CN113479910A - Method for sequentially releasing chlorine and ammonia by decomposing ammonium chloride - Google Patents
Method for sequentially releasing chlorine and ammonia by decomposing ammonium chloride Download PDFInfo
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- CN113479910A CN113479910A CN202110889209.8A CN202110889209A CN113479910A CN 113479910 A CN113479910 A CN 113479910A CN 202110889209 A CN202110889209 A CN 202110889209A CN 113479910 A CN113479910 A CN 113479910A
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- ammonia
- ammonium chloride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/26—Carbonates or bicarbonates of ammonium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B7/00—Halogens; Halogen acids
- C01B7/01—Chlorine; Hydrogen chloride
- C01B7/03—Preparation from chlorides
- C01B7/05—Preparation from ammonium chloride
- C01B7/055—Preparation of hydrogen chloride from ammonium chloride
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- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
A method for sequentially releasing chlorine and ammonia by decomposing ammonium chloride uses ammonium chloride as a raw material for releasing chlorine and ammonia, uses an acid sulfate melt or solution as a decomposition medium of ammonium chloride, and sequentially releases chlorine and ammonia under the synergistic effect of water vapor and carrier gas to realize that the ammonium chloride is decomposed at 100-200 ℃ and 210-380 ℃ to sequentially release chlorine and ammonia, and has the advantages of low chlorine release decomposition temperature, HCl and NH4The method has the advantages of good Cl separation effect, high operation efficiency, convenient operation and the like, and is suitable for large-scale industrial application of decomposing, separating and recovering hydrochloric acid and ammonium carbonate salt or ammonia by ammonium chloride.
Description
Technical Field
The invention belongs to the field of chemical metallurgy, and particularly relates to a method for sequentially releasing chlorine and ammonia by decomposing ammonium chloride.
Background
A large amount of ammonium chloride is produced as a byproduct of enterprises in metallurgy and chemical industry, which is related to chlorine and ammonia, and the ammonium chloride has side effect on soil quality as an agricultural fertilizer, but the application of the ammonium chloride as an industrial raw material is very limited, so that the ammonium chloride product is not sold smoothly, and the development of a method for recycling the ammonium chloride becomes urgent. As is well known, NH4Cl is decomposed into HCl and NH by heating3Cooled and recombined to NH4And (4) Cl. To add NH to4HCl and NH released by Cl decomposition under heating3Separately, attempts have been made to employ chemical chainsBy decomposing NH in basic or acidic medium4Separation of Cl to recover hydrochloric acid and ammonia, e.g. absorption of NH by magnesium oxide or magnesium hydroxide4HCl released by Cl decomposition under heating at-350 ℃ is converted into basic magnesium chloride, thereby separating NH3Then heating the obtained basic magnesium chloride to 600 ℃ to release HCl, regenerating to obtain magnesium oxide or magnesium hydroxide, and returning to be used as a decomposition medium of ammonium chloride continuously; absorption of NH by ammonium bisulfate melt4NH released by Cl heated and decomposed at 220-270 DEG C3Converting the ammonium sulfate into ammonium sulfate, separating HCl, heating the ammonium sulfate to 290-350 ℃ to decompose NH3And the regenerated ammonium bisulfate is returned for recycling. Both of these methods are designed to be elaborate, but have problems in practical applications: first, NH4Cl is easy to sublimate when heated, the existing alkaline medium or acidic medium chemical chain decomposition method is difficult to avoid the sublimation of ammonium chloride, and more than 10 percent of ammonium chloride is usually sublimated directly in the decomposition process; second, NH at elevated temperature4Cl has strong corrosivity to decomposition equipment, chlorine-resistant and acid-resistant equipment with the temperature of more than 200 ℃ is expensive to manufacture, basic magnesium chloride is heated to the temperature of 600 ℃ to be in a static decomposition efficiency, and dynamic decomposition equipment is not mature enough to manufacture; third, ammonium chloride is difficult to release chlorine completely in alkaline media, and difficult to release ammonia completely in acidic media.
Disclosure of Invention
The invention provides a method for sequentially releasing chlorine and ammonia by decomposing ammonium chloride, which aims at overcoming the defects of the prior art and has the advantages of low operation temperature, high decomposition efficiency and convenient operation.
The invention relates to a method for decomposing ammonium chloride to release chlorine and ammonia in turn, which takes ammonium chloride as a raw material for releasing chlorine and ammonia and acid sulfate melt or solution as a decomposition medium of the ammonium chloride to realize the decomposition of the ammonium chloride to release chlorine and ammonia in turn; the acid sulfate comprises at least NaHSO4And NH4HSO4One of (1);
the specific process comprises the following steps:
(1) firstly, adding water into ammonium chloride to prepare solution or slurry, and then adding water into ammonium chloride to prepare solution or slurrySlowly adding the obtained solution or slurry into a decomposition medium with the temperature of 100-200 ℃, and stirring to decompose ammonium chloride into HCl and NH3Generation of NH3By NaHSO in acidic sulfates4Or/and NH4HSO4Absorption and conversion into NH4NaSO4Or/and (NH)4)2SO4HCl is quickly separated from the reaction system under the action of water vapor or/and carrier gas to release chlorine to obtain chlorine-containing gas;
(2) to be reacted in (NH)4NaSO4Or/and (NH)4)2SO4)/(NaHSO4Or/and NH4HSO4) When the molar ratio is increased to 0.1-1, stopping feeding, and purging residual HCl in a reaction system with water vapor or/and carrier gas;
(3) heating to 210-380 ℃, and blowing water vapor or/and carrier gas into the reaction system to promote NH4NaSO4Or/and (NH)4)2SO4Releasing ammonia to obtain ammonia-containing gas and regenerating to obtain NaHSO4Or/and NH4HSO4The ammonia-releasing raffinate.
The invention relates to a method for sequentially releasing chlorine and ammonia by decomposing ammonium chloride, wherein the acid sulfate at least comprises NaHSO4And NH4HSO4And which may or may not contain NH4NaSO4Or/and (NH)4)2SO4A sulfate melt or solution having a melting point of 100 ℃ or lower, wherein NH4NaSO4/NaHSO4The molar ratio of (NH) to (NH) is 0-0.1: 14)2SO4/NH4NaSO4The molar ratio is 0-0.5: 1.
The invention relates to a method for sequentially releasing chlorine and ammonia by decomposing ammonium chloride, which comprises the step (1) of adding water into ammonium chloride solid according to a solid/liquid ratio of 1: 0.2-2 g/mL to prepare solution or slurry with the temperature of more than or equal to 25 ℃.
The invention relates to a method for sequentially releasing chlorine and ammonia by decomposing ammonium chloride, wherein in step (1), chlorine-containing gas is directly condensed to obtain hydrochloric acid, or is firstly subjected to H at the temperature of more than or equal to 60 DEG C2SO4Washing with sulfuric acid solution with concentration of 4mol/L or more, and absorbing with water to obtainHydrochloric acid.
The invention discloses a method for sequentially releasing chlorine and ammonia by decomposing ammonium chloride, wherein in the step (1), the step (2) and the step (3), the carrier gas is selected from gases which do not chemically react with a reaction system, and preferably at least one of air, nitrogen and carbon dioxide gas.
The invention relates to a method for sequentially releasing chlorine and ammonia by decomposing ammonium chloride, in the step (3), ammonia-containing gas is cooled and absorbed by water to obtain ammonia water or ammonium bicarbonate crystals, and the cooled and absorbed tail gas is directly returned or supplemented with water vapor or/and carrier gas and then returned to continuously release ammonia; the residual liquid after releasing ammonia is cooled to less than or equal to 200 deg.c before being returned for further decomposing ammonium chloride.
The invention relates to a method for decomposing ammonium chloride to sequentially release chlorine and ammonia, wherein in the step (3), the ammonium bicarbonate crystals are formed by using CO2As a carrier gas, according to NH3/CO2Blowing humidified CO into the reaction system at a molar ratio of 1: 1-10002To make NH4NaSO4And (NH)4)2SO4Explaining that the temperature of ammonia is reduced, the decomposition speed is accelerated, and ammonia-containing gas generated by releasing ammonia is condensed to obtain ammonium carbonate salt crystals which are directly sold as products.
The invention relates to a method for sequentially releasing chlorine and ammonia by decomposing ammonium chloride, and humidified CO2Medium, water vapor and CO2The molar ratio is 0.01-1: 1.
The invention relates to a method for sequentially releasing chlorine and ammonia by decomposing ammonium chloride, which uses acid sulfate melt or solution as decomposition medium of ammonium chloride to sequentially release chlorine and ammonia under the synergistic action of water vapor or/and carrier gas, wherein the direct yield of chlorine and ammonia is more than or equal to 95%.
The invention relates to a method for decomposing ammonium chloride to release chlorine and ammonia in turn, which has the following basic principle:
NH4Cl＝Cl-+NH4 + (1)
NH4 ++NH4HSO4＝(NH4)2SO4+H+ (2)
NH4 ++NaHSO4＝NH4NaSO4+H+ (3)
CO2+2NH3+H2O＝(NH4)2CO3 (7)
(NH4)2CO3+CO2＝2NH4HCO3 (8)
compared with the prior art, the invention has the following advantages and effects:
1. according to the invention, water is firstly added to prepare ammonium chloride into a solution or slurry, the obtained solution or slurry is added into a melt or solution of the acidic sulfate to release chlorine instead of ammonium chloride solid, the introduction of water is favorable for overflowing HCl, so that the temperature of chlorine in the acidic sulfate is reduced from 220-270 ℃ to 100-200 ℃, and the reduction of the chlorine release temperature is realized, thus not only is the sublimation of ammonium chloride effectively avoided, but also the selection of industrial equipment for decomposing ammonium chloride to release chlorine becomes possible, and the highest service temperature of an industrial enamel reaction kettle, a lining tetrafluoro reactor and a lining graphite reactor is less than or equal to 200 ℃.
2. The present invention skillfully prefers to use humidified CO2As ammonia releasing carrier gas, the initial temperature of ammonia releasing is reduced from 290 ℃ to 210 ℃, and CO is humidified2Can effectively prevent NH4HSO4Further decomposition of (3), released NH3At H2O and CO2Smoothly separate from the reaction system under the synergistic action of (A) and (B), so that NH is generated4NaSO4And (NH)4)2SO4Explaining the reduction of the temperature of ammonia and the acceleration of the decomposition speed, the generated ammonia-containing gas is cooled and absorbed by water to directly obtain ammonium bicarbonate crystals, and the condensed tail gas is supplemented with proper amount of CO2Returning to continue to blow into the reaction system for recycling, and ensuring the high-efficiency recycling of ammonia.
Detailed Description
The invention will now be further described with reference to the following examples, which are intended to illustrate the invention but not to limit it further.
Example 1
Adding water into ammonium chloride to prepare a saturated ammonium chloride solution with the temperature of 95 ℃, and slowly adding the saturated ammonium chloride solution into a container with the volume of 2m3A molar ratio of 1:5 of NaHSO at a temperature of 150 DEG C4/NH4HSO45m of the melt3In enamel chlorine-releasing reactor, ammonium chloride is decomposed into HCl and NH by stirring at constant temp3Generation of NH3Reacting NaHSO4And NH4HSO4Conversion to NH4NaSO4And (NH)4)2SO4HCl rapidly separates from a reaction system under the action of water vapor and air to release chlorine to obtain chlorine-containing gas, the chlorine-containing gas is directly sprayed and condensed by three-stage countercurrent at 0-5 ℃ to obtain-30% industrial hydrochloric acid, and after 5.5 hours of feeding, the solution is subjected to reaction (NH)4NaSO4+(NH4)2SO4)/(NaHSO4+NH4HSO4) The molar ratio was raised to 0.6, the feed was stopped, the HCl remaining in the melt was purged with air and the melt was then taken to 5m3In a stainless steel ammonia release reactor, the temperature of the melt is raised to 240 ℃, and humidified CO at 80 ℃ is blown into the melt2Gas (water vapor and CO therein)2At a molar ratio of 1:8) to promote NH therein4NaSO4And (NH)4)2SO4Conversion of ammonia to NaHSO4And NH4HSO4The volatilized ammonia-containing gas is directly condensed and crystallized to obtain ammonium bicarbonate crystals, and the condensed tail gas supplements CO2Then returning to continuously release ammonia, and releasing after 3hAnd (3) after the ammonia is finished, reducing the temperature of the ammonia release residue to 150 ℃, returning the ammonia release residue to be continuously used for decomposing ammonium chloride, and selling the obtained hydrochloric acid and ammonium bicarbonate as products, wherein the primary separation recovery rate of chlorine and the primary separation recovery rate of ammonia in the process are respectively 95.2% and 95.8%.
Example 2
Adding solid ammonium chloride into water according to the solid/liquid ratio of 1:1g/mL to prepare ammonium chloride slurry with the temperature of 45 ℃, and slowly adding the ammonium chloride slurry into a container with the volume of 1.2m3NH of (2)4HSO4/NaHSO4The molar ratio of (NH) to (1: 10)4)2SO4/NH4HSO43m of melt at 80 ℃ in a molar ratio of 1:1003Heating and stirring the polytetrafluoroethylene lining chlorine release reactor, and decomposing ammonium chloride into HCl and NH at a constant temperature of 180 DEG C3Generation of NH3Reacting NaHSO4And NH4HSO4Conversion to NH4NaSO4And (NH)4)2SO4HCl rapidly departs from the reaction system under the action of water vapor and nitrogen to release chlorine to obtain chlorine-containing gas, the chlorine-containing gas is firstly sprayed and washed by sulfuric acid of 6mol/L at 80 ℃, then is subjected to three-stage countercurrent spraying and absorption by water of 0-5 ℃ to obtain industrial hydrochloric acid of-30%, and after 3 hours of feeding, the industrial hydrochloric acid is added into a melt (NH)4NaSO4+(NH4)2SO4)/(NaHSO4+NH4HSO4) The mol ratio is increased to 0.8, the feeding is stopped, the temperature of the reaction materials is increased to 185-200 ℃, residual HCl in the reaction materials is purged by water vapor, and then the reaction materials are put into a container with the volume of 3m3In the stainless steel ammonia releasing reactor, the temperature of the reaction material is firstly raised to 330 ℃, then nitrogen is blown into the reaction material, and NH is added4NaSO4And (NH)4)2SO4Conversion to NaHSO4And NH4HSO4The released ammonia gas is brought out, the volatilized ammonia-containing gas is sprayed and absorbed by water at 0-10 ℃ to obtain ammonia water, the tail gas after spraying and absorption is returned to continuously release ammonia, the ammonia release is finished after 4.5 hours, finally, the temperature of ammonia-releasing residue is reduced to 180 ℃, the ammonia-releasing residue is returned to be continuously used for decomposing ammonium chloride, the obtained hydrochloric acid and ammonium bicarbonate are sold as products, and the chlorine and the ammonia are separated back in the technical processThe yields were 96.1% and 95.2%, respectively.
Claims (9)
1. A method for sequentially releasing chlorine and ammonia by decomposing ammonium chloride is characterized in that: ammonium chloride is used as a raw material for releasing chlorine and ammonia, and an acid sulfate melt or solution is used as a decomposition medium of the ammonium chloride to realize the decomposition of the ammonium chloride and sequentially release the chlorine and the ammonia, wherein the acid sulfate at least comprises NaHSO4And NH4HSO4One of (1);
the specific process comprises the following steps:
(1) firstly, adding water into ammonium chloride to prepare solution or slurry, then slowly adding the obtained solution or slurry into a decomposition medium with the temperature of 100-200 ℃, and stirring to decompose the ammonium chloride into HCl and NH3Generation of NH3By NaHSO in acidic sulfates4Or/and NH4HSO4Absorption and conversion into NH4NaSO4Or/and (NH)4)2SO4HCl is quickly separated from the reaction system under the action of water vapor or/and carrier gas to release chlorine to obtain chlorine-containing gas;
(2) to be reacted in (NH)4NaSO4Or/and (NH)4)2SO4)/(NaHSO4Or/and NH4HSO4) When the molar ratio is increased to 0.1-1, stopping feeding, and purging residual HCl in a reaction system with water vapor or/and carrier gas;
(3) heating to 210-380 ℃, and blowing water vapor or/and carrier gas into the reaction system to promote NH4NaSO4Or/and (NH)4)2SO4Releasing ammonia to obtain ammonia-containing gas and regenerating to obtain NaHSO4Or/and NH4HSO4The ammonia-releasing raffinate.
2. The method for decomposing ammonium chloride to release chlorine and ammonia sequentially according to claim 1, characterized in that: the acid sulfate at least comprises NaHSO4And NH4HSO4And which may or may not contain NH4NaSO4Or/and (NH)4)2SO4A sulfate melt or solution having a melting point of 100 ℃ or lower, wherein NH4NaSO4/NaHSO4The molar ratio of (NH) to (NH) is 0-0.1: 14)2SO4/NH4NaSO4The molar ratio is 0-0.5: 1.
3. The method for decomposing ammonium chloride to release chlorine and ammonia sequentially according to claim 1, characterized in that: in the step (1), water is added into the ammonium chloride solid according to the solid/liquid ratio of 1: 0.2-2 g/mL to prepare a solution or slurry with the temperature of more than or equal to 25 ℃.
4. The method for decomposing ammonium chloride to release chlorine and ammonia sequentially according to claim 1, characterized in that: in the step (1), the chlorine-containing gas is directly condensed to obtain hydrochloric acid or is firstly subjected to H with the temperature of more than or equal to 60 DEG C2SO4After being washed by sulfuric acid solution with the concentration of more than or equal to 4mol/L, hydrochloric acid is obtained by absorption with water.
5. The method for decomposing ammonium chloride to release chlorine and ammonia sequentially according to claim 1, characterized in that: in the step (1), the step (2) and the step (3), the carrier gas is selected from gases which do not react with the reaction system, preferably at least one of air, nitrogen and carbon dioxide.
6. The method for decomposing ammonium chloride to release chlorine and ammonia sequentially according to claim 1, characterized in that: in the step (3), cooling and absorbing the ammonia-containing gas with water to obtain ammonia water or ammonium bicarbonate crystals, and returning the cooled and absorbed tail gas directly or supplementing water vapor or/and carrier gas and then returning to continuously release ammonia; the residual liquid after releasing ammonia is cooled to less than or equal to 200 deg.c before being returned for further decomposing ammonium chloride.
7. The method for decomposing ammonium chloride to release chlorine and ammonia sequentially according to claim 6, wherein: in the step (3), the ammonium bicarbonate crystals are CO2As a carrier gas, according to NH3/CO2Blowing humidified CO into the reaction system at a molar ratio of 1: 1-10002To make NH4NaSO4And (NH)4)2SO4Explaining that the temperature of ammonia is reduced, the decomposition speed is accelerated, and ammonia-containing gas generated by releasing ammonia is condensed to obtain ammonium carbonate salt crystals which are directly sold as products.
8. The method for decomposing ammonium chloride to release chlorine and ammonia sequentially according to claim 7, wherein: in step (3), the humidified CO2Medium, water vapor and CO2The molar ratio is 0.01-1: 1.
9. A method for the decomposition of ammonium chloride to release chlorine and ammonia sequentially according to any one of claims 1 to 8, wherein: acid sulfate melt or solution is used as decomposition medium of ammonium chloride, and chlorine and ammonia are released in turn under the synergistic action of water vapor and/or carrier gas, and the direct yield of chlorine and ammonia is greater than or equal to 95%.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58156505A (en) * | 1982-03-08 | 1983-09-17 | Toyo Soda Mfg Co Ltd | Process for separating and recovering hydrogen chloride and ammonia from ammonium chloride |
| CN101486474A (en) * | 2008-01-18 | 2009-07-22 | 中国科学院过程工程研究所 | Method for preparing hydrochloric acid and ammonia sulfate by decomposing ammonium chloride in sulfuric acid medium |
| CN102009954A (en) * | 2010-11-30 | 2011-04-13 | 宜宾天原集团股份有限公司 | Method for preparing hydrogen chloride and ammonia by utilizing ammonium chloride |
| CN103145100A (en) * | 2011-09-25 | 2013-06-12 | 云南省化工研究院 | Continuous loop process for preparing hydrogen chloride and ammonia gas by decomposition of ammonium chloride |
| CN108726552A (en) * | 2018-06-13 | 2018-11-02 | 贵阳开磷化肥有限公司 | A method of preparing precipitated calcium carbonate using ammonium chloride decomposing phosphate rock cycle |
-
2021
- 2021-08-04 CN CN202110889209.8A patent/CN113479910B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58156505A (en) * | 1982-03-08 | 1983-09-17 | Toyo Soda Mfg Co Ltd | Process for separating and recovering hydrogen chloride and ammonia from ammonium chloride |
| CN101486474A (en) * | 2008-01-18 | 2009-07-22 | 中国科学院过程工程研究所 | Method for preparing hydrochloric acid and ammonia sulfate by decomposing ammonium chloride in sulfuric acid medium |
| CN102009954A (en) * | 2010-11-30 | 2011-04-13 | 宜宾天原集团股份有限公司 | Method for preparing hydrogen chloride and ammonia by utilizing ammonium chloride |
| CN103145100A (en) * | 2011-09-25 | 2013-06-12 | 云南省化工研究院 | Continuous loop process for preparing hydrogen chloride and ammonia gas by decomposition of ammonium chloride |
| CN108726552A (en) * | 2018-06-13 | 2018-11-02 | 贵阳开磷化肥有限公司 | A method of preparing precipitated calcium carbonate using ammonium chloride decomposing phosphate rock cycle |
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