CN1224694A - Ammonium chloride recovering process from ammonium chloride containing waste liquid - Google Patents

Ammonium chloride recovering process from ammonium chloride containing waste liquid Download PDF

Info

Publication number
CN1224694A
CN1224694A CN99100015A CN99100015A CN1224694A CN 1224694 A CN1224694 A CN 1224694A CN 99100015 A CN99100015 A CN 99100015A CN 99100015 A CN99100015 A CN 99100015A CN 1224694 A CN1224694 A CN 1224694A
Authority
CN
China
Prior art keywords
effect
liquid
pump
evaporation
ammonium chloride
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN99100015A
Other languages
Chinese (zh)
Other versions
CN1084298C (en
Inventor
赵景利
任宝山
胡修慈
史小平
张少峰
阎文军
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hebei University of Technology
Hebei Polytechnic University
Original Assignee
Hebei University of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hebei University of Technology filed Critical Hebei University of Technology
Priority to CN99100015A priority Critical patent/CN1084298C/en
Publication of CN1224694A publication Critical patent/CN1224694A/en
Application granted granted Critical
Publication of CN1084298C publication Critical patent/CN1084298C/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

Links

Classifications

    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/10Process efficiency
    • Y02P20/129Energy recovery, e.g. by cogeneration, H2recovery or pressure recovery turbines

Abstract

The present invention adopts multiple effect heat pump vacuum evaporation technology and the technological processes include double-effect downstream process, triple-effect or quadruple-effect mixing process and cooling crystallization of the evaporated liquid in the crystallizer to produce ammonium chloride solid. The cooling water is used circularly. The said process eliminates the environmental pollution of waste liquid, produces no secondary pollution, has low production cost and high production efficiency, and is suitable for recovering ammonium chloride from various ammonium chloride containing waste liquid.

Description

A kind of method that from the waste liquid that contains ammonium chloride, reclaims ammonium chloride
The invention belongs to a kind of method that reclaims ammonium chloride, particularly a kind of method that from the waste liquid that contains ammonium chloride, reclaims ammonium chloride.
In the process of method for producing potassium carbonate by ion exchange, give off a large amount of waste liquids at present, contain about ammonium chloride of about 10% in the waste liquid, almost suitable with the output of salt of wormwood.A large amount of undressed waste liquids directly discharge, and are not only the waste of industrial chemicals, and the more important thing is environment is caused serious pollution.From the waste liquid that contains ammonium chloride, reclaim ammonium chloride two big difficult points are arranged: the one, because it is lower to contain the concentration of ammonium chloride in the waste liquid, reclaim ammonium chloride and just must remove large quantity of moisture earlier, thereby energy consumption is bigger, cost is too high.The 2nd, ammonium chloride solution is extremely strong to the corrodibility of equipment, and it is not all right that its equipment adopts the common metal material, must use expensive titanium material, and this has increased the weight of to reclaim the cost of ammonium chloride again.Even adopt titanium material equipment, under temperature, concentration condition with higher, still there is stronger etching problem.A kind of ammonium chloride by combined alkali process evaporation technology and equipment are disclosed in the CN1075694A patent document, though what describe in the file also is to adopt triple effect evaporation to analyse crystalline ammonium, but, second effect is the flasher that does not heat, be actually two effects and add the flash distillation operation, therefore, steam utilization is lower, energy saving is less, and cost is still higher.The pump feed evaporator that uses in vapo(u)rization system in addition need be equipped with the forced circulation pump of big flow first in vaporizer, this kind pump leaks easily, maintenance often, each maintenance needs to stop; Second the recycle pump current consumption of the big flow of this kind is higher; Three are easy to generate fouling owing to containing crystallization in the solution in the vaporizer, and not only influence is conducted heat, and often parking is cleaned, so working rate is not high, and wastes energy, production efficiency is lower.
The objective of the invention is to overcome weak point of the prior art and a kind of method that reclaims ammonium chloride from the waste liquid that contains ammonium chloride is provided.This method adopts multiple-effect vacuum-evaporation, the Low Temperature Steam heating, and secondary steam and recirculated water are reused.Therefore can reduce the corrosion of ammonium chloride solution to equipment, save energy reduces cost, and enhances productivity, and reduces environmental pollution.
Purpose of the present invention can realize by following measure:
The processing step that reclaims ammonium chloride from the waste liquid that contains ammonium chloride is as follows:
1. stock liquid (1) (waste liquid that contains ammonium chloride) (below be evaporated liquid all represent with fine line) is after concentrate pump (2) pressurization, the exhaust steam preheater (3) and first of flowing through is imitated after each later single-effect evaporator heating chamber is preheated to 70~85 ℃, enter the evaporation of first single-effect evaporator heating chamber (6) internal heating again, its solution boiling point control is at 85~96 ℃, concentration reaches 20~25%, and in the first effect vapor-liquid separation chamber (7), carry out vapour, liquid separates, the liquid of separating is squeezed in the flasher (9) with an effect pump (8), liquid after flash distillation enters in last single-effect evaporator heating chamber again and continues to be heated evaporation, its solution boiling point control is at 55~75 ℃, concentration reaches 30~35%, and at the indoor vapour that carries out of this single-effect evaporator vapor-liquid separation, liquid separates, the steam of separating enters the exhaust steam preheater and carries out condensation, simultaneously stock liquid and mother liquor is heated; The liquid of separating continues to be heated evaporation with this effect pump 1st effective evaporator heating chamber of reaching the last, its solution boiling point control is at 65~85 ℃, after being evaporated to concentration and being 32~37%, separate at the indoor vapour, liquid of carrying out of this single-effect evaporator vapor-liquid separation, the liquid of separating is squeezed in the crystallizer tank (14) with this effect pump and is carried out crystallisation by cooling, and the solid ammonium chloride that crystallization goes out is finished product (27) after whizzer (25) drying, moisture eliminator (26) drying;
2. the mother liquor (representing) in the crystallizer tank with fine line with mother liquor pump (15) squeeze into be preheating to 50~65 ℃ in the exhaust steam preheater (3) after, enter single-effect evaporator heating chamber second from the bottom and carry out heating evaporation;
3. livings steam (16) that comes by boiler and the shell side that after heat pump (17) compresses, enters the first single-effect evaporator heating chamber (6) through the part secondary steam (all representing) that the first single-effect evaporator vapor-liquid separation chamber (7) separates jointly with heavy line, the heating chamber temperature is 100~105 ℃, another part secondary steam of being separated by the first single-effect evaporator vapor-liquid separation chamber (7) enters the shell side of the second single-effect evaporator heating chamber, as thermal source second single-effect evaporator being carried out Heating temperature is 80~90 ℃, and the like, the last secondary steam of being separated by last evaporator vapor-liquid separation chamber enters exhaust steam preheater (3) condensation, simultaneously to stoste, mother liquor heats, condensing temperature is at 60~70 ℃, the tail vapour that is come out by the exhaust steam preheater enters in the barometric condenser (18), the direct condensation of water vapor is wherein got off, what condensation was got off drops in the water sealed tank (19) under water, use pump (20) that water is wherein squeezed in the water cooling tower (21) again, portion water in the water cooling tower is returned barometric condenser (18) internal recycle by pump (22) and is used, and the non-condensable gases in the barometric condenser (representing with thick dotted line) is taken emptying away with vacuum pump (23);
4. water of condensation in each single-effect evaporator heating chamber shell side and the water of condensation (dotting) in the exhaust steam preheater are taken away with pump (24).
Above-mentioned technology vaporizer in multi-effect evaporation system adopts falling-film evaporator.Because in multi-effect evaporation system, adopted Low Temperature Steam heating and vacuum-evaporation, make total effectively heat transfer temperature difference diminish.Total be exactly falling-film evaporator is realized a kind of mode of heating evaporation preferably of multiple-effect evaporation under less heat transfer temperature difference.
The steam heat pump adopts steam jet heat pump in the above-mentioned technology.The secondary steam compression back that first single-effect evaporator is evaporated is heated first single-effect evaporator together with giving birth to steam, and this just makes low-grade steam (secondary steam) become higher-grade steam and uses, thereby can further cut down the consumption of energy.
Adopting barometric condenser and vacuum pump in the above-mentioned technology, is vacuum-evaporation to guarantee multi-effect evaporation system.In multi-effect evaporation system, liquid phase is a negative-pressure operation, or first single-effect evaporator be micro-pressure operation, all the other each effects are negative-pressure operation, therefore can reduce the boiling point of solution in each single-effect evaporator, generally speaking, the boiling point control of solution is at 85~104 ℃ in first single-effect evaporator, and the boiling point control of solution is between 55~75 ℃ in the third effect evaporator.Thereby can reduce the corrosion of ammonium chloride solution to equipment.
Two effects or triple effect or quadruple effect evaporation technology are adopted in the evaporation that contains the chlorination waste liquor of ammonium, and imitate use steam thermo-compression evaporation first, its flow process mode is two effect following current flow processs, and triple effect or quadruple effect are the mixed flow flow process, and extremely last effect is mobile in proper order in order to imitate from first for the vapour phase trend.Liquid phase enters triple effect for imitating from first to flasher, come out second to imitate from triple effect again, finishes liquid and imitates from second and be discharged to crystallizer tank; The quadruple effect evaporation technology is first to imitate second and imitate and to arrive flasher again, and flasher comes out to quadruple effect again to triple effect, finishes liquid and is discharged to the crystallizer tank crystallization from triple effect.
The cooling water that uses among the present invention recycles in its internal system.The water that the barometric condenser condensation is got off is squeezed into water cooling tower by pump, by pump portion water is returned barometric condenser again and recycles.Only need to replenish a small amount of water in the production and can satisfy production requirement, saved water resources, environment is not produced secondary pollution.
The present invention compared with prior art has following advantage:
1, save energy.Process using multiple-effect evaporation of the present invention (two imitate following current, triple effect and quadruple effect mixed flow flow process) is repeatedly utilized secondary steam, thereby has reduced the consumption of living steam; Imitate first and to have used thermo-compression evaporation, become higher-grade steam after making low-grade steam through the heat pump compression to use, thus further save energy; Recirculated water in the production process is reused, thereby has saved water consumption one time.This has just solved and reclaimed the big difficult problem of ammonium chloride energy consumption from the waste liquid that contains ammonium chloride.
2, process using multiple-effect of the present invention vacuum-evaporation has reduced and has respectively imitated the boiling point of solution, thereby reduced the corrosion of ammonium chloride solution to equipment, has solved from the waste liquid that contains ammonium chloride when reclaiming ammonium chloride ammonium chloride solution to another difficult problem of equipment corrosion.
3, production efficiency height.The present invention uses falling-film evaporator; the recycle pump of two low discharges is set outside vaporizer; open one and be equipped with one; guarantee not shut down in the falling-film evaporator production, in addition, the present invention does not reach capacity the solution in the vapo(u)rization system; thereby there is not crystallization to separate out in the vaporizer; it is few to produce dirt layer chance, makes and cleans the vaporizer cycle stretch-out, and working rate is higher.In addition, the present invention has used the recycle pump of low discharge, and current consumption is less.
4, reduced production cost.Owing to reduced the corrosion of ammonium chloride solution to equipment, prolonged the work-ing life of equipment, thereby reduced facility investment; Energy consumption in the production process has reduced, and its comprehensive production cost is reduced greatly.
The drawing of accompanying drawing is described as follows:
Fig. 1 is a Production Flow Chart synoptic diagram of the present invention.
Fine line express liquid among the figure; Dotted line is represented recirculated water; Heavy line is represented steam; Dotted line is represented water of condensation.
Below in conjunction with accompanying drawing the embodiment of the invention is described in further detail:
Embodiment 1
1. concentrate pump (2) will contain ammonium chloride 10%, temperature is that 20 ℃ ion-exchange waste liquid (1) (below be evaporated liquid all represent with fine line) is got to exhaust steam preheater (3) and triple effect, second imitates the interior continuously pre-heating to 82 of falling-film evaporator heating chamber (4) and (5) ℃, the flow of pump is 5000kg/h, then enter first and imitate the evaporation of falling-film evaporator heating chamber (6) internal heating, the solution boiling point control is at 96 ℃, concentration reaches 25%, and in the first effect vapor-liquid separation chamber (7), carry out vapour, liquid separates, the liquid of separating is squeezed into flasher (9) with an effect pump (8), steam after flash distillation enters triple effect falling-film evaporator heating chamber shell side, liquid after flash distillation enters in the triple effect falling-film evaporator (4) again and continues to be heated evaporation, the solution boiling point control is at 70 ℃, concentration reaches 32%, and in triple effect falling-film evaporator vapor-liquid separation chamber (10), carry out vapour, liquid separates, the steam of separating enters the exhaust steam preheater and carries out condensation, and stock liquid and mother liquor are heated; The liquid of separating is squeezed into the second effect falling-film evaporator (5) with triple effect pump (11) and is continued to be heated evaporation, the solution boiling point control is at 78 ℃, concentration reaches 36%, and second imitate carry out vapour in the falling-film evaporator vapor-liquid separation chamber (12), liquid separates, the liquid of separating is squeezed in the crystallizer tank (14) with two effect pumps (13) and is carried out crystallisation by cooling, and the solid ammonium chloride that crystallizes out carries out finished product (27) packing after whizzer (25) drying and moisture eliminator (26) drying.Its crystallization content is the 500kg/h anhydrous ammonium chloride.
2. be that flow density falls in the minimum that guarantees the normal evaporation of falling-film evaporator, each single-effect evaporator all has the part evaporated liquor to carry out self-circulation.Squeeze into the interior preheating of exhaust steam preheater (3) by the mother liquor that crystallizer tank comes out with mother liquor pump (15), be preheating to after 62 ℃ and and imitate in the stoste pipe of falling-film evaporator (5), enter the second effect falling-film evaporator heating chamber with stoste and carry out heating evaporation to entering second.The internal circulating load of mother liquor is 8000kg/h.
3. livings steam (16) (pressure is the 0.8MPa gauge pressure) that comes by boiler and the shell side that after pump (17) compression, enters the first effect falling-film evaporator heating chamber (6) through the part secondary steam (all representing) that the first single-effect evaporator vapor-liquid separation chamber (7) separates jointly with heavy line, the first single-effect evaporator heating chamber is heated, and the heating chamber temperature is controlled at 100 ℃.Imitate another part secondary steam that falling-film evaporator vapor-liquid separation chamber (7) separates by first and enter second shell side of imitating falling-film evaporator heating chamber (5), as thermal source the second single-effect evaporator heating chamber is heated, the heating chamber temperature is controlled at 88 ℃.Imitate secondary steam that falling-film evaporator vapor-liquid separation chamber (12) separates by second and enter triple effect falling-film evaporator heating chamber (4) and heat, the heating chamber temperature is controlled at 76 ℃.The secondary steam of being separated by triple effect falling-film evaporator vapor-liquid separation chamber (10) enters exhaust steam preheater (3) and carries out partial condensation, simultaneously stoste and mother liquor is heated, and condensing temperature is controlled at 62 ℃.Enter in the barometric condenser (18) directly water vapor condensation wherein to be got off by the exhaust steam preheater uncooled tail vapour that comes out, water of condensation enters in the water sealed tank (19), squeeze in the water cooling tower (21) by pump (20), cooled water is squeezed into barometric condenser by pump (22) again.Non-condensable gases is taken away with vacuum pump (23)., keeping vacuum tightness is 650mmHg, to guarantee vapo(u)rization system vacuum-evaporation.
4. respectively imitating water of condensation in the falling-film evaporator heating chamber shell side and the water of condensation (all dotting) in the exhaust steam preheater takes away with pump (24).
Total steam consumption is 1520kg/h.
Embodiment 2
1. concentrate pump (2) will contain ammonium chloride 11.5%, temperature is that 20 ℃ ion-exchange waste liquid (1) (below be evaporated liquid all represent with fine line) is got to exhaust steam preheater (3) and triple effect, second imitates the interior continuously pre-heating to 82 of falling-film evaporator heating chamber (4) and (5) ℃, the flow of pump is 4350kg/h, then enter first and imitate the evaporation of falling-film evaporator heating chamber (6) internal heating, the solution boiling point control is at 94 ℃, concentration reaches 25%, and in the first effect vapor-liquid separation chamber (7), carry out vapour, liquid separates, the steam of separating enters the exhaust steam preheater and carries out condensation, and stock liquid and mother liquor are heated; The liquid of separating is squeezed into flasher (9) with an effect pump (8), steam after flash distillation enters triple effect falling-film evaporator heating chamber shell side, liquid after flash distillation enters and continues heating evaporation in the triple effect falling-film evaporator (4), the solution boiling point control is at 70 ℃, concentration reaches 32%, and in triple effect falling-film evaporator vapor-liquid separation chamber (10), carry out vapour, liquid separates, the liquid of separating is squeezed into the second effect falling-film evaporator (5) with triple effect pump (11) and is continued to be heated evaporation, the solution boiling point control is at 80 ℃, concentration reaches 37%, and in the second effect falling-film evaporator vapor-liquid separation chamber (12), carry out vapour, liquid separates, the liquid of separating is squeezed in the crystallizer tank (14) with two effect pumps (13) and is carried out crystallisation by cooling, and the solid ammonium chloride that crystallizes out carries out finished product (27) packing after whizzer (25) drying and moisture eliminator (26) drying.Its crystallization content is the 500kg/h anhydrous ammonium chloride.
2. be that flow density falls in the minimum that guarantees the normal evaporation of falling-film evaporator, each single-effect evaporator all has the part evaporated liquor to carry out self-circulation.Squeeze into the interior preheating of exhaust steam preheater (3) by the mother liquor that crystallizer tank comes out with mother liquor pump (15), be preheating to after 65 ℃ and and imitate in the stoste pipe of falling-film evaporator (5), enter the second effect falling-film evaporator heating chamber with stoste and carry out heating evaporation to entering second.The internal circulating load of mother liquor is 3850kg/h.
3. livings steam (16) (pressure is the 0.8MPa gauge pressure) that comes by boiler and the shell side that after pump (17) compression, enters the first effect falling-film evaporator heating chamber (6) through the part secondary steam (all representing) that the first single-effect evaporator vapor-liquid separation chamber (7) separates jointly with heavy line, the first single-effect evaporator heating chamber is heated, and the heating chamber temperature is controlled at 104 ℃.Imitate another part secondary steam that falling-film evaporator vapor-liquid separation chamber (7) separates by first and enter second shell side of imitating falling-film evaporator heating chamber (5), as thermal source the second single-effect evaporator heating chamber is heated, the heating chamber temperature is controlled at 90 ℃.Imitate secondary steam that falling-film evaporator vapor-liquid separation chamber (12) separates by second and enter triple effect falling-film evaporator heating chamber (4) and heat, the heating chamber temperature is controlled at 78 ℃.The secondary steam of being separated by triple effect falling-film evaporator vapor-liquid separation chamber (10) enters exhaust steam preheater (3) and carries out partial condensation, and condensing temperature is controlled at 65 ℃.Entered in the barometric condenser (18) directly water vapor condensation wherein to be got off by the exhaust steam preheater uncooled tail vapour that comes out, water of condensation enters in the water sealed tank (19), squeezes in the water cooling tower (21) by pump (20), squeezes into barometric condenser by pump (22) again.Non-condensable gases is taken away with vacuum pump (23)., keeping vacuum tightness is 640mmHg, to guarantee vapo(u)rization system vacuum-evaporation.
4. respectively imitating water of condensation in the falling-film evaporator heating chamber shell side and the water of condensation (all dotting) in the exhaust steam preheater takes away with pump (24).
Total steam consumption is 1420kg/h.
Embodiment 3
1. concentrate pump (2) will contain ammonium chloride 11.5%, temperature is that 20 ℃ ion-exchange waste liquid (1) (below be evaporated liquid all represent with fine line) is got to exhaust steam preheater (3) and second and imitated the interior continuously pre-heating to 75 of falling-film evaporator heating chamber (5) ℃, the flow of pump is 4350kg/h, then enter first and imitate the evaporation of falling-film evaporator heating chamber (6) internal heating, the solution boiling point control is at 86 ℃, concentration reaches 33%, and in the first effect vapor-liquid separation chamber (7), carry out vapour, liquid separates, the liquid of separating is squeezed into flasher with an effect pump (8), steam after flash distillation enters second and imitates falling-film evaporator heating chamber shell side, the liquid of being separated by flasher enters second and imitates in the falling-film evaporator (5) and continue to be heated evaporation, the solution boiling point control is at 66 ℃, concentration reaches 35%, and in the second effect falling-film evaporator vapor-liquid separation chamber (12), carry out vapour, liquid separates, the steam of separating enters the exhaust steam preheater and carries out condensation, and stock liquid and mother liquor are heated; The liquid of separating is squeezed in the crystallizer tank (14) with two effect pumps (13) and is carried out crystallisation by cooling, and the solid ammonium chloride that crystallizes out carries out finished product (27) packing after whizzer (25) drying and moisture eliminator (26) drying.Its crystallization content is the 500kg/h anhydrous ammonium chloride.
2. be that flow density falls in the minimum that guarantees the normal evaporation of falling-film evaporator, each single-effect evaporator all has the part evaporated liquor to carry out self-circulation.Squeeze into the interior preheating of exhaust steam preheater (3) by the mother liquor that crystallizer tank comes out with mother liquor pump (15), be preheating to after 55 ℃ and and imitate in the stoste pipe of falling-film evaporator heating chamber (5), enter the second effect falling-film evaporator heating chamber with stoste and carry out heating evaporation to entering second.The internal circulating load of mother liquor is 8000kg/h.
3. livings steam (16) (pressure is the 0.8MPa gauge pressure) that comes by boiler and the shell side that after pump (17) compression, enters the first effect falling-film evaporator heating chamber (6) through the part secondary steam (all representing) that the first single-effect evaporator vapor-liquid separation chamber (7) separates jointly with heavy line, the first single-effect evaporator heating chamber is heated, and the heating chamber temperature is controlled at 100 ℃.Imitate another part secondary steam that falling-film evaporator vapor-liquid separation chamber (7) separates by first and enter second shell side of imitating falling-film evaporator heating chamber (5), as thermal source the second single-effect evaporator heating chamber is heated, the heating chamber temperature is controlled at 82 ℃.Imitate secondary steam that falling-film evaporator vapor-liquid separation chamber (12) separates by second and enter exhaust steam preheater (3) and carry out partial condensation, condensing temperature is controlled at 60 ℃.Enter in the barometric condenser (18) directly water vapor condensation wherein to be got off by the exhaust steam preheater uncooled tail vapour that comes out, water of condensation enters in the water sealed tank (19), squeeze in the water cooling tower (21) by pump (20), squeeze into barometric condenser by pump (22) again when needing.Non-condensable gases is taken away with vacuum pump (23), and keeping vacuum tightness is 620mmHg, to guarantee vapo(u)rization system vacuum-evaporation.
4. respectively imitating water of condensation in the falling-film evaporator heating chamber shell side and the water of condensation (all dotting) in the exhaust steam preheater takes away with pump (24).
Total steam consumption is 1780kg/h.

Claims (6)

1, a kind of method that from the waste liquid that contains ammonium chloride, reclaims ammonium chloride, it is characterized in that: the processing step of this method is as follows:
1. stock liquid (1) (waste liquid that contains ammonium chloride) (below be evaporated liquid all represent with fine line) is after concentrate pump (2) pressurization, the exhaust steam preheater (3) and first of flowing through is imitated after each later single-effect evaporator heating chamber is preheated to 70~90 ℃, enter the evaporation of first single-effect evaporator heating chamber (6) internal heating again, its solution boiling point control is at 85~104 ℃, concentration reaches 20~25%, and in the first effect vapor-liquid separation chamber (7), carry out vapour, liquid separates, the liquid of separating is squeezed in the flasher (9) with an effect pump (8), liquid after flash distillation enters in last single-effect evaporator heating chamber again and continues heating evaporation, its solution boiling point control is at 55~75 ℃, concentration reaches 30~33%, and at the indoor vapour that carries out of this single-effect evaporator vapor-liquid separation, liquid separates, the steam of separating enters the exhaust steam preheater and carries out condensation, simultaneously stock liquid and mother liquor are heated, the liquid of separating continues to be heated evaporation with this effect pump 1st effective evaporator heating chamber of reaching the last, its solution boiling point control is at 65~85 ℃, after being evaporated to concentration and being 32~37%, at the indoor vapour that carries out of this single-effect evaporator vapor-liquid separation, liquid separates, the liquid of separating is squeezed in the crystallizer tank (14) with this effect pump and is carried out crystallisation by cooling, and the solid ammonium chloride that crystallization goes out is finished product (27) behind whizzer (25) and moisture eliminator (26);
2. the mother liquor (representing) in the crystallizer tank with fine line with mother liquor pump (15) squeeze into be preheating to 50~65 ℃ in the exhaust steam preheater (3) after, enter single-effect evaporator heating chamber second from the bottom and carry out heating evaporation;
3. livings steam (16) that comes by boiler and the shell side that after heat pump (17) compresses, enters the first single-effect evaporator heating chamber (6) through the part secondary steam (all representing) that the first single-effect evaporator vapor-liquid separation chamber (7) separates jointly with heavy line, the heating chamber temperature is 100~110 ℃, another part secondary steam of being separated by the first single-effect evaporator vapor-liquid separation chamber (7) enters the shell side of the second single-effect evaporator heating chamber (5), as thermal source second single-effect evaporator being carried out Heating temperature is 80~90 ℃, and the like, the last secondary steam of being separated by last evaporator vapor-liquid separation chamber enters exhaust steam preheater (3) condensation, simultaneously to stoste, mother liquor heats, condensing temperature is at 60~70 ℃, the tail vapour that is come out by the exhaust steam preheater enters in the barometric condenser (18), water vapor condensation is wherein got off, water of condensation drops in the water sealed tank (19), use pump (20) that water is wherein squeezed in the water cooling tower (21) again, portion water in the water cooling tower is returned barometric condenser (18) internal recycle by pump (22) and is used, and the non-condensable gases in the barometric condenser (representing with thick dotted line) is taken emptying away with vacuum pump (23);
4. water of condensation in each single-effect evaporator heating chamber shell side and the water of condensation (dotting) in the exhaust steam preheater are taken away with pump (24).
2, according to the said method of claim 1, it is characterized in that: heat pump adopts steam jet heat pump, and each single-effect evaporator adopts falling-film evaporator.
3, according to claim 1 or 2 said methods, it is characterized in that: vapo(u)rization system adopts vacuum-evaporation, and its vacuum tightness is 600~700mmHg.
4, according to the said method of claim 1 to 3, it is characterized in that: adopt two to imitate evaporation technology to the evaporation that contains the chlorination waste liquor of ammonium, its flow process mode is two effect following current flow processs, and the vapour phase trend is mobile in proper order to second effect for imitating from first; Liquid phase enters second effect again for imitating to flasher from first, finishes liquid and is discharged to the crystallizer tank crystallization from second effect.
5, according to the said method of claim 1 to 3, it is characterized in that: triple effect evaporation technology is adopted in the evaporation that contains the chlorination waste liquor of ammonium, and its flow process mode is a triple effect mixed flow flow process, and the vapour phase trend is mobile in proper order to triple effect again for imitating to second effect from first; Liquid phase enters triple effect for imitating from first again to flasher, come out second to imitate from triple effect again, finishes liquid and imitates from second and be discharged to the crystallizer tank crystallization.
6, according to the said method of claim 1 to 3, it is characterized in that: the quadruple effect evaporation technology is adopted in the evaporation that contains the chlorination waste liquor of ammonium, and its flow process mode is a quadruple effect mixed flow flow process, and the vapour phase trend is for mobile in proper order to quadruple effect again to second effect, triple effect from first effect; Liquid phase is imitated for imitating second from first, imitates from second and enters quadruple effect again after coming out to flasher, comes out to finish liquid and to be discharged to the crystallizer tank crystallization from triple effect to triple effect from quadruple effect again.
CN99100015A 1999-01-06 1999-01-06 Ammonium chloride recovering process from ammonium chloride containing waste liquid Expired - Fee Related CN1084298C (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN99100015A CN1084298C (en) 1999-01-06 1999-01-06 Ammonium chloride recovering process from ammonium chloride containing waste liquid

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN99100015A CN1084298C (en) 1999-01-06 1999-01-06 Ammonium chloride recovering process from ammonium chloride containing waste liquid

Publications (2)

Publication Number Publication Date
CN1224694A true CN1224694A (en) 1999-08-04
CN1084298C CN1084298C (en) 2002-05-08

Family

ID=5269730

Family Applications (1)

Application Number Title Priority Date Filing Date
CN99100015A Expired - Fee Related CN1084298C (en) 1999-01-06 1999-01-06 Ammonium chloride recovering process from ammonium chloride containing waste liquid

Country Status (1)

Country Link
CN (1) CN1084298C (en)

Cited By (24)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100415645C (en) * 2006-09-30 2008-09-03 阮玉根 Process of producing ammonium chloride with waste circuit board etching solution
CN100537428C (en) * 2006-07-13 2009-09-09 中芯国际集成电路制造(上海)有限公司 Device for reclaiming ammonium chloride and titanium tetrachloride complex compound
CN101935128A (en) * 2010-07-22 2011-01-05 上海西恩化工设备有限公司 Process for treating wastewater comprising high-concentration ammonium salt and sodium salt
CN102020389A (en) * 2010-11-19 2011-04-20 杭州蓝然环境技术有限公司 Process for recycling ammonium chloride waste water
CN102020327A (en) * 2010-09-21 2011-04-20 广州市心德实业有限公司 Ammonia nitrogen waste water treatment equipment
CN101445449B (en) * 2008-12-17 2011-09-21 山东凯翔生物化工有限公司 Production method and device for sodium gluconate energy-saving triple effect concentration and crystallization
CN102489028A (en) * 2011-12-27 2012-06-13 赵晨 Mother liquor evaporation system
CN102657946A (en) * 2012-04-20 2012-09-12 中国天辰工程有限公司 Method for recovering and preparing ammonium sulfate from acrylonitrile device
CN102690010A (en) * 2011-03-24 2012-09-26 镇江市丹徒区江南热镀锌有限公司 Resource integrated utilization and treatment method of hydrochloric acid pickling waste liquid
CN103083931A (en) * 2013-02-06 2013-05-08 四川省洪雅青衣江元明粉有限公司 Multiple-effect forced circulation vacuum evaporation system
CN103303942A (en) * 2013-06-08 2013-09-18 湖北兴发化工集团股份有限公司 Method and device for recycling ammonium chloride from glycine mother liquor
CN103708487A (en) * 2013-12-25 2014-04-09 河北工业大学 Process for recycling boric acid and magnesium sulfate from boric acid mother solution
CN104860460A (en) * 2014-12-05 2015-08-26 浙江龙盛集团股份有限公司 Processing device for aniline intermediate production waste water
CN103768808B (en) * 2014-01-23 2015-09-09 南京航空航天大学 Some vapor recompression evaporation concentration system and method
CN106277117A (en) * 2016-08-27 2017-01-04 闫三朋 The ammonium chloride waste-water independent low temperature double-effect evaporation method and apparatus of double adverse current
CN107058732A (en) * 2017-05-29 2017-08-18 新疆新鑫矿业股份有限公司阜康冶炼厂 A kind of nickel minerals pressurization method of invading out
CN107381911A (en) * 2017-06-09 2017-11-24 石家庄新奥环保科技有限公司 A kind of integrated conduct method of amion acetic acid waste water
CN107504823A (en) * 2016-12-30 2017-12-22 华北水利水电大学 A kind of organic Rankine bottoming cycle afterheat generating system based on falling film evaporator
CN108469355A (en) * 2018-06-08 2018-08-31 华能国际电力股份有限公司 A kind of power plant carbonated drink sampler and sampling method on the spot
CN108585089A (en) * 2018-05-24 2018-09-28 苏州鼎昌节能环保科技有限公司 A kind of sodium chloride ammonium chloride divides salt crystallization processes and device
CN108715496A (en) * 2018-06-07 2018-10-30 全南县新资源稀土有限责任公司 A method of recycling ammonia from Rare Earth Separation waste liquid
CN109437238A (en) * 2018-12-29 2019-03-08 广州市迈源科技有限公司 A kind of ammonium chloride solution processing system and ammonium chloride solution processing method
CN111013170A (en) * 2019-12-26 2020-04-17 聊城鲁西聚酰胺新材料科技有限公司 Caprolactam water solution energy-saving evaporation system and method
CN111302419A (en) * 2020-01-06 2020-06-19 中伟新材料股份有限公司 Process for solving problem of high evaporation boiling point of ammonia chloride by utilizing MVR

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101544437B (en) * 2009-04-30 2011-04-27 河北工业大学 Process method for recovering ammonium chloride and sodium chloride from waste water containing ammonium chloride and sodium chloride

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS534800A (en) * 1976-07-02 1978-01-17 Hitachi Ltd Recovery method of ammonium halide
JPS5435200A (en) * 1977-08-25 1979-03-15 Toyo Soda Mfg Co Ltd Separating method of ammonium chloride from mixture of ammonium chloride and ethylene amine hydrochloride
JPS60212288A (en) * 1984-04-05 1985-10-24 Mitsubishi Metal Corp Treatment of waste water containing ammonium ion and fluorine ion
CN1075694A (en) * 1992-02-25 1993-09-01 邓天洲 Ammonium chloride by combined alkali process evaporation technology and equipment

Cited By (28)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100537428C (en) * 2006-07-13 2009-09-09 中芯国际集成电路制造(上海)有限公司 Device for reclaiming ammonium chloride and titanium tetrachloride complex compound
CN100415645C (en) * 2006-09-30 2008-09-03 阮玉根 Process of producing ammonium chloride with waste circuit board etching solution
CN101445449B (en) * 2008-12-17 2011-09-21 山东凯翔生物化工有限公司 Production method and device for sodium gluconate energy-saving triple effect concentration and crystallization
CN101935128A (en) * 2010-07-22 2011-01-05 上海西恩化工设备有限公司 Process for treating wastewater comprising high-concentration ammonium salt and sodium salt
CN102020327A (en) * 2010-09-21 2011-04-20 广州市心德实业有限公司 Ammonia nitrogen waste water treatment equipment
CN102020389A (en) * 2010-11-19 2011-04-20 杭州蓝然环境技术有限公司 Process for recycling ammonium chloride waste water
CN102690010A (en) * 2011-03-24 2012-09-26 镇江市丹徒区江南热镀锌有限公司 Resource integrated utilization and treatment method of hydrochloric acid pickling waste liquid
CN102489028A (en) * 2011-12-27 2012-06-13 赵晨 Mother liquor evaporation system
CN102657946A (en) * 2012-04-20 2012-09-12 中国天辰工程有限公司 Method for recovering and preparing ammonium sulfate from acrylonitrile device
CN103083931A (en) * 2013-02-06 2013-05-08 四川省洪雅青衣江元明粉有限公司 Multiple-effect forced circulation vacuum evaporation system
CN103303942B (en) * 2013-06-08 2015-04-29 湖北兴发化工集团股份有限公司 Method and device for recycling ammonium chloride from glycine mother liquor
CN103303942A (en) * 2013-06-08 2013-09-18 湖北兴发化工集团股份有限公司 Method and device for recycling ammonium chloride from glycine mother liquor
CN103708487B (en) * 2013-12-25 2015-09-02 河北工业大学 The technique of boric acid and magnesium sulfate is reclaimed from mother liquid of boric acid
CN103708487A (en) * 2013-12-25 2014-04-09 河北工业大学 Process for recycling boric acid and magnesium sulfate from boric acid mother solution
CN103768808B (en) * 2014-01-23 2015-09-09 南京航空航天大学 Some vapor recompression evaporation concentration system and method
CN104860460A (en) * 2014-12-05 2015-08-26 浙江龙盛集团股份有限公司 Processing device for aniline intermediate production waste water
CN106277117A (en) * 2016-08-27 2017-01-04 闫三朋 The ammonium chloride waste-water independent low temperature double-effect evaporation method and apparatus of double adverse current
CN107504823A (en) * 2016-12-30 2017-12-22 华北水利水电大学 A kind of organic Rankine bottoming cycle afterheat generating system based on falling film evaporator
CN107504823B (en) * 2016-12-30 2019-01-11 华北水利水电大学 A kind of Organic Rankine Cycle afterheat generating system based on falling film evaporator
CN107058732A (en) * 2017-05-29 2017-08-18 新疆新鑫矿业股份有限公司阜康冶炼厂 A kind of nickel minerals pressurization method of invading out
CN107058732B (en) * 2017-05-29 2019-03-01 新疆新鑫矿业股份有限公司阜康冶炼厂 A kind of nickel minerals pressure leaching method
CN107381911A (en) * 2017-06-09 2017-11-24 石家庄新奥环保科技有限公司 A kind of integrated conduct method of amion acetic acid waste water
CN108585089A (en) * 2018-05-24 2018-09-28 苏州鼎昌节能环保科技有限公司 A kind of sodium chloride ammonium chloride divides salt crystallization processes and device
CN108715496A (en) * 2018-06-07 2018-10-30 全南县新资源稀土有限责任公司 A method of recycling ammonia from Rare Earth Separation waste liquid
CN108469355A (en) * 2018-06-08 2018-08-31 华能国际电力股份有限公司 A kind of power plant carbonated drink sampler and sampling method on the spot
CN109437238A (en) * 2018-12-29 2019-03-08 广州市迈源科技有限公司 A kind of ammonium chloride solution processing system and ammonium chloride solution processing method
CN111013170A (en) * 2019-12-26 2020-04-17 聊城鲁西聚酰胺新材料科技有限公司 Caprolactam water solution energy-saving evaporation system and method
CN111302419A (en) * 2020-01-06 2020-06-19 中伟新材料股份有限公司 Process for solving problem of high evaporation boiling point of ammonia chloride by utilizing MVR

Also Published As

Publication number Publication date
CN1084298C (en) 2002-05-08

Similar Documents

Publication Publication Date Title
CN1084298C (en) Ammonium chloride recovering process from ammonium chloride containing waste liquid
CN101544437B (en) Process method for recovering ammonium chloride and sodium chloride from waste water containing ammonium chloride and sodium chloride
CN102616973B (en) Method and device for processing high-saline organic wastewater
CN105110542A (en) Zero-discharge salt separation and purification method for industrial high-salt wastewater
CN207877494U (en) Lithium battery nickel-cobalt-manganese ternary presoma waste water treatment system
WO2006094437A1 (en) A method and an multi-effect evaporation for waste water of alkylene oxides
CN209052424U (en) A kind of high-salt wastewater energy conservation evaporation and crystallization system
CN103935966A (en) Recycling process of waste sulfuric acid from corrosion of electrode foil
CN106746136A (en) The technique of zero discharge and system of a kind of desulfurization wastewater
CN108558098A (en) A kind of method for treating desulfurized wastewater and device
CN109095531A (en) Garbage flying ash wash water recycling treatment process and equipment
CN103394206B (en) High-efficiency energy-saving hydrochloric acid pickling waste liquor triple-effect negative-pressure graphite evaporation crystallizer
CN105417510A (en) Method for achieving ammonium chloride cooperative production through ADC foaming agent wastewater by means of total-hydrochloric acid pure hydrazine hydrate condensation
CN103833050A (en) Treatment method of ammonium chloride-containing aminoacetic acid dealcoholization mother liquor
CN109053424A (en) System and method of the field of new materials from multiple types acetic acid devil liquor recovery purification acetic acid
CN205528218U (en) One imitates useless water separator of limbs MVR mixed salt
CN105439184A (en) Resource utilization method of distilled ammonia waste liquid during sodium carbonate production and preparation system
CN109809437A (en) Novel energy-saving environment-friendly heavy soda ash production technology and system
CN205528225U (en) Desulfurization waste water zero release processing system
CN1927702A (en) Energy-saving process of producing hydrazine hydrate
CN209922933U (en) Sodium chloride forced circulation crystallization device in flue gas desulfurization waste water
CN108658353B (en) Calcium chloride wastewater treatment process
CN102464346A (en) Seven-effect falling film evaporation technology for sodium aluminate solution
CN206970384U (en) A kind of Zero discharging system of desulfurization wastewater
CN1608716A (en) Method of recovering waste sulfuric acid and waste gas produced in tatanium dioxide production

Legal Events

Date Code Title Description
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C06 Publication
PB01 Publication
C14 Grant of patent or utility model
GR01 Patent grant
C56 Change in the name or address of the patentee
CP03 Change of name, title or address

Inventor after: Zhao Jingli

Inventor after: Ren Baoshan

Inventor after: Hu Xiuci

Inventor after: Shi Xiaoping

Inventor after: Zhang Shaofeng

Inventor after: Yan Wenjun

Inventor before: Zhao Jingli

Inventor before: Ren Baoshan

Inventor before: Hu Xiuci

Inventor before: Shi Xiaoping

Inventor before: Zhang Shaofeng

Inventor before: Yan Wenjun

CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20020508

Termination date: 20130106

CF01 Termination of patent right due to non-payment of annual fee