CN109942013A - A kind of technique of industrial production alchlor - Google Patents
A kind of technique of industrial production alchlor Download PDFInfo
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- CN109942013A CN109942013A CN201910395285.6A CN201910395285A CN109942013A CN 109942013 A CN109942013 A CN 109942013A CN 201910395285 A CN201910395285 A CN 201910395285A CN 109942013 A CN109942013 A CN 109942013A
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Abstract
A kind of technique of industrial production alchlor is by induction furnace, the chlorination furnace of sieve plate containing chlorine and scum pipe, aluminium powder feeding chamber, three sections of concatenated chilling collets and the three alchlor product feed bins coupled, chlorination tube, offgas duct, cyclone separator, vibrator is formed, reaction raw materials aluminium oxide, petroleum coke self-inductance enters chlorination furnace after should heating stove heating, reaction raw materials aluminium powder enters chlorination furnace from aluminium powder feeding chamber, chlorine is entered from chlorination tube by chlorination furnace bottom, after chlorination furnace extraction plate is uniformly distributed, so that aluminium oxide, petroleum coke, aluminium powder is in fluidized state in chlorination furnace, reaction generates alchlor at high temperature, the closed alchlor product for collecting different size is distinguished by chilling, clinker is discharged from chlorination furnace bottom in chlorination furnace, tail gas passes through three-level spray-absorption and comprehensively utilizes.
Description
Technical field
The invention belongs to inorganic fine powder body material fields, and in particular to a kind of technique of industrial production alchlor.
Background technique
Alchlor is a kind of important inorganic chemical, and industrial goods are yellowish coloured particles or powder, phase due to containing green
To 2.44 grams of density (25 DEG C) per cubic centimeter, 1.23 grams of apparent density per cubic centimeter, 190 DEG C of fusing point (0.25MPa), inhales
It is aqueous strong, it easily deliquesces, dew empties hygroscopic decomposition in gas and generates hydrogen chloride, meets water or steam hydrolysis explosive, has strong
Corrosivity, alchlor are widely used in fields such as petrochemical industries.
It is anti-to be put into chlorination that is, by aluminium ingot heating melting using aluminium ingot fusion method for domestic production alchlor major part producer
It answers in furnace, with the chlorine reaction being passed through, is distilled, condense and alchlor is made.Reaction heat when aluminium ingot is individually reacted with chlorine
895.5KJ/mol, is strong exothermal reaction, and it is anti-with chlorine to greatly exceed aluminium ingot more than more than 1,000 degrees Celsius for chlorination in-furnace temperature
The optimization reaction temperature answered, while the heatproof of chlorination furnace equipment material is also a big problem.It is so limited, at present industrial production
In, it is typically only capable to be arranged small-sized chlorination furnace to control exothermic heat of reaction amount, by natural environment cooling and heat dissipation, maximum production capacity is only
1.2 ton/days, it is unfavorable for device enlargement, and execute-in-place bad environments.
Domestic small part enterprise uses alumina method, and roaster is added according to a certain ratio with alumdum and petroleum coke and is roasted
It burns, the material being fired and the chlorine reaction being passed through, purified, cooling, crystallization is made.Although aluminium oxide, petroleum coke and chlorine
Though reaction is exothermic reaction, it is not enough to maintaining reaction temperature, it must external heating.Either charging preheating in this way, or reaction
Heating all expends a large amount of energy, and heating temperature generally reaches 1000 DEG C or more, and the high requirements on the equipment, investment is greatly.
No matter which kind of above-mentioned technique, gaseous aluminum trichloride is all mingled with raw material, reactant enters trap together, by fixed
Phase taps trap or the cooling progress blanking of crystallizer, gaseous aluminum trichloride are captured together with impurity, and product quality is not protected
Barrier.In view of the industrial problem above of existing production alchlor, the present invention proposes to use the chlorination furnace of lower dreg discharging, not instead
The raw material answered, large granular impurity are from chlorination furnace lower part just by timely discharge system, and reaction gas is by cyclone dust collectors to divide
Quencher is entered back into after separating out the impurity or unreacting material ultra-fine grain of gas entrainment, to guarantee that gaseous aluminum trichloride is relatively pure
Only.Further, the present invention is high boiling by what is carried secretly in gaseous aluminum trichloride by the way that concatenated three sections of chilling collection devices are arranged
Object, low-boiling-point substance alchlor collect respectively, middle section chilling collection device obtains high-purity grade of alchlor product, avoids anhydrous three
Aluminium chloride product and the humid air contact moisture absorption lead to the problem of hydrochloric acid mist, substantially improve alchlor product packaging environment, really
It is nonhygroscopic to protect product, in this way to provide a kind of new method of the technique of industrial production alchlor.
Summary of the invention
The purpose of the present invention: the defect of system and device and technology for existing industrial production alchlor provides
A kind of new method of the technique of industrial production alchlor.
Technical scheme is as follows:
Chlorination furnace, the aluminium powder of a kind of technique of industrial production alchlor by induction furnace, sieve plate containing chlorine and scum pipe
Feeding chamber, three sections of concatenated chilling collets and the three alchlor product feed bins coupled, chlorination tube, offgas duct, whirlwind point
It is formed from device, vibrator, reaction raw materials aluminium oxide, petroleum coke self-inductance enter chlorination furnace after should heating stove heating, and reaction is former
Expect that aluminium powder enters chlorination furnace from aluminium powder feeding chamber, chlorine is entered from chlorination tube by chlorination furnace bottom, equal through chlorination furnace extraction plate
After even distribution, so that aluminium oxide, petroleum coke, aluminium powder are in fluidized state in chlorination furnace, reaction generates alchlor at high temperature,
The closed alchlor product for collecting different size is distinguished by chilling, and clinker is discharged from chlorination furnace bottom in chlorination furnace, tail gas
By three-level spray-absorption and comprehensively utilize, specific as follows:
A, it preheats: by the mixed of the reaction raw materials aluminium oxide of 150 ~ 170 parts of weight and the reaction raw materials petroleum coke of 75 ~ 85 parts of weight
Object is closed, is heated to 800 ~ 1000 DEG C by induction furnace；The reaction raw materials aluminum oxide grain size is 60 ~ 150 μm, petroleum coke
Granularity is 100 ~ 150 μm；
B, monochlorinated: first lead to chlorine, and control chlorine in chlorination furnace in 0.1 ~ 0.55m/s of flow velocity, then will warm up 800
~ 1000 DEG C of aluminium oxide and the hot mixture of petroleum coke are continuously put into chlorination furnace, pass through sieve plate with from chlorination furnace bottom
The reaction raw materials chlorine of 320 ~ 340 parts of weight after being uniformly distributed carries out fluidised reduction chlorination；
C, when chlorination furnace case temperature reaches 450 DEG C, three feed openings of aluminium powder point joint chlorination: are entered into chlorine from different location
Change furnace investment chlorination furnace and carries out joint chlorination, while the corresponding specific gravity for reducing aluminium oxide and petroleum coke, it is final to control in chlorination furnace
25 ~ 30 parts of 105 ~ 115 parts of weight of aluminium oxide, 52 ~ 57 parts of weight of petroleum coke, 320 ~ 340 parts of weight of chlorine, aluminium powder weight, reaction
Joint chlorination is carried out at 800 ~ 850 DEG C of temperature；The reaction raw materials aluminum powder particle size is 3 ~ 5mm；
D, thermal balance: after entering joint chlorination process, as system investment aluminium powder gradually increases, induction furnace gradually drops
Low heating power, to maintain in chlorination furnace reaction temperature at 800 ~ 850 DEG C, when aluminium powder and chlorine thermal discharge and aluminium oxide and chlorine
When reduction calorific requirement reaches balance, induction furnace stops heating, and the addition of each reaction raw materials is controlled by DCS system, with
Ensure the thermal balance of fluidization reactiveness and reaction system in chlorination furnace and the stabilization of reaction temperature simultaneously, allows entire technique
System stable operation；
E, three sections of adverse current chillings are collected: reaction product gaseous aluminum trichloride removes surpassing for entrained in gas by cyclone separator
After fine powder impurity, enters back into three sections of concatenated chilling collets and adverse current cooling water exchanges heat, control its different cooling temperature, then
The closed alchlor collected containing high-boiling components, high-purity grade of alchlor are distinguished, containing low-boiling-point substance by three alchlor feed bins
Alchlor, is convenient for the grading of alchlor in this way, and aluminum trichloride (anhydrous) product is avoided to contact suction with humid air
Tide leads to the problem of hydrochloric acid mist, substantially improves alchlor product packaging environment, it is ensured that alchlor product is nonhygroscopic；
F, deslagging and vent gas treatment: clinker is discharged from chlorination furnace bottom in chlorination furnace, and tail gas enters the absorption of three-level spray absorber,
Respectively one-stage water wash removes alchlor or other impurity, generates alchlor aqueous solution and is sent to aluminium polychloride workshop, second level
Water spray absorbs hydrochloric acid mist, generates hydrochloric acid and is sent to aluminium polychloride workshop, three-level Alkali absorption chlorine generates sodium hypochlorite and enters
Sewage treatment plant's integrated treatment.
Further, the induction furnace drive when as aluminium oxide, the heat effect of petroleum coke, normal
It only uses as charging surge bunker after operation, such as the more situation of moisture in aluminium oxide, petroleum coke, is removed by electrical induction
Moisture therein, to avoid the influence to alchlor product quality.
Further, the chlorination furnace is the chlorination furnace for the lower dreg discharging formula that sieve plate is arranged at bottom, and first leads to chlorine, adds again
Aoxidize reactive aluminum for a period of time after, then plus aluminium powder reaction, in this way with ensure chlorine by sieve plate arrangement uniformly and make chlorination
Aluminium oxide, aluminium powder and chlorine in furnace are in fluidization reactiveness.
Further, the chlorination furnace is the regular deslagging of bottom, so that ferric trichloride, heavy metal etc. in chlorination furnace
Impurity and unreacted aluminium oxide etc. are discharged without bringing chilling collector by gaseous aluminum trichloride, to ensure that alchlor produces
Quality.
Further, the reaction speed of aluminium powder and chlorine is very fast, and the reaction speed of aluminium oxide and chlorine is slower, therefore chlorination
The ratio of height to diameter of furnace is larger, and reaction temperature gradually decreases from bottom to top, therefore by three aluminium powder feed openings to chlorination furnace upper, middle and lower
Duan Wendu is controlled, it is ensured that aluminium oxide good reduction chlorination when thermal balance, middle upper section temperature controls respectively under chlorination furnace
840~850℃、830~840℃、820~830℃。
Further, reaction product gaseous aluminum trichloride, which enters three sections of concatenated chilling collet adverse current chilling steps, is: 10 ~
30 DEG C of cooling waters are introduced into third chilling collet and 200 DEG C of gaseous aluminum trichloride counterflow heat exchanges, and then 50 DEG C of water outlet enters the
The gaseous aluminum trichloride of two chilling collets and 280 DEG C carries out counterflow heat exchange, then 70 DEG C of water outlet enter the first chilling collet with
360 DEG C of gaseous aluminum trichloride counterflow heat exchange；Due to carrying out big three sections of counterflow heat exchanges of temperature difference cooling temperature different from control, the
One, two, three alchlor feed bins distinguish it is closed collect the alchlor of such as ferric trichloride containing high-boiling components, high-purity grade of alchlor,
Alchlor containing low-boiling-point substance such as silicon tetrachloride and titanium tetrachloride, in this way to ensure to acquire high-purity tri-chlorination in the second feed bin
Aluminium product, the first, second and third alchlor feed bin alchlor product crystal granularity is respectively 2 ~ 5mm, 3 ~ 6mm, 4 ~ 8mm.
Further, when entire process system starts operation, induction furnace preheats the initial temperature of aluminium oxide, petroleum coke
Degree is 900 ~ 1000 DEG C, is higher than 800 ~ 850 DEG C of normal buffer system temperature, which will be used for the shell liter of chlorination furnace
Temperature；Chlorination furnace is passed through chlorine, and the induction furnace aluminium oxide that feeds intake carries out buffer system, this reaction last it is longer, due to chlorine
Change furnace shell heat absorption, the unreacted chlorine of system may be more, and subsequent exhaust system must fully absorb；Furnace shell to be chlorinated reaches
When to 400 ~ 450 DEG C, gradually puts into aluminium powder and carry out joint chlorination, accelerate chlorination furnace heating, until chlorination furnace case temperature reaches
800 ~ 850 DEG C, induction furnace stops heating, by DCS system control device heat balance.
Further, entire process system is all closed, induction furnace (and feeding chamber of aluminium oxide and petroleum coke),
Aluminium powder feeding chamber, alchlor feed bin are all made of nitrogen-sealed or logical nitrogen protection, are on the one hand adhered to pipeline by nitrogen purging
On solid powder, on the other hand reduce oxygen enter with aluminium occur side reaction, also assure that chlorine does not leak, to guarantee system
Safe and environment-friendly, efficient operation.
Further, entire process system is stopped operation to be divided to and be stopped in emergency with two kinds of situations of Programmed Stop: when stopping in emergency
Cut off the logical material valve of all raw feed materials valves, chlorine immediately by safety system, while nitrogen enters from chlorination tube, continues to
Fluidized state in chlorination furnace, it is ensured that chlorination furnace, quenching apparatus, tail gas unit cooling, while chlorine in exchange system makes its quilt
Subsequent exhaust system absorbs, and chlorinated exhaust system must be equipped with emergency power supply, it is ensured that system safety；It, should be gradually when Programmed Stop
The additional amount of aluminium oxide, petroleum coke is reduced until complete stopping charging, keeps it complete with chlorine reaction as far as possible, reduce chlorine after parking
Change the inventory in furnace, in order to overhaul and handle；Due to being necessary to ensure that goods fluid state in chlorination tower, system are unreacted
Chlorine may be more, and subsequent exhaust system must fully absorb；The decrement of aluminium powder is controlled by DCS system, with putting by aluminium powder
Heat promotes the complete reaction of aluminium oxide, petroleum coke, and remaining aluminium powder influences smaller when driving next time；It stops the later period, stops
Chlorine is passed through, and is changed to nitrogen heat dissipation and displacement.
Beneficial effects of the present invention:
(1) by induction furnace preheating material, the pollution with generations such as fuel such as diesel oil, coal is avoided, it is easy to operate,
Convenient for employee's operation, and induction furnace is convenient for temperature automation control, and when driving as aluminium oxide, petroleum coke
Heat effect is only used as charging surge bunker after normal operation, such as the more situation of moisture in aluminium oxide, petroleum coke, is led to
It crosses electrical induction and removes moisture therein, to avoid the influence to alchlor product quality；
(2) by solving aluminium powder/aluminium ingot method using the exothermic heat of reaction of aluminium powder and chlorine as the endothermic heat of reaction of aluminium oxide and chlorine
Device can not radiate in time because highly exothermic limits the enlarged problem of chlorination furnace apparatus, while not needing the feelings of external heat source
It maintains aluminium oxide and chlorine reaction to need heat under condition, kills two birds with one stone；
(3) combination settings chlorination furnace lower dreg discharging formula and upper cyclone separator, by inferior bulky grain raw material and silica, dioxy
Change titanium, the impurity such as manganese oxide from lower row mouthful discharge, but will fluidize the impurity carried secretly in alchlor gas vent in chlorination furnace or
Unreacting material ultra-fine grain is through cyclonic separation and returns to fluidisation chlorination furnace, it is ensured that the quality of chlorination top gas state alchlor
Yield and product purity；
(4) it is radiated by setting chilling collet, aluminum trichloride (anhydrous) is avoided to contact with humid air, greatly reduce existing cooling receipts
Acquisition means natural heat dissipation and execute-in-place environment is poor, avoids the alchlor product moisture absorption and leading to the problem of hydrochloric acid mist；
(5) by three sections of collections of setting, alchlor product quality has further been segmented, it is ensured that middle section alchlor can be made
For medical grade products, remaining is applied to different field, segments market convenient for enterprise according to the difference of dopant type, improves profit；
(6) entire process system is all closed, induction furnace (and aluminium oxide, petroleum coke feeding chamber), aluminium powder feeding chamber, three
Aluminium chloride feed bin is all made of nitrogen-sealed or logical nitrogen protection, on the one hand purges the solid powder being adhered on pipeline by nitrogen,
On the other hand reduce that oxygen enters and side reaction occurs for aluminium, it is ensured that chlorine does not leak, to ensure entire process unit and system
Safe and environment-friendly, efficient operation.
Detailed description of the invention
Fig. 1 is the system and device and artwork of industrial production alchlor, wherein 1 induction furnace (aluminium oxide, petroleum
Burnt feeding chamber), 2 chlorination furnaces, 3 aluminium powder feeding chambers, 4-1,4-2,4-3 be respectively the first, second and third chilling collet, 5-1,5-2,5-3
Respectively the first, second and third alchlor product feed bin, 6 chlorine sieve plates, 7 scum pipes, 8 chlorination tubes, 9 offgas ducts, 10 cyclonic separations
Device, 11-1,11-2,11-3 are respectively the first, second and third vibrator.
Specific embodiment
The invention will be further described with the following Examples.
Embodiment 1
A, preheat: by the granularity of 160 parts of weight be 60 ~ 150 μm reaction raw materials aluminium oxide and 100 ~ 150 μm of 80 parts of weight
Reaction raw materials petroleum coke, the premix feed bin that the band stirring with weighing apparatus is added in ingredient is carried out by respective weighing belt respectively, it is mixed
It closes object and quantifying feed is carried out to induction furnace by baiting valve, calculate electricity by two weighing belts and premix feed bin weighing instrument
The inlet amount of induction heater, premix feed bin and induction furnace and it is extraneous seal, and persistently lead to nitrogen, nitrogen is set when driving
It changes, nitrogen keeps certain pressure after driving, prevents chlorination furnace chlorine from returning and alters.Mixture is heated to 1000 by induction furnace
DEG C, it is contemplated that initial reaction stage, chlorination furnace integrally need to absorb heat, and unreacted chlorine can also take away heat, properly increase mixing
Object temperature helps to shorten the time of driving, and is rapidly achieved stable monochlorinated.The temperature of induction furnace is by its included control
System processed is completed, and signal is transmitted to present apparatus DCS system.
B, monochlorinated: chlorination furnace first completes nitrogen displacement before dosing, prevents oxygen, moisture from entering system, generates secondary
Reaction and generation corrosive liquids, polluted product and corrosion follow-up equipment；Subsequent quenching apparatus is run, subsequent exhaust system is improved
Load, mainly raising alkali internal circulating load and alkali concentration, it is ensured that the absorption of chlorine when driving；It is passed through and passes through sieve from chlorination furnace bottom
Plate be uniformly distributed after 340 weight chlorine, chlorine in chlorination furnace in flow velocity 0.5m/s, by the heat of aluminium oxide and petroleum coke
State mixture is continuously put into chlorination furnace, carries out fluidised reduction chlorination；Due to chlorination furnace bulky, examined for investment
Consider, do not take chlorination furnace body heating device, therefore the monochlorinated time is longer, and is carried out along with reaction, induction furnace
Control mixture temperature is reduced to 950 DEG C.
C, joint chlorination: by the reaction raw materials aluminium powder of 3 ~ 5mm of 27 parts of weight, ingredient is carried out by weighing belt, band title is added
The aluminium powder feeding chamber of treasure, calculates the inventory of aluminium powder by weighing belt and aluminium powder feeding chamber weighing instrument, aluminium powder feeding chamber and outer
Boundary sealing, and persistently lead to nitrogen, into aluminium powder before nitrogen replace, into aluminium powder after nitrogen keep certain pressure, to aluminium powder be added chlorination furnace
Pipeline is purged, and prevents from blocking, and is also avoided chlorine from returning and is altered, the step by step input aluminium powder when chlorination furnace case temperature reaches 450 DEG C
Start joint chlorination, aluminium powder point three feed openings are put into from different location, inventory gradually increases, aluminium oxide and petroleum coke
Feeding quantity gradually decreases, and chlorination furnace carries out joint chlorination；The aluminium powder investment of 27 parts of weight gradually increases, and increment control algorithm exists
5kg/min, corresponding oxidation aluminium are reduced to 10kg/min, and petroleum coke is reduced to 5k/min, which is the automatic adjustment of DCS ratio.
The control of chlorination furnace reaction temperature is paid close attention to when joint chlorination at 800 ~ 850 DEG C and avoids larger fluctuation, the too low Shi Yingti of temperature
High electric induction furnace output mixture temperature should reduce electric induction furnace output mixture temperature when the temperature is excessively high, should reduce when necessary
Chlorine intake simultaneously supplements nitrogen maintenance fluidisation state.
D, thermal balance: enter joint chlorination process after, with system put into aluminium powder gradually increase, induction furnace by
Step reduces heating power, and reaction temperature is at 800 ~ 850 DEG C to maintain in chlorination furnace, in 107 parts of weight of aluminium oxide, 54 parts of petroleum coke
Chlorination furnace reaction system reaches heat balance, aluminium powder and chlorine thermal discharge when weight, 340 parts of 27 parts of weight of aluminium powder, chlorine weight
When reaching balance with aluminium oxide and chlorine reduction calorific requirement, induction furnace stops heating, is controlled by DCS system dynamic each
The addition of reaction raw materials, to ensure the thermal balance and reaction temperature of fluidization reactiveness and reaction system in chlorination furnace simultaneously
Stabilization, allow entire process system stable operation；By three aluminium powder feed openings, chlorination furnace upper, middle and lower section temperature is controlled
System, it is ensured that aluminium oxide good reduction chlorization condition when thermal balance, middle upper section temperature is controlled respectively 840 ~ 850 under chlorination furnace
℃、830~840℃、820~830℃。
E, three sections of adverse current chillings are collected: reaction product gaseous aluminum trichloride enters three sections of concatenated chilling collet adverse current chillings
Step is: 10 ~ 30 DEG C of cooling waters are introduced into third chilling collet and 200 DEG C of gaseous aluminum trichloride counterflow heat exchanges, and then 50 DEG C
Water outlet enters the second chilling collet and 280 DEG C of gaseous aluminum trichloride carries out counterflow heat exchange, then 70 DEG C of water outlet enters first suddenly
Cold collet and 360 DEG C of gaseous aluminum trichloride counterflow heat exchange；Due to carrying out cold different from control of big three sections of counterflow heat exchanges of the temperature difference
But temperature, the first, second and third alchlor feed bin distinguish closed alchlor, the Gao Chunji for collecting such as ferric trichloride containing high-boiling components
Alchlor, the alchlor containing low-boiling-point substance such as silicon tetrachloride and titanium tetrachloride ensure to acquire in the second feed bin so high-purity
Alchlor product, the first, second and third alchlor feed bin alchlor product crystal granularity is respectively 2 ~ 5mm, 3 ~ 6mm, 4
~8mm。
F, deslagging and vent gas treatment: clinker is discharged from chlorination furnace bottom in chlorination furnace, and tail gas enters three-level spray absorber
It absorbs, respectively one-stage water wash removes alchlor or other impurity, and it generates alchlor aqueous solution and is sent to aluminium polychloride workshop,
Second level water spray absorbs hydrochloric acid mist, generates hydrochloric acid and is sent to aluminium polychloride workshop, three-level Alkali absorption chlorine generates sodium hypochlorite
Into sewage treatment plant's integrated treatment.
Comparative example 2
Difference from Example 1 is to be added without aluminium powder, directly uses aluminium oxide, the independent chlorination of petroleum coke, first electric induction
Heating furnace need to be heated always, alchlor power consumption about 1500kw per ton；Secondly three sections of temperature difference of upper, middle and lower are larger in chlorination furnace,
The oxidation aluminium reducing chlorination residence time is longer, and not exclusively, chlorine cannot react completely for reaction, increases subsequent chilling collection, tail gas
The load of processing.
Comparative example 3
Difference from Example 1 is to be added without aluminium oxide, petroleum coke, using the independent chlorination of aluminium powder, since reaction heat compares
Greatly, exothermic heat of reaction is relatively more, and without aluminium oxide, the endothermic equilibrium of petroleum coke, reaction temperature is too high, and chlorination furnace material is difficult to
It bears；Secondly the independent chlorination of aluminium powder has been melted before reaching 800 DEG C of reaction temperatures due to 660 DEG C of fusing point of aluminium, can not
Fluidization reaction is realized in chlorination furnace.
Comparative example 4
Difference from Example 1 is that aluminum powder particle size is greater than 5mm, reaction speed too small with chlorine reaction gross contact area
It is low, it is difficult to realize the fluidization reaction in chlorination furnace.
Comparative example 5
Difference from Example 1 is that aluminum powder particle size is less than 3mm, and crushing is at high cost, and fine solid particle during charging
It is easy aggregation to explode, threatens safety in production.
Comparative example 6
It is air-cooled that difference from Example 1 is that chilling collector uses, and cooling effect is very poor, it is difficult to effective cooling gas trichlorine
Change aluminium is crystal product；Next is difficult to realize the counterflow heat exchange of the different temperature difference, it is difficult to control different cooling temperatures, also just be difficult to
Substandard alchlor product is collected respectively in three product feed bins.
Claims (9)
1. a kind of technique of industrial production alchlor, it is characterised in that: a kind of technique of industrial production alchlor
By the chlorination furnace of induction furnace, sieve plate containing chlorine and scum pipe, aluminium powder feeding chamber, three sections of concatenated chilling collets and joined
Three alchlor product feed bins, chlorination tube, offgas duct, cyclone separator, the vibrators connect are formed, reaction raw materials oxidation
Aluminium, petroleum coke self-inductance enter chlorination furnace after should heating stove heating, and reaction raw materials aluminium powder enters chlorination furnace, chlorine from aluminium powder feeding chamber
Gas is entered from chlorination tube by chlorination furnace bottom, after chlorination furnace extraction plate is uniformly distributed, so that aluminium oxide, petroleum coke, aluminium powder
It is in fluidized state in chlorination furnace, reaction generates alchlor at high temperature, distinguishes closed collection different size by chilling
Alchlor product, clinker is discharged from chlorination furnace bottom in chlorination furnace, and tail gas passes through three-level spray-absorption and comprehensively utilizes, specifically
It is as follows:
Preheating: by the mixing of the reaction raw materials aluminium oxide of 150 ~ 170 parts of weight and the reaction raw materials petroleum coke of 75 ~ 85 parts of weight
Object is heated to 800 ~ 1000 DEG C by induction furnace；The reaction raw materials aluminum oxide grain size is 60 ~ 150 μm, petroleum char particle
Degree is 100 ~ 150 μm；
It is monochlorinated: first lead to chlorine, and control chlorine in chlorination furnace in 0.1 ~ 0.55m/s of flow velocity, then will warm up 800 ~
1000 DEG C of aluminium oxide and the hot mixture of petroleum coke are continuously put into chlorination furnace, equal with sieve plate is passed through from chlorination furnace bottom
The reaction raw materials chlorine of 320 ~ 340 parts of weight after even distribution carries out fluidised reduction chlorination；
Joint chlorination: when chlorination furnace case temperature reaches 450 DEG C, three feed openings of aluminium powder point are entered into chlorination from different location
Furnace investment chlorination furnace carries out joint chlorination, while the corresponding specific gravity for reducing aluminium oxide and petroleum coke, final to control oxygen in chlorination furnace
Change 105 ~ 115 parts of weight of aluminium, 52 ~ 57 parts of weight of petroleum coke, 25 ~ 30 parts of 320 ~ 340 parts of weight of chlorine, aluminium powder weight, reaction temperature
Joint chlorination is carried out at 800 ~ 850 DEG C of degree；The reaction raw materials aluminum powder particle size is 3 ~ 5mm；
Thermal balance: after entering joint chlorination process, as system investment aluminium powder gradually increases, induction furnace, which gradually reduces, to be added
Thermal power, to maintain in chlorination furnace reaction temperature at 800 ~ 850 DEG C, when aluminium powder and chlorine thermal discharge and aluminium oxide and chlorine restore
When calorific requirement reaches balance, induction furnace stops heating, controls the addition of each reaction raw materials, by DCS system with simultaneously
Ensure the thermal balance of the fluidization reactiveness and reaction system in chlorination furnace and the stabilization of reaction temperature, allows entire process system
Stable operation；
Three sections of adverse current chillings are collected: reaction product gaseous aluminum trichloride by cyclone separator removing gas entrained with it is ultra-fine
After powder impurity, enters back into three sections of concatenated chilling collets and adverse current cooling water exchanges heat, control different cooling temperatures, then pass through
Three alchlor feed bins distinguish closed alchlor, high-purity grade alchlor, trichlorine containing low-boiling-point substance of the collection containing high-boiling components
Change aluminium, be convenient for the grading of alchlor in this way, and avoids aluminum trichloride (anhydrous) product and humid air from contacting the moisture absorption and produce
Raw hydrochloric acid mist problem, substantially improves alchlor product packaging environment, it is ensured that alchlor product is nonhygroscopic；
Deslagging and vent gas treatment: clinker is discharged from chlorination furnace bottom in chlorination furnace, and tail gas enters the absorption of three-level spray absorber, point
Not Wei one-stage water wash remove alchlor or other impurity, generate alchlor aqueous solution be sent to aluminium polychloride workshop, second level water
Spray-absorption hydrochloric acid mist generates hydrochloric acid and is sent to aluminium polychloride workshop, and three-level Alkali absorption chlorine generates sodium hypochlorite and enters dirt
Water treatment plant's integrated treatment.
2. a kind of technique of industrial production alchlor according to claim 1, it is characterised in that: the electric induction adds
Hot stove, as aluminium oxide, the heat effect of petroleum coke, is only used as charging surge bunker when driving after normal operation, in case of
The more situation of moisture in aluminium oxide, petroleum coke removes moisture therein by electrical induction, to avoid to alchlor product
The influence of quality.
3. a kind of technique of industrial production alchlor according to claim 1, it is characterised in that: the chlorination furnace is
The chlorination furnace of the lower dreg discharging formula of sieve plate is arranged at bottom, and first lead to chlorine, again oxygenation reactive aluminum for a period of time after, then plus aluminium powder it is anti-
It answers, in this way to ensure that chlorine is uniform by sieve plate arrangement and makes aluminium oxide, aluminium powder and chlorine in chlorination furnace in fluidization
Reactiveness.
4. a kind of technique of industrial production alchlor according to claim 1, it is characterised in that: the chlorination furnace is
The regular deslagging of bottom so that the impurity and unreacted aluminium oxide etc. such as ferric trichloride, heavy metal in chlorination furnace be discharged and
Chilling collector is not brought by gaseous aluminum trichloride, to ensure alchlor product quality.
5. a kind of technique of industrial production alchlor according to claim 1, it is characterised in that: aluminium powder and chlorine it is anti-
Fast speed is answered, and the reaction speed of aluminium oxide and chlorine is slower, therefore the ratio of height to diameter of chlorination furnace is larger, reaction temperature is from bottom to top
It gradually decreases, therefore chlorination furnace upper, middle and lower section temperature is controlled by three aluminium powder feed openings, it is ensured that aoxidized when thermal balance
The good reduction chlorination of aluminium, middle upper section temperature is controlled respectively at 840 ~ 850 DEG C, 830 ~ 840 DEG C, 820 ~ 830 DEG C under chlorination furnace.
6. a kind of technique of industrial production alchlor according to claim 1, it is characterised in that: reaction product gaseous state
Alchlor enters three sections of concatenated chilling collet adverse current chilling steps: 10 ~ 30 DEG C of cooling waters are introduced into third chilling collet
With 200 DEG C of gaseous aluminum trichloride counterflow heat exchanges, then 50 DEG C of water outlet enters the second chilling collet and 280 DEG C of gaseous state tri-chlorination
Aluminium carries out counterflow heat exchange, then 70 DEG C of water outlet enters the first chilling collet and 360 DEG C of gaseous aluminum trichloride counterflow heat exchange；By
In carrying out big three sections of counterflow heat exchanges of temperature difference cooling temperature different from control, the first, second and third alchlor feed bin distinguishes closed receipts
Collect the alchlor of such as ferric trichloride containing high-boiling components, high-purity grade of alchlor, containing low-boiling-point substance such as silicon tetrachloride and titanium tetrachloride
Alchlor ensures to acquire so high-purity alchlor product, the first, second and third alchlor feed bin three in the second feed bin
Aluminium chloride product crystal granularity is respectively 2 ~ 5mm, 3 ~ 6mm, 4 ~ 8mm.
7. a kind of technique of industrial production alchlor according to claim 1, it is characterised in that: entire process system is opened
When beginning operation, induction furnace preheats aluminium oxide, the initial temperature of petroleum coke is 900 ~ 1000 DEG C, is higher than normally monochlorinated anti-
800 ~ 850 DEG C of temperature are answered, which heats up the shell for being used for chlorination furnace；Chlorination furnace is passed through chlorine, induction furnace
The aluminium oxide that feeds intake carry out buffer system, this reaction last it is longer, due to chlorination furnace shell absorb heat, the unreacted chlorine of system can
Can be more, subsequent exhaust system must fully absorb；When furnace shell to be chlorinated reaches 400 ~ 450 DEG C, gradually puts into aluminium powder and carry out
Chlorination furnace heating is accelerated in joint chlorination, and until chlorination furnace case temperature reaches 800 ~ 850 DEG C, induction furnace stops heating,
By DCS system control device heat balance.
8. a kind of technique of industrial production alchlor according to claim 1, it is characterised in that: entire process system is complete
Portion's closing, induction furnace (and aluminium oxide, petroleum coke feeding chamber), aluminium powder feeding chamber, alchlor feed bin are all made of nitrogen
Sealing or logical nitrogen protection, on the one hand purge the solid powder being adhered on pipeline by nitrogen, on the other hand reduce oxygen and enter
Side reaction occurs with aluminium, also assures that chlorine does not leak, to guarantee safe and environment-friendly, the efficient operation of system.
9. a kind of technique of industrial production alchlor according to claim 1, it is characterised in that: entire process system stops
Only operation, which is divided to, stops in emergency and two kinds of situations of Programmed Stop: cutting off all raw materials immediately by safety system when stopping in emergency and supplies
Expect the logical material valve of valve, chlorine, while nitrogen enters from chlorination tube, continues to fluidized state in chlorination furnace, it is ensured that chlorination furnace, chilling
The cooling of device, tail gas unit, while chlorine in exchange system absorb it by subsequent exhaust system, and chlorinated exhaust system must
Emergency power supply must be equipped with, it is ensured that system safety；When Programmed Stop, the additional amount of aluminium oxide, petroleum coke should be gradually decreased until complete
Full cut-off only feeds, and keeps it complete with chlorine reaction as far as possible, the inventory in parking afterchlorinate furnace is reduced, in order to overhaul and locate
Reason；Due to being necessary to ensure that goods fluid state in chlorination tower, the unreacted chlorine of system may be more, and subsequent exhaust system is necessary
It fully absorbs；The decrement of aluminium powder is controlled by DCS system, to promote the complete reaction of aluminium oxide, petroleum coke by the heat release of aluminium powder,
Remaining aluminium powder influences smaller when driving next time；It stops the later period, stops chlorine and be passed through, be changed to nitrogen heat dissipation and displacement.
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| CN112933830A (en) * | 2021-01-30 | 2021-06-11 | 成都易态科技有限公司 | Heat exchange dust removal structure, heat exchange dust removal device and high-temperature dust-containing gas treatment method |
| CN113860338A (en) * | 2021-11-01 | 2021-12-31 | 上海翰军实验设备有限公司 | Preparation and purification device and method for high-purity anhydrous beryllium chloride |
| US11996281B1 (en) | 2023-06-07 | 2024-05-28 | Applied Materials, Inc. | System and method for introducing aluminum to an ion source |
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| CN104671268A (en) * | 2013-11-28 | 2015-06-03 | 常州校果信息服务有限公司 | Method for manufacturing aluminum trichloride from aluminum oxide |
| CN109231248A (en) * | 2018-11-27 | 2019-01-18 | 攀钢集团攀枝花钢铁研究院有限公司 | The method of carburizing chlorination production alchlor |
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