CN102806011A - Method for preparing automobile urea liquid reducing agent - Google Patents
Method for preparing automobile urea liquid reducing agent Download PDFInfo
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- CN102806011A CN102806011A CN2012100654711A CN201210065471A CN102806011A CN 102806011 A CN102806011 A CN 102806011A CN 2012100654711 A CN2012100654711 A CN 2012100654711A CN 201210065471 A CN201210065471 A CN 201210065471A CN 102806011 A CN102806011 A CN 102806011A
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Abstract
The invention provides a method for preparing an automobile urea liquid reducing agent, which comprises the steps of: step A, taking urea to synthetize reaction solution, removing unconverted product ammonia and carbon dioxide in the urea, enabling the ammonia concentration to be less than 0.4wt%, and obtaining high-purity urea liquid with the urea concentration of 70-75wt% and biuret content of being equal to or less than 0.6wt%; and step B, according to the proportion that the final urea concentration is between 31.8-33.3wt%, mixing the high-purity urea of the step A with high-purity water with the resistivity of 14-18MOmega.cm, then filtering, and thus obtaining the urea liquid reducing agent. The invention further provides an intermediate product which is suitable for the method for preparing the long-distance transport automobile urea liquid reducing agent. According to the method, the urea is taken to synthetize the reaction solution instead of solid urea which is taken as the raw material of the automobile urea liquid reducing agent in the prior art, so the production cost of a product is greatly lowered, and obvious economic benefit is obtained; and in addition, the method does not need to use activated carbon or ion exchange resin for adsorption treatment, also does not have harmful mother liquid discharge, and is an environment-friendly production technology.
Description
Technical field
The present invention relates to the preparation method of a kind of diesel vehicle with urea liquid reducing agent required in the vent gas treatment catalytic reduction device.
Background technology
Diesel-engined vehicle is compared with gasoline automobile, and power performance is good, and the thermal efficiency is high, saves fuel oil, and greenhouse gas emission is lower; But nitrogen oxide and particle are high than gasoline engine in the diesel car exhaust emissions.In order to reduce nitrogen oxide and the particle in the diesel car exhaust emissions, state's car manufactures such as America and Europe have adopted a kind of SCR (SCR) technical finesse exhaust gas from diesel vehicle, make it to reach the discharge standard of Europe IV, Europe V even Europe VI.
In December, 2010, the heavy-duty diesel oil motor vehicle emission that national environmental protection portion requires China automobile factory to play sale since on January 1st, 2012 reaches state's IV discharge standard, and SCR becomes the main separation technology path of heavy-duty diesel oil automobile for this reason.Diesel vehicle urea liquid reducing agent cooperates the SCR technology just, is the reducing agent of ammonia G&W with the conversion of nitrogen oxides in the engine exhaust emission.
One Chinese patent application CN101695669A discloses a kind of preparation method of automobile-used urea seeding liquid, wherein uses urea to make raw material, adopts two kinds of technology of charcoal absorption and recrystallization removal of impurities.The method of this patent application can be brought following problem, and the one, recrystallization causes high energy consumption; The 2nd, charcoal adsorption process has increased the consumption of material, thereby has increased the production cost of urea liquid reducing agent; The 3rd, recrystallization back mother liquor is difficult to handle, and Biuret Content is very high in the mother liquor (aqueous solution of urea), can not remake to be the common urea sale, and its direct discharging can cause the environmental pollution of body eutrophication.One Chinese patent application CN101811065A discloses a kind of production technology of tail gas catalytic reducer, wherein uses industrial urea or agricultural urea to make raw material, and uses the ion exchange resin switching technology to remove impurity.The major defect of this patent application is that the urea course of dissolution needs a large amount of heat absorptions, causes energy consumption high; Move the complex technical process of ion exchange resin in addition, cost is higher.The applicant does not find the advanced technology with low cost of relevant automobile-used urea liquid reducing agent production method through retrieval comprehensively both at home and abroad.
The experience of developed countries such as America and Europe shows that diesel vehicle is indispensable running stores of realizing diesel vehicle Europe IV, Europe V even the discharging of Europe VI with urea liquid reducing agent, in the extensive use of countries such as America and Europe.Along with China improves constantly what emission of diesel engine required, will increase fast the demand of urea liquid reducing agent.For this reason, the inventor is through studying for a long period of time, and more existing production technology has obtained a kind of brand-new urea liquid reducing agent production method.
Summary of the invention
The objective of the invention is to: the preparation method of a kind of diesel vehicle with urea liquid reducing agent is provided, this method ability large-scale industrial production; Do not influencing under the fertilizer urea working condition, can produce diesel vehicle simultaneously with urea liquid reducing agent, its constant product quality, with low cost.In addition, need not use active carbon or ion exchange resin to carry out adsorption treatment in the inventive method, also not have harmful mother liquor discharging, be a kind of environment-friendly type production technology.
Biuret Content exceeds standard at present commercially available industrial urea, the agriculture urea; And high purity reagent urea cost is too high, and the market competitiveness is poor.Therefore, just can obtain urea liquid reducing agent product after in prior aries such as patent application CN101695669A and CN101811065A, all need purifying, remove impurity such as biuret to solid urea.
In the prior art, the main flow process of solid urea production is that ammonia and carbon dioxide react under certain condition and generate urea synthesis reaction liquid, and this urea synthesis reaction liquid carries out processes such as flush distillation, double evaporation-cooling, granulation and obtains solid urea then.
It is very low that the present invention is based on the Biuret Content of finding the urea synthesis reaction liquid in the urea synthesizer, thereby directly use this liquid as the automobile-used urea liquid of feedstock production reducing agent.And prior art; After comprising that automobile-used urea liquid among above-mentioned patent application CN101695669A and the CN101811065A is purified through recrystallization by agricultural urea or industrial urea (being solid) product; The means such as active carbon or ion-exchange that re-use make; To make that so energy consumption is high, and the production process contaminated environment.And the present invention has saved evaporation and granulation process during solid urea is produced when having avoided these drawbacks, thereby has remarkable economical and social effect.
The present invention provides the preparation method of first kind of automobile-used urea liquid reducing agent; Comprise: steps A; Get urea synthesis reaction liquid; Remove wherein unconverted thing ammonia and carbon dioxide, make ammonia concentration≤0.4wt%, obtaining urea concentration is high-purity urea liquid of 70～75wt%, Biuret Content≤0.6wt%; Step B is that the ratio of 31.8～33.3wt% is the high purity water allotment of 14～18M Ω cm with high-purity urea liquid described in the steps A and resistivity in final urea concentration, filters then, promptly gets described urea liquid reducing agent.
The present invention also provides the preparation method of second kind of automobile-used urea liquid reducing agent; Comprise: steps A; Get urea synthesis reaction liquid; Remove wherein unconverted thing ammonia and carbon dioxide, make ammonia concentration≤0.4wt%, obtaining urea concentration is high-purity urea liquid of 70～75wt%, Biuret Content≤0.6wt%; But crystallization of said high-purity urea liquid cooling, Separation of Solid and Liquid are made high-purity urea crystal of Biuret Content≤0.5wt%; Step B is that the ratio of 31.8～33.3wt% is dissolved in the high-purity urea crystal described in the steps A in the high purity water that resistivity is 14～18M Ω cm in final urea concentration, filters then, promptly gets described urea liquid reducing agent.
In the preparation method of second kind of automobile-used urea liquid reducing agent of the present invention, prepare high-purity urea crystal in the steps A after, remain urea liquid (mother liquor) accordingly and come back in the urea synthesizer production that continues common agricultural urea.Thereby there is not mother liquor to discharge and environmental pollution problems in this method.
In the preparation method of second kind of automobile-used urea liquid reducing agent of the present invention, the Separation of Solid and Liquid described in the preferred steps A is that centrifugal filtration separates; Said centrifugal filtration separates to adopt and anyly can guarantee that urea crystal smoothly and the centrifugation apparatus of fluid separation applications; Being dissolved as at 25～30 ℃ described in the step B heated 30～40 minutes down.In addition, Biuret Content≤0.45wt% in preferred said high-purity urea crystal.
Among two kinds of urea liquid reducing agent preparation methods according to the invention, above-mentioned first kind of preparation method is adapted at using in the 500 kilometers radiuses in urea production place.And be to practice thrift cost of transportation, second kind of preparation method is fit to the region far away apart from the urea production place and uses, and transport high-purity urea crystal of the present invention and get final product this moment.
Aforesaid two kinds of preparation methods according to the present invention preferably in steps A, make ammonia concentration≤0.1wt% in the urea synthesis reaction liquid.In addition, preferably in steps A, urea concentration is 72～73wt%, Biuret Content≤0.45wt% in said high-purity urea liquid.
Aforesaid two kinds of preparation methods according to the present invention, the preparation method of preferred said high purity water are that 96%～98% ion makes its resistivity reach 10M Ω cm in the removal running water, makes elementary pure water; Remove in the elementary pure water 99% ion then, make its resistivity reach 14～18M Ω cm, obtain required high purity water.More preferably, utilize the two-pass reverse osmosis technology to remove the ion in the running water, utilize the electrodeionization technology to remove the ion in the elementary pure water.
Aforesaid two kinds of preparation methods according to the present invention, preferred said urea synthesis reaction liquid is derived from urea synthesizer; Urea synthesis reaction liquid is the removing before ammonia and the carbon dioxide of embodiment of the present invention method among the present invention, and its ammonia concentration is 0.7～1.0wt%, and urea concentration is 70～72wt%, and biuret concentration is≤0.6wt%.
Aforesaid two kinds of preparation methods according to the present invention, preferably in steps A, through urea synthesis reaction liquid is heated to earlier 70～90 ℃ then the method for vacuum flashing remove unconverted thing ammonia and carbon dioxide in the urea synthesis reaction liquid; Filter type described in the step B is ultrafiltration, and wherein the aperture of milipore filter is 0.5～0.8 μ m.
Urea liquid reducing agent with the present invention produces is handled exhaust gas from diesel vehicle; Method according to HJ451-2008 " environmental protection product specification requirement emission of diesel engine after-treatment device " is tested; The oxynitrides conversion ratio is up to 94%; Satisfy state's IV fully, even state's V exhaust gas from diesel vehicle discharge standard requirement.
The specific embodiment
The detection method of ammonia concentration adopts ISO 22241-2:2006 among the present invention;
The detection method of urea concentration adopts ISO 22241-2:2006 among the present invention;
The detection method of resistivity adopts SL 78-1994 among the present invention;
The detection method of Biuret Content adopts ISO 22241-2:2006 among the present invention;
Embodiment 1
Utilize the two-pass reverse osmosis technology that the raw material running water is handled, remove wherein 96%～98% ion, resistivity reaches 10M Ω cm, makes elementary pure water.Remove in the elementary pure water 99% ion then through EDI technology, resistivity reaches 17.5M Ω cm, obtains required high purity water.With 500 kilograms from the urea synthesis reaction liquid of urea synthesizer through the heating vacuum flashing; With unconverted thing ammonia and carbon dioxide separation; After particularly ammonia being separated to concentration≤0.1wt%; Obtaining temperature is 80～90 ℃, and urea concentration is 73%, 460 kilograms of high-purity urea liquid of Biuret Content≤0.45%.In the high-purity urea liquid of gained, add 573.5 kilograms of above-mentioned high purity waters that prepared, at room temperature constantly stir, and filter with 0.5～0.8 μ m milipore filter device, obtaining 1033.5 kilograms of filtratings is that concentration is 32.5% urea liquid reducing agent product.
Urea liquid reducing agent with this embodiment produces is handled exhaust gas from diesel vehicle, satisfies ISO 22241-2006 " Diesel engines-NOx reduction agent AUS32 " standard-required; Method according to HJ 451-2008 " environmental protection product specification requirement emission of diesel engine after-treatment device " is tested, and the oxynitrides conversion ratio satisfies state's IV fully up to 94%, even state's V exhaust gas from diesel vehicle discharge standard requirement.
Embodiment 2
The preparation of high purity water is identical with embodiment 1.With 500 kilograms from the urea synthesis reaction liquid of urea synthesizer through the heating vacuum flashing; Unconverted thing is separated, particularly ammonia is separated to concentration≤0.1wt% after, obtaining temperature is 80～90 ℃; Urea concentration is 73%, 460 kilograms of high-purity urea liquid of Biuret Content≤0.45%.Then will this high-purity urea liquid be cooled to 20 ℃ of crystallizations, centrifugal filtrations and make 210 kilograms of high-purity urea crystals of Biuret Content≤0.5%, residue urea liquid is pumped into the urea synthesizer storage tank again and makes common agricultural urea.Said high-purity urea crystal is dissolved in 436 kilograms of above-mentioned high purity waters that prepared; Heating while stirring; Heating-up temperature is 30 ℃; Be 40 minutes heat time heating time, filters with 0.5～0.8 μ m milipore filter then, and obtaining 646 kilograms of filtratings is that concentration is 32.5% urea liquid reducing agent product.
Urea liquid reducing agent with this embodiment produces is handled exhaust gas from diesel vehicle, satisfies ISO 22241-2006 " Diesel engines-NOx reduction agent AUS32 " standard-required; Method according to HJ 451-2008 " environmental protection product specification requirement emission of diesel engine after-treatment device " is tested, and the oxynitrides conversion ratio satisfies state's IV fully up to 94%, even state's V exhaust gas from diesel vehicle discharge standard requirement.
Embodiment 3
The preparation of high purity water is identical with embodiment 1.With 500 kilograms from the urea synthesis reaction liquid of urea synthesizer through the heating vacuum flashing; Unconverted thing is separated, particularly ammonia is separated to concentration≤0.4wt% after, obtaining temperature is 80～90 ℃; Urea concentration is 75%, 460 kilograms of high-purity urea liquid of Biuret Content≤0.45%.Then will this high-purity urea liquid be cooled to 30 ℃ of crystallizations, centrifugal filtrations and make 192 kilograms of high-purity urea crystals of Biuret Content≤0.5%, residue urea liquid is pumped into the urea synthesizer storage tank again and makes common agricultural urea.Said high-purity urea crystal is dissolved in 398 kilograms of above-mentioned high purity waters that prepared; Heating while stirring; Heating-up temperature is 30 ℃; Be 40 minutes heat time heating time, filters with 0.5～0.8 μ m milipore filter then, and obtaining 590 kilograms of filtratings is that concentration is 32.5% urea liquid reducing agent product.
Urea liquid reducing agent with this embodiment produces is handled exhaust gas from diesel vehicle, satisfies ISO 22241-2006 " Diesel engines-NOx reduction agent AUS32 " standard-required; Method according to HJ 451-2008 " environmental protection product specification requirement emission of diesel engine after-treatment device " is tested, and the oxynitrides conversion ratio satisfies state's IV fully up to 94%, even state's V exhaust gas from diesel vehicle discharge standard requirement.
Comparative Examples 1
The preparation of high purity water is identical with embodiment 1.500 kilograms of urea synthesis reaction liquid from urea synthesizer are joined into 577 kilograms of above-mentioned high purity waters that prepared; At room temperature constantly stir; And with the filtration of 0.5～0.8 μ m milipore filter device, obtaining 1077 kilograms of urea concentrations is 32.5% urea liquid.
Urea liquid reducing agent with this embodiment produces is handled exhaust gas from diesel vehicle, and ammonia content＞0.2wt% does not satisfy ISO 22241-2006 " Diesel engines-NOx reduction agent AUS32 " standard-required.
Above-mentioned instance only is explanation technical conceive of the present invention and characteristics; Its objective is in order to let the personnel that are familiar with this technology can understand content of the present invention; Can not limit protection scope of the present invention with this; All equivalences that spirit is done according to the present invention change or modify, and all should be encompassed within protection scope of the present invention.
Claims (10)
1. the preparation method of an automobile-used urea liquid reducing agent comprises:
Steps A is got urea synthesis reaction liquid, removes wherein unconverted thing ammonia and carbon dioxide, makes ammonia concentration≤0.4wt%, and obtaining urea concentration is high-purity urea liquid of 70～75wt%, Biuret Content≤0.6wt%;
Step B is that the ratio of 31.8～33.3wt% is the high purity water allotment of 14～18M Ω cm with high-purity urea liquid described in the steps A and resistivity in final urea concentration, filters then, promptly gets described urea liquid reducing agent.
2. the preparation method of an automobile-used urea liquid reducing agent comprises:
Steps A is got urea synthesis reaction liquid, removes wherein unconverted thing ammonia and carbon dioxide, makes ammonia concentration≤0.4wt%, and obtaining urea concentration is high-purity urea liquid of 70～75wt%, Biuret Content≤0.6wt%; But crystallization of said high-purity urea liquid cooling, Separation of Solid and Liquid are made high-purity urea crystal of Biuret Content≤0.5wt%;
Step B is that the ratio of 31.8～33.3wt% is dissolved in the high-purity urea crystal described in the steps A in the high purity water that resistivity is 14～18M Ω cm in final urea concentration, filters then, promptly gets described urea liquid reducing agent.
3. preparation method according to claim 2 is characterized in that: the Separation of Solid and Liquid described in the steps A is that centrifugal filtration separates; Being dissolved as at 25～30 ℃ described in the step B heated 30～40 minutes down.
4. preparation method according to claim 1 and 2 is characterized in that: in steps A, make ammonia concentration≤0.1wt% in the urea synthesis reaction liquid.
5. preparation method according to claim 1 and 2 is characterized in that: in steps A, urea concentration is 72～73wt%, Biuret Content≤0.45wt% in said high-purity urea liquid.
6. preparation method according to claim 1 and 2 is characterized in that: the preparation method of said high purity water is that 96%～98% ion makes its resistivity reach 10M Ω cm in the removal running water, makes elementary pure water; Remove in the elementary pure water 99% ion then, make its resistivity reach 14～18M Ω cm, obtain required high purity water.
7. preparation method according to claim 6 is characterized in that: utilize the two-pass reverse osmosis technology to remove the ion in the running water, utilize the electrodeionization technology to remove the ion in the elementary pure water.
8. preparation method according to claim 1 and 2 is characterized in that: said urea synthesis reaction liquid is derived from urea synthesizer.
9. preparation method according to claim 1 and 2 is characterized in that: in steps A, remove unconverted thing ammonia and carbon dioxide in the urea synthesis reaction liquid through the method that urea synthesis reaction liquid is heated to vacuum flashing after 70～90 ℃.
10. preparation method according to claim 1 and 2 is characterized in that: the filter type described in the step B is ultrafiltration, and wherein the aperture of milipore filter is 0.5～0.8 μ m.
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