CN112316723A - Automobile urea solution for efficiently solving crystallization blockage - Google Patents
Automobile urea solution for efficiently solving crystallization blockage Download PDFInfo
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- B01D53/34—Chemical or biological purification of waste gases
- B01D53/92—Chemical or biological purification of waste gases of engine exhaust gases
- B01D53/94—Chemical or biological purification of waste gases of engine exhaust gases by catalytic processes
- B01D53/9404—Removing only nitrogen compounds
- B01D53/9409—Nitrogen oxides
- B01D53/9413—Processes characterised by a specific catalyst
- B01D53/9418—Processes characterised by a specific catalyst for removing nitrogen oxides by selective catalytic reduction [SCR] using a reducing agent in a lean exhaust gas
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- C07C273/14—Separation; Purification; Stabilisation; Use of additives
- C07C273/16—Separation; Purification
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
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- F01N3/00—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust
- F01N3/08—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous
- F01N3/10—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust
- F01N3/18—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by methods of operation; Control
- F01N3/20—Exhaust or silencing apparatus having means for purifying, rendering innocuous, or otherwise treating exhaust for rendering innocuous by thermal or catalytic conversion of noxious components of exhaust characterised by methods of operation; Control specially adapted for catalytic conversion
- F01N3/206—Adding periodically or continuously substances to exhaust gases for promoting purification, e.g. catalytic material in liquid form, NOx reducing agents
- F01N3/2066—Selective catalytic reduction [SCR]
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- B01D2258/012—Diesel engines and lean burn gasoline engines
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- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F01—MACHINES OR ENGINES IN GENERAL; ENGINE PLANTS IN GENERAL; STEAM ENGINES
- F01N—GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR MACHINES OR ENGINES IN GENERAL; GAS-FLOW SILENCERS OR EXHAUST APPARATUS FOR INTERNAL-COMBUSTION ENGINES
- F01N2610/00—Adding substances to exhaust gases
- F01N2610/02—Adding substances to exhaust gases the substance being ammonia or urea
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Abstract
The invention discloses a vehicle urea solution for efficiently solving crystallization blockage, which is characterized by comprising the following components in parts by weight: 13-14 parts of urea, 5-6 parts of ethanolamine, 4-5 parts of simethicone, 4-6 parts of glycerol, 0.5-1.5 parts of alkyl glucoside,100 parts of ultrapure water, 0.6-0.7 part of carbon smoke catalytic material and 3.5-4.5 parts of silicon type antifreezing solution. To solve the existing urea NOXThe tail gas emission is not up to standard due to the crystallization blockage and the high solidification point.
Description
Technical Field
The invention relates to the technical field of production of automobile urea solution, in particular to automobile urea solution for efficiently solving crystallization blockage.
Background
High-purity urea solution suitable for SCR (selective catalytic reduction) system of vehicle ureaUnder the condition of high temperature (above 300 ℃), the urea solution is firstly decomposed into ammonia gas, and at the high temperature, the urea solution is gasified and then decomposed to generate NH3In the presence of a catalyst, NH3With NO in the exhaust gasXReaction to produce harmless H2O and N2。
However, the urea of the diesel engine for vehicles is decomposed into NH3Production of intermediate product NO in the processx，NOxIs a general term for all nitrogen oxides, the harm to human health is great, NOxThe harm of the formed secondary pollutant ozone to the human respiratory system is also obvious, because the particulate matter is suspended in the air, the lung and heart diseases can be caused, and the carcinogenic probability is increased. NOxComprises urea biuret, cyanuric acid, melamine and the like,
the undecomposed urea, cyanuric acid, melamine and the like are deposited and attached to an exhaust pipeline, a mixer and an SCR catalyst for a long time, so that the original gas fluency is influenced, and the SCR system is blocked.
"ZL 201710409586.0" discloses a urea solution for diesel vehicles with low temperature performance; the automobile urea solution has a lower freezing point than that of common automobile urea, although the damage to the automobile caused by the solidification of the urea solution at low temperature is solved; however, this urea has poor dispersibility, so that NO is producedxThe conversion rate is low, the discharged particles are adhered to the smoke exhaust pipe, and the technical problem of urea blockage cannot be solved in the using process.
Disclosure of Invention
The invention aims to solve the technical problem of providing a vehicle urea solution for efficiently solving the problem of crystal blockage so as to solve the problem of the existing urea NOXThe tail gas emission is not up to standard due to the crystallization blockage and the high solidification point.
In order to solve the technical problems, the invention adopts the following technical scheme:
a vehicle urea solution for efficiently solving crystallization blockage is designed, and comprises the following components in parts by weight: 13-14 parts of urea, 5-6 parts of ethanolamine, 4-5 parts of simethicone, 4-6 parts of glycerol, 0.5-1.5 parts of alkyl glucoside, 100 parts of ultrapure water, 0.6-0.7 part of soot catalytic material and 3.5-4.5 parts of silicon antifreezing solution.
Preferably, the soot catalytic material is prepared as follows:
1) taking La (NO)3) 3•6H2O、KNO3、Co(NO3) 3•6H2O and Ni (NO)3) 3•6H2O, ammonium metavanadate and citric acid, preparing a solution with the mass fraction of 0.9-1.0% by using deionized water, adding 0.45-0.50% of sodium metaaluminate according to the mass of the solution, and adding nanoscale WO in the stirring process3/TiO2Performing ultrasonic oscillation on the mixture powder for 20-45 min, putting the mixture powder into an electric furnace, roasting the mixture powder for 1.5-2 hours at the temperature of 550-560 ℃, and naturally cooling the mixture powder to room temperature;
2) putting the substance obtained in the step 1) into 650-680 ℃, heating for 20-30 minutes, and naturally cooling to room temperature, wherein the weight ratio of the substance to the substance is 1: 3 addition of V2O5。
Preferably, the preparation of urea comprises the following steps:
1) reacting high-purity ammonia and carbon dioxide at high temperature and high pressure in a first reactor and a second reactor; collecting and compressing the gas in the second reactor, then passing the gas through the first reactor again, and collecting the liquid urea melt fluid in the first reactor and the second reactor;
2) flash evaporating liquid urea melt under reduced pressure to remove ammonia and CO2Adding high-purity water with the temperature of 75-80 ℃ and uniformly mixing to obtain a urea saturated solution, collecting gas subjected to flash evaporation treatment and introducing the gas into the first reactor;
3) filtering the urea aqueous solution obtained in the step 2) by using a filter membrane with the aperture of 0.2-0.5 mu m;
4) putting the urea saturated solution obtained in the step 3) into a multistage liquid film crystallization kettle to obtain urea crystals.
Preferably, in the step 1), the pressure in the first reactor is controlled to be 1.55-1.80 Mpa, and the temperature is controlled to be 175-200 ℃; the pressure in the second reactor is controlled to be 0.2-0.50 Mpa, and the temperature is controlled to be 100-110 ℃.
Preferably, in step 2), the ammonium carbamate is gradually decomposed in the liquid urea melt under the conditions of heat supply, reduced pressure and flash evaporation.
Preferably, in the step 2), the reduced pressure condition is controlled to be 0.10 to 14 MPa.
Preferably, in the step 4), the multistage liquid film crystallization kettle comprises 3 cold sections with gradually reduced temperatures, the temperature difference of each cold section is at least 10 ℃, and the temperature difference between the urea saturated solution and the first cold section is 30-50 ℃.
Preferably, in step 4), the filtrates from the crystallization kettles are collected separately and introduced into the crystallization kettle of the next stage.
Compared with the prior art, the invention has the beneficial technical effects that:
the alkyl glucoside has excellent dispersion and diffusion characteristics, and can improve the dispersibility of urea, thereby promoting the decomposition of the urea to generate more NH3Increase of NOxThe conversion of (a); under the heating condition, the urea is promoted to decompose to generate ammonia gas, and the ammonia gas is decomposed at high temperature to generate ammonia gas which has a synergistic effect with the ammonia gas generated by the decomposition of the urea, so that the conversion rate of the catalytic reduction of the nitrogen oxide is greatly improved.
The soot catalytic material and the silicon type antifreeze solution added in the invention can effectively reduce the melting point of urea and improve NOXThe conversion rate of the urea can effectively reduce the problem of heavy metal environmental pollution of the urea for vehicles and improve the efficiency of degrading and absorbing nitrogen oxides of the urea for vehicles; and simultaneously, under the combined action of the carbon smoke catalytic material and the silicon type antifreezing solution, the problem of crystallization blockage is solved. NO of the urea for vehicles of the present inventionxThe conversion rate is more than 96.8 percent, the obtained automobile urea effectively degrades nitrogen oxides, and the problem that an SCR system is easy to block is solved; the emission of the automobile exhaust meets the national IV emission standard requirement.
Preferably, V is added into the carbon smoke catalytic material2O5And TiO2In TiO2Into which WO is introduced3/MoO3Can increase the pore diameter of the inner pores formed between the particles, thereby promoting the dispersion of the active components and increasing the contact between the catalyst and the ureaArea, increase NOxThe conversion of (a).
Preferably, the invention adopts a first reactor and a second reactor, and the arrangement of the two reactors helps to improve the reaction rate.
Preferably, the present invention provides that the liquid urea melt stream is subjected to a gradual decomposition of ammonium carbamate under heat supply and reduced pressure conditions under reduced pressure conditions, thereby increasing the purity of the produced urea.
Detailed Description
The following examples are given to illustrate specific embodiments of the present invention, but are not intended to limit the scope of the present invention in any way. The instruments and devices referred to in the following examples are conventional instruments and devices unless otherwise specified; the raw materials are all conventional commercial industrial raw materials if not specifically indicated; the processing and manufacturing methods are conventional methods unless otherwise specified.
Example 1: a vehicle urea solution for efficiently solving crystallization blockage comprises the following components, by weight, 13 parts of urea, 5 parts of ethanolamine, 5 parts of simethicone, 6 parts of glycerol, 0.5 part of alkyl glucoside, 100 parts of ultrapure water, 0.6 part of carbon smoke catalytic material and 3.5 parts of silicon type antifreeze solution; the preparation method of the soot catalytic material comprises the following steps:
1) taking La (NO)3) 3•6H2O、KNO3、Co(NO3) 36H 2O and Ni (NO)3) 3•6H2Preparing 0.9 mass percent solution from O, ammonium metavanadate and citric acid by using deionized water, adding 0.45-0.50 mass percent of sodium metaaluminate according to the mass of the solution, adding nanoscale WO3/TiO2 mixture powder in the stirring process, performing ultrasonic oscillation for 20min, placing the mixture into a temperature-controlled electric furnace, roasting the mixture at the high temperature of 550 ℃ for 1.5 hours, and naturally cooling the mixture to the room temperature;
2) heating the substance obtained in the step 1) at 680 ℃ for 30 minutes, naturally cooling to room temperature, and mixing the substances according to a weight ratio of 1: 3 addition of V2O5。
Wherein, La (NO)3) 3•6H2O、KNO3、Co(NO3) 36H 2O and Ni (NO)3) 3•6H2The mass ratio of O, ammonium metavanadate and citric acid is 1: 1-2: 1.5-2: 2: 4: 3.
the preparation method of the urea in the vehicle urea solution for efficiently solving the crystallization blockage comprises the following steps:
1) passing high purity ammonia and carbon dioxide through a first reactor, a second reactor at elevated temperature and pressure; collecting and compressing the gas in the second reactor, then passing the gas through the first reactor again, and collecting the liquid urea melt fluid in the first reactor and the second reactor; controlling the pressure in the first reactor to be 1.55-1.80 Mpa and the temperature to be 175-200 ℃; the pressure in the second reactor is controlled to be 0.2-0.50 Mpa, and the temperature is controlled to be 100-110 DEG C
2) Flash evaporating liquid urea melt under reduced pressure to remove ammonia and CO2Adding high-purity water with the temperature of 78 ℃ and uniformly mixing to obtain a urea saturated solution, collecting gas subjected to flash evaporation treatment and introducing the gas into the first reactor; the obtained liquid urea melt is placed under the conditions of heat supply, pressure reduction and flash evaporation to gradually decompose ammonium carbamate, and the pressure reduction condition is controlled to be 14 MPa;
3) filtering the urea aqueous solution obtained in the step 2) by using a filter membrane with the aperture of 0.2 mu m;
4) putting the urea saturated solution obtained in the step 3) into a multistage liquid film crystallization kettle, and adding the obtained urea crystal into deionized water for dissolving; wherein the multistage liquid film crystallization kettle comprises 3 cold sections with gradually reduced temperature, the temperature of the first cold section is 60 ℃, the temperature of the second cold section is 30 ℃, and the temperature of the third cold section is 5 ℃.
The urea production capacity of the invention is up to 2016MTD urea, the utilization rate of NOx conversion rate can reach 97.3%, and the urea does not crystallize at minus 40 ℃.
1. The urea for the present invention was tested at low temperature:
the engine is normally started at the temperature of more than-30 ℃ of the environment, the cooling liquid is introduced into a unfreezing pipeline of the urea box for unfreezing after the temperature of the cooling liquid of the engine is raised to 70 ℃, when the temperature of the urea solution reaches-5 ℃, the SCR system starts to normally inject urea, and the SCR system is not in fault after being processed during the unfreezing period. Tests prove that the vehicle runs normally in suburbs, the vehicle speed is 60km/h, the unfreezing time is about 45 minutes, the SCR works normally, and the SCR can meet the requirements under the condition that the freezing point is-35 ℃ urea.
2. The urea for the present invention was tested at high temperature:
under the full-load state of the whole vehicle, the accelerator is the largest on a continuous uphill road section, the vehicle speed is maintained within the range of 75-85 km/h, the gear is adjusted according to the road condition to increase the rotating speed of the engine, and the temperature of the antifreeze and the engine oil is observed.
Running at 6 grades, wherein the highest temperature of the antifreeze is 85 ℃ and the temperature of the engine oil is 102 ℃; and 5, running at the gear, wherein the highest temperature of the antifreeze is 80 ℃ and the highest temperature of the engine oil is 111 ℃. The temperature of the antifreeze and the temperature of the engine oil both meet the use requirements under the high-temperature condition.
3. Smoke intensity optimization
The air input in plateau areas is low, and visible smoke is easier to appear in tail gas. And at each altitude, the engine works at each gear, the accelerator is stepped to the bottom to work at the maximum oil quantity, and the tail gas condition of the exhaust pipe is observed. Blue smoke is not allowed to appear, the altitude is more than 3000m, and a small amount of black smoke is allowed to appear in quick acceleration; above the altitude of 4000m, dynamic behavior is prioritized.
Example 2: the difference from example 1 is that:
a vehicle urea solution for efficiently solving crystallization blockage comprises the following components in parts by weight: 14 parts of urea, 5 parts of ethanolamine, 5 parts of simethicone, 5 parts of glycerol, 0.5 part of alkyl glucoside, 100 parts of ultrapure water, 0.7 part of carbon smoke catalytic material and 4.5 parts of silicon type antifreeze solution.
The urea production capacity of the invention is as high as 2019MTD urea, the utilization rate of NOx conversion rate can reach more than 96.9%, and the urea is not crystallized at minus 40 ℃. SCR works normally, and the SCR can meet the requirement under the condition that the freezing point is urea at minus 35 ℃.
Example 3: the difference from example 1 is that: the preparation method of the soot catalytic material comprises the following steps:
1) taking La (NO)3) 3•6H2O、KNO3、Co(NO3) 36H 2O and Ni (NO)3) 3•6H2Preparing a solution with the mass fraction of 1.0% by using deionized water, adding 0.50% of sodium metaaluminate according to the mass of the solution, adding nanoscale WO3/TiO2 mixture powder in the stirring process, performing ultrasonic oscillation for 30min, placing the mixture into a temperature-controlled electric furnace, roasting the mixture at the high temperature of 560 ℃ for 1.5 hours, and naturally cooling the mixture to the room temperature;
2) heating the substance obtained in the step 1) at 680 ℃ for 30 minutes, naturally cooling to room temperature, and mixing the substances according to a weight ratio of 1: 3 addition of V2O5。
The urea production capacity of the invention is up to 2003MTD urea, the utilization rate of NOx conversion rate can reach more than 96.8%, and the urea is not crystallized at minus 40 ℃.
Although the present invention has been described in detail with reference to the embodiments, it will be understood by those skilled in the art that various changes in the specific parameters of the embodiments may be made without departing from the spirit of the present invention, and a plurality of specific embodiments are formed, which are common variations of the present invention, and will not be described in detail herein.
Claims (8)
1. The vehicle urea solution for efficiently solving the problem of crystallization blockage is characterized by comprising the following components in parts by weight: 13-14 parts of urea, 5-6 parts of ethanolamine, 4-5 parts of simethicone, 4-6 parts of glycerol, 0.5-1.5 parts of alkyl glucoside, 100 parts of ultrapure water, 0.6-0.7 part of soot catalytic material and 3.5-4.5 parts of silicon antifreezing solution.
2. The vehicle urea solution for efficiently solving the crystal blockage problem according to claim 1, wherein the soot catalytic material is prepared by the following method:
1) taking La (NO)3) 3•6H2O、KNO3、Co(NO3) 3•6H2O and Ni (NO)3) 3•6H2O, ammonium metavanadate and citric acid, preparing a solution with the mass fraction of 0.9-1.0% by using deionized water, adding 0.45-0.50% of sodium metaaluminate according to the mass of the solution, and adding nanoscale WO in the stirring process3/TiO2Performing ultrasonic oscillation on the mixture powder for 20-45 min, putting the mixture powder into an electric furnace, roasting the mixture powder for 1.5-2 hours at the temperature of 550-560 ℃, and naturally cooling the mixture powder to room temperature;
2) putting the substance obtained in the step 1) into 650-680 ℃, heating for 20-30 minutes, and naturally cooling to room temperature, wherein the weight ratio of the substance to the substance is 1: 3 addition of V2O5。
3. The vehicular urea solution for efficiently solving the crystal blockage according to claim 1, wherein the preparation of the urea comprises the following steps:
1) reacting high-purity ammonia and carbon dioxide at high temperature and high pressure in a first reactor and a second reactor; collecting and compressing the gas in the second reactor, then passing the gas through the first reactor again, and collecting the liquid urea melt fluid in the first reactor and the second reactor;
2) flash evaporating liquid urea melt under reduced pressure to remove ammonia and CO2Adding high-purity water with the temperature of 75-80 ℃ and uniformly mixing to obtain a urea saturated solution, collecting gas subjected to flash evaporation treatment and introducing the gas into the first reactor;
3) filtering the urea aqueous solution obtained in the step 2) by using a filter membrane with the aperture of 0.2-0.5 mu m;
4) putting the urea saturated solution obtained in the step 3) into a multistage liquid film crystallization kettle to obtain urea crystals.
4. The vehicular urea solution for efficiently solving the crystal blockage according to claim 3, characterized in that: in the step 1), the pressure in the first reactor is controlled to be 1.55-1.80 Mpa, and the temperature is controlled to be 175-200 ℃; the pressure in the second reactor is controlled to be 0.2-0.50 Mpa, and the temperature is controlled to be 100-110 ℃.
5. The vehicular urea solution for efficiently solving the crystal blockage according to claim 3, characterized in that: in step 2), the ammonium carbamate is gradually decomposed in the liquid urea melt under the conditions of heat supply, reduced pressure and flash evaporation.
6. The vehicular urea solution for efficiently solving the crystal blockage according to claim 3, characterized in that: in the step 2), the decompression condition is controlled to be 0.10-14 MPa.
7. The vehicular urea solution for efficiently solving the crystal blockage according to claim 3, characterized in that: in the step 4), the multistage liquid film crystallization kettle comprises 3 cold sections with gradually reduced temperatures, the temperature difference of each cold section is at least 10 ℃, and the temperature difference between the urea saturated solution and the first cold section is 30-50 ℃.
8. The vehicular urea solution with high efficiency for solving the crystal blockage according to claim 3, wherein in the step 4), the filtered liquid from the crystallization kettle is collected respectively and introduced into the crystallization kettle of the next stage.
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