CN109985507A - A kind of method and system for realizing phenol salt de using high-sulfur nitrogen flue gas - Google Patents
A kind of method and system for realizing phenol salt de using high-sulfur nitrogen flue gas Download PDFInfo
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- CN109985507A CN109985507A CN201910361476.0A CN201910361476A CN109985507A CN 109985507 A CN109985507 A CN 109985507A CN 201910361476 A CN201910361476 A CN 201910361476A CN 109985507 A CN109985507 A CN 109985507A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/60—Simultaneously removing sulfur oxides and nitrogen oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
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- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D1/00—Oxides or hydroxides of sodium, potassium or alkali metals in general
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- C—CHEMISTRY; METALLURGY
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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Abstract
The present invention relates to a kind of method and system that phenol salt de is realized using high-sulfur nitrogen flue gas, it carries out acid-base reaction with crude phenols salt after flue gas is pressurized and is translated into phenols, the sulphur nitrogen in flue gas is converted into sulfur-bearing and nitrogenous carbonate solution simultaneously, then converts by-product diluted alkaline and by-product mud for the carbonate solution of sulfur-bearing, nitrogen.The system comprises decomposition tower, decomposition and separation slot, limeslaker, mud clarifier and oil water separators；The top of decomposition tower sets crude phenols salt entrance, and lower part sets smoke inlet, and the gaseous phase outlet at the top of decomposition tower connects oil-water separation tank；The liquid-phase outlet for decomposing tower bottom connects decomposition and separation slot, decomposition and separation slot sets crude phenols outlet and sodium carbonate wastewater outlet, sodium carbonate wastewater outlet connects limeslaker, limeslaker is equipped with quick lime and mouth, grey slag outlet and mud outlet is added, mud outlet connects mud clarifier, and mud clarifier sets the outlet of by-product diluted alkaline and by-product slurry outlet.
Description
Technical field
The present invention relates to tar deep processing and flue gas utilization technical fields more particularly to a kind of utilization high-sulfur nitrogen flue gas to realize
The method and system of phenol salt de.
Background technique
The flue gas of sulfur-bearing nitrogen is the pollution item that attention rate is most concentrated in current atmospheric environmental protection, from the work run at present
From the point of view of industry desulfuring and denitrifying apparatus, the pollution treatment treatment scale of desulphurization denitration is generally all bigger, the adjusting control of each process procedure
Technical requirements processed are harsh, cause whole operating cost high.In addition, chemically angle analysis, carbon, sulphur in sulphur nitrogen flue gas and
Nitrogen is mainly to exist with the compound of oxidation state, and its aqueous solution state is in acidity, if finding one in industrial application
Need the occasion of a large amount of sour gas, and the chemical property of this kind of sour gas is required it is not harsh, then completely can will be such
The flue gas of sulfur-bearing nitrogen is turned waste into wealth.
Staple product of the phenolic compound as coal tar, is usually converted into water soluble salt from coal tar with alkaline process
In separate, then produce crude phenols with sulfuric acid process or carbon dioxide+sulfuric acid process decomposition.Sulfuric acid process decomposes net phenates and has been included in country
Explicit order eliminates technique, and majority enterprise all uses carbon dioxide+sulfuric acid process to produce crude phenols at present.The method is first used carbonated
Flue gas decomposes net phenates, and resolution ratio is generally up to 95%, and subsequent need plus a small amount of dilute sulfuric acid promote to decompose, so that phenates is complete
Portion is converted to crude phenols, and decomposition by-products aqueous sodium carbonate needs after processing generally as waste water for other industries
Recycled water.
Summary of the invention
The present invention provides it is a kind of using high-sulfur nitrogen flue gas realize phenol salt de method and system, flue gas it is pressurized after with
Crude phenols salt carries out acid-base reaction and is translated into phenols, while the sulphur nitrogen in flue gas is converted into sulfur-bearing and nitrogenous carbonate is molten
Then liquid converts by-product diluted alkaline and by-product mud for the carbonate solution of sulfur-bearing, nitrogen；The present invention realizes gas cleaning and phenol
The comprehensive utilization of salt decomposition product, and simple process, operating cost is low, is suitable for large-scale tar deep processing enterprise.
In order to achieve the above object, the present invention is implemented with the following technical solutions:
A method of phenol salt de, SO in the high-sulfur nitrogen flue gas are realized using high-sulfur nitrogen flue gas2Mass percent
Content >=2%, NOXMass percentage content >=0.5%；The high-sulfur nitrogen flue gas hereinafter referred to as flue gas；The method includes
Following steps:
1) flue gas after pressurized introduces in decomposition tower from tower bottom is decomposed, and introduces raw material crude phenols salt at the top of decomposition tower；It is former
Material crude phenols salt is contacted with flue gas adverse current, and remaining gas phase and aqueous neutral oil are together from decomposition tower top evolution, gas phase master after reaction
It to include carbon dioxide, nitrogen and water vapour, gas phase and aqueous neutral oil are transformed into liquid phase after condensation is cooling and enter grease point
From carrying out water-oil separating in slot；
2) liquid phase of decomposition tower bottom outflow is mainly sodium carbonate waste water and crude phenols containing a small amount of sodium sulphate, and liquid phase, which enters, divides
Solve the separation that sodium carbonate waste water and crude phenols are carried out in separating tank；
3) quick lime is added into the sodium carbonate waste water of the sulfur-bearing, nitrogen isolated, is converted by digestion and causticizing reaction
The calcium salt mud of alkali and sulfur-bearing, for calcium salt mud by isolating by-product diluted alkaline and by-product mud after clarification, by-product diluted alkaline returns to coke
It is used as the dephenolize auxiliary agent of each fraction in oily process, by-product mud main component is calcium carbonate, contains a small amount of calcium sulfate, by-product mud
Slurry is used to prepare building building cement after vacuum filters pressing, washing and drying.
The decomposition tower uses stainless steel helices tower, and raw material crude phenols salt and flue gas are in filler surface counter current contacting.
A kind of system for realizing phenol salt de using high-sulfur nitrogen flue gas for realizing the method, including decomposition tower, point
Solve separating tank, limeslaker, mud clarifier and oil water separator；The top side of the decomposition tower sets crude phenols salt entrance,
The lower part other side sets smoke inlet, and smoke inlet connects chimney by flue, sets flue gas blower on flue；Decomposition tower
Top set gaseous phase outlet, oil-water separation tank is connected by gas phase pipeline, sets flue gas condensing cooler on gas phase pipeline；Decomposition tower
Bottom set liquid-phase outlet, liquid-phase outlet passes through the material inlet that pipeline connects decomposition and separation slot；Decomposition and separation slot sets crude phenols and goes out
Mouth and sodium carbonate wastewater outlet, sodium carbonate wastewater outlet connect limeslaker by pipeline, and limeslaker is equipped with quick lime
Mouth, grey slag outlet and mud outlet is added, grey slag outlet connects screw conveyor, and mud outlet is connected by pipeline
The mud entrance of mud clarifier, mud clarifier are equipped with the outlet of by-product diluted alkaline and by-product slurry outlet.
Agitating device is respectively equipped in the limeslaker and mud clarifier.
Compared with prior art, the beneficial effects of the present invention are:
1) present invention realizes phenol salt de using high-sulfur nitrogen flue gas, while realizing gas cleaning, saves flue gas desulfurization
Denitration cost, reduces carbon emission, is conducive to atmospheric environment protection；
2) sulfur dioxide in flue gas mostlys come from fuels such as coal or coal gas etc., makes high-sulfur using the method for the invention
Thermal coal or high-sulfur coal gas are used as fuel to be possibly realized, and can be effectively reduced the cost of power consumption；
3) chimney breast flue-gas temperature is generally 100~250 DEG C, and heat itself is also a kind of pollution, according to environmental law
It needs to cool down if externally discharge；The present invention directly removes the neutral oil that this partial heat is used for phenates, so as to avoid routine
The consumption of phenol salt de technique low pressure steam；
4) since using the method for the invention after funnel exiting flue gas, without cooling down, the water vapour in flue gas will not be cold
Solidifying, sulfide and nitride would not also form for example dilute chloroazotic acid of strongly acidic solution etc., just be not necessarily to the material of flue in this way
Special preservative treatment is done, equipment cost can also be substantially reduced；
5) high-sulfur nitrogen flue gas and raw material crude phenols salt use reflux type haptoreaction in decomposition tower, can give full play to flue gas
The characteristic of middle power sour gas, fundamentally solves the problems, such as that carbon dioxide gas is halfway to phenol salt de；
6) the by-product sodium carbonate after phenol salt de carries out causticization digestion reaction, by-product diluted alkaline using quick lime (calcium oxide)
It is circularly used for the separating technology of phenols in tarry distillate, further saves cost；
7) sulphur in flue gas, nitrogen pollutant are eventually converted into the calcium salt easily precipitated, can effectively fix sulphur, nitrogen, reduce sulphur
The pollution of nitrogen, finally obtaining the calcium carbonate sludge containing micro calcium sulfate can be used for preparing construction material such as cement etc., realize full mistake
The maximization of journey product comprehensively utilizes.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of system that phenol salt de is realized using high-sulfur nitrogen flue gas of the present invention.
In figure: 1. chimney, 2. flue gas blower, 3. decomposition tower, 4. flue gas condensing cooler, 5. oil-water separation tank, 6. decomposition and separation slot
7. 8. mud clarifier of limeslaker, 9. screw conveyor
Specific embodiment
Specific embodiments of the present invention will be further explained with reference to the accompanying drawing:
A kind of method for realizing phenol salt de using high-sulfur nitrogen flue gas of the present invention, SO in the high-sulfur nitrogen flue gas2's
Mass percentage content >=2%, NOXMass percentage content >=0.5%；The high-sulfur nitrogen flue gas hereinafter referred to as flue gas；Institute
The method of stating includes the following steps:
1) flue gas after pressurized introduces in decomposition tower 3 from 3 bottom of decomposition tower, and raw material crude phenols salt is introduced at the top of decomposition tower 3；
Raw material crude phenols salt is contacted with flue gas adverse current, and remaining gas phase and aqueous neutral oil are together from decomposition tower top evolution, gas phase after reaction
It mainly include carbon dioxide, nitrogen and water vapour, gas phase and aqueous neutral oil are transformed into liquid phase after condensation is cooling and enter grease
Water-oil separating is carried out in separating tank 5；
2) liquid phase of decomposition tower bottom outflow is mainly sodium carbonate waste water and crude phenols containing a small amount of sodium sulphate, and liquid phase, which enters, divides
Solve the separation that sodium carbonate waste water and crude phenols are carried out in separating tank 6；
3) quick lime is added into the sodium carbonate waste water of the sulfur-bearing, nitrogen isolated, is converted by digestion and causticizing reaction
The calcium salt mud of alkali and sulfur-bearing, for calcium salt mud by isolating by-product diluted alkaline and by-product mud after clarification, by-product diluted alkaline returns to coke
It is used as the dephenolize auxiliary agent of each fraction in oily process, by-product mud main component is calcium carbonate, contains a small amount of calcium sulfate, by-product mud
Slurry is used to prepare building building cement after vacuum filters pressing, washing and drying.
The decomposition tower 3 uses stainless steel helices tower, and raw material crude phenols salt and flue gas are in filler surface counter current contacting.
As shown in Figure 1, a kind of utilization high-sulfur nitrogen flue gas realization phenol salt de for realizing the method for the present invention
System, including decomposition tower 3, decomposition and separation slot 6, limeslaker 7, mud clarifier 8 and oil water separator 5；The decomposition
The top side of tower 3 sets crude phenols salt entrance, and the lower part other side sets smoke inlet, and smoke inlet connects chimney 1 by flue,
Flue gas blower 2 is set on flue；The top of decomposition tower 3 sets gaseous phase outlet, connects oil-water separation tank 5, gas by gas phase pipeline
Flue gas condensing cooler 4 is set on phase pipeline；The bottom of decomposition tower 3 sets liquid-phase outlet, and liquid-phase outlet is decomposed by pipeline connection to be divided
Material inlet from slot 6；Decomposition and separation slot 6 sets crude phenols outlet and sodium carbonate wastewater outlet, sodium carbonate wastewater outlet pass through pipeline
Limeslaker 7 is connected, limeslaker 7 is equipped with quick lime and mouth, grey slag outlet and mud outlet, grey slag outlet is added
Screw conveyor 9 is connected, mud outlet connects the mud entrance of mud clarifier 8 by pipeline, and mud clarifier 8 is equipped with pair
Produce diluted alkaline outlet and by-product slurry outlet.
Agitating device is respectively equipped in the limeslaker 7 and mud clarifier 8.
Following embodiment is implemented under the premise of the technical scheme of the present invention, gives detailed embodiment and tool
The operating process of body, but protection scope of the present invention is not limited to following embodiments.Method therefor is such as without spy in following embodiments
Not mentionleting alone bright is conventional method.
[embodiment]
In the present embodiment, realizing phenol salt de using high-sulfur nitrogen flue gas, detailed process is as follows:
1) the high-sulfur nitrogen flue gas from 1 bottom of chimney leads to flue gas blower 2,1 original pair of chimney empty diffuse channel first
The pipeline of connection system for desulfuration and denitration can give over to spare.High-sulfur nitrogen flue gas pressures after the pressurization of flue gas blower 2 can generally increase
Add 10~20kPa, while the temperature of flue gas can also increase 10 DEG C or so, since the temperature and pressure of flue gas during this all increases
Add, does not have water vapour under normal conditions and condense out；
2) high-sulfur nitrogen flue gas with pressure enters in decomposition tower 3 from 3 bottom side interface of decomposition tower, and raw material crude phenols salt is then by dividing
The interface of the solution 3 top other side of tower enters in decomposition tower 3, and decomposition tower 3 uses stainless steel helices tower.Two phase materials are in decomposition tower 3
Interior counter current contacting, crude phenols salt flow through filler surface from top to bottom, and high-sulfur nitrogen flue gas from bottom to top with after crude phenols reactant salt from point
It is escaped at the top of solution tower 3.
3) 3 internal upper part region of decomposition tower, lower area carry out different chemical reactions respectively, when flue gas flows up,
The crude phenols salt initially contacted, which has, is largely converted into crude phenols, only remains the phenates that 10% or so carbon dioxide can not decompose and exists,
And contain the stronger oxysulfide of a certain amount of acidity and a small amount of nitrogen oxides in high-sulfur nitrogen flue gas fresh at this time, it is very suitable
Close the phenates of processing low concentration.
4) as flue gas continues up flowing in decomposition tower 3, sulfur and nitrogen oxides therein can consume quickly
Totally, remaining most of carbon dioxide begins participating in phenol salt de, and the chemical reaction of upper area is also entire phenol salt de
The main reaction region of process.In this conversion zone, to guarantee that phenol salt de is complete, it can also be passed through high-sulfur nitrogen flue gas in right amount.
5) gas phase being discharged at the top of decomposition tower 3 mainly includes carbon dioxide, nitrogen, water vapour and neutral oil, temperature one
As at 70~80 DEG C, while can also carry a small amount of liquid water or oil secretly.Gas phase is cooling through cooling water in flue gas condensing cooler 4
Afterwards, condensate liquid neutral oil and water enter back into oil-water separation tank with purified flue gas and to carry out gas and water, oil separates, and isolate
Neutral oil can make fuel oil or other purposes.
6) it is mainly sodium carbonate waste water (containing a small amount of sodium sulphate) and crude phenols from the liquid phase that 3 bottom of decomposition tower is discharged, is decomposing
Water-oil phase can be completely separated in separating tank 6, and the crude phenols isolated can be further used for processing various purification phenol.
7) digestion and causticizing reaction are carried out in limeslaker 7 using quick lime (calcium oxide) and sodium carbonate waste water, it will
The sodium salt solution of high-dissolvability is converted into the calcium salt of low solubility, is conducive to calcium salt (such as calcium carbonate, calcium sulfate) in this way by sinking
The mode in shallow lake separates sig water and calcium salt mud in mud clarifier 8.
8) the by-product diluted alkaline isolated is recycled into the dephenolize auxiliary agent that each fraction is used in Process of Tar Processing, by-product mud
Middle major part is calcium carbonate (containing a small amount of calcium sulfate), and by-product mud can be used for building building cement after vacuum filters pressing, washing and drying
Production.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (4)
1. a kind of method for realizing phenol salt de using high-sulfur nitrogen flue gas, which is characterized in that SO in the high-sulfur nitrogen flue gas2Matter
Measure degree >=2%, NOXMass percentage content >=0.5%；The high-sulfur nitrogen flue gas hereinafter referred to as flue gas；It is described
Method includes the following steps:
1) flue gas after pressurized introduces in decomposition tower from tower bottom is decomposed, and introduces raw material crude phenols salt at the top of decomposition tower；Raw material is thick
Phenates is contacted with flue gas adverse current, and together from tower top evolution is decomposed, gas phase is mainly wrapped for remaining gas phase and aqueous neutral oil after reaction
Carbon dioxide, nitrogen and water vapour are included, gas phase and aqueous neutral oil are transformed into liquid phase after condensation is cooling and enter oil-water separation tank
Middle carry out water-oil separating；
2) liquid phase of decomposition tower bottom outflow is mainly sodium carbonate waste water and crude phenols containing a small amount of sodium sulphate, and liquid phase enters decomposition point
From the separation for carrying out sodium carbonate waste water and crude phenols in slot；
3) quick lime is added into the sodium carbonate waste water of the sulfur-bearing, nitrogen isolated, by digestion and causticizing reaction be converted into alkali and
The calcium salt mud of sulfur-bearing, by isolating by-product diluted alkaline and by-product mud after clarification, by-product diluted alkaline returns to tar and adds calcium salt mud
It is used as the dephenolize auxiliary agent of each fraction during work, by-product mud main component is calcium carbonate, contains a small amount of calcium sulfate, by-product mud warp
Building building cement is used to prepare after vacuum filters pressing, washing and drying.
2. a kind of method for realizing phenol salt de using high-sulfur nitrogen flue gas according to claim 1, which is characterized in that described
Decomposition tower uses stainless steel helices tower, and raw material crude phenols salt and flue gas are in filler surface counter current contacting.
3. a kind of system for realizing phenol salt de using high-sulfur nitrogen flue gas for realizing claim 1 the method, feature
It is, including decomposition tower, decomposition and separation slot, limeslaker, mud clarifier and oil water separator；The top of the decomposition tower
Side sets crude phenols salt entrance, and the lower part other side sets smoke inlet, and smoke inlet connects chimney by flue, on flue
If flue gas blower；Gaseous phase outlet is set at the top of decomposition tower, and oil-water separation tank is connected by gas phase pipeline, sets flue gas on gas phase pipeline
Condensate cooler；The bottom of decomposition tower sets liquid-phase outlet, and liquid-phase outlet connects the material inlet of decomposition and separation slot by pipeline；Point
Solution separating tank sets crude phenols outlet and sodium carbonate wastewater outlet, and sodium carbonate wastewater outlet connects limeslaker, lime by pipeline
Digester is equipped with quick lime and mouth, grey slag outlet and mud outlet is added, and grey slag outlet connects screw conveyor, mud row
Outlet connects the mud entrance of mud clarifier by pipeline, and mud clarifier is equipped with the outlet of by-product diluted alkaline and by-product mud goes out
Mouthful.
4. a kind of system for realizing phenol salt de using high-sulfur nitrogen flue gas according to claim 1, which is characterized in that described
Agitating device is respectively equipped in limeslaker and mud clarifier.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110975770A (en) * | 2019-12-23 | 2020-04-10 | 中冶焦耐(大连)工程技术有限公司 | Decomposition process and device of phenate in coal tar processing process |
| CN112050654A (en) * | 2020-09-25 | 2020-12-08 | 济南尚德瑞化工科技有限公司 | Wastewater treatment system and method for crude phenol extraction process |
| CN114409170A (en) * | 2022-01-29 | 2022-04-29 | 陕西东鑫垣化工有限责任公司 | Water-oil ammonia-sulfur residue separation system and method for phenol-ammonia wastewater treatment |
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| CN208726970U (en) * | 2018-06-19 | 2019-04-12 | 邸润东 | A kind of purification device of petrochemical industry exhaust gas |
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| DE2431611A1 (en) * | 1974-07-02 | 1976-01-22 | Heinz Hoelter | Two-step washing of carbon dioxide-contg. gaseous effluents - first with sulphuric acid and then, briefly, with alkali to remove phenols |
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| CN202265523U (en) * | 2011-08-30 | 2012-06-06 | 河南宝舜化工科技有限公司 | Production system for coking crude phenol |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110975770A (en) * | 2019-12-23 | 2020-04-10 | 中冶焦耐(大连)工程技术有限公司 | Decomposition process and device of phenate in coal tar processing process |
| CN112050654A (en) * | 2020-09-25 | 2020-12-08 | 济南尚德瑞化工科技有限公司 | Wastewater treatment system and method for crude phenol extraction process |
| CN114409170A (en) * | 2022-01-29 | 2022-04-29 | 陕西东鑫垣化工有限责任公司 | Water-oil ammonia-sulfur residue separation system and method for phenol-ammonia wastewater treatment |
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