CN103145176A - High-activity empty frame zinc oxide production method by means of industrial zinciferous smoke dust - Google Patents
High-activity empty frame zinc oxide production method by means of industrial zinciferous smoke dust Download PDFInfo
- Publication number
- CN103145176A CN103145176A CN2013100417316A CN201310041731A CN103145176A CN 103145176 A CN103145176 A CN 103145176A CN 2013100417316 A CN2013100417316 A CN 2013100417316A CN 201310041731 A CN201310041731 A CN 201310041731A CN 103145176 A CN103145176 A CN 103145176A
- Authority
- CN
- China
- Prior art keywords
- zinc
- empty frame
- industrial
- ammonia
- zinc oxide
- 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.)
- Granted
Links
Abstract
The invention discloses a high-activity zinc oxide production method by means of industrial zinciferous smoke dust, and relates to a high-activity nanometer empty frame zinc oxide preparation method which comprises the following steps: (1) mixing, stirring and heating industrial ammonia, reclaimed ammonia, ammonium bicarbonate, water, and industrial zinciferous smoke dust; (2) converting zinc in the step (1) into zinc ammonia complex which is dissolved in water; (3) obtaining qualified zinc ammonia complex purged liquid through purification steps such as oxidization deferrization and demanganization, and reduction heavy metal removing; (4) constructing an empty frame by adding constructing materials, stilling ammonia for adsorption of zinc carbonate and zinc hydroxide, and forming empty-frame-structured basic zinc carbonate; (5) and obtaining high-activity nanometer empty frame zinc oxide through calcining. The high-activity empty frame zinc oxide production method by means of the industrial zinciferous smoke dust has the advantages of being capable of recycling industrial wastes and easily controlling the technological process, low in cost, high in product activity and stable in performance.
Description
Technical field:
The present invention relates to the preparation method of the empty frame zinc oxide of a kind of high-activity nano, particularly a kind of method of utilizing industrial zinc smoke and specific empty frame core to manufacture the empty frame zinc oxide of high-activity nano.
Background technology:
Zinc oxide is the requisite additive of rubber and tire industry, also can make vulcanization leveller and strengthening agent and the painted Ji of natural rubber, synthetic rubber and latex.Nano zine oxide is used for rubber industry can give full play to the sulfuration promoter action, improves the performance of rubber, and its consumption is only the 30%-50% of common zinc oxide.
Summary of the invention:
The purpose of this invention is to provide a kind of method of utilizing industrial zinc smoke to produce the empty frame zinc oxide of high reactivity, its raw material sources is extensive, and technical process is simple, need not complex apparatus, cost is low, Product Activity is high.In the process of producing empty frame zinc ammonia complex, adopt effective catalyst, make Product Activity higher.
In order to solve the existing problem of background technology, the present invention adopts following production method:
1) the industrial zinc smoke of choosing wide material sources belongs to industrial waste and recycles, clean environment firendly as main raw material.
2) coordinate appropriate recovery ammoniacal liquor, bicarbonate of ammonia, industrial ammonia, tap water to mix by a certain percentage dosing industrial zinc smoke, leach under 50 ℃ of-60 ℃ of conditions, obtain thick leaching liquid.
3) with step 2) the thick leaching liquid that obtains filters, under the condition of 50 ℃-60 ℃,
Oxidizer is with Fe
2+Be oxidized to Fe
3+, stroke Fe(OH)
3Colloidal precipitation is filtered.
4) leaching liquid that step 3) is obtained adds purificant under 50 ℃ of-60 ℃ of conditions, the impurity such as removing heavy metals obtain containing the qualified leaching liquids such as Pb, Cd, As, Cu, Ni, Co, Sb, filters.
5) the qualified leaching liquid that step 4) is obtained, this place chooses calcium hydroxide as the empty frame of core for the particular case that is fit to the rubber industry use, content according to zinc oxide wherein coordinates appropriate calcium hydroxide and sucrose, carry out the ammonia still process crystallization, filter, obtain sky frame zinc subcarbonate.The ammonia that wherein is evaporated and CO
2Mixture is recycled ammoniacal liquor through collection, returns to step 2) leach recycling, realize recycling of material.
6) solubility salt impurity is wherein removed in the empty frame zinc subcarbonate pure water rinsing that step 5) is obtained.Obtain the qualified empty frame zinc subcarbonate of the water solubles.
7) the qualified empty frame zinc subcarbonate that step 6) is obtained through 600 ℃ of quick burnings, is collected, and obtains the empty frame nano zine oxide of qualified high reactivity.
Described recovery ammonia concn is 12% left and right, and industrial ammonia is 18% left and right, and bicarbonate of ammonia is agricultural level bicarbonate of ammonia, and nitrogen content is 17% left and right, and water is tap water; Reaction times is 2 hours.
Oxygenant in described step 3 is potassium permanganate, and the reaction times is 30 minutes.
Purificant in described step 4 is zinc powder, and the reaction times is 1 hour.
Empty frame core in described step 5 is various inorganicss and organism, and Heating temperature is that 1 standard atmosphere is depressed 100 ℃, and under other pressure, temperature is suitably adjusted, and keeping the solution slight boiling condition is purpose.The heating terminal point be in solution zinc content lower than 0.2g/l.
The zinc oxide activity that the present invention has overcome the traditional method manufacturing is low, metallic zinc content is high, so that the high shortcoming of heavy metal loss speed in rubber item afterwards, effectively reduce the content of metallic zinc, but improved simultaneously the activity of zinc oxide, under the prerequisite that ensures the rubber indices, reached the purpose that reduces heavy metal in the rubber item that uses this product, and then reduction heavy metal loss speed, the purpose of environmental protection have been realized.
The present invention has following beneficial effect:
1) take Industrial fumes as raw material, belong to the secondary recovery utilization of resource, clean environment firendly is the recycling economy that country advocates, and obtains the support of national departments concerned.Raw material sources are extensive, and are alternative large.Auxiliary material belongs to general chemical raw material, wide material sources, low price.
2) adopt the main process of basic solution wet-leaching, equipment requirements is simple, and equipment corrosion is little, and the various foreign matter contents of product are low, and except incidental expense is cheap, process control is easy, makes that the finished product stability is high, quality good.
3) adopt the calcining of low temperature flash, calcining temperature is low, and equipment corrosion is little, and process is easy to control, dispersed number of the finished product, and specific surface area is large, and is active high.
Outstanding advantages of the present invention is to improve the activity of empty frame zinc oxide, effectively reduces cost, and will to hang down be the content of heavy metal, has reached the purpose of clean environment firendly.
Embodiment:
Embodiment 1: this embodiment by the following technical solutions: with ammoniacal liquor 623.7ml proportioning bicarbonate of ammonia 67g, strong aqua 300ml, strong aqua contains NH
3Be 14.084%, contain CO
3 2-Be 6.1%.Tap water 85ml adds the Industrial fumes of 212g sweat zinc 59.2%.Be heated with stirring to 55 ℃, insulation reaction 2 hours is filtered, is cleaned filter mud, obtains containing the solution 934ml of zinc 157.2g/l, and the rate of recovery is 94.01%.
Embodiment 2: the 934ml solution that obtains in embodiment 1 is added 0.24g potassium permanganate, be incubated 50 ℃ of stirring reactions 30 minutes, filter the solution 926ml that obtains iron content 7ppm.
Embodiment 3: will add the 1g zinc powder in the 926ml solution that obtain in embodiment 2, be incubated 50 ℃ of stirring reactions 1 hour, filter the solution 918ml that obtains leaded 6ppm.
Embodiment 4: the scavenging solution 918ml that obtains in embodiment 3 is placed in the 1800ml beaker, add tap water 300ml, stir, 76.9g calcium hydroxide is slowly evenly added wherein, make calcium hydroxide disperse fully, do not unite, add sucrose 0.8g, heated and boiled, keep little boiling, the gas that produces reclaims with condenser, and in little process of boiling, keeping liquid volume wherein is the 1250ml left and right.With the gas that the PH detection paper volatilizes, when gas pH value to be volatilized is 7, stop boiling.
Embodiment 5: well-done material liquid mixture in embodiment 4 is filtered, clean filter mud with pure water, obtain moistening filter mud 479g.Detecting moisture is 35.3%.The ammoniacal liquor of collecting is detected, be recycled ammoniacal liquor 921ml, wherein contain NH
3Be 10.1265%, CO
3 2-Be 9.286%.
Embodiment 6: the filter mud that obtains in embodiment 5 through 600 ℃ of calcinings 30 minutes, is obtained the empty frame nano zine oxide of high reactivity 234.67g.It is 50.2% that detection wherein contains zinc, and leaded is 43ppm, and containing manganese is 6ppm, and cupric is 3ppm, and containing cadmium is 21ppm, and the water solubles is 0.08%, and hydrochloric acid insoluble substance is 0.02%.
Claims (5)
1. method of utilizing industrial zinc smoke to produce the empty frame zinc oxide of high reactivity is characterized in that its production method is:
1) the industrial zinc smoke of choosing wide material sources belongs to industrial waste and recycles, clean environment firendly as main raw material;
2) coordinate appropriate recovery ammoniacal liquor, bicarbonate of ammonia, industrial ammonia, tap water to mix by a certain percentage dosing industrial zinc smoke, leach under 50 ℃ of-60 ℃ of conditions, obtain thick leaching liquid;
3) with step 2) the thick leaching liquid that obtains filters, under the condition of 50 ℃-60 ℃,
Oxidizer is with Fe
2+Be oxidized to Fe
3+, stroke Fe(OH)
3Colloidal precipitation is filtered;
4) leaching liquid that step 3) is obtained adds purificant under 50 ℃ of-60 ℃ of conditions, the impurity such as removing heavy metals obtain containing the qualified leaching liquids such as Pb, Cd, As, Cu, Ni, Co, Sb, filters;
5) the qualified leaching liquid that step 4) is obtained, this place chooses calcium hydroxide as the empty frame of core for the particular case that is fit to the rubber industry use, content according to zinc oxide wherein coordinates appropriate calcium hydroxide and sucrose, carry out the ammonia still process crystallization, filter, obtain sky frame zinc subcarbonate; The ammonia that wherein is evaporated and CO
2Mixture is recycled ammoniacal liquor through collection, returns to step 2) leach recycling, realize recycling of material;
6) solubility salt impurity is wherein removed in the empty frame zinc subcarbonate pure water rinsing that step 5) is obtained; Obtain the qualified empty frame zinc subcarbonate of the water solubles;
7) the qualified empty frame zinc subcarbonate that step 6) is obtained through 600 ℃ of quick burnings, is collected, and obtains the empty frame nano zine oxide of qualified high reactivity.
2. a kind of method of utilizing industrial zinc smoke to produce the empty frame zinc oxide of high reactivity according to claim 1, it is characterized in that described recovery ammonia concn is 12% left and right, industrial ammonia is 18% left and right, and bicarbonate of ammonia is agricultural level bicarbonate of ammonia, nitrogen content is 17% left and right, and water is tap water; Reaction times is 2 hours.
3. a kind of method of utilizing industrial zinc smoke to produce the empty frame zinc oxide of high reactivity according to claim 1, is characterized in that the oxygenant in described step 3 is potassium permanganate, and the reaction times is 30 minutes.
4. a kind of method of utilizing industrial zinc smoke to produce the empty frame zinc oxide of high reactivity according to claim 1, is characterized in that the purificant in described step 4 is zinc powder, and the reaction times is 1 hour.
5. a kind of method of utilizing industrial zinc smoke to produce the empty frame zinc oxide of high reactivity according to claim 1, it is characterized in that the empty frame core in described step 5 is various inorganicss and organism, Heating temperature is that 1 standard atmosphere is depressed 100 ℃, under other pressure, temperature is suitably adjusted, and keeping the solution slight boiling condition is purpose; The heating terminal point be in solution zinc content lower than 0.2g/l.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310041731.6A CN103145176B (en) | 2013-02-04 | 2013-02-04 | High-activity empty frame zinc oxide production method by means of industrial zinciferous smoke dust |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310041731.6A CN103145176B (en) | 2013-02-04 | 2013-02-04 | High-activity empty frame zinc oxide production method by means of industrial zinciferous smoke dust |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103145176A true CN103145176A (en) | 2013-06-12 |
| CN103145176B CN103145176B (en) | 2015-07-08 |
Family
ID=48543564
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310041731.6A Expired - Fee Related CN103145176B (en) | 2013-02-04 | 2013-02-04 | High-activity empty frame zinc oxide production method by means of industrial zinciferous smoke dust |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103145176B (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103663541A (en) * | 2013-11-15 | 2014-03-26 | 洛阳市蓝天化工科技有限公司 | Method for preparing high-efficiency zinc oxide complex by using ammonia-ammonium method |
| CN103818945A (en) * | 2013-11-15 | 2014-05-28 | 洛阳市蓝天化工科技有限公司 | Production method of efficient zinc oxide |
| 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 |
| CN108046307A (en) * | 2017-12-18 | 2018-05-18 | 东北大学 | A kind of waste water extraction zinc of iron content containing zinc and the method for preparing zinc oxide |
| CN110468287A (en) * | 2019-08-26 | 2019-11-19 | 中南大学 | A method of utilize flue dust containing manganese to make catalyst for separation of iron in goethite form |
| WO2020019834A1 (en) * | 2018-07-24 | 2020-01-30 | 重庆东群科技有限公司 | Mineral processing method for low-grade zinc-containing raw ore |
| WO2020019854A1 (en) * | 2018-07-24 | 2020-01-30 | 重庆东群科技有限公司 | Method for producing zinc oxide by means of double leaching |
| WO2020019777A1 (en) * | 2018-07-24 | 2020-01-30 | 重庆东群科技有限公司 | Method for producing zinc-containing complex or zinc oxide using zinc-containing raw ore via intermediate step for synthesis of calcium zincate |
| CN112125327A (en) * | 2020-09-23 | 2020-12-25 | 衡阳市大宇锌业有限公司 | Preparation process of active zinc oxide |
| CN112299471A (en) * | 2020-11-25 | 2021-02-02 | 中南大学 | Method for synchronously preparing nano zinc oxide by efficiently separating zinc from zinc-containing electronic waste |
| CN112408460A (en) * | 2020-12-10 | 2021-02-26 | 平江县吉成科技有限责任公司 | Preparation method of nano zinc oxide |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045956A (en) * | 1989-03-27 | 1990-10-10 | 吉林市金刚化工厂 | Produce zinc subcarbonate and active zinc flower with ammonium bicarbonate precipitation method |
| US6423281B2 (en) * | 1999-06-22 | 2002-07-23 | Allan S. Myerson | Method for reducing the formation of Zn(NH4)4Cl2 from ZnO/NH4Cl solutions |
| CN101643236A (en) * | 2009-09-11 | 2010-02-10 | 赵月华 | Production of zinc oxide by ammonia water circulation method |
-
2013
- 2013-02-04 CN CN201310041731.6A patent/CN103145176B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045956A (en) * | 1989-03-27 | 1990-10-10 | 吉林市金刚化工厂 | Produce zinc subcarbonate and active zinc flower with ammonium bicarbonate precipitation method |
| US6423281B2 (en) * | 1999-06-22 | 2002-07-23 | Allan S. Myerson | Method for reducing the formation of Zn(NH4)4Cl2 from ZnO/NH4Cl solutions |
| CN101643236A (en) * | 2009-09-11 | 2010-02-10 | 赵月华 | Production of zinc oxide by ammonia water circulation method |
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103663541A (en) * | 2013-11-15 | 2014-03-26 | 洛阳市蓝天化工科技有限公司 | Method for preparing high-efficiency zinc oxide complex by using ammonia-ammonium method |
| CN103818945A (en) * | 2013-11-15 | 2014-05-28 | 洛阳市蓝天化工科技有限公司 | Production method of efficient zinc oxide |
| CN103818945B (en) * | 2013-11-15 | 2016-01-20 | 洛阳市蓝天化工科技有限公司 | A kind of production method of efficient oxidation zinc |
| CN103663541B (en) * | 2013-11-15 | 2016-05-11 | 洛阳市蓝天化工科技有限公司 | Ammonia azanium method is prepared the method for efficient oxidation zinc complex |
| 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 |
| CN108046307A (en) * | 2017-12-18 | 2018-05-18 | 东北大学 | A kind of waste water extraction zinc of iron content containing zinc and the method for preparing zinc oxide |
| WO2020019834A1 (en) * | 2018-07-24 | 2020-01-30 | 重庆东群科技有限公司 | Mineral processing method for low-grade zinc-containing raw ore |
| WO2020019854A1 (en) * | 2018-07-24 | 2020-01-30 | 重庆东群科技有限公司 | Method for producing zinc oxide by means of double leaching |
| WO2020019777A1 (en) * | 2018-07-24 | 2020-01-30 | 重庆东群科技有限公司 | Method for producing zinc-containing complex or zinc oxide using zinc-containing raw ore via intermediate step for synthesis of calcium zincate |
| CN110468287A (en) * | 2019-08-26 | 2019-11-19 | 中南大学 | A method of utilize flue dust containing manganese to make catalyst for separation of iron in goethite form |
| CN110468287B (en) * | 2019-08-26 | 2020-05-15 | 中南大学 | Method for removing iron by goethite method by using manganese-containing smoke dust as catalyst |
| CN112125327A (en) * | 2020-09-23 | 2020-12-25 | 衡阳市大宇锌业有限公司 | Preparation process of active zinc oxide |
| CN112125327B (en) * | 2020-09-23 | 2023-09-29 | 衡阳市大宇锌业有限公司 | Preparation process of active zinc oxide |
| CN112299471A (en) * | 2020-11-25 | 2021-02-02 | 中南大学 | Method for synchronously preparing nano zinc oxide by efficiently separating zinc from zinc-containing electronic waste |
| CN112299471B (en) * | 2020-11-25 | 2022-02-15 | 中南大学 | Method for synchronously preparing nano zinc oxide by efficiently separating zinc from zinc-containing electronic waste |
| CN112408460A (en) * | 2020-12-10 | 2021-02-26 | 平江县吉成科技有限责任公司 | Preparation method of nano zinc oxide |
| CN112408460B (en) * | 2020-12-10 | 2022-09-13 | 平江县吉成科技有限责任公司 | Preparation method of nano zinc oxide |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103145176B (en) | 2015-07-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103145176B (en) | High-activity empty frame zinc oxide production method by means of industrial zinciferous smoke dust | |
| Nayaka et al. | An environmental friendly attempt to recycle the spent Li-ion battery cathode through organic acid leaching | |
| CN103602819B (en) | Comprehensive recovery method of vanadate-chromate-containing solution | |
| CN105695751B (en) | A kind of purification technique of electrolytic manganese anode mud | |
| CN104018184A (en) | Brand new method of producing electrolytic manganese metal | |
| CN104762474B (en) | Method for preparing ammonium molybdate through molybdenite | |
| KR20210089142A (en) | Nitrogen Oxide Absorbent Slurry and Method of Preparation and Use thereof | |
| CN103320613A (en) | Method for recovering cobalt nickel through electrolytic manganese industrial ion exchange method | |
| CN104310690A (en) | Process of regenerating metal nitric acid and hydrofluoric acid pickling wastewater and recycling metal elements | |
| CN109825708A (en) | Method for recovering positive and negative electrode substances in waste alkaline zinc-manganese dioxide battery | |
| CN113184926A (en) | Method for preparing Ni-Cu LDH material by using electroplating sludge and application | |
| CN103991893A (en) | Preparing method of high-purity basic cupric carbonate | |
| CN101307462A (en) | Deironing method for ferric manganese ore by leaching method | |
| CN102154553A (en) | Method for removing iron and aluminum by autoxidation of iron-based waste material containing high-value elements | |
| CN106512677B (en) | Zinc oxide desulfurizer and preparation method thereof | |
| TWI552960B (en) | Processes for dissolving copper and preparing copper salts | |
| CN103395825B (en) | A kind of method utilizing steel-smelting electric furnace flue dust to produce nano zine oxide | |
| Yuan et al. | Immobilization of antimony in soil and groundwater using ferro-magnesium bimetallic organic frameworks | |
| CN103060561B (en) | Method for removing chlorine from chlorine-containing zinc sulfate solution | |
| CN105543500B (en) | The method that reclaims zinc is discarded in mud cake containing zinc from electrogalvanizing | |
| CN110627179B (en) | Method for treating arsenic-containing wastewater by using recyclable composite salt precipitator | |
| CN100513315C (en) | Method for preparing cuprous chloride using ion liquid | |
| CN101525692A (en) | Method for environment-friendly utilization of copper-nickel-tungsten alloy | |
| CN102070436A (en) | Method for recovering oxalate and acid liquor from acidic etching waste liquor | |
| CN111717930A (en) | Method for producing basic copper carbonate based on copper-containing etching waste liquid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150708 Termination date: 20200204 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |