CN103319038A - Processing method for waste mixed acid - Google Patents
Processing method for waste mixed acid Download PDFInfo
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- CN103319038A CN103319038A CN2012100921479A CN201210092147A CN103319038A CN 103319038 A CN103319038 A CN 103319038A CN 2012100921479 A CN2012100921479 A CN 2012100921479A CN 201210092147 A CN201210092147 A CN 201210092147A CN 103319038 A CN103319038 A CN 103319038A
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Abstract
The invention relates to a processing method for waste mixed acid. The method comprises following steps: (1) the waste mixed acid is delivered into a concentration tower, contacted with acid mist exhausted by a roasting furnace, the heated waste mixed acid is delivered to the roasting furnace, and the produced acid mist is exhausted to the concentration tower; (2) heat exchanges between the acid mist and the waste mixed acid, and cooled acid mist is delivered to a first stage washing tower; (3) recycled acid is produced from part of the acid mist and water in the first stage washing tower; (4) unabsorbed acid mist is delivered into a droplet separator, produced liquid is delivered into a second stage washing tower, and acid water is produced from part of the acid mist and water; (5) the acid mist washed in the second washing tower is delivered into the droplet separator, condensed liquid is delivered into a third stage washing tower, and the acid water is produced from a small amount of the acid mist and water; (6) the acid mist washed in the third washing tower is delivered into the droplet separator, condensed acid mist is delivered to the bottom of a fourth stage washing tower, and the acid water is produced from a small amount of the acid mist and water; and (7) the acid mist exhausted out of the fourth stage washing tower is directly delivered into a nitric oxide processing device. Recovery rate of the method is relatively high.
Description
Technical field
A kind of method of processing waste mixed acid.
Background technology
Adopt at present spray roasting art breading waste mixed acid both at home and abroad, the recovery and purification of nitric acid rate generally maintains about 30%, and not only the nitric acid rate of recovery is lower, brings simultaneously discharged nitrous oxides also larger.Carrying out specially spent acid restored acid regeneration unit, after the waste mixed acid process stoving oven heat, the whole evaporation, decomposition of the nitric acid in the waste mixed acid and nitrate become oxides of nitrogen gas.Hydrofluoric acid is because concentration own is lower, and difficult decomposition volatilization, also easily absorb in the process of washing absorption, so the rate of recovery of hydrofluoric acid is higher.But nitric acid easily decomposes volatilization, therefore also is difficult to washing and recycling, so the recovery and purification of nitric acid rate is lower, the nitric acid rate of recovery≤30%, but nitric acid is as the main component in the waste mixed acid, if the nitric acid rate of recovery is lower, will produce a very large impact realizing the waste mixed acid regeneration.Oxynitride can not reclaim formation nitric acid and will strengthen the intractability of follow-up oxynitride simultaneously, and then causes the too much discharging of oxynitride.
Summary of the invention
In order to overcome the existing above-mentioned deficiency of processing the method for waste mixed acid, the invention provides the method for the high processing waste mixed acid of a kind of nitric acid rate of recovery.
Solve oxynitride washing and recycling technology and will become the key that improves the nitric acid rate of recovery, and the equipment for washing tower of the main waste acid recovery of acid regeneration unit is the key of dealing with problems, the concentration of one-level washing tower washings is not as the secondary washing tower, and the concentration of three grades of washing towers is also higher.The nitric acid recovery has much relations with the temperature of wash cooling liquid as can be known, and temperature is lower, and washing absorption oxynitride effect is better; After next washed progression and more leans on, temperature was relatively low, and assimilation effect is also better.
The method of this processing waste mixed acid comprises following step successively:
Waste mixed acid of the present invention is the waste mixed acid that acid-washing stainless steel produces, and the waste mixed acid composition is: nitric acid, hydrofluoric acid, iron ion, ferric fluoride, iron nitrate.
I is input to the waste mixed acid of acid-washing stainless steel line discharging the top of upgrading tower with sour pump, and directly contact with acid mist gas that stoving oven top flue is discharged and to carry out heat exchange, waste mixed acid is heated to 75 ± 5 ℃ by the top lance of pump delivery to stoving oven, by spray gun acid mist is ejected into and carries out roasting in the stoving oven, temperature in the stoving oven is 750 ± 20 ℃, waste mixed acid carries out thermal degradation, evaporation in stoving oven, metal ion is deposited to the stoving oven bottom and automatically collects the brown iron oxide collection device by pipeline with oxide form; The acid mist that waste mixed acid produces after roasting, 280 ± 10 ℃ ℃ of acid mist temperature are discharged to the bottom of upgrading tower by the flue at stoving oven top under the negative pressure of acid fog blower fan.
The II acid mist directly contacts with waste mixed acid in upgrading tower from the bottom to top, carries out heat exchange, and waste mixed acid is heated, and acid mist gas is cooled to 90 ± 2 ℃, and cooled gas enters into the bottom of one-level washing tower under the effect of pipeline at acid fog blower fan.
Temperature in the III one-level washing tower is 80 ± 2 ℃, and wherein 30 ± 2% acid mist is at the water formation regenerating acid of one-level washing tower with input one-level washing tower, and regenerating acid to the acid-washing stainless steel unit, is used for stainless steel production pickling through pump delivery.
IV enters acid mist pipeline through the unabsorbed acid mist of one-level washing tower under the effect of acid fog blower fan, acid mist pipeline is installed droplet separator, the liquid self-flowing of the acid mist condensation of collecting in the droplet separator is to the bottom of secondary washing tower, acid mist is contacted with water in the moving process of top by the bottom of secondary washing tower, wherein 20 ± 2% acid mist this and water form concentration lower contain sour water;
V enters acid mist pipeline through the acid mist of secondary washing tower under the effect of acid fog blower fan, acid mist pipeline is installed droplet separator, the bottom of liquid self-flowing to the three grade washing tower of the acid mist condensation of collecting in the droplet separator, acid mist is contacted with water in the moving process of top by the bottom of three grades of washing towers, wherein 10 ± 2%% acid mist this and water form concentration lower contain sour water;
VI enters acid mist pipeline through the acid mist of three grades of washing towers under the effect of acid fog blower fan, acid mist pipeline is installed droplet separator, the liquid self-flowing of the acid mist condensation of collecting in the droplet separator is to the bottom of level Four washing tower, acid mist is contacted with water in the moving process of top by the bottom of level Four washing tower, wherein 5 ± 2% acid mist this and water form concentration lower contain sour water, contain sour water and be disposed to neutralization station and carry out neutralizing treatment.
VII because acid content is less, absorbs difficulty from level Four washing tower top acid mist out, and therefore directly entering into the oxynitride treatment unit carries out conversion processing, and conversion of nitrogen oxides is become nitrogen and water vapour qualified discharge.
The present invention is main to be by the liquid of cooling acid mist washing, uses the level Four washing tower, fills filtrate in the tower, guarantees that acid mist gas fully contacts with washings; Utilize the board-like water cooler cooling of big area, control washings temperature promotes washing effect; Droplet separator is set in the middle of acid mist pipeline, and the condensation acid solution that reclaims in the droplet separator reaches the effect that promotes the nitric acid rate of recovery in the spent acid.The nitric acid rate of recovery brings up to 60% by original 30%.Hydrofluoric acid 97%.
Embodiment
Describe the specific embodiment of the present invention in detail below in conjunction with implementing, but the specific embodiment of the present invention is not limited to following embodiment.
Embodiment
The used one-level of the present embodiment is to the washing tower of level Four, the in-built heat interchanging area 100m of each washing tower
2Plate-type heat exchanger strengthens heat interchanging area, and washing tower is all by water cooling.The inner filtrate of filling of washing tower, (washing tower generally has filtrate) filtrate adopts PVDF material, contact surface area 110m
2/ m
3Nitric acid behind the acid-washing stainless steel that the present embodiment is processed and the mixing acid of hydrofluoric acid are called for short waste mixed acid.
The embodiment of the method for this processing waste mixed acid is following step successively:
The waste mixed acid that this instance processes acid-washing stainless steel produces, the waste mixed acid composition is: nitric acid, hydrofluoric acid, iron ion, ferric fluoride, iron nitrate.
I is input to the waste mixed acid of acid-washing stainless steel line discharging the top of upgrading tower, flow 7.5m with sour pump
3/ h, and directly contact with acid mist gas that stoving oven top flue is discharged and to carry out heat exchange, waste mixed acid is heated to 75 ℃ by the top lance of pump delivery to stoving oven, by spray gun acid mist is ejected into and carries out roasting in the stoving oven, temperature in the stoving oven is 750 ℃, waste mixed acid carries out thermal degradation, evaporation in stoving oven, metal ion is deposited to the stoving oven bottom and automatically collects the brown iron oxide collection device by pipeline with oxide form; The acid mist that waste mixed acid produces after roasting, 280 ℃ of acid mist temperature are discharged to the bottom of upgrading tower by the flue at stoving oven top under the negative pressure of acid fog blower fan.Be waste mixed acid before entering stoving oven, be introduced into upgrading tower contact with acid mist gas carry out heat exchange after, enter into again the stoving oven roasting and form acid mist gas, acid mist gas directly enters the one-level washing tower at upgrading tower after heat exchange.
The II acid mist directly contacts with waste mixed acid in upgrading tower from the bottom to top, carries out heat exchange, and waste mixed acid is heated, and acid mist gas is cooled to below 90, and cooled gas enters into the bottom of one-level washing tower under the effect of pipeline at acid fog blower fan.
III under the effect of acid mist in exhaust gas blower of stoving oven heating evaporation by upgrading tower after heat exchange, under the effect of acid fog blower fan, enter the bottom of one-level washing tower, temperature in the one-level washing tower is 80 ± 5 ℃, wherein the acid mist of 28-32% is at the water formation regenerating acid of one-level washing tower with input one-level washing tower, regenerating acid to the acid-washing stainless steel unit, is used for stainless steel production pickling through pump delivery.
IV enters acid mist pipeline through the unabsorbed acid mist of one-level washing tower under the effect of acid fog blower fan, acid mist pipeline is installed droplet separator, the liquid self-flowing of the acid mist condensation of collecting in the droplet separator is to the bottom of secondary washing tower, acid mist is contacted with water in the moving process of top by the bottom of secondary washing tower, wherein 20 ± 2% acid mist this and water form concentration lower contain sour water;
V enters acid mist pipeline through the acid mist of secondary washing tower under the effect of acid fog blower fan, acid mist pipeline is installed droplet separator, the bottom of liquid self-flowing to the three grade washing tower of the acid mist condensation of collecting in the droplet separator, acid mist is contacted with water in the moving process of top by the bottom of three grades of washing towers, wherein 10 ± 2% acid mist this and water form concentration lower contain sour water;
VI enters acid mist pipeline through the acid mist of three grades of washing towers under the effect of acid fog blower fan, acid mist pipeline is installed droplet separator, the liquid self-flowing of the acid mist condensation of collecting in the droplet separator is to the bottom of level Four washing tower, acid mist is contacted with water in the moving process of top by the bottom of level Four washing tower, wherein 5 ± 2% acid mist this and water form concentration lower contain sour water, contain sour water and be disposed to neutralization station and carry out neutralizing treatment.
VII because acid content is less, absorbs difficulty from level Four washing tower top acid mist out, and therefore directly entering into the oxynitride treatment unit carries out conversion processing, and conversion of nitrogen oxides is become nitrogen and water vapour qualified discharge.
The concentration of regenerating acid is definite according to the waste mixed acid of different concns, and the composition of regenerating acid is: nitric acid and hydrofluoric acid.Waste mixed acid reaches 60% through the nitric acid rate of recovery after regenerating in this example, and hydrofluoric acid reclaims and reaches 97%.(hydrofluoric acid in the regenerating acid and nitric acid are from waste mixed acid)
The contrast base figure of the nitric acid rate of recovery of the present invention is the nitrate ion content in the waste mixed acid, and the contrast base figure of the hydrofluoric acid rate of recovery is fluorion total amount in the waste mixed acid.
Specific algorithm:
Claims (1)
1. method of processing waste mixed acid, described waste mixed acid are the waste mixed acids that acid-washing stainless steel produces, and the waste mixed acid composition is nitric acid, hydrofluoric acid, iron ion, ferric fluoride and iron nitrate, and it comprises following step successively:
I is input to the waste mixed acid of acid-washing stainless steel line discharging the top of upgrading tower with sour pump, and directly contact with acid mist gas that stoving oven top flue is discharged and to carry out heat exchange, waste mixed acid is heated to 75 ± 5 ℃ by the top lance of pump delivery to stoving oven, by spray gun acid mist is ejected into and carries out roasting in the stoving oven, temperature in the stoving oven is 750 ± 20 ℃, waste mixed acid carries out thermal degradation, evaporation in stoving oven, metal ion is deposited to the stoving oven bottom and automatically collects the brown iron oxide collection device by pipeline with oxide form; The acid mist that waste mixed acid produces after roasting, 280 ± 10 ℃ of acid mist temperature are discharged to the bottom of upgrading tower by the flue at stoving oven top under the negative pressure of acid fog blower fan;
The II acid mist directly contacts with waste mixed acid in upgrading tower from the bottom to top, carries out heat exchange, and waste mixed acid is heated, and acid mist gas is cooled to 90 ± 2 ℃, and cooled gas enters into the bottom of one-level washing tower under the effect of pipeline at acid fog blower fan;
Temperature in the III one-level washing tower is 80 ± 2 ℃, and wherein 30 ± 2% acid mist is at the water formation regenerating acid of one-level washing tower with input one-level washing tower, and regenerating acid to the acid-washing stainless steel unit, is used for stainless steel production pickling through pump delivery;
IV enters acid mist pipeline through the unabsorbed acid mist of one-level washing tower under the effect of acid fog blower fan, acid mist pipeline is installed droplet separator, the liquid self-flowing of the acid mist condensation of collecting in the droplet separator is to the bottom of secondary washing tower, acid mist is contacted with water in the moving process of top by the bottom of secondary washing tower, wherein 20 ± 2% acid mist this and water form concentration lower contain sour water;
V enters acid mist pipeline through the acid mist of secondary washing tower under the effect of acid fog blower fan, acid mist pipeline is installed droplet separator, the bottom of liquid self-flowing to the three grade washing tower of the acid mist condensation of collecting in the droplet separator, acid mist is contacted with water in the moving process of top by the bottom of three grades of washing towers, wherein 10 ± 2%% acid mist this and water form concentration lower contain sour water;
VI enters acid mist pipeline through the acid mist of three grades of washing towers under the effect of acid fog blower fan, acid mist pipeline is installed droplet separator, the liquid self-flowing of the acid mist condensation of collecting in the droplet separator is to the bottom of level Four washing tower, acid mist is contacted with water in the moving process of top by the bottom of level Four washing tower, wherein 5 ± 2% acid mist this and water form concentration lower contain sour water, contain sour water and be disposed to neutralization station and carry out neutralizing treatment;
VII directly enters into the oxynitride treatment unit from level Four washing tower top acid mist out and carries out conversion processing, and conversion of nitrogen oxides is become nitrogen and water vapour qualified discharge.
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| CN2012100921479A CN103319038A (en) | 2012-03-23 | 2012-03-23 | Processing method for waste mixed acid |
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| CN2012100921479A CN103319038A (en) | 2012-03-23 | 2012-03-23 | Processing method for waste mixed acid |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104310690A (en) * | 2014-10-28 | 2015-01-28 | 中冶南方工程技术有限公司 | Process of regenerating metal nitric acid and hydrofluoric acid pickling wastewater and recycling metal elements |
| CN107601605A (en) * | 2017-10-20 | 2018-01-19 | 鞍山创新废酸除硅再生工程有限公司 | A kind of technique and system for improving stainless steel acid-washing waste liquid nitric acid regeneration yield |
| CN109467065A (en) * | 2018-11-30 | 2019-03-15 | 中冶南方工程技术有限公司 | A kind of stainless steel mixed acid waste liquor regenerated acid equipment |
| CN111704344A (en) * | 2020-06-05 | 2020-09-25 | 中冶南方工程技术有限公司 | Acid pickling process waste zero-emission recycling treatment device and process |
| WO2021017940A1 (en) * | 2019-07-29 | 2021-02-04 | 中冶南方工程技术有限公司 | Method for hazard-free treatment of sludge from spent solution of mixed acids after acid washing of stainless steel |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104310690A (en) * | 2014-10-28 | 2015-01-28 | 中冶南方工程技术有限公司 | Process of regenerating metal nitric acid and hydrofluoric acid pickling wastewater and recycling metal elements |
| CN104310690B (en) * | 2014-10-28 | 2016-01-20 | 中冶南方工程技术有限公司 | Metal nitrate, the regeneration of hydrofluoric acid spent pickle liquor and the recovery process of metallic element |
| CN107601605A (en) * | 2017-10-20 | 2018-01-19 | 鞍山创新废酸除硅再生工程有限公司 | A kind of technique and system for improving stainless steel acid-washing waste liquid nitric acid regeneration yield |
| CN107601605B (en) * | 2017-10-20 | 2023-05-09 | 鞍山创鑫环保科技股份有限公司 | Technology and system for improving yield of regenerated nitric acid from stainless steel pickling waste liquid |
| CN109467065A (en) * | 2018-11-30 | 2019-03-15 | 中冶南方工程技术有限公司 | A kind of stainless steel mixed acid waste liquor regenerated acid equipment |
| CN109467065B (en) * | 2018-11-30 | 2023-09-19 | 中冶南方工程技术有限公司 | Stainless steel mixed acid waste liquid regenerated acid equipment |
| WO2021017940A1 (en) * | 2019-07-29 | 2021-02-04 | 中冶南方工程技术有限公司 | Method for hazard-free treatment of sludge from spent solution of mixed acids after acid washing of stainless steel |
| CN111704344A (en) * | 2020-06-05 | 2020-09-25 | 中冶南方工程技术有限公司 | Acid pickling process waste zero-emission recycling treatment device and process |
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Application publication date: 20130925 |