CN105731389B - The process and device of a kind of utilization sour gas production NaHS - Google Patents
The process and device of a kind of utilization sour gas production NaHS Download PDFInfo
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- CN105731389B CN105731389B CN201410732140.8A CN201410732140A CN105731389B CN 105731389 B CN105731389 B CN 105731389B CN 201410732140 A CN201410732140 A CN 201410732140A CN 105731389 B CN105731389 B CN 105731389B
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Abstract
The invention discloses a kind of process of utilization sour gas production NaHS and device, process of the invention, refluxing portion NaHS product solutions to middle liquid storage tank, with NaOH reaction generations Na2S, with Na2S solution is absorbing liquid, processing sour gas production NaHS；Weary gas is introduced in middle order reaction, gas liquid ratio is improved, reduced to CO2Uptake.The process units of the present invention, is made up of liquid film absorbing reaction device, fluid reservoir, middle liquid storage tank, pump, instrument and pipe valve.Absorbing liquid point all the way in reactor wall formation liquid film, is prevented wall overheat from causing vulcanized sodium, sodium carbonate crystallization wall built-up by the absorption process；Liquid film separation layer is manufactured, vulcanized sodium, sodium carbonate crystalline particle attachment reaction device inwall is prevented.Compared with prior art, reduce to CO2Absorption, solid content in reduction system.The present invention realizes the double goal of sour gas purification and pollutant resources.
Description
Technical field
The present invention relates to a kind of process of utilization sour gas production NaHS and device, belong to Chemical Engineering neck
Domain, it is adaptable to the comprehensive utilization of petrochemical industry sour gas, is particularly suitable for use in containing H2S、CO2Deng sour gas purification and
The process for producing device of pollutant resources.
Background technology
Element sulphur is prevalent in fossil fuel, when oil enters fine fractionation with deep-processing process, is formed with hydrogen
Hydrogen sulfide gas, the process is toward contact association carbon dioxide, ammonia etc..There is also element sulphur in the raw material of metallurgy industry,
But because its process is generally worst hot case, element sulphur is oxidized, and mainly generates sulfur dioxide sour gas.It is other to produce acidity
The operating mode of gas mostly occurs and uses process in chemical process or chemical products.
The sour gas of petroleum chemical industry mostlys come from natural gas extraction, associated gas, coal chemical industry, oil-refining chemical row
Industry.Can have a negative impact again to follow-up processing during the energy is processed（As catalyst poisoning, pipeline are rotten
Erosion）, it is therefore necessary to control the sulfur content in raw materials technology and product.During desulfurization element sulphur in the form of hydrogen sulfide from
Go into operation to discharge into outside process system and burned into boiler, air is discharged into the form of sulphur dioxide.China's flue gas desulfurization technique starting is compared
Evening, desulfuration byproduct utilization rate is lower.So, most desulfuration byproducts are idle to be stacked, and is taken a large amount of land resources and is made
Into secondary pollution.And use desulfurizing agent circular regeneration to use, reclaim the desulfurization technology of Sulphur ressource, its reclaim product be elemental sulfur and
Sulfuric acid etc., can be as industrial chemicals, for other sulfur removal technologies, and it, which reclaims product, more preferable market prospects.
The processing of China's sour gas, mainly uses sour gas to prepare sulphur, and the more commonly used at present has two kinds of works
Skill technology, one kind is two grades of claus process combination tail gas hydrogenation reducing process, and solvent absorption process technology.Another technique
Technology is the LO-CAT technologies of gas technology Products Co., Ltd of Merichem companies of U.S. exploitation.
Crouse's sulphur recovery technology have passed through a series of development and perfect, form a more huge skill
Art system.Initial Claus method is that hydrogen sulfide and oxygen are first mixed, and catalysis oxidation generation is single in a certain temperature conditions
Matter sulphur.Being mainly characterized by using air as oxidant for original Claus method, reacts and is carried out in a fixed bed adiabatic reactor.
German method our company is improved to original Claus method within 1938, and the oxidation reaction of hydrogen sulfide is divided into two ranks
Duan Jinhang：First stage is that 1/3 Oxidation of Hydrogen Sulfide is sulfur dioxide, reaction heat Steam Recovery；Second stage is residue 2/3
Hydrogen sulfide and sulfur dioxide reaction generation elemental sulfur.This technological innovation solves original 3 problems of Claus method：One is gram
Louth reacting furnace is mainly the reaction that Oxidation of Hydrogen Sulfide is sulfur dioxide, it is not necessary to maintain low reaction temperature；Two be 80% it is anti-
Heat is answered to reclaim, way of recycling is steam；Three be that the treating capacity of hydrogen sulfide improves 50 times than original Claus method.This skill
Art is referred to as improveing Claus method.In actual applications, in order to adapt to different sour gas compositions and meet increasingly strict two
Sulfur oxide emissions requirement, improvement Claus method forms four kinds of basic technical process：Direct current method, shunting, sulfur cycle method and
Direct oxidation method.
Improvement Claus method is called Crouse's technology for short, or is referred to as classical Claus method.Claus method is as existing
Modern most widely used sulphur recovery technology, people have done substantial amounts of research to this technology.Oxygen-enriched gram is proposed on this basis
Louth technology, super Claus technology（Super Claus99）, super excellent Crouse's technology（Super Claus99.5）Deng.
So far, the processing topmost means of hydrogen sulfide are hydramine method absorption technique and Claus unit sulfur recovery unit, especially
It is after super Claus Sulfur Recovery Technique exploitation, and the removal efficiency of hydrogen sulfide has reached more than 99%.At present, the method is at home and abroad obtained
To extensive use.
LO-CAT techniques make hydrogen sulfide be converted into elementary sulfur, the removing of hydrogen sulfide using the iron catalyst of multicomponent chelate
Rate is more than 99.9%.LO-CAT techniques can be adapted to that the fluctuation of acid tolerance is larger, and hydrogen sulfide content 0~100% it is various
Operating mode, raw material condition of compatibility is wide in range, adapts to the actual conditions of sour gas fluctuating change.And LO-CAT liquid redox technical office
Reason scheme will not produce any harmful exhaust gas by-products without using any poisonous chemicals, environmentally safe
Catalyst can be constantly regenerating in processing procedure.The stability and economic benefit of LO-CAT sulfur removal technologies operation are depended primarily on
The stability of doctor solution and the consumption of chemicals.According to its different stability that complex compound is formed between iron ion and complexing agent
Also different characteristics, LO-CAT have selected different complexing agents to configure complexing ferrous solution, the generation for preventing ferrous sulfide from precipitating.
LO-CAT technology features are that technological process is simple, and operating flexibility is big, and floor space is small, first investment cost
It is low；But operating cost is too high, chemical solvent consumption is big, is not suitable for larger desulfurizer, and iron content waste water is difficult, sulphur
Product quality is not high.LO-CAT techniques foreign countries are directed generally to reduce production cost, reduce equipment size and improve sulphur
Quality etc..Domestic aspect, dominant catalyst used in LO-CAT techniques and other chemical agents are import, associated catalysts
Research work also in the research and development of starting stage LO-CAT catalyst also need put into extensive work.
Sulfuric acid is widely used in all trades and professions as one of basic industrial chemicals.Made with the hydrogen sulfide contained in sour gas
For raw material, many processing steps can be saved, that is, saves investment, cost is reduced again, sulphur can also be effectively recycled
Resource.Because small-sized sour gas tolerance is smaller, the industrial sulphuric acid of low concentration can only be produced, it is impossible to which productive value is higher
Oleum, economic benefit is not high, simultaneously as the transport of sulfuric acid, storage acquire a certain degree of difficulty, it is therefore, steady near oil plant
The fixed market demand is the key factor for limiting its development.Patent CN101143714A discloses a kind of acidity of utilization high hydrocarbon-containing
The method that gas prepares sulfuric acid, acid hydrogen sulfide gas is respectively enterd in first, second sulfureted hydrogen burning stove in proportion to burn, from the
The high-temperature furnace gas that one combustion furnace comes out, by burner-gas cooler, certain temperature is cooled to by air, subsequently into the second combustion furnace
Continue and the combust of surplus air one, the high-temperature furnace gas that the second combustion furnace comes out in furnace gas with the sulfide hydrogen sour gas of supplement
Into waste heat boiler heat accumulation, enter back into purification section, conversion section, dry absorption section and carry out conventional relieving haperacidity.This process can only
98% industrial sulphuric acid is produced, it is impossible to the higher oleum of productive value, simultaneously as the transport of sulfuric acid, storage have certain difficulty
Degree, therefore, the stable market demand is the key factor for limiting its development near oil plant.
The comprehensive utilization of sour gas, can using investing less absorption process sulfur removal technology technology, the technology using alkaline agent as
Absorbent, sulphite is prepared by vulcanization hydrogen retrieval.Sour gas is carried out burning generation sulfur dioxide by the technology, is then fed into suction
Receive tower and carry out chemical absorbing generation sulfite solution, then solution and alkaline absorbent are reacted, prepare the production of sulphite liquid
Product, or generation sulphite crystal, sulphite solid product is prepared into through the process such as separation, dry.The process unit
Flow is shorter, and reaction is simple, and operating flexibility is big, is applicable to the sour gas operating mode of medium and small tolerance, and tolerance fluctuation was to producing
Journey can select different absorbents to produce difference without influence by selecting different processes to produce solid or fluid product
The sulphite of type, and tail gas qualified discharge is realized by three sections of absorptions, realize the purpose of cleaning of off-gas.But actual production
There is equipment corrosion in journey serious, the higher determination of maintenance cost.
The comprehensive utilization of sour gas, it would however also be possible to employ the less novel absorbent method sulfur removal technology technology of investment, produces chemical industry
Product akali sulphide.Akali sulphide is widely used in the industry such as ore dressing, agricultural chemicals, dyestuff, tanning production and organic synthesis.Wherein, contaminate
NaHS is used to synthesize organic intermediate and prepares the auxiliary agent of sulfur dye in material industry；Leather industry is used for the depilation of rawhide
And tanning, routinely soaked applied to leather industry, energy uniform loose's cladding fibr tissue enables cladding slowly to expand, with bright
Aobvious crease-resistant and raising leather yield effect, and can ensure that the color of the blue skin of cladding, it is ensured that the sense organ and quality of cladding；Chemical fertilizer industry
Middle NaHS can be used for sloughing the free sulfur in activated carbon desulphurization agent；It is manufacture ammonium sulfide and agricultural chemicals ethyl mercaptan in pesticide industry
The raw material of semi-finished product；NaHS is largely used to copper ore dressing in mining industry；It is used for sulfurous acid dyeing in staple fibre production
In terms of；NaHS can be additionally used in wastewater treatment.With increasingly harsh, the consumption of sulfur product commercially of environmental regulation
Reduction, price also increasingly drops, about 600 yuan/ton of Sulfur price, and the market price of vulcanized sodium is 2600 yuan/ton, NaHS
The market price be even more to reach 3200 yuan/ton.
Low concentration solution product is produced using sour gas：Low concentration is prevented effectively from crystallization, but solution product does not use valency
Value, it is necessary to carry out multistage evaporation concentration, energy consumption is very high, without economy.
Patent CN102515112 A《The hydrogen sulfide waste gas produced in a kind of utilization viscose rayon production prepares vulcanized sodium
Method》Spray-absorption, double flash evaporation and crystallisation by cooling process are set, and the technology can only produce the extremely low solution of concentration, there is stream
The problems such as journey length, the low concentration product liquid evaporation of generation, concentration process high energy consumption.
Patent CN103466559 A《Continuous production technology of three kettle type sodium hydrosulfide》, using sodium hydroxide as absorbing liquid, use
Three-level counter-current absorption process, realizes the continuous production of sodium hydrosulfide.The unstripped gas of the technology need to carry out removing titanium dioxide
The pretreatment of carbon, has that long flow path, process units be complicated, particularly feed gas preprocessing energy consumption is very high, the problems such as device is complicated.
Patent CN101654226 A《The method of preparing alkali sulphide by using sulfur dye waste gas》, using hydrogen sulfide containing sulfur dye waste gas as original
Material, adds alkali and is reacted, generate akali sulphide.The technology production process is intermittently operated, there is alkaline agent and product low concentration, clearly
Cleaning device is numerous and diverse, produces waste water, example 3,4 is also easy to produce blocking, can not continuously generated, and there are problems that solid waste.Patent
CN103495329 A《A kind of technique for removing hydrogen sulfide and Recovered sulphur》, hydrogen sulfide, sodium carbonate are removed by sewage stripping and inhaled
Receive hydrogen sulfide, rich solution and sulphur foam is produced under desulphurization catalyst effect, and filtering, molten sulphur production elemental sulfur four part are constituted.Should
There is desulphurization catalyst costliness in technology, sulphur foam entrained catalyst causes sulphur product purity not high, the problems such as having solid waste generation.
Sour gas is the mixed gas of hydrogen sulfide and carbon dioxide：In petrochemical industry, sour gas is usually sulphur
Change hydrogen, carbon dioxide mix body, by absorbent of alkaline agent, production vulcanized sodium or during sodium hydrosulfide product, it will usually formed
The materials such as vulcanized sodium, NaHS, sodium carbonate, sodium acid carbonate, when concentration reaches certain value, can produce crystallization, cause device
Block and can not normally realize continuous production.
For the Acidic Gas Treating of petrochemical industry, also stay at present " basic reason utilized be hydrogen sulfide be pole
The extensive thoughtcast of dangerous toxic gas, it is necessary to be used or convert ".At present, " efficiency multiplication, economy can hold
, it is necessary to the Acidic Gas Treating method of a kind of new " energy-conservation, consumption reduction, environmental protection " under the new demand of supervention exhibition ".
The content of the invention
In view of the shortcomings of the prior art, the present invention provides one kind and produces NaHS method and device using sour gas, with
Prior art is compared, and the inventive method and device can realize the double goal of sour gas purification and pollutant resources, be applicable
In the processing of sour gas.
The present invention provides the device that a kind of utilization sour gas produces NaHS, and described device includes absorbing reaction device, storage
Flow container and pans, the absorbing reaction device set N grades, and N=2-9, the absorbing reaction device is made up of upper, middle and lower segment, its
In, epimere is liquid film generator tube, and stage casing is reaction tube, and hypomere is gas-liquid separation pipe, the liquid film generator tube, reaction tube, gas-liquid
Separating pipe, which is gone to upper and lower, to be connected in series, and is same axis arrangement；The liquid film generator tube is sealed by outer cylinder body, inner barrel, upper annular
Stifled disk and lower annular closure disk are constituted, and some liquid channels in level, annular spread are opened up on the inner barrel of liquid film generator tube,
Liquid film generator tube is provided with gas phase entrance and liquid phase material entrance；The reaction tube is from top to bottom followed successively by feed zone, contraction section, larynx
Pipeline section, expansion segment and discharging section, the feed zone upper end of the reaction tube are connected with the inner barrel lower end of liquid film generator tube, reaction tube
Tube wall be provided with absorbing liquid entrance, absorbing liquid entrance be located at trunnion section top；The gas-liquid separation pipe is by upper cover plate, gas-liquid separation
Pipe inner barrel, gas-liquid separation pipe outer cylinder body and bottom plate are constituted；The inner barrel top of gas-liquid separation pipe and the discharging section of reaction tube
Lower end is connected, and gas-liquid separation pipe is provided with gaseous phase outlet and liquid-phase outlet；The fluid reservoir sets quantity identical with absorbing reaction device
Liquid storage area, separated by overflow plate between adjacent liquid storage area, the liquid of the outer cylinder body of the gas-liquid separation pipe of the absorbing reaction device
Mutually outlet is extend into liquid storage area corresponding in fluid reservoir, and every grade of liquid storage area bottom is equipped with the outlet of generation liquid, and generation liquid goes out
Mouth is connected with the liquid phase material entrance and absorbing liquid entrance of absorbing reaction device respectively through pipeline, and the gas phase of first order absorption reactor enters
Mouth is connected with sour gas suction line, and buffering area is provided with before one-level liquid storage area, and the buffering area is provided with outlet for product, production
Product discharging opening point two-way, is connected, another road is connected through pipeline with pans with product discharge pipeline all the way, the pans also with
Alkali liquor inlet pipeline is connected, and the outlet of pans is connected through pipeline with the treatment fluid entrance of afterbody liquid storage area.
In sour gas production NaHS device of the present invention, the outlet of the pans is removed and afterbody liquid storage through pipeline
The treatment fluid entrance connection in area is outer, can also be connected simultaneously with the treatment fluid entrance of other optional liquid storage areas.
In sour gas production NaHS device of the present invention, the absorbing reaction device contacted at first with sour gas is first order absorption
Reactor, corresponding liquid storage area is one-level liquid storage area, is then two grades of absorbing reaction devices, and corresponding liquid storage area is two grades of liquid storages
Area, the rest may be inferred below.
In sour gas of the present invention production NaHS device, the gas phase entrances of the M grades of absorbing reaction devices also with weary gas
Suction line is connected, described when N is even number, M=N/2, when N is odd number, and M=（N+1）/2.
In sour gas production NaHS device of the present invention, the absorbing reaction device sets 4~6.
In sour gas production NaHS device of the present invention, the liquid film generator tube in the absorbing reaction device enters provided with gas phase
Mouth and liquid phase material entrance, the gas phase entrance are arranged on the upper end of the inner barrel of liquid film generator tube, the liquid phase material entrance
It is arranged on the side wall of the outer cylinder body of liquid film generator tube.
In sour gas production NaHS device of the present invention, the liquid channel is triangle, circle, strip or continuous
One kind in annular space, preferably continuous annular space.The gross area of liquid channel is absorbing reaction device on liquid film generator tube inner barrel
1~12 times of liquid phase material entrance cross-sectional area, preferably 3~5 times.
In sour gas production NaHS device of the present invention, the absorbing liquid entrance connection liquid phase distributor of the reaction tube,
Liquid phase distributor is arranged on reaction tube center line, and absorbing liquid is sprayed from top to bottom, and liquid phase distributor is settable 1~10, excellent
Select 4~6.
In sour gas production NaHS device of the present invention, the inner barrel bottom of the gas-liquid separation pipe opens up teeth groove, tooth
Slot structure is fan-shaped teeth groove, square teeth groove, preferably triangle teeth groove, lance tooth slot structure, space width be 3mm~
20mm, preferably 5mm~8mm；Its bottom angle is 15~90 °, preferably 30~60 °.
In sour gas production NaHS device of the present invention, the gas-liquid separation pipe is provided with gaseous phase outlet and liquid-phase outlet,
Gaseous phase outlet is arranged on the side wall of the outer cylinder body of gas-liquid separation pipe, and inner cylinder of the position higher than gas-liquid separation pipe of gaseous phase outlet
The lower end outlet of body, liquid-phase outlet is located at the bottom of the outer cylinder body of gas-liquid separation pipe.
In sour gas production NaHS device of the present invention, the overflow plate is highly the 1/2~4/5 of reservoir diameter,
Preferably 2/3~3/4.According to sour gas flow direction, the height of the overflow plate gradually increases.Outside the gas-liquid separation pipe
Cylinder bottom is located at the 1/4~2/3 of overflow plate radial height, and preferably 1/3~1/2.
In sour gas production NaHS device of the present invention, the setting buffers level control device, when in buffering area
When liquid level is the 1/2~3/4 of overflow plate height, when liquid level is the 2/3 of overflow plate height preferably in buffering area, product is pumped up out
Device.
In sour gas production NaHS device of the present invention, the absorbing reaction device inwall, pipeline and fluid reservoir are lining
In material, specially serve as a contrast tetrafluoro material.
In sour gas production NaHS device of the present invention, the gas phase suction line of the penultimate stage absorbing reaction device
Control valve is set on upper setting hydrogen sulfide on-line computing model, the alkali liquor inlet pipeline, passes through hydrogen sulfide on-line computing model, detection
Fluctuated into the concentration of hydrogen sulfide in the gas of penultimate stage absorbing reaction device between 1000ppm~9000mmp, output 4 ~
20mA continuous signal, sets the regulation for sodium hydroxide solution inlet amount in alkali liquor inlet pipeline, realizes the automatic of device
Change production process.
The present invention provides the process that a kind of utilization sour gas produces NaHS, is handled using said apparatus of the present invention
Sour gas produces NaHS, and sour gas enters from first order absorption reactor, and weary gas draws from M grades of absorbing reaction device gas phase entrances
Enter, sour gas enters corresponding liquid storage area with the reacted reaction generation liquid of absorbing liquid, then the liquid phase thing through absorbing reaction device
Material entrance and absorbing liquid entrance return to absorbing reaction device respectively, and reacted sour gas enters next stage absorbing reaction device and continues anti-
Should, until qualified discharge after being reacted through afterbody absorbing reaction device, the material of the buffering area is all the way as product, Ling Yilu
Into pans with being used after alkaline reaction as absorbing liquid.
In the process of sour gas production NaHS of the present invention, the sour gas includes hydrogen sulfide and carbon dioxide,
Can be various sources contain H2S sour gas.
In the process of sour gas of the present invention production NaHS, the reaction temperature of the absorbing reaction device for 70~
100 DEG C, preferably 80~95 DEG C.
In the process of sour gas of the present invention production NaHS, absorbing liquid and sour gas in the absorbing reaction device
Liquid-gas ratio is 3~20L/m3, preferably 5~10 L/m3。
In the process of sour gas production NaHS of the present invention, in every grade of liquid storage area, the liquid phase through absorbing reaction device
The reaction generation liquid that material inlet enters absorbing reaction device enters absorbing reaction device with the absorbing liquid entrance through absorbing reaction device
Reaction generation liquid volume flow ratio is 1/20~9/10, preferably 1/10~1/3.
In the process of sour gas production NaHS of the present invention, the buffering area is provided with outlet for product, and product goes out
Material mouth point two-way, is connected, another road is connected through pipeline with pans with product discharge pipeline all the way, wherein into the production of pans
The volume flow ratio of product and the product through product discharge pipeline is 1/6~1/2, preferably 1/4~1/2.
In the process of sour gas production NaHS of the present invention, NaOH solution mass concentration is 20%~60%, preferably
For 32%~38%.
In the process of sour gas production NaHS of the present invention, the weary gas is not anti-with sour gas and NaOH solution
Any of the arbitrary gas answered, specially low-pressure gas, nitrogen, inert gas.The volume flow of the weary gas and acid
Property gas suction line at sour gas volume flow ratio be 1:1~3:1, preferably 1.5:1~2:1.
Compared with prior art, the present invention is had the following advantages that using sour gas production NaHS method and device：
1st, the present invention is produced using sour gas in the process and device of NaHS, and the absorbing reaction device is by setting
Liquid film generator tube is put, by absorbing liquid point all the way in reactor wall formation liquid film, liquid film is between reaction tube and reacting field
Form separation layer：First effect is to prevent the H in sour gas2S and alkaline reaction react on wall, generates vulcanized sodium,
Sodium carbonate crystalline particle, causes to crystallize wall built-up；Second effect is the sodium acid carbonate for preventing from having generated, having mixed in absorbing liquid
Grain adheres to wall in droplets, and heated rear liquid phase evaporates, causes sodium bicarbonate particle residual wall to cause to crystallize wall built-up；The
Three be liquid film heat-blocking action, the drop that can effectively prevent temperature higher be attached to is easy to radiating wall on cause cooling,
Drop cooling easily produces TDS and separates out and produce crystallization wall built-up.The wall protected using liquid film can effectively be reduced, even be disappeared
Except crystallization wall built-up phenomenon, so as to realize stable production process, continuous long-term operation.
2nd, the present invention is produced using sour gas in the process and device of NaHS, is returned using portioned product liquid NaHS
It flow to pans and NaOH reaction generations Na2S, then with Na2S is used as absorbing liquid, the CO in reduction absorption system2, reduction
Solid holdup in system, it is ensured that device is stable, continuously run.
3rd, the present invention is produced using sour gas in the process and device of NaHS, by setting weary gas inlet tube
Line, supplements gas gas-phase objects doses, improves gas liquid ratio, improves the uniformity in flow field, greatly reduces H in sour gas2S and CO2Concentration,
Improve its degree of exchange.Especially CO in reduction sour gas2Concentration, most of CO2Device is carried over together with carrier gas, is controlled
Na2CO3And NaHCO3Content, prevent from producing a large amount of Na2CO3Crystallization is caused, blocking pipeline not only ensures product NaHS
Quality, and Hydrogen Sulfide Tail Gas decontamination index is realized, the resultant effect of waste gas purification and production qualified chemical products is reached, simultaneously
Ensure device long period, continuous, steady running.
4th, the present invention produces the device of NaHS using sour gas, and structure composition is simple, small scale.Using reactor and
Fluid reservoir subregion is set, and fluid reservoir realizes automatic overflow by overflow plate, it is possible to reduce the use of conveying equipment and pipeline, prevents
Radiating and cooling causes conveying equipment and pipeline to block, and realizes the homogeneity in temperature field, while reducing heat exchange heat tracing equipment；Every grade anti-
It should set up self-loopa absorption process, improve reaction depth, realize that liquid-phase product is up-to-standard, purified gas is up to standard.
5th, the present invention using sour gas produce NaHS process and device compared with prior art, equipment scale
Small, energy consumption is low, and operating cost is few, and generation can be used for the NaHS products of the industries such as printing and dyeing, papermaking, be readily transported, and has certain
Market, it is adaptable to the processing of sour gas, realize sour gas purification and pollutant resources double goal.
Brief description of the drawings
Fig. 1 is the process and schematic device that the present invention produces NaHS using sour gas.
Fig. 2 is absorbing reaction device structural representation of the present invention.
Embodiment
As shown in figure 1, a kind of device of utilization sour gas production NaHS of the present invention reacts including first order absorption
Device 15, two grades of absorbing reaction devices 16, three-level absorbing reaction device 17, level Four absorbing reaction device 18, Pyatyi absorbing reaction device 19, six grades
Absorbing reaction device 20, fluid reservoir 10 and pans 8, fluid reservoir 10 set the liquid storage area of quantity identical with absorbing reaction device, respectively
For one-level liquid storage area 22, two grades of liquid storage areas 23, three-level liquid storage area 24, level Four liquid storage area 25, Pyatyi liquid storage area 26, six grades of liquid storage areas
27th, separated between adjacent liquid storage area by overflow plate 11, buffering area 21, the reactor are additionally provided with before the one-level liquid storage area
It is made up of upper, middle and lower segment, wherein, epimere is liquid film generator tube, and stage casing is reaction tube, and hypomere is gas-liquid separation pipe, the liquid
Film generator tube, reaction tube, gas-liquid separation pipe go to upper and lower and are connected in series, and are same axis arrangement；The liquid film generator tube is by outer
Cylinder 34, inner barrel 33, upper annular closure disk 32 and lower annular closure disk 36 are constituted, and are opened up on the inner barrel 33 of liquid film generator tube
In some liquid channels 35 of level, annular spread, liquid film generator tube is provided with gas phase entrance 32 and liquid phase material entrance 30, described
Gas phase entrance 32 is arranged on the upper end of the inner barrel 33 of liquid film generator tube, and the liquid phase material entrance 30 is arranged on liquid film generator tube
Outer cylinder body 34 side wall on, the liquid channel 35 be triangle, circle, strip or continuous annular space in one kind, preferably
For continuous annular space.The reaction tube is from top to bottom followed successively by feed zone 39, contraction section 40, trunnion section 41, expansion segment 42 and discharging
Section 43, the upper end of feed zone 39 of the reaction tube is connected with the lower end of inner barrel 33 of liquid film generator tube, and the tube wall of reaction tube is provided with
Absorbing liquid entrance 37, absorbing liquid entrance 37 is located at 41 tops of trunnion section, the connection liquid phase point of absorbing liquid entrance 37 of the reaction tube
Cloth device 38, liquid phase distributor 38 is arranged on reaction tube center line, and absorbing liquid is sprayed from top to bottom, and liquid phase distributor 38 can be set
1~10, preferably 4~6；The gas-liquid separation pipe is by upper cover plate 47, gas-liquid separation pipe inner barrel 45, gas-liquid separation pipe outer barrel
Body 46 and bottom plate 49 are constituted；The top of inner barrel 45 of gas-liquid separation pipe and the lower end of discharging section 43 of reaction tube are connected, gas-liquid point
Gaseous phase outlet 44 and liquid-phase outlet 50 are provided with from pipe, the bottom of inner barrel 45 for stating gas-liquid separation pipe opens up teeth groove 48, teeth groove 48
Structure is fan-shaped teeth groove, square teeth groove, preferably triangle teeth groove, lance tooth slot structure, and space width is 3mm~20mm,
It is preferred that 5mm~8mm；Its bottom angle is 15~90 °, preferably 30~60 °, and the gaseous phase outlet 44 is arranged on gas-liquid separation pipe
On the side wall of outer cylinder body 46, and the position of gaseous phase outlet 44 is exported higher than the lower end of the inner barrel 45 of gas-liquid separation pipe, and liquid phase goes out
Mouth 50 is located at the bottom of the outer cylinder body 46 of gas-liquid separation pipe, and the bottom of outer cylinder body 46 of the gas-liquid separation pipe of the absorbing reaction device is stretched
Enter in the liquid storage area corresponding into fluid reservoir 10, every grade of liquid storage area bottom is equipped with generation liquid outlet 12, generation liquid outlet 12
It is connected respectively with the liquid phase material entrance 30 and absorbing liquid entrance 37 of absorbing reaction device through pipeline, the buffering area 21 is provided with product
Discharging opening, outlet for product point two-way, is connected 4, another road is connected through pipeline 9 with pans 8, institute with product discharge pipeline all the way
State pans 8 to be also connected with alkali liquor inlet pipeline 3, the outlet of pans 8 is through pipeline and level Four liquid storage area 25, Pyatyi liquid storage area
26th, the treatment fluid entrance 13 of six grades of liquid storage areas 27 is connected.The buffering area 21 is provided with level control device 6.The Pyatyi absorbs
The gas phase suction line of reactor 19 is provided with hydrogen sulfide on-line computing model 7, the alkali liquor inlet pipeline 3 and sets control valve
14。
The present invention produces the process of NaHS using sour gas, and the sour gas from sour gas suction line 1 is first
First order absorption reactor 15 is introduced into, using the solution in one-level liquid storage area 22 as absorbing liquid, the absorbing liquid is divided into two-way, led to
The generation liquid for crossing the bottom of one-level liquid storage area 22 exports the 12 absorbing liquid entrance 37 and liquid through pipeline respectively with first order absorption reactor
Phase materials entrance 30 returns to first order absorption reactor, wherein the generation liquid for returning to absorbing reaction device by liquid phase material entrance 30 is first
The liquid film generator tube of absorbing reaction device is introduced into, then reactor wall forms liquid film again, if the presence without liquid film, absorbed
Drop can stick to wall, and reaction heat temperature is higher, can produce evaporation, and causing vulcanized sodium to separate out causes crystallization；In addition, absorbing
There is the tiny sodium bicarbonate solid particle formed in liquid, if the presence without liquid film, the particle can be with absorbing liquid
Drop is attached in wall of reactor, because reaction temperature is higher, particle attachment wall after drop evaporation, causes the stifled of reactor
Plug；Set after liquid film, Na can be prevented effectively from2S crystallizes the attachment of wall built-up and sodium bicarbonate particle.Inhaled for gas-liquid on another road of absorbing liquid
The absorbing liquid of reaction is received, the vulcanized sodium in absorbing liquid is converted into NaHS by the course of reaction, and by the carbon in being partly dissolved
Sour sodium is converted into NaHS.At the gas-liquid separation pipe of absorbing reaction device, the sour gas for eliminating partial vulcanization hydrogen is entered
Two grades of absorbing reaction devices continue absorption process.The gas phase entrance of the three-level absorbing reaction device 17 is drawn by weary gas suction line 5
Enter weary gas into three-level absorbing reaction device 17, enter after being mixed with the sour gas after two grades of absorbing reaction device processing with absorbing liquid
Row reaction, due to the very high concentrations of hydrogen sulfide in sour gas, after first order absorption reactor, two grades of absorbing reaction device reactions
Gas phase amount can be caused to drastically reduce, the reduction of gas liquid ratio can cause residence time of the sour gas in reactor to greatly prolong, instead
Answer intensity to increase suddenly, reaction heat is excessive to cause NaHS to decompose, by introducing weary gas, adjust gas phase amount, improve gas liquid ratio, reduce
The uptake of carbon dioxide, reduces crystallization, it is to avoid block, finally, and the sour gas after six grades of absorbing reaction device processing passes through
The qualified discharge of clean gas outlet pipeline 2；The liquid phase of generation gas-liquid separation pipe of the liquid through absorbing reaction device of every grade of absorbing reaction device
Outlet enters in correspondence liquid storage area, and absorbing liquid is sequentially conveyed step by step from maximum order of reaction through overflow plate in the way of overflow, until
First order conversion zone, sequentially step by step in course of conveying, vulcanization na concn is gradually reduced, NaHS concentration from maximum order of reaction
Gradually step up, until during first order conversion zone, the NaHS in solution reaches national chemical products quality requirement, produces
Qualified sodium hydrosulfide product.Solution product is drawn from the buffering area of fluid reservoir, the solution point two-way of extraction：Conduct all the way
Product liquid enters finished pot, all the way solution input pans, and pans inject sodium hydroxide solution simultaneously, and both occur instead herein
Should, vulcanized sodium is produced, enters level Four absorbing reaction device, Pyatyi absorbing reaction device and six grades of absorbing reactions as the absorbing liquid of device
Device.
Illustrate the reaction effect of the present invention with reference to embodiment, but therefore do not limit the scope of the invention.
Embodiment 1
Using processing method and processing device as shown in Figure 1, using sour gas and NaOH solution as raw material, reacted.It is acid
CO in gas2Volume fraction is 7%, H2S volume fractions are 92%, and hydro carbons volume fraction is 1%.NaOH solution mass concentration is 38%.
In embodiment 1,6 grades of absorbing reaction devices are set, 6 grades of liquid storage areas and 1 grade of buffering area are correspondingly arranged.The absorbing reaction
Device is structure shown in Fig. 2.In embodiment 1, the NaHS products liquid of backflow and the volume flow ratio of generation NaHS products are 1/4.Often
The liquid-gas ratio of absorbing liquid and sour gas is 5L/m in level absorbing reaction device3.The generation liquid of every grade of absorbing reaction device is through liquid phase material
The generation liquid volume flow ratio that entrance and absorbing liquid entrance return to absorbing reaction device is 1/3.Reactor reaction device control reaction temperature
Spend between 80 DEG C -85 DEG C, reaction result is shown in Table 1.
Comparative example 1
Same as Example 1, difference is not provided with NaHS backflows directly to use NaOH as absorbing liquid.
Comparative example 2
Same as Example 1, difference is not provided with NaHS backflows to be not introduced into weary gas.
The embodiment of table 1 and comparative example reaction result
Claims (39)
1. a kind of utilization sour gas produces the device of NaHS, described device includes absorbing reaction device, fluid reservoir and pans,
The absorbing reaction device sets N grades, and N=2-9, the absorbing reaction device is made up of upper, middle and lower segment, wherein, epimere is liquid film
Generator tube, stage casing is reaction tube, and hypomere is gas-liquid separation pipe, and the liquid film generator tube, reaction tube, gas-liquid separation pipe are gone to upper and lower
It is connected in series, and is same axis arrangement；The liquid film generator tube is by outer cylinder body, inner barrel, upper annular closure disk and lower annular
Block disk to constitute, some liquid channels in level, annular spread are opened up on the inner barrel of liquid film generator tube, liquid film generator tube is set
There are gas phase entrance and liquid phase material entrance；The reaction tube is from top to bottom followed successively by feed zone, contraction section, trunnion section, expansion segment
And discharging section, the feed zone upper end of the reaction tube is connected with the inner barrel lower end of liquid film generator tube, and the tube wall of reaction tube is provided with
Absorbing liquid entrance, absorbing liquid entrance is located at trunnion section top；The gas-liquid separation pipe by upper cover plate, gas-liquid separation pipe inner barrel,
Gas-liquid separation pipe outer cylinder body and bottom plate are constituted；The inner barrel top of gas-liquid separation pipe and the discharging section lower end of reaction tube are connected,
Gas-liquid separation pipe is provided with gaseous phase outlet and liquid-phase outlet；The fluid reservoir sets the liquid storage area of quantity identical with absorbing reaction device,
Separated between adjacent liquid storage area by overflow plate, the liquid-phase outlet of the outer cylinder body of the gas-liquid separation pipe of the absorbing reaction device is stretched into
In to fluid reservoir in corresponding liquid storage area, every grade of liquid storage area bottom is equipped with the outlet of generation liquid, and the outlet of generation liquid is through pipeline point
It is not connected with the liquid phase material entrance and absorbing liquid entrance of absorbing reaction device, the gas phase entrance and sour gas of first order absorption reactor
Suction line is connected, and buffering area is provided with before one-level liquid storage area, and the buffering area is provided with outlet for product, outlet for product point
Two-way, is connected with product discharge pipeline all the way, and another road is connected through pipeline with pans, the pans also with alkali liquor inlet pipe
Line is connected, and the outlet of pans is connected through pipeline with the treatment fluid entrance of afterbody liquid storage area.
2. according to the device described in claim 1, it is characterised in that：Described is one with sour gas is contacted at first absorbing reaction device
Level absorbing reaction device, corresponding liquid storage area is one-level liquid storage area, is then two grades of absorbing reaction devices, and corresponding liquid storage area is two grades
Liquid storage area, the rest may be inferred below.
3. according to the device described in claim 1, it is characterised in that：The gas phase entrance of the M grades of absorbing reaction devices also with it is weary
Gas suction line is connected, when N is even number, M=N/2, when N is odd number, and M=（N+1）/2.
4. according to the device described in claim 1, it is characterised in that：Remove and stored up with afterbody through pipeline in the outlet of the pans
The treatment fluid entrance connection of liquid zone is outer, is also connected simultaneously with the treatment fluid entrance of other optional liquid storage areas.
5. according to the device described in claim 4, it is characterised in that：Liquid film generator tube in the absorbing reaction device is provided with gas phase
Entrance and liquid phase material entrance, the gas phase entrance are arranged on the upper end of the inner barrel of liquid film generator tube, and the liquid phase material enters
Mouth is arranged on the side wall of the outer cylinder body of liquid film generator tube.
6. according to the device described in claim 1, it is characterised in that：The liquid channel is triangle, circle, strip or company
One kind in continuous annular space.
7. according to the device described in claim 6, it is characterised in that：The liquid channel is continuous annular space.
8. according to the device described in claim 1, it is characterised in that：The absorbing liquid entrance connection liquid phase distribution of the reaction tube
Device, liquid phase distributor is arranged on reaction tube center line, and absorbing liquid is sprayed from top to bottom, and liquid phase distributor sets 1~10.
9. according to the device described in claim 8, it is characterised in that：The liquid phase distributor sets 4~6.
10. according to the device described in claim 1, it is characterised in that：The inner barrel bottom of the gas-liquid separation pipe opens up teeth groove,
Tooth slot structure is fan-shaped teeth groove, square teeth groove, triangle teeth groove, and space width is 3mm~20mm, its bottom angle is 15~
90°。
11. according to the device described in claim 10, it is characterised in that：The tooth slot structure is lance tooth slot structure, teeth groove
Width is 5mm~8mm, and its bottom angle is 30~60 °.
12. according to the device described in claim 1, it is characterised in that：The gas-liquid separation pipe goes out provided with gaseous phase outlet and liquid phase
Mouthful, gaseous phase outlet is arranged on the side wall of the outer cylinder body of gas-liquid separation pipe, and the position of gaseous phase outlet is higher than gas-liquid separation pipe
The lower end outlet of inner barrel, liquid-phase outlet is located at the bottom of the outer cylinder body of gas-liquid separation pipe.
13. according to the device described in claim 1, it is characterised in that：The overflow plate is highly the 1/2~4/ of reservoir diameter
5。
14. according to the device described in claim 13, it is characterised in that：The overflow plate highly for reservoir diameter 2/3~
3/4。
15. according to the device described in claim 1, it is characterised in that：According to sour gas flow direction, the height of the overflow plate
Gradually increase.
16. according to the device described in claim 1, it is characterised in that：The outer cylinder body bottom of the gas-liquid separation pipe is located at overflow
At the 1/4~2/3 of plate radial height.
17. according to the device described in claim 16, it is characterised in that：The outer cylinder body bottom of the gas-liquid separation pipe is located at overflow
At the 1/3~1/2 of plate radial height.
18. according to the device described in claim 1, it is characterised in that：The setting buffers level control device, works as buffering area
When interior liquid level is the 1/2~3/4 of overflow plate height, product is pumped up out device.
19. according to the device described in claim 18, it is characterised in that：When liquid level is the 2/3 of overflow plate height in buffering area,
Product is pumped up out device.
20. according to the device described in claim 1, it is characterised in that：The absorbing reaction device inwall, pipeline and fluid reservoir are
Lining material.
21. according to the device described in claim 20, it is characterised in that：The absorbing reaction device inwall, pipeline and fluid reservoir are equal
For lining tetrafluoro material.
22. according to the device described in claim 1, it is characterised in that：The gas phase entrance of the penultimate stage absorbing reaction device
Set on pipeline on hydrogen sulfide on-line computing model, the alkali liquor inlet pipeline and control valve is set, by hydrogen sulfide on-line computing model,
The concentration of hydrogen sulfide that detection enters in the gas of penultimate stage absorbing reaction device is fluctuated between 1000ppm~9000mmp, is exported
4 ~ 20mA continuous signal, sets the regulation for sodium hydroxide solution inlet amount in alkali liquor inlet pipeline, realizes device oneself
Dynamicization production process.
23. a kind of utilization sour gas produces the process of NaHS, using the dress any one of claim 1-22
Put, processing sour gas production NaHS, sour gas enters from first order absorption reactor, and weary gas is from M grades of absorbing reaction device gas
Phase entrance is introduced, and sour gas enters corresponding liquid storage area with the reacted reaction generation liquid of absorbing liquid, then through absorbing reaction device
Liquid phase material entrance and absorbing liquid entrance return to absorbing reaction device respectively, reacted sour gas enters next stage absorbing reaction
Device continues to react, until qualified discharge after being reacted through afterbody absorbing reaction device, the material of the buffering area is all the way as production
Product, another road enters pans with being used after alkaline reaction as absorbing liquid.
24. in accordance with the method for claim 23, it is characterised in that：The sour gas is various sources containing H2S sour gas.
25. in accordance with the method for claim 24, it is characterised in that：The sour gas includes hydrogen sulfide and carbon dioxide.
26. in accordance with the method for claim 23, it is characterised in that：The reaction temperature of the absorbing reaction device is 70~100
℃。
27. in accordance with the method for claim 26, it is characterised in that：The reaction temperature of the absorbing reaction device is 80~95
℃。
28. in accordance with the method for claim 23, it is characterised in that：The liquid of absorbing liquid and sour gas in the absorbing reaction device
Gas ratio is 3~20L/m3。
29. according to the method any one of claim 28, it is characterised in that：Absorbing liquid and acid in the absorbing reaction device
Property gas liquid-gas ratio be 5~10 L/m3。
30. in accordance with the method for claim 23, it is characterised in that：In every grade of liquid storage area, the liquid through absorbing reaction device
The reaction generation liquid that phase materials entrance enters absorbing reaction device enters absorbing reaction device with the absorbing liquid entrance through absorbing reaction device
Reaction generation liquid volume flow ratio be 1/20~9/10.
31. in accordance with the method for claim 30, it is characterised in that：In every grade of liquid storage area, the liquid through absorbing reaction device
The reaction generation liquid that phase materials entrance enters absorbing reaction device enters absorbing reaction device with the absorbing liquid entrance through absorbing reaction device
Reaction generation liquid volume flow ratio be 1/10~1/3.
32. in accordance with the method for claim 23, it is characterised in that：The buffering area is provided with outlet for product, product discharge
Mouthful point two-way, is connected, another road is connected through pipeline with pans with product discharge pipeline all the way, wherein into the product of pans
Volume flow ratio with the product through product discharge pipeline is 1/6~1/2.
33. according to the method described in claim 32, it is characterised in that：The product of the entrance pans with through product discharge pipe
The volume flow ratio of the product of line is 1/4~1/2.
34. in accordance with the method for claim 23, it is characterised in that：NaOH solution mass concentration is 20%~60%.
35. according to the method described in claim 34, it is characterised in that：NaOH solution mass concentration is 32%~38%.
36. in accordance with the method for claim 23, it is characterised in that：The weary gas is not reacted with sour gas and NaOH solution
Arbitrary gas.
37. according to the method described in claim 36, it is characterised in that：The weary gas is low-pressure gas, nitrogen, inert gas
Any of.
38. in accordance with the method for claim 23, it is characterised in that：The volume flow of the weary gas and sour gas suction line
The volume flow ratio of the sour gas at place is 1:1~3:1.
39. according to the method described in claim 38, it is characterised in that：The volume flow of the weary gas and sour gas suction line
The volume flow ratio of the sour gas at place is 1.5:1~2:1.
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|---|---|---|---|---|
| CN2870957Y (en) * | 2006-02-17 | 2007-02-21 | 中北大学 | Apparatus for removing hydrogen sulfide from industrial gas |
| EP1938886B1 (en) * | 2006-12-29 | 2012-11-14 | Casals Cardona Industrial, S.A. | Biological procedure for H2S removal from a gas |
| CN102921277A (en) * | 2012-10-23 | 2013-02-13 | 中国石油化工股份有限公司 | Hydrogen sulfide tail gas treatment system and method |
| CN103111177A (en) * | 2013-02-26 | 2013-05-22 | 余国贤 | Method and device for removing hydrogen sulfide in gas phase through oxidation |
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2014
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2870957Y (en) * | 2006-02-17 | 2007-02-21 | 中北大学 | Apparatus for removing hydrogen sulfide from industrial gas |
| EP1938886B1 (en) * | 2006-12-29 | 2012-11-14 | Casals Cardona Industrial, S.A. | Biological procedure for H2S removal from a gas |
| CN102921277A (en) * | 2012-10-23 | 2013-02-13 | 中国石油化工股份有限公司 | Hydrogen sulfide tail gas treatment system and method |
| CN103111177A (en) * | 2013-02-26 | 2013-05-22 | 余国贤 | Method and device for removing hydrogen sulfide in gas phase through oxidation |
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