CN102786073A - Method for preparing high-concentration calcium chloride solution by decomposing ammonium chloride with lime powder - Google Patents
Method for preparing high-concentration calcium chloride solution by decomposing ammonium chloride with lime powder Download PDFInfo
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- CN102786073A CN102786073A CN2012103073931A CN201210307393A CN102786073A CN 102786073 A CN102786073 A CN 102786073A CN 2012103073931 A CN2012103073931 A CN 2012103073931A CN 201210307393 A CN201210307393 A CN 201210307393A CN 102786073 A CN102786073 A CN 102786073A
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Abstract
The invention discloses a method for preparing high-concentration calcium chloride solution by decomposing ammonium chloride with lime powder. The method is characterized by including steps of mixing wet ammonium chloride in soda production process II with lime powder to feed into a primary reactor, adding light liquid from a light liquid distillation tower for sufficient reaction, subjecting generated primary reaction liquid to ammonia distillation process by a primary distillation tower, subjecting primary distillation liquid overflowing into a secondary reactor for subsequent reaction, and pumping generated secondary reaction liquid for ammonia distillation in a secondary distillation tower, and subjecting the obtained secondary distillation liquid to flash steam distillation to obtain high-concentration calcium chloride solution. The high-concentration calcium chloride solution is fed to a calcium chloride production system by a concentrated-calcium conveying pump, gas discharged by the secondary distillation tower is used as heat source for ammonia distillation of the primary distillation tower, and ammonia gas of the primary distillation tower and the light liquid distillation tower is recovered by an ammonia cooler and fed to an ammonia absorption tower. The method for preparing high-concentration calcium chloride solution has the advantages that concentration of the calcium chloride solution can reach 38% or above, ammonia content is lower than 100mg/L, consumption of 0.5MPa steam for producing double-water calcium chloride per ton is reduced by more than 30% as compared with before, and discharge of dry white-base mud is reduced by about 30% as well.
Description
Technical field
The present invention relates to a kind of method of utilizing the lime powder decomposing ammonium chloride to prepare high calcium chloride concentration solution.
Background technology
As maximum in the world soda ash producing country, the present soda ash YO of China has reached more than 2,000 ten thousand tons, solvay soda process is arranged, join alkaline process and three kinds of working methods of natural alkaline process, and wherein solvay soda process accounts for about 20 ~ 40% of ultimate production.The ammonia alkali white clay mainly results from distillation and reclaims ammonia operation and salt refining process, the about 9 ~ 10m of slops
3/ t soda ash produces 200 ~ 300kg butt white clay/t soda ash approximately, contains the calcium chloride about 10% in the waste liquid, and about 5% sodium-chlor because the discharging of waste liquid amount is big, is difficult to realize thorough improvement, and not only contaminate environment also causes the waste of materials such as sodium-chlor and calcium chloride.Present most of ammonia alkali enterprise utilizes Greenwaltrecovery process Greenwalt NSCC to produce calcium chloride, but this method is with direct evaporation behind the slops defecate and purify, because calcium chloride concentration low (about 10%) wherein, steam consumption is big, and cost is high.Therefore seek a kind of reduction waste liquid growing amount, improve the waste liquid calcium chloride concentration and become the big problem that is related to alkali calcium combination producing Business survival.This not only can reduce the discharging wastes amount greatly, reduces the harm to environment, and because the waste liquid calcium chloride concentration raises, the production cost of calcium chloride will reduce at double.Company has introduced dry method in nineteen ninety from Dutch Aksu and has added grey distil process, and the slops calcium chloride concentration is upgraded to 13 ~ 14% from about 10%, produces CaCl with the dry method waste liquid
2.2H
2The steam that O consumes 0.5MPa reduces about 8% than the wet method distillation, butt white clay quantity discharged reduces by 5% approximately.
Summary of the invention
The object of the invention is exactly in order to solve the deficiency of above-mentioned technology, to adopt solvay soda process and join alkali II process process combined, utilizing the lime powder decomposing ammonium chloride to prepare the method for high calcium chloride concentration solution.
The present invention to achieve these goals, the technical scheme of being taked is:
(1) decomposition reaction of ammonium chloride: get into through feed bin respectively through metering from wet ammonium chloride that joins alkali II process and lime powder and to mix conveying auger from the lime pulverized coal preparation system, entering I stage reactor after the mixing, lime powder CaO excess quantity is more than 3% in the I stage reactor; Temperature of reaction is 70 ~ 90 ℃, adds a certain amount of light liquid that comes from light liquid distillation tower through stirring thorough mixing, partial reaction, generates I order reaction liquid; Carry through I level transferpump, wherein some I order reaction liquid returns the I stage reactor and circulates, and all the other deliver to I level distillation tower top; With the steam of discharging from II level distillation tower top that gets into from I level distillation tower bottom and the gas mixture counter current contact of ammonia, carry out heat and mass, ammonia still process, reaction, become I level distillate; Overflow got into II stage reactor continuation reaction at the bottom of I level distillate distilled Tata from the I level, a certain amount of LP steam of II stage reactor bottom feeding, and temperature of reaction is more than 100 ℃; Generate II order reaction liquid; Carried by II level transferpump, wherein some II order reaction liquid returns the II stage reactor and circulates, and all the other deliver to II level distillation tower top; The steam that sprays through steam injector gets into from the bottom of II level distillation tower; Steam remaining ammonia in the II order reaction liquid, become II level distillate, go out from II level distillation tower tower bottom flow;
(2) generation of high calcium chloride concentration solution: the II level distillate that goes out from II level distillation tower tower bottom flow becomes high calcium chloride concentration solution through the flash evaporation shwoot; High calcium chloride concentration solution contains ammonia and is lower than 100mg/L; Calcium chloride mass percentage content >=38%; Deliver to the Calcium Chloride Production system by dense calcium transferpump, the secondary steam that shwoot goes out gets into steam injector;
(3) recovery of ammonia: the ammonia that discharge at I, II stage reactor top gets into I level distillation tower middle part, and I level distillation tower cat head air outlet temperature is 90 ~ 100 ℃, and the ammonia that steams is discharged from cat head, through 1
#The condensed ammonia of ammonia cooler is delivered to ammonia absorption tower, and its phlegma gets into light liquid distillation tower, and the ammonia that light liquid distillation tower top steams is through 2
#Also deliver to ammonia absorption tower after the ammonia cooler condensation, the light liquid that light liquid distillation tower tower bottom flow goes out returns the I stage reactor and is used for chloride leach and lime powder digestion reaction.
The I stage reactor drops into the amount of ammonium chloride and lime powder according to ammonium chloride complete reaction batching, and lime powder CaO excess quantity is best by 3 ~ 10% batchings.
The temperature of reaction of II stage reactor between 100 ~ 120 ℃, decomposing ammonium chloride fully.
For guaranteeing I level distillate calcium chloride concentration and react completely that the temperature of I level distillate is answered >=115 ℃.
For guaranteeing II level distillate calcium chloride concentration and react completely that the temperature of II level distillate is answered >=115 ℃.
The preferred mass degree can prolong the device fabrication cycle at the lime powder more than 75%, improves equipment capacity, reduces waste discharge.
Major advantage of the present invention:
The present invention utilizes the lime powder decomposing ammonium chloride to prepare the method for high calcium chloride concentration solution; Compare and utilize milk of lime in the production of traditional solvay soda process soda ash and filter the slops that the mother liquor reaction obtains; Calcium chloride concentration increases to more than 38% by 10% ~ 13%; Can significantly reduce the steam consumption of two water Calcium Chloride Production, the 0.5MPa steam consumption reduces more than 30% than the wet method distillation, and butt white clay quantity discharged also reduces about 30%.
Description of drawings
Accompanying drawing is a schematic flow sheet of the present invention.
Among the figure: 1-ammonium chloride feed bin; 2-lime powder feed bin; 3-I stage reactor; 4-I level transferpump; 5-II stage reactor; 6-II level transferpump; 7-I level distillation tower; 8-II level distillation tower; 9-steam injector; 10-flash evaporation; 11-1
#Ammonia cooler; 12-light liquid distillation tower; 13-2
#Ammonia cooler; 14-dense calcium transferpump; 15-mixing conveying auger.
Embodiment
As shown in the figure, the structure of I, II level distillation tower is sieve-tray tower, and this tower vapour-liquid mass heat-transfer effect is good.The figure low pressure steam adopts 0.5MPa steam.
In conjunction with accompanying drawing narration flow process of the present invention: mix conveying auger 15 with sending into through metering from the lime powder of lime powder feed bin 2 from the wet ammonium chloride of ammonium chloride feed bin 1; Mix the back and get into I stage reactor 3; Add a certain amount of light liquid and carry out thorough mixing and partial reaction through stirring from light liquid distillation tower 12; The I order reaction liquid that generates is delivered to I level distillation tower 7 tops and is carried out heat and mass from the steam of II level distillation tower 8 and the gas mixture counter current contact of ammonia through I level transferpump 4, and the overflow at the bottom of I level distillation tower 7 towers of gained I level distillate goes II stage reactor 5 further to react; Complete for guaranteeing the ammonium chloride decomposition reaction, in II stage reactor 5, add a certain amount of steam, 100 ~ 120 ℃ of temperature of reaction, and lime powder CaO excess quantity is 3 ~ 10% in the control I stage reactor 3; II order reaction liquid in that II stage reactor 5 generates is delivered to II level distillation tower 8 tops by II level transferpump 6; 0.5MPa spraying through steam injector 9 together, the secondary steam that LP steam and II level distillate reclaim gets into II level distillation tower 8 bottoms behind flash evaporation 10 shwoots; Steam remaining ammonia in the II order reaction liquid; I stage reactor 3 gets into I level distillation tower 7 middle parts with the ammonia that II stage reactor 5 produces, and the ammonia that I level distillation tower 7 steams is discharged from cat head, through 1
#Phlegma removes light liquid distillation tower 12 after ammonia cooler 11 condensations, and the solution of phlegma after light liquid distillation tower 12 steams ammonia is light liquid, and this light liquid gets into I stage reactor 3 dissolving ammonium chlorides and the reaction that digests lime powder, and the ammonia that light liquid distillation tower 12 steams is through 2
#After ammonia cooler 13 condensations and from 1
#The ammonia of ammonia cooler 11 comes along ammonia absorption tower and reclaims ammonia; Solution is II level distillate after the ammonia still process of discharging at the bottom of II level distillation tower 8 towers.For strengthening that the stirring of reaction solution is carried out to promote reaction, I level, II order reaction liquid all some reactor drum that returns respectively separately circulate.II level distillate is a high calcium chloride concentration solution from the solution that tower bottom flow goes out behind flash evaporation 10 shwoots, and its calcium chloride concentration reaches more than 38%, contains ammonia and is lower than 100mg/L, delivers to the Calcium Chloride Production system by dense calcium transferpump 14.
Below in conjunction with specific embodiment the present invention is further specified:
Embodiment 1:
Flow process as shown in the figure adds 95% ammonium chloride 300kg/h and lime powder (CaO content 77.32%) 215kg/h from lime powder feed bin 2 and sends into and mixes conveying auger 15 and mix entering I stage reactors 3 afterwards from ammonium chloride feed bin 1, add 0.24m simultaneously
3The light liquid of/h carries out thorough mixing and partial reaction through stirring; 89.5 ℃ of temperature of reaction; I order reaction liquid lime powder CaO excess quantity 9.91% is delivered to I level distillation tower 7 tops and is carried out heat and mass from the steam of II level distillation tower 8 and the gas mixture counter current contact of ammonia by I level transferpump 4, and excessive effusive I level distillate temperature is 118.1 ℃ at the bottom of I level distillation tower 7 towers; I level distillate goes II stage reactor 5 further to react from the overflow of I level base product; For guaranteeing the ammonium chloride decomposition reaction, add 10kg/h steam, 120 ℃ of temperature at II stage reactor 5.The reaction solution of II stage reactor 5 is delivered to II level distillation tower 8 tops by II level transferpump 6; 0.5MPa the secondary steam of LP steam and II level distillate shwoot gets into bottom, II level distillation tower 8 foundation ring to steam remaining ammonia through steam injector 9 together; The ammonia that I, II stage reactor produce gets into I level distillation tower 7 middle parts; I level distillation tower 7 air outlet temperatures are 99.1 ℃ and discharge from cat head; Go the solution after light liquid distillation tower 12 steams ammonia to be called light liquid through gained phlegma after 11 condensations of 1# ammonia cooler; Go to get into I stage reactor 3 with lime powder, ammonium chloride thorough mixing, partial reaction takes place, the ammonia that light liquid distillation tower 12 steams comes along ammonia absorption tower with ammonia from 1# ammonia cooler 11 and reclaims ammonia after 13 condensations of 2# ammonia cooler.Solution is called II level distillate after the ammonia still process that II level base product is discharged, 119.8 ℃ of temperature, and the solution behind flash evaporation 10 shwoots is high calcium chloride concentration solution, and its calcium chloride mass percent concentration is 39.76%, and total ammonia is 96. 37 mg/L.
Embodiment 2:
Flow process as shown in the figure adds 95% ammonium chloride 300kg/h and lime powder (CaO content 75.76%) 210kg/h from lime powder feed bin 2 and sends into and mixes conveying auger 15 and mix entering I stage reactors 3 afterwards from ammonium chloride feed bin 1, add 0.25m simultaneously
3The light liquid of/h carries out thorough mixing and partial reaction through stirring; 79.7 ℃ of temperature of reaction; I order reaction liquid lime powder CaO excess quantity 5.30% is delivered to I level distillation tower 7 tops and is carried out heat and mass from the steam of II level distillation tower 8 and the gas mixture counter current contact of ammonia by I level transferpump 4, and excessive effusive I level distillate temperature is 117.6 ℃ at the bottom of I level distillation tower 7 towers; I level distillate goes II stage reactor 5 further to react from the overflow of I level base product; For guaranteeing the ammonium chloride decomposition reaction, add 7.8kg/h steam, 114.7 ℃ of temperature at II stage reactor 5.The reaction solution of II stage reactor 5 is delivered to II level distillation tower 8 tops by II level transferpump 6; 0.5MPa the secondary steam of LP steam and II level distillate shwoot gets into bottom, II level distillation tower 8 foundation ring to steam remaining ammonia through steam injector 9 together; The ammonia that I, II stage reactor produce gets into I level distillation tower 7 middle parts; I level distillation tower 7 air outlet temperatures are 94.7 ℃ and discharge from cat head; Go the solution after light liquid distillation tower 12 steams ammonia to be called light liquid through gained phlegma after 11 condensations of 1# ammonia cooler, remove to get into I stage reactor 3 and lime powder, ammonium chloride thorough mixing, generation partial reaction, the ammonia that light liquid distillation tower 12 steams is after 13 condensations of 2# ammonia cooler and from 1
#The ammonia of ammonia cooler 11 comes along ammonia absorption tower and reclaims ammonia.Solution is called II level distillate after the ammonia still process that II level base product is discharged, 116.9 ℃ of temperature, and the solution behind flash evaporation 10 shwoots is high calcium chloride concentration solution, and its calcium chloride mass percent concentration is 38.45%, and total ammonia is 56.12 mg/L.
Embodiment 3:
Flow process as shown in the figure adds 95% ammonium chloride 200kg/h and lime powder (CaO content 80.26%) 128kg/h from lime powder feed bin 2 and sends into and mixes conveying auger 15 and mix entering I stage reactors 3 afterwards from ammonium chloride feed bin 1, add 0.20m simultaneously
3The light liquid of/h carries out thorough mixing and partial reaction through stirring; 70.7 ℃ of temperature of reaction; I order reaction liquid lime powder CaO excess quantity 3.21% is delivered to I level distillation tower 7 tops and is carried out heat and mass from the steam of II level distillation tower 8 and the gas mixture counter current contact of ammonia by I level transferpump 4, and excessive effusive I level distillate temperature is 117.2 ℃ at the bottom of I level distillation tower 7 towers; I level distillate goes II stage reactor 5 further to react from the overflow of I level base product; For guaranteeing the ammonium chloride decomposition reaction, add 5.4kg/h steam, 100.8 ℃ of temperature at II stage reactor 5.The reaction solution of II stage reactor 5 is delivered to II level distillation tower 8 tops by II level transferpump 6; 0.5MPa the secondary steam of LP steam and II level distillate shwoot gets into bottom, II level distillation tower 8 foundation ring to steam remaining ammonia through steam injector 9 together; The ammonia that I, II stage reactor produce gets into I level distillation tower 7 middle parts; I level distillation tower 7 air outlet temperatures are 90.2 ℃ and discharge from cat head; Go the solution after light liquid distillation tower 12 steams ammonia to be called light liquid through gained phlegma after 11 condensations of 1# ammonia cooler; Go to get into I stage reactor 3 with lime powder, ammonium chloride thorough mixing, partial reaction takes place, the ammonia that light liquid distillation tower 12 steams comes along ammonia absorption tower with ammonia from 1# ammonia cooler 11 and reclaims ammonia after 13 condensations of 2# ammonia cooler.Solution is called II level distillate after the ammonia still process that II level base product is discharged, 118.4 ℃ of temperature, and the solution behind flash evaporation 10 shwoots is high calcium chloride concentration solution, and its calcium chloride mass percent concentration is 38.73%, and total ammonia is 71.63 mg/L.
Claims (6)
1. method of utilizing the lime powder decomposing ammonium chloride to prepare high calcium chloride concentration solution is characterized in that may further comprise the steps:
(1) decomposition reaction of ammonium chloride: get into through feed bin respectively through metering from wet ammonium chloride that joins alkali II process and lime powder and to mix conveying auger from the lime pulverized coal preparation system, entering I stage reactor after the mixing, lime powder CaO excess quantity is more than 3% in the I stage reactor; Temperature of reaction is 70 ~ 90 ℃, adds a certain amount of light liquid that comes from light liquid distillation tower through stirring thorough mixing, partial reaction, generates I order reaction liquid; Carry through I level transferpump, wherein some I order reaction liquid returns the I stage reactor and circulates, and all the other deliver to I level distillation tower top; With the steam of discharging from II level distillation tower top that gets into from I level distillation tower bottom and the gas mixture counter current contact of ammonia, carry out heat and mass, ammonia still process, reaction, become I level distillate; Overflow got into II stage reactor continuation reaction at the bottom of I level distillate distilled Tata from the I level, a certain amount of LP steam of II stage reactor bottom feeding, and temperature of reaction is more than 100 ℃; Generate II order reaction liquid; Carried by II level transferpump, wherein some II order reaction liquid returns the II stage reactor and circulates, and all the other deliver to II level distillation tower top; The steam that sprays through steam injector gets into from the bottom of II level distillation tower; Steam remaining ammonia in the II order reaction liquid, become II level distillate, go out from II level distillation tower tower bottom flow;
(2) generation of high calcium chloride concentration solution: the II level distillate that goes out from II level distillation tower tower bottom flow becomes high calcium chloride concentration solution through the flash evaporation shwoot; High calcium chloride concentration solution contains ammonia and is lower than 100mg/L; Calcium chloride mass percentage content >=38%; Deliver to the Calcium Chloride Production system by dense calcium transferpump, the secondary steam that shwoot goes out gets into steam injector;
(3) recovery of ammonia: the ammonia that discharge at I, II stage reactor top gets into I level distillation tower middle part, and I level distillation tower cat head air outlet temperature is 90 ~ 100 ℃, and the ammonia that steams is discharged from cat head, through 1
#The condensed ammonia of ammonia cooler is delivered to ammonia absorption tower, and its phlegma gets into light liquid distillation tower, and the ammonia that light liquid distillation tower top steams is through 2
#Also deliver to ammonia absorption tower after the ammonia cooler condensation, the light liquid that light liquid distillation tower tower bottom flow goes out returns the I stage reactor and is used for chloride leach and lime powder digestion reaction.
2. the method for utilizing the lime powder decomposing ammonium chloride to prepare high calcium chloride concentration solution according to claim 1 is characterized in that lime powder CaO excess quantity is 3 ~ 10% in the described I stage reactor.
3. the method for utilizing the lime powder decomposing ammonium chloride to prepare high calcium chloride concentration solution according to claim 1, the temperature of reaction that it is characterized in that described II stage reactor is 100 ~ 120 ℃.
4. the method for utilizing the lime powder decomposing ammonium chloride to prepare high calcium chloride concentration solution according to claim 1, temperature >=115 of the I level distillate that it is characterized in that going out at the bottom of the described I level distillation Tata ℃.
5. the method for utilizing the lime powder decomposing ammonium chloride to prepare high calcium chloride concentration solution according to claim 1 is characterized in that temperature >=115 ℃ of the II level distillate that described II level base product goes out.
6. the method for utilizing the lime powder decomposing ammonium chloride to prepare high calcium chloride concentration solution according to claim 1 is characterized in that the total quicklime mass percentage content of lime powder is more than 75%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103693701A (en) * | 2013-12-30 | 2014-04-02 | 唐山三友化工股份有限公司 | Ammonia distillation device and technology by mother liquor and total ash powder with alkaline method |
| CN104609441A (en) * | 2015-01-05 | 2015-05-13 | 河北科技大学 | Method for decomposing ammonium chloride by semidry method and reactor |
| CN110184185A (en) * | 2019-05-10 | 2019-08-30 | 孟州市厚源生物科技有限公司 | The secondary liquefaction device and liquefaction process of starchy material production alcohol |
| CN114716161A (en) * | 2022-06-09 | 2022-07-08 | 天津市新天钢钢铁集团有限公司 | Method for quickly digesting sintered lime |
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| JPS605023A (en) * | 1983-06-22 | 1985-01-11 | Tokuyama Soda Co Ltd | Production of aqueous solution of calcium chloride |
| JP4050864B2 (en) * | 2000-08-21 | 2008-02-20 | 株式会社トクヤマ | Method for producing calcium chloride aqueous solution |
| CN101941719A (en) * | 2010-05-25 | 2011-01-12 | 河北科技大学 | Method for combined production of ammonia and basic calcium chloride by decomposing ammonium chloride |
| CN102145912A (en) * | 2011-03-01 | 2011-08-10 | 大连大化工程设计有限公司 | Process for preparing calcium chloride solution by utilizing ammonia soda filtration mother liquor |
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2012
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS605023A (en) * | 1983-06-22 | 1985-01-11 | Tokuyama Soda Co Ltd | Production of aqueous solution of calcium chloride |
| JP4050864B2 (en) * | 2000-08-21 | 2008-02-20 | 株式会社トクヤマ | Method for producing calcium chloride aqueous solution |
| CN101941719A (en) * | 2010-05-25 | 2011-01-12 | 河北科技大学 | Method for combined production of ammonia and basic calcium chloride by decomposing ammonium chloride |
| CN102145912A (en) * | 2011-03-01 | 2011-08-10 | 大连大化工程设计有限公司 | Process for preparing calcium chloride solution by utilizing ammonia soda filtration mother liquor |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103693701A (en) * | 2013-12-30 | 2014-04-02 | 唐山三友化工股份有限公司 | Ammonia distillation device and technology by mother liquor and total ash powder with alkaline method |
| CN104609441A (en) * | 2015-01-05 | 2015-05-13 | 河北科技大学 | Method for decomposing ammonium chloride by semidry method and reactor |
| CN110184185A (en) * | 2019-05-10 | 2019-08-30 | 孟州市厚源生物科技有限公司 | The secondary liquefaction device and liquefaction process of starchy material production alcohol |
| CN114716161A (en) * | 2022-06-09 | 2022-07-08 | 天津市新天钢钢铁集团有限公司 | Method for quickly digesting sintered lime |
| CN114716161B (en) * | 2022-06-09 | 2022-09-09 | 天津市新天钢钢铁集团有限公司 | Method for quickly digesting sintered lime |
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Owner name: QINGDAO ALKALI INDUSTRY DEVELOPMENT CO., LTD. Free format text: FORMER OWNER: QINGDAO ALKALI INDUSTRY CO., LTD. Effective date: 20150727 |
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Effective date of registration: 20150727 Address after: 266043 No. four, No. 78 North Stream Road, Licang District, Shandong, Qingdao Patentee after: QINGDAO SODA ASH INDUSTRIAL DEVELOPMENT CO., LTD. Patentee after: Qingdao Haiwan Chemical Engineering Design & Research Institute Limited Address before: 266043 No. four, No. 78 North Stream Road, Licang District, Shandong, Qingdao Patentee before: Qingdao Alkali Industry Co., Ltd. Patentee before: Qingdao Haiwan Chemical Engineering Design & Research Institute Limited |