CN102583438A - Process for preparing ammonia by utilizing calcium oxide - Google Patents
Process for preparing ammonia by utilizing calcium oxide Download PDFInfo
- Publication number
- CN102583438A CN102583438A CN2012100337656A CN201210033765A CN102583438A CN 102583438 A CN102583438 A CN 102583438A CN 2012100337656 A CN2012100337656 A CN 2012100337656A CN 201210033765 A CN201210033765 A CN 201210033765A CN 102583438 A CN102583438 A CN 102583438A
- Authority
- CN
- China
- Prior art keywords
- ammonium chloride
- reaction
- ammonia
- add
- reaction kettle
- 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
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 120
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 59
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 239000000292 calcium oxide Substances 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title abstract description 9
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 title abstract 2
- 238000000034 method Methods 0.000 claims abstract description 20
- 238000005520 cutting process Methods 0.000 claims abstract description 7
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 132
- 238000006243 chemical reaction Methods 0.000 claims description 121
- 235000019270 ammonium chloride Nutrition 0.000 claims description 59
- 239000000843 powder Substances 0.000 claims description 23
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 22
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 22
- 235000012255 calcium oxide Nutrition 0.000 claims description 22
- 239000004571 lime Substances 0.000 claims description 22
- 239000002245 particle Substances 0.000 claims description 20
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 17
- 239000001110 calcium chloride Substances 0.000 claims description 17
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 238000002425 crystallisation Methods 0.000 claims description 9
- 229920006395 saturated elastomer Polymers 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 230000008025 crystallization Effects 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 238000001694 spray drying Methods 0.000 claims description 2
- 239000006227 byproduct Substances 0.000 claims 1
- 238000010924 continuous production Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 14
- 235000011148 calcium chloride Nutrition 0.000 description 13
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 6
- 239000000920 calcium hydroxide Substances 0.000 description 6
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 6
- 239000007787 solid Substances 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 239000011575 calcium Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 235000019633 pungent taste Nutrition 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Classifications
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
Landscapes
- Treating Waste Gases (AREA)
Abstract
The invention discloses a process for preparing ammonia by utilizing calcium oxide. The process is simple, has low investment, is energy-saving and is very suitable for enterprises which need to be supplied with a small amount of ammonia. The ammonia can be prepared by respectively adopting a feeding and cutting process and a continuous process.
Description
Technical field
The present invention relates to chemical field, particularly relate to and a kind ofly produce the technology of ammonia with the reaction of quicklime and ammonium chloride solution, technology is simple, invests little.
Background technology
Ammonia, mineral compound, chemical formula: NH3; Normal temperature is down gas, and colourless have a malodorous smell of pungency, soluble in water.In chemical engineering industry, ammonia is to process through N2 and H2 direct chemical combination in the presence of HTHP and catalyzer with aber process.The working method of this ammonia is fit to industrial mass production, for example several ten thousand tons, hundreds of thousands of ton/year.Yet, sometimes, need the production of ammonia on a small scale in the industry, for example, 500-5000 ton/year.At this moment, aber process is obviously inapplicable.
Can be used for laboratory system ammonia with calcium hydroxide (solid)+ammonium chloride (solid), still, be inappropriate for the production of ammonia on a small scale.Therefore, a kind of technology that adapts to small-scale production ammonia of invention will have fine current demand.
Summary of the invention
The object of the present invention is to provide a kind of technology of small-scale production ammonia, can be suitable for the production of 500-3000 ton/year ammonia.
The present invention adopts quicklime and ammonium chloride solution reaction, produces ammonia, and reaction formula is following:
CaO
+?H2O?=?Ca(OH)
2 （1）
2NH
4Cl?+?Ca(OH)
2=2NH3↑+?CaCl
2?+?2H
2O （2）
Net reaction:
H
2O
CaO
+2NH
4Cl = 2NH
3↑+?CaCl2?+?H
2O （3）
This process using mode of treating different things alike adds entry, ammonium chloride in reaction kettle, add lime powder then; Quicklime reacts with water immediately; Generate calcium hydroxide, owing to be connected to ammonium chloride in the reaction solution, so; The calcium hydroxide that generates reacts with ammonium chloride immediately, and calcium hydroxide does not form solid precipitation.Because reaction is for homogeneous reaction, so speed of response is fast.On the contrary, if with calcium hydroxide powder (because its solubleness is very little, being actually solid) and ammonium chloride solution reaction, then reaction is inhomogeneous reaction, and speed of response is very slow, is far smaller than homogeneous reaction.So, adopt this technology, significantly be superior to the reaction of calcium hydroxide (solid)+chloride solid or solution.
In addition, reaction (1) is thermopositive reaction, is thermo-negative reaction and react (2), and the heat that reaction (1) produces can be used for adding reaction solution, and provides reaction (2) required heat.It is thus clear that the present invention saves the energy.
The present invention can use 2 kinds of concrete technologies to realize.
1, stream adds+division process (technology 1)
Add entry in the reaction kettle, add ammonium chloride, obtain certain density ammonium chloride solution, 200-600kg/m
3(partly dissolving) then, adds lime powder and ammonium chloride particle simultaneously, and the mol ratio that the adding speed of lime powder and ammonium chloride particle is pressed 1:2 adds, reaction beginning, the ammonia that the discharge of reaction kettle top produces.Temperature of reaction is 50-80 ℃.When calcium chloride concentration in the reaction kettle when saturated, carry out cutting operation, stop to add ammonium chloride, continue reaction, make that ammonium chloride concentration reduces in the reaction solution, stop to add quicklime, reduce quicklime concentration, discharge the 70-90% reaction solution.Begin a new operational cycle, add ammonium chloride, water, quicklime, continue reaction, generate ammonia.The reaction solution of discharging from reaction kettle mainly contains calcium chloride, and near saturated, can use several different methods dry, for example spraying drying, or crystallization after drying etc.For continous-stable externally provides ammonia, an ammonia hold tank can be set.
2, continuous processing (technology 2)
Add in the reaction kettle in the reaction kettle and add entry, add ammonium chloride, obtain certain density ammonium chloride solution, 200-600kg/m
3(partly dissolving) then, adds lime powder and ammonium chloride particle and water simultaneously, and the adding speed mol ratio of lime powder and ammonium chloride particle is 1:2, and the adding speed mass ratio of water and ammonium chloride is 0.1667-1.5:1.Temperature of reaction is 50-80 ℃.Meanwhile, begin to discharge reaction solution, discharge rate and feed material amount balance make the reaction kettle liquid level keep stable, discharge the calcium chloride in the reaction solution, can reclaim with crystallization or spray-drying process.The reaction kettle top begins the stable ammonia of discharging.For continous-stable externally provides ammonia, an ammonia hold tank can be set.
Compare with technology 1, the ammonium chloride concentration in technology 2 relief liquors is higher, and ammonia-nitrogen content is high in the subsequent waste water.The ammonia generation of technology 2 is comparatively even, and still, each link control requires high to technology.Technology 1 is when cutting operation, and the ammonia generation has certain fluctuation.
Obviously, technical process of the present invention is simple, investment is little, needing to be particularly suitable for the enterprise demand of small-scale production ammonia.
Below in conjunction with specific embodiment the present invention is further described.
Embodiment
Embodiment 1
Adopt stream to add+division process, produce 500 tons of ammonia per year, year 300 days working dayss.7m
3Reaction kettle adds entry 4.8m in the reaction kettle
3, add ammonium chloride, making concentration is 500kg/m
3Ammonium chloride solution, the part the dissolving, then, add lime powder (content 90%) and ammonium chloride particle (content 97%) simultaneously, the adding speed of lime powder and ammonium chloride particle is respectively 127.04kg/h and 224.85kg/h.Reaction beginning, reaction kettle top are discharged and are produced ammonia, 68-70kg/h.80 ° of C of temperature of reaction kettle, reaction 24h, when calcium chloride concentration in the reaction kettle when saturated, carry out cutting operation, stop to add ammonium chloride, continue reaction, make that ammonium chloride concentration reduces in the reaction solution, stop to add quicklime, discharge 80% reaction solution.Begin a new operational cycle, add ammonium chloride, water, quicklime, add-on is the same, continues reaction, generates ammonia.The reaction solution crystallisation by cooling that reaction kettle is discharged is dry, obtain the calcium chloride product.For continous-stable externally provides ammonia, be provided with a 5m
3The ammonia hold tank.
Embodiment 2
Adopt continuous processing, produce 500 tons of ammonia per year, year 300 days working dayss.1m
3Reaction kettle adds entry 0.75m in the reaction kettle
3, add ammonium chloride, obtaining concentration is 500kg/m
3Ammonium chloride solution; Add quicklime; After question response is stable, add lime powder (content 90%), ammonium chloride particle (content 97%) and water simultaneously, the adding speed of lime powder, ammonium chloride particle and water is respectively 127.04kg/h, 224.85kg/h and 37.7kg/h.70 ° of C of temperature of reaction kettle, meanwhile, beginning filtering emission reaction solution, discharge rate and feed material amount balance make the reaction kettle level stability.The ammonia that produces, 68-70kg/h are discharged in the reaction kettle top.The reaction solution that reaction kettle is discharged, spraying drying obtains the calcium chloride product.Contain ammonia in the dry waste gas, need through removing.
Embodiment 3
Adopt stream to add+division process, produce 1000 tons of ammonia per year, year 300 days working dayss.13m
3Reaction kettle adds entry 9.6m in the reaction kettle
3, add ammonium chloride, obtaining concentration is 200kg/m
3Ammonium chloride solution (part dissolving), then, add lime powder (content 90%) and ammonium chloride particle (content 97%) simultaneously, the adding speed of lime powder and ammonium chloride particle is respectively 228.67kg/h and 436.21kg/h.60 ° of C of temperature of reaction kettle, the reaction beginning, the ammonia that produces, 135-143kg/h are discharged in the reaction kettle top.Reaction 24h, when calcium chloride concentration in the reaction kettle when saturated, carry out cutting operation, stop to add ammonium chloride, continue reaction, make that ammonium chloride concentration reduces in the reaction solution, stop to add quicklime, discharge 80% reaction solution.Begin a new operational cycle, add ammonium chloride, water, quicklime, add-on is the same, continues reaction, generates ammonia.The reaction solution crystallisation by cooling that reaction kettle is discharged is dry, obtain the calcium chloride product.
Embodiment 4
Adopt continuous processing, produce 1000 tons of ammonia per year, year 300 days working dayss.2m
3Reaction kettle adds entry 1.5m in the reaction kettle
3, add ammonium chloride, obtaining concentration is 600kg/m
3Ammonium chloride solution; Add quicklime; After question response is stable, add lime powder (content 90%), ammonium chloride particle (content 97%) and water simultaneously, the adding speed of lime powder, ammonium chloride particle and water is respectively 228.67kg/h, 436.21kg/h and 678kg/h.80 ° of C of temperature of reaction kettle, the reaction beginning, the ammonia that produces, 135-143kg/h are discharged in the reaction kettle top.Meanwhile, begin to discharge reaction solution, discharge rate and feed material amount balance make the reaction kettle level stability.The reaction solution crystallisation by cooling that reaction kettle is discharged is dry, obtains the calcium chloride product.Contain ammonia in the waste liquid, need remove, to subdue ammonia nitrogen value in the waste water.
Embodiment 5
Adopt stream to add+division process, produce 3000 tons of ammonia per year, year 300 days working dayss.20m
3Reaction kettle adds entry 9.6m in the reaction kettle
3, add ammonium chloride, obtaining concentration is 400kg/m
3Ammonium chloride solution (part dissolving), then, add lime powder (content 90%) and ammonium chloride particle (content 97%) simultaneously, the adding speed of lime powder and ammonium chloride particle is respectively 686kg/h, 1357.571kg/h.60 ° of C of temperature of reaction kettle, the reaction beginning, the ammonia that produces, 410-430kg/h are discharged in the reaction kettle top.Reaction 12h, when calcium chloride concentration in the reaction kettle when saturated, carry out cutting operation, stop to add ammonium chloride, continue reaction, make that ammonium chloride concentration reduces in the reaction solution, stop to add quicklime, discharge 80% reaction solution.Begin a new operational cycle, add ammonium chloride, water, quicklime, add-on is the same, continues reaction, generates ammonia.The reaction solution crystallisation by cooling that reaction kettle is discharged is dry, obtain the calcium chloride product.For continous-stable externally provides ammonia, be provided with a 20m
3The ammonia hold tank.
Embodiment 6
Adopt continuous processing, produce 3000 tons of ammonia per year, year 300 days working dayss.2.5m
3Reaction kettle adds entry 2m in the reaction kettle
3, add ammonium chloride, obtaining concentration is 500kg/m
3Ammonium chloride solution; Add quicklime; After question response is stable, add lime powder (content 90%), ammonium chloride particle (content 97%) and water simultaneously, the adding speed of lime powder, ammonium chloride particle and water is respectively 686kg/h, 1357.571kg/h and 1131kg/h.80 ° of C of temperature of reaction kettle, the reaction beginning, the ammonia that produces, 410-430kg/h are discharged in the reaction kettle top.Meanwhile, begin to discharge reaction solution, discharge rate and feed material amount balance make the reaction kettle level stability.The reaction solution crystallisation by cooling that reaction kettle is discharged is dry, obtains the calcium chloride product.Contain ammonia in the waste liquid, need remove, to subdue ammonia nitrogen value in the waste water.
Claims (3)
1.
OnePlant the quicklime Ammonia Process, it is characterized in that lime powder is added ammonium chloride solution reacted ammonia, and obtain the calcium chloride by product.
2.
The described Ammonia Process of claim 1 is characterized in that adopting stream to add+division process, and concrete reactions step is following: add entry in the reaction kettle, add ammonium chloride, make 200-600kg/m
3Ammonium chloride solution, then, add lime powder and ammonium chloride particle simultaneously, the adding speed mol ratio of lime powder and ammonium chloride particle is 1:2, reaction beginning, the reaction kettle top is discharged and is produced ammonia; Temperature of reaction is 50-80 ℃; When calcium chloride concentration in the reaction kettle when saturated, carry out cutting operation, stop to add ammonium chloride, continue reaction, make that ammonium chloride concentration reduces in the reaction solution, stop to add quicklime, reduce quicklime concentration, discharge the 70-90% reaction solution; Begin a new operational cycle, add ammonium chloride, water, quicklime, continue reaction, generate ammonia; The reaction solution of discharging from reaction kettle mainly contains calcium chloride, can use several different methods dry, for example spraying drying, or crystallization after drying; For continous-stable externally provides ammonia, an ammonia hold tank can be set.
3.
The described Ammonia Process of claim 1; It is characterized in that to adopt continuous processing, add entry and ammonium chloride in the reaction kettle, make the ammonium chloride solution of 200-600kg/m3; Then; Add lime powder, ammonium chloride particle and water simultaneously, the adding speed mol ratio of lime powder and ammonium chloride particle is 1:2, and the adding speed mass ratio of water and ammonium chloride is 0.1667-1.5:1; Temperature of reaction is 50-80 ℃; Meanwhile, reaction kettle begins to discharge reaction solution, and discharge rate and feed material amount balance make the reaction kettle liquid level keep stable; Discharge the calcium chloride in the reaction solution, can reclaim with crystallization or spray-drying process; The reaction kettle top begins to stablize the output ammonia; For continous-stable externally provides ammonia, an ammonia hold tank can be set.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210033765.6A CN102583438B (en) | 2012-02-15 | 2012-02-15 | Process for preparing ammonia by utilizing calcium oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210033765.6A CN102583438B (en) | 2012-02-15 | 2012-02-15 | Process for preparing ammonia by utilizing calcium oxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102583438A true CN102583438A (en) | 2012-07-18 |
| CN102583438B CN102583438B (en) | 2014-04-23 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210033765.6A Expired - Fee Related CN102583438B (en) | 2012-02-15 | 2012-02-15 | Process for preparing ammonia by utilizing calcium oxide |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976355A (en) * | 2012-10-31 | 2013-03-20 | 四川大学 | Production process for ammonia gas and calcium chloride through utilization of ammonium chloride and carbide slag |
| CN104609441A (en) * | 2015-01-05 | 2015-05-13 | 河北科技大学 | Method for decomposing ammonium chloride by semidry method and reactor |
Citations (5)
| 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 |
| CN101823695A (en) * | 2010-04-30 | 2010-09-08 | 汪晋强 | Method for co-production of light calcium carbonate and ammonium chloride in preparation of potassium chlorate by carbide slag |
| 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 |
| CN102070159A (en) * | 2010-11-19 | 2011-05-25 | 浙江海虹控股集团有限公司 | Method for recovering ammonia from solid-state inorganic strong acid ammonium salt by utilizing quick lime |
| CN102267713A (en) * | 2011-07-07 | 2011-12-07 | 贵州大学 | Method for producing high-quality light calcium carbonate by ammonium salt circulation process |
-
2012
- 2012-02-15 CN CN201210033765.6A patent/CN102583438B/en not_active Expired - Fee Related
Patent Citations (5)
| 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 |
| CN101823695A (en) * | 2010-04-30 | 2010-09-08 | 汪晋强 | Method for co-production of light calcium carbonate and ammonium chloride in preparation of potassium chlorate by carbide slag |
| 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 |
| CN102070159A (en) * | 2010-11-19 | 2011-05-25 | 浙江海虹控股集团有限公司 | Method for recovering ammonia from solid-state inorganic strong acid ammonium salt by utilizing quick lime |
| CN102267713A (en) * | 2011-07-07 | 2011-12-07 | 贵州大学 | Method for producing high-quality light calcium carbonate by ammonium salt circulation process |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102976355A (en) * | 2012-10-31 | 2013-03-20 | 四川大学 | Production process for ammonia gas and calcium chloride through utilization of ammonium chloride and carbide slag |
| CN104609441A (en) * | 2015-01-05 | 2015-05-13 | 河北科技大学 | Method for decomposing ammonium chloride by semidry method and reactor |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102583438B (en) | 2014-04-23 |
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