CN106145180B - A kind of technique that synthetical recovery processing is carried out to high-fluorine chlorine zinc oxide fume dust and high-fluorine chlorine waste acid - Google Patents
A kind of technique that synthetical recovery processing is carried out to high-fluorine chlorine zinc oxide fume dust and high-fluorine chlorine waste acid Download PDFInfo
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- CN106145180B CN106145180B CN201610487189.0A CN201610487189A CN106145180B CN 106145180 B CN106145180 B CN 106145180B CN 201610487189 A CN201610487189 A CN 201610487189A CN 106145180 B CN106145180 B CN 106145180B
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- fluorine chlorine
- zinc
- fluorine
- zinc oxide
- waste acid
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- C01—INORGANIC CHEMISTRY
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- C01G9/00—Compounds of zinc
Abstract
A kind of technique that synthetical recovery processing is carried out to high-fluorine chlorine zinc oxide fume dust and high-fluorine chlorine waste acid of the present invention,A kind of effectively de- fluorine and chlorine removal is provided and utilizes waste acid and the method for zinc oxide fume dust,High-fluorine chlorine zinc oxide is once leached,Leachate uses the waste acid of high-fluorine chlorine,Solid-liquor separation is carried out using filter press after the completion of once leaching,Filter out filter residue,Press filtration separates after liquid is once neutralized again with high-fluorine chlorine zinc oxide,It neutralizes slag and returns to once leaching recycling metal therein,Neutralising fluid adds in zinc powder purification and impurity removal,Press filtration separates after purification,Filter out filter residue,Liquid adds the heavy zinc of the secondary neutralization of sodium carbonate,Press filtration separates after secondary neutralization,The high liquid of fluorine-containing chlorine beats sewage disposal process,Pulp water containing basic zinc carbonate washes press filtration,Washing waste liquid beats sewage disposal process,Basic zinc carbonate is obtained after slag drying,The present invention comprehensively utilizes the industrial waste product that two kinds are difficult to recycle,Only generate a kind of waste liquid of the ripe simple high-fluorine chlorine for the treatment of process,Remarkable in economical benefits.
Description
Technical field
The invention belongs to nonferrous smelting waste synthetical recovery processing technology fields more particularly to one kind to give birth in heavy non-ferrous metal
The technique that synthetical recovery processing is carried out to the zinc oxide fume dust and waste acid of output during production.
Background technology
The sulfuric acid product recycled from nonferrous smelting process, is generally controlled by gas cleaning, drying, conversion, absorption and tail gas
The technological processes such as reason.The gas cleaning of lead-zinc smelting at present is mostly using the sulfur trioxide in high energy scrubber washing flue gas and on a small quantity
The waste acid that the heavy metals nonferrous smelting such as flue dust, lead zinc process generates, acidity about 15% containing a small amount of heavy metal ion, are gone back simultaneously
Fluorine chlorion containing higher concentration, is difficult to be utilized it, it has to which, using complicated waste acid treatment process, waste water reaches country
It is arranged outside standard, the waste residue for handling generation also is difficult to recycle, and output part neutralizes slag muck and deposits, and the utilization of waste acid is also as industry
Problem.Some enterprises improve concentration using high temperature concentration and remove the method for part fluorine chlorine, and high temperature dilute sulfuric acid carrys out equipment belt huge
Large impact, some handle separating beavy metal using membrane processing method, and effect is not ideal enough, enterprise's also three oxidations from control flue gas
Sulphur generation is set about, but the waste acid of acid manufacturing processes output is also made not utilize slowly, and need to force to handle without obtaining ideal effect
Waste water reaches outer row.
There are the intermediate products of part high-fluorine chlorine zinc oxide, such as the zinc oxide cigarette of steel mill in steel and Lead-Zinc Sintering Process
ZnO of fuming furnace cigarette ash, the multiple hearth furnace zinc oxide fume dust of zinc abstraction that ash, lead are smelted, fluorine-containing chlorine is all very high, can not directly return
It receives, it is necessary to could synthetical recovery after de- fluorine and chlorine removal.
Current fluorine and chlorine removal mode is mostly：Thorium salt fluorine removal, silica gel fluorine removal, silver nitride precipitation dechlorination, ion-exchange dechlorination,
The modes such as chlorine removal from copper residue, the relatively large or removal efficiency of investment is low, not widely used.
The content of the invention
The sewage generated it is an object of the invention to solve prior art nonferrous heavy metal smelting process is difficult to handle and profit
With, in the heavy metals such as steel and lead zinc smelting process to the process problem of the intermediate products of high-fluorine chlorine zinc oxide, and provide and fill
Divide the high-fluorine chlorine zinc oxide fume dust of high-fluorine chlorine waste acid and metal smelt the process generation using metallurgical off-gas acid-making process output
A kind of technique that synthetical recovery processing is carried out to high-fluorine chlorine zinc oxide fume dust and high-fluorine chlorine waste acid.
The technical solution adopted in the present invention is：
A kind of technique that synthetical recovery processing is carried out to high-fluorine chlorine zinc oxide fume dust and high-fluorine chlorine waste acid, including walking as follows
Suddenly：
Step 1）, high-fluorine chlorine zinc oxide fume dust once leached, leachate uses the waste acid of high-fluorine chlorine.
Step 2）, once leach after the completion of solid-liquor separation carried out using filter press, filter residue filters out, is enriched in filter residue useful
Heavy metal and a small amount of zinc, it is 4.5-5.0 that remaining liq is once neutralized to pH value with high-fluorine chlorine zinc oxide fume dust again；
Step 3）, once neutralize after press filtration separate, neutralize slag and return once to leach and recycle useful heavy metal therein, neutralize
Liquid adds in zinc powder purification and impurity removal；
Step 4）, after purification press filtration separate, filter out the filter residue of cupric cadmium, remaining liq add sodium carbonate it is secondary neutralize it is heavy
Zinc, until pH value reaches 6.0-6.5；
Step 5）, after secondary neutralization press filtration separate, the high waste liquid of fluorine-containing chlorine beats sewage disposal process, containing basic zinc carbonate
Pulp water washes 1h press filtrations, and water lotion beats sewage disposal process, basic zinc carbonate is obtained after filter residue and drying.
Further, the acidity of the step a kind waste acid is 150g/l-200g/l, and one time extraction temperature is maintained at 60 DEG C -80
DEG C, the acidity of acid eventually is once leached as 30g/l-60g/l, reacts 4h, liquid-solid ratio 5-7:1.
Further, a neutral temperature is maintained at 55 DEG C -75 DEG C in the step 2, reacts two hours.
Further, in the step 3 during purification and impurity removal, purification temperature is 60 DEG C -75 DEG C, when reaction 1.5 is small, zinc
Powder dosage is 2-5 times of theoretical amount needed for reaction, and zinc powder contains zinc more than 98%.
Further, in the step 4, reaction temperature is maintained at 80 DEG C -85 DEG C during the secondary heavy zinc of neutralization, reaction
1.5h, carbonate content are more than 98%.
The beneficial effects of the present invention are：
The present invention utilizes to produce in the high-fluorine chlorine waste acid of metallurgical off-gas acid-making process output and steel iron and Lead-Zinc Sintering Process
Raw high-fluorine chlorine zinc oxide fume dust output basic carbonate zinc product, the industrial waste product that two kinds are difficult to recycle carry out comprehensive profit
With only generating a kind of waste liquid of the ripe simple high-fluorine chlorine for the treatment of process, reduce environmental pollution caused by production, economic benefit is shown
It writes.
A kind of technique that synthetical recovery processing is carried out to high-fluorine chlorine zinc oxide fume dust and high-fluorine chlorine waste acid provided by the invention
Integrated treatment defluorinate chlorine is carried out with the industrial waste product recycled are difficult to two kinds of high-fluorine chlorine waste acid and high-fluorine chlorine zinc oxide fume dust
And it recycles useful products, only generate a kind of the advantages of waste liquid of the ripe simple high-fluorine chlorine for the treatment of process.
Description of the drawings
Fig. 1 is provided by the invention a kind of to high-fluorine chlorine zinc oxide fume dust and the progress synthetical recovery processing of high-fluorine chlorine waste acid
The process structure schematic diagram of technique.
Specific embodiment
The invention will be further described in the following with reference to the drawings and specific embodiments.
Embodiment 1, a kind of technique that synthetical recovery processing is carried out to high-fluorine chlorine zinc oxide fume dust and high-fluorine chlorine waste acid, specifically
Include the following steps：
Step 1：High-fluorine chlorine zinc oxide fume dust is once leached, leachate uses the waste acid of high-fluorine chlorine；Waste acid acidity
For 150g/l-200g/l, extraction temperature is maintained at 60 DEG C -80 DEG C, leaches acid 30g/l-60g/l eventually, reacts 4h, liquid-solid ratio 5-7:
1；
Step 2：Solid-liquor separation is carried out using filter press after the completion of once leaching, filter residue is filtered out, is enriched in filter residue useful
Heavy metal and a small amount of zinc, it is 4.5-5.0 that remaining liq is once neutralized to pH value with high-fluorine chlorine zinc oxide fume dust again, neutral temperature
55 DEG C -75 DEG C, react 2h；
Step 3：Press filtration separates after once neutralizing, and neutralizing slag return, once useful heavy metal therein is recycled in leaching, neutralizes
Liquid adds in zinc powder purification and impurity removal, and purification temperature is maintained at 60 DEG C -75 DEG C, reaction time 1.5h, and zinc powder dosage is theoretical amount
2-5 times, zinc powder contains zinc more than 98%；
Step 4：Press filtration separates after purification, filters out the filter residue of cupric cadmium, liquid adds the secondary neutralization of sodium carbonate after purification
Heavy zinc, until pH value reaches 6.0-6.5,80 DEG C -85 DEG C of temperature reacts 1.5h, and carbonate content is more than 98%；
Step 5：Press filtration separates after secondary neutralization, and the high waste liquid of fluorine-containing chlorine beats sewage disposal process, containing basic zinc carbonate
Pulp water washes 1h press filtrations, and water lotion beats sewage disposal process, basic zinc carbonate is obtained after slag drying.
Embodiment 2, a kind of technique that synthetical recovery processing is carried out to high-fluorine chlorine zinc oxide fume dust and high-fluorine chlorine waste acid, specifically
Include the following steps：
Step 1：High-fluorine chlorine zinc oxide fume dust is once leached, leachate uses the waste acid of high-fluorine chlorine；Waste acid acidity
For 150g/l-200g/l, extraction temperature is maintained at 70 DEG C, leaches acid 30g/l-60g/l eventually, reacts 4h, liquid-solid ratio 6.5:1；
Step 2：Solid-liquor separation is carried out using filter press after the completion of once leaching, filter residue is filtered out, is enriched in filter residue useful
Heavy metal and a small amount of zinc, it is 4.8 that remaining liq is once neutralized to pH value with high-fluorine chlorine zinc oxide fume dust again, neutral temperature 70
DEG C, react 2h；
Step 3：Press filtration separates after once neutralizing, and neutralizing slag return, once useful heavy metal therein is recycled in leaching, neutralizes
Liquid adds in zinc powder purification and impurity removal, and purification temperature is maintained at 65 DEG C, reaction time 1.5h, and zinc powder dosage is 4 times of theoretical amount, zinc
Powder contains zinc more than 98%；
Step 4：Press filtration separates after purification, filters out the filter residue of cupric cadmium, liquid adds the secondary neutralization of sodium carbonate after purification
Heavy zinc, until pH value reaches 6.5,83 DEG C of temperature reacts 1.5h, and carbonate content is more than 98%；
Step 5：Press filtration separates after secondary neutralization, and the high waste liquid of fluorine-containing chlorine beats sewage disposal process, containing basic zinc carbonate
Pulp water washes 1h press filtrations, and water lotion beats sewage disposal process, basic zinc carbonate is obtained after slag drying.
Embodiment 3, a kind of technique that synthetical recovery processing is carried out to high-fluorine chlorine zinc oxide fume dust and high-fluorine chlorine waste acid, specifically
Include the following steps：
Step 1：High-fluorine chlorine zinc oxide fume dust is once leached, leachate uses the waste acid of high-fluorine chlorine；Waste acid acidity
For 150g/l-200g/l, extraction temperature is maintained at 60 DEG C, leaches acid 55g/l eventually, reacts 4h, liquid-solid ratio 7:1；
Step 2：Solid-liquor separation is carried out using filter press after the completion of once leaching, filter residue is filtered out, is enriched in filter residue useful
Heavy metal and a small amount of zinc, it is 5.0 that remaining liq is once neutralized to pH value with high-fluorine chlorine zinc oxide fume dust again, neutral temperature 75
DEG C, react 2h；
Step 3：Press filtration separates after once neutralizing, and neutralizing slag return, once useful heavy metal therein is recycled in leaching, neutralizes
Liquid adds in zinc powder purification and impurity removal, and purification temperature is maintained at 75 DEG C, reaction time 1.5h, and zinc powder dosage is 2-5 times of theoretical amount,
Zinc powder contains zinc more than 98%；
Step 4：Press filtration separates after purification, filters out the filter residue of cupric cadmium, liquid adds the secondary neutralization of sodium carbonate after purification
Heavy zinc, until pH value reaches 6.5,85 DEG C of temperature reacts 1.5h, and carbonate content is more than 98%；
Step 5：Press filtration separates after secondary neutralization, and the high waste liquid of fluorine-containing chlorine beats sewage disposal process, containing basic zinc carbonate
Pulp water washes 1h press filtrations, and water lotion beats sewage disposal process, basic zinc carbonate is obtained after slag drying.
The present invention is a kind of to high-fluorine chlorine zinc oxide fume dust and high-fluorine chlorine waste acid it can be seen from above specific embodiment
The technique of progress synthetical recovery processing has is difficult to the Industry Waste recycled to two kinds of high-fluorine chlorine waste acid and high-fluorine chlorine zinc oxide fume dust
Product are abandoned to carry out integrated treatment defluorinate chlorine and recycle useful products, the waste liquid for only generating a kind of ripe simple high-fluorine chlorine for the treatment of process
The advantages of.
Claims (5)
- A kind of 1. technique that synthetical recovery processing is carried out to high-fluorine chlorine zinc oxide fume dust and high-fluorine chlorine waste acid, which is characterized in that bag Include following steps：Step 1）, high-fluorine chlorine zinc oxide fume dust once leached, leachate uses the waste acid of high-fluorine chlorine；Step 2）, once leach after the completion of solid-liquor separation carried out using filter press, filter residue filters out, and a useful huge sum of money is enriched in filter residue Category and a small amount of zinc, it is 4.5-5.0 that remaining liq is once neutralized to pH value with high-fluorine chlorine zinc oxide fume dust again；Step 3）, once neutralize after press filtration separate, neutralize slag and return once to leach and recycle useful heavy metal therein, neutralising fluid Add in zinc powder purification and impurity removal；Step 4）, after purification press filtration separate, filter out the filter residue of cupric cadmium, remaining liq adds that sodium carbonate is secondary to neutralize heavy zinc, Until pH value reaches 6.0-6.5；Step 5）, after secondary neutralization press filtration separate, the high waste liquid of fluorine-containing chlorine beats sewage disposal process, the pulp water containing basic zinc carbonate 1h press filtrations are washed, water lotion beats sewage disposal process, basic zinc carbonate is obtained after filter residue and drying.
- A kind of synthetical recovery processing is carried out to high-fluorine chlorine zinc oxide fume dust and high-fluorine chlorine waste acid 2. according to claim 1 Technique, which is characterized in that the acidity of waste acid described in step 1 is 150 g/L -200g/L, and one time extraction temperature is maintained at 60 DEG C -80 DEG C, the acidity of acid eventually is once leached as 30 g/L -60 g/L, reacts 4h, liquid-solid ratio 5-7:1.
- A kind of synthetical recovery processing is carried out to high-fluorine chlorine zinc oxide fume dust and high-fluorine chlorine waste acid 3. according to claim 1 Technique a, which is characterized in that neutral temperature is maintained at 55 DEG C -75 DEG C in the step 2, reacts two hours.
- A kind of synthetical recovery processing is carried out to high-fluorine chlorine zinc oxide fume dust and high-fluorine chlorine waste acid 4. according to claim 1 Technique, which is characterized in that in the step 3 during purification and impurity removal, purification temperature is 60 DEG C -75 DEG C, when reaction 1.5 is small, Zinc powder dosage is 2-5 times of theoretical amount needed for reaction, and zinc powder contains zinc more than 98%.
- A kind of synthetical recovery processing is carried out to high-fluorine chlorine zinc oxide fume dust and high-fluorine chlorine waste acid 5. according to claim 1 Technique, which is characterized in that in the step 4, reaction temperature is maintained at 80 DEG C -85 DEG C during the secondary heavy zinc of neutralization, reaction 1.5h, carbonate content are more than 98%.
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| CN112522520A (en) * | 2020-12-02 | 2021-03-19 | 陕西锌业有限公司 | Method for directly producing electrolytic zinc by using secondary zinc oxide |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101818254A (en) * | 2009-12-23 | 2010-09-01 | 株洲冶炼集团股份有限公司 | Comprehensive recovery method of zinc oxide fume dust |
| CN102286759A (en) * | 2011-07-31 | 2011-12-21 | 红河锌联科技发展有限公司 | Method for preparing electrodeposited zinc from high-fluorine high-chlorine secondary zinc oxide powder |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101818254A (en) * | 2009-12-23 | 2010-09-01 | 株洲冶炼集团股份有限公司 | Comprehensive recovery method of zinc oxide fume dust |
| CN102286759A (en) * | 2011-07-31 | 2011-12-21 | 红河锌联科技发展有限公司 | Method for preparing electrodeposited zinc from high-fluorine high-chlorine secondary zinc oxide powder |
Non-Patent Citations (1)
| Title |
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| 锌烟灰制取碱式碳酸锌及活性氧化锌;康俊峰;《有色矿冶》;20030630;第19卷(第3期);第28-31页 * |
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