CN106277031A - Solvent extraction method prepares the method for Zinc oxide powder - Google Patents
Solvent extraction method prepares the method for Zinc oxide powder Download PDFInfo
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- CN106277031A CN106277031A CN201610606634.0A CN201610606634A CN106277031A CN 106277031 A CN106277031 A CN 106277031A CN 201610606634 A CN201610606634 A CN 201610606634A CN 106277031 A CN106277031 A CN 106277031A
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- zinc oxide
- oxide powder
- ammonia
- method preparing
- leachate
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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
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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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 present invention relates to the method that solvent extraction method prepares Zinc oxide powder, it includes adding in ammonia spirit Second-rate zinc oxide powder leaching；Drip ammonium bicarbonate solution again to leach, then filter, obtain leachate；Again leachate is carried out remove impurity, filtration；Solid after filtering first washs with ammonia spirit, then uses dehydrated alcohol drip washing；Then carry out being aged, sucking filtration, obtain presoma；Presoma is dried, calcines, obtain nanometer Zinc oxide powder.The present invention uses ammonia and ammonium bicarbonate solution that Second-rate zinc oxide powder carries out substep and leaches, and then by techniques such as washing, calcinings, prepares nano-scale oxidized zinc powder；The method not only technological process is shorter, and equipment investment is less, and significant for improving the economic worth of Second-rate zinc oxide powder.
Description
Technical field
The present invention relates to oxide powder and zinc preparation.
Background technology
Zinc oxide is a kind of new and high technology material of discovered in recent years, and being that only a few is several can realize quantum size effect
Oxide semiconductor material.Traditional zinc oxide material is widely used in pottery, piezoelectric transducer, catalyst and luminous organ
The fields such as part.Along with the further investigation of nano zine oxide preparation technology, the super-refinement of zinc oxide particles so that it is present tradition oxygen
Change property not available for zinc, such as nontoxic and non-migratory, fluorescence, piezoelectricity, absorption and scatters ultraviolet ability etc.,
Thus have broad application prospects.
For the application of nano-powder, its dispersibility and stability are most important.But owing to nano particle diameter is little,
Specific surface area is big, and interface atoms number is many, there is a large amount of unsaturated bond and dangling bond, and chemism is high, adds intergranular model moral
Hua Li, electrostatic force and surface tension etc., easily make nano-particle form larger-size aggregate.Nano powder after reunion
Body, has excellent specific property by the many losing himself so that it is usefulness cannot give full play to, and also will have a strong impact on nano-powder
Use value and application prospect.At present, the technology of preparing of Zinc oxide powder is varied, but big multiple process routes is long, investment
Greatly, and Zinc oxide powder particle diameter is relatively big, is difficult to meet the demand of nano material.
Summary of the invention
For above-mentioned technical problem, the present invention provides a kind of and invests solvent extraction method little, that technological process is shorter and prepare zinc oxide
The method of powder body.
The technical solution used in the present invention is: solvent extraction method prepares the method for Zinc oxide powder, and it comprises the following steps:
(1) Second-rate zinc oxide powder is added in ammonia spirit leach；
(2) drip ammonium bicarbonate solution again to leach, then filter, obtain leachate；
(3) again leachate is carried out remove impurity, filtration；
(4) solid after filtering first washs with ammonia spirit, then uses dehydrated alcohol drip washing；
(5) then carry out being aged, sucking filtration, obtain presoma；
(6) presoma is dried, calcines, obtain nanometer Zinc oxide powder.
As preferably, when using ammonia to leach, the concentration of ammonia spirit is 8 10mol/L, and extraction time is 0.5
1.5h, extraction temperature is 25 35 DEG C.
As preferably, the concentration of ammonium hydrogencarbonate is 1 1.5mol/L, is added dropwise to complete in 10-20min, drips bicarbonate
1 1.5h is leached again after ammonia.
As preferably, in leachate, zinc ion is 1:(5 7 with the ratio of the amount of the material of ammonium ion).
As preferably, remove impurity uses sulfuration ammonia.
As preferably, during washing, ammonia spirit adds 0.5wt% surfactant.
As preferably, digestion time is 50 70min.
As preferably, temperature when presoma is dried is 70 90 DEG C.
As preferably, temperature during calcining is 400 500 DEG C, and the time is 80 100min.
As can be known from the above technical solutions, the present invention use ammonia and ammonium bicarbonate solution Second-rate zinc oxide powder is carried out substep soak
Go out, then by techniques such as washing, calcinings, prepare nano-scale oxidized zinc powder；The method not only technological process is shorter, equipment
Invest less, and significant for improving the economic worth of Second-rate zinc oxide powder.
Detailed description of the invention
The present invention is described more detail below, and illustrative examples and explanation in this present invention are used for explaining the present invention,
But it is not as a limitation of the invention.
Solvent extraction method prepares the method for Zinc oxide powder, and it comprises the following steps:
(1) first being added in ammonia spirit by Second-rate zinc oxide powder and leach, the concentration of ammonia spirit is 8 10mol/L, leaches
Time is 0.5 1.5h, and extraction temperature is 25 35 DEG C, thus the zinc hydroxide nucleus that can generate and thin crystalline substance；Drip carbonic acid again
Hydrogen ammonia solution leaches；Wherein the concentration of ammonium hydrogencarbonate is 1 1.5mol/L, is added dropwise to complete in 10-20min, drips carbon
1 1.5h is leached again after acid hydrogen ammonia；Use above-mentioned concentration, can separate out rapidly so that substantial amounts of zinc hydroxide crystal seed, cause molten
Matter concentration reduces rapidly, thus obtains the most tiny granule；In implementation process, ammonium bicarbonate solution should be in 10-20min
It is added dropwise to complete, it is to avoid interparticle coagulation is grown up.
(2) then filtering, obtain leachate, in leachate, zinc ion is 1:(5 with the ratio of the amount of the material of ammonium ion
7), excess of ammonia ion makes the pH value that leachate holding is bigger, is conducive to the carrying out leached, and leaching rate can bring up to 99.3%
Left and right；Leachate carries out remove impurity, filtration, and remove impurity uses sulfuration ammonia, can remove the impurity in Second-rate zinc oxide powder leaching process, remove
Miscellaneous effect is notable.
(3) solid after filtering first washs with ammonia spirit, then uses dehydrated alcohol drip washing；The pH value of ammonia spirit is
10 11, use this pH value, the absolute value of presoma grain surface current potential increases, and repulsive force increases, thus dispersibility improves, and makes
Obtain particle diameter to diminish；Washing process the most just removes the process of foreign ion, is also to manage to reduce the mistake reunited between granule simultaneously
Journey.When using ammonia scrubbing, the electric charge on precursor compound surface moves due to the existence of ion concentration difference, needs certain time
Can be only achieved balance；And during dehydrated alcohol drip washing, owing to absorption water and constitution water exist with capillary form, ethanol dilution adsorbs
Water and destruction constitution water reach poised state and need also exist for certain time；Therefore, can reduce and reunite between granule.During washing,
Adding 0.5wt%PAA surfactant in ammonia spirit, it has dispersion effect to lead compound, and its dispersion effect is to make
Particle surface produces protective layer.
(4) then carry out being aged, sucking filtration, obtain presoma；Digestion time is 50 70min, and ageing contributes to protective layer
Formation and reinforcing；Finally being dried by presoma, calcine, obtain nanometer Zinc oxide powder, temperature when presoma is dried is
70 90 DEG C, temperature during calcining is 400 500 DEG C, and the time is 80 100min.Being dried to make the particle diameter of product become more
Little, calcining can make basic zinc carbonate decompose, and reaches the Zinc oxide particles of relatively small particle.
Embodiment 1
First being added in ammonia spirit by Second-rate zinc oxide powder and leach, the concentration of ammonia spirit is 8mol/L, and extraction time is
0.5h, extraction temperature is 25 DEG C；Drip ammonium bicarbonate solution again to leach；Wherein the concentration of ammonium hydrogencarbonate is 1mol/L,
It is added dropwise to complete in 10min, after dropping ammonium hydrogencarbonate, leaches 1.5h again；Then filter, zinc ion and the thing of ammonium ion in leachate
The ratio of the amount of matter is 1:5, then leachate uses sulfuration ammonia carry out remove impurity, filtration, and pH value first used by the solid after then filtering
It is the ammonia spirit washing of 10, ammonia spirit adds 0.5wt%PAA surfactant, then uses dehydrated alcohol drip washing；The oldest
Change 50min, then sucking filtration, obtain presoma；Presoma is dried with 70 DEG C, at temperature is 400 DEG C, then calcines 80min,
Obtain Zinc oxide particles.The total recovery recording zinc reaches 92.1%, and the particle diameter of Zinc oxide particles is 31.5nm.
Embodiment 2
First being added in ammonia spirit by Second-rate zinc oxide powder and leach, the concentration of ammonia spirit is 9mol/L, and extraction time is
1h, extraction temperature is 30 DEG C；Drip ammonium bicarbonate solution again to leach；Wherein the concentration of ammonium hydrogencarbonate is 1.5mol/L,
It is added dropwise to complete in 15min, after dropping ammonium hydrogencarbonate, leaches 1.5h again；Then filter, zinc ion and the thing of ammonium ion in leachate
The ratio of the amount of matter is 1:6, then leachate uses sulfuration ammonia carry out remove impurity, filtration, and pH value first used by the solid after then filtering
It is the ammonia spirit washing of 10.8, ammonia spirit adds 0.5wt%PAA surfactant, then uses dehydrated alcohol drip washing；Then
Ageing 60min, then sucking filtration, obtain presoma；Presoma is dried with 80 DEG C, then calcines at temperature is 450 DEG C
90min, obtains Zinc oxide particles.The total recovery recording zinc reaches 93.8%, and the particle diameter of Zinc oxide particles is 20.4nm.
Embodiment 3
First being added in ammonia spirit by Second-rate zinc oxide powder and leach, the concentration of ammonia spirit is 10mol/L, and extraction time is
1.5h, extraction temperature is 35 DEG C；Drip ammonium bicarbonate solution again to leach；Wherein the concentration of ammonium hydrogencarbonate is 1.5mol/L,
It is added dropwise to complete in 20min, after dropping ammonium hydrogencarbonate, leaches 1h again；Then filter, zinc ion and the thing of ammonium ion in leachate
The ratio of the amount of matter is 1:7, and leachate is using sulfuration ammonia carry out remove impurity, filtration, and pH value first used by the solid after then filtering
It is the ammonia spirit washing of 11, ammonia spirit adds 0.5wt%PAA surfactant, then uses dehydrated alcohol drip washing；The oldest
Change 70min, then sucking filtration, obtain presoma；Presoma is dried with 90 DEG C, at temperature is 500 DEG C, then calcines 100min,
Obtain Zinc oxide particles.The total recovery recording zinc reaches 92.6%, and the particle diameter of Zinc oxide particles is 25.3nm.
The technical scheme provided the embodiment of the present invention above is described in detail, specific case used herein
Principle and embodiment to the embodiment of the present invention are set forth, and the explanation of above example is only applicable to help to understand this
The principle of inventive embodiments；Simultaneously for one of ordinary skill in the art, according to the embodiment of the present invention, in specific embodiment party
All will change in formula and range of application, in sum, this specification content should not be construed as limitation of the present invention.
Claims (9)
1. the method that solvent extraction method prepares Zinc oxide powder, it comprises the following steps:
(1) Second-rate zinc oxide powder is added in ammonia spirit leach；
(2) drip ammonium bicarbonate solution again to leach, then filter, obtain leachate；
(3) again leachate is carried out remove impurity, filtration；
(4) solid after filtering first washs with ammonia spirit, then uses dehydrated alcohol drip washing；
(5) then carry out being aged, sucking filtration, obtain presoma；
(6) presoma is dried, calcines, obtain nanometer Zinc oxide powder.
The method preparing Zinc oxide powder the most according to claim 1, it is characterised in that: when using ammonia to leach, ammonia is molten
The concentration of liquid is 8 10mol/L, and extraction time is 0.5 1.5h, and extraction temperature is 25 35 DEG C.
The method preparing Zinc oxide powder the most as claimed in claim 1, it is characterised in that: the concentration of ammonium hydrogencarbonate is 1
1.5mol/L, is added dropwise to complete in 10-20min, leaches 1 1.5h again after dropping ammonium hydrogencarbonate.
The method preparing Zinc oxide powder the most as claimed in claim 1, it is characterised in that: zinc ion and ammonium ion in leachate
The ratio of the amount of material is 1:(5 7).
The method preparing Zinc oxide powder the most as claimed in claim 1, it is characterised in that: remove impurity uses sulfuration ammonia.
The method preparing Zinc oxide powder the most as claimed in claim 1, it is characterised in that: during washing, add in ammonia spirit
0.5wt% surfactant.
The method preparing Zinc oxide powder the most as claimed in claim 1, it is characterised in that: digestion time is 50 70min.
The method preparing Zinc oxide powder the most as claimed in claim 1, it is characterised in that: temperature when presoma is dried is 70
90℃。
The method preparing Zinc oxide powder the most as claimed in claim 1, it is characterised in that: temperature during calcining is 400 500
DEG C, the time is 80 100min.
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| CN201610606634.0A CN106277031A (en) | 2016-07-29 | 2016-07-29 | Solvent extraction method prepares the method for Zinc oxide powder |
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| CN201610606634.0A CN106277031A (en) | 2016-07-29 | 2016-07-29 | Solvent extraction method prepares the method for Zinc oxide powder |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1210813A (en) * | 1998-07-24 | 1999-03-17 | 山西省稷山县福利化工厂 | Alkaline process for producing active zinc oxide |
| CN1270144A (en) * | 2000-04-30 | 2000-10-18 | 杨国华 | Process for preparing high-purity active zinc oxide by immersing in ammonia water and ammonium carbonate solution and complexing |
| CN1616354A (en) * | 2003-11-14 | 2005-05-18 | 湘潭大学 | Uniformly coordinating precipitation method for preparing nano zinc oxide |
| CN102863007A (en) * | 2012-09-25 | 2013-01-09 | 四川巨宏科技有限公司 | Method for producing high-purity nano-zinc oxide by ammonia method using electrolytic zinc acid-leaching residues |
-
2016
- 2016-07-29 CN CN201610606634.0A patent/CN106277031A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1210813A (en) * | 1998-07-24 | 1999-03-17 | 山西省稷山县福利化工厂 | Alkaline process for producing active zinc oxide |
| CN1270144A (en) * | 2000-04-30 | 2000-10-18 | 杨国华 | Process for preparing high-purity active zinc oxide by immersing in ammonia water and ammonium carbonate solution and complexing |
| CN1616354A (en) * | 2003-11-14 | 2005-05-18 | 湘潭大学 | Uniformly coordinating precipitation method for preparing nano zinc oxide |
| CN102863007A (en) * | 2012-09-25 | 2013-01-09 | 四川巨宏科技有限公司 | Method for producing high-purity nano-zinc oxide by ammonia method using electrolytic zinc acid-leaching residues |
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Application publication date: 20170104 |