CN108408760A - A method of high-purity zinc oxide is prepared with high zinc dedusting ash - Google Patents
A method of high-purity zinc oxide is prepared with high zinc dedusting ash Download PDFInfo
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- CN108408760A CN108408760A CN201810382633.1A CN201810382633A CN108408760A CN 108408760 A CN108408760 A CN 108408760A CN 201810382633 A CN201810382633 A CN 201810382633A CN 108408760 A CN108408760 A CN 108408760A
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- zinc
- dedusting ash
- zinc oxide
- filtrate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a kind of method preparing high-purity zinc oxide with high zinc dedusting ash, by high zinc dedusting ash vitriolization solution, by stirring, filtering and collecting filter liquid；Then filtrate is carried out successively removing iron, the impurity such as copper removal, cadmium, the scavenging solution after being cleaned；Sodium carbonate liquor is added in scavenging solution, fully it is washed after reaction, is filtered, obtains presoma basic zinc carbonate after removing sulfate ion and sodium ion therein, after drying, finished product basic zinc carbonate is obtained, high-purity zinc oxide is obtained after finally being calcined finished product basic zinc carbonate.Compared with prior art, the method provided by the invention for preparing high-purity zinc oxide with high zinc dedusting ash is easy to operate, and each reaction raw materials used are substances cheap and easy to get, and reaction condition is mild, low energy consumption, and gained purity zinc oxide is higher, and up to 99.7% or more.
Description
Technical field
The invention belongs to Metallurgical resources field of comprehensive utilization, and in particular to one kind preparing high-purity zinc oxide with high zinc dedusting ash
Method.
Background technology
With the continuous rapid growth of China's economy, the consumption figure of zinc also increases substantially.According to relevant information, China
It is the country that smart zinc consumption figure is most in the world, the average consumption speedup of 2006~2011 years zinc is 10.54%, far above the whole world
Average level.Although China is the abundant country of a led-zinc-silver deposit, per capita ownership is relatively poor.And steel industry contains
Zinc powder dirt is a kind of important zinc regenerated resources, and deriving from mainly has blast furnace dust, electric furnace dust and converter dust etc..For
This kind of zinc-containing dust, existing many enterprises of the country are using direct-reduction dezincification method, such as kiln process, rotary hearth furnace method, Weir hereby work
Skill etc. is used as the raw material of zinc abstraction industry after so that zinc is further enriched with.
High-purity zinc oxide (ZnO >=99.5%) is widely used in the row such as rubber, chemical fertilizer, pigment, plastics, cosmetics, feed
Industry, price is 1.2~1.8 ten thousand yuan/ton at present, if can be used for producing high-purity zinc oxide with high zinc dedusting ash, will be increased substantially
Its added value.
The method for preparing high-purity zinc oxide at present is mainly dry process, and preparation process energy consumption is higher.
Invention content
The present invention provides a kind of methods preparing high-purity zinc oxide with high zinc dedusting ash, and high pure oxygen is prepared with wet processing
Change zinc, simple for process, low energy consumption, cleanliness without any pollution, the high-purity zinc oxide performance indicator of preparation reaches zinc oxide (indirect method)
Grade A performance indicator in standard GB/T/T 3185-1992.
The technical solution that the present invention takes is：
A method of high-purity zinc oxide is prepared with high zinc dedusting ash, is included the following steps：
S1, by high zinc dedusting ash vitriolization solution, be stirred to react 30~120min, filter and collect filtrate.
High zinc dedusting ash main component is zinc and lead, and contains iron and a small amount of copper, cadmium etc..It is leaching with aqueous sulfuric acid
Go out agent to handle high zinc dedusting ash and be filtered, obtained filter residue main component is the lead sulfate of slightly solubility；Obtained filtrate master
The zinc sulfate that ingredient is soluble is wanted, and contains the foreign ions such as a small amount of iron, copper, cadmium, the leaching rate of zinc is reachable in this step
To 94% or more；
S2, the filtrate for obtaining step S1 preheat, and adjust the initial pH=3 of filtrate through carbonate solution, continue constant temperature 10min
Afterwards, it is slowly added to hydrogen peroxide, after reacting 1h, sodium carbonate liquor is slowly added to and adjusts pH value of solution=5, after reacting 1h, through filtering
To except the solution of zinc sulfate after iron, wherein also containing the foreign ions such as a small amount of copper, cadmium, the removal rate of iron is reachable in the process
To 99.7% or more；Its principle and key reaction are as follows：
For high zinc dedusting ash after aqueous sulfuric acid leaches, iron is with Fe3+And Fe2+What form coexisted always, mainly with Fe2+
Form exists.The pH that leachate is adjusted by adding aqueous slkali, complies with the primary condition of goethite precipitation, reaction equation
For：
Fe3++3OH-=FeOOH ↓+H2O (1)
But goethite process cannot completely remove iron, need further to remove iron with oxydrolysis method.It i.e. will with oxidant
Fe2+It is oxidized to Fe3+, then it is hydrolyzed to Fe (OH)3Precipitation removes.In view of not introducing impurity in iron removal, therefore using double
Oxygen water H2O2When as oxidant, reaction equation is：
2Fe2++H2O2+2H+=2Fe3++2H2O (2)
Fe3++3H2O=Fe (OH)3↓+3H+ (3)
As can be seen that improving pH value to generating goethite precipitation and Fe (OH) from above (1) (2) (3) reaction equation3Precipitation
Favorably, the pH value of reduction is to Fe2+Oxidation it is advantageous, and Zn2+It hydrolyzes near pH=5.5, therefore considers to choose and remove the first of iron
Beginning pH=3, terminal pH=5 can not only ensure the removal rate of iron but also can avoid Zn2+Hydrolysis production precipitation.
S3, the filtrate for obtaining step S2 preheat, and zinc powder is added in batches thereto to replace copper, cadmium and other traces
Metal ion is stirred to react 30~120min after zinc powder is added every time, is filtered after the completion of reaction, and collect filtrate；Filtrate at this time
In main component be zinc sulfate, wherein copper, cadmium content be respectively less than 0.0001g/L.The reaction mainly occurred is as follows：
Zn+CuSO4=Cu ↓+ZnSO4 (4)
Zn+CdSO4=Cd ↓+ZnSO4 (5)
S4, the filtrate obtained to step S3 preheating, be slowly added to carbonate solution thereto, and be stirred to react precipitation 30~
90min is filtered after the completion of reaction, and is collected filter cake；Filter cake is presoma basic zinc carbonate, and filter cake is washed with water until not having
Sulfate radical exists；Key reaction is：
3ZnSO4+3Na2CO3+3H2O=ZnCO3·2Zn(OH)2·H2O+2CO2+3Na2SO4 (6)
S5, the filter cake for obtaining step S4 are dried, and then calcine 2~8h in 900~1200 DEG C, you can obtain described high-purity
Zinc oxide.Key reaction is：
ZnCO3·2Zn(OH)2·H2O=3ZnO+CO2+3H2O (7)
In the step S1, a concentration of 150~230g/L of sulfuric acid solution, the solid-to-liquid ratio of high zinc dedusting ash and sulfuric acid solution
It is 1:2~1:8, the rate of stirring is 200~600r/min.
In the step S2, the pH of filtrate is adjusted using the sodium carbonate of a concentration of 150~230g/L, the hydrogen peroxide is work
The ratio of industry grade, high zinc dedusting ash and industrial grade hydrogen peroxide is 1g:0.02~0.08mL.
In the step S3, the quality of the zinc powder is the 0.2%~1.0% of high zinc dedusting ash quality, the zinc powder point
Be added in filtrate twice, be added the 50%~80% of zinc powder total amount for the first time, second be added zinc powder total amount 20%~
50%.Zinc powder, which is added in two portions, can utmostly ensure the removal rate of the impurity such as copper, cadmium.
In the step S4, the carbonate solution is the sodium carbonate liquor of a concentration of 150~230g/L, carbonate solution
The amount of the substance of middle carbonate is 1.1~2.2 times of the amount of the substance of zinc in the filtrate component that step S3 is obtained.
Controlled at 30~70 DEG C in the step S1, within this temperature range when zinc leaching rate 94% or more.
Controlled at 30~70 DEG C in the step S2, within this temperature range when iron removal rate 99.7% with
On, and the loss late of zinc is below 5%.
Controlled at 60~90 DEG C in the step S3, preheating time 10min.Within this temperature range, go copper removal,
The impurity ion contents such as copper, cadmium are within 0.0001g/L in the scavenging solution of the foreign ions such as cadmium.
Controlled at 60~90 DEG C in the step S4, preheating time is 20~60min.It titrates within this temperature range
Be conducive to the formation of presoma basic zinc carbonate.
In the step S5, the temperature and time of the drying be be not 105 DEG C, 5~10h.
Mass fraction >=99.70% of zinc oxide in the high-purity zinc oxide being prepared according to method disclosed by the invention,
Its property indices reaches the Grade A performance indicator in zinc oxide (indirect method) standard GB/T/T 3185-1992.
The method provided by the invention for preparing high-purity zinc oxide with high zinc dedusting ash, can successfully realize and utilize Zn >=20%
High zinc dedusting ash prepares the purpose that purity is up to 99.7% or more high-purity zinc oxide.
Compared with prior art, the method provided by the invention for preparing high-purity zinc oxide with high zinc dedusting ash is easy to operate,
Each reaction raw materials used are substances cheap and easy to get, and reaction condition is mild, low energy consumption, and gained purity zinc oxide is higher,
Up to 99.7% or more.
Description of the drawings
Fig. 1 is the process flow chart that high-purity zinc oxide is prepared with high zinc dedusting ash.
Specific implementation mode
The following describes the present invention in detail with reference to examples.
Embodiment 1
A method of high-purity zinc oxide, the high zinc dedusting ash main component and particle diameter distribution are prepared with high zinc dedusting ash
As shown in embodiment 1 in embodiment 1, table 2 in table 1.
1 high zinc dedusting ash main chemical compositions of table, wt%
| Zn | Pb | Fe | Cu | Cd | Ag | Mn | |
| Embodiment 1 | 30.5208 | 7.9226 | 12.6802 | 0.0307 | 0.1159 | 0.0208 | 0.0116 |
| Embodiment 2 | 39.0102 | 11.8408 | 4.3370 | 0.0382 | 0.0986 | 0.0197 | 0.0109 |
| Embodiment 3 | 38.1227 | 10.0576 | 6.5931 | 0.0269 | 0.0109 | 0.0217 | 0.0127 |
2 high zinc dedusting ash granularmetric analysis of table, %
| Granule size | 80 mesh of ＞ | 80~120 mesh | 120~150 mesh | 150~200 mesh | 200 mesh of ＜ |
| Embodiment 1 | 3.31 | 3.20 | 3.81 | 12.11 | 77.57 |
| Embodiment 2 | 3.09 | 3.36 | 3.91 | 11.29 | 78.35 |
| Embodiment 3 | 3.18 | 3.09 | 3.88 | 12.02 | 77.86 |
Concrete operation step is as follows：
S1,200g high zinc dedusting ash is taken, the sulfuric acid 700mL of 150g/L is added, controlling reaction temperature is 65 DEG C, speed of agitator
It for 300r/min, mixing time 30min, is filtered after complete reaction, collects filtrate and filter residue respectively；
S2, filtrate collected by step S1 is placed in 40 DEG C of waters bath with thermostatic control and stirs 10min, be slowly added to a concentration of
Its pH value is adjusted to 3 by the sodium carbonate liquor of 170g/L, after continuing constant temperature 15min, is slowly added to industrial hydrogen peroxide 8.5mL, 1h
It is filtered after solution ph is adjusted to 5,1h with the sodium carbonate of 170g/L afterwards, removes the iron in filtrate, collected except after iron
Filtrate；
S3, it the step S2 filtrates collected is placed in 60 DEG C of waters bath with thermostatic control preheats 10min, 0.2g zinc powders are added, wait reacting
0.2g zinc powders are added after 30min, filtrate is filtered after reacting 30min, remove the impurity such as copper therein, cadmium, are collected
Filtrate after removal of impurities；
S4, it the step S3 filtrates collected is placed in 60 DEG C of water bath with thermostatic control preheats 60min, under conditions of magnetic agitation
The sodium carbonate liquor 680mL, 30min to be precipitated that 170g/L is added dropwise are filtered to obtain filter cake later, and filter is washed with clear water
Cake is complete to sulfate radical removal, and the filter cake after washing is dried 8h at 105 DEG C, obtains finished product basic zinc carbonate；
S5, finished product basic zinc carbonate obtained by step S4 is calcined into 2h at 1100 DEG C, obtains high-purity zinc oxide, performance
In index such as table 3 shown in embodiment 1, reach the Grade A performance in zinc oxide (indirect method) standard GB/T/T3185-1992
Index.
3 high-purity zinc oxide product performance index detection data of table
Embodiment 2
A method of high-purity zinc oxide, the high zinc dedusting ash main component and particle diameter distribution are prepared with high zinc dedusting ash
As shown in embodiment 2 in embodiment 2, table 2 in table 1.
Concrete operation step is as follows：
S1,100g high zinc dedusting ash is taken, the sulfuric acid 400mL of 180g/L is added, controlling reaction temperature is 65 DEG C, speed of agitator
It for 300r/min, mixing time 30min, is filtered after complete reaction, collects filtrate and filter residue respectively；
S2, filtrate collected by step S1 is placed in 40 DEG C of waters bath with thermostatic control and stirs 10min, be slowly added to the carbon of 150g/L
Its pH value is adjusted to 3 by acid sodium solution, after continuing constant temperature 15min, is slowly added to industrial hydrogen peroxide 6.0mL.150g/L is used after 1h
Sodium carbonate solution ph is adjusted to 5,1h after be filtered, remove the iron in filtrate, collect except the filtrate after iron；
S3, it the step S2 filtrates collected is placed in 60 DEG C of waters bath with thermostatic control preheats 10min, 0.2g zinc powders are added, wait reacting
0.1g zinc powders are added after 30min, filtrate is filtered after reacting 30min, remove the impurity such as copper therein, cadmium, are collected
Filtrate after removal of impurities；
S4, it the step S3 filtrates collected is placed in 70 DEG C of water bath with thermostatic control preheats 60min, under conditions of magnetic agitation
The sodium carbonate liquor 550mL, 30min to be precipitated that 150g/L is added dropwise are filtered to obtain filter cake later, and filter is washed with clear water
Cake is complete to sulfate radical removal, and the filter cake after washing is dried 8h at 105 DEG C, obtains finished product basic zinc carbonate；
S5, finished product basic zinc carbonate obtained by step S4 is calcined into 2h at 1100 DEG C, obtains high-purity zinc oxide, performance
In index such as table 3 shown in embodiment 2, reach the Grade A performance in zinc oxide (indirect method) standard GB/T/T3185-1992
Index.
Embodiment 3
A method of high-purity zinc oxide, the high zinc dedusting ash main component and particle diameter distribution are prepared with high zinc dedusting ash
As shown in embodiment 3 in embodiment 3, table 2 in table 1.
Concrete operation step is as follows：
S1,100g high zinc dedusting ash is taken, the sulfuric acid 500mL of 190g/L is added, controlling reaction temperature is 65 DEG C, speed of agitator
It for 300r/min, mixing time 30min, is filtered after complete reaction, collects filtrate and filter residue respectively；
S2, filtrate collected by step S1 is placed in 40 DEG C of waters bath with thermostatic control and stirs 10min, be slowly added to the carbon of 160g/L
Its pH value is adjusted to 3 by acid sodium solution, after continuing constant temperature 15min, is slowly added to industrial hydrogen peroxide 5.0mL, 160g/L is used after 1h
Sodium carbonate solution ph is adjusted to 5,1h after be filtered, remove the iron in filtrate, collect except the filtrate after iron；
S3, it the step S2 filtrates collected is placed in 70 DEG C of waters bath with thermostatic control preheats 10min, 0.2g zinc powders are added, wait reacting
0.1g zinc powders are added after 30min, filtrate is filtered after reacting 30min, remove the impurity such as copper therein, cadmium, are collected
Filtrate after removal of impurities；
S4, it the step S3 filtrates collected is placed in 80 DEG C of water bath with thermostatic control preheats 60min, under conditions of magnetic agitation
The sodium carbonate liquor 430mL, 30min to be precipitated that 160g/L is added dropwise are filtered to obtain filter cake later, and filter is washed with clear water
Cake is complete to sulfate radical removal, and the filter cake after washing is dried 8h at 105 DEG C, obtains finished product basic zinc carbonate；
S5, finished product basic zinc carbonate obtained by step S4 is calcined into 2h at 900 DEG C, obtains high-purity zinc oxide, performance
In index such as table 3 shown in embodiment 3, reach the Grade A performance in zinc oxide (indirect method) standard GB/T/T3185-1992
Index.
It is above-mentioned with reference to embodiment to it is a kind of with high zinc dedusting ash prepare high-purity zinc oxide method carry out detailed description, be
It is illustrative without being restrictive, several embodiments can be enumerated according to limited range, therefore do not departing from the present invention
Change and modification under general plotting should belong within protection scope of the present invention.
Claims (9)
1. a kind of method preparing high-purity zinc oxide with high zinc dedusting ash, which is characterized in that include the following steps：
S1, by high zinc dedusting ash vitriolization solution, be stirred to react 30~120min, filter and collect filtrate；
S2, the filtrate for obtaining step S1 preheat, and adjust filtrate pH=3 through carbonate solution, and hydrogen peroxide is added into filtrate,
After reacting 1h, pH=5 is adjusted through carbonate solution, after reacting 1h, filtrate is collected in filtering；
S3, the filtrate for obtaining step S2 preheat, and are added zinc powder is added in batches thereto, be stirred to react after zinc powder is added every time
30~120min is filtered after the completion of reaction, and is collected filtrate；
S4, the filtrate obtained to step S3 preheating, are added carbonate solution thereto, and precipitate 30~90min after being stirred to react,
It is filtered after the completion of reaction, and collects filter cake；
S5, the filter cake for obtaining step S4 are dried, and then calcine 2~8h in 900~1200 DEG C, you can obtain the high pure zirconia
Zinc.
2. the method according to claim 1 for preparing high-purity zinc oxide with high zinc dedusting ash, which is characterized in that the step
In S1, the solid-to-liquid ratio of a concentration of 150~230g/L of sulfuric acid solution, high zinc dedusting ash and sulfuric acid solution are 1:2~1:8.
3. the method according to claim 1 for preparing high-purity zinc oxide with high zinc dedusting ash, which is characterized in that the step
In S2, the pH of filtrate is adjusted using the sodium carbonate of a concentration of 150~230g/L, the hydrogen peroxide is technical grade, high zinc dedusting ash
Ratio with industrial grade hydrogen peroxide is 1g：0.02~0.08mL.
4. the method according to claim 1 for preparing high-purity zinc oxide with high zinc dedusting ash, which is characterized in that the step
In S3, the quality of the zinc powder is the 0.2%~1.0% of high zinc dedusting ash quality, and the zinc powder is added in two portions in filtrate,
The 50%~80% of zinc powder total amount, the 20%~50% of second of addition zinc powder total amount is added for the first time.
5. the method according to claim 1 for preparing high-purity zinc oxide with high zinc dedusting ash, which is characterized in that the step
In S4, the carbonate solution is the sodium carbonate liquor of a concentration of 150~230g/L, dosage be the obtained filtrates of step S3 at
1.1~2.2 times of the amount of the substance of zinc in point.
6. the method for preparing high-purity zinc oxide with high zinc dedusting ash according to claim 1 or 3 or 4 or 5, feature exist
In the reaction temperature of described step S1, S2, S3, S4 are respectively 30~70 DEG C, 30~70 DEG C, 60~90 DEG C, 60~90 DEG C.
7. the method for preparing high-purity zinc oxide with high zinc dedusting ash according to claim 1 or 3 or 4 or 5, feature exist
In the preheating time of step S3, S4 is 10min, 20~60min.
8. the method according to claim 1 for preparing high-purity zinc oxide with high zinc dedusting ash, which is characterized in that the step
In S5, the temperature and time of the drying be be not 105 DEG C, 5~10h.
9. the method according to claim 1 for preparing high-purity zinc oxide with high zinc dedusting ash, which is characterized in that described high-purity
Mass fraction >=99.70% of zinc oxide in zinc oxide.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110129551A (en) * | 2019-06-20 | 2019-08-16 | 桂阳县皓钰新材料有限公司 | The method for preparing high-grade zinc oxide and feed grade zinc oxide simultaneously using rotary kiln |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1080265A (en) * | 1993-04-09 | 1994-01-05 | 洛阳蓝天化工厂 | The full wet method of improved bicarbonate of ammonia is produced high-active zinc oxide |
| KR100625521B1 (en) * | 2005-06-21 | 2006-09-20 | 심재윤 | Production of ultra fine zinc oxide particle from zinc ash and the products thereby |
-
2018
- 2018-04-26 CN CN201810382633.1A patent/CN108408760B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1080265A (en) * | 1993-04-09 | 1994-01-05 | 洛阳蓝天化工厂 | The full wet method of improved bicarbonate of ammonia is produced high-active zinc oxide |
| KR100625521B1 (en) * | 2005-06-21 | 2006-09-20 | 심재윤 | Production of ultra fine zinc oxide particle from zinc ash and the products thereby |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110129551A (en) * | 2019-06-20 | 2019-08-16 | 桂阳县皓钰新材料有限公司 | The method for preparing high-grade zinc oxide and feed grade zinc oxide simultaneously using rotary kiln |
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