CN104710037B - A kind of method of ammonium salt waste water deliming - Google Patents
A kind of method of ammonium salt waste water deliming Download PDFInfo
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Abstract
The present invention relates to a kind of method of ammonium salt waste water deliming, hydrometallurgy field of waste water treatment is applied particularly to；The calcium removal methods being related in the present invention comprise the following steps：Step one：Ammoniacal liquor is added into ammonium salt waste water or liquefied ammonia is pre-processed, and the hydroxyl concentration in regulation ammonium salt waste water makes ammonium salt waste water in alkalescence；Step 2：NH is added in the ammonium salt waste water obtained to step one4HCO3Depth deliming is carried out, reaction temperature is controlled at 20~60 DEG C；Step 3：The ammonium salt waste water obtained in step 2 is subjected to separation of solid and liquid, solid and waste water solution is obtained, Ca in the waste water solution after separation of solid and liquid2+≤20mg/L；Due to calcium concentration relatively low in waste water so that ammonium salt reclamation process fouling risk is substantially reduced, the product purity of output is high；Processing ammonium salt waste water can accomplish that waste water is recycled completely in this way, discharge factory without any waste liquid, can accomplish wastewater zero discharge, there is very big value to enterprise or even entire society.
Description
Technical field
The present invention relates to a kind of method of ammonium salt waste water deliming, hydrometallurgy field of waste water treatment is applied particularly to.
Background technology
Existing ammonium salt waste water can be to people when being and containing a large amount of ammonium salt waste water in the important pollutant of pollutant water body, water body
Class and animals and plants cause great damage, hydrometallurgy enterprise can produce in process of production one complicated component, amounts of ammonium salt compared with
High waste water, its content is significantly larger than national sewage discharge requirement, and because the processing of its complicated component is more difficult, processing cost
It is higher it is also possible to causing secondary pollution.The method of processing ammonium salt waste water has following several at present：Break point chlorination, stripping deamination
Outside method, chemical precipitation method etc., upper described method discharged wastewater met the national standard, the waste water of discharge are intended merely to including some other method
In also have that substantial amounts of ammonium salt is unrecovered to cause the waste of water and ammonium salt, while secondary pollution be able to can be produced in processing procedure.
Compare many processing methods at present and use counter-infiltration-electroosmose process, divided ammonium salt and water using the characteristic of film
From this method is easy to operate, and collection efficiency of ammonium salts is high, but must be pre-processed in the presence of higher calcium content in waste water, otherwise can
Cause fouling and influence equipment to run.
The method of ammonium salt waste water deliming mainly has：
1st, ion-exchange, using ion exchange resin to Ca2+Ion exchange is carried out to reach and remove in ammonium salt waste water to purify
The purpose of calcium, this method water outlet Ca2+Content is very low, but ion exchange resin is needed at the operation such as regeneration, regeneration and regenerated liquid
Reason is costly, and is not suitable for high concentration calcic waste water；
2nd, calcium phosphate precipitation：By adding phosphate into waste water, because calcium phosphate is insoluble in the characteristic deliming of water, remove
Calcium is worked well, but the introducing of phosphate radical can be enriched with during subsequent concentration or evaporation process, cause subsequent product purity
It is affected.
The content of the invention
The invention provides a kind of method of ammonium salt waste water deliming, the difficulty of current ammonium salt Wastewater Pretreatment deliming is solved
Topic, makes calcium precipitate without influenceing subsequent product purity, with very high economic benefit and social benefit by adding a small amount of reagent.
The calcium removal methods being related in the present invention comprise the following steps：
Step one：Ammoniacal liquor is added into ammonium salt waste water or liquefied ammonia is pre-processed, the hydroxyl in regulation ammonium salt waste water
Concentration, makes ammonium salt waste water in alkalescence；
Step 2：NH is added in the ammonium salt waste water obtained to step one4HCO3Depth deliming is carried out, reaction temperature control exists
20~60 DEG C；
Step 3：The ammonium salt waste water obtained in step 2 is subjected to separation of solid and liquid, solid and waste water solution is obtained, by solid
Ca in waste water solution after liquid separation2+≤20mg/L。
Preferably, the ammonium salt waste water in a kind of method of described ammonium salt waste water deliming is mainly derived from hydrometallurgy, institute
The ammonium salt stated mainly includes the NH in the one or more in ammonium chloride, ammonium sulfate, ammonium nitrate, the ammonium salt waste water4 +Concentration is 5
~60g/L, Ca2+Concentration is 0.1~10g/L.
Preferably, the addition ammoniacal liquor or liquefied ammonia and Ca in a kind of method of described ammonium salt waste water deliming2+Molar ratio
For 0.2~1.5, preferred molar ratio value is 0.5~1；The reaction time added after ammoniacal liquor or liquefied ammonia is 5 minutes~120 minutes, excellent
It is 30 minutes~90 minutes to select the reaction time.
Preferably, the addition NH in a kind of method of described ammonium salt waste water deliming4HCO3With Ca2+Mol ratio be 0.5
~5, preferred molar ratio value is 2~4, adds NH4HCO3Reaction time afterwards is 5 minutes~120 minutes, and preferred reaction time is
30 minutes~90 minutes.
Preferably, the separation of solid and liquid in a kind of method of described ammonium salt waste water deliming using gravitational settling, tubular type micro-filtration,
One or more combination in sloping plate deposition, tube settling, multi-medium filtering, ultrafiltration, it is heavy using swash plate (pipe) precipitation or gravity
Its water outlet SS≤50mg/L drops, and turbidity≤30NTU is follow-up to carry out multi-medium filtering and ultrafiltration progress secondary filter, makes solid-liquid point
Separate out water SS≤3mg/L, turbidity≤1NTU；If the solution obtained in step 2 directly carries out separation of solid and liquid using tube type filter membrance,
Water outlet is that can reach SS≤3mg/L.
Preferably, the ammonium salt waste water after separation of solid and liquid in a kind of method of described ammonium salt waste water deliming uses acid
PH=6~8 are adjusted, condensing crystallizing is carried out using embrane method and MVR to the ammonium salt waste water after toning pH, ammonium salt is reclaimed.
Because the medicament added in such scheme is the compound of ammonia, while deliming does not introduce new impurity, to calcium
Removal effect is good, Ca in ammonium salt waste water after deliming2+≤ 20mg/L, makes during follow-up ammonium salt reclamation without fouling risk, ammonium salt is pure
Degree is high.
Brief description of the drawings
Fig. 1 is to carry out separation of solid and liquid ammonium salt waste water deliming and ammonium salt reclamation work using gravitational settling or swash plate (pipe) precipitation
Skill flow chart.
Fig. 2 is to use the ammonium salt waste water deliming of tube type filter membrance separation of solid and liquid and ammonium salt reclamation process chart.
Embodiment
Referring to the drawings, to the present invention technique carry out step one processing, i.e., added into ammonium salt waste water a certain amount of ammoniacal liquor/
Hydroxyl concentration in liquefied ammonia, regulation waste water, enters step 2 after question response certain time；The ammonium salt that step one is obtained is given up
Water adds a certain amount of NH4HCO3Carry out depth deliming, NH4HCO3The product for reacting generation with ammoniacal liquor/liquefied ammonia and calcium continues to react life
Into the precipitation of calcium carbonate of indissoluble, the purpose of calcium removing is reached, makes Ca2+≤ 20mg/L, it is solid that depth deliming, which produces water into step 3,
Liquid separating treatment；
Step 3 is implemented by two kinds of separation of solid and liquid patterns：
1st, as shown in Figure 2, deliming production water step 2 obtained is handled with tubular type micro-filtration, the ammonium after depth deliming
Salt waste water is carried out after separation of solid and liquid operation, and most of calcium carbonate granule is separated in solid slurry form with ammonium salt waste water, point
PH regulations are carried out from obtained ammonium salt solution；
2nd, as shown in Figure 1, deliming step 2 obtained is produced water and settled according to swash plate (pipe), at gravitational settling
Reason, the then supernatant (ammonium salt solution) isolated is filtered into multi-medium filtering, and multi-medium filtering water outlet enters ultrafiltration, most
Whole water outlet SS and turbidity meet ammonium salt reclamation procedure calls, and ultra-filtration water carries out pH regulations；
The separation of solid and liquid water outlet acid adding that step 3 is obtained adjusts pH=6~8, and the ammonium salt waste water after toning pH can be adopted
Condensing crystallizing is carried out with embrane method and MVR, ammonium salt is reclaimed.
Ammonium salt waste water after step 3 is handled can enter ammonium salt reclamation process, because calcium relatively low in waste water is dense
Degree so that ammonium salt reclamation process fouling risk is substantially reduced, the product purity of output is high；Processing ammonium salt waste water can be with this way
Accomplish that waste water is recycled completely, discharge factory without any waste liquid, wastewater zero discharge can be accomplished, had to enterprise or even entire society
Very big value.
This method focuses on pre- deliming and depth deliming additional examination dosage and reaction time, therefore only useless to ammonium salt in embodiment
Calcium ion concentration, the depth deliming additional examination parameter such as dosage and reaction time are investigated in the temperature of water, ammonium salt waste water, and right
The processes such as follow-up separation of solid and liquid are repeated no more.
1st, 20 DEG C of control ammonium salt wastewater temperature, measures ammonium salt waste water Ca2+Concentration is 8g/L, and ammoniacal liquor/liquefied ammonia is added and Ca2+
Mol ratio be 0.2,30 minutes reaction time；NH4HCO3With Ca2+Mol ratio be 0.5, the reaction time be 30 minutes, reaction
Suction filtration is carried out to ammonium salt waste water after finishing, ammonium salt waste water Ca is measured2+Concentration is 7.8g/L；
2nd, 20 DEG C of control ammonium salt wastewater temperature, measures ammonium salt waste water Ca2+Concentration is 8g/L, and ammoniacal liquor/liquefied ammonia is added and Ca2+
Mol ratio be 0.2,120 minutes reaction time；NH4HCO3With Ca2+Mol ratio be 0.5, the reaction time be 120 minutes, instead
Suction filtration is carried out to ammonium salt waste water after should finishing, ammonium salt waste water Ca is measured2+Concentration is 6.5g/L；
3rd, 20 DEG C of control ammonium salt wastewater temperature, measures ammonium salt waste water Ca2+Concentration is 0.8g/L, and ammoniacal liquor/liquefied ammonia is added and Ca2 +Mol ratio be 0.2,30 minutes reaction time；NH4HCO3With Ca2+Mol ratio be 0.5, the reaction time be 30 minutes, reaction
Suction filtration is carried out to ammonium salt waste water after finishing, ammonium salt waste water Ca is measured2+Concentration is 0.75g/L；
4th, 20 DEG C of control ammonium salt wastewater temperature, measures ammonium salt waste water Ca2+Concentration is 0.8g/L, and ammoniacal liquor/liquefied ammonia is added and Ca2 +Mol ratio be 0.2,120 minutes reaction time；NH4HCO3With Ca2+Mol ratio be 0.5, the reaction time be 120 minutes, instead
Suction filtration is carried out to ammonium salt waste water after should finishing, ammonium salt waste water Ca is measured2+Concentration is 0.67g/L；
5th, 60 DEG C of control ammonium salt wastewater temperature, measures ammonium salt waste water Ca2+Concentration is 0.8g/L, and ammoniacal liquor/liquefied ammonia is added and Ca2 +Mol ratio be 0.2,120 minutes reaction time；NH4HCO3With Ca2+Mol ratio be 0.5, the reaction time be 120 minutes, instead
Suction filtration is carried out to ammonium salt waste water after should finishing, ammonium salt waste water Ca is measured2+Concentration is 0.62g/L；
6th, 20 DEG C of control ammonium salt wastewater temperature, measures ammonium salt waste water Ca2+Concentration is 0.8g/L, and ammoniacal liquor/liquefied ammonia is added and Ca2 +Mol ratio be 1.5,5 minutes reaction time；NH4HCO3With Ca2+Mol ratio be 8, the reaction time be 5 minutes, reaction is finished
Suction filtration is carried out to ammonium salt waste water afterwards, ammonium salt waste water Ca is measured2+Concentration is 0.05g/L；
7th, 20 DEG C of control ammonium salt wastewater temperature, measures ammonium salt waste water Ca2+Concentration is 0.8g/L, and ammoniacal liquor/liquefied ammonia is added and Ca2 +Mol ratio be 1.5,120 minutes reaction time；NH4HCO3With Ca2+Mol ratio be 8, the reaction time be 120 minutes, reaction
Suction filtration is carried out to ammonium salt waste water after finishing, ammonium salt waste water Ca is measured2+Concentration is 3mg/L；
8th, 20 DEG C of control ammonium salt wastewater temperature, measures ammonium salt waste water Ca2+Concentration is 0.8g/L, and ammoniacal liquor/liquefied ammonia is added and Ca2 +Mol ratio be 1,60 minutes reaction time；NH4HCO3With Ca2+Mol ratio be 4, the reaction time be 60 minutes, reaction is finished
Suction filtration is carried out to ammonium salt waste water afterwards, ammonium salt waste water Ca is measured2+Concentration is 10mg/L；
9th, 40 DEG C of control ammonium salt wastewater temperature, measures ammonium salt waste water Ca2+Concentration is 0.8g/L, and ammoniacal liquor/liquefied ammonia is added and Ca2 +Mol ratio be 1,60 minutes reaction time；NH4HCO3With Ca2+Mol ratio be 4, the reaction time be 60 minutes, reaction is finished
Suction filtration is carried out to ammonium salt waste water afterwards, ammonium salt waste water Ca is measured2+Concentration is 8mg/L；
10th, 60 DEG C of control ammonium salt wastewater temperature, measures ammonium salt waste water Ca2+Concentration is 0.8g/L, ammoniacal liquor/liquefied ammonia add with
Ca2+Mol ratio be 1.5,120 minutes reaction time；NH4HCO3With Ca2+Mol ratio be 5, the reaction time be 120 minutes, instead
Suction filtration is carried out to ammonium salt waste water after should finishing, ammonium salt waste water Ca is measured2+Concentration is 2mg/L；
11st, 40 DEG C of control ammonium salt wastewater temperature, measures ammonium salt waste water Ca2+Concentration is 0.8g/L, ammoniacal liquor/liquefied ammonia add with
Ca2+Mol ratio be 1.5,120 minutes reaction time；NH4HCO3With Ca2+Mol ratio be 5, the reaction time be 120 minutes, instead
Suction filtration is carried out to ammonium salt waste water after should finishing, ammonium salt waste water Ca is measured2+Concentration is 2mg/L；
12nd, 40 DEG C of control ammonium salt wastewater temperature, measures ammonium salt waste water Ca2+Concentration is 0.8g/L, ammoniacal liquor/liquefied ammonia add with
Ca2+Mol ratio be 1,90 minutes reaction time；NH4HCO3With Ca2+Mol ratio be 2, the reaction time be 120 minutes, reaction
Suction filtration is carried out to ammonium salt waste water after finishing, ammonium salt waste water Ca is measured2+Concentration is 35mg/L；
13rd, 40 DEG C of control ammonium salt wastewater temperature, measures ammonium salt waste water Ca2+Concentration is 10g/L, and ammoniacal liquor/liquefied ammonia is added and Ca2 +Mol ratio be 1,90 minutes reaction time；NH4HCO3With Ca2+Mol ratio be 2, the reaction time be 90 minutes, reaction is finished
Suction filtration is carried out to ammonium salt waste water afterwards, ammonium salt waste water Ca is measured2+Concentration is 80mg/L；
14th, 40 DEG C of control ammonium salt wastewater temperature, measures ammonium salt waste water Ca2+Concentration is 10g/L, and ammoniacal liquor/liquefied ammonia is added and Ca2 +Mol ratio be 1,90 minutes reaction time；NH4HCO3With Ca2+Mol ratio be 2, the reaction time be 90 minutes, reaction is finished
Suction filtration is carried out to ammonium salt waste water afterwards, ammonium salt waste water Ca is measured2+Concentration is 80mg/L；
15th, 40 DEG C of control ammonium salt wastewater temperature, measures ammonium salt waste water Ca2+Concentration is 10g/L, and ammoniacal liquor/liquefied ammonia is added and Ca2 +Mol ratio be 1,90 minutes reaction time；NH4HCO3With Ca2+Mol ratio be 3, the reaction time be 90 minutes, reaction is finished
Suction filtration is carried out to ammonium salt waste water afterwards, ammonium salt waste water Ca is measured2+Concentration is 45mg/L.
In addition, the equivalent or simple change that all features and principle according to described in inventional idea of the present invention are done, is included in
In the protection domain of patent of the present invention；Those skilled in the art can do to described specific embodiment
It is various modification supplement or using similar mode substitute, without departing from the present invention structure or surmount this right
Scope defined in claim, all should belong to protection scope of the present invention.
Claims (3)
1. a kind of method of ammonium salt waste water deliming, it is characterised in that comprise the following steps：
Step one：Ammoniacal liquor is added into ammonium salt waste water or liquefied ammonia is pre-processed, the hydroxyl concentration in regulation ammonium salt waste water,
Make ammonium salt waste water in alkalescence；
Step 2：NH is added in the ammonium salt waste water obtained to step one4HCO3Carry out depth deliming, reaction temperature control 20~
60℃；
Step 3：The ammonium salt waste water obtained in step 2 is subjected to separation of solid and liquid, solid and waste water solution is obtained；
Ammonium salt waste water in the step one is mainly derived from hydrometallurgy, described ammonium salt mainly include ammonium chloride, ammonium sulfate,
NH in one or more in ammonium nitrate, the ammonium salt waste water4 +Concentration is 5~60g/L, Ca2+Concentration is 0.1~10g/L；
Ammoniacal liquor or liquefied ammonia and Ca are added in described step one2+Mol ratio be 0.2~1.5, add anti-after ammoniacal liquor or liquefied ammonia
It is 5 minutes~120 minutes between seasonable；
Described addition NH4HCO3With Ca2+Mol ratio be 0.5~5, add NH4HCO3Reaction time afterwards is 5 minutes~120
Minute；
Described separation of solid and liquid is used in gravitational settling, tubular type micro-filtration, sloping plate deposition, tube settling, multi-medium filtering, ultrafiltration
One or more combination；
Ca in waste water solution in described step three after separation of solid and liquid2+≤20mg/L；
Waste water in described step three after separation of solid and liquid uses acid for adjusting pH=6~8, and the ammonium salt after toning pH is given up
Water carries out condensing crystallizing using embrane method and MVR, reclaims ammonium salt.
2. the method for a kind of ammonium salt waste water deliming according to claim 1, it is characterised in that described addition ammoniacal liquor or liquid
Ammonia and Ca2+Mol ratio be 0.5~1, the reaction time added after ammoniacal liquor or liquefied ammonia is 30 minutes~90 minutes.
3. a kind of method of ammonium salt waste water deliming according to claim 1, it is characterised in that described addition NH4HCO3With
Ca2+Mol ratio be 2~4, add NH4HCO3Reaction time afterwards is 30 minutes~90 minutes.
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Denomination of invention: A method of removing calcium from ammonium salt wastewater Effective date of registration: 20220630 Granted publication date: 20170818 Pledgee: Hangzhou Qingchun sub branch of Guangfa Bank Co.,Ltd. Pledgor: HANGZHOU TIAN CHUANG ENVIRONMENTAL TECHNOLOGY Co.,Ltd. Registration number: Y2022330001189 |
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Date of cancellation: 20230629 Granted publication date: 20170818 Pledgee: Hangzhou Qingchun sub branch of Guangfa Bank Co.,Ltd. Pledgor: HANGZHOU TIAN CHUANG ENVIRONMENTAL TECHNOLOGY Co.,Ltd.|Zhejiang Yimo New Material Technology Co.,Ltd. Registration number: Y2022330001189 |