CN101125666A - Technique for preparing ammonia from urea by pyrolysis method - Google Patents
Technique for preparing ammonia from urea by pyrolysis method Download PDFInfo
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- CN101125666A CN101125666A CNA2007100926077A CN200710092607A CN101125666A CN 101125666 A CN101125666 A CN 101125666A CN A2007100926077 A CNA2007100926077 A CN A2007100926077A CN 200710092607 A CN200710092607 A CN 200710092607A CN 101125666 A CN101125666 A CN 101125666A
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Abstract
The invention discloses a technique to prepare ammonia from urea through thermolysis, comprising the steps that: step 1: a storage and dissolution system (1) for urea particles is set; step 2: a storage system (2) for urea solution is set; step 3: an urea thermolysis system is set; step 4: a waste liquid treatment system (4) is set; step 5: all systems of the whole technique are communicated; step 6: urea particles are stored and dissolved; step 7: urea is cleaved and ammonia is acquisited; and step 8: waste liquid is treated. The preparation method of ammonia of the invention has the advantages of low cost, simple operation, needing not high pressure, quick respond (the reaction can begin in 5 to 30 sec.), various heating means, and gas fuel or diesel and so on can be used.
Description
Technical field
The invention belongs to the denitrating flue gas field, relate to the preparation technology of denitrification reducing agent-ammonia specifically.
Background technology
Selective catalytic reduction (being SCR) is meant under the effect of catalyzer, is reductive agent with NH3, with oxynitride (NOX) reaction nontoxic, free of contamination N2 of generation and the H2O in the flue gas.The material that can produce denitrification reducing agent NH3 has three kinds in liquefied ammonia, ammoniacal liquor and urea.
Anhydrous ammonia has another name called liquefied ammonia, is hazardous chemical.Anhydrous ammonia is leaked in the air, forms cloud with airborne water, is difficult for diffusion, and near people personnel safety is worked the mischief.The limits of explosion of ammonia steam and air mixture is 16%～25%, and ammonia and air mixture reach above-mentioned concentration range chance naked light and can burn and explode, and exist if any oils or other inflammable substances, and then danger is higher.Ammoniacal liquor also belongs to hazardous substance, its concentration of ammoniacal liquor that is used for denitration is generally 20%～29%, and ammoniacal liquor is comparatively safe than anhydrous ammonia, but also has explosion hazard when airborne ammonia reaches 15%-28%, therefore, anhydrous ammonia and ammoniacal liquor have the blue law laws and regulations requirement in country aspect storage and the transportation.
Than anhydrous ammonia and ammoniacal liquor, urea is nontoxic, harmless chemical, is convenient to transportation and storage, can transport with train or automobile, and transportation and storage process do not need special security measures.Urea allows environment better as denitrification reducing agent, can avoid causing danger when storage, pipeline and valve are revealed, and therefore, more and more people adopt urea as denitrification reducing agent.
The method of urea system ammonia mainly contains two kinds of hydrolysis method and pyrolysis methods.Pyrolysis method does not also have the sophisticated technology of a cover, and hydrolysis of urea legal system ammonia is not too commonly used again, and, mainly there is following problem:
(1) water consumption is big;
(2) easily generate the residual urea polymkeric substance;
(3) hydrolytic process needs the High Temperature High Pressure operation, is prone to safety problem;
(4) cost compares higher;
Summary of the invention
The purpose of this invention is to provide a kind of can be under condition of normal pressure, the technique for preparing ammonia from urea by pyrolysis method that the time of response is fast.
Technical scheme of the present invention is as follows:
Step 2, the urea soln stocking system is set, the urea soln hold-up vessel is set earlier, this urea soln hold-up vessel bottom is connected with solution input tube and output tube, dispose agitator in the jar of bottom, described input tube is provided with No. 4 control valves and described output tube is provided with control valve No. 5, is provided with Send out pump on the output tube between these No. 5 control valves and the urea soln hold-up vessel; Described urea soln hold-up vessel inner bottom part is provided with No. 2 well heaters and waste liquid output tube;
Step 3, the urea pyrolysis system is set, the pyrolysis chamber is set earlier, its bottom is connected with the waste material output tube, and this pyrolysis chamber is made up of the atomization tank of vertical layout and decomposition storehouse two portions of lateral arrangement, and described atomization tank lower end is communicated with decomposition storehouse head end, this atomization tank top is provided with the solution atomization input tube, this input tube one end extend in the pyrolysis chamber, and is provided with atomizing nozzle, and the described input tube the other end is provided with solution flow totalizer and No. 6 control valves; There are oil gun and air input tube in described atomizing nozzle below, and this air input tube outer end is provided with air filter, is positioned at described air input tube between this air filter and the vertical atomization tank of arranging and is provided with air flowmeter and gas blower; The decomposition Cang Ding storehouse of described pyrolysis chamber lateral arrangement is provided with and the gapped dividing plate of Lower Hold; Lower Hold is provided with and pushes up the gapped dividing plate in storehouse, and dividing plate laterally is interspersed, and the tail end in described decomposition storehouse is connected with gas output tube;
Step 4 is provided with the waste liquid disposal system, and the waste collection jar is set earlier, and this waste collection jar upper end is connected with the waste liquid input tube, and agitator is equipped with in the below in jar; Described waste collection jar bottom connects the waste liquid vent pipe;
Step 6, the storage of urea granules and dissolving, after the outsourcing urea granules is sent here by truck, be stored in the urea granules hold-up vessel, and keep the drying of urea granules by gasification wind well heater, and prevent the urea granules crystallization of making moist, be discharged in the dissolving vessel after weighing by Weighing feeder, open No. 1 valve then by water delivery flow totalizer metering input water dissolution, be mixed with 40% urea soln; No. 1 well heater is kept whole urea soln about 35 degree, open No. 2 control valve, close No. 3 control valve agitator stirrings simultaneously, mixing pump is started working, urea soln is fully dissolved and mix, open No. 3 control valves and No. 4 control valves and close control valve simultaneously No. 2, above-mentioned urea soln enters the urea soln hold-up vessel through input tube, keeps whole urea soln stand-by in the 35 degree left and right sides with No. 2 well heaters;
Step 7, urea decomposition is produced ammonia, open No. 5 control valves and No. 6 control valves, flow totalizer is delivered to atomizing nozzle by metering with the urea soln of needs and is injected in the pyrolysis chamber, it is 300 ℃～650 ℃ that the while oil gun is kept the indoor decomposition temperature of pyrolysis, dividing plate in the spray chamber increases the residence time of urea in decomposition chamber, makes urea fully decompose generation ammonia, and principal reaction is: CO (NH
2)
2→ NH
3+ HNCO HNCO+H
2O → NH
3+ CO
2, in whole decomposition course, gas blower blasts air dilution ammonia, makes ammonia concentration＜5% in the gas of pyrolysis chamber's outlet, and the mixed gas temperature is controlled at 260 ℃～400 ℃ scopes;
Step 8, liquid waste disposal, more than operation half a year, dissolving vessel, urea soln hold-up vessel, pyrolysis chamber need clean, and clean waste liquid and enter the waste collection tank stores through the waste liquid output tube, discharge after being diluted with water to 5～7% concentration;
The water that is used for dissolved urea in the described dissolving vessel is de-mineralized water, and this de-mineralized water water quality requirement is:
(1) total hardness (representing)＜150 μ g/g with CaCO3
(2) electroconductibility＜250 μ s/cm
(3)SiO2＜15μg/g
(4) metal object (iron, zinc, lead, manganese, chromium, nickel, copper) total amount＜1 μ g/g
(5) sodium＜5 μ g/g
(6) orthophosphoric acid salt, arsenic, mercury＜1 μ g/g
(7) suspended solid＜10NTU
(8) vitriol＜10 μ g/g
(9) the pH value about 7～9
Above-mentioned de-mineralized water can promote the abundant dissolving of urea, and the by product of dissolution process generation simultaneously is less.
Between the solution output tube of described urea storage dissolution system and the solution input tube of described urea soln stocking system; Be equipped with strainer between the solution output tube of urea soln stocking system and the urea pyrolysis system solution input tube solution in each step is filtered, the most of impurity of elimination is beneficial to better carrying out and the decomposition reaction of urea in the pyrolysis chamber of whole flow process.
Described urea granules hold-up vessel is a glass-reinforced plastic material, and the stirring rod of the agitator in the whole technology, pump, dissolving vessel, solution hold-up vessel, decomposition chamber and atomizing nozzle are stainless steel, and erosion resistance is stronger, is beneficial to the long-term circulation of whole technology and carries out.
Advantage of the present invention:
1. cost is low;
2. simple to operate, need not high pressure, normal pressure gets final product.
Time of response fast, begin reaction in 5～30 seconds; And the time of response of hydrolysis method is very slow, needs 5～15 minutes.
4. type of heating variation can be adopted geseous fuel or diesel oil etc.; And hydrolysis method can only adopt steam heating.
Description of drawings
Fig. 1 is the technique for preparing ammonia from urea by pyrolysis method schema;
Embodiment
Embodiment
See also Fig. 1, be that the urea system ammonia system of 14.2Kg/h is that example describes with the hydrazine yield:
1, urea granules stores and dissolution system
After the outsourcing urea granules is sent here by truck, be stored in the urea granules hold-up vessel 1-3, gasification wind-powered electricity generation well heater 1-4 keeps the drying of urea granules, prevents the urea granules crystallization of making moist.Hydrazine yield is 14.2Kg/h, calculates in 5 hours with continuous operation, and the volume of urea granules warehouse is 120L,
Urea dissolving vessel 1-1 is stainless steel, volume 200L, flow into the de-mineralized water dissolving through hydraulic pipe 1-6, be mixed with 40% urea soln, hydraulic pipe 1-6 is provided with water delivery flow totalizer 1-7 to guarantee that the urea concentration after the preparation is 40%, and the 40Kg urea granules needs de-mineralized water 60L to dissolve; No. 1 well heater 1-13 remains on about 35 ℃ solution temperature.Also dispose the stirring rod of stainless steel in the urea dissolving vessel 1-1, stir urea soln, promote dissolving; Urea dissolving vessel 1-1 adopts stainless steel mixing pump 1-10 that urea soln is circulated to sidepiece from pot bottom outward, and the promotion urea soln fully dissolves and mixes.
2, urea soln stocking system
Urea soln comes out after strainer 4 is stored in the urea soln hold-up vessel 2-1 after filtering from dissolving vessel 1-1, by about 35 ℃ of the urea soln temperature in No. 2 well heater 2-7 maintenance hold-up vessels, prevents the urea soln low temperature crystallization.
3, urea pyrolysis system
The 3-1 of pyrolysis chamber need carry out insulation, and volume is at 1m
3, warm air maintains decomposition temperature about 450 ℃ by oil gun 3-5, needs the 0# diesel oil of 15kg/h.11 seconds residence time in the pyrolysis chamber of urea, urea is converted into ammonia.Urea is injected in the warm air decomposition chamber after through stainless steel atomizing nozzle 3-2 urea soln being atomized, and the emitted dose of urea soln is to need the ammonia amount to decide by solution flow quantity recorder 3-3 by the SCR reactor to measure; Hydrazine yield is 14.2Kg/h, and 40% urea soln demand is 62.5Kg/h.In reaction process, needing gas blower gas blower 3-8 to blast air dilution ammonia is measured by air flowmeter 3-7, obtain the air/ammonia mixture of ammonia concentration＜5% in the exit, pyrolysis chamber, and the temperature that guarantees the outlet mixed gas is in 260 ℃～400 ℃ scopes, so that follow-up SCR reactor uses.
5. waste liquid disposal system
The ammonia waste liquid unification of discharging is collected among the waste collection jar 4-1 and is stored, and agitator 4-2 stirs, and waste liquid is discharged by waste liquid vent pipe 4-3 after being diluted to 6% concentration.
Claims (4)
1. technique for preparing ammonia from urea by pyrolysis method is characterized in that carrying out as follows:
Step 1, urea granules is set to be stored and dissolution system (1), dissolving vessel (1-1) is set earlier, this dissolving vessel (1-1) top is by the pipe connection urea granules hold-up vessel (1-3) of band Weighing feeder (1-2), and this urea granules hold-up vessel (1-3) sidewall opening is provided with gasification wind well heater (1-4); Described dissolving vessel (1-1) upper portion side wall has stretched into hydraulic pipe (1-5), and this hydraulic pipe (1-5) is provided with No. 1 valve (1-6) and water delivery flow totalizer (1-7); Dispose agitator (1-9) in the jar of described dissolving vessel (1-1) bottom, dissolving vessel (1-1) bottom is connected with pipeline (1-8), described pipeline (1-8) is provided with mixing pump (1-10), this mixing pump (1-10) output terminal is connected with Y-tube, an outlet of this Y-tube is connected and is communicated with tank body with described dissolving vessel (1-1) top sidewall through No. 2 control valves (1-11), and it is the solution output tube that another outlet is provided with No. 3 control valves (1-12); Described dissolving vessel (1-1) inner bottom part is provided with No. 1 well heater (1-13) and waste liquid output tube (1-14);
Step 2, urea soln stocking system (2) is set, urea soln hold-up vessel (2-1) is set earlier, this urea soln hold-up vessel (2-1) bottom is connected with solution input tube (2-8) and output tube (2-9), dispose agitator (2-2) in the jar of bottom, described input tube is provided with No. 4 control valves (2-3) and described output tube is provided with No. 5 control valves (2-4), is provided with Send out pump (2-5) on the output tube (2-9) between these No. 5 control valves (2-4) and the urea soln hold-up vessel (2-1); Described urea soln hold-up vessel (2-1) inner bottom part is provided with No. 2 well heaters (2-7) and waste liquid output tube (2-10);
Step 3, urea pyrolysis system (3) is set, pyrolysis chamber (3-1) is set earlier, its bottom is connected with waste material output tube (3-13), this pyrolysis chamber (3-1) is made up of the atomization tank of vertical layout and decomposition storehouse two portions of lateral arrangement, described atomization tank lower end is communicated with decomposition storehouse head end, this atomization tank top is provided with solution atomization input tube (3-12), this input tube (3-12) end extend in the pyrolysis chamber (3-1), and being provided with atomizing nozzle (3-2), described input tube (3-12) the other end is provided with solution flow totalizer (3-3) and No. 6 control valves (3-4); There are oil gun (3-5) and air input tube (3-14) in described atomizing nozzle (3-2) below, this air input tube (3-14) outer end is provided with air filter (3-6), is positioned at described air input tube (3-14) between this air filter (3-6) and the vertical atomization tank of arranging and is provided with air flowmeter (3-7) and gas blower (3-8); The decomposition Cang Ding storehouse of described pyrolysis chamber (3-1) lateral arrangement is provided with and the gapped dividing plate of Lower Hold (3-9); Lower Hold is provided with and pushes up the gapped dividing plate in storehouse (3-10), and dividing plate (3-9,3-10) laterally is interspersed, and the tail end in described decomposition storehouse is connected with gas output tube (3-11);
Step 4 is provided with waste liquid disposal system (4), and waste collection jar (4-1) is set earlier, and this waste collection jar (4-1) upper end is connected with the waste liquid input tube, and agitator (4-2) is equipped with in the below in jar; Described waste collection jar (4-1) bottom connects waste liquid vent pipe (4-3);
Step 5, be communicated with all systems in the whole technology, the solution output tube that described urea granules is stored dissolution system (1) is connected with the solution input tube (2-8) of described urea soln stocking system (2), and the solution output tube (2-9) of this urea soln stocking system (2) is connected with urea pyrolysis system (3) solution input tube (3-12) again; The waste liquid output tube (1-14,2-10,3-13) that described urea granules stores dissolution system (1), urea soln stocking system (2), urea pyrolysis system (3) is connected with the waste collection jar (4-1) of described waste liquid disposal system (4);
Step 6, the storage of urea granules and dissolving, after the outsourcing urea granules is sent here by truck, be stored in the urea granules hold-up vessel (1-3), and keep the drying of urea granules by gasification wind well heater (1-4), and prevent the urea granules crystallization of making moist, be discharged in the dissolving vessel after weighing by Weighing feeder (1-2), open No. 1 valve (1-6) then by water delivery flow totalizer (1-7) metering input water dissolution, be mixed with 40% urea soln; No. 1 well heater (1-13) is kept whole urea soln about 35 degree, open No. 2 control valves (1-11), close No. 3 control valves (1-12) agitator (1-9) stirring simultaneously, mixing pump (1-10) is started working, urea soln is fully dissolved and mix, open No. 3 control valves (1-12) and No. 4 control valves (2-3) and close No. 2 control valves (1-11) simultaneously, above-mentioned urea soln enters urea soln hold-up vessel (2-1) through input tube, keeps whole urea soln stand-by in the 35 degree left and right sides with No. 2 well heaters (2-7);
Step 7, urea decomposition is produced ammonia, open No. 5 control valves (2-4) and No. 6 control valves (3-4), flow totalizer (3-3) is delivered to atomizing nozzle (3-2) by metering with the urea soln of needs and is ejected in the pyrolysis chamber (3-1), keeping the interior decomposition temperature in pyrolysis chamber (3-1) by oil gun (3-5) simultaneously is 300 ℃～650 ℃, dividing plate (3-9,3-10) in the spray chamber increases the residence time of urea in decomposition chamber, makes urea fully decompose generation ammonia, and principal reaction is: CO (NH
2)
2→ NH
3+ HNCO HNCO+H
2O → NH
3+ CO
2, in whole decomposition course, gas blower (3-8) blasts air dilution ammonia, makes ammonia concentration＜5% in the gas of pyrolysis chamber's outlet, and the mixed gas temperature is controlled at 260 ℃～400 ℃ scopes.
Step 8, liquid waste disposal was moved more than half a year, and dissolving vessel (1-1), urea soln hold-up vessel (2-1), pyrolysis chamber (3-1) need clean, clean waste liquid and enter waste collection jar (4-1) through the waste liquid output tube and store, and be diluted to 5～7% concentration and discharge.
2. according to the described technique for preparing ammonia from urea by pyrolysis method of claim 1, it is characterized in that: the water that is used for dissolved urea in the described dissolving vessel (1-1) is de-mineralized water, and this de-mineralized water water quality requirement is:
(1) total hardness is (with CaCO
3Expression)＜150 μ g/g
(2) electroconductibility＜250 μ s/cm
(3)SiO
2＜15μg/g
(4) metal object (iron, zinc, lead, manganese, chromium, nickel, copper) total amount＜1 μ g/g
(5) sodium＜5 μ g/g
(6) orthophosphoric acid salt, arsenic, mercury＜1 μ g/g
(7) suspended solid＜10NTU
(8) vitriol＜10 μ g/g
(9) the pH value about 7～9.
3. according to the described technique for preparing ammonia from urea by pyrolysis method of claim 1, it is characterized in that: between the solution output tube of described urea storage dissolution system (1) and the solution input tube of described urea soln stocking system (2); Be equipped with strainer (5) between the solution output tube of urea soln stocking system (2) and urea pyrolysis system (3) the solution input tube.
4. according to the described technique for preparing ammonia from urea by pyrolysis method of claim 1, it is characterized in that: described urea granules hold-up vessel (1-3) is a glass-reinforced plastic material, and the stirring rod of the agitator in the whole technology, pump, dissolving vessel (1-1), solution hold-up vessel (2-1), decomposition chamber (3-1) and atomizing nozzle (3-2) are stainless steel.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101797469A (en) * | 2010-03-18 | 2010-08-11 | 南京耦联科技有限公司 | Urea pyrolysis reactor for flue gas denitrification |
| CN101928014A (en) * | 2010-08-13 | 2010-12-29 | 朱红路 | Process for producing ammonia from urea used for denitration of boiler smoke and system thereof |
| CN102580529A (en) * | 2012-02-27 | 2012-07-18 | 环境保护部华南环境科学研究所 | Electro-pyrolytic urea solution ammonia production device used for selective catalytic denitration and application thereof |
| CN104474892A (en) * | 2014-12-09 | 2015-04-01 | 邹英奎 | Production method of denitrification powder |
| CN105883853A (en) * | 2016-06-28 | 2016-08-24 | 盐城工学院 | Method for preparing ammonia with urea |
| CN108019758A (en) * | 2017-12-08 | 2018-05-11 | 大唐洛阳热电有限责任公司 | A kind of method of modifying of pyrolysis oven in pyrolysis denitrating technique |
| CN109437237A (en) * | 2018-12-21 | 2019-03-08 | 广东工业大学 | A method of automation fixed nitrogen ammonia |
| CN109641743A (en) * | 2016-08-30 | 2019-04-16 | 全耐塑料高级创新研究公司 | System and method for increasing urea concentration of an aqueous solution on board a vehicle |
| CN114115390A (en) * | 2020-08-28 | 2022-03-01 | 陕西青朗万城环保科技有限公司 | Urea pyrolysis method based on microwaves and control system thereof |
| CN115259179A (en) * | 2022-07-14 | 2022-11-01 | 华能国际电力股份有限公司大连电厂 | Urea pyrolysis ammonia production system and application method thereof |
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| US5809775A (en) * | 1997-04-02 | 1998-09-22 | Clean Diesel Technologies, Inc. | Reducing NOx emissions from an engine by selective catalytic reduction utilizing solid reagents |
| US5968464A (en) * | 1997-05-12 | 1999-10-19 | Clean Diesel Technologies, Inc. | Urea pyrolysis chamber and process for reducing lean-burn engine NOx emissions by selective catalytic reduction |
| ITMI981155A1 (en) * | 1998-05-25 | 1999-11-25 | Siirtec Nigi S P A | PROCESS FOR THE PRODUCTION OF AMMONIA BY HYDROLYSIS OF THE UREA |
| DE10206028A1 (en) * | 2002-02-14 | 2003-08-28 | Man Nutzfahrzeuge Ag | Process and apparatus for producing ammonia |
| EP1533018A1 (en) * | 2003-11-05 | 2005-05-25 | Urea Casale S.A. | Method for the treatment of combustion flue gas |
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| CN101797469A (en) * | 2010-03-18 | 2010-08-11 | 南京耦联科技有限公司 | Urea pyrolysis reactor for flue gas denitrification |
| CN101928014A (en) * | 2010-08-13 | 2010-12-29 | 朱红路 | Process for producing ammonia from urea used for denitration of boiler smoke and system thereof |
| CN102580529A (en) * | 2012-02-27 | 2012-07-18 | 环境保护部华南环境科学研究所 | Electro-pyrolytic urea solution ammonia production device used for selective catalytic denitration and application thereof |
| CN102580529B (en) * | 2012-02-27 | 2014-10-08 | 环境保护部华南环境科学研究所 | Electro-pyrolytic urea solution ammonia production device used for selective catalytic denitration and application thereof |
| CN104474892A (en) * | 2014-12-09 | 2015-04-01 | 邹英奎 | Production method of denitrification powder |
| CN105883853B (en) * | 2016-06-28 | 2019-01-04 | 盐城工学院 | A kind of method that urea prepares ammonia |
| CN105883853A (en) * | 2016-06-28 | 2016-08-24 | 盐城工学院 | Method for preparing ammonia with urea |
| CN109641743A (en) * | 2016-08-30 | 2019-04-16 | 全耐塑料高级创新研究公司 | System and method for increasing urea concentration of an aqueous solution on board a vehicle |
| CN108019758A (en) * | 2017-12-08 | 2018-05-11 | 大唐洛阳热电有限责任公司 | A kind of method of modifying of pyrolysis oven in pyrolysis denitrating technique |
| CN108019758B (en) * | 2017-12-08 | 2023-09-19 | 大唐洛阳热电有限责任公司 | Modification method of pyrolysis furnace used in pyrolysis denitration process |
| CN109437237A (en) * | 2018-12-21 | 2019-03-08 | 广东工业大学 | A method of automation fixed nitrogen ammonia |
| CN114115390A (en) * | 2020-08-28 | 2022-03-01 | 陕西青朗万城环保科技有限公司 | Urea pyrolysis method based on microwaves and control system thereof |
| CN115259179A (en) * | 2022-07-14 | 2022-11-01 | 华能国际电力股份有限公司大连电厂 | Urea pyrolysis ammonia production system and application method thereof |
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Assignee: Chongqing Puyuan Chemical Industry Co., Ltd. Assignor: Chongqing University|CPI Yuanda Environmental Protection Engineering Co. Ltd. Contract record no.: 2010500000025 Denomination of invention: Technique for preparing ammonia from urea by pyrolysis method Granted publication date: 20100210 License type: Exclusive License Open date: 20080220 Record date: 20100428 |