CN105439184A - Resource utilization method of distilled ammonia waste liquid during sodium carbonate production and preparation system - Google Patents
Resource utilization method of distilled ammonia waste liquid during sodium carbonate production and preparation system Download PDFInfo
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Abstract
The invention relates to a resource utilization method of distilled ammonia waste liquid during sodium carbonate production and a preparation system. The preparation system mainly comprises a collection tank, a pretreatment filter, an evaporator, a quadruple-effect sodium chloride crystallizer, a triple-effect sodium chloride crystallizer, a double-effect sodium chloride crystallizer and a single-effect calcium chloride crystallizer which are connected sequentially, wherein a steam outlet of the single-effect calcium chloride crystallizer is sequentially connected with the double-effect sodium chloride crystallizer, the triple-effect sodium chloride crystallizer and the quadruple-effect sodium chloride crystallizer; a steam outlet of the quadruple-effect sodium chloride crystallizer is connected with a condenser. The resource utilization method of distilled ammonia waste liquid during sodium carbonate production is implemented through a pretreatment filtrating system, a one-section evaporation and concentration system, a two-section forced circulation and crystallized concentration system and a three-section forced circulation and crystallized concentration system. Pretreatment and substep evaporation methods are adopted, multiple-effect forced circulation and crystallization are used, useful resources including sodium chloride and calcium chloride are extracted respectively, and separated water can be recycled.
Description
Technical field
The present invention relates to a kind of soda manufacture evaporated waste ammonia liquid resource utilization method and preparation system, belong to liquid waste disposal technique field.
Background technology
Soda manufacture all causes pollution to a certain degree to environment, and characteristic contamination is the connection ammonia-containing water of alkali and the evaporated waste ammonia liquid of ammonia alkali.Solvay soda process is with salt and Wingdale for main raw material, with ammonia for the method for soda ash produced by middle subsidiary material.After crude salt water (or seawater) dissolves and becomes crude brine, through refining Ca2+ and the Mg2+ impurity removed in crude brine, the absorbing ammonia in ammonia absorption tower of the salt solution after refining generates ammoniated brine.Ammoniated brine is absorbing carbon dioxide in carbonating tower, generates NaHCO3 suspension.Suspension carries out solid-liquid separation through vacuum filter, and the filter cake obtained is soda ash product after calcining.The carbon dioxide that calcining generates returns carbonating tower and recycles.Filter the mother liquor obtained to react with milk of lime in ammonia still, the ammonia recycle distilled out uses.In ammonia-soda process soda ash process, discharge the evaporated waste ammonia liquid of a large amount of high salt amounts, the main sodium chloride-containing of evaporated waste ammonia liquid and calcium chloride useful resources.
Steam, inhale the master operation that ammonia operation is ammonia-soda process, object is with the ammonia in refined brine recovery filtrated stock and carbonic acid gas, thus the obtained ammoniated brine producing soda ash.In mother liquor, total ammonia is divided into free ammonia and Stagnant ammonium, could decompose after Stagnant ammonium must add ash charge breast.Ammonia still process process produces slops, and slops, through clarification or press filtration, produces waste clear solution (L1) and solid slag (S1).Part waste clear solution is for the production of calcium chloride, and remainder discharges; Part solid slag is for the manufacture of engineering soil, building daub etc., and remainder is stored up.Slops is about 10m3/t alkali, is about 200-300kg/ alkali (butt) containing solid slag.In waste liquid, solids basic source is in ash breast, and waste residue generation depends on the effective rate of decomposition etc. after Wingdale quality, limestone calcination.Waste residue pH value is less than 12.5, belongs to Ordinary solid waste.For ensureing the rate of recovery of ammonia, reducing the ammonia nitrogen concentration in discharge waste liquid, ash breast must be kept superfluous.Containing superfluous ash about 2 titre (1 titre equals 1/20th volumetric molar concentration) in waste liquid, containing Ca (OH) 2 about 800mg/L in waste clear solution.After the mode process such as clarification, waste clear solution pH value, generally between 11-11.5, is wherein about about 50mg/L containing NaCl about 50 ~ 55g/L, CaCl2 about 100 ~ 130g/L, ammonia.Affect the factor more complicated of waste liquid containing ammonia, principal element has opening by relative quantity of the composition fluctuation of cycle, mother liquor, the fluctuation of grey composition of milk, mother liquor and ash breast etc. of ammonia still, has larger association with the automatic control level of equipment level, production process, the quality of raw material.
Summary of the invention
The present invention is directed to above problem, propose a kind of soda manufacture evaporated waste ammonia liquid resource utilization method and preparation system, adopt pre-treatment, substep method of evaporating, utilize the crystallization of multiple-effect pump circulation, extract sodium-chlor and calcium chloride useful resources respectively, the water after separation can cyclically utilizing.
Object of the present invention is achieved through the following technical solutions: a kind of soda manufacture evaporated waste ammonia liquid resource utilization method and preparation system, preparation system mainly comprises: the collection pond connected successively, pretreatment filters, vaporizer, quadruple effect sodium chloride crystallizer, triple effect sodium chloride crystallizer, two effect sodium chloride crystallizer and an effect crystallization of calcium chloride device, the vapour outlet of a described effect crystallization of calcium chloride device connects two effect sodium chloride crystallizer, triple effect sodium chloride crystallizer, quadruple effect sodium chloride crystallizer successively, and the vapour outlet of described quadruple effect sodium chloride crystallizer connects condenser;
Wherein, soda manufacture evaporated waste ammonia liquid resource utilization method is realized by following four steps:
Step one: pre-treatment filtering system, filters impurity in waste liquid by pretreatment filters, and removes calcium sulfate;
Step 2: one section of evaporation concentration system, one section concentrated adopts falling film evaporator, adopts the latent heat of vapour compressor recycling steam, evaporation concentration to concentrated solution close to saturated;
Step 3: two sections of pump circulation crystallization concentration systems, after one section of concentration systems is concentrated, concentrated solution enters in two sections of concentration systems, successively after quadruple effect crystallizer, triple effect crystallizer, two effect three grades, crystallizers concentrate, calcium chloride concentration is concentrated into 38 ~ 42% through pump circulation flasher, sodium-chlor is substantially all separated out with the form of crystal salt, and the crystallizer of two sections of concentration systems all adopts the pump circulation flash evaporation technology of band salt leg particular design, obtains pure NaCl crystal salt;
Step 4: three sections of pump circulation crystallization concentration systems, the mother liquor isolating sodium-chlor flows into three sections of concentration systems (an effect crystallizer), one effect crystallizer adopts pump circulation flash process, mother liquor is finally processed, because this system boiling point temperature rise is higher, system directly adopts the raw steam of 1.0MPA as heat source, be evaporated to calcium chloride to contain close to saturated, then concentrated solution is put into the storage tank of steam insulation, gravity flow enters drum-type pelleter, produce sheet Calcium dichloride dihydrate product, pelleter sprays to drum inner surface with water coolant, the liquid gasification calcium closing outer surface of cylinder is frozen into the solid calcium chloride of 1 ~ 2mm thickness, scrape through scraper and be flake calcium chloride.
Crystallizer salt leg can play the effects such as collection salt, classification, washing, back dissolving soluble impurity, conveying, is improve one of the quality of salt, the key part reducing system energy consumption.One section of concentration systems concentrated solution is at two sections of concentration systems after triple effect evaporation, and 2nd effect evaporator is arranged mother liquor outward and flowed into three sections of concentration systems, reclaims calcium chloride further.The magma of two sections of concentrated triple effect evaporations flows into settling vessel and centrifuge carries out solid-liquid separation, and obtain solid sodium chloride crystal salt, settling vessel supernatant liquor and water extracter filtrate return in quadruple effect crystallizer, improves the NaCl rate of recovery.
The secondary steam that two sections of concentrated employings, three sections of concentration systems produce is as heat source, and two sections of concentration systems itself are made up of triple effect evaporation, adopt 2nd effect evaporator secondary steam as triple-effect evaporator heat source by the boiling point temperature rise of different concns, triple-effect evaporator secondary steam is as quadruple effect evaporator heat source, the latent heat of recycling steam, saves running cost.Final quadruple effect evaporator secondary steam carries out condensation by condenser, and water of condensation is pumped into the water inlet of preheater heating system by condensate pump.
In two sections of concentration systems, in order to reduce quadruple effect evaporator boiling temperature, separate chamber can be made to form certain negative pressure by vacuum pump, making solution reach the boiling temperature under this relevant pressure thus produce boiling.The condenser that system provides, system is discharged by the gas in the continuous extraction system of vacuum pump, system is made to form certain vacuum tightness, by this special design, make quadruple effect evaporator solution boiling point lowering, thus make quadruple effect evaporator that triple-effect evaporator secondary steam can be utilized as heat source, reach energy-conservation object.
The phlegma of three sections of concentration systems generations enters distilled water tank, and pumped into into water preheater by distilled water pump, its partial heat is recovered, and temperature declines, and finally carries out recycle as high-quality distilled water.To consider in NaCl-CaCl2-H2O three-phase system the features such as sodium-chlor, calcium chloride solubility with temperature variation characteristic, boiling point temperature rise, native system selects the saturation steam of 1.0MPA as driving steam, to obtain higher working temperature.
Principle of work of the present invention: the main sodium chloride-containing of evaporated waste ammonia liquid and calcium chloride, what can be similar to regards waste water as NaCl-CaCl2-H2O three-phase system.NaCl-CaCl2-H2O three-phase system has following features: the first, and the solubleness of calcium chloride in water has along with temperature rising to be increased by a relatively large margin, and aqueous solution boiling point increases simultaneously; And the change of sodium-chlor solubility with temperature is seldom, and lower with the temperature rise of change in concentration boiling point.The second, under certain pressure condition, the temperature rise of NaCl-CaCl2-H2O system boiling point sharply increases with the rising of CaCl2 concentration.3rd, NaCl-CaCl2-H2O system is in evaporating concentration process, sodium-chlor, calcium chloride concentration increase gradually, due to common-ion effcet, sodium-chlor solubleness solubleness in this system significantly reduces, first sodium-chlor reach capacity, System Priority crystallization sodium-chlor crystal salt, thus realize the separation of sodium-chlor.Mother liquor after Isolating chlorinated sodium continues evaporation concentration, can the Calcium dichloride dihydrate sheet of the main chloride containing calcium of output through pelleter.
The present invention has following advantage and beneficial effect: consider evaporated waste ammonia liquid amount of inlet water and water quality characteristics, the vaporizer (one section concentrates) that first evaporated waste ammonia liquid arranges carrying vapour compressor carries out initial concentration to waste water, concentrated waste water reduces System steam consumption as far as possible, saves working cost.After initial concentration, waste water enters quadruple effect pump circulation crystal system (two sections concentrated+three sections concentrate) again and carries out evaporative crystallization, isolates sodium-chlor and crystallization of calcium chloride.The feature that quadruple effect pump circulation crystal system utilizes calcium chloride to be increased sharply with the temperature rise of concentration rising boiling point, the secondary steam that system for recycling produces, steam saving and water coolant, reduce working cost further.
Accompanying drawing explanation
Fig. 1 is process schematic representation of the present invention.
In accompanying drawing, mark and corresponding component title: 1-collect pond, 2-pretreatment filters, 3-vaporizer, 4-quadruple effect sodium chloride crystallizer, 5-triple effect sodium chloride crystallizer, 6-bis-imitates sodium chloride crystallizer, 7-mono-imitates crystallization of calcium chloride device, and 8-recirculated cooling water is intake, 9-cooling water return, 10-condenser, 11-vapour compressor, 12-water extracter, 13-sodium-chlor collecting bin, 14-pelleter, 15-calcium chloride collecting bin, 16-steam, 17-reuse water tank.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment one: as shown in Figure 1, the present invention includes: a kind of soda manufacture evaporated waste ammonia liquid resource utilization method and preparation system, preparation system mainly comprises: the collection pond (1) connected successively, pretreatment filters (2), vaporizer (3), quadruple effect sodium chloride crystallizer (4), triple effect sodium chloride crystallizer (5), two effects sodium chloride crystallizer (6) and effect crystallization of calcium chloride device (7), the vapour outlet of described effect crystallization of calcium chloride device (7) connects two effect sodium chloride crystallizer (6) successively, triple effect sodium chloride crystallizer (5), quadruple effect sodium chloride crystallizer (4), the vapour outlet of described quadruple effect sodium chloride crystallizer (4) connects condenser (10).
A kind of soda manufacture evaporated waste ammonia liquid resource utilization method is realized by following four steps:
Step one: pre-treatment filtering system, filters impurity in waste liquid by pretreatment filters, and removes calcium sulfate;
Step 2: one section of evaporation concentration system, one section concentrated adopts falling film evaporator, adopts the latent heat of vapour compressor recycling steam, evaporation concentration to concentrated solution close to saturated;
Step 3: two sections of pump circulation crystallization concentration systems, after one section of concentration systems is concentrated, concentrated solution enters in two sections of concentration systems, successively after quadruple effect crystallizer, triple effect crystallizer, two effect three grades, crystallizers concentrate, calcium chloride concentration is concentrated into 38 ~ 42% through pump circulation flasher, sodium-chlor is substantially all separated out with the form of crystal salt, and the crystallizer of two sections of concentration systems all adopts the pump circulation flash evaporation technology of band salt leg particular design, obtains pure NaCl crystal salt;
Step 4: three sections of pump circulation crystallization concentration systems, the mother liquor isolating sodium-chlor flows into three sections of concentration systems (an effect crystallizer), one effect crystallizer adopts pump circulation flash process, mother liquor is finally processed, because this system boiling point temperature rise is higher, system directly adopts the raw steam of 1.0MPA as heat source, be evaporated to calcium chloride to contain close to saturated, then concentrated solution is put into the storage tank of steam insulation, gravity flow enters drum-type pelleter, produce sheet Calcium dichloride dihydrate product, pelleter sprays to drum inner surface with water coolant, the liquid gasification calcium closing outer surface of cylinder is frozen into the solid calcium chloride of 1 ~ 2mm thickness, scrape through scraper and be flake calcium chloride.
Embodiment two: such as certain preparation system water inlet is soda manufacture waste water, and the maximum flooding quantity 130t/h of system, carries out system design by maximum amount of water 130t/h.This sewage main component is calcium chloride: 125g/L, sodium-chlor: 55g/L, calcium sulfate 2g/L, and this sewage enters this evaporation concentration system after pre-treatment refining minimizing impurities in water and calcium sulfate as far as possible.System finally produces 118.7t/h distillate, generally can be used as recirculated cooling water moisturizing or DW system demineralized water system moisturizing reuse.Produced by native system and obtain NaCl crystal salt: about 6.8t/h(>=90% solid content, about containing NaCl6.3t/h), CaCl22H2O crystal salt: about 19t/h.
The above is only preferred embodiment of the present invention, and not do any pro forma restriction to the present invention, every any simple modification, equivalent variations done above embodiment according to technical spirit of the present invention, all falls within protection scope of the present invention.
Claims (1)
1. a soda manufacture evaporated waste ammonia liquid resource utilization method and preparation system, preparation system mainly comprises: the collection pond (1) connected successively, pretreatment filters (2), vaporizer (3), quadruple effect sodium chloride crystallizer (4), triple effect sodium chloride crystallizer (5), two effects sodium chloride crystallizer (6) and effect crystallization of calcium chloride device (7), the vapour outlet of described effect crystallization of calcium chloride device (7) connects two effect sodium chloride crystallizer (6) successively, triple effect sodium chloride crystallizer (5), quadruple effect sodium chloride crystallizer (4), the vapour outlet of described quadruple effect sodium chloride crystallizer (4) connects condenser (10),
Wherein, soda manufacture evaporated waste ammonia liquid resource utilization method is realized by following four steps:
Step one: pre-treatment filtering system, filters impurity in waste liquid by pretreatment filters, and removes calcium sulfate;
Step 2: one section of evaporation concentration system, one section concentrated adopts falling film evaporator, adopts the latent heat of vapour compressor recycling steam, evaporation concentration to concentrated solution close to saturated;
Step 3: two sections of pump circulation crystallization concentration systems, after one section of concentration systems is concentrated, concentrated solution enters in two sections of concentration systems, successively after quadruple effect crystallizer, triple effect crystallizer, two effect three grades, crystallizers concentrate, calcium chloride concentration is concentrated into 38 ~ 42% through pump circulation flasher, sodium-chlor is substantially all separated out with the form of crystal salt, and the crystallizer of two sections of concentration systems all adopts the pump circulation flash evaporation technology of band salt leg particular design, obtains pure NaCl crystal salt;
Step 4: three sections of pump circulation crystallization concentration systems, the mother liquor isolating sodium-chlor flows into three sections of concentration systems (an effect crystallizer), one effect crystallizer adopts pump circulation flash process, mother liquor is finally processed, because this system boiling point temperature rise is higher, system directly adopts the raw steam of 1.0MPA as heat source, be evaporated to calcium chloride to contain close to saturated, then concentrated solution is put into the storage tank of steam insulation, gravity flow enters drum-type pelleter, produce sheet Calcium dichloride dihydrate product, pelleter sprays to drum inner surface with water coolant, the liquid gasification calcium closing outer surface of cylinder is frozen into the solid calcium chloride of 1 ~ 2mm thickness, scrape through scraper and be flake calcium chloride.
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Cited By (7)
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| CN106365179A (en) * | 2016-08-26 | 2017-02-01 | 张勇军 | Environment-friendly ammonia-soda-method sodium carbonate production process, production system therefor, treatment method of ammonia distilling waste liquid, and treatment system used for the treatment method |
| CN106976899A (en) * | 2017-04-24 | 2017-07-25 | 潍坊天圣环保科技有限公司 | The production technology of anhydrous calcium chloride is extracted by calcium chloride solution |
| CN107089675A (en) * | 2017-05-27 | 2017-08-25 | 石家庄科林威尔环保科技有限公司 | A kind of new method for the distilled ammonia wastewater recycling that ammonia-soda process soda ash is discharged |
| CN108249467A (en) * | 2017-12-28 | 2018-07-06 | 中国海洋石油集团有限公司 | A kind of method of Calcium Chloride Production good antiscale property |
| CN109534570A (en) * | 2018-11-26 | 2019-03-29 | 启东亚太化工厂有限公司 | A kind for the treatment of process of high concentration production waste water |
| CN111392792A (en) * | 2020-04-07 | 2020-07-10 | 清华大学 | Steel plant waste heat method sewage zero discharge and blast furnace slag dechlorination purification method and system |
| CN117923731A (en) * | 2024-03-20 | 2024-04-26 | 天津高能时代水处理科技有限公司 | Recycling system and method for high-concentration calcium chloride and sodium chloride mixed salt wastewater |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106365179A (en) * | 2016-08-26 | 2017-02-01 | 张勇军 | Environment-friendly ammonia-soda-method sodium carbonate production process, production system therefor, treatment method of ammonia distilling waste liquid, and treatment system used for the treatment method |
| CN106365179B (en) * | 2016-08-26 | 2019-10-29 | 黄新强 | Processing method, the processing system used of environment-friendly type ammonia-soda process soda manufacture technique, production system used and evaporated waste ammonia liquid |
| CN106976899A (en) * | 2017-04-24 | 2017-07-25 | 潍坊天圣环保科技有限公司 | The production technology of anhydrous calcium chloride is extracted by calcium chloride solution |
| CN106976899B (en) * | 2017-04-24 | 2019-01-01 | 潍坊天圣环保科技有限公司 | The production technology of anhydrous calcium chloride is extracted by calcium chloride solution |
| CN107089675A (en) * | 2017-05-27 | 2017-08-25 | 石家庄科林威尔环保科技有限公司 | A kind of new method for the distilled ammonia wastewater recycling that ammonia-soda process soda ash is discharged |
| CN107089675B (en) * | 2017-05-27 | 2019-11-08 | 石家庄科林威尔环保科技有限公司 | A kind of method for the distilled ammonia wastewater recycling that ammonia-soda process soda ash is discharged |
| CN108249467A (en) * | 2017-12-28 | 2018-07-06 | 中国海洋石油集团有限公司 | A kind of method of Calcium Chloride Production good antiscale property |
| CN109534570A (en) * | 2018-11-26 | 2019-03-29 | 启东亚太化工厂有限公司 | A kind for the treatment of process of high concentration production waste water |
| CN109534570B (en) * | 2018-11-26 | 2021-12-14 | 启东亚太药业有限公司 | Treatment process of high-concentration production wastewater |
| CN111392792A (en) * | 2020-04-07 | 2020-07-10 | 清华大学 | Steel plant waste heat method sewage zero discharge and blast furnace slag dechlorination purification method and system |
| CN111392792B (en) * | 2020-04-07 | 2024-04-26 | 清华大学 | Zero-emission sewage and blast furnace slag dechlorination purification method and system by waste heat method in steel plant |
| CN117923731A (en) * | 2024-03-20 | 2024-04-26 | 天津高能时代水处理科技有限公司 | Recycling system and method for high-concentration calcium chloride and sodium chloride mixed salt wastewater |
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Application publication date: 20160330 |