CN104724778A - 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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- CN104724778A CN104724778A CN201510177706.XA CN201510177706A CN104724778A CN 104724778 A CN104724778 A CN 104724778A CN 201510177706 A CN201510177706 A CN 201510177706A CN 104724778 A CN104724778 A CN 104724778A
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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 that desulfurization waste liquor multiple-effect evaporation carries salt, specifically, the present invention relates to the method for the desulfurization waste liquor of HPF method coal gas being carried out to multiple-effect evaporation, crystallization, extraction mixed salt.
Background technology
Current most of coal chemical enterprise employing HPF method removes the hydrogen sulfide in coke-oven gas, in the process of desulfurization, a series of side reaction occurs, creates the salt byproducts such as ammonium thiosulfate, ammonium thiocyanate, ammonium sulfate.The accumulation of these salt can cause the reduction of desulfuration efficiency.For ensureing coal gas desulfurization efficiency, still kettle in prior art, is adopted to carry salt or be directly assigned in coking coal by desulfurization waste liquor often.
When adopting still kettle to carry salt, desulfurization waste liquor adopts and extracts ammonium sulfate and ammonium thiosulfate, the process of ammonium thiocyanate refined salt method, complex process, the many investments of equipment are large, and benefit is low, it is high to consume, the method is periodical operation, labour intensity is large, staffing is many, and the ammonium thiocyanate purity extracted can not reach requirement, and impact is sold, be mixed with ammonium sulfate in ammonium thiosulfate, there is no marketable value.
For another kind of method, if saliferous desulfurization waste liquor is directly injected to coal yard, easily forms secondary pollution, and meeting etching apparatus; Containing a large amount of free ammonia in desulfurization waste liquor, again can degradation manipulation environment, the physical and mental health of employee is worked the mischief.
In addition, a kind of technique adopting desulfurization waste liquor relieving haperacidity is also had in prior art, its by catalyzed conversion, be condensed into acid etc. step desulfurization waste liquor is transformed into the vitriol oil, although each single technology of this technique is ripe, but be totally novel process, not practice in the industrial production, and invest relatively large.
Therefore, a kind of efficient, environmental protection, economic desulfurization waste liquor treatment technology is still needed in prior art.
Summary of the invention
According to above-mentioned the problems of the prior art, one of object of the application is to provide a kind of method of HPF method coal gas desulfurization waste liquid being carried out to multiple-effect evaporation, crystallization, extraction mixed salt, the method adopts continuous processing process desulfurization waste liquor, can realize continuous seepage, thus drastically increase productivity; Also hydro-peening is carried out to tail gas sulfur acid solution simultaneously, decrease the pollution of ammonia to air, improve operating environment.In addition, the method successfully adopts multiple-effect evaporation to process coal gas desulfurization waste liquid, thus improves heat utilization efficiency, decreases energy consumption.
In order to realize the object of the application, according to an embodiment of the application, which provide a kind of method of desulfurization waste liquor multiple-effect evaporation, the method comprises the following steps:
A) an effect evaporation step: by desulfurization waste liquor evaporation concentration in 1st effective evaporator, obtains the secondary steam of the effect desulfurization waste liquor after concentrating and an effect evaporation;
B) two effect evaporation steps: the effect desulfurization waste liquor after concentrated is sent into evaporation concentration in 2nd effect evaporator, to obtain the secondary steam of two effect desulfurization waste liquors after concentrating and two effect evaporations;
C) nonessential triple effect evaporation step: two effect desulfurization waste liquors after concentrated are sent into evaporation concentration in triple-effect evaporator, to obtain the secondary steam of the triple effect desulfurization waste liquor after concentrating and triple effect evaporation;
D) nonessential four-effect evaporation step: the triple effect desulfurization waste liquor after concentrated is sent into evaporation concentration in quadruple effect evaporator, to obtain the secondary steam of the quadruple effect desulfurization waste liquor after concentrating and four-effect evaporation;
E) crystallisation step: by finally obtain concentrated after desulfurization waste liquor send into crystallizer tank crystallization, be separated and obtain mixed salt, crystallization raffinate;
F) condensing steps: the secondary steam of most aftereffect is sent into exhaust steam preheater and/or pipe bundle condenser, and phlegma enters phlegma storage tank;
Wherein in described step a) in d), the secondary steam of front effect evaporation is used to the thermal source of rear single-effect evaporator,
Steam and non-condensable gas is comprised in the secondary steam of wherein said each effect evaporation.
Preferably, before a described a) effect evaporation step, also additionally pre-heating step is comprised: by desulfurization waste liquor by exhaust steam preheater and/or water of condensation preheater preheats;
Preferably, before described a) an effect evaporation step and/or pre-heating step, also filtration step is comprised: filtered by grade one filter and (alternatively) secondary filter by desulfurization waste liquor;
Preferably, described strainer is porcelain filter;
Preferably, a part for the desulfurization waste liquor in described each effect evaporation step sends into rear single-effect evaporator, and other are still in same 1st effective evaporator internal recycle evaporation;
Preferably, the pressure in rear single-effect evaporator is lower than the pressure in front single-effect evaporator;
Preferably, last single-effect evaporator is negative pressure;
Preferably, after described f) condensing steps, g) non-condensable gas treatment step is also comprised: discharge after non-condensable gas ammonium sulfate liquor hydro-peening, process;
Preferably, at described step e) described crystallization raffinate in crystallisation step returns step a) to the arbitrary step cycle in d);
According to an embodiment of the application, which provide a kind of device realizing desulfurization waste liquor multiple effective evaporation method described in the application, this device comprises:
1st effective evaporator; 2nd effect evaporator; Nonessential triple-effect evaporator; Nonessential quadruple effect evaporator; Crystallizer tank; Exhaust steam preheater and/or pipe bundle condenser; Phlegma storage tank;
Wherein, front single-effect evaporator is connected by pipeline with rear single-effect evaporator successively, described crystallizer tank is connected by pipeline with last single-effect evaporator, described exhaust steam preheater and/or pipe bundle condenser and described phlegma storage tank are also connected by pipeline with last single-effect evaporator, and the secondary steam obtained by front single-effect evaporator is used as the thermal source of rear single-effect evaporator;
Preferably, this device also comprises water of condensation preheater; It is connected by pipeline with described 1st effective evaporator;
Preferably, this device also comprises grade one filter and nonessential secondary filter; Its with described 1st effective evaporator or exhaust steam preheater or water of condensation preheater be connected by pipeline;
Preferably, described strainer is porcelain filter;
Preferably, the pressure in rear single-effect evaporator is lower than the pressure in front single-effect evaporator;
Preferably, this device also comprises pickling tower, and it is connected by pipeline with described exhaust steam preheater and/or pipe bundle condenser;
In this application, before described, effect is relative with aftereffect, and such as, for 1st effective evaporator, 2nd effect evaporator is rear single-effect evaporator, and for triple-effect evaporator, 2nd effect evaporator is then front single-effect evaporator; Such as, when only having 1st effective evaporator and 2nd effect evaporator, an effect is front effect, and two effects are aftereffect.
Preferably, in this application, two effect evaporative processes are adopted.
Unnecessary desulfurization waste liquor HPF method coal gas desulfurization being produced according to the method for the desulfurization waste liquor multiple-effect evaporation of the application is first through two-stage filtration, again through twice preheating, then multiple-effect evaporator is entered, desulphurization system or sulphur ammonium system is entered respectively after secondary steam condensation, desulfurization concentrated solution enters crystallizer tank, enter whizzer after cooling to be separated, mixing salt is packed, further purification, be mixed into the relieving haperacidity of sulphur cream or allocate pyrolysis in coking coal into, crystallization raffinate returns multi-effect evaporation system and recycles, the method can realize continuous seepage, and can various heat be reclaimed in process of production and be used, can also process tail gas, improve operating environment.
Accompanying drawing explanation
Fig. 1 is according to one of the application process flow sheet preferred embodiment.
Description of reference numerals
1 grade one filter 2 secondary filter 3 desulfurization waste liquor storage tank
4 feedstock pump 5 water of condensation preheater 6 one effect well heaters
7 one effect separators 8 one are imitated scum dredger 9 one and are imitated recycle pump
10 2 effect well heaters 11 2 are imitated separator 12 2 and are imitated scum dredger
13 2 effect recycle pump 14 exhaust steam preheater 15 pipe bundle condensers
16 crystallization pump 17 crystallizer tank 18 whizzers
19 mother liquor pond 20 submerged pumps 21 1 imitate phlegma storage tank
22 1 effect condensate pumps 23 2 are imitated phlegma storage tank 24 2 and are imitated condensate pump
25 vapor condensation water pot 26 condensate pump 27 pickling towers
28 vacuum pump 29 flowing full mouth 30 sulphur ammonium flowing full grooves
The little mother liquor pump of 31 sulphur ammonium
Embodiment
Describe the application hereinafter with reference to accompanying drawing in detail according to the preferred implementation of the application, but, following embodiment be only for illustration of object, instead of in order to limit the application.
As described in Figure 1, to filter out the solid particulate such as sulphur, tar in desulfurization waste liquor through grade one filter 1, secondary filter 2 from the desulfurization waste liquor of 20-40 DEG C of sweetening process.Filtered desulfurization waste liquor enters desulfurization waste liquor storage tank 3, exhaust steam preheater 14, water of condensation preheater 5 heat exchange is delivered to again with feedstock pump 4, in exhaust steam preheater 14, two of desulfurization waste liquor and 40-90 DEG C is imitated secondary steam and is carried out heat exchange, in water of condensation preheater 5, the steam condensate that desulfurization waste liquor and imitates well heater carries out heat exchange; After heat exchange, the desulfurization waste liquor of 50-90 DEG C mixes with 1st effective evaporator circulation fluid, after being steam heated to 105-130 DEG C, an effect separator 7 circulating and evaporating separation is entered in an effect well heater 6, the secondary steam of one effect evaporation, final dusting, foam removal in an effect separator 7, enter after the outer effect scum dredger 8 of device removes entrained drip again again, enter two effect well heaters 10 to heat the circulation fluid of 2nd effect evaporator, a condensed effect secondary vapour phlegma enters separately an effect phlegma storage tank 21, sends into desulphurization system and recycles; Most of desulfurization waste liquor of one effect separator 7 enters an effect well heater 6 by an effect recycle pump 9 and heats Posterior circle evaporation concentration, sub-fraction enters two effect separators 11 and evaporates separation, and mix with the two circulation desulfurization waste liquids of imitating separator 11, send into two effect well heaters 10 heat by two effect recycle pumps 13, then enter two effect separator 11 circulating and evaporating and concentrate; Another small portion two effect be separated concentrated desulfurization waste liquor by crystallization pump 16 send into crystallizer tank 17 stir, lower the temperature after enter whizzer 18, isolate mixed salt, after packaging, export trade after can purifying further, also can be mixed in sulphur cream and remove Sulphuric acid, or be assigned in coal, the pyrolysis when coking; The crystallization raffinate retrieval system circulating and evaporating of centrifugation concentrates; The desulfurization waste liquor steam of two effect separators 11 enters exhaust steam preheater 14 and the heat exchange of desulfurization of raw material waste liquid after foam removal in device, two effect scum dredger 12 foam removals, or enter pipe bundle condenser 15 and cool, two effect secondary vapour phlegmas enter two effect phlegma storage tanks 23, send sulphur ammonium system to use after process; Non-condensable gas enters pickling tower 27, uses ammonium sulfate liquor hydro-peening, washes rear ammonium sulfate liquor and sends into sulphur ammonium system, non-condensable gas discharge after vacuum pump 28 further process; Steam condensate tank 25 is entered after the steam that main steam header is next enters effect well heater 6 shell side and desulfurization waste liquor heat exchange condensation, after condensate pump 26 pressurizes, enter water of condensation preheater 5 carry out heat exchange with desulfurization of raw material waste liquid, after heat exchange, condensate system utilizes again.
Concrete preferred implementation according to the method for the desulfurization waste liquor multiple-effect evaporation of the application comprises:
1) desulfurization waste liquor come from desulfurization enters two-stage porcelain filter and filters;
2) desulfurization waste liquor after filtering with being pumped into exhaust steam preheater 14 preheating, then enters water of condensation preheater 5 preheating;
3) desulfurization waste liquor after preheating enters effect well heater 6 import, imitates and enters an effect well heater 6 after circulation desulfurization waste liquid mixes with one and heat;
4) the effect circulation desulfurization waste liquid after heating enters an effect separator 7 to carry out evaporation and is separated, and the liquid in an effect separator 7 enters an effect well heater 6, by an effect recycle pump 9 and imitates separator 7 circulating and evaporating, concentrates; Secondary steam in one effect separator 7 enters the thermal source of two effect well heater 10 shell sides as two effect well heaters 10, and after its condensation, phlegma enters an effect phlegma storage tank 21, finally returns coal gas desulfurization system;
5) the component loops liquid that an effect recycle pump 9 exports enters two effect separators 11, evaporates and be separated under subnormal ambient, and the liquid in two effect separators 11 enters two effect well heaters 10, two by two effect recycle pumps 13 and imitates separator 11 circulating and evaporating, concentrates; The circulation fluid that two effect recycle pumps 13 export delivers to crystallization pump 16, enters in crystallizer tank 17, after stirring, cooling, crystallization enters whizzer 18 and is separated, filtrate, from flowing into mother liquor pond 19, is delivered to two effect recycle pump 13 imports and is recycled, and it is to be packaged that solid enters mixed salt hopper etc.;
6) secondary steam of 2nd effect evaporator enters exhaust steam preheater 14 respectively, pipe bundle condenser 15, two imitates phlegma storage tank 23, send sulphur ammonium to use after treatment;
7) non-condensable gas enters pickling tower 27 ammonium sulfate liquor and carries out sprinkling absorbing ammonia, and ammonium sulfate liquor turns back to sulphur ammonium flowing full groove 30;
8) crystallizer tank 17 flowing full mouth 29 liquid return is to the pump inlet of two effect recycle pumps 13, recycles.
9) vacuum pump 28 overflow water is used as whizzer wash water.
According to the method for desulfurization waste liquor multiple-effect evaporation of the present invention, can process continuously desulfurization waste liquor.Confirm through experiment, method of the present invention can realize following advantage:
1, process desulfurization waste liquor per ton and only need 0.5 ton of steam (or other energy), compared with not adopting the technique of multiple-effect evaporator and various heat reclaim unit in prior art, save energy 75%.
2, in tail gas, ammonia content is 0.1g/m
3, compared with prior art reduce 90%.
Claims (10)
1. a method for desulfurization waste liquor multiple-effect evaporation, the method comprises the following steps:
A) an effect evaporation step: by desulfurization waste liquor evaporation concentration in 1st effective evaporator, obtains the secondary steam of the effect desulfurization waste liquor after concentrating and an effect evaporation;
B) two effect evaporation steps: the effect desulfurization waste liquor after concentrated is sent into evaporation concentration in 2nd effect evaporator, to obtain the secondary steam of two effect desulfurization waste liquors after concentrating and two effect evaporations;
C) nonessential triple effect evaporation step: two effect desulfurization waste liquors after concentrated are sent into evaporation concentration in triple-effect evaporator, to obtain the secondary steam of the triple effect desulfurization waste liquor after concentrating and triple effect evaporation;
D) nonessential four-effect evaporation step: the triple effect desulfurization waste liquor after concentrated is sent into evaporation concentration in quadruple effect evaporator, to obtain the secondary steam of the quadruple effect desulfurization waste liquor after concentrating and four-effect evaporation;
E) crystallisation step: the most aftereffect desulfurization waste liquor after concentrated is sent into crystallizer tank crystallization, is separated and obtains mixed salt, crystallization raffinate;
F) condensing steps: the secondary steam of most aftereffect is sent into exhaust steam preheater and/or pipe bundle condenser, and phlegma enters phlegma storage tank;
Wherein in described step a) in d), the secondary steam of front effect evaporation is used to the thermal source of rear single-effect evaporator,
Steam and non-condensable gas is comprised in the secondary steam of wherein said each effect evaporation.
2. method according to claim 1, wherein, also additionally comprised pre-heating step: by desulfurization waste liquor by exhaust steam preheater and/or water of condensation preheater preheats before a described a) effect evaporation step.
3. method according to claim 2, wherein, also comprised filtration step: filtered by grade one filter and (alternatively) secondary filter by desulfurization waste liquor before described a) an effect evaporation step and/or pre-heating step.
4. method according to claim 3, wherein, described strainer is porcelain filter.
5. method according to claim 1, wherein, also comprises g) non-condensable gas treatment step after described d) condensing steps: non-condensable gas sulfur acid solution discharges after carrying out hydro-peening, process.
6. realize a device for desulfurization waste liquor multiple effective evaporation method described in claim 1, this device comprises:
1st effective evaporator; 2nd effect evaporator; Nonessential triple-effect evaporator; Nonessential quadruple effect evaporator; Crystallizer tank;
Wherein, front single-effect evaporator is connected by pipeline with rear single-effect evaporator successively, and described crystallizer tank is connected by pipeline with described last single-effect evaporator, and the secondary steam of described front effect evaporation is used to the thermal source of rear single-effect evaporator.
7. device according to claim 6, wherein,
This device also comprises water of condensation preheater; It is connected by pipeline with described 1st effective evaporator.
8. device according to claim 7, wherein,
This device also comprises grade one filter and nonessential secondary filter; Its with described 1st effective evaporator or exhaust steam preheater or water of condensation preheater be connected by pipeline.
9. device according to claim 8, wherein,
Described strainer is porcelain filter.
10. device according to claim 6, wherein,
This device also comprises pickling tower, and it is connected by pipeline with described exhaust steam preheater and/or pipe bundle condenser.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105399168A (en) * | 2015-12-18 | 2016-03-16 | 许达人 | Multi-effect evaporation and concentration device and technology thereof for solution containing sulfuric acid and salts thereof |
| 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 |
| CN109775909A (en) * | 2017-11-15 | 2019-05-21 | 北京旭阳科技有限公司 | A kind of reuse method of benzene hydrogenation sulfur-containing waste water |
| CN113582142A (en) * | 2021-08-09 | 2021-11-02 | 唐山金硕化工有限公司 | Method and device for purifying sodium thiosulfate 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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2015
- 2015-04-15 CN CN201510177706.XA patent/CN104724778B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105399168A (en) * | 2015-12-18 | 2016-03-16 | 许达人 | Multi-effect evaporation and concentration device and technology thereof for solution containing sulfuric acid and salts thereof |
| 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 |
| CN109775909A (en) * | 2017-11-15 | 2019-05-21 | 北京旭阳科技有限公司 | A kind of reuse method of benzene hydrogenation sulfur-containing waste water |
| 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 |
| CN113582142A (en) * | 2021-08-09 | 2021-11-02 | 唐山金硕化工有限公司 | Method and device for purifying sodium thiosulfate 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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