CN105129852B - The system that a kind of high-efficiency self-circulation wet method continuously prepares sodium dichromate - Google Patents
The system that a kind of high-efficiency self-circulation wet method continuously prepares sodium dichromate Download PDFInfo
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- CN105129852B CN105129852B CN201510589639.2A CN201510589639A CN105129852B CN 105129852 B CN105129852 B CN 105129852B CN 201510589639 A CN201510589639 A CN 201510589639A CN 105129852 B CN105129852 B CN 105129852B
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Abstract
The invention discloses the system that a kind of high-efficiency self-circulation wet method continuously prepares sodium dichromate, including：Tank is beaten, the first delivery pump, preheating device, liquid phase oxidation reaction device, flash distillation plant, the first separator, the first enrichment facility, carbonizing plant, the second separator, electrolytic cell, the second enrichment facility, equipment of crystallisation by cooling and the centrifugal device being sequentially connected with mashing tank by feed liquid conveyance conduit；Apparatus of oxygen supply, it is used to be passed through oxygen to liquid phase oxidation reaction device；Wherein, the CO that pre- thermal decomposition is produced2, oxidation produce CO2The steam produced with steam and flash distillation can be delivered to enrichment facility, and steam is concentrated for feed liquid, CO2Gas input carbonizing plant is used for carburizing reagent；Isolated sodium acid carbonate containing chromium can be delivered to mashing tank as dispensing in second separator.In the present invention, by by-product, steam and sodium acid carbonate be used to being carbonized, feed liquid concentration and dispensing, realize sodium element, CO2Utilized with heat energy high-efficiency self-circulation, reduce the waste of the energy.
Description
Technical field
The invention belongs to the preparation field of sodium dichromate, more particularly to a kind of high-efficiency self-circulation wet method continuously prepares sodium dichromate
System.
Background technology
Sodium dichromate is one of important Inorganic Chemicals as chromic salts basic product, is occupied importantly in national economy
Position, with quite varied purposes.Its traditional processing technology front end is using raw materials such as chromite, soda ash, return slags in rotary kiln
In more than 1000 DEG C calcinings, roasting clinker obtains chromium acid sodium solution through leaching, and rear end obtains arsenic using sulfuric acid acidifying sodium chromate
Sodium solution, sodium dichromate product is obtained through evaporative crystallization dehydration.But there is serious secondary pollution, resource wave in the production technology device
Take, high energy consumption, low production efficiency the problems such as, high risks are caused to local environment, the sustainable development of serious restriction Chrome Salt Industry
Exhibition.Therefore, to solve the defect that traditional handicraft device is present, new technology is sought extremely urgent.
The system that sodium dichromate is mentioned in " method that one-step method prepares sodium dichromate ", document is disclosed in CN201210466756
It is standby using chrome iron powder, the dispersion containing soda and water in the presence of oxygen, in the presence of carbon dioxide catalyst in a constant temperature
Hydrothermal oxidization reaction is carried out under degree and pressure, sodium dichromate solution is obtained through supplementing acidifying, the technique breaches traditional handicraft, greatly
Technological process is shortened greatly, and energy consumption is low, production environment is friendly, is the favourable production ways for preparing sodium dichromate.But the technique pair
Production equipment has great requirement, and need to calcine accessory substance sodium acid carbonate, and hand labor intensity increase, process units can not be met
Continuous production, resource can not be fully exploited, and produced heat recovery and utilization rate is low.Therefore, new process units is improved
Into trend.
The content of the invention
It is an object of the invention to solve at least the above and/or defect, and provide at least will be described later excellent
Point.
It is a still further object of the present invention to provide the system that a kind of high-efficiency self-circulation wet method continuously prepares sodium dichromate, it is realized
The high-efficiency self-circulation for preparing sodium element, carbon dioxide and heat energy during sodium dichromate is utilized, and reduces the waste of the energy, comprehensive
It make use of the accessory substance produced in technical process.
Continuously made there is provided a kind of high-efficiency self-circulation wet method according to object of the present invention and other advantages to realize
The system of standby sodium dichromate, including：
Tank is beaten, the feeding mouth of input oxide spinel hydrogen sodium, ferrochrome powder, sodium carbonate and water is provided with；
Mashing tank is sequentially connected the first delivery pump, preheating device, liquid phase oxidation reaction device, sudden strain of a muscle by feed liquid conveyance conduit
Steam device, it is the first separator, the first enrichment facility, carbonizing plant, the second separator, electrolytic cell, the second enrichment facility, cold
But crystallization apparatus and centrifugal device；
Apparatus of oxygen supply, it is connected with the liquid phase oxidation reaction device by pipeline；For to the liquid phase oxidation reaction
Device is passed through oxygen；
Wherein, the CO that pre- thermal decomposition is produced in the preheating device2, in liquid phase oxidation reaction device oxidation produce
CO2The first enrichment facility is delivered to and second dense by gas transmission pipeline with the steam produced in steam and flash distillation plant
Compression apparatus, steam is concentrated for feed liquid；CO2Gas is exported simultaneously from the blowing mouth of the first enrichment facility and the second enrichment facility respectively
Removed water by freeze drier, CO2The carbonizing plant is inputted after compressor compresses is used for carburizing reagent；The second separation dress
Isolated sodium acid carbonate containing chromium can be used as dispensing by pipeline to the feeding mouth for being beaten tank in putting.
Preferably, the feeding mouth of the mashing tank has four, respectively sodium acid carbonate entrance, ferrochrome powder entrance, carbonic acid
Sodium entrance and water inlet.
Preferably, the apparatus of oxygen supply includes oxygen air separation unit, oxygen compressor and oxygen surge tank, oxygen compression
Machine is connected with the oxygen air separation unit and oxygen surge tank respectively, the oxygen surge tank and the liquid phase oxidation reaction device
Pass through pipeline communication.
Preferably, the first enrichment facility steam drain, second enrichment facility are provided with first enrichment facility
On be provided with the second enrichment facility steam drain.
Preferably, first separator and the second separator are vertical automatic plate frame press filter.
Preferably, the thermometer for detecting temperature in preheating device is provided with the preheating device.
Preferably, the flash distillation plant is level Four flash tank.
Preferably, connection second is defeated on the feed liquid conveyance conduit between the liquid phase oxidation reaction device and flash distillation plant
Send pump；The 3rd delivery pump is connected on feed liquid conveyance conduit between the flash distillation plant and the first separator；Described first is dense
The 4th delivery pump is connected on feed liquid conveyance conduit between compression apparatus and carbonizing plant；The carbonizing plant and the second separator
Between feed liquid conveyance conduit on connect the 5th delivery pump；Feed liquid conveyance conduit between the electrolytic cell and the second enrichment facility
The 6th delivery pump of upper connection；Connection the 7th is defeated on feed liquid conveyance conduit between second enrichment facility and equipment of crystallisation by cooling
Send pump；The 8th delivery pump is connected on feed liquid conveyance conduit between the equipment of crystallisation by cooling and centrifugal device.
The present invention at least includes following beneficial effect：
(1) clean manufacturing：The continuous fabricating technology of sodium dichromate whole process wet method is completed, traditional rotation is revolutionized
Kiln calcines production model, realizes that sodium dichromate manufacturing process system is totally-enclosed, three-waste free discharge, reduces environmental pollution, reaches industry
The sodium dichromate clean manufacturing of scale.
(2) realize that resource high-efficiency circulation comprehensive utilizes system：In the present invention, the bicarbonate produced by rear end carbonization workshop section
Sodium is passed through front end ferrochrome liquid phase oxidation workshop section through conveyance conduit, and the carbon dioxide and steam of oxidation reaction by-product are used for into rear end chromium
Sour sodium carbonization and feed liquid concentration, realize sodium element, carbon dioxide and heat energy high-efficiency self-circulation and utilize, reduce the waste of the energy,
Accessory substance produced by comprehensive utilization process process.
(3) sodium dichromate manufacturing cost is reduced：The present invention changes the modes such as reaction, filtering, the evaporation of the traditional extensive style of chromic salts,
Introduce simultaneously independent development vertical automatic plate frame press filter, high-efficiency evaporator, oxidation reactor, carbonization reactor, chemical pump cold
But the key device such as water automatic control system and corollary equipment, system solve that sodium acid carbonate " scabbing ", equipment attrition be big, chromium
The low problem of yield, is greatly lowered sodium dichromate manufacturing cost.
Further advantage, target and the feature of the present invention embodies part by following explanation, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Brief description of the drawings：
Fig. 1 is the structural representation for the system that high-efficiency self-circulation wet method of the present invention continuously prepares sodium dichromate；
Fig. 2 is the structural representation of the horizontal reacting kettle described in one embodiment of the invention.
Embodiment：
The present invention is described in further detail below in conjunction with the accompanying drawings, to make those skilled in the art with reference to specification text
Word can be implemented according to this.
It should be appreciated that such as " having ", "comprising" and " comprising " term used herein do not allot one or many
The presence or addition of individual other elements or its combination.
Fig. 1 shows the system that a kind of high-efficiency self-circulation wet method of the present invention continuously prepares sodium dichromate, including：
Tank 5 is beaten, sodium acid carbonate entrance 1, ferrochrome powder entrance 2, sodium carbonate entrance 3 and the water of input raw material is provided with
Entrance 4；
Mashing tank 5 is sequentially connected the first delivery pump 7, preheating device 8, liquid phase oxidation reaction device by feed liquid conveyance conduit
17th, flash distillation plant 21, the first separator 26, the first enrichment facility 30, carbonizing plant 35, the second separator 39, electrolytic cell
43rd, the second enrichment facility 46, equipment of crystallisation by cooling 51 and centrifugal device 54；
Apparatus of oxygen supply 12, it is connected with the liquid phase oxidation reaction device 17 by pipeline；For to the liquid phase oxidation
Reaction unit 17 is passed through oxygen；
Wherein, the CO that pre- thermal decomposition is produced in the preheating device 82, in liquid phase oxidation reaction device 17 oxidation produce
CO2The and of the first enrichment facility 30 is delivered to by gas transmission pipeline 64 with the steam produced in steam and flash distillation plant 21
Second enrichment facility 46, the steam that conveying comes is concentrated for feed liquid；CO2Gas is respectively from the first gas transmission of the first enrichment facility 30
Second blowing mouth 65 of the enrichment facility 46 of mouth 19 and second is exported and removed water by freeze drier 66, CO2Compressor 67 compresses
After input the carbonizing plant 35 be used for carburizing reagent；Isolated sodium acid carbonate containing chromium can in second separator 39
Dispensing is used as by pipeline to the sodium acid carbonate entrance 1 for being beaten tank 5.
In this technical scheme, oxide spinel hydrogen sodium, ferrochrome powder, sodium carbonate and water are respectively from sodium acid carbonate entrance 1, chromium
Iron powder entrance 2, sodium carbonate entrance 3 and water inlet 4 add mashing tank 5 and are beaten, and the feed liquid after mashing is exported from slurry outlet 6, warp
Cross the first delivery pump 7 and be delivered to from feed liquid conveyance conduit after preheating device feeding mouth 9 and enter preheating device 8, the feed liquid of preheating is passed through
Feed liquid conveyance conduit, which is delivered to after liquid phase oxidation reaction device feeding mouth 11, enters liquid phase oxidation reaction device 17；Meanwhile, oxygen supply
Oxygen is delivered to after liquid phase oxidation reaction device oxygen intake 16 by device 12 enters liquid phase oxidation reaction device for reacting；
The feed liquid produced after being reacted in liquid phase oxidation reaction device 17 passes through flash distillation after the output of liquid phase oxidation reaction device discharging opening 20
Device feeding mouth 22 enters flash distillation plant 21；After being handled in flash distillation plant 21 feed liquid, feed liquid is gone out from flash distillation plant
Material mouth 24 enters the first separator 26 after exporting by the first separator feeding mouth 25；In the process, the pre- hot charging
Put the CO that pre- thermal decomposition is produced in 82, the CO of generation is aoxidized in liquid phase oxidation reaction device 172With steam and flash distillation plant 21
The steam of middle generation passes through thermal gas vent 10, liquid phase oxidation reaction device gas vent 18 and flash distillation plant gas respectively
Outlet 23 exports and is delivered to the first enrichment facility gas access 33 and the second enrichment facility gas by gas transmission pipeline 64
The first enrichment facility 30 and the second enrichment facility 46 are respectively enterd after entrance 48, steam is used to concentrate feed liquid, with liquid after concentration
Body form is utilized, and realizes recycling for steam；And CO2Still exist in gaseous form, and then CO2Gas is respectively from
First blowing mouth 19 of one enrichment facility 30 and the second blowing mouth 65 of the second enrichment facility 46 are exported and by freeze drier
66 water removals, CO2Input carbonizing plant gas access 36 enters the carbonizing plant 35 for carburizing reagent after compressor 67 compresses；
Realize recycling for carbon dioxide；Feed liquid passes through separation of solid and liquid in the first separator 26, and the solid filtered to isolate is rich
Siderochrome slag is discharged through rich siderochrome slag outlet 27, and the rich siderochrome slag of discharge is washed with water, and washings can input the water inlet of mashing tank 5
4 are used to be beaten, and realize water circulation use；The feed liquid filtered to isolate is chromium acid sodium solution, and feed liquid is through the first separator feed liquid
First enrichment facility 30 is entered by the first enrichment facility feeding mouth 29 after the output of outlet 28 and carries out concentration, while available
Steam in liquid phase oxidation device 17 and flash distillation plant 21 is concentrated to feed liquid, and the feed liquid after concentration is dense through first
Compression apparatus discharging opening 32 enters carbonizing plant 35 by carbonizing plant feeding mouth 34 after exporting and carries out carburizing reagent, while available
CO is produced in preheating device 8 and liquid phase oxidation reaction device 172Carburizing reagent is carried out, CO is realized2Recycle；In carbon
Makeup puts the feed liquid that carburizing reagent is completed in 35 after the output of carbonizing plant discharging opening 37 by the second separator feeding mouth 38
Into the second separator 39, feed liquid is separated in the second separator 39, and obtained sodium acid carbonate containing chromium passes through the second separation
The sodium acid carbonate outlet 41 of device 39 is discharged, and is entered the sodium acid carbonate that sodium acid carbonate containing chromium is delivered to mashing tank 5 by pipeline
Mouth 1 is used as raw material, realizes recycling for sodium acid carbonate；After isolated feed liquid is exported through the second separator discharging opening 40
Electrolytic cell 43 is entered by electrolytic cell feeding mouth 42, electrolytic cell 43 carries out electrolysis supplement acidification to feed liquid, improves feed liquid
Acidification rate, the feed liquid by electrolysis supplement acidification passes through the second enrichment facility feeding mouth after being exported through electrolytic cell discharging opening 44
45 are concentrated into the second enrichment facility 46, while using the steam in liquid phase oxidation device 17 and flash distillation plant 21
Feed liquid is concentrated, the feed liquid after concentration is entered after being exported through the second enrichment facility discharging opening 49 by equipment of crystallisation by cooling
Material mouth 50 enters equipment of crystallisation by cooling 51 and carries out crystallisation by cooling, and obtained crystal solution passes through after the output of crystallization apparatus discharging opening 52
Centrifugal device feeding mouth 53 enters centrifugal device 54 and carries out centrifugal treating, and the feed liquid handled by centrifugal device 54 is from centrifugal device
Material liquid outlet 55 is deviate from, and obtained sodium dichromate is exported from centrifugal device sodium dichromate outlet 56, obtains sodium dichromate.
In the above-mentioned technical solutions, the liquid phase oxidation reaction device 17 is horizontal reacting kettle, and its structure includes：Kettle
68, it is to be provided with charging aperture 11 and discharging opening 20 on the hollow cylinder in horizontal placement, the kettle；Discharging opening 20 and level
Face is connected in 45 degree of angles with hollow cylinder by stainless steel tube；Three overflow baffles 69, it is arranged on inside the kettle,
And kettle inner space is divided into I, II, III and IV chamber along kettle length direction, I, II, III chamber carries out oxidation reaction,
IV chamber discharges；Four agitators 70, it is separately positioned in I, II, III and IV chamber, and each agitator is by puddler 71
The first blade 72 and the second blade 73 being fixedly connected with puddler are constituted, and the first blade is self-priming, and the second blade is to open
Formula worm gear, puddler is connected to a drive device 74, and the first blade is arranged on the second blade top, and is kept off less than adjacent overflow
The blade of height first of plate seethes feed liquid upwards, and material is pressed downward by the second blade, so that material is well mixed, and energy
Fully reacted with oxygen, improve conversion ratio；Wherein, charging aperture 11 and discharging opening 20 respectively with the chamber of kettle I and IV chamber
Connection, and the bottom of II, III and IV chamber of kettle is provided with oxygen intake 16, oxygen intake 16 connects with apparatus of oxygen supply 12
Connect；Inserted filtering element stainless steel gas distributor is installed, aperture can effectively prevent that material from blocking up for 1~5 μm at oxygen intake 16
Plug；Material is entered I chamber of kettle by charging aperture, is passed through oxygen and is stirred so that material and oxygen are sufficiently mixed and anti-
Should, when material reaches I chamber overflow baffle height, material overflows to II chamber, and the oxygen inlet port opened in II chamber leads to
Enter oxygen, material is subjected to secondary oxidation reaction, when material reaches II chamber overflow baffle height, material overflows to III chamber
Room, the oxygen inlet port opened in III chamber is passed through oxygen, and material is carried out into three oxidation reactions, when material reaches that III chamber overflows
When flowing height of baffle plate, material overflows to IV chamber, and flash distillation plant 21 is delivered to by discharging opening 20；Chuck condensing unit 75, its
The kettle periphery is set in, the side lower part of chuck condensing unit one, which is provided with cooling water inlet 76, to be used to be passed through cooling water, another
Upper lateral part, which is provided with coolant outlet 77, to be used to discharge cooling water；Gas vent 18, it is arranged on kettle top close to cooling water
Outlet, for CO2With the output of steam；Multiple upper drains 78 have been issued on kettle top, and four cavity bottoms have been issued down
Drain 79；Kettle bottom is provided with cooling groove 80, and is connected with lower drain, and upper and lower drain needs parking in reactor
For thoroughly quickly being cleared up the material in kettle during technological transformation, and the material after cleaning is passed through at cooling groove progress cooling
Reason and storage；It is used for pressure, liquid level in real-time monitored kettle provided with pressure gauge 81, liquid level gauge 82 and temperature monitor 83 outside kettle
With the change of temperature, in order to adjust, the high order end of kettle, which offers inspection manhole 84, to be used for after reactor failure
It is easy to staff to come in and go out to be overhauled.
In the above-mentioned technical solutions, overflow baffle is provided between each chamber of horizontal reacting kettle of use, when continuous feed is participated in
Reacted material rises along baffle plate, and the residence time is longer, and reaction is abundant, when reaching height of baffle plate, it will overflow to next
Chamber, this chamber enters oxygen simultaneously, and secondary oxidation is carried out in the presence of stirring, when feed liquid reaches the height of baffle plate of this chamber,
Next chamber can be overflowed to again to continue to aoxidize, and until feed liquid reaches last chamber, arranged feed liquid by pressure itself in kettle
Go out, be delivered to feed liquid storage tank.In the process, material is constantly added oxidation, and reaction is abundant, and transformation efficiency and conversion ratio are obtained
Greatly improve.In addition, the agitator that the reactor is used, its middle and upper part blade is self-priming, bottom blade is open type turbine, on
Lower paddle is each divided the work, and material prevents material formation dead band, be evenly distributed, oxygen is filtered by plug-in type in being seethed up and down in kettle
Core stainless steel gas distributor enters in kettle from air inlet, and the gas distributor aperture is 1~5 μm, can effectively prevent that material from blocking up
Plug, it is ensured that preferable oxygen-enriched environment, as the rotation of stirring blade is fully contacted with material, is allowed to fully reaction, reaches ideal
Oxidation effectiveness.
In another embodiment, compressed as shown in figure 1, the apparatus of oxygen supply 12 includes oxygen air separation unit 13, oxygen
Machine 14 and oxygen surge tank 15, oxygen compressor 14 connect 15, institute with the oxygen air separation unit 13 and oxygen surge tank respectively
Oxygen surge tank 15 is stated with the liquid phase oxidation reaction device 17 by pipeline communication, can be abundant by this apparatus of oxygen supply 12
The oxygen in air is compressed utilization, realizing showing for oxygen does existing use, takes full advantage of air resource.
In another embodiment, as shown in figure 1, being provided with the first enrichment facility steam discharge on first enrichment facility 30
Mouthfuls 31, it is provided with the second enrichment facility steam drain 47 on second enrichment facility 46, the first enrichment facility exhaust outlet 31 and the
The effect of two enrichment facility exhaust outlets 47 is after the effective concentration by the enrichment facility 46 of the first enrichment facility 30 second is utilized
Steam discharge, it is ensured that the normal operation of equipment, realize feed liquid concentration purpose.
In another embodiment, the separator 39 of the first separator 26 and second is vertical automatic sheet frame pressure
Filter, the equipment has the high spy of big filter area, filtering production capacity height, unimpeded input and output material, high degree of automation, filtration cakes torrefaction degree
Point, and the service life of filter cloth can be extended.
In another embodiment, the temperature for detecting temperature in preheating device 8 is provided with the preheating device 8
Meter, thermometer can detect the temperature of preheating, and preheating temperature can be adjusted in warm to anti-by the display of thermometer
The temperature answered.
In another embodiment, the flash distillation plant 21 is level Four flash tank, when there is level Four flash tank material to be heated
Between short, evaporation rate it is fast, cocnentration factor is great, effectively keeps material original effect, the characteristics of anti-scaling property is good.
In another embodiment, the feed liquid conveyance conduit between the liquid phase oxidation reaction device 17 and flash distillation plant 21
The second delivery pump 57 of upper connection；The 3rd is connected on feed liquid conveyance conduit between the separator 26 of flash distillation plant 21 and first
Delivery pump 58；The 4th delivery pump 59 is connected on feed liquid conveyance conduit between first enrichment facility 30 and carbonizing plant 35；
The 5th delivery pump 60 is connected on feed liquid conveyance conduit between the separator 39 of carbonizing plant 35 and second；The electrolytic cell
43 and the second feed liquid conveyance conduit between enrichment facility 46 on connect the 6th delivery pump 16；Second enrichment facility 46 with it is cold
But the 7th delivery pump 62 is connected on the feed liquid conveyance conduit between crystallization apparatus 51；The equipment of crystallisation by cooling 51 and centrifugal device
The 8th delivery pump 63 is connected on feed liquid conveyance conduit between 54, these delivery pumps are metering diaphragm pump, the metering diaphragm pump
Feed liquid effectively can be delivered to corresponding equipment, and corresponding transfer rate can be set, improve the life of sodium dichromate
Produce production capacity.
In another embodiment, the soda ash for being 99% by ferrochrome that Cr containing simple substance is 68%, content, content are 89%
The sodium acid carbonate containing chromium that is obtained from the second separator 39, the wash water containing chromium from the rich siderochrome slag of washing are by mass fraction 1：
0.65：1.13：2.89 ratios are added in mashing tank 5 and are configured to mixed slurry；
Mixed slurry is pressed into 2.0m with the first delivery pump 73/ h continuously squeezes into preheating device 8, is preheated to 180 DEG C of continuous inputs
Liquid phase oxidation reaction device 17 (oxidation dissolution tank), the CO that pre- thermal decomposition is produced2Gas inputs carburizing reagent after water removal, compression
Device 35 is used for carburizing reagent；
Control liquid phase oxidation reaction device 17 (oxidation dissolution tank) interior 250 DEG C of reaction material liquid temperature, apparatus of oxygen supply 12 is to liquid
The uniform oxygen that is passed through maintains stagnation pressure 4.5MPa in phase oxidation reaction unit 17 (oxidation dissolution tank), and steam input first is dense in exhaust
The enrichment facility 46 of compression apparatus 30 and second is concentrated for rear end feed liquid, and carbon dioxide input carbonization after water removal, compression is anti-
Answer device 35 be used for be used for carburizing reagent；
Control liquid phase oxidation reaction device 17 (oxidation dissolution tank) discharging flow 2.0m3/ h continuous discharges, reaction material liquid is led to
Cross flash distillation plant (level Four flash tank) step by step cool, be depressured, final stage flash tank out-feed liquid temperature, which is down to after 110 DEG C, enters drop
Middle benefit gas turn trough；
With pump will cool groove in feed liquid squeeze into the first separator 26 (vertical board and frame machine), filter to isolate rich siderochrome slag from
Rich siderochrome slag outlet 27, obtains Na2CrO4Content is 426.8g/L chromium acid sodium solution, and Cr conversion ratios are 92.3% in ferrochrome, are washed
The wash water for washing rich siderochrome slag can be used for front end to be beaten the dispensing of tank 5；
Obtained chromium acid sodium solution squeezes into carbonizing plant with the 4th delivery pump after being concentrated through the first enrichment facility 30 and carries out carbon
Change, steam and sudden strain of a muscle that steam used by the first enrichment facility is produced all from the oxidation reaction of front end liquid phase oxidation reaction device 17
Steam CO used in the indirect steam that device 21 is produced, carbonizing plant 352It all is from front end preheating device 8 thermal decomposition and liquid phase in advance
The CO that oxidation unit 17 (oxidation dissolution tank) oxidation reaction is produced2, the feed liquid after carbonization passes through the (vertical board of the first separator 39
Frame machine) it is filtrated to get the carbodiimide solution that acidification rate is 90.2%, carbon of the sodium acid carbonate containing chromium isolated from the second separator 39
Sour hydrogen sodium outlet 41 is discharged, and the sodium acid carbonate entrance 1 that sodium acid carbonate containing chromium is delivered to mashing tank 5 is used as into original by pipeline
Material；
Carbodiimide solution input electrolytic cell is acidified, and acidification rate brings up to 100.5%, and acidifying solution is dense through the second enrichment facility 46
Contracting, the crystallisation by cooling of equipment of crystallisation by cooling 51, obtained crystal solution deviate from mother liquor by centrifugal device 54 and obtain sodium dichromate, sampled
Detect Na in this obtained sodium dichromate product2Cr2O7·H2O content 99.61%, SO4 2 -Content 0.17%, Cl-Content is
0.06%.
In another embodiment, the soda ash for being 99% by ferrochrome that Cr containing simple substance is 68%, content, content are 89%
The sodium acid carbonate containing chromium that is obtained from the second separator 39, the wash water containing chromium from the rich siderochrome slag of washing are by mass fraction 1：
0.76：0.98：2.75 ratios are added in mashing tank 5 and are configured to mixed slurry；
Mixed slurry is pressed into 3.5m with the first delivery pump 73/ h continuously squeezes into preheating device 8, is preheated to 170 DEG C of continuous inputs
Liquid phase oxidation reaction device 17 (horizontal reacting kettle), the CO that pre- thermal decomposition is produced2Gas inputs carburizing reagent after water removal, compression
Device 35 is used for carburizing reagent；
Liquid phase oxidation reaction device 17 (horizontal reacting kettle) interior 280 DEG C of reaction material liquid temperature is controlled, apparatus of oxygen supply 12 is to liquid
The uniform oxygen that is passed through maintains stagnation pressure 6.5MPa in phase oxidation reaction unit 17 (horizontal reacting kettle), and steam input first is dense in exhaust
The enrichment facility 46 of compression apparatus 30 and second is concentrated for rear end feed liquid, and carbon dioxide input carbonization after water removal, compression is anti-
Answer device 35 be used for be used for carburizing reagent；
Control (horizontal reacting kettle) the discharging flow 3.5m of liquid phase oxidation reaction device 173/ h continuous discharges, reaction material liquid is led to
Cross flash distillation plant (level Four flash tank) step by step cool, be depressured, final stage flash tank out-feed liquid temperature, which is down to after 120 DEG C, enters drop
Middle benefit gas turn trough；
With pump will cool groove in feed liquid squeeze into the first separator 26 (vertical board and frame machine), filter to isolate rich siderochrome slag from
Rich siderochrome slag outlet 27, obtains Na2CrO4Content is 473.7g/L chromium acid sodium solution, and Cr conversion ratios are 93.3% in ferrochrome, are washed
The wash water for washing rich siderochrome slag can be used for front end to be beaten the dispensing of tank 5；
Obtained chromium acid sodium solution squeezes into carbonizing plant with the 4th delivery pump after being concentrated through the first enrichment facility 30 and carries out carbon
Change, steam used by the first enrichment facility is produced all from front end liquid phase oxidation reaction device 17 (horizontal reacting kettle) oxidation reaction
CO used in the indirect steam that raw steam and flash distillation plant 21 are produced, carbonizing plant 352It all is from front end preheating device 8 pre-
The CO that thermal decomposition and the oxidation reaction of liquid phase oxidation device 17 are produced2, the feed liquid after carbonization passes through the (vertical board of the first separator 39
Frame machine) it is filtrated to get the carbodiimide solution that acidification rate is 94.6%, carbon of the sodium acid carbonate containing chromium isolated from the second separator 39
Sour hydrogen sodium outlet 41 is discharged, and the sodium acid carbonate entrance 1 that sodium acid carbonate containing chromium is delivered to mashing tank 5 is used as into original by pipeline
Material；
Carbodiimide solution input electrolytic cell is acidified, and acidification rate brings up to 100.5%, and acidifying solution is dense through the second enrichment facility 46
Contracting, the crystallisation by cooling of equipment of crystallisation by cooling 51, obtained crystal solution deviate from mother liquor by centrifugal device 54 and obtain sodium dichromate, sampled
Detect Na in this obtained sodium dichromate product2Cr2O7·H2O content 99.64%, SO4 2-Content 0.16%, Cl-Content is
0.06%.
In another embodiment, the soda ash for being 99% by ferrochrome that Cr containing simple substance is 68%, content, content are 89%
The sodium acid carbonate containing chromium that is obtained from the second separator 39, the wash water containing chromium from the rich siderochrome slag of washing are by mass fraction 1：
0.48：1.42：3.07 ratios are added in mashing tank 5 and are configured to mixed slurry；
Mixed slurry is pressed into 5m with the first delivery pump 73/ h continuously squeezes into preheating device 8, is preheated to 150 DEG C of continuous input liquid
Phase oxidation reaction unit 17 (oxidizing reactor group), the CO that pre- thermal decomposition is produced2Gas inputs carburizing reagent after water removal, compression
Device 35 is used for carburizing reagent；
Liquid phase oxidation reaction device 17 (horizontal reacting kettle) interior 260 DEG C of reaction material liquid temperature is controlled, apparatus of oxygen supply 12 is to liquid
The uniform oxygen that is passed through maintains stagnation pressure 5.5MPa in phase oxidation reaction unit 17 (oxidizing reactor group), steam input first in exhaust
The enrichment facility 46 of enrichment facility 30 and second is concentrated for rear end feed liquid, and carbon dioxide is inputted after water removal, compression and is carbonized
Reaction unit 35 is used for carburizing reagent；
Control (oxidizing reactor group) the discharging flow 5m of liquid phase oxidation reaction device 173/ h continuous discharges, reaction material liquid is led to
Cross flash distillation plant (level Four flash tank) step by step cool, be depressured, final stage flash tank out-feed liquid temperature, which is down to after 100 DEG C, enters drop
Middle benefit gas turn trough；
With pump will cool groove in feed liquid squeeze into the first separator 26 (vertical board and frame machine), filter to isolate rich siderochrome slag from
Rich siderochrome slag outlet 27, obtains Na2CrO4Content is 451.9g/L chromium acid sodium solution, and Cr conversion ratios are 91.3% in ferrochrome, are washed
The wash water for washing rich siderochrome slag can be used for front end to be beaten the dispensing of tank 5；
Obtained chromium acid sodium solution squeezes into carbonizing plant with the 4th delivery pump after being concentrated through the first enrichment facility 30 and carries out carbon
Change, steam used by the first enrichment facility is all from front end liquid phase oxidation reaction device 17 (oxidizing reactor group) oxidation reaction
CO used in the indirect steam that the steam and flash distillation plant 21 of generation are produced, carbonizing plant 352It all is from front end preheating device 8
The CO that pre- thermal decomposition and liquid phase oxidation device 17 (oxidizing reactor group) oxidation reaction are produced2, the feed liquid after carbonization passes through first
Separator 39 (vertical board and frame machine) is filtrated to get the carbodiimide solution that acidification rate is 91.8%, and the sodium acid carbonate containing chromium isolated is from the
The sodium acid carbonate outlet 41 of two separators 39 is discharged, and sodium acid carbonate containing chromium is delivered to the carbonic acid for being beaten tank 5 by pipeline
Hydrogen sodium entrance 1 is used as raw material；
Carbodiimide solution input electrolytic cell is acidified, and acidification rate brings up to 100.5%, and acidifying solution is dense through the second enrichment facility 46
Contracting, the crystallisation by cooling of equipment of crystallisation by cooling 51, obtained crystal solution deviate from mother liquor by centrifugal device 54 and obtain sodium dichromate, sampled
Detect Na in this obtained sodium dichromate product2Cr2O7·H2O content 99.71%, SO4 2-Content 0.15%, Cl-Content is
0.05%.
Number of devices and treatment scale described herein are the explanations for simplifying the present invention.To the present invention efficiently from
It is apparent to one skilled in the art that circulation wet method, which continuously prepares the systematic difference of sodium dichromate, modifications and variations,
's.
Although embodiment of the present invention is disclosed as above, it is not restricted in specification and embodiment listed
With it can be applied to various suitable the field of the invention completely, can be easily for those skilled in the art
Other modification is realized, therefore under the universal limited without departing substantially from claim and equivalency range, the present invention is not limited
In specific details and shown here as the legend with description.
Claims (8)
1. the system that a kind of high-efficiency self-circulation wet method continuously prepares sodium dichromate, it is characterised in that including：
Tank is beaten, the feeding mouth of input oxide spinel hydrogen sodium, ferrochrome powder, sodium carbonate and water is provided with；
Mashing tank is sequentially connected the first delivery pump, preheating device, liquid phase oxidation reaction device, flash distillation dress by feed liquid conveyance conduit
Put, the first separator, the first enrichment facility, carbonizing plant, the second separator, electrolytic cell, the second enrichment facility, cooling knot
Brilliant device and centrifugal device；
Apparatus of oxygen supply, it is connected with the liquid phase oxidation reaction device by pipeline；For to the liquid phase oxidation reaction device
It is passed through oxygen；
Wherein, the CO that pre- thermal decomposition is produced in the preheating device2, the CO of generation is aoxidized in liquid phase oxidation reaction device2With
The steam produced in steam and flash distillation plant is delivered to the first enrichment facility by gas transmission pipeline and the second concentration is filled
Put, steam is concentrated for feed liquid；CO2Gas is exported and passed through from the blowing mouth of the first enrichment facility and the second enrichment facility respectively
Freeze drier water removal, CO2The carbonizing plant is inputted after compressor compresses is used for carburizing reagent；In second separator
Isolated sodium acid carbonate containing chromium can be used as dispensing by pipeline to the feeding mouth for being beaten tank.
2. the system that high-efficiency self-circulation wet method as claimed in claim 1 continuously prepares sodium dichromate, it is characterised in that the mashing
The feeding mouth of tank has four, respectively sodium acid carbonate entrance, ferrochrome powder entrance, sodium carbonate entrance and water inlet.
3. the system that high-efficiency self-circulation wet method as claimed in claim 1 continuously prepares sodium dichromate, it is characterised in that the oxygen supply
Device include oxygen air separation unit, oxygen compressor and oxygen surge tank, oxygen compressor respectively with the oxygen air separation unit
Connected with oxygen surge tank, the oxygen surge tank passes through pipeline communication with the liquid phase oxidation reaction device.
4. the system that high-efficiency self-circulation wet method as claimed in claim 1 continuously prepares sodium dichromate, it is characterised in that described first
It is provided with enrichment facility on the first enrichment facility steam drain, second enrichment facility and is provided with the second enrichment facility steam discharge
Mouthful.
5. the system that high-efficiency self-circulation wet method as claimed in claim 1 continuously prepares sodium dichromate, it is characterised in that described first
Separator and the second separator are vertical automatic plate frame press filter.
6. the system that high-efficiency self-circulation wet method as claimed in claim 1 continuously prepares sodium dichromate, it is characterised in that the preheating
The thermometer for detecting temperature in preheating device is provided with device.
7. the system that high-efficiency self-circulation wet method as claimed in claim 1 continuously prepares sodium dichromate, it is characterised in that the flash distillation
Device is level Four flash tank.
8. the system that high-efficiency self-circulation wet method as claimed in claim 1 continuously prepares sodium dichromate, it is characterised in that the liquid phase
The second delivery pump is connected on feed liquid conveyance conduit between oxidation reaction apparatus and flash distillation plant；The flash distillation plant and first point
From the 3rd delivery pump of connection on the feed liquid conveyance conduit between device；Feed liquid between first enrichment facility and carbonizing plant
The 4th delivery pump is connected on conveyance conduit；Is connected on feed liquid conveyance conduit between the carbonizing plant and the second separator
Five delivery pumps；The 6th delivery pump is connected on feed liquid conveyance conduit between the electrolytic cell and the second enrichment facility；Described second
The 7th delivery pump is connected on feed liquid conveyance conduit between enrichment facility and equipment of crystallisation by cooling；The equipment of crystallisation by cooling with from
The 8th delivery pump is connected on feed liquid conveyance conduit between center device.
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| CN108101109A (en) * | 2017-12-22 | 2018-06-01 | 四川省银河化学股份有限公司 | A kind of sodium, carbon, the system of recycle heat system production chromic salts series of products |
| CN110394138A (en) * | 2019-08-27 | 2019-11-01 | 青海省博鸿化工科技股份有限公司 | A kind of continuous reaction apparatus and application thereof |
| CN110482605B (en) * | 2019-08-29 | 2021-08-03 | 昆明理工大学 | Method and device for preparing sodium bichromate by taking chromite as raw material in one step |
| CN113860356B (en) * | 2021-09-30 | 2023-10-31 | 沈阳工业大学 | Device and method for producing nano zinc oxide based on resource utilization |
| CN113683103B (en) * | 2021-09-30 | 2023-11-07 | 沈阳工业大学 | Light magnesium carbonate production device and method based on resource utilization |
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| CN103193271A (en) * | 2013-04-02 | 2013-07-10 | 四川省银河化学股份有限公司 | Method for producing high-quality sodium bichromate |
| CN103446776A (en) * | 2013-07-24 | 2013-12-18 | 深圳市捷晶能源科技有限公司 | Sodium bichromate concentration and crystallization equipment and technology |
| CN205023875U (en) * | 2015-09-15 | 2016-02-10 | 四川省银河化学股份有限公司 | System for sodium dichromate is prepared in succession to high -efficient self -loopa wet process |
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| JPS56139103A (en) * | 1980-03-31 | 1981-10-30 | Yoshio Aoyama | Crystallization of purified crystal |
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|---|---|---|---|---|
| CN103193271A (en) * | 2013-04-02 | 2013-07-10 | 四川省银河化学股份有限公司 | Method for producing high-quality sodium bichromate |
| CN103446776A (en) * | 2013-07-24 | 2013-12-18 | 深圳市捷晶能源科技有限公司 | Sodium bichromate concentration and crystallization equipment and technology |
| CN205023875U (en) * | 2015-09-15 | 2016-02-10 | 四川省银河化学股份有限公司 | System for sodium dichromate is prepared in succession to high -efficient self -loopa wet process |
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Denomination of invention: A system for continuous preparation of sodium jarosite by high efficiency self circulation wet method Effective date of registration: 20220413 Granted publication date: 20170711 Pledgee: China Construction Bank Corporation Mianyang Branch Pledgor: SICHUAN YINHE CHEMICAL Co.,Ltd. Registration number: Y2022980004215 |
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