CN105480988B - A kind of method that high-purity ammonium salt is prepared from impurity ammonium salt waste liquid high - Google Patents
A kind of method that high-purity ammonium salt is prepared from impurity ammonium salt waste liquid high Download PDFInfo
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- CN105480988B CN105480988B CN201510937718.8A CN201510937718A CN105480988B CN 105480988 B CN105480988 B CN 105480988B CN 201510937718 A CN201510937718 A CN 201510937718A CN 105480988 B CN105480988 B CN 105480988B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/28—Methods of preparing ammonium salts in general
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/047—Treatment of water, waste water, or sewage by heating by distillation or evaporation using eolic energy
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/048—Purification of waste water by evaporation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
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Abstract
The present invention relates to sewage treatment area, and in particular to a kind of multinomial technology of combination effectively processes the technique that impurity high ammonia-nitrogen wastewater high reclaims ammonium salt.Ammonium salt is including ammonium chloride, ammonium sulfate, ammonium nitrate and ammonium phosphate salt etc., the impurity high ammonia-nitrogen wastewater high for producing in process of production is after CNO oil expeller efficient degreasings, using continuous level Four overflow consersion unit, pH adjusting agent regulation solution is added in first order reactive tank, the second level to fourth stage reactive tank generates the ammonium salt solution of corresponding high concentration high-purity by processing.During ammonium salt solution pumped into triple effect evaporator, the ammonium salt of crystallization is separated and dried by centrifuge, finally obtain ammonium salt product, condensed water is arranged with fourth stage reactive tank water outlet ammonia nitrogen for production or outward.The ammonium salt product purity that this technique productions goes out is high, realizes the zero-emission to ammonia nitrogen waste water.The present invention has technological operation simple, and labour intensity is low, does not cause environmental pollution, meets clean production standard, is adapted to large-scale production.
Description
Technical field
The invention belongs to sewage treatment area, and in particular to one kind effectively processes impurity high ammonia nitrogen high and gives up with reference to multinomial technology
The technique of water.
Background technology
In non-ferrous metal wet smelting process, such as in extraction puies forward cobalt technical process, through frequently with ammoniacal liquor to organic
Mutually carry out saponification；Such as in compound synthesis technology, synthesis filtered fluid and ion exchange process etc. contain substantial amounts of height
Impurity high-concentration ammonia nitrogenous wastewater.Because its discharge capacity is big, complicated component, strong toxicity is big to environmental hazard, and intractability is big, such as
Directly to discharging ammonia nitrogen waste water in environment, will certainly polluted river, soil, wide range of pollution can be caused to environment, also make
Into the waste of water resource.Treatment high-concentration ammonia nitrogenous wastewater reclaims ammonium sulfate technology at present purification by liquid extraction method, chemical precipitation method, sky
Gas blow-off method, zeolite deamination method etc..Purification by liquid extraction method be using heavy metal components such as cobalt, nickel, the magnesium in extract and separate waste water, by
Big in ammonia nitrogen waste water amount, one time cost of investment is high with operating cost, while the heavy metal separated also is difficult to further purification
Treatment, selective to metal along with extracting, the ammonium salt product impurity content of production is high, it is impossible to further purification；Chemistry is heavy
Using sodium hydrate regulator solution pH value or using precipitation of heavy metals such as vulcanized sodium, fluorides in the method for shallow lake, although can effectively go
Removing heavy metals, reach discharge of wastewater requirement, but due to such chemical raw material selling at exorbitant prices, are difficult to realize large-scale industry metaplasia
Produce.Therefore, this causes that the improvement of high-concentration ammonia nitrogenous wastewater is constantly subjected to the great attention of various countries' field of Environment Protection.
In the prior art, the method for production ammonium salt has a lot, but reclaims high-purity from the ammonium salt waste water of high impurity content
Ammonium salt product yet there are no corresponding report.Therefore, a kind of new technology for processing impurity high-concentration ammonia nitrogenous wastewater high, Ji Nengman are developed
Sufficient discharged wastewater met the national standard, it is problem demanding prompt solution in treatment high-concentration ammonia nitrogenous wastewater that the ammonium salt in waste water can be reclaimed again.
The content of the invention
(1) technical problem to be solved
The present invention produces impurity high and high-concentration ammonia nitrogenous wastewater conventional processes to overcome non-ferrous metal hydrometallurgy
The complicated, shortcoming of high cost, the technical problem to be solved in the present invention is to provide a kind of process is simple, low cost, is located by reasonable
Reason impurity concentration high ammonia-nitrogen wastewater high, reaches realization and reclaims ammonium salt simultaneously, the purpose of wastewater zero discharge.
(2) technical scheme
In order to solve the above-mentioned technical problem, high-purity ammonium is prepared from impurity ammonium salt waste liquid high the invention provides such a
The method of salt, it is specific as follows：
Step one:The ammonia nitrogen waste water of the high impurity content produced from production workshop section is in advance through CNO oil expeller efficient degreasings；
Step 2:Using continuous level Four overflow consersion unit, pH adjusting agent regulation solution is added in first order reactive tank
PH is more than 11, and the second level to fourth stage reactive tank is warming up to more than 85 DEG C by outer supplying heat source, while carrying out air blast；
Step 3:Combined using film tower and inhale ammonia technique, ammonia is absorbed with film in advance in absorption tower, using two stage countercurrents
Diluted acid is sprayed, and prepares the ammonium salt solution of high concentration high-purity；
Step 4:During ammonium salt solution pumped into triple effect evaporator, MVR is used to provide secondary heat source for triple effect evaporator, when
Part solution pumps into crystallization in crystallizer when Baume degrees reaches 30~50 ° of B é, is separated the ammonium salt of crystallization by centrifuge
And dry, finally obtain corresponding ammonium salt product；
Step 5:The water outlet of fourth stage reactive tank is less than 8mg/L, reuse or outer row with ammonia control in the condensed water of evaporation,
Sold after filtering the filter residue drying for producing.
Preferably, the ammonium salt of preparation is mainly including ammonium chloride, ammonium sulfate, ammonium nitrate and MAP etc..
Preferably, the CNO-2 type resins for being used in CNO oil expellers in the step one, control waste liquid in oil content≤
1ppm。
Preferably, pH adjusting agent is one kind of quick lime or white lime in the step 2.
Preferably, 20~40m of waste liquid flooding velocity in the step 23/ h, blast velocity is 200~600m3/h。
Preferably, the acid solution for being used in the step 3 is sulfuric acid, hydrochloric acid, nitric acid, one kind of phosphoric acid solution.
Preferably, it is more than 95 DEG C that a heating steam temperature is used in the step 4, through the secondary heat source that MVR is supplied
Temperature is more than 90 DEG C.
Preferably, the ammonium salt product for being produced in the step 4 can reach industrial Grade A requirement.
Preferably, in the step 5 condensed water of reuse and fourth stage reactive tank water outlet ammonia nitrogen in below 8mg/L, reuse
Or outer row.
Preferably, MVR described in the step 4 is mechanical steam recompression technology.
(3) beneficial effect
A. ammonium salt waste liquor PH is adjusted using quick lime or white lime in this technique, with low cost, system itself provides heat
Amount, greatlys save the energy.
B. the ammonium salt product of this technique productions reaches industrial Grade A requirement.
C. this technique uses CNO oil expeller efficient degreasings, greatly reduces containing the oil content in waste liquor of ammonium.
D. this technique is mutually tied when ammonia is reclaimed using the membrane method ammonia recovery technology tower technology that reclaims inversely spraying with two grades
Close, greatly improve the rate of recovery of ammonia.
E. this technique contributes to ammonia to escape during ammonium salt waste water is processed by ventilation, and recycle-water ammonia nitrogen is smaller than
8mg/L, useful resources are recycled completely, not only solve pollution problem, also achieve certain economic benefit, are reached
Wastewater zero discharge.
F. technique is combined with triple effect evaporator using MVR technologies in this technique, compared with other techniques, is greatlyd save
Energy consumption.
Brief description of the drawings
Fig. 1 is that ammonium salt crystal process chart is reclaimed in impurity ammonium salt waste water high purification.
Specific embodiment
With reference to embodiment, the present invention is further illustrated.
Embodiment 1
Containing NH4 +Concentration for 8g/L impurity ammonium chloride waste-water high, by CNO high-efficiency degreasing devices carry out oil removing to 1ppm with
Under, liquid enters continuous level Four regulation pH reactive tanks after oil removing, adds quick lime in first order reactive tank under agitation, adjusts
Solution final pH is 11, and flooding velocity is 20m3/ h, starts to warm up and is with ventilation, wind speed successively since the reactive tank of the second level
200m3/ h, 85 DEG C of temperature, fourth stage reactive tank overfall ammonia nitrogen is overanxious less than being carried out after 8mg/L, and embrane method is used in absorption tower
Ammonia recovery technology reclaims NH3, sprayed using the concentration watery hydrochloric acid of two stage countercurrent 5%, prepare high strength ammonium-chloride solution.It is most laggard
Entering triple effect evaporator carries out condensing crystallizing, and more than 95 DEG C of primary steam temperature uses MVR to provide second heat for triple effect evaporator
Source, more than 90 DEG C of indirect steam temperature, when ammonium chloride solution Baume degrees is 40 ° of B é in crystallizing pan, is opened discharge valve and is gone out
Material, into horizontal spiral centrifuge, the ammonium chloride after crystallization is separated, and dried ammonium chloride packaging and storage.Point
Liquid after is back to mother liquor pond and is concentrated again, recycling condensing water or discharge that this technique is produced, filters the filter for producing
Sold after slag drying.
The ammonium chloride constituent analysis table of table 1
Embodiment 2
Containing NH4 +Concentration for 24g/L impurity ammonium sulfate waste water high, by CNO high-efficiency degreasing devices carry out oil removing to 1ppm with
Under, liquid enters continuous level Four regulation pH reactive tanks after oil removing, adds white lime in first order reactive tank under agitation, adjusts
Solution final pH is 12, and flooding velocity is 25m3/ h, starts to warm up and is with ventilation, wind speed successively since the reactive tank of the second level
250m3/ h, 85 DEG C of temperature, fourth stage reactive tank overfall ammonia nitrogen is overanxious less than being carried out after 8mg/L, and embrane method is used in absorption tower
Ammonia recovery technology reclaims NH3, sprayed using the concentration dilute sulfuric acid of two stage countercurrent 8%, prepare high-concentration sulfuric acid ammonium salt solution.It is most laggard
Entering triple effect evaporator carries out condensing crystallizing, and more than 95 DEG C of primary steam temperature uses MVR to provide second heat for triple effect evaporator
Source, more than 90 DEG C of indirect steam temperature, when ammonia nitrogen liquid Baume degrees high is 45 ° of B é in crystallizing pan, is opened discharge valve and is gone out
Material, into horizontal spiral centrifuge, the ammonium sulfate after crystallization is separated, and dried ammonium sulfate packaging and storage.Point
Liquid after is back to mother liquor pond and is concentrated again, recycling condensing water or discharge that this technique is produced, filters the filter for producing
Sold after slag drying.
The ammonium sulfate constituent analysis table of table 2
Embodiment 3
Containing NH4 +Concentration for 25g/L impurity ammonium nitrate wastewater high, by CNO high-efficiency degreasing devices carry out oil removing to 1ppm with
Under, liquid enters continuous level Four regulation pH reactive tanks after oil removing, adds quick lime in first order reactive tank under agitation, adjusts
Solution final pH is 12, and flooding velocity is 35m3/ h, starts to warm up and is with ventilation, wind speed successively since the reactive tank of the second level
400m3/ h, 85 DEG C of temperature, fourth stage reactive tank overfall ammonia nitrogen is overanxious less than being carried out after 8mg/L, and embrane method is used in absorption tower
Ammonia recovery technology reclaims NH3, sprayed using the concentration dust technology of two stage countercurrent 8%, prepare high concentration ammonium nitrate solution.It is most laggard
Entering triple effect evaporator carries out condensing crystallizing, and more than 95 DEG C of primary steam temperature uses MVR to provide second heat for triple effect evaporator
Source, more than 90 DEG C of indirect steam temperature, when ammonia nitrogen liquid Baume degrees high is 50 ° of B é in crystallizing pan, is opened discharge valve and is gone out
Material, into horizontal spiral centrifuge, the ammonium nitrate after crystallization is separated, and dried ammonium nitrate packaging and storage.Point
Liquid after is back to mother liquor pond and is concentrated again, recycling condensing water or discharge that this technique is produced, filters the filter for producing
Sold after slag drying.
The ammonium nitrate component analytical table of table 3
| Nitrogen content (in terms of butt) % | Acidity | Ignition residue % | |
| 99.5 | 0.42 | Methyl orange indicator does not develop the color | 0.05 |
Embodiment 4
Containing NH4 +Concentration for 15g/L impurity ammonium phosphate waste water high, by CNO high-efficiency degreasing devices carry out oil removing to 1ppm with
Under, liquid enters continuous level Four regulation pH reactive tanks after oil removing, adds quick lime in first order reactive tank under agitation, adjusts
Solution final pH is 12, and flooding velocity is 25m3/ h, starts to warm up and is with ventilation, wind speed successively since the reactive tank of the second level
400m3/ h, 85 DEG C of temperature, fourth stage reactive tank overfall ammonia nitrogen is overanxious less than being carried out after 8mg/L, and embrane method is used in absorption tower
Ammonia recovery technology reclaims NH3, two stage countercurrent concentration are used for 25% phosphoric acid is sprayed, by degree of neutralization control in 1.00 or so, system
Standby high-concentration phosphoric acid ammonium salt solution.Finally entering triple effect evaporator carries out condensing crystallizing, and more than 95 DEG C of primary steam temperature is used
MVR provides secondary heat source, more than 90 DEG C of indirect steam temperature, when solution Baume degrees is 45 ° of B é in crystallizing pan for triple effect evaporator
When, then turn on discharge valve and discharged, into horizontal spiral centrifuge, the MAP after crystallization is separated, and
Dried MAP packaging and storage.Liquid after separation is back to mother liquor pond and is concentrated again, what this technique was produced
Recycling condensing water or discharge, sell after filtering the filter residue drying for producing.
The MAP constituent analysis table of table 4
Claims (9)
1. a kind of method that high-purity ammonium salt is prepared from impurity ammonium salt waste liquid high, it is characterised in that comprise the following steps：
Step one:The ammonia nitrogen waste water of the high impurity content produced from production workshop section is in advance through CNO oil expeller efficient degreasings；
Step 2:Using continuous level Four overflow consersion unit, addition pH adjusting agent regulation pH value of solution is in first order reactive tank
More than 11, the second level to fourth stage reactive tank is warming up to more than 85 DEG C by outer supplying heat source, while carrying out air blast；
Step 3:Combined using film tower and inhale ammonia technique, ammonia is absorbed with film in advance in absorption tower, using two stage countercurrent diluted acids
Spray, prepares the ammonium salt solution of high concentration high-purity；
Step 4:During ammonium salt solution pumped into triple effect evaporator, use MVR to provide secondary heat source for triple effect evaporator, work as Baume
Part solution pumps into crystallization in crystallizer when degree reaches 30~50 ° of B é, and the ammonium salt of crystallization is separated and dried by centrifuge
It is dry, finally obtain corresponding ammonium salt product；
Step 5:The water outlet of fourth stage reactive tank is less than 8mg/L, reuse or outer row, filtering with ammonia control in the condensed water of evaporation
Sold after the filter residue drying of generation.
2. a kind of method that high-purity ammonium salt is prepared from impurity ammonium salt waste liquid high according to claim 1, it is characterised in that institute
State the CNO-2 type resins used in CNO oil expellers in step one, oil content≤1ppm in control waste liquid.
3. a kind of method that high-purity ammonium salt is prepared from impurity ammonium salt waste liquid high according to claim 1, it is characterised in that institute
PH adjusting agent is quick lime or one kind of white lime in stating step 2.
4. a kind of method that high-purity ammonium salt is prepared from impurity ammonium salt waste liquid high according to claim 1, it is characterised in that institute
State 20~40m of waste liquid flooding velocity in step 23/ h, blast velocity is 200~600m3/h。
5. a kind of method that high-purity ammonium salt is prepared from impurity ammonium salt waste liquid high according to claim 1, it is characterised in that institute
It is sulfuric acid, hydrochloric acid, nitric acid, one kind of phosphoric acid solution to state the acid solution used in step 3.
6. a kind of method that high-purity ammonium salt is prepared from impurity ammonium salt waste liquid high according to claim 1, it is characterised in that institute
It is more than 95 DEG C to state and use in step 4 a heating steam temperature, and the secondary heat source temperature supplied through MVR is more than 90 DEG C.
7. a kind of method that high-purity ammonium salt is prepared from impurity ammonium salt waste liquid high according to claim 1, it is characterised in that institute
State the ammonium salt product produced in step 4 and can reach industrial Grade A requirement.
8. a kind of method that high-purity ammonium salt is prepared from impurity ammonium salt waste liquid high according to claim 1, it is characterised in that institute
The condensed water and fourth stage reactive tank water outlet ammonia nitrogen of reuse in step 5 are stated in below 8mg/L, reuse or outer row.
9. a kind of method that high-purity ammonium salt is prepared from impurity ammonium salt waste liquid high according to claim 1, it is characterised in that institute
MVR described in step 4 is stated for mechanical steam recompression technology.
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| CN106746114A (en) * | 2016-12-18 | 2017-05-31 | 南通江山农药化工股份有限公司 | The production method of amide-type by-product industrial ammonium chloride |
| CN107352726A (en) * | 2017-09-05 | 2017-11-17 | 陈雪薇 | A kind of MVR ammonia still processs recovery ammonium sulfate processing high ammonia-nitrogen wastewater technology |
| CN108275819B (en) * | 2018-02-06 | 2020-07-10 | 华友新能源科技（衢州）有限公司 | Method for recycling ternary precursor washing wastewater |
| CN110002474A (en) * | 2019-05-06 | 2019-07-12 | 澧县腾飞化工有限公司 | Ammonia recovery technique containing ammonium salt solution after a kind of purification of potassium nitrate crude product |
| CN110482740B (en) * | 2019-08-16 | 2023-09-01 | 联峰钢铁（张家港）有限公司 | Sewage acid treatment method |
| CN110342720A (en) * | 2019-08-19 | 2019-10-18 | 常州中源工程技术有限公司 | Ammonium sulfate waste water MVR evaporates deamination processing system and its treatment process |
| CN110697814B (en) * | 2019-09-29 | 2021-09-03 | 赣州腾远钴业新材料股份有限公司 | Ammonia-containing sulfate wastewater treatment system and process |
| CN111017961A (en) * | 2019-12-31 | 2020-04-17 | 贵州瓮福蓝天氟化工股份有限公司 | Method for preparing sodium fluoride and ammonium salt from fluorine-containing ammonia nitrogen wastewater |
| CN112357934B (en) * | 2020-11-13 | 2023-03-14 | 江西思远再生资源有限公司 | Method for preparing ammonia water and anhydrous calcium chloride from ammonium salt solution |
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