CN101823758B - Novel method for producing nanometer grade zinc carbonate and zinc oxide - Google Patents
Novel method for producing nanometer grade zinc carbonate and zinc oxide Download PDFInfo
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- CN101823758B CN101823758B CN201010172445.XA CN201010172445A CN101823758B CN 101823758 B CN101823758 B CN 101823758B CN 201010172445 A CN201010172445 A CN 201010172445A CN 101823758 B CN101823758 B CN 101823758B
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- zinc
- sodium carbonate
- zinc oxide
- carbonate
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Abstract
The invention relates to a novel method for producing nanometer grade zinc carbonate and zinc oxide, which comprises the following process steps: firstly, placing a metered zinc sulfate (ZnSO4) solution with the specific gravity of 30 to 31 baumes into a double decomposition kettle; then, slowly adding a sodium carbonate water solution containing 28 to 30 percent of sodium carbonate (Na2CO3) into the double decomposition kettle in two times after the filtration for forming mixed material pulp mainly containing nanometer grade (the fineness degree reaches 600 to 800 nanometers) basic zinc carbonate (Zn(OH)2.ZnCO3); then, carrying out pressure filtration on the mixed material pulp mainly containing the nanometer grade basic zinc carbonate; using water for washing sulfate radical (SO4<2->) ions in a filter press; then, sending the materials into a drying chamber to be dried; then, using a crushing machine for sending the materials into a rotary flash evaporation drying machine to be calcined; and next, sending the materials into a dust collection chamber to obtain the nanometer grade zinc carbonate (ZnO). Compared with the prior art, the invention has the characteristics of fine fineness degree of the zinc carbonate, large specific surface area, short calcining time, low energy consumption and the like.
Description
Technical field
The present invention relates to a kind of double decomposition and produce the method for zinc carbonate, zinc oxide, particularly a kind of novel method of producing nanometer grade zinc carbonate, zinc oxide.
Background technology
The technique of existing production zinc oxide is: by proportion, be first the zinc sulfate (ZnSO of 30-31 Baume
4) aqueous solution puts into metathesis still, then will be containing sodium carbonate (Na
2cO
3) aqueous sodium carbonate of 28%-30% adds in metathesis still after filtering, and the pH value of the zinc sulfate solution in metathesis still is neutralized to 6.8-7.0, forms that mainly to contain fineness be the zinc subcarbonate (Zn (OH) of 300-800 micron
2.ZnCO
3) mixed slurry, by upper fast mixed slurry press filtration, and in pressure filter, wash sulfate radical (SO
4) after ion, deliver to kiln dry, bake out temperature is 110-140 ℃, do to the zinc subcarbonate of zinc (Zn) content 50-55%, with delivering to calcination in incinerator after crusher in crushing, calcination temperature 450-500 ℃, reaches to content after the zinc oxide (ZnO) of 95-96%, enter in dust chamber, zinc oxide.
Because being adopts one-time reaction to the normal temperature chemical combination technique of current potential pH6.8-7.0, therefore there is following weak point:
1, the molecular structure of zinc subcarbonate is unreasonable: during due to metathesis, aqueous sodium carbonate is disposable joining in metathesis still, and the pH value of the zinc sulfate solution in metathesis still is directly neutralized to 6.8-7.0, cause the zinc subcarbonate (Zn (OH) forming
2.ZnCO
3) molecular structure in the quantity of zinc carbonate molecule more than the quantity of zinc hydroxide molecule, reduced the content of zinc in zinc subcarbonate, cause the molecular lattice of zinc subcarbonate thick, decarburization power consumption time delay;
2, the fineness of zinc oxide is thick, specific surface area is little: due to the bake out temperature low (110-140 ℃) of zinc subcarbonate, when dry, carbonic acid gas is overflowed slow, can not form carbon dioxide sublimes air pressure (carbon dioxide sublimes air pressure plays dissemination when calcining), so the fineness of zinc oxide is thick, specific surface area is little, and use range is restricted;
3, calcination time is grown, consumes energy high: due to the calcination temperature low (450-500 ℃) of zinc subcarbonate, the sublimation temperature of the carbonic acid gas of only considering, do not consider that carbonic acid gas can absorb heat, while causing calcining, the actual temperature of product only has 250-300 ℃, thereby calcination time is long, consume energy high, quality product is affected.
Summary of the invention
The object of the invention is to overcome the above-mentioned deficiency of prior art, and a kind of novel method of producing nanometer grade zinc carbonate, zinc oxide is provided.
Technical scheme of the present invention is: a kind of novel method of producing nanometer grade zinc carbonate, zinc oxide, it comprises following processing step: by the proportion measuring, be first the zinc sulfate (ZnSO of 30-31 Baume
4) aqueous solution puts into metathesis still, then will be containing sodium carbonate (Na
2cO
3) aqueous sodium carbonate of 28%-30% adds in metathesis still after filtering at twice lentamente, forms main containing sodium meter level (fineness reaches 600-800 nanometer) zinc subcarbonate (Zn (OH)
2.ZnCO
3) mixed slurry, then will be mainly containing the mixed slurry press filtration of sodium meter level zinc subcarbonate, and in pressure filter, wash sulfate radical (SO
4) after ion, deliver to kiln dry, then deliver in Rotatingandflashstreamingdrier after calcining with crusher, enter in dust chamber, Nano-class zinc oxide (ZnO).
The further technical scheme of the present invention is: while adding lentamente in metathesis still after for the first time the aqueous sodium carbonate containing sodium carbonate 28%-30% being filtered, in 2-2.5 hour, the pH value of the zinc sulfate solution in metathesis still is neutralized to 6.0, temperature of reaction is controlled at 45-50 ℃, allow it fully break and to attenuate, then put into for the second time the aqueous sodium carbonate containing sodium carbonate 28%-30%, in 30-40 minute, the pH value of solution in metathesis still is neutralized to 6.5-6.8, temperature of reaction is controlled at 60 ± 5 ℃.
The present invention further technical scheme is: deliver to kiln when dry, bake out temperature is 160-200 ℃, is dried to the zinc subcarbonate of zinc (Zn) content 50-60%.
The present invention further technical scheme is: with crusher, deliver to while calcining in Rotatingandflashstreamingdrier, the zinc subcarbonate of flow-like is calcined to 20-50 second in the gas flow tube of temperature 800-900 ℃.
The present invention compared with prior art has following features:
1, the molecular structure of zinc subcarbonate is reasonable: during due to metathesis, aqueous sodium carbonate is to join at twice in metathesis still, reaction minute two stages complete: the first stage is to heat 45-50 ℃ time, pH value is adjusted to 5.0-6.0, and the time is 2-2.5 hour, now CO
2quantity discharged is large, the broken effect of air pressure rising crack initiation; Subordinate phase is that the formation of zinc carbonate is adjusted to 6.8 with pH from 6.0, the time is 30-40 minute, and temperature is carried out at 60 ± 5 ℃, so the zinc subcarbonate (Zn (OH) forming
2.ZnCO
3) molecular structure in the quantity of zinc carbonate molecule be less than the quantity of zinc hydroxide molecule, improved the content of zinc in zinc subcarbonate, cause the molecular lattice of zinc subcarbonate tiny;
2, the fineness of zinc oxide is thin, specific surface area is large: due to the bake out temperature high (160-200 ℃) of zinc subcarbonate, when dry, carbonic acid gas is overflowed fast, form carbon dioxide sublimes air pressure (carbon dioxide sublimes air pressure plays dissemination when calcining), so the fineness of zinc oxide is thin, fineness reaches 50-650 nanometer, and specific surface area is large, reaches 5.5g/m
2, use range is wide, is applicable to desulfurization catalyst, paint, ceramic industry, and price is per ton exceeds 5000-10000 unit, has greatly improved quality product and benefit;
3, calcination time short, consume energy low: the inventive method calcining temperature is 800-900 ℃, and calcination time only needs 20-50 second, has not lightly obtained nanometer superfine product, but also the time that greatly shortened is improved work efficiency.
Below in conjunction with embodiment, detailed content of the present invention is further described.
Embodiment
Produce a novel method for nanometer grade zinc carbonate, zinc oxide, it comprises following processing step: by the proportion measuring, be first the zinc sulfate (ZnSO of 30-31 Baume
4) aqueous solution puts into metathesis still, then will be containing sodium carbonate (Na
2cO
3) aqueous sodium carbonate of 28%-30% adds in metathesis still after filtering lentamente, in 2-2.5 hour, the pH value of the zinc sulfate solution in metathesis still is neutralized to 6.0, temperature of reaction is controlled at 45-50 ℃, allow it fully break and to attenuate, then put into the aqueous sodium carbonate containing sodium carbonate 28%-30%, in 30-40 minute, the pH value of solution in metathesis still is neutralized to 6.5-6.8, temperature of reaction is controlled at 60 ± 5 ℃, forms main containing sodium meter level (fineness reaches 600-800 nanometer) zinc subcarbonate (Zn (OH)
2.ZnCO
3) mixed slurry, and zinc subcarbonate (Zn (OH)
2.ZnCO
3) molecular structure in the quantity of zinc carbonate molecule be greatly less than the quantity of zinc hydroxide molecule, then will be mainly containing the mixed slurry press filtration of sodium meter level zinc subcarbonate, and in pressure filter, wash sulfate radical (SO
4) after ion, deliver to kiln dry, bake out temperature is 160-200 ℃, be dried to the zinc subcarbonate of zinc (Zn) content 50-60%, with crusher, deliver in Rotatingandflashstreamingdrier and calcine, the zinc subcarbonate of flow-like is calcined to 20-50 after second in the gas flow tube of temperature 800-900 ℃, enters in dust chamber, the fineness content that reaches 50-500 nanometer reach 99.7% zinc oxide (ZnO).
Principle of work of the present invention is: the equation of replacement(metathesis)reaction of the present invention is:
2ZnSO
4+2Na
2CO
3+H
2O＝Zn(OH)2·ZnCO
3+co
2↑+2Na
2SO
4
At zinc sulfate (ZnSO
4), sodium carbonate (Na
2cO
3) during metathesis, utilize carbonate (CO
3) resolve into carbonic acid gas (CO
2) time the air pressure timely adjustment current potential and the temperature that produce, split the broken new zinc subcarbonate molecule of forming and form, make zinc subcarbonate (Zn (OH)
2.ZnCO
3) molecular structure in the quantity of zinc carbonate molecule be greatly less than the quantity of zinc hydroxide molecule, obtain the following zinc carbonate product of micron, when calcining decarburization, utilize carbonic acid gas (CO
2) distillation performance, adopt the high-temperature calcination flash distillation broken formation zinc oxide of secondary fissure (ZnO) molecule again, obtain Nano-class zinc oxide product.
Claims (1)
1. a method of producing Nano-class zinc oxide, it comprises following processing step: the zinc sulfate solution that by the proportion measuring is first 30-31 Baume is put into metathesis still, after again the aqueous sodium carbonate containing sodium carbonate 28%-30% being filtered, add in metathesis still, form the main mixed slurry containing nano level zinc subcarbonate, the mixed slurry press filtration of nano level zinc subcarbonate will mainly be contained again, and in pressure filter, wash after sulfate ion, deliver to kiln dry, with crusher, deliver in Rotatingandflashstreamingdrier after calcining again, enter in dust chamber, Nano-class zinc oxide, while adding in metathesis still after it is characterized in that the aqueous sodium carbonate containing sodium carbonate 28%-30% to filter, add lentamente at twice: while adding lentamente in metathesis still after for the first time the aqueous sodium carbonate containing sodium carbonate 28%-30% being filtered, in 2-2.5 hour, the pH value of the zinc sulfate solution in metathesis still is neutralized to 6.0, temperature of reaction is controlled at 45-50 ℃, allow it fully break and to attenuate, then put into for the second time the aqueous sodium carbonate containing sodium carbonate 28%-30%, in 30-40 minute, the pH value of solution in metathesis still is neutralized to 6.5-6.8, temperature of reaction is controlled at 60 ± 5 ℃.
2. the method for production Nano-class zinc oxide according to claim 1, is characterized in that delivering to kiln when dry, and bake out temperature is 160-200 ℃, is dried to the zinc subcarbonate of zinc content 50-60%.
3. the method for production Nano-class zinc oxide according to claim 1 and 2, is characterized in that delivering to while calcining in Rotatingandflashstreamingdrier with crusher, and the zinc subcarbonate of flow-like is calcined to 20-50 second in the gas flow tube of temperature 800-900 ℃.
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| CN201010172445.XA CN101823758B (en) | 2010-05-14 | 2010-05-14 | Novel method for producing nanometer grade zinc carbonate and zinc oxide |
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| CN201010172445.XA CN101823758B (en) | 2010-05-14 | 2010-05-14 | Novel method for producing nanometer grade zinc carbonate and zinc oxide |
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| CN101823758B true CN101823758B (en) | 2014-01-22 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153131B (en) * | 2011-05-19 | 2012-08-01 | 洛阳师范学院 | Preparation method for zinc oxide nano particles |
| CN102531037A (en) * | 2012-01-16 | 2012-07-04 | 沭阳县飞宏金属新材料有限公司 | Chemical preparation method of nanoscale zinc oxide powder |
| CN104671278A (en) * | 2015-02-10 | 2015-06-03 | 济源市鲁泰纳米材料有限公司 | Method for preparing high-activity nano zinc oxide |
| CN105366707A (en) * | 2015-12-14 | 2016-03-02 | 苏州市泽镁新材料科技有限公司 | Preparation method of high-purity zinc carbonate |
| CN106167273B (en) * | 2016-07-07 | 2017-11-14 | 安徽省含山县锦华氧化锌厂 | High-specific area nano zinc oxide preparation method |
| CN109363184A (en) * | 2018-11-08 | 2019-02-22 | 大连工业大学 | The preparation method of nanometer zinc ionophoric in steamed beef soup |
| CN110817934A (en) * | 2019-09-30 | 2020-02-21 | 成都理工大学 | Pyrophyllite loaded nano ZnO composite uvioresistant agent and preparation technology thereof |
| CN115304094B (en) * | 2022-08-23 | 2023-09-05 | 扬州金霞塑胶有限公司 | Method for continuously preparing nano zinc oxide material by carbon dioxide |
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