CN104724778B - Method for salt extraction from desulfurization waste solution through multi-effect evaporation - Google Patents
Method for salt extraction from desulfurization waste solution through multi-effect evaporation Download PDFInfo
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Abstract
The invention relates to a method for salt extraction from a desulfurization waste solution through multi-effect evaporation, and specifically relates to a method of multi-effect evaporation, crystallization, and extraction of mixed salt from the desulfurization waste solution of coal gases of the HPF method. With the method, continuous production can be realized, various heat can be recycled and utilized during production, tail gas can be treated, and operation environment is improved.
Description
Technical field
The present invention relates to a kind of method of desulfurization waste liquor multiple-effect evaporation salt extraction, specifically, the present invention relates to hpf method coal
The desulfurization waste liquor of gas carries out multiple-effect evaporation, crystallization, the method extracting mixed salt.
Background technology
Most of coal chemical enterprises adopt hpf method to remove the hydrogen sulfide in coke-stove gas at present, occur during desulfurization
A series of side reactions, create the salt side-product such as Ammonium hyposulfite., ammonium thiocyanate, ammonium sulfate.The accumulation of these salt can lead to
The reduction of desulfuration efficiency.For ensureing coal gas desulfurization efficiency, often adopt distillating still salt extraction in prior art or directly by desulfurization
Waste liquid is assigned in coking coal.
In the case of distillating still salt extraction, desulfurization waste liquor is using extraction ammonium sulfate and Ammonium hyposulfite., ammonium thiocyanate essence
Salt method is processed, complex process, and more than equipment, investment is big, and benefit is low, consumption is high, and the method is intermittently operated, high labor intensive, staffing
Many, and the ammonium thiocyanate purity extracted can not reach requirement, and impact is sold, is mixed with ammonium sulfate, does not have city in Ammonium hyposulfite.
Field is worth.
For another kind of method, if saliferous desulfurization waste liquor is directly injected to coal yard, easily forms secondary pollution,
And can etching apparatus；Substantial amounts of free ammonia is contained, meeting degradation manipulation environment, makes to the physical and mental health of employee again in desulfurization waste liquor
Become harm.
Additionally, also having a kind of technique of employing desulfurization waste liquor antacid in prior art, it passes through catalyzed conversion, is condensed into acid
Etc. step, desulfurization waste liquor is transformed into concentrated sulphuric acid, although each single technology of this technique is ripe, generally new technology, not in industry
Practice in production, and invest relatively large.
Therefore, in prior art there is still a need for a kind of efficiently, environmental protection, economic desulfurization waste liquor treatment technology.
Content of the invention
According to above-mentioned the problems of the prior art, one of purpose of the application is that offer is a kind of gives up to hpf method coal gas desulfurization
Liquid carries out multiple-effect evaporation, crystallization, the method extracting mixed salt, and the method adopts continuous processing to process desulfurization waste liquor, the company of being capable of
Continuous production, thus drastically increase productivity ratio；Also with sulfur-bearing acid solution, hydro-peening is carried out to tail gas simultaneously, decrease ammonia to air
Pollution, improve operating environment.Additionally, the method is successfully processed to coal gas desulfurization waste liquid using multiple-effect evaporation,
Thus improve heat utilization efficiency, decrease energy resource consumption.
In order to realize the purpose of the application, according to an embodiment of the application, it is many that it provides a kind of desulfurization waste liquor
The method of effect evaporation, the method comprises the following steps:
A) one effect evaporation step: by desulfurization waste liquor in 1st effective evaporator evaporation and concentration, the effective desulfuryzation after being concentrated
Waste liquid and the indirect steam of an effect evaporation；
B) two effect evaporation step: the effective desulfuryzation waste liquid after concentrating is sent into evaporation and concentration in 2nd effect evaporator, to obtain
Two effect desulfurization waste liquors after concentration and the indirect steam of two effect evaporations；
C) nonessential triple effect evaporation step: evaporate dense in two effect desulfurization waste liquors feeding triple effect evaporators after concentrating
Contracting, with the indirect steam of the triple effect desulfurization waste liquor after being concentrated and triple effect evaporation；
D) nonessential four-effect evaporation step: evaporate dense in the triple effect desulfurization waste liquor feeding four-effect evaporator after concentrating
Contracting, with the indirect steam of the quadruple effect desulfurization waste liquor after being concentrated and four-effect evaporation；
E) crystallisation step: the desulfurization waste liquor after the concentration finally giving is sent into crystallization tank crystallization, separates and obtain mixed salt, knot
Brilliant residual liquid；
F) condensing steps: the indirect steam of aftereffect is sent into exhaust steam preheater and/or pipe bundle condenser, condensed fluid enters cold
Lime set storage tank；
Wherein in described step a) in d), the indirect steam of front effect evaporation is used for the thermal source of aftereffect vaporizer,
Steam and fixed gas is comprised in the indirect steam of wherein said each effect evaporation.
Preferably, the also extra preheating step that includes before a described a) effect evaporation step: desulfurization waste liquor is passed through exhaust steam
Preheater and/or condensation water preheater preheating；
Preferably, also included filtration step before described a) an effect evaporation step and/or preheating step: by desulfurization waste liquor
Filtered by grade one filter and (alternatively) secondary filter；
Preferably, described filter is ceramic filter；
Preferably, a part for the desulfurization waste liquor in described each effect evaporation step sends into aftereffect vaporizer, and other are still same
1st effective evaporator interior circulation is evaporated；
Preferably, the pressure in aftereffect vaporizer is lower than the pressure in front effect vaporizer；
Preferably, aftereffect vaporizer is negative pressure；
Preferably, also include g) fixed gas process step after described f) condensing steps: fixed gas ammonium sulfate liquor sprays
Wash, process after discharge；
Preferably, in the described crystallization residual liquid return to step a) in described step e) crystallisation step to the either step in d)
Circulation；
According to an embodiment of the application, it provides one kind and realizes herein described desulfurization waste liquor multiple-effect evaporation side
The device of method, this device includes:
1st effective evaporator；2nd effect evaporator；Nonessential triple effect evaporator；Nonessential four-effect evaporator；Crystallization tank；Weary
Vapour preheater and/or pipe bundle condenser；Condensed fluid storage tank；
Wherein, front effect vaporizer is connected by pipeline with aftereffect vaporizer successively, described crystallization tank and aftereffect vaporizer
Connected by pipeline, described exhaust steam preheater and/or pipe bundle condenser and described condensed fluid storage tank also with aftereffect vaporizer
Connected by pipeline, and be used as the thermal source of aftereffect vaporizer by the indirect steam that front effect vaporizer obtains；
Preferably, this device also includes condensing water preheater；It is connected by pipeline with described 1st effective evaporator；
Preferably, this device also includes grade one filter and nonessential secondary filter；It is with described 1st effective evaporator
Or exhaust steam preheater or condensation water preheater are connected by pipeline；
Preferably, described filter is ceramic filter；
Preferably, the pressure in aftereffect vaporizer is lower than the pressure in front effect vaporizer；
Preferably, this device also includes pickling tower, and it is connected by pipeline with described exhaust steam preheater and/or pipe bundle condenser
Connect；
In this application, described front effect is relative with aftereffect, such as, for 1st effective evaporator, 2nd effect evaporator is
Aftereffect vaporizer, and for triple effect evaporator, 2nd effect evaporator is then front effect vaporizer；For example, in only one effect evaporation
In the case of device and 2nd effect evaporator, one imitates as front effect, and two imitate as aftereffect.
Preferably, in this application, using two effect evaporation processes.
The method of the desulfurization waste liquor multiple-effect evaporation according to the application makes the unnecessary desulfurization waste liquor that hpf method coal gas desulfurization produces
First pass around double-filtration, then preheat through twice, subsequently into multi-effect evaporator, after indirect steam condensation, respectively enter desulfurization
System or sulphur ammonium system, desulfurization concentrated solution enters crystallization tank, enters centrifuge and separates, salt-mixture is packed, and carries further after cooling
Pure, be mixed into sulfur cream antacid or allocate in coking coal pyrolysis into, crystallization residual liquid returns multi-effect evaporation system and recycles, and the method can be real
Now continuously produce, and various heats can be reclaimed in process of production and be used moreover it is possible to process to tail gas, improve operation
Environment.
Brief description
Fig. 1 is a process chart preferred embodiment according to the application.
Description of reference numerals
1 grade one filter, 2 secondary filter 3 desulfurization waste liquor storage tank
4 raw material pump 5 condensation water preheater 6 one effect heater
7 one effect separator 8 one effect demister 9 one effect circulating pumps
10 2 effect heater 11 2 effect separator 12 2 effect demisters
13 2 effect circulating pump 14 exhaust steam preheater 15 pipe bundle condensers
16 crystallization pump 17 crystallization tank 18 centrifuges
19 mother solution pond, 20 submerged pump 21 1 imitates condensed fluid storage tank
22 1 effect condensate pump 23 2 effect condensed fluid storage tank 24 2 effect condensate pumps
25 steam condensate (SC) tank, 26 condensate pump 27 pickling tower
28 vacuum pump, 29 flowing full mouth 30 sulphur ammonium flowing full groove
31 sulphur ammoniums little mother solution pump
Specific embodiment
Hereinafter with reference to accompanying drawing, the application is described in detail according to the preferred implementation of the application, however, following enforcement
Mode is only for descriptive purpose, rather than in order to limit the application.
As described in Figure 1, from 20-40 DEG C of sweetening process of desulfurization waste liquor through grade one filter 1, secondary filter 2
Filter out the solid particles such as sulfur in desulfurization waste liquor, tar.Filtered desulfurization waste liquor enters desulfurization waste liquor storage tank 3, then with former
Material pump 4 delivers to exhaust steam preheater 14, condensation water preheater 5 heat exchange, in exhaust steam preheater 14, desulfurization waste liquor with 40-90 DEG C
Two effect indirect steams carry out heat exchange, and in condensation water preheater 5, desulfurization waste liquor is changed with the steam condensate (SC) of an effect heater
Heat；After heat exchange, 50-90 DEG C of desulfurization waste liquor is mixed with 1st effective evaporator circulation fluid, with being steam heated in an effect heater 6
Enter effect separator 7 circulating and evaporating after 105-130 DEG C to separate, the indirect steam of an effect evaporation, secondary in an effect separator 7
Dedusting, foam removal, enter back into after the outer effect demister 8 of device removes entrained drip again, enter two and imitate heaters 10 to heat two effects
The circulation fluid of vaporizer, a condensed secondary vapour condensed fluid of effect individually enters an effect condensed fluid storage tank 21, sends into desulphurization system
Recycle；Most of desulfurization waste liquor of one effect separator 7 enters an effect heater 6 by an effect circulating pump 9 and heats Posterior circle
Evaporation and concentration, sub-fraction enters two effect separator 11 evaporations and separates, and mixes with the circulation desulfurization waste liquid of two effect separators 11,
Send into two effect heaters 10 by two effect circulating pumps 13 to heat, enter back into two effect separator 11 circulating and evaporating and concentrate；Another little portion
Points two effects separate the desulfurization waste liquor concentrating by crystallize pump 16 send into crystallization tank 17 stir, lower the temperature after enter centrifuge 18, isolate
Mixed salt, after packaging, export trade after can purifying further, also can be mixed in sulfur cream and remove Sulphuric acid, or be assigned in coal, in coking intermittent fever
Solution；The crystallization residual liquid return system circulating and evaporating of centrifugation concentrates；The desulfurization waste liquor steam of two effect separators 11 removes through in device
Enter exhaust steam preheater 14 and desulfurization of raw material waste liquid heat exchange after foam, two effect demister 12 foam removals, or it is cold to enter pipe bundle condenser 15
But, the secondary vapour condensed fluid of two effects enters two effect condensed fluid storage tanks 23, send sulphur ammonium system to use after process；Fixed gas enters pickling tower
27, use ammonium sulfate liquor hydro-peening, wash rear ammonium sulfate liquor and send into sulphur ammonium system, fixed gas discharges after processing further through vacuum pump 28；
Enter after effect heater 6 shell side is condensed with desulfurization waste liquor heat exchange from the steam that main steam header is come and enter steam condensate (SC) tank 25,
Enter condensed water preheater 5 after the pressurization of condensed water pump 26 and carry out heat exchange with desulfurization of raw material waste liquid, after heat exchange condensate system is again
Secondary utilization.
The concrete preferred implementation of the method for the desulfurization waste liquor multiple-effect evaporation according to the application includes:
1) desulfurization waste liquor coming from desulfurization enters two-stage ceramic filter and is filtered；
2) desulfurization waste liquor after filtering is preheated with being pumped into exhaust steam preheater 14, enters back into condensation water preheater 5 and preheats；
3) desulfurization waste liquor after preheating enters effect heater 6 import, enters one after mixing with an effect circulation desulfurization waste liquid
Effect heater 6 heats；
4) the effect circulation desulfurization waste liquid after heating enters an effect separator 7 and is evaporated separating, in an effect separator 7
Liquid enters an effect heater 6, by an effect circulating pump 9 and imitates separator 7 circulating and evaporating, concentration；In one effect separator 7 two
Secondary steam enters the thermal source as two effect heaters 10 for two effect heater 10 shell sides, and after its condensation, condensed fluid enters an effect condensed fluid
Storage tank 21, finally returns that coal gas desulfurization system；
5) the part circulation fluid of effect circulating pump 9 outlet enters two effect separators 11, and evaporation under subnormal ambient separates, and two
Liquid in effect separator 11 enters two effect heaters 10, two by two effect circulating pumps 13 and imitates separator 11 circulating and evaporating, concentration；
Two effect circulating pumps 13 output circulation fluids deliver to crystallization pump 16, enter crystallization tank 17 in, agitated, cooling after, crystallization enter from
Scheming 18 separates, and filtrate, from flowing into mother solution pond 19, is delivered to two effect circulating pump 13 import and recycled, solid enters mixed salt hopper etc.
To be packaged；
6) indirect steam of 2nd effect evaporator respectively enters exhaust steam preheater 14, pipe bundle condenser 15, two effect condensed fluid storage
Groove 23, send sulphur ammonium to use after treatment；
7) fixed gas enters pickling tower 27 ammonium sulfate liquor and carries out spraying absorbing ammonia, and ammonium sulfate liquor returns to sulphur ammonium flowing full groove
30；
8) crystallization tank 17 flowing full mouth 29 liquid is back to the pump inlet of two effect circulating pumps 13, recycles.
9) vacuum pump 28 overflow water is used as centrifuge wash water.
The method of the desulfurization waste liquor multiple-effect evaporation according to the present invention, can carry out continuous processing to desulfurization waste liquor.Through reality
Checking is real, and the method for the present invention can realize advantages below:
1st, process desulfurization waste liquor per ton only need 0.5 ton of steam (or other energy), with prior art in do not adopt multiple-effect
The technique of vaporizer and various heat reclaim unit is compared, energy saving 75%.
2nd, in tail gas, ammonia content is 0.1g/m3, compared with prior art reduce 90%.
Claims (4)
1. a kind of method of desulfurization waste liquor multiple-effect evaporation, the method comprises the following steps:
A) one effect evaporation step: by desulfurization waste liquor in 1st effective evaporator evaporation and concentration, the effective desulfuryzation waste liquid after being concentrated
Indirect steam with an effect evaporation；
B) two effect evaporation step: the effective desulfuryzation waste liquid after concentrating is sent into evaporation and concentration in 2nd effect evaporator, to be concentrated
Two effect desulfurization waste liquors afterwards and the indirect steam of two effect evaporations；
C) nonessential triple effect evaporation step: two effect desulfurization waste liquors after concentrating send into evaporation and concentration in triple effect evaporator, with
Triple effect desulfurization waste liquor after being concentrated and the indirect steam of triple effect evaporation；
D) nonessential four-effect evaporation step: the triple effect desulfurization waste liquor after concentrating is sent into evaporation and concentration in four-effect evaporator, with
Quadruple effect desulfurization waste liquor after being concentrated and the indirect steam of four-effect evaporation；
E) crystallisation step: the desulfurization waste liquor of aftereffect after concentrating is sent into crystallization tank crystallization, separates and obtain mixed salt, crystallization residual liquid；
F) condensing steps: the indirect steam of aftereffect is sent into exhaust steam preheater and/or pipe bundle condenser, condensed fluid enters condensed fluid
Storage tank；
Wherein in described step a) in d), the indirect steam of front effect evaporation is used for the thermal source of aftereffect vaporizer,
Steam and fixed gas is comprised in the indirect steam of wherein said each effect evaporation,
Wherein, also included filtration step before a described a) effect evaporation step and/or preheating step: desulfurization waste liquor is passed through one
Level filter and nonessential secondary filter filter,
Wherein, described grade one filter and nonessential secondary filter are ceramic filter,
Wherein, also include g) fixed gas process step after described f) condensing steps: fixed gas sulfur-bearing acid solution is sprayed
Wash, process after discharge.
2. method according to claim 1, wherein, also extra inclusion preheating step before a described a) effect evaporation step
Rapid: desulfurization waste liquor is passed through exhaust steam preheater and/or condensation water preheater preheating.
3. a kind of device realizing desulfurization waste liquor multiple effective evaporation method described in claim 1, this device includes:
1st effective evaporator；2nd effect evaporator；Nonessential triple effect evaporator；Nonessential four-effect evaporator；Crystallization tank；
Wherein, front effect vaporizer is connected by pipeline with aftereffect vaporizer successively, described crystallization tank and the described vaporizer of aftereffect
Connected by pipeline, and the indirect steam of described front effect evaporation be used for the thermal source of aftereffect vaporizer,
Wherein, this device also includes grade one filter and nonessential secondary filter；It is with described 1st effective evaporator or exhaust steam
Preheater or condensation water preheater are connected by pipeline,
Wherein, described grade one filter and nonessential secondary filter are ceramic filter,
Wherein, this device also includes pickling tower, and it is connected by pipeline with described exhaust steam preheater and/or pipe bundle condenser.
4. device according to claim 3, wherein,
This device also includes condensing water preheater；It is connected by pipeline with described 1st effective evaporator.
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| CN105399168B (en) * | 2015-12-18 | 2018-01-02 | 许达人 | The Multi-effect evaporation compression apparatus and technique of sulfur acid and its salting liquid |
| CN109775909B (en) * | 2017-11-15 | 2021-11-02 | 北京旭阳科技有限公司 | Recycling method of benzene hydrogenation sulfur-containing wastewater |
| CN108217690A (en) * | 2018-03-14 | 2018-06-29 | 湖南华菱涟源钢铁有限公司 | Process for extracting secondary salt from desulfurization waste liquid |
| CN115974005A (en) * | 2022-12-22 | 2023-04-18 | 中冶焦耐(大连)工程技术有限公司 | Raw material pretreatment process for coking desulfurization waste liquid and liquid sulfur incineration acid making technology |
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| CN101456635A (en) * | 2008-12-17 | 2009-06-17 | 深圳市能源环保有限公司 | Process and system for treating electric power plant waste water |
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| CN101456635A (en) * | 2008-12-17 | 2009-06-17 | 深圳市能源环保有限公司 | Process and system for treating electric power plant waste water |
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