of the invention, it is added after sulfuric acid shown in mainly generating polynomial (1)~formula (6) and chemically reacts:
ZnO+H2SO4=ZnSO4+H2O (1)
PbO+H2SO4=PbSO4↓+H2O (2)
FeO+H2SO4=FeSO4+H2O (3)
CuO+H2SO4=CuSO4+H2O (4)
CdO+H2SO4=CdSO4+H2O (5)
MnO+H2SO4=MnSO4+H2O (6)
Wherein, the molar ratio of zinc oxide and sulfuric acid should be 1:1.In order to ensure zinc oxide fully reacting, should suitably increase
The dosage of sulfuric acid, the amount ratio of the two is with 1:(1.2~1.5) it is advisable.
During this, preferably 60~80 DEG C of reaction temperature, reaction rate can be improved.Substandard products zinc oxide volume no longer
Stop reaction when reduction, the pH value of solution A is 4.8~5.2 at this time, wherein mainly containing ZnSO4, also contain PbSO4Precipitating,
FeSO4、CuSO4、CdSO4、MnSO4Equal substances.Zinc sulfate mass concentration in solution A is about 25%.
(2) after the completion of step (1), potassium permanganate is added into solution A, is filtered after being stirred to react, obtains solution B.
In one embodiment of the invention, the use of potassium permanganate is determined according to Fe the and Mn content in substandard products zinc oxide
Amount.Potassium permanganate can by solution A ferrous ion and divalent manganesetion be converted into manganese dioxide and ferric hydroxide precipitate,
It can be removed after filtering.Shown in reaction process such as formula (7) and formula (8):
2H2O+3MnSO4+2KMnO4=K2SO4+5MnO2↓+2H2SO4 (7)
14H2O+6FeSO4+2KMnO4=K2SO4+6Fe(OH)3↓+5H2SO4+2MnO2↓ (8)
(3) after the completion of step (2), zinc powder is added into solution B, is filtered after being stirred to react, obtains solution C.
In one embodiment of the invention, the dosage of zinc powder is determined according to Cu and Cd content in substandard products zinc oxide.Zinc powder
The torpescence heavy metal such as Cd, Cu can be replaced into simple substance, be equally removed after filtration.Reaction process such as formula (9) and formula
(10) shown in:
CuSO4+ Zn=Cu+ZnSO4 (9)
CdSO4+ Zn=Cd+ZnSO4 (10)
Its dosage is about 0.1% of metallic zinc quality in secondary zinc oxide.
In order to accelerate reaction rate, the reaction temperature of step (2) and (3) is 40~60 DEG C.For certain a batch of substandard products
Zinc oxide, potassium permanganate dosage are about 0.15% of metallic zinc quality in secondary zinc oxide, and zinc powder dosage is about in substandard products zinc oxide
The 0.1% of metallic zinc quality.The solution C obtained after filtering is pure solution of zinc sulfate.
(4) after the completion of step (3), carbonate solution is added into solution C, liquid phase A is obtained after being stirred to react.
In one embodiment of the invention, the alkali in carbonate solution is Na2CO3Or K2CO3.When use Na2CO3When,
Shown in reaction process such as formula (11):
3ZnSO4+3Na2CO3+3H2O=ZnCO3·2Zn(OH)2·H2O+3Na2SO4+CO2↑ (11)
In order to keep precipitation reaction complete, accelerate reaction rate, the preferably reaction temperature of this step is 45~65 DEG C, when reaction
Between be 0.5~1h, the molar ratio of substandard products zinc oxide and carbonate is 1:(1~1.5).The pH value of liquid phase A is 6.7 after reaction
~7.5.
(5) after step (4), after liquid phase A is successively filtered, is washed, is dried, calcining obtains activated zinc oxide.
In one embodiment of the invention, it is filtered with chamber filter press, is examined with originally water washing to sulfate radical-free
Out.To prevent product from reuniting, obtained filter cake is dried using Rotatingandflashstreamingdrier.After material enters, in drying machine
Bottom, larger wetter cluster of grains is by Mechanical Crushing under the action of blender, and moisture content is lower, the lesser particle quilt of granularity
Swirling eddy entrainment rises, and is further dried in uphill process.Since gas-particle two-phase makees rotational flow, solid phase inertia is greater than gas
Phase, the alternate relative velocity of solid gas two is larger, strengthens two alternate mass-and heat-transfers, so machine production intensity is high, and effectively keeps away
The generation of agglomeration is exempted from.
After the completion of drying, desciccate is separated using cyclone collector, is collected with cloth bag, obtains alkali formula carbon
Sour zinc particle.Basic zinc carbonate particle is calcined at 550~650 DEG C using rotary calciner, calcination time be 1~
3h occurs to react as shown in formula (12):
ZnCO3·2Zn(OH)2·H2O=3ZnO+CO2↑+3H2O (12)
In the above process, the hierarchy system that Rotatingandflashstreamingdrier is carried by equipment, while realizing dry and crushing function
Energy.The basic zinc carbonate content of beary metal of production is low, and fineness and whiteness are good, and purity is high reaches professional standard high-class product.Pass through rotation
Turn the zinc oxide large specific surface area of calcining furnace production, product colour is good.And treating capacity is big, quality is stablized.
The invention further relates to the activated zinc oxide that the above method produces, partial size is 30~80nm, and specific surface area is
50~80m2/g。
This method has been able to carry out large-scale continuous production.Activated zinc oxide single process units can give birth to per hour at present
Produce 1 ton.In one embodiment of the invention, it using 1.5 tons of substandard products zinc oxide, wherein containing 0.8 ton of metallic zinc, can produce
1 ton of activated zinc oxide out.
Embodiment 1
Activated zinc oxide is produced by the following method:
(1) Zn content in this batch of substandard products zinc oxide is tested in advance.Substandard products zinc oxide is added to sulfuric acid solution
In, reaction obtains solution A at 65 DEG C.The molar ratio of substandard products zinc oxide and sulfuric acid is 1:1.2.
(2) potassium permanganate is added into solution A, is filtered after being stirred to react at 50 DEG C, obtains solution B.Potassium permanganate dosage
It is 0.15% of Zn-ef ficiency quality in secondary zinc oxide.
(3) zinc powder is added into solution B, is filtered after being stirred to react at 50 DEG C, obtains solution C.Zinc powder dosage about time oxygen
Change 0.1% of metallic zinc quality in zinc.
(4) Na is added after solution C being warming up to 55 DEG C2CO3Solution obtains liquid phase A after reacting 1h.Substandard products zinc oxide with
Na2CO3Molar ratio be 1:1.2, Na2CO3The mass concentration of solution is 20%.
(5) liquid phase A is filtered with chamber filter press, filter cake is detected with originally water washing to sulfate radical-free.Then will
Filter cake is dried with Rotatingandflashstreamingdrier, after being collected using cyclone collector and cloth bag to desciccate, at 600 DEG C
Lower calcining 1h, obtains active oxidation zinc product.
Atomic spectrum detection is carried out to obtained product, zinc oxide content (after calcination) is 99.6%.It is surveyed through particle size analyzer
Examination, product average grain diameter are 2 μm.Under transmission electron microscope, it can be observed that the particle is 30~80nm by partial size
Grain is reunited.
Embodiment 2
Activated zinc oxide is produced by the following method:
(1) Zn content in this batch of substandard products zinc oxide is tested in advance.Substandard products zinc oxide is added to sulfuric acid solution
In, reaction obtains solution A at 70 DEG C.The molar ratio of substandard products zinc oxide and sulfuric acid is 1:1.5.
(2) potassium permanganate is added into solution A, is filtered after being stirred to react at 60 DEG C, obtains solution B.Potassium permanganate dosage
It is 0.13% of Zn-ef ficiency quality in secondary zinc oxide.
(3) zinc powder is added into solution B, is filtered after being stirred to react at 60 DEG C, obtains solution C.Zinc powder dosage about time oxygen
Change 0.2% of metallic zinc quality in zinc.
(4) Na is added after solution C being warming up to 65 DEG C2CO3Solution obtains liquid phase A after being stirred to react 1h.Substandard products zinc oxide
With Na2CO3Molar ratio be 1:1.5, Na2CO3The mass concentration of solution is 20%.
(5) liquid phase A is filtered with chamber filter press, filter cake is detected with originally water washing to sulfate radical-free.Then will
Filter cake is dried with Rotatingandflashstreamingdrier, after being collected using cyclone collector and cloth bag to desciccate, at 650 DEG C
Lower calcining 0.5h, obtains active oxidation zinc product.
Atomic spectrum detection is carried out to obtained product, zinc oxide content is (after calcination) 99.7%.It is surveyed through particle size analyzer
Examination, particle size are 3 μm.Under transmission electron microscope, it can be observed that the cluster of grains that the particle is 30~80nm by partial size
It is poly- to form.
Embodiment 3
Activated zinc oxide is produced by the following method:
(1) Zn content in this batch of substandard products zinc oxide is tested in advance.Substandard products zinc oxide is added to sulfuric acid solution
In, reaction obtains solution A at 75 DEG C.The molar ratio of substandard products zinc oxide and sulfuric acid is 1:1.
(2) potassium permanganate is added into solution A, is filtered after being stirred to react at 50 DEG C, obtains solution B.Potassium permanganate dosage
It is 0.15% of Zn-ef ficiency quality in secondary zinc oxide.
(3) zinc powder is added into solution B, is filtered after being stirred to react at 50 DEG C, obtains solution C.Zinc powder dosage about time oxygen
Change 0.1% of metallic zinc quality in zinc.
(4) Na is added after solution C being cooled to 45 DEG C2CO3Solution obtains liquid phase A after being stirred to react 0.5h.Substandard products oxidation
Zinc and Na2CO3Molar ratio be 1:1, Na2CO3The mass concentration of solution is 20%.
(5) liquid phase A is filtered with chamber filter press, filter cake is detected with originally water washing to sulfate radical-free.Then will
Filter cake is dried with Rotatingandflashstreamingdrier, after being collected using cyclone collector and cloth bag to desciccate, at 550 DEG C
Lower calcining 1h, obtains active oxidation zinc product.
Atomic spectrum detection is carried out to obtained product, zinc oxide content is (after calcination) 99.2%.It is surveyed through particle size analyzer
Examination, particle size are 4 μm.Under transmission electron microscope, it can be observed that the cluster of grains that the particle is 30~80nm by partial size
It is poly- to form.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (10)
1. a kind of production method of activated zinc oxide, which comprises the following steps:
(1) zinc oxide is added in sulfuric acid solution, reaction obtains solution A；
(2) potassium permanganate is added into the solution A, is filtered after being stirred to react, obtains solution B；
(3) zinc powder is added into the solution B, is filtered after being stirred to react, obtains solution C；
(4) carbonate solution is added into the solution C, liquid phase A is obtained after being stirred to react；
(5) after being successively filtered the liquid phase A, wash, dry, calcining obtains the activated zinc oxide.
2. the zinc oxide is substandard products zinc oxide the method according to claim 1, wherein in step (1),
In contain other metallic elements oxide.
3. according to the method described in claim 2, it is characterized in that, other metallic elements are selected from Pb, Fe, Cu, Cd, Mn's
It is at least one.
4. the method according to claim 1, wherein in step (1), mole of the substandard products zinc oxide and sulfuric acid
Than for 1:(1~1.5).
5. the method according to claim 1, wherein reaction temperature is 60~80 DEG C in step (1).
6. the method according to claim 1, wherein in step (2) according in substandard products zinc oxide Fe and Mn contain
The dosage for determining potassium permanganate is measured, determines the dosage of zinc powder in step (3) according to Cu and Cd content in substandard products zinc oxide.
7. the method according to claim 1, wherein reaction temperature is 40~60 DEG C in step (2) and (3).
8. the method according to claim 1, wherein the carbonate is Na in step (4)2CO3Or K2CO3, institute
The molar ratio for stating substandard products zinc oxide and the carbonate is 1:(1~1.5).
9. the method according to claim 1, wherein in step (5), using Rotatingandflashstreamingdrier to obtaining
Filter cake is dried, and is collected using cyclone collector to desciccate, and calcination temperature is 550~650 DEG C, obtains active oxygen
Change zinc.
10. according to claim 1 to the activated zinc oxide that any one of 9 the methods produce, which is characterized in that the activity
The partial size of zinc oxide is 30~80nm, and specific surface area is 50~80m2/g。
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| CN112028111A (en) * | 2020-08-05 | 2020-12-04 | 衡阳华宏化工实业有限公司 | Production process for preparing active zinc oxide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106241857A (en) * | 2016-08-18 | 2016-12-21 | 江苏万祥锌业有限公司 | A kind of nano zine oxide preparation technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106241857A (en) * | 2016-08-18 | 2016-12-21 | 江苏万祥锌业有限公司 | A kind of nano zine oxide preparation technology |
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| CN112028111A (en) * | 2020-08-05 | 2020-12-04 | 衡阳华宏化工实业有限公司 | Production process for preparing active zinc oxide |
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