CN101823758A - 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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- CN101823758A CN101823758A CN 201010172445 CN201010172445A CN101823758A CN 101823758 A CN101823758 A CN 101823758A CN 201010172445 CN201010172445 CN 201010172445 CN 201010172445 A CN201010172445 A CN 201010172445A CN 101823758 A CN101823758 A CN 101823758A
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- zinc
- nanometer grade
- carbonate
- zinc oxide
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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
Existing technology of producing zinc oxide is: be the zinc sulfate (ZnSO of 30-31 Baume with proportion earlier
4) aqueous solution puts into the metathesis still, will contain yellow soda ash (Na again
2CO
3) aqueous sodium carbonate of 28%-30% filters the back and add in the metathesis still, and the pH value of the zinc sulfate solution in the metathesis still is neutralized to 6.8-7.0, formation mainly contains the zinc subcarbonate that fineness is the 300-800 micron (Zn (OH)
2.ZnCO
3) mixed slurry, will go up fast mixed slurry press filtration, and in pressure filter, wash sulfate radical (SO
4) behind the ion, deliver to the kiln drying, bake out temperature is 110-140 ℃, do zinc subcarbonate to zinc (Zn) content 50-55%, with delivering to calcination in the incinerator after the crusher in crushing, calcination temperature 450-500 ℃, reach the zinc oxide (ZnO) of 95-96% to content after, enter in the dust chamber, zinc oxide.
Since be to adopt the normal temperature chemical combination technology of one-time reaction to current potential pH6.8-7.0, so there is following weak point:
1, the molecular structure of zinc subcarbonate is unreasonable: aqueous sodium carbonate is disposable joining in the metathesis still during owing to metathesis, and the pH value of the zinc sulfate solution in the metathesis still directly is neutralized to 6.8-7.0, cause the zinc subcarbonate (Zn (OH) that forms
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 the 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: because the bake out temperature low (110-140 ℃) of zinc subcarbonate, carbonic acid gas is overflowed slow when dry, 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 long, power consumption is high: because the calcination temperature low (450-500 ℃) of zinc subcarbonate, the sublimation temperature of the carbonic acid gas of considering only, do not consider that carbonic acid gas can absorb heat, the actual temperature of product has only 250-300 ℃ when causing calcining, thereby calcination time is long, power consumption is high, and quality product is affected.
Summary of the invention
The objective 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: be the zinc sulfate (ZnSO of 30-31 Baume with the proportion that measures earlier
4) aqueous solution puts into the metathesis still, will contain yellow soda ash (Na again
2CO
3) aqueous sodium carbonate of 28%-30% adds in the metathesis still after filtering at twice lentamente, form mainly to contain sodium meter level (fineness reaches the 600-800 nanometer) zinc subcarbonate (Zn (OH)
2.ZnCO
3) mixed slurry, will mainly contain the mixed slurry press filtration of sodium meter level zinc subcarbonate again, and in pressure filter, wash sulfate radical (SO
4) behind the ion, deliver to the kiln drying, deliver in the Rotatingandflashstreamingdrier after the calcining with crusher again, enter in the dust chamber, Nano-class zinc oxide (ZnO).
The further technical scheme of the present invention is: when adding in the metathesis still lentamente after the aqueous sodium carbonate that will contain for the first time yellow soda ash 28%-30% filters, in 2-2.5 hour, the pH value of the zinc sulfate solution in the metathesis still is neutralized to 6.0, temperature of reaction is controlled at 45-50 ℃, allowing it fully break attenuates, then put into for the second time the aqueous sodium carbonate that contains yellow soda ash 28%-30%, pH value with solution in the metathesis still in 30-40 minute is neutralized to 6.5-6.8, and temperature of reaction is controlled at 60 ± 5 ℃.
The further again technical scheme of the present invention is: when delivering to the kiln drying, 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: deliver to when calcining in the Rotatingandflashstreamingdrier with crusher, the zinc subcarbonate of flow-like is calcined 20-50 second in temperature 800-900 ℃ gas flow tube.
The present invention compared with prior art has following characteristics:
1, the molecular structure of zinc subcarbonate is reasonable: aqueous sodium carbonate is to join at twice in the metathesis still during owing to metathesis, i.e. reaction divides two stages to finish: the fs is to heat 45-50 ℃ the time, the pH value transfers to 5.0-6.0, and the time is 2-2.5 hour, at this moment CO
2Quantity discharged is big, the broken effect of air pressure rising crack initiation; Subordinate phase is that the formation of zinc carbonate transfers 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) that forms
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 the zinc subcarbonate, cause the molecular lattice of zinc subcarbonate tiny;
2, the fineness of zinc oxide is thin, specific surface area is big: because the bake out temperature height (160-200 ℃) of zinc subcarbonate, carbonic acid gas is overflowed fast when dry, 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 the 50-650 nanometer, and specific surface area is big, 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 improved quality product and benefit greatly;
3, calcination time is short, power consumption is low: the inventive method calcining temperature is 800-900 ℃, and calcination time only needs 20-50 second, has not lightly obtained the nanometer superfine product, but also the time that shortened is greatly improved work efficiency.
Below in conjunction with embodiment detailed content of the present invention is further described.
Embodiment
A kind of novel method of producing nanometer grade zinc carbonate, zinc oxide, it comprises following processing step: be the zinc sulfate (ZnSO of 30-31 Baume with the proportion that measures earlier
4) aqueous solution puts into the metathesis still, will contain yellow soda ash (Na again
2CO
3) aqueous sodium carbonate of 28%-30% adds in the metathesis still after filtering lentamente, in 2-2.5 hour, the pH value of the zinc sulfate solution in the metathesis still is neutralized to 6.0, temperature of reaction is controlled at 45-50 ℃, allowing it fully break attenuates, then put into the aqueous sodium carbonate that contains yellow soda ash 28%-30%, pH value with solution in the metathesis still in 30-40 minute is neutralized to 6.5-6.8, temperature of reaction is controlled at 60 ± 5 ℃, forms mainly to contain sodium meter level (fineness reaches the 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 less than the quantity of zinc hydroxide molecule greatly, will mainly contain the mixed slurry press filtration of sodium meter level zinc subcarbonate again, and in pressure filter, wash sulfate radical (SO
4) behind the ion, deliver to the kiln drying, bake out temperature is 160-200 ℃, be dried to the zinc subcarbonate of zinc (Zn) content 50-60%, deliver in the Rotatingandflashstreamingdrier with crusher and to calcine, the zinc subcarbonate of flow-like is calcined 20-50 after second in temperature 800-900 ℃ gas flow tube, enters in the dust chamber, the fineness content that reaches the 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), yellow soda ash (Na
2CO
3) during metathesis, utilize carbonate (CO
3) resolve into carbonic acid gas (CO
2) time air pressure timely adjustment current potential and the temperature that are produced, 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 less than the quantity of zinc hydroxide molecule greatly, obtain the following zinc carbonate product of micron, when the calcining decarburization, utilize carbonic acid gas (CO
2) the distillation performance, adopt the high-temperature calcination flash distillation broken formation zinc oxide of secondary fissure (ZnO) molecule again, obtain the Nano-class zinc oxide product.
Claims (5)
1. produce nanometer grade zinc carbonate for one kind, the novel method of zinc oxide, it comprises following processing step: the zinc sulfate solution that with the proportion that measures is the 30-31 Baume is earlier put into the metathesis still, the aqueous sodium carbonate that will contain yellow soda ash 28%-30% again filters the back and adds in the metathesis still, form the mixed slurry that mainly contains sodium meter level zinc subcarbonate, to mainly contain the mixed slurry press filtration of sodium meter level zinc subcarbonate again, and after in pressure filter, washing sulfate ion, deliver to the kiln drying, after delivering in the Rotatingandflashstreamingdrier calcining with crusher again, enter in the dust chamber, Nano-class zinc oxide.The aqueous sodium carbonate that it is characterized in that containing yellow soda ash 28%-30% filters the back when adding in the metathesis still, adds lentamente at twice.
2. the novel method of production nanometer grade zinc carbonate according to claim 1, zinc oxide is characterized in that will containing yellow soda ash (Na for the first time
2CO
3) when the aqueous sodium carbonate of 28%-30% adds in the metathesis still after filtering lentamente, in 2-2.5 hour, the pH value of the zinc sulfate solution in the metathesis still is neutralized to 6.0, temperature of reaction is controlled at 45-50 ℃, allowing it fully break attenuates, then for the second time put into the aqueous sodium carbonate that contains yellow soda ash 28%-30%, the pH value with solution in the metathesis still in 30-40 minute is neutralized to 6.5-6.8, and temperature of reaction is controlled at 60 ± 5 ℃.
3. the novel method of production nanometer grade zinc carbonate according to claim 1 and 2, zinc oxide, when it is characterized in that delivering to the kiln drying, bake out temperature is 160-200 ℃, is dried to the zinc subcarbonate of zinc (Zn) content 50-60%.
4. the novel method of production nanometer grade zinc carbonate according to claim 1 and 2, zinc oxide, it is characterized in that delivering to when calcining in the Rotatingandflashstreamingdrier, the zinc subcarbonate of flow-like is calcined 20-50 second in temperature 800-900 ℃ gas flow tube with crusher.
5. the novel method of production nanometer grade zinc carbonate according to claim 3, zinc oxide is characterized in that delivering to when calcining in the Rotatingandflashstreamingdrier with crusher, and the zinc subcarbonate of flow-like is calcined 20-50 second in temperature 800-900 ℃ gas flow tube.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153131A (en) * | 2011-05-19 | 2011-08-17 | 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 |
| CN106167273A (en) * | 2016-07-07 | 2016-11-30 | 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 |
| CN115304094A (en) * | 2022-08-23 | 2022-11-08 | 扬州金霞塑胶有限公司 | Method for continuously preparing nano zinc oxide material by using carbon dioxide |
-
2010
- 2010-05-14 CN CN201010172445.XA patent/CN101823758B/en active Active
Non-Patent Citations (1)
| Title |
|---|
| 《铅锌冶金学》 20031231 《铅锌冶金学》编委会 铅锌冶金学 科学出版社 第733-734页 1-5 , * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102153131A (en) * | 2011-05-19 | 2011-08-17 | 洛阳师范学院 | Preparation method for zinc oxide nano particles |
| 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 |
| CN106167273A (en) * | 2016-07-07 | 2016-11-30 | 安徽省含山县锦华氧化锌厂 | High-specific area nano zinc oxide preparation method |
| 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 |
| CN115304094A (en) * | 2022-08-23 | 2022-11-08 | 扬州金霞塑胶有限公司 | Method for continuously preparing nano zinc oxide material by using carbon dioxide |
| 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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| CN101823758B (en) | 2014-01-22 |
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Owner name: LIU SONGLIN Free format text: FORMER OWNER: CHANGNING XIANGJIANG CHEMICAL CO., LTD. Effective date: 20131223 |
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Effective date of registration: 20170330 Address after: 421002 Hunan city of Hengyang province Zhuhui District Jintang river farm gold Jia Ling Kun Thai company Patentee after: HENGYANG KUNTAI CHEMICAL INDUSTRIAL CO., LTD. Address before: 421500 Changning City of Hunan Province Office of Grand Tang tin Peiyuan District No. 108 Patentee before: Liu Songlin |