CN105268963A - Method for decreasing granularity of zinc powder produced with alkaline process - Google Patents
Method for decreasing granularity of zinc powder produced with alkaline process Download PDFInfo
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- CN105268963A CN105268963A CN201510662882.2A CN201510662882A CN105268963A CN 105268963 A CN105268963 A CN 105268963A CN 201510662882 A CN201510662882 A CN 201510662882A CN 105268963 A CN105268963 A CN 105268963A
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Abstract
The invention relates to a method for decreasing the granularity of zinc powder produced with an alkaline process. Zinc-contained waste serves as raw materials, a strong alkaline solution is used in the alkaline process for leaching, and leach liquid is purified; polyethylene glycol and Twain are added into the leach liquid; and zinc electrolysis is carried out on the solution; after electrolysis is stopped, the zinc powder is taken out immediately, absolute ethyl alcohol and deionized waterare used for washing in sequence until the pH of the washing liquid is neutral, and the high-purity fine-particle zinc powder is obtained after vacuum drying is carried out, wherein additives have no adverse effects on the electrolytic process, the current efficiency is still higher than 97%, operation is simple, the product granularity is small, and quality is stable.
Description
Technical field
The invention belongs to the high-valued recovery field containing zinc in zinc refuse, relate to a kind of thin zinc powder is prepared in utilization method containing zinc refuse, be specially a kind of method that alkaline process production zinc powder particle size is diminished.
Background technology
Along with the remarkable achievement acquired by more than ten years in past three China's economy, the large scale mining of various mineral not only causes Mineral Resources in China exhausted trend in various degree, but also has caused the environmental problem more and more received publicity.It is reported, the static state of the current zinc reserves of China ensures the time limit only about 8.8 years, and rich ore is fewer and feweri, and exploitation difficulty is increasing.Therefore the recycling of secondary zinc resource just seems ever more important.Secondary zinc resource mainly come from the industrial process such as mining, zinc abstraction, plating, battery, steel-making, copper metallurgy produce a large amount of containing zinc mine tailing, flue dust, mud, waste residue etc., the zinc containing certain grade and enormous amount.
At present, there is the method utilizing sulfide base release agent to realize the selective Quantitative Separation of plumbous zinc in alkali lye electrolysis process, alkaline process electrolytic zinc powder technique is made to give full play to the suitability for industrialized production that alkaline process advantage achieves zinc powder, but this flow process utilizes the zinc powder particle diameter produced containing zinc refuse bigger than normal, the zinc powder proportion that particle diameter is less than 150 μm (crossing 100 mesh sieves) only has 10%-30%, specific area is relatively little, active low, on market, to be greater than the zinc powder price of 150 μm low for particle diameter, need to sell through levigate processing further, cost becomes large, seriously constrain and utilize this technique high-valued recovery secondary zinc resource.
Summary of the invention
The present invention is in order to solve in actual production, and alkali process utilizes containing the thicker problem of zinc refuse electrolytic preparation gained zinc powder particle size, and provide a kind of method that alkaline process production zinc powder particle size is diminished, the method technique is simple, products obtained therefrom steady quality.
The present invention is achieved by the following technical solutions: a kind of method that alkaline process production zinc powder particle size is diminished, and its processing step is:
1) to contain zinc refuse for raw material, in alkali process, strong base solution is utilized to leach and purify leachate;
2) in scavenging solution, polyethylene glycol and tween is added;
3) above-mentioned solution is carried out to the electrolysis of zinc, electrode insertion in the solution, positive and negative electrode distance between plates 1 ~ 10cm, temperature 0 ~ 70 DEG C, logical direct current electrolysis, current density is 800 ~ 1500A/m
2;
4) after stopping electrolysis, take out zinc powder immediately, utilize the successively cleaning of absolute ethyl alcohol and deionized water to be neutral to cleaning fluid pH, after vacuum drying, namely obtain high-purity fine grained zinc powder.
When described polyethylene glycol is liquid, its addition is volume fraction 0.002% ~ 0.015%, and when described polyethylene glycol is solid-state, its addition is 10mg/L ~ 150mg/L.
The volume fraction of described tween is 0.002% ~ 0.015%.
The anode of described battery lead plate is corrosion resistant plate, and negative electrode is the alloy sheets containing magnalium.
Described electrolysis time is 2min ~ 60min.
Theoretical according to classical crystallization nucleation, zinc crystallization process comprises the formation of zinc nucleus and growing up of zinc nucleus, and the crystallization nucleation process of zinc belongs to instantaneous nucleation, and electro-deposition is just starting in a period of time, and ion reduction nucleation can be represented by following relational expression:
N＝N
0[1-exp(-At)]
In formula: N-be distributed in unitized electrode instantaneous nucleation number of loci on the surface;
N
0the number of densities of-corresponding wherein avtive spot;
The velocity constant of A-single nucleation site stable state nucleation;
T-crystallization time;
In conjunction with this formula, in experimentation, after adding polyethylene glycol and tween in electrolyte, matched curve peak width strengthens, and nucleation rate is faster, and this illustrates that the polyethylene glycol of low concentration and tween coupling can activate alkali zinc ion, change the Potential distribution near electrode surface, reduce the nucleating surface energy of electrode reaction ion in alkali zinc solution, make alkali zinc ion easier in electrode surface nucleation, the number of densities N of corresponding avtive spot
0increase, namely electrode active surface nucleation site N increases, and nucleation rate is accelerated, and is far longer than the growth rate of nucleus, finally makes ripe zinc crystalline particle diminish and attenuate.
Ratio that zinc powder particle diameter is less than 150 μm is not less than 80% to utilize method of the present invention to obtain, be up to 99.82%, great refinement zinc powder particle diameter, increase specific area and the activity of Direct Electrolysis gained zinc powder, improve the value of Direct Electrolysis gained zinc powder, eliminate further mechanical grinding step; The zinc powder proportion that wherein particle diameter is less than 45 μm (cross 325 mesh sieves) has been up to 52.94%, directly can meet the requirement of national standard primes after screening.
The invention has the beneficial effects as follows: a kind of method that alkaline process production zinc powder particle size is diminished, additive does not wherein have adverse effect to electrolytic process, and current efficiency is still up to more than 97%, simple to operate, and products obtained therefrom particle diameter is little, steady quality.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further described.
Accompanying drawing 1 is the comparison diagram of gained zinc powder of the present invention and the pure zinc powder of commercially available top grade.
Accompanying drawing 2 is the particle size distribution figure of the embodiment of the present invention 1.
Accompanying drawing 3 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 1 gained zinc powder.
Accompanying drawing 4 is the particle size distribution figure of the embodiment of the present invention 2.
Accompanying drawing 5 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 2 gained zinc powder.
Accompanying drawing 6 is the particle size distribution figure of the embodiment of the present invention 3.
Accompanying drawing 7 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 3 gained zinc powder.
Detailed description of the invention
Embodiment one
With Jiangsu steel plant zinc smoke for object, after highly basic leaches and purifies, then according to the present invention, in scavenging solution, add volume fraction be 0.005% liquid polyethylene glycol and volume fraction is the tween of 0.005%, polar plate spacing 3cm, temperature 25 DEG C, logical direct current electrolysis, current density is 800A/m
2.Electrolysis time 10min, take out zinc powder immediately, utilize the successively cleaning of absolute ethyl alcohol and deionized water to cleaning fluid pH in neutral, namely high-purity fine grained zinc powder is obtained after vacuum drying, wherein zinc powder particle diameter is less than the ratio of 150 μm for (99.82%), is less than the ratio of 45 μm for (52.94%).
Embodiment two
With Hebei steel plant zinc smoke for object, after highly basic leaches and purifies, then according to the present invention, in scavenging solution, add volume fraction be 50mg/L solid polyethylene glycol and volume fraction is the tween of 0.015%, polar plate spacing 3cm, temperature 60 C, logical direct current electrolysis, current density is 1000A/m
2.Electrolysis time 20min, take out zinc powder immediately, utilize the successively cleaning of absolute ethyl alcohol and deionized water to cleaning fluid pH in neutral, namely high-purity fine grained zinc powder is obtained after vacuum drying, wherein zinc powder particle diameter is less than the ratio of 150 μm for (82.44%), is less than the ratio of 45 μm for (35.62%).
Embodiment three
With Hebei steel plant zinc smoke for object, after highly basic leaches and purifies, then according to the present invention, in scavenging solution, add volume fraction be 100mg/L solid polyethylene glycol and volume fraction is the tween of 0.010%, polar plate spacing 5cm, temperature 25 DEG C, logical direct current electrolysis, current density is 1000A/m
2.Electrolysis time 30min, take out zinc powder immediately, utilize absolute ethyl alcohol and washed with de-ionized water to cleaning fluid pH in neutral, namely high-purity fine grained zinc powder is obtained after vacuum drying, wherein zinc powder particle diameter is less than the ratio of 150 μm for (97.44%), is less than the ratio of 45 μm for (37.33%).
By example of the present invention, original production present situation is obtained zinc powder and the pure spherical zinc powder of commercially available top grade directly, zinc flake national standard primes parameter is compared and can be found out: greatly improve thin zinc particle degree in the product by the present invention, reduce the production cost of the thin zinc powder of high added value, substantially increase the specific area of zinc powder simultaneously, with under equigranular condition being approximately 10 times of the pure spherical zinc powder specific area of commercially available top grade, product reactivity strengthens, full Zn content, metallic zinc content and apparent density all meet zinc flake Standard, this technique whole process does not have grease to participate in, grease is not had to generate yet, therefore grease is not contained in product, additive add the electrolytic efficiency (see table one) not reducing production process.
Table one
Claims (6)
1. make the method that alkaline process production zinc powder particle size diminishes, it is characterized in that, its processing step is:
1) to contain zinc refuse for raw material, in alkali process, strong base solution is utilized to leach and purify leachate;
2) in scavenging solution, polyethylene glycol and tween is added;
3) above-mentioned solution is carried out to the electrolysis of zinc, electrode insertion in the solution, positive and negative electrode distance between plates 1 ~ 10cm, temperature 0 ~ 70 DEG C, logical direct current electrolysis, current density is 800 ~ 1500A/m
2;
4) after stopping electrolysis, take out zinc powder immediately, utilize the successively cleaning of absolute ethyl alcohol and deionized water to be neutral to cleaning fluid pH, after vacuum drying, namely obtain high-purity fine grained zinc powder.
2. a kind of method that alkaline process production zinc powder particle size is diminished according to claim 1, it is characterized in that, when described polyethylene glycol is liquid, its addition is volume fraction 0.002% ~ 0.015%, when described polyethylene glycol is solid-state, its addition is 10mg/L ~ 150mg/L.
3. a kind of method that alkaline process production zinc powder particle size is diminished according to claim 1, it is characterized in that, the volume fraction of described tween is 0.002% ~ 0.015%.
4. a kind of method that alkaline process production zinc powder particle size is diminished according to claim 1, it is characterized in that, the anode of described battery lead plate is corrosion resistant plate, and negative electrode is the alloy sheets containing magnalium.
5. a kind of method that alkaline process production zinc powder particle size is diminished according to claim 1, it is characterized in that, described electrolysis time is 2min ~ 60min.
6. zinc powder prepared by a kind of according to right 1 ~ 5 any one claim alkaline process is produced method that zinc powder particle size diminishes, is characterized in that, the ratio that described zinc powder particle diameter is less than 150 μm is 80% ~ 99.82%; The ratio that zinc powder particle diameter is less than 45 μm is up to 52.94%.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11246988A (en) * | 1997-10-29 | 1999-09-14 | Sogepass | Method for conditioning material powder obtained by electrodeposition in basic medium |
| CN101969144A (en) * | 2010-08-20 | 2011-02-09 | 华南师范大学 | Alkaline zinc battery cathode electrolyte and preparation method and application thereof |
| CN102181886A (en) * | 2011-04-08 | 2011-09-14 | 同济大学 | Method for producing one-dimensional nanometer flake zinc powder by directly electrolyzing strong alkaline solution |
| CN102776532A (en) * | 2012-07-18 | 2012-11-14 | 同济大学 | Method for preparing ultrafine zinc powder by adding aluminum-containing compound alkaline liquor through electrolysis |
| CN103938229A (en) * | 2014-04-10 | 2014-07-23 | 同济大学 | Method for preparing ultrafine flake zinc powder by adding antimony compound alkali liquor to electrolyze |
-
2015
- 2015-10-14 CN CN201510662882.2A patent/CN105268963A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH11246988A (en) * | 1997-10-29 | 1999-09-14 | Sogepass | Method for conditioning material powder obtained by electrodeposition in basic medium |
| CN101969144A (en) * | 2010-08-20 | 2011-02-09 | 华南师范大学 | Alkaline zinc battery cathode electrolyte and preparation method and application thereof |
| CN102181886A (en) * | 2011-04-08 | 2011-09-14 | 同济大学 | Method for producing one-dimensional nanometer flake zinc powder by directly electrolyzing strong alkaline solution |
| CN102776532A (en) * | 2012-07-18 | 2012-11-14 | 同济大学 | Method for preparing ultrafine zinc powder by adding aluminum-containing compound alkaline liquor through electrolysis |
| CN103938229A (en) * | 2014-04-10 | 2014-07-23 | 同济大学 | Method for preparing ultrafine flake zinc powder by adding antimony compound alkali liquor to electrolyze |
Non-Patent Citations (3)
| Title |
|---|
| 冯绍彬等: "电解液中有机添加剂对锌电极性能的影响", 《化学研究与应用》 * |
| 张承龙等: "含锌危险废物碱法再生锌的生命周期评价", 《环境工程》 * |
| 蒋家超，赵由才: "碱法炼锌生产中锌粉返溶问题及其影响因素", 《有色冶金设计与研究》 * |
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