CN104294041A - Technology for preparing activated zinc oxide by using low grade zinc oxide ores - Google Patents
Technology for preparing activated zinc oxide by using low grade zinc oxide ores Download PDFInfo
- Publication number
- CN104294041A CN104294041A CN201310307733.5A CN201310307733A CN104294041A CN 104294041 A CN104294041 A CN 104294041A CN 201310307733 A CN201310307733 A CN 201310307733A CN 104294041 A CN104294041 A CN 104294041A
- Authority
- CN
- China
- Prior art keywords
- zinc
- ammonia
- zinc oxide
- calcination
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a technology for preparing activated zinc oxide by using low grade zinc oxide ores. The activated zinc oxide is prepared through a wet method by using the technology, an appropriate leaching mode and technological parameters in all flows are selected, the technology for processing the low grade zinc oxide ores and preparing the activated zinc oxide has the advantages of high efficiency, cleaning, easy realization, short flow, low energy consumption, easy control of technological conditions, and the like. The technology is suitable for processing like ores, and providing guidance for the alleviation of the insufficiency of the zinc raw material in China and the recycling of the zinc resource. All the indexes of the obtained activated zinc oxide product accord chemical industry standards HG/T2572-2006.
Description
Technical field
The present invention relates to active zinc flower field, be specifically related to the technique that a kind of low-grade zinc oxide ore prepares active zinc flower.
Background technology
Zinc oxide, is commonly called as zinc white, is a kind of important inorganic chemical product.Zinc oxide is widely used in the aspects such as rubber, coating, pottery, chemical industry, medicine, food.Active zinc flower refers generally to the zinc oxide of surperficial activated process, white or micro-yellow powder, spherical in shape.Compare with common zinc oxide, active zinc flower principal feature is: crystallization is thin, particle is little, good dispersity, specific surface are large.The specific surface area of general zinc oxide is at 4-6m2/g, and the specific surface area of active zinc flower is greater than 35m2/g, even can up to 50m2/g.Active zinc flower possesses the features such as granularity is little, specific surface area is large, thus except the character of common zinc oxide and purposes, also has character and the purposes of many uniquenesses, as surface effects, small-size effect and quantum size effect etc.Active zinc flower, as a kind of important artificial powder body material, has important use in fields such as rubber, pottery, coating, oil, medicine and daily-use chemical industries:
In recent years, Chinese scholars has carried out large quantity research to the preparation method of active zinc flower, and main method is as follows:
(1) the alkaline reduction method of organic compound
Useless zinc washes by this method, then mixes with organism, adds alkali lye regulator solution pH value, and mixed with a small amount of sulphur after being heated to high temperature, the active zinc flower obtained can be used for loading material of rubber.
(2) carborization
In the encloses container being full of water vapour and carbonic acid gas, add high pure macroparticle zinc oxide, make zinc oxide be converted into basic carbonate zinc precursor, then washing, dry, calcination, can obtain the active zinc flower that particle diameter is about 0.05um.
(3) zinc oxalate decomposition method
Oxalic acid is all heated to 70 DEG C by with liquor zinci chloridi, then by two kinds of solution mix and blends, zinc oxalate precipitation can be obtained, then wash, dry and calcination under the condition of 400 DEG C, obtain active zinc flower.This method is simple to operate, but shortcoming to be raw materials cost too high, be not suitable for industrial production.
(4) alkaline process
With dilute sulphuric acid or hydrochloric acid leaching zinc gray or cadmia, be reacted in the scope that solution ph is 7-11 with sodium hydroxide solution after leaching liquid purification, then zinc hydroxide precipitation is made active zinc flower.
(5) methyl alcohol and soluble glass method is added
Add NaOH mix and blend after zinc salt is dissolved in the water, add industrial waterglass and methyl alcohol reaction simultaneously, the sedimentation and filtration of generation, washing, drying are obtained active zinc flower.Gained active zinc flower particle is used for vulcanization rate being made to improve about 2 times in rubber industry.
(6) method for making of bigger serface active zinc flower
Alkaline carbonate or alkali metal hydroxide and zinc salt react in the solution, are precipitated thing spraying dry at 450-900 DEG C, can obtain the active zinc flower of tap density 400-600g/L and specific surface area 100-130m2/g.
(7) ammonium bicarbonate method
The method adopts dilute sulphuric acid leaching various containing zinc raw material, obtains solution of zinc sulfate.Adopt zinc dust precipitation except the impurity such as de-iron, manganese, the solution of zinc sulfate after purification coordinates with ammoniacal liquor and bicarbonate of ammonia and generates zinc ammonia complex under stirring at room temperature condition.Heating ammonia still process can obtain precursor zinc subcarbonate, zinc subcarbonate precipitation after filtration, washing, at high temperature carry out calcination after drying and decompose and obtain active zinc flower.The method use cheap bicarbonate of ammonia and ammoniacal liquor, so cost is lower, be easy to realize industrialization.
(8) sodium carbonate method
Zinc sulfate or liquor zinci chloridi are added in certain density sodium carbonate solution, generate zinc subcarbonate precipitation.Then filter, wash, dry, calcination obtains active zinc flower.Carbonic acid gas containing trace in product and the moisture of about 1%.
Current domestic active zinc flower production method has direct method, indirect method and wet method.The raw materials for production of direct method are enrichment zinc ore, its unstable product quality; Indirect method is raw material mainly with zinc ingot metal, and cost is too high, develops limited.
In recent years, China's zinc ore resource provisioning growing tension, and the capacity and output of zinc metal increases substantially.Along with a large amount of exploitations of zinc ore, its grade constantly declines, foreign matter content increases gradually, and the sustainable development of China's smelting Zn Cr coating faces increasingly serious challenge.Therefore, active development utilizes the various zinc resource zinc oxide ore tool that especially grade is lower to be of great significance.
The present invention adopts low-grade zinc oxide ore to be raw material, prepares active zinc flower by wet-leaching, has selected the processing parameter in suitable Leaching way and each flow process, the effect achieved.
Summary of the invention
For the deficiencies in the prior art, an object of the present invention is to provide a kind of low-grade zinc oxide ore to prepare the technique of active zinc flower.Described technique prepares active zinc flower by wet-leaching, select the processing parameter in suitable Leaching way and each flow process, prepare the technique of active zinc flower for a kind of process low-grade zinc oxide ore that is efficient, clean, that easily realize, there is the advantages such as flow process is short, energy consumption is low, technical qualification are easy to control.This technique is applicable to process similar ore, for alleviating China zinc insufficient raw material, realizes zinc resource recycle and provides guidance.The active oxidation zinc product indices obtained all meets chemical industry standard HG/T2572-2006.
Present invention employs following technical scheme:
Low-grade zinc oxide ore prepares a technique for active zinc flower, comprises following operation: two sections of ammonia leachings; Purification; Ammonia still process, ageing, calcination;
Wherein, two sections of ammonia soaking technologies are: ammonia concn 6.5-7.5mo1/L, NH
4hCO
3concentration 0.58-0.66mo1/L, extraction temperature 45-55 DEG C, extraction time 2.5-3.5h, sample ore granularity-80 order, liquid-solid ratio 4.5-5.5:1.
Wherein, purification process is: adopt zinc powder reduction, zinc powder consumption 0.9-1.1g/L, reaction times 1.5-2.5h, temperature of reaction 25-35 DEG C.
Wherein, ammonia still process, ageing, calcination process are: ammonia still process temperature 110-130 DEG C, time of ammonia distillation 1.5-2.5h, digestion time 8-12min, calcination temperature 330-370 DEG C, calcination time 0.5h.
Described low grade oxidation ore composition (mass percentage/%): 11.81Zn, 0.15Pb, 0.008Cu, 0.038Cd, 4.8TFe, 0.5FeO, 2.68SiO
2, 0.084TiO
2, 1.05A1
2o
3, 30.32CaO, 7.88MgO, 0.057MnO, 0.096K
2o, 0.53Na
2o, 3.1S, 0.016P, 8.86C, other are 30.97 years old.
In described mineral, zinc is mainly with smithsonite (ZnCO
3) and lapis calaminaris (Zn
4si
2o
7(OH)
2h
2o) form exists.
Preferred processing condition are as follows:
Wherein, two sections of ammonia soaking technologies are: ammonia concn 7mo1/L, NH
4hCO
3concentration 0.62mo1/L, extraction temperature 50 DEG C, extraction time 3h, sample ore granularity-80 order, liquid-solid ratio 5:1.The leaching yield of one section of Leaching Zinc is 79.1%, and leaching slag zinc content is 3.26%; Two sections of Leaching Zinc leaching yields are 80.3%, and leaching slag zinc content is 0.67%, and total leaching yield reaches 95.9%.
Wherein, purification process is: adopt zinc powder reduction, zinc powder consumption 1.00g/L, reaction times 2h, temperature of reaction 30 DEG C.
Wherein, ammonia still process, ageing, calcination process are: ammonia still process temperature 120 DEG C, time of ammonia distillation 2.0h, digestion time 10min, calcination temperature 350 DEG C, calcination time 0.5h.
The present invention has the following advantages: the present invention determines a kind of process low-grade zinc oxide ore that is efficient, clean, that easily realize and prepares the technique of active zinc flower, has the advantages such as flow process is short, energy consumption is low, technical qualification are easy to control.This technique is applicable to process similar ore, for alleviating China zinc insufficient raw material, realizes zinc resource recycle and provides guidance.The active oxidation zinc product indices obtained all meets chemical industry standard HG/T2572-2006.
Embodiment
For ease of understanding the present invention, it is as follows that the present invention enumerates embodiment.Those skilled in the art should understand, described embodiment is only help to understand the present invention, should not be considered as concrete restriction of the present invention.
Embodiment one
Low grade oxidation ore composition (mass percentage/%): 11.81Zn, 0.15Pb, 0.008Cu, 0.038Cd, 4.8TFe, 0.5FeO, 2.68SiO
2, 0.084TiO
2, 1.05A1
2o
3, 30.32CaO, 7.88MgO, 0.057MnO, 0.096K
2o, 0.53Na
2o, 3.1S, 0.016P, 8.86C, other are 30.97 years old.
In mineral, zinc is mainly with smithsonite (ZnCO
3) and lapis calaminaris (Zn
4si
2o
7(OH)
2h
2o) form exists.
The technique that low-grade zinc oxide ore prepares active zinc flower comprises following operation: two sections of ammonia leachings; Purification; Ammonia still process, ageing, calcination;
Two sections of ammonia soaking technologies are: ammonia concn 7mo1/L, NH
4hCO
3concentration 0.62mo1/L, extraction temperature 50 DEG C, extraction time 3h, sample ore granularity-80 order, liquid-solid ratio 5:1.The leaching yield of one section of Leaching Zinc is 79.1%, and leaching slag zinc content is 3.26%; Two sections of Leaching Zinc leaching yields are 80.3%, and leaching slag zinc content is 0.67%, and total leaching yield reaches 95.9%.
Purification process is: adopt zinc powder reduction, zinc powder consumption 1.00g/L, reaction times 2h, temperature of reaction 30 DEG C.
Ammonia still process, ageing, calcination process are: ammonia still process temperature 120 DEG C, time of ammonia distillation 2.0h, digestion time 10min, calcination temperature 350 DEG C, calcination time 0.5h.
The active oxidation zinc product indices obtained all meets chemical industry standard HG/T2572-2006.
Embodiment two
Low grade oxidation ore composition (mass percentage/%): 11.81Zn, 0.15Pb, 0.008Cu, 0.038Cd, 4.8TFe, 0.5FeO, 2.68SiO
2, 0.084TiO
2, 1.05A1
2o
3, 30.32CaO, 7.88MgO, 0.057MnO, 0.096K
2o, 0.53Na
2o, 3.1S, 0.016P, 8.86C, other are 30.97 years old.
In mineral, zinc is mainly with smithsonite (ZnCO
3) and lapis calaminaris (Zn
4si
2o
7(OH)
2h
2o) form exists.
The technique that low-grade zinc oxide ore prepares active zinc flower comprises following operation: two sections of ammonia leachings; Purification; Ammonia still process, ageing, calcination;
Two sections of ammonia soaking technologies are: ammonia concn 6.5mo1/L, NH4HCO3 concentration 0.58mo1/L, extraction temperature 45 DEG C, extraction time 2.5h, sample ore granularity-80 order, liquid-solid ratio 4.5:1.
Purification process is: adopt zinc powder reduction, zinc powder consumption 0.9g/L, reaction times 1.5h, temperature of reaction 25 DEG C.
Ammonia still process, ageing, calcination process are: ammonia still process temperature 110 DEG C, time of ammonia distillation 1.5h, digestion time 8min, calcination temperature 330 DEG C, calcination time 0.5h.
The active oxidation zinc product indices obtained all meets chemical industry standard HG/T2572-2006.
Embodiment three
Low grade oxidation ore composition (mass percentage/%): 11.81Zn, 0.15Pb, 0.008Cu, 0.038Cd, 4.8TFe, 0.5FeO, 2.68SiO
2, 0.084TiO
2, 1.05A1
2o
3, 30.32CaO, 7.88MgO, 0.057MnO, 0.096K
2o, 0.53Na
2o, 3.1S, 0.016P, 8.86C, other are 30.97 years old.
In mineral, zinc is mainly with smithsonite (ZnCO
3) and lapis calaminaris (Zn
4si
2o
7(OH)
2h
2o) form exists.
The technique that low-grade zinc oxide ore prepares active zinc flower comprises following operation: two sections of ammonia leachings; Purification; Ammonia still process, ageing, calcination;
Wherein, two sections of ammonia soaking technologies are: ammonia concn 7.5mo1/L, NH4HCO3 concentration 0.66mo1/L, extraction temperature 55 DEG C, extraction time 3.5h, sample ore granularity-80 order, liquid-solid ratio 5.5:1.
Wherein, purification process is: adopt zinc powder reduction, zinc powder consumption 1.1g/L, reaction times 2.5h, temperature of reaction 35 DEG C.
Wherein, ammonia still process, ageing, calcination process are: ammonia still process temperature 130 DEG C, time of ammonia distillation 2.5h, digestion time 12min, calcination temperature 330-370 DEG C, calcination time 0.5h.
The active oxidation zinc product indices obtained all meets chemical industry standard HG/T2572-2006.
Applicant states, the present invention illustrates detailed process equipment and process flow process of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned detailed process equipment and process flow process, namely do not mean that the present invention must rely on above-mentioned detailed process equipment and process flow process and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (6)
1. low-grade zinc oxide ore prepares a technique for active zinc flower, comprises following operation: two sections of ammonia leachings; Purification; Ammonia still process, ageing, calcination;
Wherein, two sections of ammonia soaking technologies are: ammonia concn 6.5-7.5mo1/L, NH
4hCO
3concentration 0.58-0.66mo1/L, extraction temperature 45-55 DEG C, extraction time 2.5-3.5h, sample ore granularity-80 order, liquid-solid ratio 4.5-5.5:1;
Wherein, purification process is: adopt zinc powder reduction, zinc powder consumption 0.9-1.1g/L, reaction times 1.5-2.5h, temperature of reaction 25-35 DEG C;
Wherein, ammonia still process, ageing, calcination process are: ammonia still process temperature 110-130 DEG C, time of ammonia distillation 1.5-2.5h, digestion time 8-12min, calcination temperature 330-370 DEG C, calcination time 0.5h.
2. technique according to claim 1, described low grade oxidation ore composition (mass percentage/%): 11.81Zn, 0.15Pb, 0.008Cu, 0.038Cd, 4.8TFe, 0.5FeO, 2.68SiO
2, 0.084TiO
2, 1.05A1
2o
3, 30.32CaO, 7.88MgO, 0.057MnO, 0.096K
2o, 0.53Na
2o, 3.1S, 0.016P, 8.86C, other are 30.97 years old.
3. technique according to claim 1, in described mineral, zinc is mainly with smithsonite (ZnCO
3) and lapis calaminaris (Zn
4si
2o
7(OH)
2h
2o) form exists.
4. technique according to claim 1, wherein, two sections of ammonia soaking technologies are: ammonia concn 7mo1/L, NH
4hCO
3concentration 0.62mo1/L, extraction temperature 50 DEG C, extraction time 3h, sample ore granularity-80 order, liquid-solid ratio 5:1.
5. technique according to claim 1, wherein, purification process is: adopt zinc powder reduction, zinc powder consumption 1.00g/L, reaction times 2h, temperature of reaction 30 DEG C.
6. technique according to claim 1, wherein, ammonia still process, ageing, calcination process are: ammonia still process temperature 120 DEG C, time of ammonia distillation 2.0h, digestion time 10min, calcination temperature 350 DEG C, calcination time 0.5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310307733.5A CN104294041A (en) | 2013-07-19 | 2013-07-19 | Technology for preparing activated zinc oxide by using low grade zinc oxide ores |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310307733.5A CN104294041A (en) | 2013-07-19 | 2013-07-19 | Technology for preparing activated zinc oxide by using low grade zinc oxide ores |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104294041A true CN104294041A (en) | 2015-01-21 |
Family
ID=52313986
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310307733.5A Pending CN104294041A (en) | 2013-07-19 | 2013-07-19 | Technology for preparing activated zinc oxide by using low grade zinc oxide ores |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104294041A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106115767A (en) * | 2015-12-09 | 2016-11-16 | 李果 | A kind of method of zinc oxide ore comprehensive utilization |
| CN106115768A (en) * | 2015-10-05 | 2016-11-16 | 李果 | A kind of comprehensive cyclic utilization method of steel plant zinc smoke ash |
| WO2020019823A1 (en) * | 2018-07-24 | 2020-01-30 | 重庆东群科技有限公司 | Method for producing calcium zincate |
-
2013
- 2013-07-19 CN CN201310307733.5A patent/CN104294041A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106115768A (en) * | 2015-10-05 | 2016-11-16 | 李果 | A kind of comprehensive cyclic utilization method of steel plant zinc smoke ash |
| CN106115767A (en) * | 2015-12-09 | 2016-11-16 | 李果 | A kind of method of zinc oxide ore comprehensive utilization |
| WO2020019823A1 (en) * | 2018-07-24 | 2020-01-30 | 重庆东群科技有限公司 | Method for producing calcium zincate |
| US11247913B2 (en) | 2018-07-24 | 2022-02-15 | Chongqing Dongqun Technology Co., Ltd. | Method for producing calcium zincate |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103922416B (en) | A kind of method of Separation and Recovery iron from red mud | |
| CN104152687B (en) | Aluminium, vanadium, molybdenum, the production technology of nickel element three-waste free discharge are extracted from black shale | |
| CN103342394B (en) | Method for continuously preparing cobalt hydroxide with high bulk density | |
| CN102616824A (en) | Method for preparing ultrafine high-whiteness active barite powder | |
| CN108767218A (en) | A kind of post-processing approach that battery is prepared with nickel cobalt aluminium hydroxide | |
| CN102390870A (en) | Preparation method of superfine iron oxide red pigment with high glossiness and pure red tone | |
| CN108728899A (en) | A method of purity calcium carbonate whisker is mixed with using circulating mother liquor pressurization spray | |
| CN102126736A (en) | Method for preparing nano-calcium carbonate powder by using soluble carbonate | |
| CN102703982B (en) | Method for preparing magnesium carbonate trihydrate crystal whisker by utilizing serpentine | |
| CN107140671B (en) | A kind of nanometer calcium carbonate powder and preparation method thereof | |
| CN104762474A (en) | Method for preparing ammonium molybdate through molybdenite | |
| CN104294041A (en) | Technology for preparing activated zinc oxide by using low grade zinc oxide ores | |
| CN103318976B (en) | A kind of technique being prepared tricobalt tetroxide by cobalt-carrying solution | |
| CN103145194B (en) | A kind of method utilizing by-product of white titanium pigment to prepare iron oxide yellow | |
| CN109399594A (en) | A kind of cleaning method of mid low grade phosphate rock powder | |
| US20150218338A1 (en) | Method for Producing Nanometer Lithopone from Electrolytic Zinc Acid Leaching Residue | |
| CN102825058B (en) | Method for recycling calcium sulfate waste residues generated in titanium dioxide acidic waste water | |
| CN111847518A (en) | Efficient recycling method of silicomanganese slag | |
| CN110817935A (en) | Method for preparing high-purity zinc oxide by utilizing zinc renewable resources | |
| CN103771546B (en) | Process for continuously producing nickel hydroxide by using pickle liquor of nickel laterite ore | |
| CN110255591A (en) | The method of phosphorus ore de-magging co-production magnesium carbonate and calcium carbonate | |
| CN108862372A (en) | A method of nano zine oxide and compound of calcium carbonate are produced using containing zinc ore crude | |
| CN106636632B (en) | A kind of method that normal pressure decomposes wolframite or Scheelite-Wolframite Mixed Mine in alkaline system | |
| CN109321747B (en) | Method for leaching manganese concentrate from low-grade calciummanganese ore and regenerating leaching medium | |
| CN108754140A (en) | A method of it is produced containing zinc complexes using containing zinc ore crude |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150121 |