CN108726615A - A kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment technique and device - Google Patents
A kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment technique and device Download PDFInfo
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- CN108726615A CN108726615A CN201810863356.6A CN201810863356A CN108726615A CN 108726615 A CN108726615 A CN 108726615A CN 201810863356 A CN201810863356 A CN 201810863356A CN 108726615 A CN108726615 A CN 108726615A
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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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
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Abstract
The invention discloses a kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment technique and devices, belong to hydrochloric acid pickling waste liquor process field.A kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment technique and device of the present invention, utilize triple effect negative pressure evaporation, evaporating temperature is low, it can ensure continuous and stable production, reduce construction investment simultaneously, and triple effect negative pressure evaporation uses forced circulation, prevents the possibility that material crystallized in evaporator and blocked evaporator, it is ensured that the stable operation of device;Concentration of hydrochloric acid is improved by flash evaporation technology to the full extent after triple effect negative pressure evaporation, and effectively waste heat is utilized to reduce operating cost, the content of the concentration and concentrate frerrous chloride of hydrochloric acid is improved simultaneously, whole system takes full advantage of wet, latent heat, raw steam consumption has been saved, operating cost is reduced.
Description
Technical field
The present invention relates to a kind of hydrochloric acid pickling waste liquor treatment technology, more specifically to a kind of hydrochloric acid pickling waste liquor three
Imitate negative pressure counter flow flash crystallization treatment technique and device.
Background technology
Currently, annual 200000000 tons of the industrial waste acid in China generates, wherein having nearly 40% by simple neutralisation treatment, cause big
It measures the high-quality sour wasting of resources and active principle is lost in, solid dangerous waste --- the sludge that neutralisation generates, recycling rate of waterused is not
Foot 4%, thus generation environment protection pressure and risk can not be estimated.Effective waste acid resource treatment process is not advised greatly
The popularization of mould causes the puzzlement that spent acid generates enterprise more, and awkward situation is self-evident at present.Nearly 2 years, China's spent acid synthesis profit
It is increased with disposing capacity, but it can be allowed to be converted into innoxious regenerated resources, need functional government departments, state
Standard formulation department of family, the support of national relevant policies, perfect and raising.China's waste acid resource Land use systems are extensive, comprehensive profit
It is less than advanced international standard with rate, waste of resource also pollutes environment simultaneously, and it is imperative that reinforcement recycles, it is necessary to pass through policy
Adjustment, improves Top-layer Design Method.Strengthen macro adjustments and controls, take the behaves such as laws and regulations, establishes permanent mechanism, polishing short slab, really
It allows waste acid resource to handle and legal fair and sensible is only current most effective most permanent measure.
Chlorohydric acid pickling process refers to that pending metal objects are soaked in the acid solution of certain temperature or are sprayed on its surface
The acid solution of certain temperature, the method to remove surface oxide layer.Chlorohydric acid pickling process is widely used in Steel Wire Products Industry and electricity
Industry is plated, is metal surface cleaning, improves one of important procedure of steel surface structure.The hydrochloric acid acid that Steel Wire Products Industry generates
Washing waste liquid all has the characteristics that concentration of metal ions is high, acid concentration is high, corrosivity is high, environmental pollution is big, each at present
State is managed as hazardous waste.The U.S. is included in《Protection of resources and regeneration bill》, it is also included in by China《Country's danger
Dangerous waste register》.Main harm is shown as caused by the illegal outer row of hydrochloric acid pickling waste liquor:Corrode sewer pipe and armored concrete
Etc. water conservancies structures;Keep crops withered, influences aquatic crops growth;Hydrochloric acid pickling waste liquor penetrates into soil, and the time, which has been grown, to cause
Soil property calcification destroys soil layer loose condition (of surface), and then influences crop growth;People and animals drink the water by this pollution, can cause stomach
Inflammation is even burnt;It pollutes caused by water body, the murder by poisoning to biology, or even finally all very huge to the injury of human health
Greatly.National environmental protection laws and regulations expressly provide that hydrochloric acid pickling waste liquor does not allow direct emission, but the quantum of output of the such waste liquid in China
It is too big, effective management and control is not obtained, phenomenon is arranged steathily and remains incessant after repeated prohibition.
Both at home and abroad to there are many processing methods of hydrochloric acid pickling waste liquor, needing the specific spy according to different hydrochloric acid pickling waste liquors
Point selects suitable Treatment process in conjunction with the useless unit own situation of production.Currently used hydrochloric acid pickling waste liquor Treatment process has:
Neutralization precipitation method, one-step calcinations, evaporative crystallization method, ion-exchange-resin process, membrane separation process, extraction, chemical transformation etc..
Especially galvanizing industry is relatively broad using evaporative crystallization technique processing hydrochloric acid pickling waste liquor.China uses evaporative crystallization technique
Processing hydrochloric acid pickling waste liquor begins with application from late nineteen nineties in last century, by the investigation of galvanizing industry professional person and makes
Reflected with unit, there are the followings to ask for the discovery hydrochloric acid pickling waste liquor evaporated crystallization device that many specific investment costs are built in recent years
Topic:
(1) for investment reduction cost and so-called energy saving, it is found that the circulatory system of nearly all device does not install additional
Forced circulation pump causes evaporator (in counter flow evaporation plant;Especially 1st effective evaporator) blockage problem is very serious, and average is clear
Wash about 10 days/time of period;
(2) horizontal condenser and horizontal preheater that device uses, mounting height are not only unfavorable in 20 meters or so of high-altitude
It in checking maintenance, and is particularly easy to that stoste feed pipe is caused to block, condenser condensation effect is seriously affected, while also result in one
Partial oxidation hydrogen tail gas enters water sprays vacuum pump set water tank;Hydrogen cloride concentration reaches 600~800mg/m on high-rise platform3, surpass
Nearly 100 times of tag splice;Workshop ceiling is just all replaced after equipment is run four months;Even operative employee health of human body all cause compared with
Big harm;
(3) in order to reduce cost, the selection of the materials such as the main equipment of device, especially separator, pipeline, valve exists
Defect.The separator of device uses glass steel material;One effect high temperature workshop section pipe material uses RPP materials, coefficient of thermal expansion
It is excessively high, so being easy to cause evaporating, emitting, dripping or leaking of liquid or gas;Valve in device has been selected than more ancient glass fiber reinforced plastics valve, temperature resistance ability,
Seal spool performance is all very poor;
(4) the Crystallization Separation workshop section of device selects belt filter press, the metal salt crystal surface moisture content separated
It is excessively high, it cannot normal packed and transported;And mill floor sour water flows over, and causes equipment seriously corroded, especially because technological design
The mistake of unreasonable and device flow scheme design makes the crystallization kettle being least easily damaged originally occur showing using what is just scrapped within two months
As;
(5) point is generated to hydrogen chloride gas in whole device and emission point does not design collection port and respective handling technique,
Tail gas absorber only is used to full workshop to handle, do not account at all operating environment safety and can to operative employee
Body harm caused by energy;
(6) there is also a major safety risks during device is designed and constructed on the spot:Whole device installs total height nearly 30
Rice, is all highest building in many galvanizing manufacturing enterprises, and too lofty, external blowdown stack requires more than workshop roof,
It is even more potential dangerous.
For this purpose, according to steel part and the development need of Steel Wire Products Industry, there is an urgent need for seek a kind of evaporative crystallization processing steel
The energy-efficient comprehensive resource of product hydrochloric acid pickling waste liquor utilizes technology and device, fundamentally solves steel part or made of metal
The problem of practical hydrochloric acid pickling waste liquor generated of conduct industry is effectively treated assists relevant enterprise to realize cleanly production.
Invention content
1. technical problems to be solved by the inivention
It is an object of the invention to overcome existing hydrochloric acid pickling waste liquor evaporative crystallization treatment process, there are HCl recovery concentration
Low, the deficiencies of evaporation efficiency is low, operation cost is high, the plant maintenance period is short, it is inverse to provide a kind of hydrochloric acid pickling waste liquor triple effect negative pressure
Flash crystallization treatment process and device are flowed, technical solution using the present invention, using triple effect negative pressure evaporation, evaporating temperature is low, energy
Enough ensure continuous and stable production, while reducing construction investment, and triple effect negative pressure evaporation uses forced circulation, prevents material and is steaming
Send out the possibility that evaporator is crystallized and blocked in device, it is ensured that the stable operation of device;By flashing skill after triple effect negative pressure evaporation
Art improves concentration of hydrochloric acid to the full extent, and effectively waste heat is utilized to reduce operating cost, at the same improve hydrochloric acid concentration and
The content of concentrate frerrous chloride, whole system take full advantage of wet, latent heat, have saved raw steam consumption, reduce operation
Cost.
2. technical solution
In order to achieve the above objectives, technical solution provided by the invention is:
A kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment technique of the present invention, comprises the steps of:
S1, triple effect negative pressure evaporation:Under condition of negative pressure, triple effect negative pressure evaporation system is squeezed into after hydrochloric acid pickling waste liquor is preheated
In, in triple effect negative pressure evaporation system, raw steam provides saturated vapor into an effect evaporation element, what an effect evaporation element generated
Indirect steam enters in two effect evaporation elements, and the indirect steam that two effect evaporation elements generate enters in triple effect evaporation unit, triple effect
Indirect steam in evaporation element is through being cooled into dilute acid recycle;In triple effect negative pressure evaporation system, hydrochloric acid pickling waste liquor is successively
Carry out negative pressure countercurrent evaporation by triple effect evaporation unit, two effect evaporation elements and an effect evaporation element, concentrate after evaporation by
One effect evaporation element enters step flash distillation process in (2);
S2, flash distillation:The saturation concentrate obtained through triple effect negative pressure evaporation enters in flash system, into one under condition of negative pressure
Flash concentration is walked, forms HCl recovery after the steam condensation after flash distillation, the concentrate after flash distillation enters step in (3) at crystallization
Reason;
S3, crystallization:Under vacuum conditions, the concentrate obtained through flash distillation, which enters in crystal system, to be crystallized, by solid-liquid point
Crystal product is obtained from after, filtrate returns to the effect evaporation element in triple effect negative pressure evaporation system and participates in evaporating again.
Further, 5%HCL, 20%FeCL are contained in the hydrochloric acid pickling waste liquor2And 31.2%FeCL2·
4H2O。
Further, at 113~114 DEG C, two effect evaporations are single for the evaporating temperature control of an effect evaporation element in step S1
At 92~93 DEG C, the evaporating temperature of triple effect evaporation unit is controlled at 70~72 DEG C for the evaporating temperature control of member.
Further, it squeezes into crystal system and crystallizes after frerrous chloride concentration >=48% after being flashed in step S2.
Further, the hydrogen chloride gas that crystal system volatilizes in step S3 forms HCl recovery after condensation.
A kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment device of the present invention, including triple effect negative pressure evaporation
System, flash system, crystal system and vacuum system, wherein:
The triple effect negative pressure evaporation system includes an effect evaporation element, two effect evaporation elements and triple effect evaporation unit, institute
An effect evaporation element, two effect evaporation elements and the triple effect evaporation unit stated are made of evaporator, separator and circulating pump, triple effect
The feed inlet of the separator of evaporation element is connected with preheater, for squeezing into hydrochloric acid pickling waste liquor after preheater preheats
In the separator of triple effect evaporation unit, the concentrated solution outlet of the separator of triple effect evaporation unit is evaporated by two effect of punishment in advance pump connection
The feed inlet of the separator of unit, for the concentrate for reaching setting concentration in triple effect evaporation unit to be squeezed into two effect evaporation elements
In, the concentrated solution outlet of the separator of two effect evaporation elements imitates the charging of the separator of evaporation element by punishment in advance pump connection one
Mouthful, for the concentrate for reaching setting concentration in two effect evaporation elements to be squeezed into an effect evaporation element, an effect evaporation element
The concentrated solution outlet of separator connects flash system by discharging pump, reaches the dense of setting concentration in evaporation element for being imitated one
Contracting liquid is squeezed into flash system;The evaporator shell side of one effect evaporation element is connect with extraneous saturation life steam, and an effect evaporation is single
The indirect steam outlet of the separator of member is connected with the evaporator shell side of two effect evaporation elements, the separator of two effect evaporation elements
Indirect steam outlet be connected with the evaporator shell side of triple effect evaporation unit, the indirect steam of the separator of triple effect evaporation unit
Outlet is connected with condenser, and condenser accesses vacuum system by fixed gas condenser;The condensate outlet of condenser with it is dilute
Sour tank is connected, and diluted acid tank accesses diluted acid collection system by thin acid pump;
The flash system includes flash tank and flash condenser, and the feed inlet of the flash tank and an effect evaporation are single
The concentrated solution outlet of the separator of member is connected by discharging pump, and the concentrated solution outlet of flash tank squeezes into system of crystallization by discharging pump
System;The steam (vapor) outlet of the flash tank is connected with flash condenser, and flash condenser is accessed true by fixed gas condenser
Empty set is united, and the condensate outlet of flash condenser is connected with hydrochloric acid tank, and hydrochloric acid tank pumps access hydrochloric acid collection system by hydrochloric acid;
The crystal system includes crystallization kettle, centrifuge and mother liquor tank, and the feed inlet of the crystallization kettle passes through concentration
Liquid distributor is connected with the concentrated solution outlet of flash tank, and the discharge port of the crystallization kettle is connected with centrifuge, centrifuge
Filtrate (liquid be connected with mother liquor tank, mother liquor tank imitates evaporation element with the one of triple effect negative pressure evaporation system by mother liquor pump and is connected
It connects, the gas vent of centrifuge accesses vacuum system.
Further, also there is charging in an effect evaporation element, two effect evaporation elements and triple effect evaporation unit
Preheater, a shell side for imitating the feed preheater in evaporation element are connected with the shell side of the evaporator of an effect evaporation element, and two
The shell side of feed preheater in effect evaporation element is connected with the shell side of the evaporator of two effect evaporation elements, triple effect evaporation unit
In the shell side of feed preheater be connected with the shell side of the evaporator of triple effect evaporation unit, the charging in triple effect evaporation unit is pre-
Hot device is connected with the hydrochloric acid tank in flash system.
Further, an effect evaporation element of the mother liquor tank in the crystal system and triple effect negative pressure evaporation system it
Between also there is mother liquor preheater, the shell side of mother liquor preheater to be connected with the shell side of feed preheater of an effect evaporation element, mother
The condensation-water drain of liquid preheater connects boiler water reuse.
Further, there are the crystal system three groups of crystalline elements, every group of crystalline element to pass through concentrate point
Cloth device is connected with flash system, and every group of crystalline element includes crystallization kettle more than two, the crystallization kettle of every group of crystalline element
Share a desk centrifuge and mother liquor tank.
3. advantageous effect
Using technical solution provided by the invention, compared with existing known technology, there is following remarkable result:
(1) a kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment technique of the invention and device, utilize
Triple effect negative pressure evaporation, evaporating temperature is low, can ensure continuous and stable production, while reducing construction investment, and triple effect negative pressure is steamed
Hair uses forced circulation, prevents the possibility that material crystallized in evaporator and blocked evaporator, it is ensured that the stable operation of device;
Concentration of hydrochloric acid is improved by flash evaporation technology to the full extent after triple effect negative pressure evaporation, and effectively waste heat is utilized to reduce operation
Cost, while the content of the concentration and concentrate frerrous chloride of hydrochloric acid is improved, whole system takes full advantage of wet, latent heat, saves
Raw steam consumption, reduces operating cost;
(2) a kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment technique of the invention and device, triple effect
Negative pressure evaporation uses forced circulation, reduces the crystallization fouling of evaporator, extends the elutriation period of evaporator, easy to operate;Negative pressure
Evaporation, evaporating temperature is low, and to the material corrosion of equipment pipe, governance process is not required to add other auxiliary agents, equipment and pipeline
Material antiseptic is durable, processing cost is low, environmental benefit is apparent, has saved raw steam consumption, the total steam consumption of vapo(u)rization system is general
The 1/3 of logical vaporising device, operation general power is the 1/3 of conventional evaporating apparatus, takes full advantage of wet, latent heat, reduce operation at
This;Processing procedure operates under negative pressure, prevents hydrogen chloride gas from leaking;
(3) a kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment technique of the invention and device, recycling
Regenerated acid purity it is high, returning to workshop use will not be to any adverse effect of production technology generation.
Description of the drawings
Fig. 1 is the triple effect negative pressure in a kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment device of the present invention
The process flow chart of vapo(u)rization system and flash system;In figure, S201, an effect separator;S202, two effect separators;S203, triple effect
Separator;S204, flash tank;E201,1st effective evaporator;E202,2nd effect evaporator;E203, triple effect evaporator;E204, flash distillation
Condenser;E205, condenser;E206, on-condensible gas condenser;E207, diluted acid cooler;E208, level-one preheater;E209,
Two level preheater;E210, three-level preheater;E211, level Four preheater;E212, mother liquor preheater;V201, original fluid container;V202,
Hydrochloric acid tank;V203, diluted acid tank;V204, knockout drum;P201, an effect circulating pump;P202, an effect discharging pump;P203, two effects
Circulating pump;P204, two effect punishment in advance pumps;P205, triple effect cycle pump;P206, triple effect punishment in advance pump;P207, feed pump;P208, hydrochloric acid
Pump;P209, discharging pump;P210, thin acid pump;P211, vapo(u)rization system vacuum pump;P212, vapo(u)rization system cooling water pump;T201, steaming
Hair system cooling tower;
Fig. 2 is the crystal system in a kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment device of the present invention
Process flow chart;In figure, V205, the first mother liquor tank;V206, the second mother liquor tank;V207, third mother liquor tank;V208, recovered liquid
Tank;V209, the first concentration liquid distributor;V210, the second concentration liquid distributor;V211, third concentrate liquid distributor;R201,
One crystallization kettle;R202, the second crystallization kettle;R203, third crystallization kettle;R204, the 4th crystallization kettle;R205, the 5th crystallization kettle;
R206, the 6th crystallization kettle;R207, the 7th crystallization kettle;R208, the 8th crystallization kettle;R209, the 9th crystallization kettle;R210, the tenth crystallization
Kettle;R211, the 11st crystallization kettle;R212, the 12nd crystallization kettle;M201, the first centrifuge;M202, the second centrifuge;M203,
Third centrifuge;P213, the first mother liquor pump;P214, the second mother liquor pump;P215, third mother liquor pump;P216, vacuum system vacuum
Pump group;P217, crystal system cooling water pump;T202, crystal system cooling tower.
Specific implementation mode
To further appreciate that present disclosure, the present invention is described in detail in conjunction with the accompanying drawings and embodiments.
Embodiment
In conjunction with shown in Fig. 1 and Fig. 2, a kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment work of the present embodiment
Skill comprises the steps of:
S1, triple effect negative pressure evaporation:Under condition of negative pressure, triple effect negative pressure evaporation system is squeezed into after hydrochloric acid pickling waste liquor is preheated
In, in triple effect negative pressure evaporation system, raw steam provides saturated vapor into an effect evaporation element, what an effect evaporation element generated
Indirect steam enters in two effect evaporation elements, and the indirect steam that two effect evaporation elements generate enters in triple effect evaporation unit, triple effect
Indirect steam in evaporation element is through being cooled into dilute acid recycle;In triple effect negative pressure evaporation system, hydrochloric acid pickling waste liquor is successively
Carry out negative pressure countercurrent evaporation by triple effect evaporation unit, two effect evaporation elements and an effect evaporation element, concentrate after evaporation by
One effect evaporation element enters step flash distillation process in (2);
S2, flash distillation:The saturation concentrate obtained through triple effect negative pressure evaporation enters in flash system, into one under condition of negative pressure
Flash concentration is walked, forms HCl recovery after the steam condensation after flash distillation, the concentrate after flash distillation enters step in (3) at crystallization
Reason;
S3, crystallization:Under vacuum conditions, the concentrate obtained through flash distillation, which enters in crystal system, to be crystallized, by solid-liquid point
Crystal product is obtained from after, filtrate returns to the effect evaporation element in triple effect negative pressure evaporation system and participates in evaporating again.
In the present embodiment, 5%HCL, 20%FeCL are contained in hydrochloric acid pickling waste liquor2And 31.2%FeCL2·4H2O.It is excellent
Selection of land, the evaporating temperature control of an effect evaporation element is at 113~114 DEG C in step S1, the evaporating temperature control of two effect evaporation elements
At 92~93 DEG C, the evaporating temperature of triple effect evaporation unit is controlled at 70~72 DEG C system.Frerrous chloride after being flashed in step S2 is dense
It squeezes into crystal system and crystallizes after degree >=48%.The hydrogen chloride gas that crystal system volatilizes in step S3 is formed after condensation
HCl recovery.
Continue to refer to figure 1 with shown in Fig. 2, at a kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization of the present embodiment
Device, including triple effect negative pressure evaporation system, flash system, crystal system and vacuum system are managed, wherein:
Triple effect negative pressure evaporation system includes an effect evaporation element, two effect evaporation elements and triple effect evaporation unit, an effect evaporation
Unit, two effect evaporation elements and triple effect evaporation unit are made of evaporator, separator and circulating pump, point of triple effect evaporation unit
Feed inlet from device is connected with preheater, for hydrochloric acid pickling waste liquor to be squeezed into triple effect evaporation unit after preheater preheats
Separator in, the concentrated solution outlet of the separator of triple effect evaporation unit passes through the separators of two effect evaporation elements of punishment in advance pump connection
Feed inlet, for will reach in triple effect evaporation unit setting concentration concentrate squeeze into two effect evaporation elements, two effect evaporation
The concentrated solution outlet of the separator of unit is used for by the feed inlet of the separator of one effect evaporation element of punishment in advance pump connection by two effects
The concentrate for reaching setting concentration in evaporation element is squeezed into an effect evaporation element, the concentrate of the separator of an effect evaporation element
Outlet connects flash system by discharging pump, for the concentrate for reaching setting concentration in an effect evaporation element to be squeezed into flash distillation system
In system;The evaporator shell side of one effect evaporation element is connect with extraneous saturation life steam, and the two of the separator of an effect evaporation element
Secondary steam (vapor) outlet is connected with the evaporator shell side of two effect evaporation elements, the indirect steam outlet of the separator of two effect evaporation elements
It is connected with the evaporator shell side of triple effect evaporation unit, indirect steam outlet and the condenser phase of the separator of triple effect evaporation unit
Connection, condenser access vacuum system by fixed gas condenser;The condensate outlet of condenser is connected with diluted acid tank, diluted acid
Tank accesses diluted acid collection system by thin acid pump.In above-mentioned triple effect negative pressure evaporation system, an effect evaporation element, two effect evaporations
Also there is feed preheater, the shell side of the feed preheater in an effect evaporation element and an effect to steam in unit and triple effect evaporation unit
The shell side of the evaporator of bill member is connected, the steaming of the shell side of the feed preheater in two effect evaporation elements and two effect evaporation elements
The shell side of hair device is connected, the shell side of the shell side of the feed preheater in triple effect evaporation unit and the evaporator of triple effect evaporation unit
It is connected, the feed preheater in triple effect evaporation unit is connected with the hydrochloric acid tank in flash system.
Flash system includes flash tank and flash condenser, and the feed inlet of flash tank and one imitate the separator of evaporation element
Concentrated solution outlet is connected by discharging pump, and the concentrated solution outlet of flash tank squeezes into crystal system by discharging pump;The flash distillation
The steam (vapor) outlet of tank is connected with flash condenser, and flash condenser accesses vacuum system by fixed gas condenser, and flash distillation is cold
The condensate outlet of condenser is connected with hydrochloric acid tank, and hydrochloric acid tank pumps access hydrochloric acid collection system by hydrochloric acid.
Crystal system includes crystallization kettle, centrifuge and mother liquor tank, and the feed inlet of crystallization kettle is by concentrating liquid distributor and dodging
The concentrated solution outlet of steaming pot is connected, and the discharge port of crystallization kettle is connected with centrifuge, the filtrate (liquid and mother liquor tank of centrifuge
It is connected, mother liquor tank is pumped by mother liquor to be connected with an effect evaporation element of triple effect negative pressure evaporation system, and the gas of centrifuge goes out
Mouth access vacuum system.Also there is mother between mother liquor tank in crystal system and an effect evaporation element of triple effect negative pressure evaporation system
Liquid preheater, the shell side of mother liquor preheater are connected with the shell side of the feed preheater of an effect evaporation element, mother liquor preheater
Condensation-water drain connects boiler water reuse.In addition, there are crystal system three groups of crystalline elements, every group of crystalline element to pass through concentrate point
Cloth device is connected with flash system, and every group of crystalline element includes crystallization kettle more than two, the crystallization kettle of every group of crystalline element
Share a desk centrifuge and mother liquor tank.
Technical solution to further understand the present invention, in conjunction with a kind of as depicted in figs. 1 and 2, hydrochloric acid acid of the present embodiment
Waste liquid triple effect negative pressure counter flow flash crystallization treatment device is washed, workflow is as follows:
1), material flow:
The steel part hydrochloric acid pickling waste liquor that collecting pit is arranged outside Pickling-shop enters processing workshop original fluid container V201 precipitations
By feed pump P207 adverse current feedings after removal of impurities, after metering enter triple effect separator S203, passage in transit level-one preheater E208,
Two level preheater E209, indirect steam, the steam condensate of triple effect evaporator E203 for being utilized respectively triple effect separator S203 are pre-
Heat passes through the Secondary-steam heating of triple effect evaporator E203 into the waste liquid of triple effect evaporation unit, reaches the waste liquid of design boiling point
Vapor-liquid separation is completed in triple effect separator S203, waste liquid follows in triple effect evaporation unit through triple effect cycle pump more pressures of P205
After ring, the feed liquid for completing initial concentration squeezes into two effect separator S202 by triple effect punishment in advance pump P206;Passage in transit three-level preheats
Device E210 is reheated using the steam condensate of 2nd effect evaporator E202;
The Secondary-steam heating for passing through 2nd effect evaporator E202 into the waste liquid of two effect evaporation elements, reaches design boiling point
Waste liquid completes vapor-liquid separation in two effect separator S202, and waste liquid is more times strong through two effect circulating pump P203 in two effect evaporation elements
After system cycle, completes the feed liquid concentrated again and squeeze into an effect separator S201 by two effect punishments in advance pump P204;Passage in transit level Four is pre-
Hot device E211 is reheated using the steam condensate (SC) of 1st effective evaporator E201;
Waste liquid into an effect evaporation element is heated by the saturated vapor of 1st effective evaporator E201, reaches design boiling point
Waste liquid completes vapor-liquid separation in an effect separator S201, and waste liquid is more times strong through an effect circulating pump P201 in an effect evaporation element
System recycles and completes to be concentrated by evaporation;The concentrate that frerrous chloride concentration >=45% is obtained after one effect concentration passes through an effect discharging pump
P202 squeezes into flash separator S204, and the gas flashed off at the top of flash separator enters flash condenser E204, bottom chlorine
The underflow for changing ferrous iron concentration >=48% squeezes into the first concentrate distributor V209, the second concentrate point respectively by discharging pump P209
Cloth device V210 and third concentrate liquid distributor V211, then sequentially enter corresponding crystallization kettle, i.e. the first concentrate distributor
V209 is separately connected the first crystallization kettle R201, the second crystallization kettle R202, third crystallization kettle R203 and the 4th crystallization kettle R204, and second
Concentration liquid distributor V210 is separately connected the 5th crystallization kettle R205, the 6th crystallization kettle R206, the 7th crystallization kettle R207 and the 8th knot
Brilliant kettle R208, third concentration liquid distributor V211 are separately connected the 9th crystallization kettle R209, the tenth crystallization kettle R210, the 11st crystallization
Kettle R211 and the 12nd crystallization kettle R212, crystallization kettle utilize crystal system cooling tower T202 and crystal system cooling water pump P217 groups
At cooling water circulation crystallisation by cooling, crystallisation by cooling temperature be 25~35 DEG C.
Magma respectively enters the first centrifuge M201, the second centrifuge M202 and third centrifuge M203 after the completion of crystallization
Be separated by solid-liquid separation, the four water frerrous chlorides isolated carry out human metering packaging, packaged four water frerrous chloride storage or
Person transports outward.The mother liquor (centrifugate) isolated is collected into the first mother liquor tank V205, the second mother liquor tank V206 and third mother liquor tank
V207 pumps P213 by the first mother liquor respectively, the second mother liquor pumps P214, third mother liquor pumps P215 and returns an effect evaporation element again
It is concentrated by evaporation.Passage in transit mother liquor preheater E212, is preheated using the steam condensate (SC) of 1st effective evaporator E201.Concentrate
Into when crystallization kettle in higher temperature and with high concentration hydrogen chloride, in order to prevent the volatile hydrogen chloride of crystallization kettle cause vehicle
Between air pollution and influence shopwork environment, spy on crystallization kettle install additional recycling condenser E213, condensed recovered liquid
Into recycling flow container V208, recovered liquid squeezes into hydrochloric acid collecting pit using hydrochloric acid pump, and recycling flow container V208 connects vacuum system vacuum pump
Group P216, is crystallized under vacuum.
2) steam and condensed water flow, are heated:
Enter 1st effective evaporator E201 shell sides from extraneous saturation life steam, by drain valve, level Four after heat exchange condensation
It is collected after preheater E211, mother liquor preheater E212 shell side heat energy utilizations and is back to boiler or outer row.
The indirect steam of one effect separator S201 enters triple effect evaporator E202 shell sides, and the condensate liquid after heat exchange enters three-level
Preheater E210 shell sides enter triple effect evaporator E203 shell sides using pressure difference after Btu utilization and flash heat energy utilization.
The indirect steam of two effect separator S202 enters triple effect evaporator E203 shell sides, and the condensate liquid after heat exchange enters two level
Preheater E209 shell sides, have utilized heat to enter hydrochloric acid tank V202.The gas flashed off at the top of flash separator S204 enters
Flash condenser E204, enters hydrochloric acid tank V202 after condensation, hydrochloric acid pumps P208 by hydrochloric acid and gets to hydrochloric acid collecting pit.
The indirect steam of triple effect separator S203 enters triple effect condenser E205, and diluted acid tank V203 is entered after being condensed.Portion
Steam enters level-one preheater E208 shell sides in two times, and diluted acid tank V203 is entered after condensation.Diluted acid is got by thin acid pump P210
To diluted acid collecting pit.Passage in transit diluted acid cooler E207;Part diluted acid after cooling enters E206 pairs of on-condensible gas condenser
On-condensible gas carries out cooling and purifying, purifies the diluted acid after on-condensible gas and returns to diluted acid tank.Triple effect condenser E205 is using evaporation system
The cooling water circulation of system cooling tower T201 and vapo(u)rization system cooling water pump P212 compositions is cooled down.
3), vacuum system:
Evaporation section vacuum system is by flash condenser E204, triple effect condenser E205, on-condensible gas condenser E206, steaming
The compositions such as system vacuum pump P211, vapor-liquid separation tank V204 are sent out, the fixed gas in evaporation section system is extracted out, maintain evaporator man
The system vacuum of section, realizes effective negative pressure evaporation.
Crystallize section vacuum system by recycling condenser E213, crystal system vacuum pump set P216, the first mother liquor tank V205,
The compositions such as the second mother liquor tank V206, third mother liquor tank V207, recycling flow container V208 are mainly used for collection, the crystallization of centrifuge mother liquor
Recycling, centrifuge tail gas absorption of kettle hydrogen chloride vapor etc. realize that effective cleaning production and production environment meet environmental protection and wants
It asks.
A kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment technique and device of the present invention, has following excellent
Point:
1) unique multiple effect counter current flash evaporation technology improves concentration of hydrochloric acid to the full extent, and effectively waste heat is utilized to reduce
Operating cost, while improving the content of the concentration and concentrate frerrous chloride of hydrochloric acid;
2) the crystallization fouling of evaporator is reduced;Extend the elutriation period of evaporator;
3) under condition of negative pressure, evaporating temperature is low, to the material corrosion of equipment pipe, can ensure that continuous-stable is given birth to
Production, while reducing construction investment;
4) processing procedure operates under negative pressure, prevents hydrogen chloride gas from leaking;
5) external heat combination forced circulation pattern is used, the possibility that material crystallized in evaporator and blocked evaporator is prevented
Property, it is ensured that the stable operation of device;
6) the regenerated acid purity recycled is high, and any adverse effect will not be generated to production technology by returning to workshop use;
7) the total steam consumption of vapo(u)rization system is the 1/3 of common vaporising device, and operation general power is the 1/3 of conventional evaporating apparatus;
8) evaporation efficiency height, continuous and stable production, easy to operate, governance process are not required to add other auxiliary agents, equipment and pipe
Road material antiseptic is durable, processing cost is low, environmental benefit is apparent etc.;
9) whole system takes full advantage of wet, latent heat, has saved raw steam consumption, has reduced operating cost.
Schematically the present invention and embodiments thereof are described above, description is not limiting, institute in attached drawing
What is shown is also one of embodiments of the present invention, and actual structure is not limited to this.So if the common skill of this field
Art personnel are enlightened by it, without departing from the spirit of the invention, without creatively designing and the technical solution
Similar frame mode and embodiment, are within the scope of protection of the invention.
Claims (9)
1. a kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment technique, which is characterized in that comprise the steps of:
S1, triple effect negative pressure evaporation:Under condition of negative pressure, squeezed into after hydrochloric acid pickling waste liquor is preheated in triple effect negative pressure evaporation system,
In triple effect negative pressure evaporation system, raw steam provides saturated vapor into an effect evaporation element, and one imitates two that evaporation element generates
Secondary steam enters in two effect evaporation elements, and the indirect steam that two effect evaporation elements generate enters in triple effect evaporation unit, and triple effect steams
Indirect steam in bill member is through being cooled into dilute acid recycle;In triple effect negative pressure evaporation system, hydrochloric acid pickling waste liquor passes through successively
It crosses triple effect evaporation unit, two effect evaporation elements and an effect evaporation element and carries out negative pressure countercurrent evaporation, the concentrate after evaporation is by one
Effect evaporation element enters step flash distillation process in (2);
S2, flash distillation:The saturation concentrate obtained through triple effect negative pressure evaporation enters in flash system, is further dodged under condition of negative pressure
Inspissation contracts, and forms HCl recovery after the steam condensation after flash distillation, the concentrate after flash distillation enters step crystallization treatment in (3);
S3, crystallization:Under vacuum conditions, the concentrate obtained through flash distillation, which enters in crystal system, to be crystallized, after separation of solid and liquid
Crystal product is obtained, filtrate returns to the effect evaporation element in triple effect negative pressure evaporation system and participates in evaporating again.
2. a kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment technique according to claim 1, feature
It is:Contain 5%HCL, 20%FeCL in the hydrochloric acid pickling waste liquor2And 31.2%FeCL2·4H2O。
3. a kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment technique according to claim 2, feature
It is:At 113~114 DEG C, two imitate the evaporating temperature control of evaporation elements for the evaporating temperature control of an effect evaporation element in step S1
At 92~93 DEG C, the evaporating temperature of triple effect evaporation unit is controlled at 70~72 DEG C system.
4. a kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment technique according to claim 3, feature
It is:It squeezes into crystal system and crystallizes after frerrous chloride concentration >=48% after being flashed in step S2.
5. a kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment technique according to claim 4, feature
It is:The hydrogen chloride gas that crystal system volatilizes in step S3 forms HCl recovery after condensation.
6. a kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment device, it is characterised in that:It is steamed including triple effect negative pressure
Hair system, flash system, crystal system and vacuum system, wherein:
The triple effect negative pressure evaporation system includes an effect evaporation element, two effect evaporation elements and triple effect evaporation unit, described
One effect evaporation element, two effect evaporation elements and triple effect evaporation unit are made of evaporator, separator and circulating pump, triple effect evaporation
The feed inlet of the separator of unit is connected with preheater, for hydrochloric acid pickling waste liquor to be squeezed into triple effect after preheater preheats
In the separator of evaporation element, the concentrated solution outlet of the separator of triple effect evaporation unit passes through two effect evaporation element of punishment in advance pump connection
Separator feed inlet, for will reach in triple effect evaporation unit setting concentration concentrate squeeze into two effect evaporation elements,
The concentrated solution outlet of the separator of two effect evaporation elements is used by the feed inlet of the separator of one effect evaporation element of punishment in advance pump connection
It is squeezed into an effect evaporation element in imitating the concentrate for reaching setting concentration in evaporation element by two, the separator of an effect evaporation element
Concentrated solution outlet by discharging pump connect flash system, for will one imitate evaporation element in reach setting concentration concentrate beat
Enter in flash system;The evaporator shell side of one effect evaporation element is connect with extraneous saturation life steam, point of an effect evaporation element
Indirect steam outlet from device is connected with the evaporator shell side of two effect evaporation elements, and two imitate the secondary of the separator of evaporation elements
Steam (vapor) outlet is connected with the evaporator shell side of triple effect evaporation unit, the outlet of the indirect steam of the separator of triple effect evaporation unit with
Condenser is connected, and condenser accesses vacuum system by fixed gas condenser;The condensate outlet of condenser and diluted acid tank phase
Connection, diluted acid tank access diluted acid collection system by thin acid pump;
The flash system includes flash tank and flash condenser, and the feed inlet of the flash tank and one imitate evaporation element
The concentrated solution outlet of separator is connected by discharging pump, and the concentrated solution outlet of flash tank squeezes into crystal system by discharging pump;Institute
The steam (vapor) outlet for the flash tank stated is connected with flash condenser, and flash condenser accesses vacuum system by fixed gas condenser
System, the condensate outlet of flash condenser are connected with hydrochloric acid tank, and hydrochloric acid tank pumps access hydrochloric acid collection system by hydrochloric acid;
The crystal system includes crystallization kettle, centrifuge and mother liquor tank, and the feed inlet of the crystallization kettle passes through concentrate point
Cloth device is connected with the concentrated solution outlet of flash tank, and the discharge port of the crystallization kettle is connected with centrifuge, the filter of centrifuge
Liquid outlet is connected with mother liquor tank, and mother liquor tank is pumped by mother liquor to be connected with an effect evaporation element of triple effect negative pressure evaporation system,
The gas vent of centrifuge accesses vacuum system.
7. a kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment device according to claim 6, feature
It is:Described one, which is imitated, also has feed preheater in evaporation element, two effect evaporation elements and triple effect evaporation unit, an effect evaporation
The shell side of feed preheater in unit is connected with the shell side of evaporator of an effect evaporation element, in two effect evaporation elements into
Expect that the shell side of preheater is connected with the shell side of the evaporator of two effect evaporation elements, the feed preheater in triple effect evaporation unit
Shell side is connected with the shell side of the evaporator of triple effect evaporation unit, in the feed preheater and flash system in triple effect evaporation unit
Hydrochloric acid tank be connected.
8. a kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment device according to claim 7, feature
It is:Also have mother liquor pre- between mother liquor tank in the crystal system and an effect evaporation element of triple effect negative pressure evaporation system
Hot device, the shell side of mother liquor preheater are connected with the shell side of the feed preheater of an effect evaporation element, the condensation of mother liquor preheater
Water out connects boiler water reuse.
9. a kind of hydrochloric acid pickling waste liquor triple effect negative pressure counter flow flash crystallization treatment device according to claim 8, feature
It is:The crystal system has three groups of crystalline elements, and every group of crystalline element is by concentrating liquid distributor and flash system
It is connected, every group of crystalline element includes crystallization kettle more than two, and the crystallization kettle of every group of crystalline element shares a desk centrifuge
And mother liquor tank.
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CN115180594B (en) * | 2022-07-11 | 2023-12-26 | 新疆西部合盛硅业有限公司 | Recovery process of wastewater from organosilicon slurry residue treatment |
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