CN108892105A - A kind of chlorine dioxide generator and its operation method with gas-liquid separation Yu residual liquid recycling function - Google Patents
A kind of chlorine dioxide generator and its operation method with gas-liquid separation Yu residual liquid recycling function Download PDFInfo
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- CN108892105A CN108892105A CN201811000650.0A CN201811000650A CN108892105A CN 108892105 A CN108892105 A CN 108892105A CN 201811000650 A CN201811000650 A CN 201811000650A CN 108892105 A CN108892105 A CN 108892105A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B11/00—Oxides or oxyacids of halogens; Salts thereof
- C01B11/02—Oxides of chlorine
- C01B11/022—Chlorine dioxide (ClO2)
- C01B11/023—Preparation from chlorites or chlorates
- C01B11/025—Preparation from chlorites or chlorates from chlorates without any other reaction reducing agent than chloride ions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
- B01D19/0036—Flash degasification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B11/00—Oxides or oxyacids of halogens; Salts thereof
- C01B11/02—Oxides of chlorine
- C01B11/022—Chlorine dioxide (ClO2)
- C01B11/028—Separation; Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/76—Treatment of water, waste water, or sewage by oxidation with halogens or compounds of halogens
- C02F1/763—Devices for the addition of such compounds in gaseous form
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/02—Odour removal or prevention of malodour
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Abstract
The invention belongs to chlorine dioxide preparation fields, specially a kind of chlorine dioxide generator and its operation method with gas-liquid separation Yu residual liquid recycling function, generator includes tetrad liquid storage tank systems, chlorine dioxide generating system, Separate System of Water-jet, raffinate recovery system and power cooling water system, and each system is sequentially communicated by pipeline to be combined into one；Raffinate recovery system includes cooling bath column, crystal splitter.Chlorine dioxide generating system extracts raw material from tetrad reservoir and prepares ClO2Liquid, ClO occurs2After generation liquid enters Separate System of Water-jet, ClO is realized2、Cl2With the separation of liquid phase, the raffinate after separation is cooled down after entering raffinate recovery system by power cooling water, and oversaturated sodium chloride byproduct, which is precipitated, in raffinate crystallizes and settle discharge, supernatant fluid reuse.The present invention uses crystallisation by cooling isolation technics, removes oversaturated sodium chloride in residul liquid-removing, reduces the equipment fault because of caused by sodium chloride Crystallization Plugging pipeline during residual liquid recycling.
Description
Technical field
It is especially a kind of the present invention relates to a kind of chlorine dioxide preparation apparatus and process in water treatment field application
Chlorine dioxide generator with gas-liquid separation and residual liquid recycling function and the method for preparing chlorine dioxide using the generator.
Background technique
Chlorine dioxide have very strong oxidability and reactivity, water treatment field be widely used in water disinfection,
Decoloration, deodorization and pre-oxidation treatment.Using sodium chlorate (or sodium chlorite) and hydrochloric acid as the chemical process CO 2 generator of raw material
Since structure is simple, convenient operation and management, operating cost are cheap, become the master of domestic water treatment field substitution liquid chlorine disinfection
It wants one of equipment and is used widely.
It is as follows as the chemical principle of the chlorine dioxide generator of raw material using sodium chlorate (or sodium chlorite) and hydrochloric acid：
Sodium chlorate method：2NaClO3+4HCl→2ClO2+Cl2+2NaCl+2H2O (1)
Sodium chlorite method：5NaClO2+4HCl→4ClO2+5NaCl+2H2O (2)
From reaction equation (1) and (2) as can be seen that removing effective disinfection composition ClO in theoretical product2、Cl2Outside, only by-product
Object NaCl is harmless, therefore such chlorine dioxide generator mostly uses the gas-liquid containing chlorine dioxide for generating reaction in the market
Mixture is that liquid (that is, reaction solution) occurs to be added to the technique in water together, this is complete, residual without raw material based on reaction progress
The result that just achievable generation liquid pollution-free uses under the premise of staying.In fact, due to by generator process conditions and efficiency
Limitation, occur in liquid inevitably containing the substances such as a certain amount of unreacted sodium chlorate (sodium chlorite) and hydrochloric acid, these
Substance enters in water together with reaction solution, easily causes chlorate in drinking water, chlorite exceeded and the acidification of water, leads to water
The secondary pollution of body.Especially reaction temperature is too low, charge proportion imbalance, material solution concentration prepare the conditions such as unreasonable
It is arranged in the case that improper and chlorine dioxide dosage is big, it is easier to cause the appearance of the above problem.With sodium chlorate method dioxy
For changing chlorine generator, technique requires hydrochloric acid dosage generally 1~2 times more excessive than theoretical value, occurs in liquid necessarily containing a large amount of
Remaining hydrochloric acid, if being direct plungeed into water, influence to water body pH as one can imagine.
As it can be seen that liquid, which occurs, to chlorine dioxide carries out gas-liquid separation, pure disinfection composition is only exported, is to guarantee water process effect
A kind of effective way of fruit or drinking water disinfection wholesomeness.On the other hand, if hydrochloric acid, sodium chlorate will be contained after gas-liquid separation
The raffinate of (or sodium chlorite) directly presses liquid waste processing discharge, not only will increase processing cost, also will cause the wasting of resources, simultaneously
It may also cause secondary pollution.Therefore generator raffinate is properly disposed, chlorine is only discharged in reuse useful raw material therein
Change sodium by-product, has to the minimizing discharge of process of preparing chlorine dioxide waste, reduction production cost and protection use environment
There is important meaning.
Currently, occurring the gas-liquid separation device much based on negative pressure aeration principle in the market, have be independently arranged (reference can be made to
CN202415153U), also there is (reference can be made to CN201857295U) with generator one.The generally existing aerator of these products
Design the defect that too simple, aeration quantity does not monitor, cause gas liquid interfacial area is small, gas liquid ratio is unreasonable, actual separation effect
The low problem of rate；In addition there is also match the gas-liquid separation device being independently arranged with generator.Also have individually using gas
The device (reference can be made to CN202849054U) of liquid separation and residual liquid recycling and generator one, but raffinate set by this device
Reuse unit only simply sends raffinate back to reactor, does not consider the removal of side product chlorinated sodium；Longtime running is with chlorine
It after the accumulation of change sodium reaches supersaturation, easily forms crystallization and blocks pipeline, cause generator failure, it is serious it also occur that setting
The danger of standby explosion.
Summary of the invention
To overcome existing chlorine dioxide generator and its raffinate separator above shortcomings, object of the present invention is to mention
For a kind of chlorine dioxide generator and its technique with gas-liquid separation Yu residual liquid recycling function, simultaneously with integrated process equipment
Solve the problems, such as chlorine dioxide preparation, occur liquid in effectively disinfection composition purification and its raffinate in surplus stock reuse, realize
Improve the purpose of gas-liquid separation efficiency and raffinate minimizing discharge.
Realize that the technical solution of the object of the invention is as follows：
A kind of chlorine dioxide generator with gas-liquid separation Yu residual liquid recycling function, which is characterized in that the generator packet
It includes：Tetrad liquid storage tank systems, chlorine dioxide generating system, Separate System of Water-jet, raffinate recovery system and power cooling water system
System, above system are sequentially communicated and are combined into one by pipeline；The raffinate recovery system includes cooling bath column and crystal
Splitter, crystal splitter are placed in cooling bath column, the power cooling water in cooling bath column to crystal splitter into
Row cooling；
Wherein the tetrad reservoir provides raw material and storage waste liquid, chlorine dioxide system for chlorine dioxide generating system
System extracts raw material from the tetrad reservoir and prepares ClO2Liquid, ClO occurs2After generation liquid enters Separate System of Water-jet, realize
ClO2、Cl2With the separation of liquid phase, the raffinate after separation is cooled down after entering raffinate recovery system by power cooling water, is satiated in raffinate
The sodium chloride byproduct of sum, which is precipitated, to be crystallized and settles discharge, supernatant fluid reuse.
The Separate System of Water-jet includes gas-liquid separation column, aeration plate, and the aeration plate includes being uniformly distributed tiny outlet
The ball-type top surface of the aeration plate in hole, air cavity, air inlet, aeration plate are arranged in gas-liquid separation column, to the aeration quantity of aeration plate into
It row detection and adjusts, forms the fine and closely woven bubble of the high-specific surface area of certain gas liquid ratio, gas-liquid separation efficiency is up to 99%.
The aeration plate is made of corrosion resistant polyvinyl chloride, ceramics or polytetrafluoroethylene material, the diameter of aeration plate
It is the 70%~75% of gas-liquid separation column internal diameter, outlet bore dia is 1.5mm~2mm, gas flux 2m3/ h~3m3/h。
The Separate System of Water-jet further includes that liquid inlet pipe, air inlet pipe, inlet air flow meter, intake valve, exhaust pipe, jet stream occurs
Absorber, raffinate discharge pipe, check-valves, the first crystal observation tube and the first crystal drain valve；
Wherein gas-liquid separation column is cylinder, has spherical top cover and conical funnel bottom；Aeration plate setting is in gas-liquid point
From, close to conical bottom and column part connecting portion, air inlet pipe is sequentially connected inlet air flow meter and intake valve simultaneously from top to bottom in column
The air inlet for entering cylinder and aeration plate from gas-liquid separation column top connects；Liquid inlet pipe occurs to enter from close to the top of aeration plate
The central upper portion position that the outlet of liquid inlet pipe is placed in aeration plate occurs for gas-liquid separation column；Row of the exhaust pipe from gas-liquid separation column top
Port is drawn, and the bleeding point of jet stream absorber is connected to；Residual liquid discharge port is arranged in gas-liquid separation column side far from capital 20-25cm
It sets, is connected by raffinate discharge pipe and check-valves with the inlet of raffinate recovery system；First crystal observation tube is transparent pipe,
It is connect by pipeline with the first crystal discharge outlet, the first crystal observation tube lower end is connected with the first crystal drain valve, passes through
Pipeline is connected with discharging of waste liquid pipe, and the volume of gas-liquid separation column will guarantee that liquid occurs to stop in column in the Separate System of Water-jet
Time is 6~8min.
The tetrad liquid storage tank systems include 4 salt acid storage tanks being integrally machined, sodium chlorate storage tank, reuse raffinate storage tank
And liquid waste tank；The reuse raffinate storage tank and liquid waste tank bottom process funnel in 45° angle by four pieces of plates, so as to
In the heavy collection of crystal, funnel lowermost end is equipped with outlet, is connected respectively by the first valve, the second valve with discharging of waste liquid pipe,
Sediment for being discharged in slot.
The chlorine dioxide generating system includes：Hydrochloric acid metering pump, sodium chlorate metering pump, reuse liquid metering pump, raw material are pre-
Mixed device, reactor shell and generation liquid efferent duct, the volume of reactor shell will guarantee that raw material has the reaction of 50min~60min
Residence time；
The discharge nozzle of three metering pumps is connected with the bottom feed inlet of reactor shell, and liquid efferent duct occurs from reactor enclosure
Body top exit is drawn, and is connected with the generation liquid import of Separate System of Water-jet.
The raffinate recovery system further includes reuse liquid efferent duct, the second crystal observation tube, the second crystal drain valve
And discharging of waste liquid pipe；
The cooling bath column bottom and top are equipped with power cooling water outlet and inlet, respectively with the of power cooling water system
One water-supply-pipe and the second water-supply-pipe are connected, and the raffinate discharge pipe of the gas-liquid separation column introduces at the top of crystal splitter, insert
1/2 depth under liquid level in column, the top surface of crystal splitter are lower than the residual liquid discharge port at least 20cm of gas-liquid separation column；Away from knot
The brilliant object splitter capital position 10-15cm sets the outlet of reuse liquid, accesses reuse raffinate storage tank by reuse liquid efferent duct；Crystal
Splitter has a conical funnel bottom, the second crystal discharge outlet through pipeline successively with the second transparent crystal observation tube, the
Two crystal drain valves are connected with discharging of waste liquid pipe, access liquid waste tank through discharging of waste liquid pipe；It is tied in the raffinate recovery system
Brilliant object splitter is made of titanium alloy material, and the second crystal observation tube selects transparent glass tube or pvc pipe preparation.
The power cooling water system includes pressure sensor, booster pump, check-valves, the second water-supply-pipe and the first water delivery
Pipe；
Wherein, the water inlet pipe of power cooling water system is equipped with pressure sensor, and two-way, every road pipe are divided after pressure sensor
Road respectively fills a check-valves, wherein all the way the front end of pipe line check valve be equipped with booster pump；Two-way pipeline converges after check-valves
Together, it is connected through the first water-supply-pipe with the water inlet of the cooling bath column bottom of raffinate recovery system, cooling bath column top goes out
The second water-supply-pipe of the mouth of a river is connected with the power water inlet of jet stream absorber.
A method of chlorine dioxide is prepared using above-mentioned chlorine dioxide generator, which is characterized in that
Chlorine dioxide generating system extracts raw material from tetrad liquid storage tank systems by setting ratio by metering pump, by original
Material premixed device enters reactor shell after mixing, and raw material reacts in reactor shell, and generates the gas-liquid of chlorine dioxide
Liquid occurs for mixture, and liquid occurs and flows into Separate System of Water-jet through pipeline under the flow dynamic driving that metering pump provides；
The jet stream absorber of Separate System of Water-jet generates negative pressure, gas-liquid of the negative pressure through being attached thereto under the action of power water
Exhaust pipe at the top of splitter is passed in gas-liquid separation column, the negative pressure state in gas-liquid separation column force external air according to
It is secondary to be entered in column through air inlet pipe, flowmeter, intake valve and aeration plate；Into the generation liquid in column under the residence time of setting
After the completion of aeration separation, liquid level reaches residual liquid discharge port, passes through raffinate discharge pipe and check-valves under the effect of gravity
Flow into raffinate recovery system；On the other hand, newly generated sodium chloride in liquid occurs to be superimposed with the amount that reuse raffinate is brought into, through air
Cooling crystallization is precipitated in hypersaturated state, in the heavy collection in the conical funnel bottom of gas-liquid separation column, and pass through the first crystal
Discharge outlet enters the first crystal observation tube, is controlled, is emitted into liquid waste tank using the first crystal drain valve；
The crystal splitter of raffinate recovery system is immersed in cooling bath, and the raffinate after gas-liquid separation is separated in crystal
The natural temperature of water is cooled in column, wherein crystallization can be precipitated in the sodium chloride in hypersaturated state, through one timing of standing sedimentation
Between can sink collection in the conical funnel bottom of crystal splitter, and enter the second crystal observation tube, utilize the second crystal
Drain valve control, is emitted into liquid waste tank；The reuse liquid efferent duct of the crystallized object splitter of supernatant after crystal precipitating
From flowing in reuse raffinate storage tank；
Power cooling water system provides cooling water and power water simultaneously for raffinate recovery system and jet stream absorber, and power is cold
But water makees the cooling media of raffinate with the cooling bath column that the pressure set initially enters raffinate recovery system, then from cooling water
Bath column flows out into jet stream absorber and is used as power water, and pressure sensor provisioned in system, booster pump guarantee power cooling water
Pressure meets cooling and driving jet stream absorber and works normally.
In the chlorine dioxide generating system inlet amount of reuse raffinate be hydrochloric acid, sodium chlorate total feed 10%~
30%；
When working in the Separate System of Water-jet, the ratio between charge flow rate and generation flow quantity are 60~70 ﹕ 1；
Residence time of the raffinate in crystal splitter is 10min~15min in the raffinate recovery system；
The pressure of power cooling water is 0.30MPa~0.40MPa in the power cooling water system.
The sodium chlorate can be substituted using sodium chlorite.
Compared with prior art, the present invention its remarkable advantage：
(1) raffinate recovery process of the present invention uses crystallisation by cooling isolation technics, goes to the supersaturated part in part in residul liquid-removing
Sodium chloride byproduct reduces the probability that residual liquid recycling process causes equipment fault because of sodium chloride Crystallization Plugging pipeline；Simultaneously
Due to recycling the hydrochloric acid in raffinate, sodium chlorate (or sodium chlorite), the overall cost that chlorine dioxide can be made to prepare compares raffinate
In line method reduces by 20%~30%.
(2) since most of hydrochloric acid, the sodium chlorate (or sodium chlorite) in raffinate obtain reuse, system is finally discharged useless
To crystallize based on sodium chloride, this is provided conveniently liquid for the sodium chloride that is further processed and recycles of waste liquid, therefore can both be greatlyd save
Raw material resources can also reduce treatment cost of waste liquor and the secondary pollution to environment.
(3) Separate System of Water-jet of the invention is equipped with inlet air flow meter and intake valve, since use can monitor and adjust exposure
The disc type of tolerance is aerated isolation technics, is aerated, is improved convenient for obtaining the fine and closely woven bubble of best gas liquid ratio and high-specific surface area
Gas liquid interfacial area and exchange efficiency are, it can be achieved that ClO2Quick stripping, gas-liquid separation efficiency is up to 99%.
(4) present invention passes through the diameter of stomata in the diameter and aeration plate of design aeration plate, further
The fine and closely woven bubble for obtaining the high-specific surface area to match with system, to further improve gas liquid interfacial area；The present invention
Aeration plate is made by using hard materials such as corrosion resistant polyvinyl chloride, ceramics or polytetrafluoroethylene (PTFE), can achieve aeration plate
It is not easy the purpose blocked.
(5) present invention is by being processed into leakage in 45° angle by four pieces of plates for reuse raffinate storage tank and liquid waste tank bottom
It is bucket-shaped, collect convenient for further sinking for crystal in reuse liquid and waste liquid.
(6) for the present invention by the way that the material of Crystallization Separation column is set as titanium alloy, can achieve prevents hydrochloric acid, chlorine dioxide rotten
The purpose of erosion facilitates Crystallization Separation column and is realized well by power cooling water because titanium alloy has good heat conductivity
Cooling.
(7) present invention using integrated system and component solve chlorine dioxide preparation, effective disinfection composition purification,
The technical issues of reuse of surplus stock and process of preparing chlorine dioxide raffinate minimizing are discharged in raffinate, realizes chlorine dioxide system
The integrated cleaning production process of standby, gas-liquid separation and residual liquid recycling.
In conclusion implementation of the invention by disinfection by chlorine dioxide equipment running process energy-saving and emission-reduction, reduce cost
There is significant positive effect with the water quality safety for guaranteeing pending water.
Detailed description of the invention
Chlorine dioxide generator schematic diagram of Fig. 1 present invention with gas-liquid separation Yu residual liquid recycling function.
Fig. 2 aeration plate structural schematic diagram of the present invention, (a) are main view, (b) are top view.
Mark representative meaning as follows in figure：
1- hydrochloric acid metering pump, 2- sodium chlorate metering pump, 3- reuse liquid metering pump, 4- raw material premix device, 5- reactor feed
Mouthful, 6- heating mantle, the first temperature sensor of 7-, 8- second temperature sensor, 9- reactor shell, 10- generation liquid efferent duct,
Liquid inlet pipe, 14- aeration plate, 15- the first crystal discharge outlet, the first knot of 16- occur for 11- exhaust pipe, 12- gas-liquid separation column, 13-
Brilliant object observation tube, 17- the first crystal drain valve, 18- air inlet pipe, 19- flowmeter, 20- intake valve, 21- raffinate discharge pipe,
22- jet stream absorber, the second water-supply-pipe of 23-, 24- check-valves, 25- reuse liquid efferent duct, 26- cooling bath column, 27- crystal
Splitter, 28- the second crystal discharge outlet, 29- the second crystal observation tube, 30- the second crystal drain valve, 31- waste liquid row
Put pipe, the first water-supply-pipe of 32-, 33- check-valves, 34- pressure sensor, 35- check-valves, 36- booster pump, 37- salt acid storage tank,
38- sodium chlorate storage tank, 39- reuse raffinate storage tank, 40- liquid waste tank, 41- the first discharging of waste liquid valve, the second discharging of waste liquid of 42-
Valve, 43- discharging of waste liquid pipe, 1401 ball-type top surfaces, 1402- air cavity, 1403- air inlet.
Specific embodiment
The structure and working method for proposing system according to the present invention are described in detail below with reference to Fig. 1.
(1) structure and composition of system
Chlorine dioxide generator of the present invention with gas-liquid separation Yu residual liquid recycling function, including tetrad reservoir system
System, chlorine dioxide generating system, Separate System of Water-jet, raffinate recovery system and power cooling water system, each section by pipeline according to
It is secondary to connect and compose an assembly.
The tetrad liquid storage tank systems include 4 the salt acid storage tanks 37 being integrally machined, sodium chlorate storage tank 38, reuse raffinates
Storage tank 39 and liquid waste tank 40.Wherein, reuse raffinate storage tank 39 and 40 bottom of liquid waste tank are processed by four pieces of plates in 45° angle
Funnel, in order to the heavy collection of crystal, funnel lowermost end is equipped with outlet, respectively by the first discharging of waste liquid valve 41, second
Discharging of waste liquid valve 42 is connected with discharging of waste liquid pipe 43, the sediment for being discharged in slot.
The chlorine dioxide generating system include hydrochloric acid metering pump 1, sodium chlorate metering pump 2, reuse raffinate metering pump 3,
Raw material premix device 4, reactor shell 9, heating mantle 6, the first temperature sensor 7, second temperature sensor 8 and generation liquid efferent duct
10.Wherein：Reactor shell 9 is cylinder, up and down band spherical surface end cap, in order to the dispersion of feed liquid and the discharge of generation liquid；Salt
Acid, sodium chlorate and reuse raffinate metering pump feed pipe respectively with salt acid storage tank 37, sodium chlorate storage tank 38, reuse raffinate storage tank 39
Connection；Its discharge nozzle is connected by raw material premix device 4 with reactor feed mouth 5；Heating mantle 6 is coated on the outer of reactor shell 9
Portion provides thermal energy for reactor；First temperature sensor 7 and second temperature sensor 8 are mounted on the side wall of reactor, are in
Upper and lower distribution, for monitoring two-part temperature above and below in reactor；Liquid efferent duct 10 occurs from reactor shell top exit
It draws, is connected with the generation liquid import of Separate System of Water-jet.The chlorine dioxide generating system, reactor shell 9 should adopt
The alloy material preparation corroded with acidproof, resistance to oxidation, it is preferred to use titanium alloy material；The volume of reactor should ensure that raw material has
The reaction time of 50min~60min；0 DEG C~100 DEG C of the temperature-measuring range of temperature sensor, using titanium alloy casing, to increase
Add rotproofness and thermal conductivity.
The Separate System of Water-jet include gas-liquid separation column 12, aeration plate 14, air inlet pipe 18, inlet air flow meter 19, into
Air valve 20, exhaust pipe 11, jet stream absorber 22, raffinate discharge pipe 21, check-valves 24, the first crystal observation tube 16 and first are useless
Liquid drain valve 17.Wherein：Gas-liquid separation column 12 have spherical top cover and conical funnel bottom, in favor of top gas discharge and
The heavy collection of bottom crystal object；The ball-type top surface 1401 of aeration plate 14 including equally distributed tiny venthole, air cavity 1402 and
Air inlet 1403, aeration plate 14 are arranged in gas-liquid separation column 12 close to conical bottom and cylinder connecting portion, and air inlet pipe 18 is from upper
Inlet air flow meter 19 and intake valve 20 are sequentially connected under and enter at the top of gas-liquid separation column 12 cylinder and aeration plate 14 into
Port 1403 connects；Liquid inlet pipe 13 occurs and enters cylinder from the top close to aeration plate 14, outlet is placed in the upper of aeration plate 14
Portion center accelerates dispersion and ClO that liquid occurs by the aeration effect of aeration plate2Stripping；Exhaust pipe 11 divides from gas-liquid
Exhaust outlet from the top of column 12 is drawn, and the bleeding point of jet stream absorber 22 is connected to, for by the swabbing action of jet stream absorber 22
The negative pressure of generation is transmitted in gas-liquid separation column, while chlorine dioxide is isolated in discharge；Residual liquid discharge port is arranged in gas-liquid
Splitter side passes through the inlet of raffinate discharge pipe 21 and check-valves 24 and raffinate recovery system far from the capital position 20-25cm
It is connected, raffinate liquid level reaches the position, gravity Self-discharged can be leaned on by raffinate discharge pipe 21, ullage space is ease in column
The buffer area that gas out reserves；First crystal observation tube 16 is transparent pipe, passes through pipeline and the first of splitter conical bottom
Crystal discharge outlet 15 connects, and lower end is connected with the first crystal drain valve 17, is connected by pipeline with discharging of waste liquid pipe 31.Institute
The Separate System of Water-jet stated, the volume of gas-liquid separation column 12 should ensure that liquid residence time in column, which occurs, is no less than 5min, excellent
It is selected as 6~8min；Aeration plate 14 can be used corrosion resistant PVC (polyvinyl chloride), ceramics or polytetrafluoroethylene material and be made, preferably
Polytetrafluoroethylene material；The diameter of aeration plate 14 be 12 internal diameter of gas-liquid separation column 70%~75%, hole diameter be 1.5mm~
2mm, gas flux 2m3/ h~3m3/h。
The raffinate recovery system includes cooling bath column 26, crystal splitter 27, reuse liquid efferent duct 25, second
Crystal observation tube 29, the second crystal drain valve 30 and discharging of waste liquid pipe 31.Wherein：26 bottom and top of cooling bath column are set
Dynamic cooling water outlet and inlet is connected with the first water-supply-pipe 32 of power cooling water and the second water-supply-pipe 23 respectively；Crystal point
It is placed in cooling bath column 26 from column 27, the raffinate discharge pipe 21 from gas-liquid separation column 12 is at the top of crystal splitter 27
It introduces, is inserted in column 1/2 depth under liquid level, the top surface of crystal splitter 27 is lower than the residual liquid discharge port of gas-liquid separation column 12 extremely
Few 20cm, so that raffinate can lean on self gravity voluntarily to flow into；Reuse liquid is set away from the 27 capital position 10-15cm of crystal splitter to go out
Mouthful, reuse raffinate storage tank is accessed by reuse liquid efferent duct 25, for exporting reuse raffinate；Crystal splitter 27 has circular cone
Shape hopper base, the second crystal discharge outlet 28 through pipeline successively with the second transparent crystal observation tube 29, the second crystal
Drain valve 30 is connected with discharging of waste liquid pipe 31, accesses liquid waste tank 40 through discharging of waste liquid pipe 31.The raffinate recovery system,
Crystal splitter 27 selects acidproof, resistance to oxidation corrosion thermally conductive good alloy material preparation, preferably titanium alloy material；Second knot
Brilliant object observation tube 29 selects transparent acidproof, resistance to oxidation corrosion glass tube or pvc pipe preparation, preferably clear pvc pipe.
The power cooling water system includes pressure sensor 34, booster pump 36, check-valves 33,35 and the first water-supply-pipe
32 and second water-supply-pipe 23.Wherein：The water inlet pipe of power cooling water is equipped with pressure sensor 34, and two are divided to after pressure sensor
Road, every road pipeline fill check-valves 33,35, with the refluence after preventing water from entering system, pipe line check valve all the way wherein
35 front end is equipped with booster pump 36, pressurization when for source water hydraulic pressure deficiency；Two-way pipeline converges one after check-valves 33,35
It rises, is connected through the first water-supply-pipe 32 with the water inlet of 26 bottom of raffinate recovery system cooling bath column, 26 top of cooling bath column
Water outlet is connected through the second water-supply-pipe 23 with the power water inlet of jet stream absorber 22.The power cooling water system, mentions
The power cooling water pressure of confession is no less than 0.25MPa, preferably 0.30MPa~0.40MPa.
(2) working method of system
A kind of chlorine dioxide generator with gas-liquid separation Yu residual liquid recycling function of the present invention, by tetrad reservoir
System, chlorine dioxide generating system, Separate System of Water-jet, raffinate recovery system and power cooling water system composition, each section by
Liquid-transport pipe-line is sequentially communicated to form an assembly, it can be achieved that the preparation from chlorine dioxide and excess by-product in purification, raffinate
Crystallization Separation and the continuous circular flow of processes such as surplus stock reuse.
Tetrad liquid storage tank systems include 4 storage tanks for holding hydrochloric acid, sodium chlorate, reuse raffinate and waste liquid, are chlorine dioxide
Generating system provides raw material and storage waste liquid.
Chlorine dioxide generating system by metering pump 1,2,3 by setting ratio extracted from tetrad liquid storage tank systems hydrochloric acid,
Sodium chlorate and reuse raffinate enter reactor shell 9 by being attached thereto raw material premix device 4 as raw material after mixing；It is former
The material heated heating of set 6 and the first temperature sensor 7, monitoring of second temperature sensor 8 in reactor shell 9 is achieved
It is reacted under set temperature, and liquid occurs for the gas-liquid mixture for generating chlorine dioxide；The liquid that liquid is provided in metering pump occurs
Separate System of Water-jet is flowed into through pipeline under flowing power drive.The chlorine dioxide generating system, the inlet amount of reuse raffinate
For hydrochloric acid, sodium chlorate total feed 10%~30%, can be according to hydrochloric acid remaining in chlorine dioxide occurrence quantity and reuse liquid and chlorine
The concentration of sour sodium is adjusted.
The negative pressure that the jet stream absorber 22 of Separate System of Water-jet generates under the action of power water, the negative pressure is through being attached thereto
The exhaust pipe 11 of gas-liquid separation column top be passed in gas-liquid separation column 12, the negative pressure state in gas-liquid separation column 12 forces
External air successively enters in column through air inlet pipe 18, flowmeter 19, intake valve 20 and aeration plate 14；19 He of inlet air flow meter
Intake valve 20 can indicate and adjust the flow into air in gas-liquid separation column 12, to obtain suitable gas liquid ratio, aeration plate
The 14 fine and closely woven bubbles that air can be made to form high-specific surface area are aerated, and to improve gas liquid interfacial area, are realized to ClO2's
Quick stripping；After the completion of being aerated separation under the residence time of setting into the generation liquid in column, liquid level reaches raffinate discharge
Mouthful, raffinate recovery system is flowed by raffinate discharge pipe 21 and check-valves 24 under the effect of gravity；Since raffinate is discharged
Pipe 21 is inserted under the liquid level of raffinate recovery system, under the double action of check-valves and liquid level difference, it is ensured that raffinate will not be fallen
It inhales；On the other hand, newly generated sodium chloride in liquid occurs to be superimposed with the amount that reuse raffinate is brought into, the cooling through air is most probably in
Hypersaturated state and crystallization is precipitated, enter the first crystallization in the heavy collection in the conical funnel bottom of gas-liquid separation column, and by outlet
Object observation tube, controls using valve, is emitted into liquid waste tank.The Separate System of Water-jet, operating condition are：Inlet air flow
Amount is 60~70 ﹕ 1 with the ratio between flow quantity occurs.
The crystal splitter 27 of raffinate recovery system is immersed in cooling bath, and the raffinate after gas-liquid separation is in crystal point
From the natural temperature for being cooled to water in column 27, wherein crystallization can be precipitated in the sodium chloride in hypersaturated state, through standing sedimentation one
Collection can be sunk in the conical funnel bottom of crystal splitter 27 by fixing time, and enter the second crystal observation tube 29, available
Valve control, is emitted into liquid waste tank 40；2 times of sodium chloride of solubility and reaction process based on sodium chlorate are largely disappeared
The situation of consumption will not crystallize at such a temperature, thus can to the supernatant containing a large amount of hydrochloric acid and a small amount of sodium chlorate into
Row reuse；Supernatant after crystal precipitating can be flow in reuse raffinate storage tank 39 certainly through the reuse liquid efferent duct of splitter.Institute
The raffinate recovery system stated, residence time of the raffinate in crystal splitter 27 are 10min~15min.
Power cooling water system is that raffinate recovery system and jet stream absorber 22 provide cooling water and power water simultaneously.Power
Cooling water initially enters the cooling bath column 26 of raffinate recovery system as the cooling media of raffinate using the pressure set, then from
Cooling bath column 26 flows out, and enters jet stream absorber 22 as power water, and the power cooling water flowed out from jet stream absorber 22 is also
It is absorption and the pumped (conveying) medium for being purified chlorine dioxide.Pressure sensor 34, booster pump 36 provisioned in system can guarantee power
Cooling water pressure meets the needs that cooling and driving jet stream absorber 22 works normally, and when hydraulic pressure deficiency, system can be according to pressure
The data that force snesor 34 measures are opened booster pump 36 by controller and are pressurized.The power cooling water system, power
The pressure of cooling water is not lower than 0.25MPa, preferably 0.30MPa~0.40MPa.Above-mentioned side can be replaced using sodium chlorite
Sodium chlorate in method.
Claims (10)
1. a kind of chlorine dioxide generator with gas-liquid separation Yu residual liquid recycling function, which is characterized in that the generator includes：
Tetrad liquid storage tank systems, chlorine dioxide generating system, Separate System of Water-jet, raffinate recovery system and power cooling water system,
Above system is sequentially communicated and is combined into one by pipeline；The raffinate recovery system includes cooling bath column (26) and crystal
Splitter (27), crystal splitter (27) are placed in cooling bath column (26), the power cooling water in cooling bath column (26)
Crystal splitter (27) is cooled down；
Wherein the tetrad reservoir for chlorine dioxide generating system provide raw material and storage waste liquid, chlorine dioxide generating system from
The tetrad reservoir extracts raw material and prepares ClO2Liquid, ClO occurs2After generation liquid enters Separate System of Water-jet, ClO is realized2、Cl2
With the separation of liquid phase, the raffinate after separation is cooled down after entering raffinate recovery system by power cooling water, oversaturated chlorine in raffinate
Change sodium by-product crystallization is precipitated and settles discharge, supernatant fluid reuse.
2. chlorine dioxide generator according to claim 1, which is characterized in that the Separate System of Water-jet includes gas-liquid point
From column (12), aeration plate (14), the aeration plate (14) includes the ball-type top surface (1401) for being uniformly distributed tiny venthole, air cavity
(1402), air inlet (1403), aeration plate (14) setting carry out the aeration quantity of aeration plate (14) in gas-liquid separation column (12)
Detection and adjusting, forming gas liquid ratio is 60-70:The fine and closely woven bubble of 1 high-specific surface area, gas-liquid separation efficiency is up to 99%.
3. chlorine dioxide generator according to claim 2, which is characterized in that the aeration plate (14) is using corrosion resistant
Polyvinyl chloride, ceramics or polytetrafluoroethylene material are made, and the diameter of aeration plate (14) is the 70% of gas-liquid separation column (12) internal diameter
~75%, outlet bore dia is 1.5mm~2mm, gas flux 2m3/ h~3m3/h。
4. chlorine dioxide generator according to claim 3, which is characterized in that the Separate System of Water-jet further includes occurring
It is liquid inlet pipe (13), air inlet pipe (18), inlet air flow meter (19), intake valve (20), exhaust pipe (11), jet stream absorber (22), residual
Liquid discharge pipe (21), check-valves (24), the first crystal observation tube (16) and the first crystal drain valve (17)；
Wherein gas-liquid separation column (12) is cylinder, has spherical top cover and conical funnel bottom；Aeration plate (14) is arranged in gas
Close to conical bottom and column part connecting portion in liquid splitter (12), air inlet pipe (18) is sequentially connected charge flow rate from top to bottom
Meter (19) and intake valve (20) are simultaneously connect into cylinder with the air inlet of aeration plate (14) at the top of gas-liquid separation column (12)；Occur
Liquid inlet pipe (13) enters gas-liquid separation column (12) from the top close to aeration plate (14), and liquid inlet pipe (13) outlet occurs and is placed in aeration
The central upper portion position of disk (14)；Exhaust pipe (11) is drawn from the exhaust outlet at the top of gas-liquid separation column (12), is connected to jet stream absorption
The bleeding point of device (22)；Residual liquid discharge port is arranged in gas-liquid separation column (12) side far from the capital position 20-25cm, is arranged by raffinate
Outlet pipe (21) and check-valves (24) are connected with the inlet of raffinate recovery system；First crystal observation tube (16) is transparent pipe,
It is connect by pipeline with the first crystal discharge outlet (15), first crystal observation tube (16) lower end is connected with the discharge of the first crystal
Valve (17) is connected by pipeline with discharging of waste liquid pipe (31), and the volume of gas-liquid separation column (12) is wanted in the Separate System of Water-jet
Guarantee that it is 6~8min that liquid residence time in column, which occurs,.
5. chlorine dioxide generator according to claim 4, which is characterized in that the tetrad liquid storage tank systems include 4
A salt acid storage tank (37) being integrally machined, sodium chlorate storage tank (38), reuse raffinate storage tank (39) and liquid waste tank (40)；Described time
Funnel is processed in 45° angle by four pieces of plates with raffinate storage tank (39) and liquid waste tank (40) bottom, in order to crystal
Heavy collection, funnel lowermost end is equipped with outlet, passes through the first valve (41), the second valve (42) and discharging of waste liquid pipe (43) phase respectively
Even, the sediment for being discharged in slot.
6. chlorine dioxide generator according to claim 5, which is characterized in that the chlorine dioxide generating system includes：
Hydrochloric acid metering pump (1), sodium chlorate metering pump (2), reuse liquid metering pump (3), raw material premix device (4), reactor shell (9) and hair
Raw liquid efferent duct (10), the volume of reactor shell (9) will guarantee that raw material has the reaction time of 50min~60min；
The discharge nozzle of three metering pumps is connected with the bottom feed inlet of reactor shell (9), and liquid efferent duct (10) occur from reaction
Device shell (9) top exit is drawn, and is connected with the generation liquid import of Separate System of Water-jet.
7. chlorine dioxide generator according to claim 6, which is characterized in that the raffinate recovery system further includes reuse
Liquid efferent duct (25), the second crystal observation tube (29), the second crystal drain valve (30) and discharging of waste liquid pipe (31)；
Cooling bath column (26) bottom and top are equipped with power cooling water outlet and inlet, respectively with the of power cooling water system
One water-supply-pipe (32) is connected with the second water-supply-pipe (23), and the raffinate discharge pipe (21) of the gas-liquid separation column is from crystal splitter
(27) top introduces, and is inserted in column 1/2 depth under liquid level, the top surface of crystal splitter (27) is lower than gas-liquid separation column (12)
Residual liquid discharge port at least 20cm；The outlet of reuse liquid is set away from crystal splitter (27) capital position 10-15cm, it is defeated by reuse liquid
Outlet pipe (25) accesses reuse raffinate storage tank (39)；Crystal splitter (27) has conical funnel bottom, the discharge of the second crystal
Mouthful (28) through pipeline successively with the second transparent crystal observation tube (29), the second crystal drain valve (30) and discharging of waste liquid pipe
(31) it is connected, accesses liquid waste tank (40) through discharging of waste liquid pipe (31)；Crystal splitter (27) in the raffinate recovery system
It is made of titanium alloy material, the second crystal observation tube (29) selects transparent glass tube or pvc pipe preparation.
8. chlorine dioxide generator according to claim 7, which is characterized in that the power cooling water system includes pressure
Force snesor (34), booster pump (36), check-valves (33,35), the second water-supply-pipe (23) and the first water-supply-pipe (32)；
Wherein, the water inlet pipe of power cooling water system is equipped with pressure sensor (34), divides two-way after pressure sensor (34), often
Road pipeline respectively fills a check-valves (33,35), wherein all the way the front end of pipe line check valve be equipped with booster pump (36)；Two-way pipeline
Converge after check-valves (33,35) together, cooling bath column (26) bottom through the first water-supply-pipe (32) Yu raffinate recovery system
Water inlet be connected, power water of cooling bath column (26) top delivery port through the second water-supply-pipe (23) Yu jet stream absorber (22)
Import is connected.
9. a kind of method for preparing chlorine dioxide using the described in any item chlorine dioxide generators of claim 1-8, feature
It is,
Chlorine dioxide generating system extracts raw material from tetrad liquid storage tank systems by setting ratio by metering pump, pre- by raw material
Mixed device (4) enter reactor shell (9) after mixing, raw material reaction in reactor shell (9), and generate chlorine dioxide
Liquid occurs for gas-liquid mixture, and liquid occurs and flows into Separate System of Water-jet through pipeline under the flow dynamic driving that metering pump provides；
The jet stream absorber (22) of Separate System of Water-jet generates negative pressure, gas-liquid of the negative pressure through being attached thereto under the action of power water
Exhaust pipe (11) at the top of splitter (12) is passed in gas-liquid separation column (12), the negative pressure state in gas-liquid separation column (12)
External air is forced successively to enter in column through air inlet pipe (18), flowmeter (19), intake valve (20) and aeration plate (14)；Into
Enter the generation liquid in column be aerated under the residence time of setting separation after the completion of, liquid level reach residual liquid discharge port, itself weight
Raffinate recovery system is flowed by raffinate discharge pipe (21) and check-valves (24) under the action of power；On the other hand, occur new in liquid
The sodium chloride of generation is superimposed with the amount that reuse raffinate is brought into, and crystallization is precipitated in hypersaturated state in the cooling through air, in gas-liquid
The heavy collection in the conical funnel bottom of splitter (12), and the first crystal observation tube is entered by the first crystal discharge outlet (15)
(16), it is controlled, is emitted into liquid waste tank (40) using the first crystal drain valve (17)；
The crystal splitter (27) of raffinate recovery system is immersed in cooling bath, and the raffinate after gas-liquid separation is separated in crystal
The natural temperature of water is cooled in column (27), wherein crystallization can be precipitated in the sodium chloride in hypersaturated state, through standing sedimentation one
Collection can be sunk in the conical funnel bottom of crystal splitter (27) by fixing time, and enter the second crystal observation tube (29), benefit
It is controlled, is emitted into liquid waste tank (40) with the second crystal drain valve (30)；The crystallized object of supernatant after crystal precipitating
The reuse liquid efferent duct (25) of splitter (27) is flow to certainly in reuse raffinate storage tank；
Power cooling water system provides cooling water and power water, power cooling water simultaneously for raffinate recovery system and jet stream absorber
The cooling media for making raffinate with the cooling bath column (26) that the pressure of setting initially enters raffinate recovery system, then from cooling water
Bath column (26) flows out into jet stream absorber (22) and is used as power water, pressure sensor provisioned in system (34), booster pump
(36) guarantee that power cooling water pressure meets cooling and driving jet stream absorber (22) and works normally.
10. according to the method described in claim 9, it is characterized in that, in the chlorine dioxide generating system reuse raffinate into
Doses be hydrochloric acid, sodium chlorate total feed 10%~30%；
Residence time of the raffinate in crystal splitter (27) is 10min~15min in the raffinate recovery system；
The pressure of power cooling water is 0.30MPa~0.40MPa in the power cooling water system.
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| CN201811000650.0A CN108892105B (en) | 2018-08-30 | 2018-08-30 | Chlorine dioxide generator with gas-liquid separation and residual liquid recycling functions and operation method thereof |
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|---|---|---|---|---|
| US4045542A (en) * | 1974-12-13 | 1977-08-30 | Hooker Chemicals & Plastics Corporation | Production of chlorine dioxide |
| CN201777880U (en) * | 2010-07-14 | 2011-03-30 | 章艺 | Composite chlorine dioxide continuous production equipment |
| CN102502507A (en) * | 2011-11-04 | 2012-06-20 | 成都齐力水处理科技有限公司 | Preparation device and technology for chlorine dioxide |
| CN202849054U (en) * | 2012-05-22 | 2013-04-03 | 雷宁 | Residual liquid composite reaction chlorine dioxide generator |
| CN207608322U (en) * | 2017-11-29 | 2018-07-13 | 济南科琳宝环境科技有限公司 | A kind of chlorine dioxide with high purity gas producing equipment |
| CN208995136U (en) * | 2018-08-30 | 2019-06-18 | 南京理工大学 | A kind of chlorine dioxide generator with gas-liquid separation Yu residual liquid recycling function |
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2018
- 2018-08-30 CN CN201811000650.0A patent/CN108892105B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4045542A (en) * | 1974-12-13 | 1977-08-30 | Hooker Chemicals & Plastics Corporation | Production of chlorine dioxide |
| CN201777880U (en) * | 2010-07-14 | 2011-03-30 | 章艺 | Composite chlorine dioxide continuous production equipment |
| CN102502507A (en) * | 2011-11-04 | 2012-06-20 | 成都齐力水处理科技有限公司 | Preparation device and technology for chlorine dioxide |
| CN202849054U (en) * | 2012-05-22 | 2013-04-03 | 雷宁 | Residual liquid composite reaction chlorine dioxide generator |
| CN207608322U (en) * | 2017-11-29 | 2018-07-13 | 济南科琳宝环境科技有限公司 | A kind of chlorine dioxide with high purity gas producing equipment |
| CN208995136U (en) * | 2018-08-30 | 2019-06-18 | 南京理工大学 | A kind of chlorine dioxide generator with gas-liquid separation Yu residual liquid recycling function |
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| Publication number | Publication date |
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