CN103771489A - Method for preparing nano-zinc oxide from copper smelting dust at low temperature - Google Patents
Method for preparing nano-zinc oxide from copper smelting dust at low temperature Download PDFInfo
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- CN103771489A CN103771489A CN201310720941.8A CN201310720941A CN103771489A CN 103771489 A CN103771489 A CN 103771489A CN 201310720941 A CN201310720941 A CN 201310720941A CN 103771489 A CN103771489 A CN 103771489A
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Abstract
The invention provides a method for preparing nano-zinc oxide from copper smelting dust at a low temperature. The method comprises the steps of soaking the copper smelting dust in a sulfuric acid solution and then taking the clarified zinc sulfate supernatant, regulating and controlling the zinc content of the zinc sulfate solution within the range from 10g/L to 140g/L, and controlling the pH value of the zinc sulfate solution within the range from 4 to 5.5, and then removing impurity with active zinc metal, putting the zinc sulfate solution obtained in the previous steps in a reaction tank filled with a sodium hydroxide NaOH reaction liquid, regulating the pH value of the sodium hydroxide NaOH so that the pH value of the final reaction ranges from 7.5 to 9, and controlling the temperature in the reaction tank in the range from 60 to 95 DEG C and the time of stirring in the reaction tank within the range from 0.5 to 4 hours, next, filtering out and washing, with water, white precipitate obtained in the last step, and removing sodium and sulfates in the reactants to obtain white nano-zinc oxide. The method for preparing the nano-zinc oxide from the copper smelting dust at the low temperature is simple, effective, low in cost and pollution and high in purity.
Description
Technical field
The present invention relates to a kind of method of utilizing copper cigarette ash low temperature preparing nano zinc oxide, belong to the comprehensive utilization of copper metallurgy industry.
Background technology
The present invention uses raw material from enterprise of copper source mill, in copper production process, can produce dedusting ash, because the boiling point of zinc metal is low, zinc molten metal vapour pressure can be evaporated, react with airborne oxygen simultaneously, generate Zinc oxide particles, finally collected and enter in dedusting ash by dust removal installation, in general industry, be called copper cigarette ash.
Zinc oxide (ZnO), is commonly called as zinc white, is a kind of oxide compound of zinc.Be insoluble in water, dissolve in acid and highly basic.Zinc oxide is a kind of conventional chemical additive, is widely used in the making of the products such as glaze, tire, plastics, silicate product, synthetic rubber, lubricating oil, paint, ointment, tackiness agent, food, battery, fire retardant.Band gap and the exciton bind energy of zinc oxide are larger, and transparency is high, have excellent normal temperature tuorbillion to revolve rotary light performance, in the products such as the liquid-crystal display of semiconductor applications, thin film transistor, photodiode, all have application.In addition, the zinc oxide of microparticle also starts to play a role in association area as a kind of nano material.And the grain size of nano zine oxide is interregional between microcosmic particle and macroscopic view, due to surface effects, small-size effect, volume effect and macro quanta tunnel effect etc., during as catalyzer, there is high catalytic activity, also show special physics and chemistry character at aspects such as magnetic, photoabsorption, chemically reactive, thermal resistance, fusing point, solubleness.Therefore, the preparation of nano zine oxide and application have caused people's extensive concern.
The method of purchasing of nano zine oxide has the manufacture method such as Dry chemistry, hydrothermal method, electrochemical process, oxidation style.Dry chemistry is to utilize the compound of Zn (II) to react directly synthetic uniform particles with NaOH mono-step Room Temperature Solid State, and particle diameter is about the ZnO nano powder of 20 nm.This preparation process is by stoichiometric ratio, raw material to be placed in to mortar fully to grind, then with distilled water and the alternately for several times rear seasoning of washing of dehydrated alcohol.Although the method synthetic method is simple, productive rate is high but size distribution is inhomogeneous, easily introduce impurity.Hydrothermal method be by the zinc nitrate solution of 1.0 M by the equivalence ratio of material be 2:1 to add concentration be the urea soln of 1.0 M, one-step synthesis nanometer Zinc oxide powder in reaction under high pressure groove at 110～250 ℃.This method is easy and simple to handle, and raw material is easy to get, but needs pyroreaction.
Summary of the invention
The object of the invention is provides for the deficiencies in the prior art
onekind in low temperature by the method for copper cigarette ash preparing nano zinc oxide.
The processing step of the method for the invention is as follows:
(1) the copper cigarette ash of zinc content 5-50wt% being dipped in to concentration is in 5-40% sulphuric acid soln, and the weight ratio of solid and liquid is 1:1-10, gets its clarification zinc sulfate ZnSO
4upper strata liquid;
(2) by zinc sulfate ZnSO
4solution zinc content regulates and is controlled at 10g/L-140g/L, and zinc sulfate ZnSO4 pH value of solution is controlled to pH=4-5.5;
(3) zinc sulfate ZnSO step (2) being obtained
4solution is placed in the reactive tank that contains active zinc metal, and in reactive tank, temperature is controlled at 40-60 ℃, and churning time 0.5-2 hour in reactive tank gets its clarification zinc sulfate ZnSO
4upper strata liquid;
(4) zinc sulfate ZnSO step (3) being obtained
4solution is placed in the reactive tank that contains sodium hydroxide NaOH reaction solution, regulates the pH value of sodium hydroxide NaOH, makes end reaction pH value for 7.5-9, and in reactive tank, temperature is controlled at 60-90 ℃, and churning time 0.5-4 hour in reactive tank obtains white depositions;
(5) white depositions step (4) being obtained, filters and washes, and removes the soluble salts in reactant, obtains white Nano-class zinc oxide.
Beneficial effect of the present invention: a kind of method by copper cigarette ash low temperature preparing nano zinc oxide of the present invention is simple effectively, cost is low, pollute less, purity is high.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope figure of the white Nano-class zinc oxide prepared of embodiment mono-;
Fig. 2 is the transmission electron microscope figure of the white Nano-class zinc oxide prepared of embodiment bis-.
Embodiment
Embodiment mono-:
(1) the copper cigarette ash of zinc content 5wt% is dipped in sulphuric acid soln (concentration is 5%), the weight ratio of solid and liquid is 1:1-10, gets its clarification zinc sulfate ZnSO
4upper strata liquid;
(2) by zinc sulfate ZnSO
4solution zinc content regulates and is controlled at 10g/L, and by zinc sulfate ZnSO
4pH value of solution is controlled at pH=4;
(3) zinc sulfate ZnSO step (2) being obtained
4solution is placed in the reactive tank that contains active zinc metal, and in reactive tank, temperature is controlled at 40 ℃, and churning time 0.5 hour in reactive tank is got its clarification zinc sulfate ZnSO
4upper strata liquid;
(4) zinc sulfate ZnSO step (3) being obtained
4solution is placed in the reactive tank that contains sodium hydroxide NaOH reaction solution, regulates the pH value of sodium hydroxide NaOH, and making end reaction pH value is 9, and in reactive tank, temperature is controlled at 60 ℃, and in reactive tank, churning time 0.5 hour, obtains white depositions, obtains white depositions;
(5) white depositions step (4) being obtained, filters and washes, and removes the solubility salt in reactant, obtains white Nano-class zinc oxide.
Fig. 1 is the transmission electron microscope figure of the white Nano-class zinc oxide prepared under the present embodiment condition.
Embodiment bis-:
(1) the copper cigarette ash of zinc content 50wt% is dipped in sulphuric acid soln (concentration is 40%), the weight ratio of solid and liquid is 1:10, gets its clarification zinc sulfate ZnSO
4upper strata liquid;
(2) by zinc sulfate ZnSO
4solution zinc content regulates and is controlled at 140g/L, and by zinc sulfate ZnSO
4pH value of solution is controlled at pH=5.5;
(3) zinc sulfate ZnSO step (2) being obtained
4solution is placed in the reactive tank that contains active zinc metal, and in reactive tank, temperature is controlled at 60 ℃, and churning time 4 hours in reactive tank is got its clarification zinc sulfate ZnSO
4upper strata liquid;
(4) zinc sulfate ZnSO step (3) being obtained
4solution is placed in the reactive tank that contains sodium hydroxide NaOH reaction solution, regulates the pH value of sodium hydroxide NaOH, and making end reaction pH value is 7.5, and in reactive tank, temperature is controlled at 90 ℃, and in reactive tank, churning time 4 hours, obtains white depositions;
(5) white depositions step (4) being obtained, filters and washes, and removes the solubility salt in reactant, obtains white Nano-class zinc oxide.
Claims (1)
1. by a method for copper cigarette ash low temperature preparing nano zinc oxide, it is characterized in that:
(1) the copper cigarette ash of zinc content 5-50wt% being dipped in to concentration is in 5-40% sulphuric acid soln, and the weight ratio of solid and liquid is 1:1-10, gets its clarification zinc sulfate ZnSO
4upper strata liquid;
(2) by zinc sulfate ZnSO
4solution zinc content regulates and is controlled at 10g/L-140g/L, and zinc sulfate ZnSO4 pH value of solution is controlled to pH=4-5.5;
(3) zinc sulfate ZnSO step (2) being obtained
4solution is placed in the reactive tank that contains active zinc metal, and in reactive tank, temperature is controlled at 40-60 ℃, and churning time 0.5-2 hour in reactive tank gets its clarification zinc sulfate ZnSO
4upper strata liquid;
(4) zinc sulfate ZnSO step (3) being obtained
4solution is placed in the reactive tank that contains sodium hydroxide NaOH reaction solution, regulates the pH value of sodium hydroxide NaOH, makes end reaction pH value for 7.5-9, and in reactive tank, temperature is controlled at 60-90 ℃, and churning time 0.5-4 hour in reactive tank obtains white depositions;
(5) white depositions step (4) being obtained, filters and washes, and removes the soluble salts in reactant, obtains white Nano-class zinc oxide.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310720941.8A CN103771489A (en) | 2013-12-24 | 2013-12-24 | Method for preparing nano-zinc oxide from copper smelting dust at low temperature |
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| CN201310720941.8A CN103771489A (en) | 2013-12-24 | 2013-12-24 | Method for preparing nano-zinc oxide from copper smelting dust at low temperature |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1033196A (en) * | 1988-10-24 | 1989-05-31 | 营口市有色金属提炼改制厂 | Recovery technique of zinc oxide by treatment of dust during smelting copper from copper ash |
| CN101117719A (en) * | 2007-06-19 | 2008-02-06 | 张如丰 | Formula and process for producing electrolytic zinc by using zinc oxide in copper smelting waste slag |
| CN102325725A (en) * | 2008-12-23 | 2012-01-18 | Posco公司 | Method for preparing high purity zinc oxide using secondary dust |
| WO2012068620A1 (en) * | 2010-11-23 | 2012-05-31 | Metallic Waste Solutions Pty Ltd | Process for recovering zinc and/or zinc oxide ii |
-
2013
- 2013-12-24 CN CN201310720941.8A patent/CN103771489A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1033196A (en) * | 1988-10-24 | 1989-05-31 | 营口市有色金属提炼改制厂 | Recovery technique of zinc oxide by treatment of dust during smelting copper from copper ash |
| CN101117719A (en) * | 2007-06-19 | 2008-02-06 | 张如丰 | Formula and process for producing electrolytic zinc by using zinc oxide in copper smelting waste slag |
| CN102325725A (en) * | 2008-12-23 | 2012-01-18 | Posco公司 | Method for preparing high purity zinc oxide using secondary dust |
| WO2012068620A1 (en) * | 2010-11-23 | 2012-05-31 | Metallic Waste Solutions Pty Ltd | Process for recovering zinc and/or zinc oxide ii |
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Application publication date: 20140507 |