CN102786073B - 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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- CN102786073B CN102786073B CN201210307393.1A CN201210307393A CN102786073B CN 102786073 B CN102786073 B CN 102786073B CN 201210307393 A CN201210307393 A CN 201210307393A CN 102786073 B CN102786073 B CN 102786073B
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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 lime powder decomposing ammonium chloride to prepare high calcium chloride concentration solution.
Background technology
As maximum in the world soda ash producing country, the current soda ash annual production of China has reached more than 2,000 ten thousand tons, has solvay soda process, connection alkaline process and three kinds of production methods of natural alkaline process, and wherein solvay soda process accounts for 20 ~ 40% left and right of ultimate production.Ammonia alkali white clay mainly results from Distillation recovery ammonia operation and salt refining process, and slops is 9 ~ 10m approximately
3/ t soda ash, approximately produces 200 ~ 300kg butt white clay/t soda ash, and in waste liquid, containing the calcium chloride of 10% left and right, the sodium-chlor of 5% left and right, because discharging of waste liquid amount is large, is difficult to realize thorough improvement, and not only contaminate environment, also causes the waste of the materials such as sodium-chlor and calcium chloride.Most ammonia alkali enterprise utilizes Greenwaltrecovery process Greenwalt NSCC to produce calcium chloride, but the method be will be after slops defecate and purify directly evaporation, due to calcium chloride concentration low (approximately 10%) wherein, steam consumption is large, cost is high.Therefore seek a kind of waste liquid growing amount that reduces, improve waste liquid calcium chloride concentration and become the large problem that is related to alkali calcium combination producing Business survival.This not only can reduce the quantity discharged of waste greatly, reduces the harm to environment, and because 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 slops calcium chloride concentration is upgraded to 13 ~ 14% from 10% left and right, with dry method waste liquid production CaCl
2.2H
2the steam that O consumes 0.5MPa reduces approximately 8% than wet method distillation, and butt white clay quantity discharged approximately reduces by 5%.
Summary of the invention
Object of the present invention is exactly the deficiency in order to solve above-mentioned technology, adopts solvay soda process and the technique that connection alkali II process combines, and utilizes lime powder decomposing ammonium chloride to prepare the method for high calcium chloride concentration solution.
To achieve these goals, the technical scheme of taking is in the present invention:
(1) decomposition reaction of ammonium chloride: the wet ammonium chloride from connection alkali II process is entered and mixed conveying auger by feed bin respectively through metering with the lime powder from lime pulverized coal preparation system, after mixing, enter I stage reactor, in I stage reactor, lime powder CaO excess quantity is more than 3%, temperature of reaction is 70 ~ 90 ℃, add a certain amount of light liquid coming from light liquid distillation tower through stirring abundant mixing, partial reaction, generate I order reaction liquid, by I level transferpump, carry, wherein some I order reaction liquid returns to I stage reactor and circulates, all the other deliver to I level distillation tower top, with the steam of discharging from II level distillation tower top entering 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, I level distillate enters II stage reactor from overflow at the bottom of I level distillation tower tower and continues reaction, II stage reactor bottom passes into a certain amount of low-pressure steam, temperature of reaction is more than 100 ℃, generate II order reaction liquid, by II level transferpump, carried, wherein some II order reaction liquid returns to II stage reactor and circulates, all the other deliver to II level distillation tower top, the steam spraying through steam injector enters from the bottom of II level distillation tower, steam remaining ammonia in II order reaction liquid, become II level distillate, from II level distillation tower tower bottom flow, go out,
(2) generation of high calcium chloride concentration solution: the II level distillate going out from II level distillation tower tower bottom flow becomes high calcium chloride concentration solution through flash evaporation shwoot, high calcium chloride concentration solution contains ammonia lower than 100mg/L, calcium chloride mass percentage content >=38%, by dense calcium transferpump, deliver to Calcium Chloride Production system, the secondary steam that shwoot goes out enters steam injector;
(3) recovery of ammonia: the ammonia that discharge at I, II stage reactor top enters I level distillation tower middle part, and I level distillation tower tower top air outlet temperature is 90 ~ 100 ℃, and the ammonia steaming is discharged from tower top, through 1
#the condensed ammonia of ammonia cooler is delivered to ammonia absorption tower, and its phlegma enters light liquid distillation tower, and the ammonia that light liquid distillation tower top steams is through 2
#after ammonia cooler condensation, also deliver to ammonia absorption tower, the light liquid that light liquid distillation tower tower bottom flow goes out returns to I stage reactor for chloride leach and lime powder digestion reaction.
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 completely.
For guaranteeing I level distillate calcium chloride concentration and reacting completely, the temperature of I level distillate is answered >=115 ℃.
For guaranteeing II level distillate calcium chloride concentration and reacting completely, the temperature of II level distillate is answered >=115 ℃.
The lime powder of preferred mass degree more than 75%, can the extension device production cycle, improves equipment capacity, reduces waste discharge.
Major advantage of the present invention:
The present invention utilizes lime powder decomposing ammonium chloride to prepare the method for high calcium chloride concentration solution, comparing in traditional solvay soda process soda ash production utilizes milk of lime to react with filtration mother liquor the slops obtaining, calcium chloride concentration increases to more than 38% by 10% ~ 13%, can significantly reduce the steam consumption of two water Calcium Chloride Production, 0.5MPa steam consumption reduces more than 30% than wet method distillation, and butt white clay quantity discharged also reduces approximately 30%.
Accompanying drawing explanation
Accompanying drawing is schematic flow sheet of the present invention.
In 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.Figure low pressure steam adopts 0.5MPa steam.
Narrate by reference to the accompanying drawings flow process of the present invention: from the wet ammonium chloride of ammonium chloride feed bin 1, send into and mix conveying auger 15 through metering with the lime powder from lime powder feed bin 2, after mixing, enter I stage reactor 3, add a certain amount of light liquid from light liquid distillation tower 12 to carry out fully mixing and partial reaction through stirring, the I order reaction liquid generating 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, gained I level distillate goes II stage reactor 5 further to react from overflow at the bottom of I level distillation tower 7 towers, complete for guaranteeing ammonium chloride decomposition reaction, in II stage reactor 5, add a certain amount of steam, 100 ~ 120 ℃ of temperature of reaction, and in control I stage reactor 3, lime powder CaO excess quantity is 3 ~ 10%, the II order reaction liquid generating at II stage reactor 5 is delivered to II level distillation tower 8 tops by II level transferpump 6, together with the secondary steam that 0.5MPa low-pressure steam reclaims after flash evaporation 10 shwoots with II level distillate, by steam injector 9, spray and enter II level distillation tower 8 bottoms, steam remaining ammonia in II order reaction liquid, the ammonia that I stage reactor 3 and II stage reactor 5 produce enters I level distillation tower 7 middle parts, the ammonia that I level distillation tower 7 steams is discharged from tower top, through 1
#after ammonia cooler 11 condensations, phlegma removes light liquid distillation tower 12, and the solution that phlegma steams after ammonia through light liquid distillation tower 12 is light liquid, and this light liquid enters I stage reactor 3 and dissolves ammonium chloride and digest reacting of 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 goes ammonia absorption tower to reclaim ammonia together, after the ammonia still process of discharging at the bottom of II level distillation tower 8 towers, solution is II level distillate.For strengthening that the stirring of reaction solution is carried out to promote to react, I level, II order reaction liquid all some reactor returning respectively separately circulate.The solution that II level distillate goes out after flash evaporation 10 shwoots from tower bottom flow is high calcium chloride concentration solution, and its calcium chloride concentration reaches more than 38%, containing ammonia, lower than 100mg/L, by dense calcium transferpump 14, delivers to Calcium Chloride Production system.
Below in conjunction with specific embodiment, the present invention will be further described:
Embodiment 1:
Flow process as shown in the figure, adds 95% ammonium chloride 300kg/h and lime powder (the CaO content 77.32%) 215kg/h from lime powder feed bin 2 to send into mix after conveying auger 15 mixes to enter I stage reactor 3 from ammonium chloride feed bin 1, add 0.24m simultaneously
3the light liquid of/h carries out fully mixing and partial reaction through stirring, 89.5 ℃ of temperature of reaction, I order reaction liquid lime powder CaO excess quantity 9.91%, by I level transferpump 4, deliver to I level distillation tower 7 tops and carry out heat and mass from the steam of II level distillation tower 8 and the gas mixture counter current contact of ammonia, from the I level distillate temperature overflowing at the bottom of I level distillation tower 7 towers, it is 118.1 ℃, I level distillate goes II stage reactor 5 further to react from the overflow of I level base product, for guaranteeing ammonium chloride decomposition reaction, at II stage reactor 5, add 10kg/h steam, 120 ℃ of temperature.The reaction solution of II stage reactor 5 is delivered to II level distillation tower 8 tops by II level transferpump 6, together with the secondary steam of 0.5MPa low-pressure steam and II level distillate shwoot, through steam injector 9, enter II level distillation tower 8 bottoms, foundation ring to steam remaining ammonia, I, the ammonia that II stage reactor produces enters I level distillation tower 7 middle parts, I level distillation tower 7 air outlet temperatures are 99.1 ℃ and discharge from tower top, the solution that gained phlegma goes light liquid distillation tower 12 to steam after ammonia after 11 condensations of 1# ammonia cooler is called light liquid, remove to enter I stage reactor 3 and lime powder, ammonium chloride fully mixes, there is partial reaction, the ammonia that light liquid distillation tower 12 steams reclaims ammonia with removing ammonia absorption tower together with ammonia from 1# ammonia cooler 11 after 13 condensations of 2# ammonia cooler.After the ammonia still process that II level base product is discharged, solution is called II level distillate, 119.8 ℃ of temperature, and the solution after 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 (the CaO content 75.76%) 210kg/h from lime powder feed bin 2 to send into mix after conveying auger 15 mixes to enter I stage reactor 3 from ammonium chloride feed bin 1, add 0.25m simultaneously
3the light liquid of/h carries out fully mixing and partial reaction through stirring, 79.7 ℃ of temperature of reaction, I order reaction liquid lime powder CaO excess quantity 5.30%, by I level transferpump 4, deliver to I level distillation tower 7 tops and carry out heat and mass from the steam of II level distillation tower 8 and the gas mixture counter current contact of ammonia, from the I level distillate temperature overflowing at the bottom of I level distillation tower 7 towers, it is 117.6 ℃, I level distillate goes II stage reactor 5 further to react from the overflow of I level base product, for guaranteeing ammonium chloride decomposition reaction, at II stage reactor 5, add 7.8kg/h steam, 114.7 ℃ of temperature.The reaction solution of II stage reactor 5 is delivered to II level distillation tower 8 tops by II level transferpump 6, together with the secondary steam of 0.5MPa low-pressure steam and II level distillate shwoot, through steam injector 9, enter II level distillation tower 8 bottoms, foundation ring to steam remaining ammonia, I, the ammonia that II stage reactor produces enters I level distillation tower 7 middle parts, I level distillation tower 7 air outlet temperatures are 94.7 ℃ and discharge from tower top, the solution that gained phlegma goes light liquid distillation tower 12 to steam after ammonia after 11 condensations of 1# ammonia cooler is called light liquid, remove to enter I stage reactor 3 and lime powder, ammonium chloride fully mixes, there is 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 goes ammonia absorption tower to reclaim ammonia together.After the ammonia still process that II level base product is discharged, solution is called II level distillate, 116.9 ℃ of temperature, and the solution after 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 (the CaO content 80.26%) 128kg/h from lime powder feed bin 2 to send into mix after conveying auger 15 mixes to enter I stage reactor 3 from ammonium chloride feed bin 1, add 0.20m simultaneously
3the light liquid of/h carries out fully mixing and partial reaction through stirring, 70.7 ℃ of temperature of reaction, I order reaction liquid lime powder CaO excess quantity 3.21%, by I level transferpump 4, deliver to I level distillation tower 7 tops and carry out heat and mass from the steam of II level distillation tower 8 and the gas mixture counter current contact of ammonia, from the I level distillate temperature overflowing at the bottom of I level distillation tower 7 towers, it is 117.2 ℃, I level distillate goes II stage reactor 5 further to react from the overflow of I level base product, for guaranteeing ammonium chloride decomposition reaction, at II stage reactor 5, add 5.4kg/h steam, 100.8 ℃ of temperature.The reaction solution of II stage reactor 5 is delivered to II level distillation tower 8 tops by II level transferpump 6, together with the secondary steam of 0.5MPa low-pressure steam and II level distillate shwoot, through steam injector 9, enter II level distillation tower 8 bottoms, foundation ring to steam remaining ammonia, I, the ammonia that II stage reactor produces enters I level distillation tower 7 middle parts, I level distillation tower 7 air outlet temperatures are 90.2 ℃ and discharge from tower top, the solution that gained phlegma goes light liquid distillation tower 12 to steam after ammonia after 11 condensations of 1# ammonia cooler is called light liquid, remove to enter I stage reactor 3 and lime powder, ammonium chloride fully mixes, there is partial reaction, the ammonia that light liquid distillation tower 12 steams reclaims ammonia with removing ammonia absorption tower together with ammonia from 1# ammonia cooler 11 after 13 condensations of 2# ammonia cooler.After the ammonia still process that II level base product is discharged, solution is called II level distillate, 118.4 ℃ of temperature, and the solution after 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. utilize lime powder decomposing ammonium chloride to prepare a method for high calcium chloride concentration solution, it is characterized in that comprising the following steps:
(1) decomposition reaction of ammonium chloride: the wet ammonium chloride from connection alkali II process is entered and mixed conveying auger by feed bin respectively through metering with the lime powder from lime pulverized coal preparation system, after mixing, enter I stage reactor, in I stage reactor, lime powder CaO excess quantity is more than 3%, temperature of reaction is 70 ~ 90 ℃, add a certain amount of light liquid coming from light liquid distillation tower through stirring abundant mixing, partial reaction, generate I order reaction liquid, by I level transferpump, carry, wherein some I order reaction liquid returns to I stage reactor and circulates, all the other deliver to I level distillation tower top, with the steam of discharging from II level distillation tower top entering 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, I level distillate enters II stage reactor from overflow at the bottom of I level distillation tower tower and continues reaction, II stage reactor bottom passes into a certain amount of low-pressure steam, temperature of reaction is more than 100 ℃, generate II order reaction liquid, by II level transferpump, carried, wherein some II order reaction liquid returns to II stage reactor and circulates, all the other deliver to II level distillation tower top, the steam spraying through steam injector enters from the bottom of II level distillation tower, steam remaining ammonia in II order reaction liquid, become II level distillate, from II level distillation tower tower bottom flow, go out,
(2) generation of high calcium chloride concentration solution: the II level distillate going out from II level distillation tower tower bottom flow becomes high calcium chloride concentration solution through flash evaporation shwoot, high calcium chloride concentration solution contains ammonia lower than 100mg/L, calcium chloride mass percentage content >=38%, by dense calcium transferpump, deliver to Calcium Chloride Production system, the secondary steam that shwoot goes out enters steam injector;
(3) recovery of ammonia: the ammonia that discharge at I, II stage reactor top enters I level distillation tower middle part, and I level distillation tower tower top air outlet temperature is 90 ~ 100 ℃, and the ammonia steaming is discharged from tower top, through 1
#the condensed ammonia of ammonia cooler is delivered to ammonia absorption tower, and its phlegma enters light liquid distillation tower, and the ammonia that light liquid distillation tower top steams is through 2
#after ammonia cooler condensation, also deliver to ammonia absorption tower, the light liquid that light liquid distillation tower tower bottom flow goes out returns to I stage reactor for chloride leach and lime powder digestion reaction.
2. the method for utilizing lime powder decomposing ammonium chloride to prepare high calcium chloride concentration solution according to claim 1, is characterized in that in described I stage reactor, lime powder CaO excess quantity is 3 ~ 10%.
3. the method for utilizing lime powder decomposing ammonium chloride to prepare high calcium chloride concentration solution according to claim 1, is characterized in that the temperature of reaction of described II stage reactor is 100 ~ 120 ℃.
4. the method for utilizing lime powder decomposing ammonium chloride to prepare high calcium chloride concentration solution according to claim 1, temperature >=115 ℃ of the I level distillate going out at the bottom of the I level distillation tower tower described in it is characterized in that.
5. the method for utilizing lime powder decomposing ammonium chloride to prepare high calcium chloride concentration solution according to claim 1, temperature >=115 ℃ of the II level distillate that the II level base product described in it is characterized in that goes out.
6. the method for utilizing lime powder decomposing ammonium chloride to prepare high calcium chloride concentration solution according to claim 1, is characterized in that the total calcium oxide mass percentage content of lime powder is more than 75%.
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| 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 |
| 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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|---|---|---|---|---|
| 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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| JPS605023A (en) * | 1983-06-22 | 1985-01-11 | Tokuyama Soda Co Ltd | Production of aqueous solution of calcium chloride |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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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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 |