CN103145176B - 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
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- CN103145176B CN103145176B CN201310041731.6A CN201310041731A CN103145176B CN 103145176 B CN103145176 B CN 103145176B CN 201310041731 A CN201310041731 A CN 201310041731A CN 103145176 B CN103145176 B CN 103145176B
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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 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 the vulcanization leveller of natural rubber, synthetic rubber and latex and strengthening agent and painted Ji.Nano zine oxide is used for can giving full play to sulfuration promoter action in rubber industry, and improve the performance of rubber, its consumption is only the 30%-50% of common zinc oxide.
Summary of the invention:
The object of this invention is to provide a kind of method utilizing industrial zinc smoke production High-activity empty frame zinc oxide, its raw material sources is extensive, and technical process is simple, and without the need to 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 problem existing for background technology, the present invention adopts following production method:
1) the industrial zinc smoke choosing wide material sources, as main raw material, belongs to industrial waste and recycles, clean environment firendly.
2) coordinated by industrial zinc smoke appropriate recovery ammoniacal liquor, bicarbonate of ammonia, industrial ammonia, tap water to mix dosing by a certain percentage, leach under 50 DEG C of-60 DEG C of conditions, obtain thick leaching liquid.
3) by step 2) the thick leaching liquid that obtains filters, under the condition of 50 DEG C-60 DEG C,
Oxidizer is by Fe
2+be oxidized to Fe
3+, stroke Fe(OH)
3colloidal precipitation, filters.
4) leaching liquid step 3) obtained, under 50 DEG C of-60 DEG C of conditions, adds purificant, the impurity such as removing heavy metals, obtains, containing the qualified leaching liquid such as Pb, Cd, As, Cu, Ni, Co, Sb, filtering.
5) qualified leaching liquid step 4) obtained, the particular case that this place uses for applicable rubber industry, chooses calcium hydroxide as the empty frame of core, appropriate calcium hydroxide and sucrose is coordinated according to the content of wherein zinc oxide, carry out ammonia still process crystallization, filter, obtain sky frame zinc subcarbonate.The ammonia be wherein evaporated and CO
2mixture, being recycled ammoniacal liquor through collecting, returning step 2) leach recycling, realize recycling of material.
6) empty frame zinc subcarbonate pure water rinsing step 5) obtained, by solubility salt impurity removing wherein.Obtain the empty frame zinc subcarbonate that the water solubles is qualified.
7) qualified empty frame zinc subcarbonate step 6) obtained, through 600 DEG C of quick burnings, collects, obtains qualified High-activity empty frame nano zine oxide.
Described recovery ammonia concn is about 12%, and industrial ammonia is about 18%, and bicarbonate of ammonia is agriculture level bicarbonate of ammonia, and nitrogen content is about 17%, 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 inorganics and organism, and Heating temperature is that 1 standard atmosphere depresses 100 DEG C, and other pressure at temperatures suitably adjusts, and keeps for the purpose of solution slight boiling condition.Heating terminal be in solution zinc content lower than 0.2g/l.
The zinc oxide activity that instant invention overcomes traditional method manufacture is low, metallic zinc content is high, so that the shortcoming that in rubber item afterwards, heavy metal loss speed is high, effectively reduce the content of metallic zinc, but improve the activity of zinc oxide simultaneously, under the prerequisite ensureing rubber indices, reach the object of heavy metal in the rubber item reducing and use this product, and then achieve reduction heavy metal loss speed, the object of environmental protection.
The present invention has following beneficial effect:
1) take Industrial fumes as raw material, the secondary recovery belonging to resource utilizes, and clean environment firendly is the recycling economy that country advocates, obtains the support of national departments concerned.Raw material sources are extensive, 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 content of product is low, removal of impurities low cost, and process control is easy, such 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, active high.
Outstanding advantages of the present invention is the activity improving empty frame zinc oxide, effectively reduces cost, and by low be the content of heavy metal, reach the object of clean environment firendly.
Embodiment:
Embodiment 1: this embodiment by the following technical solutions: by ammoniacal liquor 623.7ml proportioning bicarbonate of ammonia 67g, strong aqua 300ml, strong aqua is containing NH
3be 14.084%, containing 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 DEG C, insulation reaction 2 hours, filter, clean filter mud, obtain the solution 934ml containing zinc 157.2g/l, the rate of recovery is 94.01%.
Embodiment 2: the 934ml solution obtained in embodiment 1 is added 0.24g potassium permanganate, is incubated 50 DEG C of stirring reactions 30 minutes, filters the solution 926ml obtaining iron content 7ppm.
Embodiment 3: add 1g zinc powder by the 926ml solution obtained in embodiment 2, is incubated 50 DEG C of stirring reactions 1 hour, filters the solution 918ml obtaining leaded 6ppm.
Embodiment 4: the scavenging solution 918ml obtained in embodiment 3 is placed in 1800ml beaker, add tap water 300ml, stir, 76.9g calcium hydroxide is slowly evenly added wherein, calcium hydroxide is disperseed completely, do not unite, add sucrose 0.8g, heated and boiled, keep micro-boiling, the gas condenser produced reclaims, and in micro-process of boiling, keeps liquid volume to be wherein about 1250ml.With the gas that PH detection paper volatilizes, to be evaporated go out gas pH value when being 7, stop boiling.
Embodiment 5: material liquid mixture well-done in embodiment 4 is filtered, cleans filter mud with pure water, obtain moistening filter mud 479g.Detecting moisture is 35.3%.The ammoniacal liquor collected is detected, is recycled ammoniacal liquor 921ml, wherein containing NH
3be 10.1265%, CO
3 2-be 9.286%.
Embodiment 6: the filter mud obtained in embodiment 5 is calcined 30 minutes through 600 DEG C, obtains High-activity empty frame nano zine oxide 234.67g.It is 50.2% that detection wherein contains zinc, and leaded is 43ppm, is 6ppm containing manganese, and cupric is 3ppm, is 21ppm containing cadmium, and the water solubles is 0.08%, and hydrochloric acid insoluble substance is 0.02%.
Claims (1)
1. utilize a method for industrial zinc smoke production High-activity empty frame zinc oxide, it is characterized in that its production method is:
1) the industrial zinc smoke choosing wide material sources, as main raw material, belongs to industrial waste and recycles, clean environment firendly;
2) coordinated by industrial zinc smoke appropriate recovery ammoniacal liquor, bicarbonate of ammonia, industrial ammonia, tap water to mix dosing by a certain percentage, leach under 50 DEG C of-60 DEG C of conditions, obtain thick leaching liquid;
3) by step 2) the thick leaching liquid that obtains filters, under the condition of 50 DEG C-60 DEG C,
Oxidizer is by Fe
2+be oxidized to Fe
3+, form Fe(OH)
3colloidal precipitation, filters;
4) leaching liquid step 3) obtained, under 50 DEG C of-60 DEG C of conditions, adds purificant, removing heavy-metal impurities, obtains, containing the qualified leaching liquid of Pb, Cd, As, Cu, Ni, Co, Sb, filtering;
5) qualified leaching liquid step 4) obtained, the particular case that this place uses for applicable rubber industry, chooses calcium hydroxide as the empty frame of core, appropriate calcium hydroxide and sucrose is coordinated according to the content of wherein zinc oxide, carry out ammonia still process crystallization, filter, obtain sky frame zinc subcarbonate; The ammonia be wherein evaporated and CO
2mixture, being recycled ammoniacal liquor through collecting, returning step 2) leach recycling, realize recycling of material;
6) empty frame zinc subcarbonate pure water rinsing step 5) obtained, by solubility salt impurity removing wherein; Obtain the empty frame zinc subcarbonate that the water solubles is qualified;
7) qualified empty frame zinc subcarbonate step 6) obtained, through 600 DEG C of quick burnings, collects, obtains qualified High-activity empty frame nano zine oxide; 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.
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| 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 |
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| CN103145176B true CN103145176B (en) | 2015-07-08 |
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Families Citing this family (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN105293564A (en) * | 2015-10-05 | 2016-02-03 | 李果 | Method for recycling zinc-containing dust ash in steel plant |
| CN105439192A (en) * | 2015-12-09 | 2016-03-30 | 李果 | Comprehensive utilization method for zinc oxide ore |
| 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 |
| CN110972479B (en) * | 2018-07-24 | 2022-05-06 | 重庆东群科技有限公司 | Method for producing zinc oxide by twice leaching method |
| CN110896643B (en) * | 2018-07-24 | 2021-11-16 | 重庆东群科技有限公司 | Method for producing zinc-containing compound or zinc oxide from zinc-containing raw ore through intermediate step of calcium zincate synthesis |
| 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 |
| 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 |
| 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 |
| 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 |
| 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 |
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 |
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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 |
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