CN105254070B - A kind of method of wastewater with high concentration of sulfide coupling reaction and separation recovery elemental sulfur - Google Patents
A kind of method of wastewater with high concentration of sulfide coupling reaction and separation recovery elemental sulfur Download PDFInfo
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- CN105254070B CN105254070B CN201510738851.0A CN201510738851A CN105254070B CN 105254070 B CN105254070 B CN 105254070B CN 201510738851 A CN201510738851 A CN 201510738851A CN 105254070 B CN105254070 B CN 105254070B
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Abstract
The invention discloses a kind of method of wastewater with high concentration of sulfide coupling reaction and separation recovery elemental sulfur, it is related to a kind of processing method of wastewater with high concentration of sulfide, comprises the following steps successively：(a) sulfur-containing waste water is pre-processed, removes the insoluble matter in waste water；(b) wastewater pH is adjusted；(c) the oxidant Sodium Metabisulfite for being dissolved as liquid and nano-powder titanium dioxide are added as absorption core, and is sufficiently mixed；(d) oxidant is made to carry out oxidation reaction under the action of the centrifugal with sulfur-containing waste water in centrifugation apparatus, and by controlling centrifugation apparatus separation factor, rotary drum rotating speed, differential speed and hydraulic detention time to control oxidation reaction, while the solid sulfur granules of centrifugal sedimentation are constantly discharged by auger conveyor during oxidation reaction；(e) after reaction terminates, separating liquid is discharged by the top overfall of centrifugal sedimentation equipment, reclaims solid sulphur simple substance.The present invention is a kind of energy low-cost processes wastewater with high concentration of sulfide, while both has higher sulfide clearance, the process for sulfur removal with higher simple substance sulfur recovery rate.
Description
Technical field
The present invention relates to a kind of processing method of wastewater with high concentration of sulfide, and in particular to utilizes sulphur in oxidizing processing waste water
The method of compound.
Background technology
In the oil and gas industries such as oil-gas field development exploitation, petroleum refining, oil coking and natural gas processing
Substantial amounts of sulfur-containing waste water can be produced, especially during high Sulfurous Gas Fields Development, in gas water sulfur content be up to 3000~
5000mg/L and complicated component, it is seriously polluted to surrounding enviroment, administer difficult.
Sulfide in sulfur-containing waste water includes deliquescent H2S、HS-、S2-With the resolvability sulphur being present in suspension
Compound and the organic and inorganic class sulfide not being electrolysed.Sulfide in sulfur-containing waste water has toxicity, corrosivity, can be to processing
The normal operation of the structures of waste water produces a very large impact, when content of the sulfide in water is 1.0~25mg/L, fresh-water fishes
Will be dead in 1~3d.
At present, the method for processing sulfur-containing waste water mainly has vaporizing extract process, oxidizing process, neutralisation, vacuum extraction method, change both at home and abroad
The precipitation method, chemical flocculation, Electrochemistry Desulfurization method, alkali absorption method and biochemical process etc. are learned, wherein neutralisation and biochemical process is applicable
In processing low concentration (sulfur content<50mg/L) sulfur-containing waste water；Oxidizing process, electrochemical process and vacuum extraction method are applied to processing sulphur and contained
The sulfur-containing waste water for 50~200mg/L is measured, but electrochemical process power consumption is big, vacuum extraction method is to equipment requirement height；Chemical precipitation
Method is applied to processing sulfur content>200mg/L sulfur-containing waste water, but its caused sludge quantity is big.
For various processing methods, most basic requirement is just desirable under low cost as far as possible, is possessed as high as possible
Sulfide clearance.Meanwhile on the premise of environmental requirement is met, in order to obtain bigger income as much as possible, therefore, going
While except sulfides from wastewater, how sulfide to be converted into elemental sulfur as much as possible, so as to reach the mesh of resource reclaim
And this area thirst for always realize.
Therefore, prior art thirsts for a kind of energy low-cost processes high strength sulfide-bearing wastewater (S2-Mass concentration is up to 2000mg/
L), while both there is higher sulfide clearance, the process for sulfur removal with higher simple substance sulfur recovery rate.
The content of the invention
It is an object of the invention to：It is proposed a kind of energy low-cost processes wastewater with high concentration of sulfide (S2-Mass concentration is up to 2000mg/
L), while both there is higher sulfide clearance, the process for sulfur removal with higher simple substance sulfur recovery rate.
The object of the invention is realized by following technical proposals：
A kind of method of wastewater with high concentration of sulfide coupling reaction and separation recovery elemental sulfur, comprises the following steps successively：
(a) sulfur-containing waste water is pre-processed, removes the insoluble matter in waste water；
(b) it is 6 to adjust wastewater pH；
(c) according to C (Na2S2O5/C(S2-The ratio that adds of)=2~2.5 adds the oxidant weighting sulfurous for being dissolved as liquid
Sour sodium, add the nano-powder titanium dioxide that 0.8mg/L sizes are 10nm and be used as absorption core, and be sufficiently mixed；
(d) oxidant is carried out oxidation reaction under the action of the centrifugal with sulfur-containing waste water in centrifugation apparatus, while aoxidizing
The solid sulfur granules of centrifugal sedimentation are constantly discharged during reaction by auger conveyor；The centrifugation apparatus separation factor is
692~2120, rotary drum rotating speed is 2000~4000r/min, and differential speed is 20~40r/min, hydraulic detention time is 10~
35min；
In such scheme, during oxidation reaction, separating liquid is discharged by the top overfall of centrifugal sedimentation equipment,
By controlling centrifugation apparatus separation factor, hydraulic detention time, while oxidation reaction generates elemental sulfur, height is constantly isolated
The simple substance sulphur granule of surface energy, it is ensured that desulfurization oxidation reaction chain rests on the elemental sulfur stage, reduces the accessory substance of reaction, improves single
Matter sulphur recovery efficiency.Separation factor Fr, refer to that suspension in centrifugal separator drum or emulsion are suffered in centrifugal force field
Centrifugal force and its gravity ratio, be the leading indicator for weighing centrifugal separator performance.Fr is bigger, the motive force of centrifugation
Bigger, the separating property of centrifugal separator is also better.
By the way that the selective paraffin oxidation of wastewater with high concentration of sulfide and separation process are coupled, the higher removal efficiency of sulphion is realized
The resource reclaim efficiency higher with elemental sulfur is the key problem in technology and innovative point of the present invention.In the present invention, by oxidation reaction
Condition, oxidation-reduction potential, oxidation reaction process are controlled, and realize that by the sulphion selective paraffin oxidation in waste water be elemental sulfur
Target, and course of reaction and separation process are coupled, reaction and the separation of elemental sulfur are realized using centrifugal sedimentation equipment, this
Technology is the key link of the present invention program.
To those skilled in the art, under the premise of foregoing basic ideas, both there is sulfide as high as possible
Clearance, there is simple substance sulfur recovery rate as high as possible again, be still a difficult, non-obvious thing.
Difficult point of the invention is that in whole oxidizing process, the chemical reaction being related to is complex, element sulphur first
Form is varied, to reach the high removal efficiency of sulfide and the high organic efficiency of elemental sulfur simultaneously, it is necessary to from reaction system
Design, the design of reaction process unit, many aspects such as the control of reaction condition carry out creative work：
The key reaction of oxidation sulfur-containing waste water of the present invention has：
S2O5 2-+2S2-+4H+=2S ↓+S2O3 2-+2H2O ①
2S2O3 2-+ S=S4O6 2-+S2- ②
S2O5 2-+H2O=2HSO3 - ③
HSO3 -+OH-=SO3 2-+H2O ④
SO3 2-+ S=S2O3 2- ⑤
1) reaction condition difficult point：Because original sulfur-containing waste water is in alkalescence, and in the basic conditions, a large amount of OH-Presence not
Beneficial to being smoothed out for desulphurization reaction, while the generation of elemental sulfur is hindered, removal effect of the sulfide in alkaline range is not
It is good.And in the environment of peracid, HS in waste water-Generation H can be protonated2S, it is unfavorable for that while reaction is carried out H can be caused2S gases
A large amount of loss.
2) oxidant dosage difficult point：Oxidant dosage directly affects the ORP value (oxidation-reduction potential) in solution, and
ORP be react whole system redox state overall target, when ORP value is excessive, although now sulfide clearance compared with
Height, but excessive ORP make it that the oxidability of solution is excessive so that the ratio that sulfide is converted into sulfate radical also accordingly increases
Add.When ORP value is too small, the ratio that sulfide is converted into sulfate radical reduces but sulfide clearance also accordingly reduces.
3) oxidant selection difficult point：For oxidant, if itself ORP value is excessive, although can guarantee that higher
Sulfide clearance, but excessive ORP make it that the oxidability of solution is excessive so that sulfide is converted into the ratio of sulfate radical
Also corresponding increase, and too small ORP value is it cannot be guaranteed that the clearance of sulfide.
4) oxidation reaction process controlling difficulties：The present invention uses Sodium Metabisulfite, S2O5 2-Middle S elements are+4 valencys, are in
The middle valence state of S elements, belongs to weak oxidant, and in oxidizing process, Sodium Metabisulfite is made oxidizing sulfur-containing waste water and existed
The course of reaction of Various Complex, and to obtain the growing amount of higher sulfide clearance and oxidation product elemental sulfur, then should
The interference of a variety of reactions is excluded, the purpose reacted 1. as Sodium Metabisulfite sulfur oxide compound is reacted, and obvious, this control
System is difficult.When oxidant dosage within the specific limits when, with the increase of oxidant dosage, occur in the unit interval
The molecular number increase of effective collision, S2O5 2-With S2-Fully contact, reaction rate are accelerated.After oxidant excess, mistake in solution
The S of amount2O5 2-The increase of thiosulfate growing amount can be caused, substantial amounts of thiosulfate can not only consume part elemental sulfur, also
The generation again of sulphion can be promoted, cause sulfide clearance and elemental sulfur yield reduction.Meanwhile when oxidant excess
Afterwards, the oxidability of solution is excessive, and the ratio that sulfide is converted into sulfate radical also accordingly increases.In addition, lay particular stress on inferior sulfate radical water
The bisulfite that solution obtains is converted into sulphite in alkaline environment, and the accumulation of sulphite can cause thiosulfate to produce
Amount increase, and excessive sulphite and thiosulfate can decompose part elemental sulfur, while cause sulfide mass concentration
Rise, reduce the clearance of sulfide.In addition to the control of reaction intermediate, the phase transformation control of course of reaction and this hair
The difficult point of bright process control, in course of reaction the form of sulphur by solubilised state S2-Reaction generation solid elemental sulfur, the process of phase transformation
In, initial single crystal solid elemental sulfur specific surface area is very big, easily generates accessory substance, it is necessary to be rolled into a ball as early as possible by further reaction
Gather, reduction surface energy, be used as absorption core by adding the nano-powder titanium dioxide that 0.8mg/L sizes are 10nm in the present invention
The heart, the elemental sulfur of generation is reunited as early as possible, realize higher simple substance sulphur recovery efficiency.
Secondly, the present invention utilizes centrifugation apparatus, realizes that reaction moves to elemental sulfur direction by the optimized synchronization of process conditions
Dynamic and elemental sulfur two big target of high efficiente callback is also the difficult point of this technology.Continued in time using centrifugation apparatus in processing procedure
Isolate caused elemental sulfur in course of reaction in ground so that reaction balance is all the time farthest towards the side required for inventor
To progress：It can prevent elemental sulfur from continuing to be oxidized to the sulfur-containing compound of more expensive state or being reduced into S2-, so as to reduce simple substance
The amount that sulphur is consumed；In addition, during the course of the reaction separating the elemental sulfur of generation, due to the reduction of product, can promote
Purpose is reacted to be carried out to positive direction, so as to improve sulfide clearance and elemental sulfur growing amount；Elemental sulfur needed for simultaneously is also same
Step is simply and rapidly reclaimed, and scheme is simply efficient, inexpensive.
In water treatment field, centrifugation apparatus is widely used, all simply conventionally as most traditional separation of solid and liquid
Equipment uses, i.e., before or after desulphurization reaction, after being more desulphurization reaction, and as just the means of product separation of solid and liquid, and
Overall control is not carried out as a part for whole reaction system.
In the prior art, the scheme using centrifugal action as core link during desulphurization reaction is had no.
In process regulation, centrifugation apparatus rotary drum rotating speed, differential speed, hydraulic detention time are most important three control
Condition.
1) rotating speed：In conventional centrifugal technological design, to improve solid-liquid separation effect, mostly using higher rotating speed and compared with
Big separation factor, the present invention are synchronous to realize reaction and the coupling separated, it is necessary to consider to improve simultaneously in centrifugal sedimentation equipment
The production rate and solid-liquid separation efficiency of elemental sulfur.S in waste water2-Content is certain, under other conditions same case, when centrifugal reel turns
When speed is relatively low, the growing amount of sulfide clearance and elemental sulfur is relatively low.Because the relative centrifugation in the case of low centrifugal rotational speed
Power is insufficient to allow caused elemental sulfur in course of reaction to be agglomerated into larger particles and depart from reaction solution rapidly, under this slow-speed of revolution
Reaction carried out equivalent to elemental sulfur in the state of overall solution is sufficiently stirred, promoting side reaction on the contrary is divided elemental sulfur
Solve, only guaranteed certain centrifugal rotational speed, could produce sufficiently large RCF makes elemental sulfur depart from reaction solution.But such as
Fruit centrifugal reel rotating speed is too big, and the solid sulfur particle breakdown that excessive operating on centrifugal force can cause to have generated crushes, and causes simple substance
Sulphur is again introduced into reaction solution so as to promote side reaction；And as the increase of rotary drum rotating speed, the mechanical wear of equipment also can
Increase.
2) differential speed：Differential speed is the difference of bowl rotating speed and revolution speed of screw, and increaseing or decreasing speed discrepancy can change
Become residence time of the solid particle in rotary drum.Only in the case of suitable differential speed is ensured, it can just make the solid of generation
Grain residence time in centrifuge is relatively reasonable, in time releases solid particle while just can guarantee that higher disposal ability,
Ensure solid recovery rate.
3) hydraulic detention time：The generation of elemental sulfur progress synchronous with separating in the present invention, the residence time is too short to be possible to
Cause S2-Do not remove completely also, cause desulfuration efficiency relatively low, the residence time is long, it is possible to make the elemental sulfur of generation further
Accessory substance is oxidized to, therefore it is to realize S to control hydraulic detention time2-Higher removal efficiency and the higher resource of elemental sulfur return
The key parameter for rate of producing effects.
In summary, the present invention passes through specific control parameter so that the present invention both there is sulfide as high as possible to go
Except rate, there is simple substance sulfur recovery rate as high as possible again.
As preferred parameter, regulation wastewater pH is 6 in the step (b), according to C (Na in step (c)2S2O5)/C(S2-)
=2.25 ratio that adds adds oxidant, adds the nano-powder titanium dioxide that 0.8mg/L sizes are 10nm, in step (d)
Centrifugation apparatus separation factor is 1558, and rotary drum rotating speed is 3000r/min, differential speed 40r/min, and hydraulic detention time is
35min。
In the present invention, as the centrifugation apparatus of key equipment, the various existing equipments with suitable centrifugation ability can be selected,
For example realize sweetening process using common horizontal spiral centrifuge.Centrifuge is by centrifugal force field caused by high speed rotation
Different factor in precipitation compounding substances are carried out with quick separating, concentration and the Special Equipment of purification.The work of horizontal spiral centrifuge
Principle is to be sent into the waste water for being mixed with oxidant in the bowl of rotation at a high speed through feed pipe, centrifuges and is generated in course of reaction
Solid particle sulphur simple substance rapid subsidence is to drum inner wall under the powerful centrifugal action of rotary drum, the phase of auger conveyor and rotary drum
The carrying capacity of a propulsion can be produced to the solid being deposited in rotary drum to differential (i.e. speed discrepancy), is passed through under the influence of centrifugal force
Slag-drip opening is discharged, and liquid phase then flows out from centrifuge top overfall.
Beneficial effects of the present invention：The present invention combines redox reaction and centrifugal separation processes, anti-
Elemental sulfur is separated from reaction solution while elemental sulfur is produced during answering, prevents elemental sulfur from continuing to be oxidized, and
Promote reaction to be carried out to positive direction, reach the purpose for improving sulfide clearance and simple substance sulfur recovery rate；Specific selection simultaneously
Control parameter so that the program can both have sulfide clearance as high as possible, have elemental sulfur as high as possible again
The rate of recovery.
Brief description of the drawings
Fig. 1 is the process flow diagram of the present invention；
Fig. 2 is the structural representation of horizontal spiral centrifuge；
In figure, 1- acid storages, 2- measuring pumps, 3- sumps, 4- sewage pumps, 5- dosing tanks, 6- measuring pumps, 7,8- pipelines mix
Close ejector, 9- horizontal spiral centrifuges, 10-PLC controllers, 11- mixed liquor delivery pumps, 12- powder mixing channels, 13- water inlets
Mouthful, the outlet of 14- solids elemental sulfur, 15- discharge channels, 16- rotary drum motors, 17- differential speed motors.
Embodiment
Following non-limiting examples are used to illustrate the present invention.
With reference to figure 1, Fig. 2, a kind of method of wastewater with high concentration of sulfide coupling reaction and separation recovery elemental sulfur, successively including following step
Suddenly：
(a) sulfur-containing waste water is pre-processed, the insoluble matter such as suspended particulate, oil slick in removal waste water.
(b) HCl that volumetric concentration in acid storage is 50% is pumped into from measuring pump while being pumped into waste water using sewage pump, is adjusted
It is 6 to save wastewater pH；It is further to select, can be in acid solution and the mixed pipeline mixing jet device of waste water in the step
PH value detecting instrument is set, passes through its control reaction initial pH value.
(c) according to C (Na2S2O5)/C(S2-)=2~2.5 add ratio to step (b) adjust pH after waste water be pumped into it is molten
Oxidant Sodium Metabisulfite and nano-powder titanium dioxide for liquid are solved as absorption core, and utilizes pipeline mixing jet
Device is sufficiently mixed；It is further to select, in the step, oxygen can be set in the pipeline mixing jet device after adding oxidant
Change reduction potential ORP value detecting instrument, ORP value in course of reaction is controlled by it.It is preferred that ORP value 132.
(d) waste water added step (c) after oxidant is introduced into centrifuge by mixing jet device, is mixed with oxidant
Waste water carries out redox reaction after entering centrifugal sedimentation equipment rotary drum, react the solid sulfur granules sulphur of generation rotary drum it is powerful from
Rapid subsidence turns to drum inner wall, relative differential (i.e. speed discrepancy) meeting of auger conveyor and rotary drum to being deposited under mental power function
Solid in drum produces the carrying capacity of a propulsion, and last solid is discharged through slag-drip opening, and liquid phase then flows out from overfall.Centrifuge
Separation factor Fr and rotary drum rotating speed into quadratic relationship, rotating speed is bigger, and separation factor is bigger, and the centrifugal force that material is received is bigger, separation
Effect is also better.The centrifugation apparatus separation factor is 692~2120, and rotary drum rotating speed is 2000~4000r/min, differential speed
For 20~40r/min, hydraulic detention time is 10~35min.
(e) after reaction terminates, separating liquid is discharged, solid sulphur simple substance is reclaimed, completes whole sweetening process.
By taking horizontal spiral centrifuge as an example, in the actual motion of centrifuge, it is necessary to by adjusting into the useless of centrifuge
Water ensures desulfurized effect of the centrifuge to sulfur-containing waste water.Wastewater flow rate is excessive, can exceed that the load that centrifuge can bear,
So that the normal operation of centrifuge is influenceed while centrifugal effect is bad；Wastewater flow rate is too small, will cause the waste of energy consumption.To ensure
The normal operation of centrifuge, and can meet the desulfurization requirement of sulfur-containing waste water, and the treating capacity of centrifuge is set into maximum processing capability
80%.In the present invention, design centrifuge works 8h daily, and the treating capacity of used horizontal spiral centrifuge is set as
18m3/h。
Embodiment one：
Pretreated sulfur-containing waste water (S will be passed through2-Mass concentration is about 2000mg/L) 100L is pumped into wastewater trough 3, then profit
Waste water is pumped into pipeline mixing jet device 7 with sewage pump 4, while is 50% by volumetric concentration in acid storage 1 using measuring pump 2
Hydrochloric acid be added in the waste water pumped out, be sufficiently mixed using pipeline mixing jet device 7, control ph 6.Adjust pH value
Waste water afterwards enters pipeline mixing jet device 8, while is laid particular stress on the oxidant that liquid is dissolved as in dosing tank 5 using measuring pump 6
Sodium sulfite presses C (Na2S2O5)/C(S2-Adding in the waste water after ratio is added to regulation pH value for)=2.25, utilizes mixed liquor
The nano-powder titanium dioxide that size in powder mixing channel 12 is 10nm is added to tune by delivery pump 11 according to 0.8mg/L dosage
Save in the waste water after pH value, be sufficiently mixed using pipeline mixing jet device 8, it is 132 to control ORP value.Add oxidant and
Waste water after nano-powder titanium dioxide is introduced into horizontal spiral centrifuge 9 by mixing jet device carries out redox reaction,
The treating capacity for controlling centrifuge is 18m3/ h, centrifuge separation factor are 692, rotating speed 2000r/min, differential speed 20r/
Min, hydraulic detention time 10min, S after reaction2-Mass concentration is 283.40mg/L, and sulfide clearance takes up to 85.83%
By the sulfur granules isolated of solid elemental sulfur outlet 14, by gravimetric method elemental sulfur growing amount is referred to as 396mg/L.
Device is controlled by PLC, by receiving the feedback signal of horizontal spiral centrifuge electric current, adjust from
Scheming separation factor, rotary drum rotating speed, differential speed and hydraulic detention time, the desulfurized effect and elemental sulfur for controlling sulfur-containing waste water return
Yield.PLC is controlled automatically by receiving pH value and the feedback signal of ORP value detecting instrument in pipeline mixing jet device simultaneously
PH value and ORP value in course of reaction processed, so as to realize the stable operation of system.
Embodiment two：
Pretreated sulfur-containing waste water (S will be passed through2-Mass concentration is about 2000mg/L) 100L is pumped into wastewater trough 3, then profit
Waste water is pumped into pipeline mixing jet device 7 with sewage pump 4, while is 50% by volumetric concentration in acid storage 1 using measuring pump 2
Hydrochloric acid be added in the waste water pumped out, be sufficiently mixed using pipeline mixing jet device 7, control ph 6.Adjust pH value
Waste water afterwards enters pipeline mixing jet device 8, while is laid particular stress on the oxidant that liquid is dissolved as in dosing tank 5 using measuring pump 6
Sodium sulfite presses C (Na2S2O5)/C(S2-Adding in the waste water after ratio is added to regulation pH value for)=2, is conveyed using mixed liquor
The nano-powder titanium dioxide that size in powder mixing channel 12 is 10nm is added to regulation pH by pump 11 according to 0.8mg/L dosage
In waste water after value, it is sufficiently mixed using pipeline mixing jet device 8, it is 132 to control ORP value.Add useless after oxidant
Water is introduced into horizontal spiral centrifuge 9 by mixing jet device and carries out redox reaction, and the treating capacity for controlling centrifuge is
18m3/ h, centrifuge separation factor are 692, rotating speed 2000r/min, differential speed 20r/min, and hydraulic detention time is
10min, S after reaction2-Mass concentration is 407.48mg/L, and sulfide clearance takes up to 79.63% and exports 14 by solid elemental sulfur
The sulfur granules isolated, by gravimetric method elemental sulfur growing amount is referred to as 298mg/L.
Embodiment three：
Pretreated sulfur-containing waste water (S will be passed through2-Mass concentration is about 2000mg/L) 100L is pumped into wastewater trough 3, then profit
Waste water is pumped into pipeline mixing jet device 7 with sewage pump 4, while is 50% by volumetric concentration in acid storage 1 using measuring pump 2
Hydrochloric acid be added in the waste water pumped out, be sufficiently mixed using pipeline mixing jet device 7, control ph 6.Adjust pH value
Waste water afterwards enters pipeline mixing jet device 8, while is laid particular stress on the oxidant that liquid is dissolved as in dosing tank 5 using measuring pump 6
Sodium sulfite presses C (Na2S2O5)/C(S2-Adding in the waste water after ratio is added to regulation pH value for)=2.5, it is defeated using mixed liquor
Send pump 11 that the nano-powder titanium dioxide that size in powder mixing channel 12 is 10nm is added into regulation according to 0.8mg/L dosage
In waste water after pH value, it is sufficiently mixed using pipeline mixing jet device 8, it is 132 to control ORP value.After adding oxidant
Waste water is introduced into horizontal spiral centrifuge 9 by mixing jet device and carries out redox reaction, and the treating capacity for controlling centrifuge is
18m3/ h, centrifuge separation factor are 692, rotating speed 2000r/min, differential speed 20r/min, and hydraulic detention time is
10min, S after reaction2-Mass concentration is 349.74mg/L, and sulfide clearance takes up to 82.51% and exports 14 by solid elemental sulfur
The sulfur granules isolated, by gravimetric method elemental sulfur growing amount is referred to as 351mg/L.
Example IV：
Pretreated sulfur-containing waste water (S will be passed through2-Mass concentration is about 2000mg/L) 100L is pumped into wastewater trough 3, then profit
Waste water is pumped into pipeline mixing jet device 7 with sewage pump 4, while is 50% by volumetric concentration in acid storage 1 using measuring pump 2
Hydrochloric acid be added in the waste water pumped out, be sufficiently mixed using pipeline mixing jet device 7, control ph 6.Adjust pH value
Waste water afterwards enters pipeline mixing jet device 8, while is laid particular stress on the oxidant that liquid is dissolved as in dosing tank 5 using measuring pump 6
Sodium sulfite presses C (Na2S2O5)/C(S2-Adding in the waste water after ratio is added to regulation pH value for)=2.25, utilizes mixed liquor
The nano-powder titanium dioxide that size in powder mixing channel 12 is 10nm is added to tune by delivery pump 11 according to 0.8mg/L dosage
Save in the waste water after pH value, be sufficiently mixed using pipeline mixing jet device 8, it is 132 to control ORP value.After adding oxidant
Waste water be introduced into by mixing jet device in horizontal spiral centrifuge 9 and carry out redox reaction, control the treating capacity of centrifuge
For 18m3/ h, centrifuge separation factor are 1558, rotating speed 3000r/min, differential speed 20r/min, and hydraulic detention time is
10min, S after reaction2-Mass concentration is 136.53mg/L, and sulfide clearance takes up to 93.17% and exports 14 by solid elemental sulfur
The sulfur granules isolated, by gravimetric method elemental sulfur growing amount is referred to as 607mg/L.
Embodiment five：
Pretreated sulfur-containing waste water (S will be passed through2-Mass concentration is about 2000mg/L) 100L is pumped into wastewater trough 3, then profit
Waste water is pumped into pipeline mixing jet device 7 with sewage pump 4, while is 50% by volumetric concentration in acid storage 1 using measuring pump 2
Hydrochloric acid be added in the waste water pumped out, be sufficiently mixed using pipeline mixing jet device 7, control ph 6.Adjust pH value
Waste water afterwards enters pipeline mixing jet device 8, while is laid particular stress on the oxidant that liquid is dissolved as in dosing tank 5 using measuring pump 6
Sodium sulfite presses C (Na2S2O5)/C(S2-Adding in the waste water after ratio is added to regulation pH value for)=2.25, utilizes mixed liquor
The nano-powder titanium dioxide that size in powder mixing channel 12 is 10nm is added to tune by delivery pump 11 according to 0.8mg/L dosage
Save in the waste water after pH value, be sufficiently mixed using pipeline mixing jet device 8, it is 132 to control ORP value.After adding oxidant
Waste water be introduced into by mixing jet device in horizontal spiral centrifuge 9 and carry out redox reaction, control the treating capacity of centrifuge
For 18m3/ h, centrifuge separation factor are 2120, rotating speed 4000r/min, differential speed 20r/min, and hydraulic detention time is
10min, S after reaction2-Mass concentration is 274.26mg/L, and sulfide clearance takes up to 86.29% and exports 14 by solid elemental sulfur
The sulfur granules isolated, by gravimetric method elemental sulfur growing amount is referred to as 483mg/L.
Embodiment six：
Pretreated sulfur-containing waste water (S will be passed through2-Mass concentration is about 2000mg/L) 100L is pumped into wastewater trough 3, then profit
Waste water is pumped into pipeline mixing jet device 7 with sewage pump 4, while is 50% by volumetric concentration in acid storage 1 using measuring pump 2
Hydrochloric acid be added in the waste water pumped out, be sufficiently mixed using pipeline mixing jet device 7, control ph 6.Adjust pH value
Waste water afterwards enters pipeline mixing jet device 8, while is laid particular stress on the oxidant that liquid is dissolved as in dosing tank 5 using measuring pump 6
Sodium sulfite presses C (Na2S2O5)/C(S2-Adding in the waste water after ratio is added to regulation pH value for)=2.25, utilizes mixed liquor
The nano-powder titanium dioxide that size in powder mixing channel 12 is 10nm is added to tune by delivery pump 11 according to 0.8mg/L dosage
Save in the waste water after pH value, be sufficiently mixed using pipeline mixing jet device 8, it is 132 to control ORP value.After adding oxidant
Waste water be introduced into by mixing jet device in horizontal spiral centrifuge 9 and carry out redox reaction, control the treating capacity of centrifuge
For 18m3/ h, centrifuge separation factor are 1558, rotating speed 3000r/min, differential speed 30r/min, and hydraulic detention time is
10min, S after reaction2-Mass concentration is 113.32mg/L, and sulfide clearance takes up to 94.33% and exports 14 by solid elemental sulfur
The sulfur granules isolated, by gravimetric method elemental sulfur growing amount is referred to as 833mg/L.
Embodiment seven：
Pretreated sulfur-containing waste water (S will be passed through2-Mass concentration is about 2000mg/L) 100L is pumped into wastewater trough 3, then profit
Waste water is pumped into pipeline mixing jet device 7 with sewage pump 4, while is 50% by volumetric concentration in acid storage 1 using measuring pump 2
Hydrochloric acid be added in the waste water pumped out, be sufficiently mixed using pipeline mixing jet device 7, control ph 6.Adjust pH value
Waste water afterwards enters pipeline mixing jet device 8, while is laid particular stress on the oxidant that liquid is dissolved as in dosing tank 5 using measuring pump 6
Sodium sulfite presses C (Na2S2O5)/C(S2-Adding in the waste water after ratio is added to regulation pH value for)=2.25, utilizes mixed liquor
The nano-powder titanium dioxide that size in powder mixing channel 12 is 10nm is added to tune by delivery pump 11 according to 0.8mg/L dosage
Save in the waste water after pH value, be sufficiently mixed using pipeline mixing jet device 8, it is 132 to control ORP value.After adding oxidant
Waste water be introduced into by mixing jet device in horizontal spiral centrifuge 9 and carry out redox reaction, control the treating capacity of centrifuge
For 18m3/ h, centrifuge separation factor are 1558, rotating speed 3000r/min, differential speed 40r/min, and hydraulic detention time is
10min, S after reaction2-Mass concentration is 98.46mg/L, and sulfide clearance takes up to 95.08% and exports 14 by solid elemental sulfur
The sulfur granules isolated, by gravimetric method elemental sulfur growing amount is referred to as 946mg/L.
Embodiment eight：
Pretreated sulfur-containing waste water (S will be passed through2-Mass concentration is about 2000mg/L) 100L is pumped into wastewater trough 3, then profit
Waste water is pumped into pipeline mixing jet device 7 with sewage pump 4, while is 50% by volumetric concentration in acid storage 1 using measuring pump 2
Hydrochloric acid be added in the waste water pumped out, be sufficiently mixed using pipeline mixing jet device 7, control ph 6.Adjust pH value
Waste water afterwards enters pipeline mixing jet device 8, while is laid particular stress on the oxidant that liquid is dissolved as in dosing tank 5 using measuring pump 6
Sodium sulfite presses C (Na2S2O5)/C(S2-Adding in the waste water after ratio is added to regulation pH value for)=2.25, utilizes mixed liquor
The nano-powder titanium dioxide that size in powder mixing channel 12 is 10nm is added to tune by delivery pump 11 according to 0.8mg/L dosage
Save in the waste water after pH value, be sufficiently mixed using pipeline mixing jet device 8, it is 132 to control ORP value.After adding oxidant
Waste water be introduced into by mixing jet device in horizontal spiral centrifuge 9 and carry out redox reaction, control the treating capacity of centrifuge
For 18m3/ h, centrifuge separation factor are 1558, rotating speed 3000r/min, differential speed 40r/min, and hydraulic detention time is
20min, S after reaction2-Mass concentration is 89.24mg/L, and sulfide clearance takes up to 95.54% and exports 14 by solid elemental sulfur
The sulfur granules isolated, by gravimetric method elemental sulfur growing amount is referred to as 1058mg/L.
Embodiment nine：
Pretreated sulfur-containing waste water (S will be passed through2-Mass concentration is about 2000mg/L) 100L is pumped into wastewater trough 3, then profit
Waste water is pumped into pipeline mixing jet device 7 with sewage pump 4, while is 50% by volumetric concentration in acid storage 1 using measuring pump 2
Hydrochloric acid be added in the waste water pumped out, be sufficiently mixed using pipeline mixing jet device 7, control ph 6.Adjust pH value
Waste water afterwards enters pipeline mixing jet device 8, while is laid particular stress on the oxidant that liquid is dissolved as in dosing tank 5 using measuring pump 6
Sodium sulfite presses C (Na2S2O5)/C(S2-Adding in the waste water after ratio is added to regulation pH value for)=2.25, utilizes mixed liquor
The nano-powder titanium dioxide that size in powder mixing channel 12 is 10nm is added to tune by delivery pump 11 according to 0.8mg/L dosage
Save in the waste water after pH value, be sufficiently mixed using pipeline mixing jet device 8, it is 132 to control ORP value.After adding oxidant
Waste water be introduced into by mixing jet device in horizontal spiral centrifuge 9 and carry out redox reaction, control the treating capacity of centrifuge
For 18m3/ h, centrifuge separation factor are 1558, rotating speed 3000r/min, differential speed 40r/min, and hydraulic detention time is
35min, S after reaction2-Mass concentration is 74.29mg/L, and sulfide clearance takes up to 96.29% and exports 14 by solid elemental sulfur
The sulfur granules isolated, by gravimetric method elemental sulfur growing amount is referred to as 1122mg/L.
Comparative example one：
Pretreated sulfur-containing waste water (S will be passed through2-Mass concentration is about 2000mg/L) 100L is pumped into wastewater trough 3, then profit
Waste water is pumped into pipeline mixing jet device 7 with sewage pump 4, while is 50% by volumetric concentration in acid storage 1 using measuring pump 2
Hydrochloric acid be added in the waste water pumped out, be sufficiently mixed using pipeline mixing jet device 7, control ph 6.Adjust pH value
Waste water afterwards enters pipeline mixing jet device 8, while is laid particular stress on the oxidant that liquid is dissolved as in dosing tank 5 using measuring pump 6
Sodium sulfite presses C (Na2S2O5)/C(S2-Adding in the waste water after ratio is added to regulation pH value for)=2.25, utilizes mixed liquor
The nano-powder titanium dioxide that size in powder mixing channel 12 is 10nm is added to tune by delivery pump 11 according to 0.8mg/L dosage
Save in the waste water after pH value, be sufficiently mixed using pipeline mixing jet device 8, it is 132 to control ORP value.After adding oxidant
Waste water be introduced into by mixing jet device in reactor and carry out redox reaction, after reacting 10min, S2-Mass concentration is
598.43mg/L, sulfide clearance 70.08%, the solid sulfur granules isolated are taken, claim to obtain elemental sulfur growing amount by gravimetric method
For 206mg/L.
Comparative example two：
Pretreated sulfur-containing waste water (S will be passed through2-Mass concentration is about 2000mg/L) 100L is pumped into wastewater trough 3, then profit
Waste water is pumped into pipeline mixing jet device 7 with sewage pump 4, while is 50% by volumetric concentration in acid storage 1 using measuring pump 2
Hydrochloric acid be added in the waste water pumped out, be sufficiently mixed using pipeline mixing jet device 7, control ph 6.Adjust pH value
Waste water afterwards enters pipeline mixing jet device 8, while is laid particular stress on the oxidant that liquid is dissolved as in dosing tank 5 using measuring pump 6
Sodium sulfite presses C (Na2S2O5)/C(S2-Adding in the waste water after ratio is added to regulation pH value for)=2, is conveyed using mixed liquor
The nano-powder titanium dioxide that size in powder mixing channel 12 is 10nm is added to regulation pH by pump 11 according to 0.8mg/L dosage
In waste water after value, it is sufficiently mixed using pipeline mixing jet device 8, it is 132 to control ORP value.Add useless after oxidant
Water is introduced into reactor by mixing jet device and carries out redox reaction, after reacting 10min, S2-Mass concentration is
757.84mg/L, sulfide clearance take the solid sulfur granules isolated, claim to obtain elemental sulfur generation by gravimetric method up to 62.11%
Measure as 145mg/L.
Comparative example three：
Pretreated sulfur-containing waste water (S will be passed through2-Mass concentration is about 2000mg/L) 100L is pumped into wastewater trough 3, then profit
Waste water is pumped into pipeline mixing jet device 7 with sewage pump 4, while is 50% by volumetric concentration in acid storage 1 using measuring pump 2
Hydrochloric acid be added in the waste water pumped out, be sufficiently mixed using pipeline mixing jet device 7, control ph 6.Adjust pH value
Waste water afterwards enters pipeline mixing jet device 8, while is laid particular stress on the oxidant that liquid is dissolved as in dosing tank 5 using measuring pump 6
Sodium sulfite presses C (Na2S2O5)/C(S2-Adding in the waste water after ratio is added to regulation pH value for)=2.25, is mixed using pipeline
Close ejector 8 to be sufficiently mixed, it is 132 to control ORP value.The waste water added after oxidant is introduced horizontal by mixing jet device
Redox reaction is carried out in screw centrifuge 9, the treating capacity for controlling centrifuge is 18m3/ h, centrifuge separation factor are
1558, rotating speed 3000r/min, differential speed 40r/min, hydraulic detention time 35min, S after reaction2-Mass concentration is
270.2mg/L, sulfide clearance take the sulfur granules isolated by solid elemental sulfur outlet 14, claimed by gravimetric method up to 86.49%
It is 287mg/L to obtain elemental sulfur growing amount.
Comparative example four：
Pretreated sulfur-containing waste water (S will be passed through2-Mass concentration is about 2000mg/L) 100L is pumped into wastewater trough 3, then profit
Waste water is pumped into pipeline mixing jet device 7 with sewage pump 4, while is 50% by volumetric concentration in acid storage 1 using measuring pump 2
Hydrochloric acid be added in the waste water pumped out, be sufficiently mixed using pipeline mixing jet device 7, control ph 6.Adjust pH value
Waste water afterwards enters pipeline mixing jet device 8, while is laid particular stress on the oxidant that liquid is dissolved as in dosing tank 5 using measuring pump 6
Sodium sulfite presses C (Na2S2O5)/C(S2-Adding in the waste water after ratio is added to regulation pH value for)=2.25, utilizes mixed liquor
The nano-powder titanium dioxide that size in powder mixing channel 12 is 10nm is added to tune by delivery pump 11 according to 0.8mg/L dosage
Save in the waste water after pH value, be sufficiently mixed using pipeline mixing jet device 8, it is 132 to control ORP value.After adding oxidant
Waste water be introduced into by mixing jet device in horizontal spiral centrifuge 9 and carry out redox reaction, control the treating capacity of centrifuge
For 18m3/ h, centrifuge separation factor are 173, rotating speed 1000r/min, differential speed 30r/min, and hydraulic detention time is
35min, S after reaction2-Mass concentration is 647.48mg/L, and sulfide clearance takes up to 67.63% and exports 14 by solid elemental sulfur
The sulfur granules isolated, by gravimetric method elemental sulfur growing amount is referred to as 198mg/L.
Comparative example five：
Pretreated sulfur-containing waste water (S will be passed through2-Mass concentration is about 2000mg/L) 100L is pumped into wastewater trough 3, then profit
Waste water is pumped into pipeline mixing jet device 7 with sewage pump 4, while is 50% by volumetric concentration in acid storage 1 using measuring pump 2
Hydrochloric acid be added in the waste water pumped out, be sufficiently mixed using pipeline mixing jet device 7, control ph 6.Adjust pH value
Waste water afterwards enters pipeline mixing jet device 8, while is laid particular stress on the oxidant that liquid is dissolved as in dosing tank 5 using measuring pump 6
Sodium sulfite presses C (Na2S2O5)/C(S2-Adding in the waste water after ratio is added to regulation pH value for)=2.25, utilizes mixed liquor
The nano-powder titanium dioxide that size in powder mixing channel 12 is 10nm is added to tune by delivery pump 11 according to 0.8mg/L dosage
Save in the waste water after pH value, be sufficiently mixed using pipeline mixing jet device 8, it is 132 to control ORP value.After adding oxidant
Waste water be introduced into by mixing jet device in horizontal spiral centrifuge 9 and carry out redox reaction, control the treating capacity of centrifuge
For 18m3/ h, centrifuge separation factor are 692, rotating speed 2000r/min, differential speed 30r/min, and hydraulic detention time is
5min, S after reaction2-Mass concentration is 839.72mg/L, and sulfide clearance takes up to 58.01% and exports 14 by solid elemental sulfur
The sulfur granules isolated, by gravimetric method elemental sulfur growing amount is referred to as 106mg/L.
Comparative example six：
Pretreated sulfur-containing waste water (S will be passed through2-Mass concentration is about 2000mg/L) 100L is pumped into wastewater trough 3, then profit
Waste water is pumped into pipeline mixing jet device 7 with sewage pump 4, while is 50% by volumetric concentration in acid storage 1 using measuring pump 2
Hydrochloric acid be added in the waste water pumped out, be sufficiently mixed using pipeline mixing jet device 7, control ph 5.Adjust pH value
Waste water afterwards enters pipeline mixing jet device 8, while is laid particular stress on the oxidant that liquid is dissolved as in dosing tank 5 using measuring pump 6
Sodium sulfite presses C (Na2S2O5)/C(S2-Adding in the waste water after ratio is added to regulation pH value for)=2.25, utilizes mixed liquor
The nano-powder titanium dioxide that size in powder mixing channel 12 is 10nm is added to tune by delivery pump 11 according to 0.8mg/L dosage
Save in the waste water after pH value, be sufficiently mixed using pipeline mixing jet device 8, it is 132 to control ORP value.After adding oxidant
Waste water be introduced into by mixing jet device in horizontal spiral centrifuge 9 and carry out redox reaction, control the treating capacity of centrifuge
For 18m3/ h, centrifuge separation factor are 1558, rotating speed 3000r/min, differential speed 40r/min, and hydraulic detention time is
35min, S after reaction2-Mass concentration is 594.38mg/L, and sulfide clearance takes up to 70.28% and exports 14 by solid elemental sulfur
The sulfur granules isolated, by gravimetric method elemental sulfur growing amount is referred to as 237mg/L.
Comparative example seven：
Pretreated sulfur-containing waste water (S will be passed through2-Mass concentration is about 2000mg/L) 100L is pumped into wastewater trough 3, then profit
Waste water is pumped into pipeline mixing jet device 7 with sewage pump 4, while is 50% by volumetric concentration in acid storage 1 using measuring pump 2
Hydrochloric acid be added in the waste water pumped out, be sufficiently mixed using pipeline mixing jet device 7, control ph 10.Adjust pH
Waste water after value enters pipeline mixing jet device 8, while using measuring pump 6 that the oxidant that liquid is dissolved as in dosing tank 5 is inclined
Sodium bisulfite presses C (Na2S2O5)/C(S2-Adding in the waste water after ratio is added to regulation pH value for)=2.25, utilizes mixing
The nano-powder titanium dioxide that size in powder mixing channel 12 is 10nm is added to by liquid delivery pump 11 according to 0.8mg/L dosage
Adjust in the waste water after pH value, be sufficiently mixed using pipeline mixing jet device 8, it is 132 to control ORP value.Add oxidant
Waste water afterwards is introduced into horizontal spiral centrifuge 9 by mixing jet device and carries out redox reaction, controls the processing of centrifuge
Measure as 18m3/ h, centrifuge separation factor are 1558, rotating speed 3000r/min, differential speed 40r/min, hydraulic detention time
For 35min, S after reaction2-Mass concentration is 625.40mg/L, and sulfide clearance takes and exported by solid elemental sulfur up to 68.73%
14 sulfur granules isolated, by gravimetric method elemental sulfur growing amount is referred to as 229mg/L.
Comparative example eight：
Pretreated sulfur-containing waste water (S will be passed through2-Mass concentration is about 2000mg/L) 100L is pumped into wastewater trough 3, then profit
Waste water is pumped into pipeline mixing jet device 7 with sewage pump 4, while is 50% by volumetric concentration in acid storage 1 using measuring pump 2
Hydrochloric acid be added in the waste water pumped out, be sufficiently mixed using pipeline mixing jet device 7, control ph 6.Adjust pH value
Waste water afterwards enters pipeline mixing jet device 8, while is laid particular stress on the oxidant that liquid is dissolved as in dosing tank 5 using measuring pump 6
Sodium sulfite presses C (Na2S2O5)/C(S2-Adding in the waste water after ratio is added to regulation pH value for)=1.5, it is defeated using mixed liquor
Send pump 11 that the nano-powder titanium dioxide that size in powder mixing channel 12 is 10nm is added into regulation according to 0.8mg/L dosage
In waste water after pH value, it is sufficiently mixed using pipeline mixing jet device 8, it is 132 to control ORP value.After adding oxidant
Waste water is introduced into horizontal spiral centrifuge 9 by mixing jet device and carries out redox reaction, and the treating capacity for controlling centrifuge is
18m3/ h, centrifuge separation factor are 1558, rotating speed 3000r/min, differential speed 40r/min, and hydraulic detention time is
35min, S after reaction2-Mass concentration is 685.39mg/L, and sulfide clearance takes up to 65.73% and exports 14 by solid elemental sulfur
The sulfur granules isolated, by gravimetric method elemental sulfur growing amount is referred to as 169mg/L.
Contrast is summarized：
By above-mentioned strict, sufficient comparative example, the specific parameter selection of the present invention, achieve significant effect and carry
Rise.Various conventional selections of the those skilled in the art outside the scope of claim all do not reach the effect of the present invention far.
Wherein, comparative example 1,2 is only pure zirconia desulfurization, is not associated with centrifugal process；Comparative example 3 is optimal for the holding present invention's
PH, oxidant addition and centrifugation control parameter, but nano-powder titanium dioxide is not added as absorption core；Comparative example 4,5
To keep the Optimal pH and oxidant addition of the present invention, but the centrifugation control parameter of non-invention, and change centrifuge successively
Rotating speed and hydraulic detention time；Comparative example 6,7 is to keep the centrifugation control parameter and oxidant addition of the present invention, but Fei Benfa
Bright pH；Comparative example 8 is to keep the centrifugation control parameter and pH of the present invention, but the oxidant addition of non-invention.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (2)
- A kind of 1. method of wastewater with high concentration of sulfide coupling reaction and separation recovery elemental sulfur, it is characterised in that comprise the following steps successively：（a）Sulfur-containing waste water is pre-processed, removes the insoluble matter in waste water；（b）It is 6 to adjust wastewater pH；（c）According to C（Na2S2O5）/C（S2-）=2~2.5 ratio that adds adds the oxidant weighting sulfurous acid for being dissolved as liquid Sodium, add the nano-powder titanium dioxide that 0.8mg/L sizes are 10nm and be used as absorption core, and be sufficiently mixed；（d）Reaction system is pumped into centrifugal sedimentation equipment, and it is 692 ~ 2120 to control centrifugal sedimentation equipment separation factor, and rotary drum rotating speed is 2000~4000r/min, differential speed are 20~40 r/min, and hydraulic detention time is 10~35min；（e）In centrifugal separation processes are reacted, separating liquid is discharged by the top overfall of centrifugal sedimentation equipment, passes through spiral transferring The solid sulfur granules that device constantly discharges centrifugal sedimentation are sent, reclaim solid sulphur simple substance.
- 2. the method for wastewater with high concentration of sulfide coupling reaction and separation recovery elemental sulfur as claimed in claim 1, it is characterised in that：It is described Step（c）According to C（Na2S2O5）/C（S2-）=2.25 ratio that adds adds oxidant, step（d）Described in centrifugal sedimentation set Standby separation factor is 1558, and rotary drum rotating speed is 3000r/min, and differential speed is 40 r/min, hydraulic detention time 35min.
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