CN103274433A - Recovery method and device for bischofite dehydration assistant by double salt method - Google Patents
Recovery method and device for bischofite dehydration assistant by double salt method Download PDFInfo
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- CN103274433A CN103274433A CN2013101755979A CN201310175597A CN103274433A CN 103274433 A CN103274433 A CN 103274433A CN 2013101755979 A CN2013101755979 A CN 2013101755979A CN 201310175597 A CN201310175597 A CN 201310175597A CN 103274433 A CN103274433 A CN 103274433A
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Abstract
The invention discloses recovery method and device for a bischofite dehydration assistant by a double salt method, and mainly provides method and a device which can efficiently recover the dehydration assistant used in the process of preparing anhydrous magnesium chloride by dehydrating bischofite by the double salt method. The method comprises the following steps: firstly, introducing water vapor containing small amount of dehydration assistant volatilized in the low temperature dehydration stage of double salt in a dehydration furnace to a condensing tower to be condensed and cooled to recover the dehydration assistant; and then filtering white smoke which is not recovered in the condensing and cooling process by a membrane cloth bag to further recover the dehydration assistant. According to the method and device, the dehydration assistant is recovered by condensing, cooling and cloth bag filtering, the recovery rate reaches near 100%, and no white smoke is overflowed at the general outlet. Therefore, the method and the device have the advantages of environment friendliness, no pollution and high assistant recovery rate.
Description
Technical field
The present invention relates to the recovery field of chemical conditioner, be specifically related to recovery method and the device of double salt method dewatering bischofite auxiliary agent.
Background technology
Contain huge magnesium resource in seawater, the salt lake brine.Salt lake brine can obtain magnesium chloride hexahydrate after extracting Repone K easily, and purity reaches 98-99%.But 10 tons of magnesium chloride hexahydrate (MgCl of 1 ton of Repone K by-product of every production
26H
2O is commonly called as bischofite).Magnesium Chloride Anhydrous and then electrolysis are made in the dehydration of magnesium chloride hexahydrate or bittern, and to produce MAGNESIUM METAL be an important channel that utilizes the magnesium elements in magnesium chloride hexahydrate or the bittern.But dewatering bischofite is produced the Magnesium Chloride Anhydrous not a duck soup, is easy to be hydrolyzed into magnesium oxide when dewatering in air because of bischofite, and obtain Magnesium Chloride Anhydrous must be with protecting gas and chemical conditioner.Traditional industrialization dewatering is to utilize chlorine or hydrogenchloride to make protection gas or chlorination gas, but these gases are serious to equipment corrosion.With aniline hydrochloride (C
6H
5NH
2HCl) making the double salt method dewatering bischofite technology of dewatering agent, is to utilize aniline hydrochloride to replace chlorine or hydrogenchloride to make protection gas and chlorination gas, can alleviate the equipment corrosion problem greatly, and temperature of reaction (350 ℃) is lower.But when dewatering with the double salt method, must be with the chemical conditioner recycle and reuse, the height of the rate of recovery is directly connected to economy and the feasibility of this technology.
United States Patent (USP) [US3962408] has reported that the double salt method dewatering bischofite of making chemical conditioner with aniline hydrochloride, pyridine produces the reaction principle of Magnesium Chloride Anhydrous, but does not propose concrete recovery method and the equipment of chemical conditioner aniline hydrochloride.
Chinese patent [CN1944261] has been reported with aniline hydrochloride and the synthetic double salt of bischofite, sloughs crystal water and aniline hydrochloride by mist projection granulating, fluidized-bed, obtains the anhydrous chlorides of rase magnesium products.But the aniline hydrochloride that the low-temperature zone of dewatering for double salt volatilizes does not reclaim (even low-temperature zone also has the part aniline hydrochloride to evaporate) measure; To the aniline hydrochloride gas that the high temperature section of desalination is volatilized, propose to adopt it is condensed into liquid, send to again and the synthetic double salt of bischofite.But in fact the fusing point of aniline hydrochloride (198 ℃) is very approaching with boiling point (245 ℃), be difficult to control aniline hydrochloride gas and just in time be condensed into liquid, the fluctuation that has slightly of temperature just causes that this liquid becomes gas or is frozen into solid, causes the obstruction of pipeline and equipment, and operation can't be carried out.
Document [Xu Riyao. metallurgy of megnesium, metallurgical industry press, 1981] introduced and adopted ammonia chloride to make the ammonium carnallitite method dewatering bischofite technology of chemical conditioner, adopted three coolings to stir tower and an eluting column recovery chemical conditioner ammonium chloride, but the rate of recovery is too low, has only 70-80%.Reason is that the ammonium chloride flue gas condensing is incomplete, and the ammonium chloride flue gas is atomic little solid particulate (white cigarette), rely on cooling and drip washing to absorb and can not reclaim complete ammonium chloride, and ammonium chloride has part to resolve into free NH
3And lose.
Summary of the invention
At the problems referred to above, the invention provides and a kind ofly can high efficiente callback prepare the method and apparatus of the chemical conditioner that uses in the process of Magnesium Chloride Anhydrous at double salt method dewatering bischofite.
For achieving the above object, the recovery method of double salt method dewatering bischofite auxiliary agent of the present invention, at first described chemical conditioner is reclaimed in the condensation of carrying out of the steam that contains a small amount of chemical conditioner that double salt was evaporated in the low-temperature heat stage, secondly the chemical conditioner gas that double salt was evaporated in the heat stage cools off and reclaims described chemical conditioner, and the remaining white cigarette that will reclaim not yet in condensation and process of cooling carries out filtered and recycled by the overlay film filter bag.
Further, concrete removal process is as follows:
Double salt is heated, when being warming up to 200-275 ℃, generation is comprised the chemical conditioner gas of steam;
The chemical conditioner gas that will comprise steam is drawn the tubular type dehydration furnace and is carried out condensation, described water of condensation is carried out obtaining chemical conditioner behind the evaporate to dryness, and described still uncooled white cigarette is carried out filtered and recycled by the overlay film filter bag;
Described double salt is proceeded heating, when being warming up to 275-350 ℃, will produce chemical conditioner gas;
Chemical conditioner gas is drawn the tubular type dehydration furnace cool off, produce the crystallization of chemical conditioner, and the white cigarette of described crystallisation by cooling is not yet carried out filtered and recycled by the overlay film filter bag;
Wherein, heat preceding to double salt and heat-processed in need in tube furnace, add shielding gas.
Preferably, described shielding gas is nitrogen.
Particularly, described chemical conditioner comprises two or more the mixture in aniline hydrochloride, pyridine, ammonium chloride, ethylenediamine-hydrochloride, triethylamine hydrochloride or these compounds.
For achieving the above object, the retrieving arrangement of double salt method dewatering bischofite auxiliary agent of the present invention, comprise the tube furnace and condensing tower, cooling tower and the film-coated fabrics bag type filter that heat double salt, wherein said tube furnace has condensing tower and cooling tower by pipe connection, and described condensing tower is connected described film-coated fabrics bag type filter simultaneously with described cooling tower.
Further, also comprise nitrogen unit processed, described nitrogen unit processed and described tube furnace are connected to described tube furnace the gas of the protection in the heat-processed are provided, and described nitrogen unit processed also is used for providing the blowback nitrogen of described film-coated fabrics bag type filter.
Further, the connecting tube between described tube furnace and cooling tower and the condensing tower is utilidor, and described pipeline is tied with the ribbon heater outward and by temperature controller pipe temperature is controlled between 245 ℃ to 255 ℃.
Further, the outer wall of described condensing tower is provided with watercooling jacket, and the outside is provided with condensate draining, and the top is provided with sprinkling equipment, and described sprinkling equipment links to each other with condensate draining, and described condensate draining pumps into condensing tower by pump with water.
Further, the outer wall of described cooling tower is provided with watercooling jacket, and scraping blade is installed in the cooling tower, described scraping blade with provide the speed reduction gearing of power to link to each other for this scraping blade.
Further, described film-coated fabrics bag filtration device comprises cylindrical shell and is installed in the interior terylene overlay film filter bag of tube and the pulse backblowing deashing device at top.
Beneficial effect of the present invention:
Double salt method dewatering bischofite auxiliary agent recovery method of the present invention, the steam that contains a small amount of chemical conditioner that double salt was evaporated in the low-temperature heat stage carries out condensation to reclaim chemical conditioner, the chemical conditioner gas that double salt was evaporated in the heat stage cools off to reclaim chemical conditioner, and the remaining white cigarette that will reclaim not yet in condensation and process of cooling filters to reclaim chemical conditioner by the overlay film filter bag; Adopted condensation, cooling, cloth bag filtration three roads to reclaim chemical conditioner, the rate of recovery is up to nearly 100%, and general export does not have white cigarette and overflows.Therefore have environmental friendliness, pollution-free, advantage that the auxiliary agent rate of recovery is high.
Double salt method chloromagnesite chemical conditioner retrieving arrangement of the present invention, compact construction, reasonable in design, three devices of condensing tower, cooling tower, film-coated fabrics bag type filter are set reclaim chemical conditioner, the rate of recovery is up to nearly 100%, and general export does not have white cigarette and overflows.Therefore have environmental friendliness, pollution-free, advantage that the auxiliary agent rate of recovery is high.
Description of drawings
Fig. 1 is the schema of double salt method dewatering bischofite auxiliary agent recovery method of the present invention;
Fig. 2 is the structural representation of double salt method dewatering bischofite auxiliary agent retrieving arrangement of the present invention.
Embodiment
The present invention will be further described below in conjunction with Figure of description.
The recovery method of double salt method dewatering bischofite auxiliary agent of the present invention, to double salt containing of evaporating in low-temperature heat stage a small amount of (probably account for total amount 7% to 8%) chemical conditioner steam carry out condensation to reclaim chemical conditioner, the chemical conditioner gas that double salt was evaporated in the heat stage cools off to reclaim chemical conditioner, and the remaining white cigarette that will reclaim not yet in condensation and process of cooling filters to reclaim chemical conditioner by the overlay film filter bag.
The retrieving arrangement of double salt method dewatering bischofite auxiliary agent of the present invention, comprise the tube furnace and condensing tower, cooling tower and the sack cleaner that heat double salt, wherein said tube furnace has condensing tower and cooling tower by pipe connection, and described condensing tower is connected described cloth envelop collector simultaneously with described cooling tower.
Below be that chemical conditioner is example with the aniline hydrochloride, the present invention is specifically described:
In aniline hydrochloride double salt method bischofite fixed bed dewatering, bischofite or bittern and aniline hydrochloride are prepared burden in proportion, add and carry out the fixed bed dehydration in the tube furnace.Deviate from most of water and small part aniline hydrochloride when at first double salt is warmed up to 200-275 ℃ in the tube furnace under feeding nitrogen protection; In the time of 275-350 ℃, deviate from remaining moisture and whole aniline hydrochloride, the Magnesium Chloride Anhydrous that output is qualified.But in fact all can there be the aniline hydrochloride flue gas that is Bai Yanzhuan to overflow in whole process, this part flue gas can not reclaim fully with the way of cooling, also once tested with acid solution, alkali lye to absorb (drip washing), but all invalid, because this white cigarette can pass solvent liquid, absorb seldom.So this aniline hydrochloride flue gas have with document [Xu Riyao. metallurgy of megnesium, metallurgical industry press, 1981] the similar character of ammonium chloride flue gas, rely on the way of cooling+drip washing absorption to reclaim fully.
Find that after deliberation white cigarette is a kind of atomic little solid particulate, reaches micron order, and has hydrophobicity.Chemical conditioner therefore of the present invention reclaims solution: condensation+cooling+cloth bag filtration, this method can reclaim the aniline hydrochloride flue gas fully.
As shown in Figure 1, the schema of the recovery method of double salt method dewatering bischofite auxiliary agent of the present invention, concrete removal process is as follows:
Double salt is heated, when being warming up to 200-275 ℃, generation is comprised the chemical conditioner gas of steam, this gas is Bai Yanzhuan;
The chemical conditioner gas that will comprise steam is drawn the tubular type dehydration furnace and is carried out condensation, described water of condensation is carried out evaporate to dryness obtain chemical conditioner, and described still uncooled white cigarette is carried out filtered and recycled by the overlay film filter bag;
Described double salt is proceeded heating, when being warming up to 275-350 ℃, will produce chemical conditioner gas, this gas is Bai Yanzhuan;
Chemical conditioner gas is cooled off, produce the crystallization of chemical conditioner, and the white cigarette of described crystallisation by cooling is not yet carried out filtered and recycled by the overlay film filter bag;
Wherein, heat preceding to double salt and heat-processed in need in tube furnace, add shielding gas.
Retrieving arrangement and recovery method that concrete chemical conditioner utilizes during for aniline hydrochloride are described below:
The difference of deviating from composition when in tube furnace fixed bed (plate), being heated to differing temps according to double salt, the recovery of aniline hydrochloride need be divided into for three steps:
The first step, what be warming up to that 200-275 ℃ of stage at first evaporate at tube furnace is most of water and small part aniline hydrochloride, the condensing tower that this part flue gas is introduced into the band water jacket carries out condensation, in the steam condensation, the aniline hydrochloride gas that evaporates also is dissolved in the water of condensation, so can regularly water of condensation be sent the tube furnace evaporate to dryness to make chemical conditioner obtain reclaiming.Because the aniline hydrochloride that is dissolved in the water of condensation has certain corrosive nature to stainless steel equipment, the condensing tower material is necessary for the titanium material.For preventing that inner wall of tower from separating out crystal sometimes and influencing heat transfer, the ON cycle pump once (continued 5 minutes) in per 8 hours, and water of condensation is sprayed to inner wall of tower to clean the aniline hydrochloride crystal of separating out once in a while by spray equipment.
Second step, be warming up to 275-350 ℃ of stage at tube furnace and deviate from remaining moisture and whole aniline hydrochloride gases, the cooling tower that this part flue gas is switched introducing band water jacket cools off, the crystallization of aniline hydrochloride condensation of gas is separated out in inner wall of tower, for preventing from making the too thick heat-transfer effect that influences of the solid layer of separating out on the inwall, scraping blade and transmission system thereof have been installed in the tower, have constantly scraped the crystal of separating out by scraping blade.
The 3rd step, no matter at the low thermophase of 200-275 ℃ of dehydration, or the hot stage at 275-350 ℃ of desalination acid aniline, tube furnace has white cigarette to be spilled over to the auxiliary agent recovery system, in condensing tower and cooling tower, all can not be recovered fully, this part remaining white cigarette is introduced in the cloth envelop collector of tape pulse blowback nitrogen, is recovered fully through overlay film filter bag high efficiency filter.
Therefore, the retrieving arrangement of described aniline hydrochloride comprises condensing tower, cooling tower, cloth envelop collector and pipeline thereof, instrument and Controlling System.
The working method that described chemical conditioner reclaims is as follows: before the tubular type dehydration furnace heats up, feed nitrogen (N earlier in tube furnace
299.8% ,-2.5Nm
3/ h) with excluding air, heat up by predefined heating schedule again.Deviate from most of water and small part aniline hydrochloride at 200-275 ℃, these steam are introduced into the condensing tower of strap clamp cover, feed water coolant in the chuck, regulate cooling water flow, and control condensing tower gas outlet temperature is 40-45 ℃, and the steam condensation rate can reach 95%.The small amount of hydrochloric acid aniline that evaporates simultaneously also is condensed and enters in the water of condensation, and this part aniline hydrochloride can evaporate again and removes moisture and obtain reclaiming by regularly condensate pump being delivered to dehydration furnace.Deviate from moisture remaining in the double salt and whole aniline hydrochloride, the Magnesium Chloride Anhydrous that output is qualified 275-350 ℃ of stage.The nitrogen flow that will enter dehydration furnace this moment is kept to 2.0Nm
3/ h, nitrogen gas concn is increased to N
299.99%, with in the high-temperature gas (mainly being aniline hydrochloride gas) that the evaporates incision cooling tower and be condensed and be crystal and separate out in inner wall of tower, scraping blade constantly scrapes crystal under the step-down gear transmission system drives, be accumulated in tower base cone body portion, regularly start tower at the bottom of spiral discharging machine draw off crystal powder.In condensation aniline hydrochloride gas process, regulating cooling water flow is 40-45 ℃ with control cooling tower gas outlet temperature, and aniline hydrochloride condensation of gas rate can reach about 90%.The white cigarette of auxiliary agent under also uncolled in condensing tower and cooling tower, introducing efficiently, cloth envelop collector filters, under periodicity blowback nitrogen (0.4-0.6MPa) effect powder constantly shaken and fall the bottom cone part, the flue gas dust collection rate reaches more than 99.5%.From the gas water white transparency that cloth envelop collector comes out, qualified discharge.
Embodiment 1
As shown in Figure 2, the device in the present embodiment comprises Nitrogen plant group 1, is used to the double salt dehydration that protection gas and carrier gas-nitrogen are provided; Fixed bed dehydration equipment tube furnace 2; One cover chemical conditioner retrieving arrangement.The aniline hydrochloride gas that needs to reclaim is from the tubular type dehydration furnace.
In tube furnace 2, synthetic double salt was deviate from most of moisture and small part aniline hydrochloride when the material that bischofite and aniline hydrochloride are formed was heated to 110 ℃ in the time of 200-275 ℃; Carry out condensation in the condensing tower 3 with this part gas introducing band water jacket, this small part aniline hydrochloride is dissolved in the water of condensation.
Double salt was deviate from remaining moisture and whole aniline hydrochloride gas when the tube furnace temperature rose to 275-350 ℃, the cooling tower 4 of this part flue gas being introduced the band water jacket cools off, makes the condensation of gas crystallization to separate out in inner wall of tower, opens the interior gearing-down system of tower 16 driving scraping blades 20 and constantly scrapes the crystal of separating out.
White cigarette under will overflowing and all can not total condensation in condensing tower and cooling tower in above two temperature stages is introduced in the cloth envelop collector 5 of tape pulse blowback nitrogen, and the high efficiency filter through overlay film filter bag 21 fully is recovered white cigarette.
According to the quantity of water of condensation in the storage tank 17, regularly water of condensation is delivered to the tube furnace evaporate to dryness to reclaim chemical conditioner wherein with pump 6.ON cycle pump 6 sprays to the condensing tower inwall with water of condensation by spray equipment 13 and cleans the aniline hydrochloride crystal of separating out once in a while before every furnace accretion bundle.
Therefore, described a kind of device that reclaims double salt method dewatering bischofite auxiliary agent aniline hydrochloride comprises a condensing tower 3, is used for most of steam and small part aniline hydrochloride gas that condensation is deviate from.
Described a kind of device that reclaims double salt method dewatering bischofite auxiliary agent aniline hydrochloride comprises a cooling tower 4, is used for most of aniline hydrochloride gas that condensation is deviate from.
Described a kind of device that reclaims double salt method dewatering bischofite auxiliary agent aniline hydrochloride comprises a film-coated fabrics bag type filter 5, is used for reclaiming with the cooling way reclaiming invalid residue aniline hydrochloride flue gas, further improves the rate of recovery of aniline hydrochloride.
Described a kind of device that reclaims double salt method dewatering bischofite auxiliary agent aniline hydrochloride, comprise two sections insulation pipelines, i.e. insulation pipeline 15 from the tube furnace to the condensing tower, and the insulation of the pipeline section between from the tube furnace to cooling tower pipeline 14, twine the ribbon heater heat tracing outside the pipe, also use temperature controller control tube channel temp between also being 245 ℃ to 255 ℃ about 250 ℃, in case gases such as aniline hydrochloride condense and blocking pipe in this pipeline.Mounting ball valve 7 and 8 on the insulation pipeline enters condensing tower or cooling tower for high-temperature flue gas is switched respectively.
The condensing tower structure is in the described auxiliary agent retrieving arrangement: the tower body outer wall has cooling water jecket 18; The tower body top has spray equipment 13, with the fouling of routine cleaning tower internal surface; The tower material is the titanium material, because the aniline hydrochloride that is dissolved in the water of condensation has certain corrosive nature to stainless steel 304 equipment, and the titanium material can be resisted this corrosion.
Cooling tower structure is in the described auxiliary agent retrieving arrangement: the tower body outer wall has scraping blade 20 and gearing-down system 16 thereof is installed in cooling water jecket 19, the tower body, and the total reduction ratio of gearing-down system is 240: 1.The tower material is stainless steel 304.
The cloth envelop collector structure is in the described auxiliary agent retrieving arrangement: pulse backblowing soot cleaning system 22 is arranged at terylene overlay film filter bag 21, top that Φ 120 * 1000mm is installed in the cylindrical shell.
In the double salt method fixed bed dewatering of bittern or bischofite, at first need to feed nitrogen to dehydration furnace and do protection gas and carrier gas, high pure nitrogen is produced by Nitrogen plant group in the left side in the accompanying drawing 2 nitrogen output 2.5Nm is provided
3/ h, nitrogen gas purity 99.999%.Get the raw materials ready then with reinforced: with 1.25: 1.0 batchings of mol ratio of aniline hydrochloride/magnesium chloride hexahydrate, add 6kg/ stove magnesium chloride hexahydrate and 2.66kg/ stove aniline hydrochloride, sabot is sent into and is carried out the fixed bed dehydration in the tube furnace that the inner chamber on the right is Φ 300 * 2000mm after stirring.Tube furnace is pressed predefined temperature programming, dehydration, desalination stage by stage, and every stove lasts 8 hours.The steam and the aniline hydrochloride gas that produce successively enter auxiliary agent recovery system condensing tower, cooling tower and cloth envelop collector, realize that auxiliary agent reclaims.Auxiliary agent hydrochloric acid aniline recovery specifically was divided into for three steps:
The first step, after the tubular type dehydration furnace began to heat up, what double salt at first evaporated in the time of 200-275 ℃ was most of water and small part aniline hydrochloride; Φ 300 * 1900mm condensing tower that this part flue gas is introduced into the band water jacket carries out condensation, regulates cooling water flow, and the control tower Outlet Gas Temperature is 35-45 ℃, and the steam condensation rate reaches 92%, and this small part aniline hydrochloride is dissolved in the water of condensation.Water of condensation temporarily is stored in the storage tank, regularly water of condensation in the storage tank is sent tube furnace again evaporate to dryness to reclaim chemical conditioner.The ON cycle pump sprays to inner wall of tower with water of condensation by spray equipment and cleans the aniline hydrochloride crystal of separating out once in a while before every furnace accretion bundle.Condensing tower has reclaimed aniline hydrochloride 0.289kg/ stove.
In second step, double salt is deviate from remaining moisture and whole aniline hydrochloride gas at 275-350 ℃.Φ 300 * 1500mm cooling tower that this part flue gas is cut the band water jacket cools off, crystal is separated out in inner wall of tower, regulates cooling water flow, and the control tower Outlet Gas Temperature is 35-45 ℃, and the aniline hydrochloride condensation rate reaches 80%.Make that the solid layer of separating out on the inwall is too thick influences heat transfer in order to prevent from making, scraping blade has been installed in the tower, under the step-down gear transmission system drove, scraping blade constantly scraped the crystal of separating out with 6 rev/mins speed.Cooling tower has reclaimed aniline hydrochloride 2.082kg/ stove.
The 3rd step in above two stages, had white cigarette to overflow, and Φ 200 * 1100mm cloth envelop collector that the white cigarette under condensing tower and cooling tower all can not condensations is introduced into tape pulse blowback nitrogen filters.Cloth envelop collector has reclaimed aniline hydrochloride 0.255kg/ stove.
More than three the step in auxiliary agent aniline hydrochloride total recovery reach 98.5%.
The condensing tower structure is in this cover auxiliary agent retrieving arrangement: the tower body outer wall has cooling water jecket, the tower body top has spray equipment.Because small amount of hydrochloric acid aniline is arranged in the water of condensation, stainless steel is had corrodibility, can resist this corrosion with the condensing tower that the titanium material replaces stainless steel to make, the water of condensation that flows out from the titanium condensing tower is water white.
Cooling tower structure is in this cover auxiliary agent retrieving arrangement: the tower body outer wall has scraping blade and gearing-down system thereof is installed in cooling water jecket, the tower body.Because material is solid crystal, stainless steel do not had corrodibility, so can make cooling tower with stainless steel 304.
The cloth envelop collector structure is in this cover auxiliary agent retrieving arrangement: the pulse backblowing soot cleaning system is arranged at 1 of terylene overlay film filter bag, top that Φ 120 * 1000mm is installed in the cylindrical shell.
This cover auxiliary agent retrieving arrangement, also comprise two sections Φ, 50 insulation pipelines, namely the insulation pipeline from the tube furnace to the condensing tower and from the tube furnace to the cooling tower between the insulation pipeline, pipe is outer twine the ribbon heater with heat tracing, and with temperature controller control tube channel temp about 250 ℃, in case aniline hydrochloride gas condenses and blocking pipe in this pipeline.On the insulation pipeline two ball valves have been installed, have been entered condensing tower or cooling tower for high-temperature flue gas is switched respectively.
The device of present embodiment is with embodiment 1, and the Nitrogen plant group is produced provides nitrogen, nitrogen output 0.5Nm
3/ h, nitrogen gas purity 99.999%.1.25: 1.0 batchings of mol ratio with aniline hydrochloride/magnesium chloride hexahydrate add 2kg/ stove magnesium chloride hexahydrate and 0.888kg/ stove aniline hydrochloride, and the back sabot that stirs is sent into and carried out the fixed bed dehydration in the tube furnace.Tube furnace is pressed predefined temperature programming, dehydration, desalination stage by stage, and every stove lasts 8 hours.The steam and the aniline hydrochloride gas that produce successively enter auxiliary agent recovery system condensing tower, cooling tower and cloth envelop collector.
After the tubular type dehydration furnace begins to heat up, what double salt at first evaporated in the time of 200-275 ℃ is that most of water and small part aniline hydrochloride are introduced condensing tower, regulate cooling water flow, the control tower Outlet Gas Temperature is 35-45 ℃, the steam condensation rate reaches 88%, and this small part aniline hydrochloride is dissolved in the water of condensation.Reclaimed aniline hydrochloride 0.118kg/ stove from condensing tower.
Double salt is deviate from remaining moisture at 275-350 ℃ and is cut cooling tower with whole aniline hydrochloride gases, regulates cooling water flow, and the control tower Outlet Gas Temperature is 35-45 ℃, and the aniline hydrochloride condensation rate reaches 84%.Cooling tower has reclaimed aniline hydrochloride 0.764kg/ stove.
White cigarette under condensing tower and cooling tower all can not condensations is introduced into cloth envelop collector and filters.Cloth envelop collector has reclaimed aniline hydrochloride 0.032kg/ stove.
Above auxiliary agent aniline hydrochloride total recovery reaches 102%.
The device of present embodiment is with embodiment 1.The Nitrogen plant group is produced provides nitrogen, nitrogen output 1.5Nm
3/ h, nitrogen gas purity 99.999%.1.25: 1.0 batchings of mol ratio with aniline hydrochloride/magnesium chloride hexahydrate add 2kg/ stove magnesium chloride hexahydrate and 0.888kg/ stove aniline hydrochloride, and the back sabot that stirs is sent into and carried out the fixed bed dehydration in the tube furnace.Tube furnace is pressed predefined temperature programming, dehydration, desalination stage by stage, and every stove lasts 8 hours.The steam and the aniline hydrochloride gas that produce successively enter auxiliary agent recovery system condensing tower, cooling tower and bagroom.
After the tubular type dehydration furnace begins to heat up, what double salt at first evaporated in the time of 200-275 ℃ is that most of water and small part aniline hydrochloride are introduced condensing tower, regulate cooling water flow, the control tower Outlet Gas Temperature is 35-45 ℃, the steam condensation rate reaches 85%, and this small part aniline hydrochloride is dissolved in the water of condensation.Reclaimed aniline hydrochloride 0.079kg/ stove from condensing tower.
Double salt is deviate from remaining moisture at 275-350 ℃ and is cut cooling tower with whole aniline hydrochloride gases, regulates cooling water flow, and the control tower Outlet Gas Temperature is 35-45 ℃, and the aniline hydrochloride condensation rate reaches 83%.Cooling tower has reclaimed aniline hydrochloride 0.731kg/ stove.
White cigarette under condensing tower and cooling tower all can not condensations is introduced into cloth envelop collector and filters.Cloth envelop collector has reclaimed aniline hydrochloride 0.057kg/ stove.
Above auxiliary agent aniline hydrochloride total recovery reaches 97.5%.
In the various embodiments described above, described chemical conditioner can also be a kind of, two or more the mixture in aniline hydrochloride, pyridine, ammonium chloride, ethylenediamine-hydrochloride, the triethylamine hydrochloride.
More than; only be preferred embodiment of the present invention, but protection scope of the present invention is not limited thereto, anyly is familiar with those skilled in the art in the technical scope that the present invention discloses; the variation that can expect easily or replacement all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain that claim was defined.
Claims (10)
1. the recovery method of a double salt method dewatering bischofite auxiliary agent, it is characterized in that: the steam that contains chemical conditioner that dehydration furnace double salt was evaporated in the low temperature dewatering stage is drawn dehydration furnace and is carried out condensation to reclaim described chemical conditioner, next chemical conditioner gas that dehydration furnace double salt is evaporated at the high temperature desalination stage is drawn dehydration furnace and is cooled off to reclaim described chemical conditioner, and the white cigarette that will not obtain yet reclaiming in condensation and process of cooling filters with the described chemical conditioner of further recovery with the overlay film cloth bag.
2. the recovery method of double salt method dewatering bischofite auxiliary agent according to claim 1, it is characterized in that: concrete removal process is as follows:
Double salt is heated, when being warming up to 200-275 ℃, generation is comprised the chemical conditioner gas of steam;
The chemical conditioner that will comprise steam is drawn the tubular type dehydration furnace and is carried out condensation, described water of condensation is carried out evaporate to dryness obtain chemical conditioner, and described still uncooled white cigarette is carried out filtered and recycled by the overlay film filter bag;
Described double salt is proceeded heating, when being warming up to 275-350 ℃, will produce chemical conditioner gas;
Chemical conditioner gas is drawn the tubular type dehydration furnace cool off, produce the crystallization of chemical conditioner, and the white cigarette of described crystallisation by cooling is not yet carried out filtered and recycled by the overlay film filter bag;
Wherein, heat preceding to double salt and heat-processed in need in tube furnace, add shielding gas.
3. the recovery method of double salt method dewatering bischofite auxiliary agent according to claim 2, it is characterized in that: described shielding gas is nitrogen.
4. the recovery method of double salt method dewatering bischofite auxiliary agent according to claim 1, it is characterized in that: described chemical conditioner comprises a kind of, two or more the mixture in aniline hydrochloride, pyridine, ammonium chloride, ethylenediamine-hydrochloride, the triethylamine hydrochloride.
5. the retrieving arrangement of a double salt method dewatering bischofite auxiliary agent, it is characterized in that: comprise the tube furnace and condensing tower, cooling tower and the pulse film-coated fabrics bag type filter that heat double salt, wherein said tube furnace has condensing tower and cooling tower by pipe connection, and described condensing tower is connected described pulse film-coated fabrics bag type filter simultaneously with described cooling tower.
6. the retrieving arrangement of double salt method dewatering bischofite auxiliary agent according to claim 5; it is characterized in that: also comprise nitrogen unit processed; described nitrogen unit processed and described tube furnace are connected to described tube furnace the gas of the protection in the heat-processed are provided, and described nitrogen unit processed also is used for providing the blowback nitrogen of described cloth envelop collector.
7. the retrieving arrangement of double salt method dewatering bischofite auxiliary agent according to claim 5, it is characterized in that: the connecting tube between described tube furnace and cooling tower and the condensing tower is utilidor, and described pipeline is tied with the ribbon heater outward and by temperature controller pipe temperature is controlled between 245 ℃ to 255 ℃.
8. the retrieving arrangement of double salt method dewatering bischofite auxiliary agent according to claim 5, it is characterized in that: the outer wall of described condensing tower is provided with watercooling jacket, the outside is provided with condensate draining, and the top is provided with sprinkling equipment, described sprinkling equipment links to each other with condensate draining, and described condensate draining pumps into condensing tower by pump with water.
9. the retrieving arrangement of double salt method dewatering bischofite auxiliary agent according to claim 5, it is characterized in that: the outer wall of described cooling tower is provided with watercooling jacket, scraping blade is installed in the cooling tower, described scraping blade with provide the speed reduction gearing of power to link to each other for this scraping blade.
10. the retrieving arrangement of double salt method dewatering bischofite auxiliary agent according to claim 5 is characterized in that: described film-coated fabrics bag filtration device comprises cylindrical shell and is installed in terylene overlay film filter bag in the tube and the pulse backblowing deashing device at top.
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| CN113214801A (en) * | 2021-05-19 | 2021-08-06 | 中国科学院上海应用物理研究所 | Low cost MgCl based on bischofite2Preparation method of (E) -KCl eutectic salt |
| CN113758292A (en) * | 2021-09-30 | 2021-12-07 | 南京华电节能环保股份有限公司 | Coke oven raw gas waste heat comprehensive utilization device |
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| CN103274433B (en) | 2018-07-24 |
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