CN114162839A - Device for preparing ammonium chloride by co-production of sodium bicarbonate - Google Patents

Device for preparing ammonium chloride by co-production of sodium bicarbonate Download PDF

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Publication number
CN114162839A
CN114162839A CN202111442206.6A CN202111442206A CN114162839A CN 114162839 A CN114162839 A CN 114162839A CN 202111442206 A CN202111442206 A CN 202111442206A CN 114162839 A CN114162839 A CN 114162839A
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kettle
ammonium chloride
cauldron
solid
sodium
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刘松林
刘金坤
刘瀚宇
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Hengyang Aijie Technology Co ltd
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Hengyang Aijie Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01DCOMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D7/00Carbonates of sodium, potassium or alkali metals in general
    • C01D7/02Preparation by double decomposition
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00Ammonia; Compounds thereof
    • C01C1/16Halides of ammonium
    • C01C1/164Ammonium chloride

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a device for preparing ammonium chloride by co-production of baking soda, which comprises a primary baking soda precipitation device and a first solid-liquid separation device which are sequentially communicated, an ammonium chloride preparation device, a secondary baking soda precipitation device and a mother liquor circulation device which are sequentially communicated, and further comprises a sodium precipitation device and a second solid-liquid separation device, wherein the sodium precipitation device comprises a first sodium precipitation kettle and a second sodium precipitation kettle which are sequentially communicated, the top end of the first sodium precipitation kettle is connected with a salt metering scale, the feed end of the first sodium precipitation kettle is connected with the first solid-liquid separation device, the discharge end of the second sodium precipitation kettle is communicated with the second solid-liquid separation device, and the second solid-liquid separation device is respectively communicated with the ammonium chloride preparation device and the primary baking soda precipitation device. The invention can avoid the phenomenon that the baking soda and the ammonium chloride generated by the residual ammonium bicarbonate and the sodium chloride are difficult to separate in the cold separation process, reduce the content of sodium salt in the ammonium chloride, improve the content of ammonia, and improve the yield of the baking soda and the ammonium chloride.

Description

Device for preparing ammonium chloride by co-production of sodium bicarbonate
Technical Field
The invention relates to the technical field of chemical production, in particular to a device for preparing ammonium chloride by co-production of sodium bicarbonate.
Background
Baking soda is also called sodium bicarbonate, is an inorganic salt, is white crystalline powder, has no odor and is easy to dissolve in water, and is widely applied to the industries of pharmaceutical industry, food processing, fire-fighting equipment and the like.
Ammonium chloride, ammonium chloride for short, is the ammonium salt of hydrochloric acid, is mostly a byproduct of the alkali manufacturing industry (such as baking soda), is white or yellowish square or octahedral small crystal, has two dosage forms of powder and granule, is easy to store, and is widely applied to the aspects of agricultural fertilizers, batteries, electroplating, metal welding, dyes, printing, medicines and the like.
Sodium chloride in brine is usually reacted with ammonium bicarbonate to generate baking soda and ammonium chloride, and ammonium chloride generated as a byproduct in the baking soda preparation process is separated and recovered, so that the loss of ammonium chloride caused by the discharge of ammonium chloride along with waste liquid is reduced, and the recovery rate of ammonium chloride is improved.
At present, there are many devices for preparing ammonium chloride by co-production of sodium bicarbonate, for example, patent application No. cn201910000923.x discloses a cyclic manufacturing device for co-production of ammonium chloride by sodium bicarbonate, which comprises a first-stage sodium bicarbonate precipitation device, a cold precipitation device, a salting-out device and a mother liquor circulating device which are sequentially communicated, and further comprises a second-stage sodium bicarbonate precipitation device, wherein one end of the second-stage sodium bicarbonate precipitation device is communicated with the salting-out device, the other end of the second-stage sodium bicarbonate precipitation device is communicated with the mother liquor circulating device, the first-stage sodium bicarbonate precipitation device comprises a reaction kettle, a brine tank and an ammonium bicarbonate feeding device, and the brine tank and the ammonium bicarbonate feeding device are communicated with the reaction kettle. The following problems mainly exist in the process of manufacturing the baking soda by adopting the device:
1) the ammonium salt content in the baking soda product prepared by the device is high, and the reason is that: in the later stage of the double decomposition reaction, the concentration of sodium ions becomes dilute, the double decomposition reaction tends to be mild from a violent trend, an atmosphere which is not suitable for the double decomposition reaction of sodium chloride and ammonium bicarbonate is formed, so that part of ammonium bicarbonate lacks reaction power and coexists with baking soda in the form of solid crystals, and enters a drying procedure together with the baking soda after being filtered and centrifugally separated, and the temperature when the baking soda is dried is 50-60 ℃, the ammonium bicarbonate crystals are difficult to decompose into free ammonia at the drying temperature for volatilization, and the content of ammonium salt in the obtained baking soda product exceeds the standard; the other part of ammonium bicarbonate is directly dissolved and can not collide with double decomposition ions under the low-sodium condition to form crystal nucleus, so that the crystal nucleus is slowly formed, the crystal growth is slower, the crystallization is finer, and the subsequent filtering effect is reduced to influence the yield of the baking soda;
2) the ammonium chloride prepared by the device contains low nitrogen and high sodium salt content, and the reason is that: the mother liquor M1 obtained by separating the sodium bicarbonate prepared by the first-stage sodium bicarbonate precipitation device in the device is high in carbonate content and higher than Na and HCO in a phase diagram3Cross plot, NaHCO formed at Low temperature3Cannot be separated from ammonium chloride, and enters an ammonium chloride treatment device from the bottom of the crystallization kettle to be carried into an ammonium chloride product together with ammonium chloride through cold separation and coprecipitation, so that the sodium salt in the ammonium chloride product is increased and the nitrogen content is low; in addition, because a large amount of sodium chloride solid salt is added into the salting-out kettle in the salting-out process, when ammonium chloride crystal slurry crystallized from the salting-out kettle is directly input into the crystallization kettle through a crystal slurry taking-out port, sodium chloride directly enters the crystallization kettle along with ammonium chloride, so that sodium ions in an ammonium chloride product crystallized from the crystallization kettle exceed the standard, the ammonium chloride is difficult to reach the agricultural standard, and the product quality of the ammonium chloride is reduced;
3) this one-level only adopts 1 reation kettle to carry out the metathesis reaction among the baking soda device of appearing, when the reaction, the formation rate of crystal nucleus is very fast, nucleation rate is big, make at unit volume, the crystal nucleus quantity that forms in unit interval is more, and because the space in 1 reation kettle is limited, make every particle grow up and the space of mutual extrusion diminishes, the growth of every crystalline grain has been hindered, the crystalline grain that forms after the crystallization is more thin, thereby seriously influence the filtration separation process of follow-up baking soda, the preparation efficiency of baking soda has not only been reduced, still reduced the yield of baking soda, the preparation cost of baking soda has been improved.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the device for preparing ammonium chloride by co-production of baking soda overcomes the defects of the prior art, has a simple structure, is convenient to operate, can reduce the content of ammonium salt in the prepared baking soda product and improve the yield of baking soda, and can also reduce the content of sodium salt in the ammonium chloride product and improve the content and yield of ammonia in ammonium chloride.
The technical scheme adopted by the invention for solving the technical problems is as follows: a device for preparing ammonium chloride by co-production of sodium bicarbonate comprises a first-stage sodium bicarbonate precipitation device, a first solid-liquid separation device, an ammonium chloride preparation device, a second-stage sodium bicarbonate precipitation device, a mother liquor circulating device, a sodium precipitation device and a second solid-liquid separation device which are sequentially communicated, the sodium precipitation device comprises a first sodium precipitation kettle and a second sodium precipitation kettle which are communicated in sequence, the top end of the first sodium precipitation kettle is connected with a salt metering scale, and the feed end of the sodium chloride is connected with the first solid-liquid separation device and is respectively used for conveying sodium chloride and the crude mother liquor M1 separated by the first solid-liquid separation device into the first sodium precipitation kettle, the discharge end of the second sodium precipitation kettle is communicated with a second solid-liquid separation device which is respectively communicated with an ammonium chloride preparation device and a primary sodium bicarbonate precipitation device, and the refined mother liquor M1 and the baking soda obtained by separating the second solid-liquid separation device are respectively input into an ammonium chloride preparation device and a first-stage baking soda precipitation device.
Further, the second sodium precipitation kettle is further connected with a heat exchange device, the heat exchange device comprises a heat exchange pipe and a steam boiler, the heat exchange pipe is coiled in the second sodium precipitation kettle, an air inlet of the heat exchange pipe is connected with an air outlet of the steam boiler, and an air outlet of the heat exchange pipe is connected with an air inlet of the steam boiler.
Further, baking soda device is appeared to one-level is including the mixed reation kettle, crystal nucleus growth cauldron, the long cauldron of particle and the reaction balance cauldron that communicate in proper order, mixed reation kettle still has brine tank and ammonium bicarbonate feeding device through the pipeline splice respectively, reaction balance cauldron and first solid-liquid separation equipment intercommunication.
Further, agitator motor is all installed at the top of mixing reation kettle, crystal nucleus growth cauldron, the long cauldron of particle and reaction balance cauldron's kettle cover, agitator motor is connected with the (mixing) shaft, in the bottom of (mixing) shaft stretched into mixing reation kettle, crystal nucleus growth cauldron, the long cauldron of particle and reaction balance cauldron respectively, and be equipped with a plurality of stirring thick liquids on it, the contained angle that is located between the stirring thick liquid of co-altitude and the horizontal plane reduces along the direction of top to bottom of (mixing) shaft gradually.
Further, the device still includes the deamination device, the deamination device is including the first deamination cauldron, second deamination cauldron and the third deamination cauldron that communicate in proper order, the feed end and the first solid-liquid separation equipment intercommunication of first deamination cauldron for carry the thick baking soda that first solid-liquid separation equipment separation obtained to first deamination cauldron in, and first deamination cauldron passes through pipeline and mother liquor circulating device intercommunication, be used for carrying the second grade that mother liquor circulating device collected to separate out baking soda device and ammonium chloride preparation facilities production mother liquor M2 and carry to first deamination cauldron in further react with thick baking soda.
Further, the third deamination kettle is sequentially connected with a third solid-liquid separation device and a drying device through a pipeline, the third solid-liquid separation device is used for separating mother liquor and fine soda generated in the third deamination kettle, and the drying device is used for drying the separated fine soda.
Further, the ammonium chloride preparation facilities includes cold separation device, salting out device and ammonium chloride processing apparatus, cold separation device is used for carrying out cold separation crystallization with smart mother liquor M1, and it includes crystallization kettle and the external cooler that communicates with crystallization kettle, the external cooler still has ice maker circulation intercommunication through pipeline circulation intercommunication, and its inside is equipped with the exchange tubulation, the salting out device is used for collecting the overflow liquid that cold separation device discharged and carries out the salting out crystallization to it, and it includes the salting out cauldron and the salt feeding device with salting out cauldron intercommunication, the ammonium chloride processing apparatus is used for filtering, dehydration and drying process to the ammonium chloride that separates out in the cold separation device.
Further, the external cooler is circularly communicated with an external washing tank through a pipeline, the external washing tank is communicated with the third solid-liquid separation device and used for storing washing liquid obtained by separation from the third solid-liquid separation device, and the washing liquid is conveyed from the top of the external cooler to the inside of the external cooler through the pipeline from the external washing tank and then returns to the external washing tank from the pipeline at the bottom of the external cooler and is used for circularly and repeatedly washing scar blocks attached to the inner wall of the external cooler and the outer wall of the exchange tube.
Further, the bottom of the external cooler is connected with a replacement tank through a pipeline, and the replacement tank is communicated with the crystallization kettle through a pipeline.
Further, the salting-out cauldron is from last to including clear liquid section, linkage segment and suspension section down, the clear liquid section is equipped with the overflow mouth, the overflow mouth is connected with dense groove, the suspension section is equipped with at least one crystal thick liquid and takes out the mouth, the crystal thick liquid is taken out the mouth and is connected with the salt separation cauldron, the lateral wall of salt separation cauldron passes through the pipeline and is connected with the top of crystallization cauldron.
The device for preparing ammonium chloride by co-producing sodium bicarbonate has the beneficial effects that:
(1) according to the invention, the sodium precipitation device and the second solid-liquid separation device are additionally arranged between the first solid-liquid separation device and the ammonium chloride preparation device, so that residual ammonium bicarbonate in the crude mother liquor M1 obtained by separation of the first solid-liquid separation device can further react with added sodium chloride to generate baking soda before cold separation crystallization, and the ammonium bicarbonate is decomposed before the subsequent cold separation crystallization, thereby avoiding the phenomenon that the baking soda and the ammonium chloride generated by the residual ammonium bicarbonate and the sodium chloride are difficult to separate in the cold separation process because the crude mother liquor M1 is directly conveyed to the ammonium chloride preparation device, further reducing the content of sodium salt in the ammonium chloride, improving the content of ammonia, and effectively improving the yield of the baking soda;
(2) according to the invention, the deamination device is arranged, the mother liquor M2 generated by the secondary sodium bicarbonate precipitation device and the ammonium chloride preparation device is conveyed into the deamination device to further react with the crude sodium bicarbonate in the deamination device, so that the solid sodium bicarbonate remained in the crude sodium bicarbonate further reacts with the sodium chloride in the mother liquor M2 to generate the sodium bicarbonate, the content of ammonium salt in the sodium bicarbonate is effectively reduced, the yield of the sodium bicarbonate is improved, the quality of the sodium bicarbonate product is improved, and the prepared sodium bicarbonate product meets the food standard;
(3) the invention also adopts the four kettles, namely the mixing reaction kettle, the crystal nucleus growing kettle, the particle growing kettle and the reaction balance kettle, to replace one kettle in the prior art for carrying out double decomposition reaction, so that the baking soda prepared by double decomposition reaction is sequentially crystallized in the mixing reaction kettle, the crystal nucleus growing kettle, the particle growing kettle and the reaction balance kettle step by step, the crystallization time is prolonged, the growth space of each crystal grain is increased, the phenomena of poor subsequent filtering effect and low efficiency caused by over-fine crystal grains after the crystallization is finished are avoided, the yield and the preparation efficiency of the baking soda are improved, and the preparation cost of the baking soda is reduced;
(4) according to the invention, the salt separation kettle is connected with the crystal slurry taking-out port of the salting-out kettle, the side wall of the salt separation kettle is connected with the crystallization kettle through a pipeline, the ammonium chloride crystals carrying solid salt are input from the salting-out kettle and enter the salt separation kettle, and the ammonium chloride is obtained from the side wall of the salt separation kettle and enter the crystallization kettle, so that the phenomenon that the salt content of the ammonium chloride is high because the ammonium chloride crystals carrying solid salt in the salting-out kettle are directly input into the crystallization kettle is avoided, the phenomenon that the sodium ions in the ammonium chloride product from the crystallization kettle exceed the standard is prevented, the produced ammonium chloride reaches the agricultural standard, and the product quality of the ammonium chloride is effectively improved;
(5) the invention also can store the lotion obtained by the separation of the third solid-liquid separation device in the external washing tank through the external washing tank which is circularly communicated with the external cooler through a pipeline, and convey the lotion into the external cooler to wash the ammonium chloride crystals scabbed on the inner wall of the external cooler and the outer wall of the exchange tube in a reciprocating and circulating manner, thereby avoiding the phenomenon that the lotion is directly discharged outside to cause that the discharge of waste liquid does not reach the standard, avoiding the scabbed phenomenon on the inner wall of the external cooler and the outer wall of the exchange tube, reducing the cleaning difficulty of the external cooler and the exchange tube, and ensuring the smooth preparation of baking soda and ammonium chloride; the liquid after the washing is finished is conveyed to the crystallization kettle through the replacement groove, so that the ammonium chloride in the washing liquid can be effectively recovered, the loss of the ammonium chloride is reduced, and the yield of the ammonium chloride is improved.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for co-producing sodium bicarbonate and preparing ammonium chloride according to the present invention;
FIG. 2-is an enlarged schematic view of the first stage sodium bicarbonate evolving apparatus and the first solid-liquid separation apparatus of FIG. 1;
FIG. 3 is an enlarged schematic view of the deamination apparatus and a third solid-liquid separation apparatus of FIG. 1;
FIG. 4-is a schematic diagram of the process at the sodium precipitation unit and the second solid-liquid separation unit in FIG. 1;
FIG. 5-is an enlarged schematic view of the cooling apparatus and salting-out apparatus of FIG. 1;
FIG. 6-is an enlarged schematic view of the secondary sodium bicarbonate evolving plant and ammonium chloride treatment plant of FIG. 1;
fig. 7-is an enlarged schematic view at the drying apparatus in fig. 1.
The above reference numerals: 1-a first-stage sodium bicarbonate precipitation device, 2-a first solid-liquid separation device, 3-a sodium precipitation device, 4-a second solid-liquid separation device, 5-a second-stage sodium bicarbonate precipitation device, 6-a deamination device, 7-a stirring slurry, 8-a heat exchange pipe, 9-a cold precipitation device, 10-a salting-out device, 11-an ammonium chloride treatment device, 12-a first deamination kettle, 13-a second deamination kettle, 14-a third deamination kettle, 15-a third solid-liquid separation device, L1101-a mixing reaction kettle, L1102-a crystal nucleus growth kettle, L1103-a particle growth kettle, L1104-a reaction balance kettle, T1102-a brine tank, an N103-ammonium bicarbonate feeding device, X101, X102, X124-a vacuum filter, P101, X129, P102, S122-a centrifugal machine and V104-a separation tank, v106-a primary liquid storage tank, X103-a belt filter, P103-a water washing tank, F109-a drying device, K110, K130-a bag sewing machine, T1116-a crystallization kettle, Y115-an external cooler, P113-an ice maker, T1118-a salting-out kettle, B120-a salt feeding device, V121-a dense tank, L2121-1-a heating kettle, V125-a tertiary liquid storage tank, V117-a low tank, L2105-a first sodium precipitation kettle, L2106-a second sodium precipitation kettle, a salt metering scale L1107, V108-a separation tank, V109-a secondary liquid storage tank, V112-a salt separation kettle, V110-a semi-brine tank, V107-an external washing tank and V111-a replacing tank. In the figure, PL denotes a liquid and PS denotes a solid.
Detailed Description
The invention is further illustrated with reference to the following figures and examples, which are not intended to limit the scope of the invention in any way.
Example 1
The utility model provides a device of baking soda coproduction preparation ammonium chloride, includes that the one-level that communicates in proper order is appeared baking soda device 1 and first solid-liquid separation equipment 2, is deposited sodium device 3, second solid-liquid separation equipment 4, ammonium chloride preparation facilities, second grade and is appeared baking soda device 5 and mother liquor circulating device, first solid-liquid separation equipment 2 still is connected with deamination device 6.
Baking soda device 1 is appeared including the mixed reation kettle L1101, crystal nucleus growth cauldron L1102, the long cauldron L1103 of particle and the reaction balance cauldron L1104 that communicate in proper order, mixed reation kettle L1101 still is connected with brine groove T1102 and ammonium bicarbonate feeding device N103 respectively through the pipeline, brine groove T1102 is used for storing brine and passes through the pipeline with brine and carry to mixed reation kettle L1101 in, ammonium bicarbonate feeding device N103 is used for carrying ammonium bicarbonate to mixed reation kettle L1101 in, reaction balance cauldron L1104 and first solid-liquid separation equipment 2 intercommunication.
All be equipped with the feed inlet on mixing reation kettle L1101, crystal nucleus growth cauldron L1102, particle growth cauldron L1103 and reaction balance cauldron L1104's the kettle cover, mixing reation kettle L1101, crystal nucleus growth cauldron L1102, particle growth cauldron L1103 and reaction balance cauldron L1104's cauldron body bottom all is equipped with the discharge gate.
The first-stage sodium bicarbonate precipitation device 1 of the invention adopts four kettles, namely a mixing reaction kettle L1101, a crystal nucleus growing kettle L1102, a particle growing kettle L1103 and a reaction balance kettle L1104, to replace one kettle in the prior art, in the double decomposition reaction process, reactants (ammonium bicarbonate and sodium chloride in brine) are firstly stirred and mixed in the mixing reaction kettle L1101, the stirred and mixed solution enters the crystal nucleus growing kettle L1102 from the mixing reaction kettle L1101, crystals with large crystal structures are firstly conveyed into the particle growing kettle L1103 from the bottom of the crystal nucleus growing kettle L1102 through a pipeline, the crystals with small crystal structures continue to grow and slowly crystallize in the crystal nucleus growing kettle L1102, and the like, the crystals with large crystal structures in each kettle are conveyed into the next kettle, so that the growing space of the crystals with small crystal structures in the kettle is enlarged, the crystallization time is prolonged, and the phenomena that the nucleation rate is high due to crystallization in one kettle are effectively avoided, The phenomenon of large crystal nucleus quantity and high crystallization speed reduces the formation of fine crystals, further improves the filtration and separation effect of subsequent baking soda crystals, further improves the yield and preparation efficiency of baking soda, and reduces the preparation cost of baking soda.
Mixing reation kettle L1101, crystal nucleus growth cauldron L1102, particle growth cauldron L1103 and reaction balance cauldron L1104's kettle cover's top all installs agitator motor, agitator motor is connected with the (mixing) shaft, in the bottom of (mixing) shaft stretches into mixing reation kettle L1101, crystal nucleus growth cauldron L1102, particle growth cauldron L1103 and reaction balance cauldron L1104 respectively, and be equipped with a plurality of stirring thick liquids 7 on it, stirring thick liquid 7 sets up respectively in the height of the three difference of (mixing) shaft, and the contained angle that is located between not co-altitude stirring thick liquid 7 and the horizontal plane reduces along the direction of top to bottom of (mixing) shaft gradually. The method specifically comprises the following steps: the stirring paddles 7 at the uppermost level are at an angle of 30 to 32 (see a in fig. 1) (31 in this embodiment), the stirring paddles 7 at the intermediate level are at an angle of 24 to 26 (see b in fig. 1) (25 in this embodiment), and the stirring paddles 7 at the lowermost level are at an angle of 22 to 24 (see c in fig. 1) (23 in this embodiment) with respect to the horizontal plane.
According to the invention, the included angles between the stirring paddles 7 at different heights and the horizontal plane are gradually reduced along the direction from the top to the bottom of the stirring shaft, so that the contact area between the crystals above the kettle bodies and the corresponding stirring shaft and the shearing stress generated by the solution on the stirring shaft are larger than those below the crystals, the number of crystal nuclei in the kettle is ensured to meet the production requirement, the number of new crystal nuclei formed by particles on the crystals below due to the shearing stress and the contact with the stirring shaft can be effectively reduced, the growth space of each crystal grain below the kettle body is increased, the crystal grains below the kettle body are coarsened and then conveyed to the next kettle body for continuous crystallization, and meanwhile, the growth space is also reserved for the growth of each crystal grain above the kettle body.
The reaction balance kettle L1104 is further connected with a heat exchange device, the heat exchange device comprises a heat exchange tube 8 and a steam boiler (not shown in the figure), the heat exchange tube 8 is coiled in the reaction balance kettle L1104, an air inlet of the heat exchange tube is connected with an air outlet of the steam boiler, and an air outlet of the heat exchange tube is connected with an air inlet of the steam boiler. The solution in the reaction equilibrium kettle L1104 is heated by a heat exchange device, so that the dissolution of ammonium chloride in the solution and the crystallization and precipitation of baking soda are promoted, and the preparation is made for the subsequent filtration of crystal mush.
First solid-liquid separation equipment 2 specifically is the centrifuge P101 of vacuum filter X101 and vacuum filter X101 intercommunication that communicates in proper order, vacuum filter X101 and reaction balance cauldron L1104 intercommunication for the magma after reaction balance cauldron L1104 filters, and it still is connected with knockout drum V104, knockout drum V104 intercommunication has one-level liquid storage pot V106, centrifuge P101 is connected with one-level liquid storage pot V106, be used for carrying the liquid that thick tassels centrifugal dehydration obtained to one-level liquid storage pot V106 in, one-level liquid storage pot V106 with sink sodium device intercommunication, and its storage has this liquid as thick mother liquor M1 of liquid through vacuum filter X101 and centrifuge P101 separation in it, centrifuge P101 still has deamination device 6 through pipe connection.
The sodium precipitation device 3 comprises a first sodium precipitation kettle L2105 and a second sodium precipitation kettle L2106 which are sequentially communicated, wherein the top end of the first sodium precipitation kettle L2105 is connected with a salt metering scale L1107 for conveying sodium chloride into the first sodium precipitation kettle L2105, the feed end of the first sodium precipitation kettle L2105 is connected with a primary liquid storage tank V106 of the first solid-liquid separation device 2, the primary liquid storage tank V106 is used for conveying crude mother liquid M1 in the primary liquid storage tank V106 into the first sodium precipitation kettle L2105 to further react the sodium chloride with residual ammonium bicarbonate in the crude mother liquid M1, and the discharge end of the second sodium precipitation kettle L2106 is communicated with a second solid-liquid separation device 4 and used for separating slurry output from the second sodium precipitation kettle L2106 to obtain baking soda and refined mother liquid M1.
The second solid-liquid separation device 4 is respectively communicated with the ammonium chloride preparation device and the first-stage sodium bicarbonate precipitation device 1, and is used for respectively inputting the refined mother liquor M1 obtained by separation of the second solid-liquid separation device 4 and sodium bicarbonate into the ammonium chloride preparation device and the first-stage sodium bicarbonate precipitation device 1, and the method specifically comprises the following steps: the vacuum filter X102, the separating tank V108 and the secondary liquid storage tank V109 are sequentially communicated, the vacuum filter X102 is further communicated with a second sodium precipitation kettle L2106 through a pipeline, is used for filtering crystal slurry input into the second sodium precipitation kettle L2106, is further communicated with a mixing reaction kettle L1101, is used for returning baking soda obtained through filtering separation into the mixing reaction kettle L1101, and is communicated with an ammonium chloride preparation device, and is used for conveying a refined mother solution M1 into the ammonium chloride preparation device to prepare ammonium chloride.
The second sodium precipitation kettle L2106 is also connected with a heat exchange device, the structure of the heat exchange device is the same as that of the heat exchange device connected with the reaction balance kettle L1104, a heat exchange tube 6 of the heat exchange device is coiled in the second sodium precipitation kettle L2106, the air inlet of the heat exchange device is connected with the air outlet of a steam boiler, and the air outlet of the heat exchange device is connected with the air inlet of the steam boiler.
According to the invention, by arranging the sodium precipitation device 3 and the second solid-liquid separation device 4, the residual ammonium bicarbonate in the crude mother liquor M1 separated by the first solid-liquid separation device 2 and the added sodium chloride can further undergo a double decomposition reaction to generate the baking soda, the baking soda separated by the second solid-liquid separation device 4 is returned to the mixing reaction kettle L1101, and the obtained refined mother liquor M1 is conveyed to the ammonium chloride preparation device, so that the content of ammonium bicarbonate in the refined mother liquor M1 in the cold separation and crystallization process performed by the ammonium chloride preparation device is effectively reduced, the reaction of ammonium bicarbonate and sodium chloride in the cold separation process is prevented, the phenomenon that the baking soda and the ammonium chloride formed in the cold separation process are difficult to separate is further avoided, the content of sodium salt in the ammonium chloride is reduced, the content of ammonia in the ammonium chloride is improved, and the yield of the baking soda is also effectively improved.
The ammonium chloride preparation device comprises a cold separation device 9, a salting-out device 10 and an ammonium chloride treatment device 11, wherein the cold separation device 9 is used for carrying out cold separation crystallization on the refined mother liquor M1 obtained by separation of the second solid-liquid separation device 4 and comprises a crystallization kettle T1116, an external cooler Y115 and an ice machine P113, the crystallization kettle T1116 is respectively communicated with the external cooler Y115 and the secondary liquid storage tank V109, and clear liquid at the upper end in the crystallization kettle T1116 is conveyed to the external cooler Y115, cooled by the external cooler Y115 and returned to the crystallization kettle T1116 for cold separation crystallization; the external cooler Y115 is circularly communicated with the ice maker P113, an exchange tube is arranged in the external cooler Y115, the ammonium chloride treatment device 11 is communicated with the cold separation device 9 and used for filtering, dehydrating and drying the ammonium chloride separated out in the cold separation device 9, and the ammonium chloride treatment device comprises a vacuum filter X124, a centrifuge X129 and a sack closer K130 which are sequentially connected.
The salting-out device 10 is used for collecting overflow liquid discharged by the cold-separating device 9 and carrying out salting-out crystallization on the overflow liquid, the salting-out device 10 comprises a salting-out kettle T1118 and a salt feeding device B120, the salt feeding device B120 is communicated with the salting-out kettle T1118 and is used for adding reaction salt into the salting-out kettle T1118, and the feeding end of the salting-out kettle T1118 is communicated with the crystallization kettle T1116 and is used for collecting overflow liquid discharged by the crystallization kettle T1116 and carrying out salting-out crystallization on the overflow liquid.
Salting out cauldron T1118 includes clear liquid section, linkage segment and suspension section, the height of suspension section is 3m, the clear liquid section is equipped with the overflow mouth, overflow mouth and second grade are appeared and are linked up with baking soda device 5, the side of linkage segment is 60 with the contained angle of vertical direction, the suspension section is equipped with two magma and takes out the mouth, the magma is taken out the mouth and is set up apart from suspension section top 3/4 department, the magma is taken out the mouth and is connected with and divides salt cauldron V112, divides the feed end and the magma at salt cauldron V112 top to take out the mouth intercommunication, be equipped with the center tube in the salt cauldron V112, the pipeline that the magma of salting out cauldron T1118 was taken out the mouth and is connected with and divides salt cauldron V112 top stretches into in the center tube through the feed end at salt cauldron V112 top for with the ammonium chloride magma input after salting out cauldron T1118 crystallization divides in the salt cauldron V112.
The middle part of the side wall of the salt separation kettle V112 is provided with a slurry taking port, and the bottom of the salt separation kettle V112 is communicated with the salting-out kettle T1118 through a pipeline, so that solid salt dissolved in the salt separation kettle V112 is returned to the salting-out kettle T1118 to be recycled, and the ammonium chloride preparation cost is saved; get the thick liquid mouth and be connected through the pipeline with the top of crystallization kettle T1116 for in carrying the ammonium chloride crystal to crystallization kettle T1116, for crystallization kettle T1116 provides the ammonium chloride crystal nucleus, promote the ammonium chloride crystal growth in the crystallization kettle T1116, precipitate the ammonium chloride crystal in making crystallization kettle T1116 fast, energy-conserving festival.
The salt separation kettle V112 is also connected with the crystal slurry taking-out port of the salting-out kettle T1118, the crystal slurry containing ammonium chloride crystals and solid salt after being salted out from the salting-out kettle T1118 can be conveyed into the salt separation kettle V112 through the crystal slurry taking-out port, the ammonium chloride crystals are light in shape, the volume of the salting-out kettle T1118 is large, the pressure discharged by the salting-out kettle T1118 is large, the ammonium chloride is suspended in the salt separation kettle V112, the solid salt is precipitated at the bottom of the salt separation kettle V112 and dissolved, the ammonium chloride crystals are separated from the solid salt after being suspended and conveyed into the crystallization kettle T1116 from the pulp taking port, the increase of the ammonium chloride crystals in the crystallization kettle T1116 is promoted, the phenomenon that the salt content of the ammonium chloride in the ammonium chloride product from the crystallization kettle T1116 is high due to the fact that the crystal slurry containing the ammonium chloride crystals and the solid salt is directly conveyed into the crystallization kettle T1116 can be effectively avoided, and the phenomenon that the sodium ions in the ammonium chloride product from the crystallization kettle T1116 exceed the standard can be prevented, the produced ammonium chloride reaches the agricultural standard, effectively improves the product quality of the ammonium chloride.
The secondary sodium bicarbonate precipitation device 5 comprises a concentration tank V121, a heating kettle L2121-1 and a centrifuge S122 which are sequentially communicated, wherein the concentration tank V121 is used for collecting overflow liquid overflowing from the salting kettle T1118, and the heating kettle L2121-1 is used for heating the overflow liquid to further precipitate sodium bicarbonate; the centrifuge S122 is used for separating the baking soda further precipitated in the heating kettle L2121-1 from the mother liquor, and the baking soda separated by the centrifuge S122 enters a drying device F109 and a bag sewing machine K110 for drying and packaging to obtain the baking soda.
The mother liquor circulating device comprises a three-stage liquid storage tank V125, a stirrer is arranged in the three-stage liquid storage tank V125 at a position far from the bottom 1/4, the bottom of the stirrer is communicated with a heating kettle L2121-1 and is used for returning suspension at the bottom in the three-stage liquid storage tank V125 to the heating kettle L2121-1, the stirrer is also communicated with a centrifugal machine S122, a vacuum filter X124 and a centrifugal machine X129 through pipelines respectively, the stirrer is used for collecting mother liquor obtained by separating the centrifugal machine S122 of the second-stage sodium bicarbonate separating device 5, the mother liquor obtained by separating the vacuum filter X124 and the centrifugal machine X129 of the ammonium chloride processing device 11, and supernatant of the mother liquor is returned to a brine tank T1102 and the deamination device for cyclic utilization as mother liquor M2.
Deamination device 6 is including the first deamination cauldron 12, second deamination cauldron 13 and the third deamination cauldron 14 that communicate in proper order, the feed end and the centrifuge P101 intercommunication of first deamination cauldron 7 for carry the coarse baking soda that obtains through centrifuge P101 centrifugation to first deamination cauldron 12 in, and first deamination cauldron 12 passes through pipeline and mother liquor circulating device intercommunication, be used for further with the coarse baking soda reaction in the first deamination cauldron 12 in carrying mother liquor M2 that mother liquor circulating device collected to first deamination cauldron 12.
According to the invention, the deamination device 6 is arranged, the secondary sodium bicarbonate precipitation device 5 and the mother liquor M2 generated by the ammonium chloride preparation device are conveyed into the first deamination kettle 12 to further react with the crude sodium bicarbonate in the first deamination kettle 12, so that the undecomposed solid sodium bicarbonate remained in the crude sodium bicarbonate further reacts with the sodium chloride in the mother liquor M2 to generate the sodium bicarbonate, the content of ammonium salt in the sodium bicarbonate is effectively reduced, the content of the ammonium salt in the sodium bicarbonate is ensured to be lower than 1000ppM, the yield of the sodium bicarbonate is improved, and the quality of the sodium bicarbonate product is improved; the three deamination kettles are arranged, so that the residual ammonium bicarbonate reacts with sodium chloride step by step, the growth space of crystal grains is enlarged, the reaction time is prolonged, the contact between the brine and the ammonium bicarbonate is effectively promoted, the formation of baking soda is promoted, and the yield of the baking soda is improved; in addition, the addition of the mother liquor M2 can further dilute the residual ammonium chloride on the crude baking soda, thereby reducing the difficulty of subsequent washing, improving the solubility of the ammonium chloride and facilitating the separation of the ammonium chloride and the baking soda.
The third deamination kettle 14 is also connected with a heat exchange device, the structure of the heat exchange device is the same as that of the heat exchange device connected with the reaction balance kettle L1104, a heat exchange tube 8 of the heat exchange device is coiled in the third deamination kettle 14, the air inlet of the heat exchange device is connected with the air outlet of a steam boiler, and the air outlet of the heat exchange device is connected with the air inlet of the steam boiler.
The bottom of the third deamination kettle 14 is sequentially connected with a third solid-liquid separation device 15 and a drying device F109 through pipelines, the third solid-liquid separation device 15 is used for separating mother liquor and fine soda generated in the third deamination kettle 9 to obtain semi-brine, fine soda and washing liquor, and specifically comprises a belt filter X103 and a centrifuge P102 communicated with the belt filter X103, a liquid outlet of the belt filter X103 is connected with a washing water tank P103 through a pipeline, the top of the belt filter X103 is also connected with a semi-brine tank V110, the semi-brine tank V110 is communicated with a first sodium precipitation kettle L2105 and used for returning front half-section filtrate filtered by the belt filter X103 as semi-brine to the first sodium precipitation kettle for recycling, a water outlet of the washing water tank P103 is connected with a spray header of the belt filter X103 through a pipeline, and a water outlet of the washing water tank is also connected with an outer washing tank V107 through a pipeline and used for storing the washing liquor into the outer washing tank V107, and then the washing liquid is conveyed into the external cooler to wash the external cooler and the exchange tubes in the external cooler. It should be noted that the belt filter of the present invention is a belt filter having a washing or rinsing function as in the prior art, such as the belt filter disclosed in patent application No. CN 201820348308.9.
The drying device F109 is used for drying the separated baking soda, and is communicated with a sack closer K110 and used for packaging the dried baking soda to obtain the finished baking soda.
The outer washing groove V107 is circularly communicated with the outer cooler Y115 through a pipeline, and the specific structure is as follows: the lower part of the side wall of the outer wash tank V107 is communicated with the top of the outer cooler Y115 through a pipeline, the top of the outer wash tank V107 is communicated with the bottom of the outer cooler Y115 through a pipeline, wash liquor stored in the outer wash tank V107 is conveyed from the top of the outer cooler Y115 through the pipeline from the outer wash tank V107, then is returned to the outer wash tank V107 from the pipeline at the bottom of the outer cooler Y115 after being conveyed from the top of the outer cooler Y115 through the pipeline, and is used for circularly and repeatedly washing scar blocks attached to the inner wall of the outer cooler Y115 and the outer wall of the exchange tube.
According to the invention, the outer washing tank V107 for storing the washing liquid obtained by separation of the third solid-liquid separation device 15 is arranged, the outer washing tank V107 is communicated with the outer cooler Y115 in a circulating manner through the pipeline, and the washing liquid in the outer washing tank V107 is adopted to wash the ammonium chloride crystals scarred on the inner wall of the outer cooler Y115 and the outer wall of the exchange column pipe in a reciprocating circulating manner.
The bottom of the external cooler Y115 is also connected with a replacement tank V111 through a pipeline, the replacement tank V111 is communicated with the crystallization kettle T1116 through a pipeline, the final flushing liquid can be stored in the replacement tank V111 after being cleaned, and is conveyed into the crystallization kettle T1116 from the replacement tank V111 through a pipeline, so that ammonium chloride crystals in the flushing liquid are further crystallized in the crystallization kettle T1116, the aim of zero discharge of the flushing liquid is fulfilled, and the problem that the discharge of waste liquid cannot reach the discharge standard due to direct discharge of the flushing liquid in the prior art is avoided; and the washing liquid is recycled to the crystallization kettle T1116 internal medicine to effectively recycle the ammonium chloride in the washing liquid, so that the loss of the ammonium chloride is reduced, and the yield of the ammonium chloride is improved.
The invention relates to a working principle and a using method of a device for preparing ammonium chloride by co-producing sodium bicarbonate, which comprises the following steps:
1) first-stage separation of sodium bicarbonate: directly adding 8.5 cubic meters of unpurified saturated brine into a mixed reaction kettle L1101 with the capacity of 11 cubic meters through a brine tank T1102, heating to 35 ℃, adding 2200 kilograms of ammonium bicarbonate into the mixed reaction kettle L1101 through an ammonium bicarbonate feeding device N103 ammonium bicarbonate metering belt, and controlling the temperature to be 25 ℃ under the stirring action to perform double decomposition reaction; when the mixing reaction kettle L1101 is nearly full, a valve at the kettle bottom of the mixing reaction kettle L1101 is opened, a pump is started, slurry is sent into a crystal nucleus growth kettle L1102, stirring is continued, and the temperature is controlled to be 28 ℃; when the crystal nucleus growing kettle L1102 is about to be full, a valve at the bottom of the crystal nucleus growing kettle L1102 is opened, a pump is started, slurry is sent into the particle growing kettle L1103, stirring is continued, and the temperature is controlled to be 28 ℃; when the particle growth kettle L1103 is nearly full, a valve at the bottom of the particle growth kettle L1103 is opened, a pump is started, slurry is sent to a reaction equilibrium kettle L1104, the temperature is kept at 29 ℃, the total reaction time is 1.30h, baking soda is generated, the slurry containing the baking soda is filtered by a vacuum filter X101, and then a centrifuge P101 is used for dehydrating to obtain crude baking soda and crude mother liquor M1;
the double decomposition reaction and the baking soda crystallization in the step are carried out step by step in a mixing reaction kettle L1101, a crystal nucleus growing kettle L1102, a particle growing kettle L1103 and a reaction equilibrium kettle L1104, when the previous kettle body is full, part of feed liquid is conveyed to the next kettle, the baking soda crystallization time is prolonged, and compared with the operation of simultaneously carrying out reaction and crystallization by only adopting one kettle body, the crystal grain growing space is increased, the obtained baking soda crystals are thicker, the filtering effect is effectively improved, the baking soda preparation efficiency is improved, and the baking soda yield is effectively improved;
2) precipitating sodium: the crude mother liquor M1 is collected into a first-stage liquid storage tank V106, then conveyed into a first sodium precipitation kettle L2105, sodium chloride is added into the first sodium precipitation kettle L2105 through a salt metering scale L1107, so that the residual ammonium bicarbonate and sodium chloride in the crude mother liquor M1 further undergo double decomposition reaction, and the mass ratio of the ammonium bicarbonate in the crude mother liquor M1 to the added sodium chloride is as follows: 80:7, controlling the temperature in the first sodium precipitation kettle L2105 to be 22 ℃, when the first sodium precipitation kettle L2105 is about to be full, opening a valve at the bottom of the first sodium precipitation kettle L2105, conveying the slurry into the second sodium precipitation kettle L2106, controlling the temperature of the second sodium precipitation kettle L2106 to be 35 ℃, and precipitating sodium for 1.5 hours; filtering the slurry reacted in the second sodium precipitation kettle L2106 by a filter X102, and then sequentially conveying the slurry to a filter to obtain a refined mother liquor M1 and baking soda, wherein the baking soda is returned to the mixed reaction kettle L1101;
according to the invention, by arranging a sodium precipitation step, the residual ammonium bicarbonate in the crude mother liquor M1 obtained by separation in the step 1) and the added sodium chloride are further subjected to double decomposition reaction, the sodium bicarbonate obtained by filtration and separation is returned to the mixing reaction kettle L1101 in the step 1), and the obtained refined mother liquor M1 is conveyed to the cold separation crystallization in the subsequent step 3), so that the ammonium bicarbonate is decomposed by the crude mother liquor M1 before entering the cold separation crystallization, the content of ammonium bicarbonate in the refined mother liquor M1 entering the cold separation crystallization is effectively reduced, the reaction of ammonium bicarbonate and sodium chloride in the cold separation process is prevented, the phenomenon that the sodium bicarbonate and the ammonium chloride formed in the cold separation process are difficult to separate is further avoided, the content of sodium salt in the ammonium chloride is reduced, the content of ammonia in the ammonium chloride is improved, and the yield of the sodium bicarbonate is also effectively improved;
3) and (3) cold separation and crystallization: collecting the refined mother liquor M1 to a secondary liquid storage tank V107, directly conveying the refined mother liquor into a 9 cubic meter crystallization kettle T1116, simultaneously adding ammonium sulfate serving as a divalent anion activator into the crystallization kettle T1116, circularly communicating the crystallization kettle T1116 with an ice maker P113 through an external cooler Y115, controlling the temperature to be 8 ℃, freezing for 6 hours, crystallizing and separating out ammonium chloride, filtering the ammonium chloride by a vacuum filter X124, dehydrating the ammonium chloride by a centrifuge X129, and packaging the ammonium chloride by a bag sewing machine X129 to obtain a finished product ammonium chloride;
4) salting out and crystallizing: overflowing the cold-separated and crystallized overflow liquid from the crystallization kettle T1116 to a salting-out kettle T1118, simultaneously adding sodium chloride into the salting-out kettle T1118 through a salt feeding device B120, controlling the temperature at 10 ℃, salting out for 6h, further crystallizing and separating out ammonium chloride, and settling to an outlet at the middle lower part of the salting-out kettle T1118, namely a crystal paddle taking outlet of a suspension section;
6) salt separation: conveying ammonium chloride which is deposited into the salt separation kettle V112 from a crystal slurry taking-out port of the salt separation kettle T1118 to the salt separation kettle V112, precipitating sodium chloride remained on ammonium chloride crystals into the bottom of the salt separation kettle V112, dissolving the sodium chloride and then returning the ammonium chloride to the salt separation kettle T1118 for recycling, floating the ammonium chloride crystals to the slurry taking-out port of the salt separation kettle V112, returning the ammonium chloride crystals to the crystallization kettle T1116 from the slurry taking-out port, collecting the ammonium chloride crystals with the ammonium chloride crystals which are frozen and separated out from the crystallization kettle T1116, conveying the ammonium chloride crystals to a low-level tank V117, filtering the ammonium chloride crystals by a vacuum filter X124, dehydrating by a centrifuge X129, and packaging by a bag sewing machine X129 to obtain a finished product of ammonium chloride;
7) and (3) secondary sodium bicarbonate precipitation: the supernatant in the salting-out kettle T1118 overflows to a thickening tank V121, flows to a heating kettle L2121-1 through the bottom of the thickening tank V121, baking soda is further separated out at the temperature of 35 ℃, the obtained baking soda is dehydrated by a centrifuge S122 and then is conveyed to a drying device F109 for drying, and the dried baking soda is packaged by a bag sewing machine K110 to obtain the finished product baking soda;
8) mother liquor circulation: collecting the brine generated by separating ammonium chloride in the steps 3) and 6) and the brine generated in the step 7) into a three-stage liquid storage tank V125, allowing the suspension to sink to the bottom under the action of stirring, returning to a heating kettle L2121-1, allowing clear liquid to float upwards to serve as mother liquid M2, heating to 35 ℃, returning a part of the mother liquid M2 to a mixing reaction kettle L1101, performing double decomposition reaction with ammonium bicarbonate to produce sodium bicarbonate, repeatedly operating, and recycling, so as to achieve the purpose of no wastewater discharge; the other part of mother liquor M2 is input into a deamination device 6 to carry out the subsequent deamination step;
9) and (3) deamination: feeding the crude baking soda into a first deamination kettle 12, mixing the crude baking soda with mother liquor M2 input into the first deamination kettle 12, and carrying out double decomposition reaction again to further carry out double decomposition reaction on ammonium bicarbonate remained in the crude baking soda and sodium chloride in the mother liquor M2, wherein the solid-to-liquid ratio is 2.5:1, when the first deamination kettle 12 is about to be full, opening a valve at the bottom of the first deamination kettle 12, and feeding the slurry into a second deamination kettle 13; when the second deamination kettle 13 is about to be full, a valve at the bottom of the second deamination kettle 13 is opened, slurry is sent into a third deamination kettle 14, the total deamination time is 1-1.3h, the temperature is controlled to be 25 ℃, fine soda is generated, the fine soda is filtered by a belt filter X103 and then washed by 100L of deionized water or saturated soda water at the temperature of 35 ℃, the first half-section filtrate obtained by filtering is used as semi-brine and sent into a first sodium precipitation kettle L2105, the washing liquid obtained by washing is used for subsequently washing an external cooler, the solid obtained by filtering is dewatered by a centrifugal machine P102 and dried by a drying device F109 drying furnace, and the dried sodium bicarbonate is packaged by a bag sewing machine K110 to obtain a finished product of sodium bicarbonate;
10) cleaning: conveying the washing liquid obtained by washing in the step 9) into an external cooler Y1115, repeatedly washing the inner wall of the external cooler Y1115 and the outer wall of an exchange tube in the external cooler Y1115, and finally conveying the final washing liquid into a crystallization kettle T1116 for cold crystallization;
the components in the crude mother liquor M1 are controlled as follows: NaCl 100-4HCO3 100-110g/L、NH4Cl 190-210g/L、SO4 2-1-8 g/L; the components in the mother liquor M1 are controlled as follows: NaCl 130-4HCO3 50-60g/L、NH4Cl 190-210g/L、SO4 2- 1-8 g/L; the components in the mother liquor M2 are controlled as follows: NaCI 230-4CI 60g-100g/L、NH4HCO3 30g-70g/L、SO4 2- 1-8g/L。
Comparative example 1
The present invention employs the device of patent application No. cn201910000923.x as comparative example 1 to the present invention.
Comparative example 2
This comparative example differs from example 1 in that: baking soda device 1 is appeared including mixing reation kettle L1101, brine groove T1102 and ammonium bicarbonate feeding device N103 to the one-level, brine groove T1102 and ammonium bicarbonate feeding device N103 and reation kettle intercommunication.
Comparative example 3
This comparative example differs from example 1 in that: does not comprise a sodium precipitation device and a second solid-liquid separation device, and directly communicates the primary liquid storage tank with the cold separation device.
Comparative example 4
This comparative example differs from example 1 in that: does not comprise a salt separation kettle, and directly communicates a crystal slurry taking-out port of the salt separation kettle with a crystallization kettle.
Comparative example 5
This comparative example differs from example 1 in that: the deamination device and the third solid-liquid separation device are not included, and the crude baking soda separated by the first solid-liquid separation device is directly conveyed to the drying device for drying.
Comparative example 6
This comparative example differs from example 1 in that: an outer wash tank in circulation communication with the outer cooler and a replacement tank in communication with the bottom of the outer cooler are not included.
The apparatus of example 1 and comparative examples 1-6 and the corresponding methods of use were used to prepare baking soda and ammonium chloride according to the present invention, with the results shown in the following table:
Figure DEST_PATH_IMAGE002
it will be further understood that the terms "first," "second," "third," "fourth," and the like, may be used herein to describe various elements, but these elements should not be limited by these terms. These terms are only used to distinguish one element from another.
As used herein, the terms "upper," "lower," "left," "right," and the like are used for convenience of description based on the orientation as shown in the figures of the drawings, which may vary from one actual device to another depending on the manner in which the device is arranged.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (10)

1. The utility model provides a device of baking soda coproduction preparation ammonium chloride, includes that the one-level that communicates in proper order is appeared baking soda device and first solid-liquid separation equipment, is the ammonium chloride preparation facilities that communicate in proper order, is appeared baking soda device and mother liquor circulating device to the second grade, its characterized in that: still including deposiing sodium device and second solid-liquid separation equipment, it includes the first cauldron of deposiing sodium and the second cauldron of deposiing sodium that communicates in proper order to deposit the sodium device, the top of the first cauldron of deposiing sodium is connected with the salt weigher, and its feed end is connected with first solid-liquid separation equipment, is used for carrying the crude mother liquor M1 of sodium chloride and first solid-liquid separation equipment separation to the first cauldron of deposiing sodium in respectively, the discharge end and the second solid-liquid separation equipment intercommunication of the second cauldron of deposiing sodium, the baking soda device intercommunication is appeared with ammonium chloride preparation facilities and one-level respectively to the second solid-liquid separation equipment for the refined mother liquor M1 and the baking soda that obtain the separation of second solid-liquid separation equipment input ammonium chloride preparation facilities respectively and one-level precipitate baking soda device.
2. The apparatus for co-producing sodium bicarbonate and preparing ammonium chloride according to claim 1, characterized in that: the second sinks the sodium cauldron and still is connected with heat exchange device, heat exchange device includes hot exchange pipe and steam boiler, the heat exchange tube dish is located the second and sinks in the sodium cauldron, and its air inlet is connected with steam boiler's gas outlet, and its gas outlet is connected with steam boiler's air inlet.
3. The apparatus for co-producing sodium bicarbonate and preparing ammonium chloride according to claim 1, characterized in that: the one-level sodium bicarbonate precipitation device comprises a mixing reaction kettle, a crystal nucleus growing kettle, a particle growing kettle and a reaction balance kettle which are sequentially communicated, the mixing reaction kettle is further respectively and simply connected with a brine tank and an ammonium bicarbonate feeding device through pipelines, and the reaction balance kettle is communicated with a first solid-liquid separation device.
4. The apparatus for co-producing sodium bicarbonate and preparing ammonium chloride according to claim 3, characterized in that: mixing reation kettle, crystal nucleus growth cauldron, the long cauldron of particle and reaction balance cauldron's kettle cover's top all installs agitator motor, agitator motor is connected with the (mixing) shaft, in the bottom of (mixing) shaft stretched into mixing reation kettle, crystal nucleus growth cauldron, the long cauldron of particle and reaction balance cauldron respectively, and be equipped with a plurality of stirring thick liquids on it, the contained angle that is located between not co-altitude stirring thick liquid and the horizontal plane reduced along the direction of top to bottom of (mixing) shaft gradually.
5. The apparatus for co-producing sodium bicarbonate and preparing ammonium chloride according to claim 1, characterized in that: the device still includes the deamination device, the deamination device is including the first deamination cauldron, second deamination cauldron and the third deamination cauldron that communicate in proper order, the feed end and the first solid-liquid separation equipment intercommunication of first deamination cauldron for carry the crude baking soda that first solid-liquid separation equipment separation obtained to first deamination cauldron in, and first deamination cauldron passes through pipeline and mother liquor circulating device intercommunication, be used for carrying the second grade that mother liquor circulating device collected to appear baking soda device and the mother liquor M2 that ammonium chloride preparation facilities produced to first deamination cauldron in with the further reaction of crude baking soda.
6. The apparatus for co-producing sodium bicarbonate and ammonium chloride according to claim 5, wherein: the third deamination cauldron has connected gradually third solid-liquid separation equipment and drying device through the pipeline, third solid-liquid separation equipment is arranged in separating the mother liquor that generates in the third deamination cauldron with tiny soda, drying device is used for the tiny soda after the drying separation.
7. The apparatus for co-producing sodium bicarbonate and ammonium chloride according to claim 6, wherein: the ammonium chloride preparation facilities includes cold separation device, salting out device and ammonium chloride processing apparatus, the cold separation device is used for carrying out the cold separation crystallization with smart mother liquor M1, and it includes crystallization kettle and the external cooler with crystallization kettle intercommunication, the external cooler still has ice maker circulation intercommunication through pipeline circulation intercommunication, and its inside exchange tubulation that is equipped with, the salting out device is used for collecting the overflow liquid of cold separation device exhaust and carries out the salting out crystallization to it, and it includes the salting out cauldron and with the salt feeding device of salting out cauldron intercommunication, the ammonium chloride processing apparatus is arranged in filtering, dehydration and drying process to the ammonium chloride that separates out in the cold separation device.
8. The apparatus for co-producing sodium bicarbonate and ammonium chloride according to claim 7, wherein: the external cooler is circularly communicated with an external washing tank through a pipeline, the external washing tank is communicated with a third solid-liquid separation device and used for storing washing liquid obtained by separation from the third solid-liquid separation device, the washing liquid is conveyed from the top of the external cooler into the external cooler through the pipeline from the external washing tank, and then returns to the external washing tank from the pipeline at the bottom of the external cooler and is used for circularly and repeatedly washing scar blocks attached to the inner wall of the external cooler and the outer pipe wall of the exchange tube.
9. The apparatus for co-producing sodium bicarbonate and ammonium chloride according to claim 7, wherein: the bottom of the external cooler is also connected with a replacement tank through a pipeline, and the replacement tank is communicated with the crystallization kettle through a pipeline.
10. The apparatus for co-producing sodium bicarbonate and ammonium chloride according to claim 7, wherein: the salting-out cauldron is from last to including clear solution section, linkage segment and suspension section down, the clear solution section is equipped with the overflow mouth, the overflow mouth is connected with dense groove, the suspension section is equipped with at least one magma and takes out the mouth, the magma is taken out the mouth and is connected with the salt separation cauldron, the lateral wall of salt separation cauldron passes through the pipeline and is connected with the top of crystallization cauldron.
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CN216426772U (en) * 2021-11-30 2022-05-03 衡阳爱洁科技股份有限公司 Device for preparing ammonium chloride by co-production of sodium bicarbonate

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114751430A (en) * 2022-04-07 2022-07-15 湖南化工设计院有限公司 Method for preparing baking soda and coproducing ammonium chloride by low-temperature bidirectional salting-out circulation method
CN114751430B (en) * 2022-04-07 2023-12-01 湖南化工设计院有限公司 Method for producing sodium bicarbonate and co-producing ammonium chloride by low-temperature bidirectional salting-out circulation method
CN117756140A (en) * 2024-02-22 2024-03-26 南京新筛分科技实业有限公司 process in sodium carbonate production

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