CN110575751A - automobile urea reagent and preparation method thereof - Google Patents
automobile urea reagent and preparation method thereof Download PDFInfo
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- CN110575751A CN110575751A CN201810595422.6A CN201810595422A CN110575751A CN 110575751 A CN110575751 A CN 110575751A CN 201810595422 A CN201810595422 A CN 201810595422A CN 110575751 A CN110575751 A CN 110575751A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- 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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/20—Reductants
- B01D2251/206—Ammonium compounds
- B01D2251/2067—Urea
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2258/00—Sources of waste gases
- B01D2258/01—Engine exhaust gases
- B01D2258/012—Diesel engines and lean burn gasoline engines
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Abstract
the invention provides a vehicle urea reagent and a preparation method thereof, wherein the preparation method comprises the following steps: s1, concentrating the urine, pumping the concentrated urine into a first crystallization kettle, cooling and crystallizing to obtain a section of urea coarse crystal, adding the section of urea coarse crystal into a reaction kettle, adding absolute ethyl alcohol and activated carbon, heating and refluxing, filtering while hot, and collecting filtrate; s2, pumping the filtrate into a second crystallization kettle, cooling to room temperature, separating out urea crystals, and cooling and filtering to obtain second-stage urea coarse crystals; s3, adding the two-stage urea coarse crystals into a third crystallization kettle, adding an ethanol-dichloromethane solvent system, heating to reflux, cooling and crystallizing to obtain a wet urea product, and drying the wet urea product to obtain a pure urea product; s4, purifying the industrial water to obtain purified water with the resistivity of 17-20 omega cm; s5, dissolving the pure urea product into purified water to prepare a vehicle urea solution crude product; and S6, filtering the vehicle urea solution crude product through an ultrafiltration membrane to obtain a finished product.
Description
Technical Field
The invention relates to the field of preparation of automobile urea, in particular to an automobile urea reagent and a preparation method thereof.
Background
the diesel vehicle is a main contributor to the emission of nitrogen oxides and PM (particulate matter), the nitrogen oxides emitted by the diesel vehicle account for more than 60% of the total emission of national motor vehicles, and the emission of the PM particulate matter accounts for nearly 100%; the nitrogen oxide and particulate matter emissions of heavy-duty vehicles are significantly higher than those of other vehicles, with nitrogen oxide and particulate matter emissions accounting for 47.1% and 61.4%, respectively.
At present, the SCR technology is mainly adopted for treating diesel vehicle tail gas in China, PM particulate matters are reduced by the SCR technology through the combustion of intensified fuel in an engine, and nitrogen oxides in the waste gas are eliminated by the reaction of vehicle urea solution and nitrogen oxides under the action of an SCR catalyst to generate nitrogen.
the purity of the vehicle urea solution has a great influence on the SCR treatment effect, and impurities in the vehicle urea solution are mainly reflected in that the catalytic effect is easily reduced and pipelines are easily blocked. Therefore, developing an energy-saving and environment-friendly vehicle urea solution is important for reducing PM particulate matters and prolonging the service life of an oil pipeline. However, at present, there are few published patent documents and journal papers on purification of urea solutions for vehicles.
Aiming at the defects of the prior art, an effective implementation mode is not provided so far.
Disclosure of Invention
technical problem to be solved
Aiming at the defects in the prior art, the invention provides the urea reagent for the vehicle and the preparation method thereof.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme:
the preparation method of the urea reagent for the vehicle comprises the following steps:
S1, pumping the urine after primary concentration into a first crystallization kettle, cooling and crystallizing, adding urea seed crystals in the crystallization process, obtaining a section of urea coarse crystals and a section of urine after crystallization is finished, filtering to obtain the section of urea coarse crystals and the section of urine, adding the section of urea coarse crystals into a reaction kettle, adding absolute ethyl alcohol with the mass of 3-5 times of that of the urea crystals, dissolving and dispersing for 15-20min, adding activated carbon, heating and refluxing for 35-40min, filtering while hot, and collecting filtrate;
s2, pumping the filtrate obtained in the step S1 into a second crystallization kettle, naturally cooling to room temperature, slowly stirring in the natural cooling process, continuously separating out urea crystals in the slow stirring process, cooling to room temperature, cooling to-5 to-10 ℃, and performing suction filtration to obtain second-stage urea coarse crystals and second-stage urine;
S3, adding the two-stage urea coarse crystals into a third crystallization kettle, adding an ethanol-dichloromethane solvent system, properly dissolving and dispersing, heating to reflux, carrying out reflux reaction for 45-55min, cooling and crystallizing to obtain a wet urea product and three-stage urine, and drying the wet urea product to obtain a pure urea product;
s4, purifying the industrial water to obtain purified water with the resistivity of 17-20 omega cm;
s5, dissolving the pure urea product obtained in the step S3 into the purified water obtained in the step S4 to prepare a vehicle urea solution crude product with the mass fraction of 35-38%;
S6, filtering the crude automobile urea solution in the step S5 by an ultrafiltration membrane to obtain an automobile urea solution finished product.
preferably, the first-stage urine, the second-stage urine and the third-stage urine are concentrated to be used as raw materials for the urine crystallization in the step S1.
preferably, in the step S1, the urine is primarily concentrated and then pumped into a first crystallization kettle, and then cooled and crystallized, urea seed crystals are added in the crystallization process, after the crystallization is finished, a section of urea coarse crystals and a section of urine are obtained after filtering, the section of urea coarse crystals are added into a reaction kettle, absolute ethyl alcohol with 4 times of the mass of the urea crystals is added to dissolve and disperse for 18min, activated carbon is added, after heating and refluxing for 40min, hot filtering is carried out, and filtrate is collected.
Preferably, in the step S2, the filtrate in the step S1 is pumped into a second crystallization kettle, and is naturally cooled to room temperature, and is slowly stirred in the natural cooling process, urea crystals are continuously separated out in the slow stirring process, and are cooled to-8 ℃ after being cooled to room temperature, and the second-stage urea coarse crystals and the second-stage urine are obtained after suction filtration.
Preferably, in the step S3, the second-stage urea coarse crystal is added into a third crystallization kettle, an ethanol-dichloromethane solvent system is added, after proper dissolution and dispersion, the temperature is raised to reflux, after reflux reaction for 45-55min, cooling and crystallization are performed to obtain a wet urea product and a third-stage urine product, and the wet urea product is dried to obtain a pure urea product.
preferably, in the step S5, the pure urea in the step S3 is dissolved in the purified water in the step S4 to prepare a crude urea solution for a vehicle with a mass fraction of 36.5%.
Advantageous effects
The invention provides a vehicle urea reagent and a preparation method thereof, for vehicle urea, impurities in urine mainly comprise substances such as biuret and metal impurities, the biuret is easy to adsorb an SCR catalyst to cause catalyst poisoning and inactivation, and metal ions are easy to block a nozzle, a spray pipe and a urea solution pipeline. The purity of the urea is improved by multi-end crystallization operation. The multi-stage recrystallization operation process disclosed by the invention effectively solves the problems of complicated process steps and low yield in the existing urea production and purification process. The crystallization method disclosed by the invention effectively improves the purity and yield of urea. And metal ions in the solution are removed through ultrafiltration membrane filtration, so that the damage of the urea solution to an oil pipeline system is increased.
Detailed Description
in order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
The preparation method of the urea reagent for the vehicle comprises the following steps:
S1, pumping the urine after primary concentration into a first crystallization kettle, cooling and crystallizing, adding urea crystal seeds in the crystallization process, obtaining a section of urea coarse crystals and a section of urine after crystallization is finished, filtering to obtain the section of urea coarse crystals and the section of urine, adding the section of urea coarse crystals into a reaction kettle, adding absolute ethyl alcohol with the mass 3-5 times of that of the urea crystals, dissolving and dispersing for 18min, adding activated carbon, heating and refluxing for 40min, filtering while hot, and collecting filtrate;
S2, pumping the filtrate obtained in the step S1 into a second crystallization kettle, naturally cooling to room temperature, slowly stirring in the natural cooling process, continuously separating out urea crystals in the slow stirring process, cooling to room temperature, cooling to-8 ℃, and performing suction filtration to obtain second-stage urea coarse crystals and second-stage urine;
s3, adding the second-stage urea coarse crystals into a third crystallization kettle, adding an ethanol-dichloromethane solvent system, properly dissolving and dispersing, heating to reflux, carrying out reflux reaction for 50min, cooling and crystallizing to obtain wet urea products and third-stage urine products, and drying the wet urea products to obtain pure urea products;
s4, purifying the industrial water to obtain purified water with the resistivity of 20 omega cm;
S5, dissolving the pure urea product obtained in the step S3 into the purified water obtained in the step S4 to prepare a crude urea solution for the vehicle with the mass fraction of 35%;
S6, filtering the crude automobile urea solution in the step S5 by an ultrafiltration membrane to obtain an automobile urea solution finished product.
example 2:
the preparation method of the urea reagent for the vehicle comprises the following steps:
S1, pumping the urine after primary concentration into a first crystallization kettle, cooling and crystallizing, adding urea crystal seeds in the crystallization process, obtaining a section of urea coarse crystals and a section of urine after crystallization is finished, filtering to obtain the section of urea coarse crystals, adding the section of urea coarse crystals into a reaction kettle, adding absolute ethyl alcohol with the mass 4 times of that of the urea crystals, dissolving and dispersing for 15min, adding activated carbon, heating and refluxing for 38min, filtering while hot, and collecting filtrate;
s2, pumping the filtrate obtained in the step S1 into a second crystallization kettle, naturally cooling to room temperature, slowly stirring in the natural cooling process, continuously separating out urea crystals in the slow stirring process, cooling to room temperature, cooling to-5 ℃, and performing suction filtration to obtain second-stage urea coarse crystals and second-stage urine;
s3, adding the second-stage urea coarse crystals into a third crystallization kettle, adding an ethanol-dichloromethane solvent system, properly dissolving and dispersing, heating to reflux, carrying out reflux reaction for 45min, cooling and crystallizing to obtain wet urea products and third-stage urine products, and drying the wet urea products to obtain pure urea products;
s4, purifying the industrial water to obtain purified water with the resistivity of 20 omega cm;
S5, dissolving the pure urea product obtained in the step S3 into the purified water obtained in the step S4 to prepare a vehicle urea solution crude product with the mass fraction of 38%;
s6, filtering the crude automobile urea solution in the step S5 by an ultrafiltration membrane to obtain an automobile urea solution finished product.
Example 3:
the preparation method of the urea reagent for the vehicle comprises the following steps:
s1, pumping the urine after primary concentration into a first crystallization kettle, cooling and crystallizing, adding urea crystal seeds in the crystallization process, filtering to obtain a section of urea coarse crystals and a section of urine after crystallization is finished, adding the section of urea coarse crystals into a reaction kettle, adding absolute ethyl alcohol with the mass 3 times of that of the urea crystals to dissolve and disperse for 15min, adding activated carbon, heating and refluxing for 40min, filtering while hot, and collecting filtrate;
s2, pumping the filtrate obtained in the step S1 into a second crystallization kettle, naturally cooling to room temperature, slowly stirring in the natural cooling process, continuously separating out urea crystals in the slow stirring process, cooling to room temperature, cooling to-7 ℃, and performing suction filtration to obtain second-stage urea coarse crystals and second-stage urine;
s3, adding the second-stage urea coarse crystals into a third crystallization kettle, adding an ethanol-dichloromethane solvent system, properly dissolving and dispersing, heating to reflux, carrying out reflux reaction for 48min, cooling and crystallizing to obtain wet urea products and third-stage urine products, and drying the wet urea products to obtain pure urea products;
s4, purifying the industrial water to obtain purified water with the resistivity of 17 omega cm;
S5, dissolving the pure urea product obtained in the step S3 into the purified water obtained in the step S4 to prepare a crude urea solution for the vehicle with the mass fraction of 35%;
S6, filtering the crude automobile urea solution in the step S5 by an ultrafiltration membrane to obtain an automobile urea solution finished product.
Example 4:
the preparation method of the urea reagent for the vehicle comprises the following steps:
s1, pumping the urine after primary concentration into a first crystallization kettle, cooling and crystallizing, adding urea crystal seeds in the crystallization process, obtaining a section of urea coarse crystals and a section of urine after crystallization is finished, filtering to obtain the section of urea coarse crystals and the section of urine, adding the section of urea coarse crystals into a reaction kettle, adding absolute ethyl alcohol with the mass 5 times that of the urea crystals, dissolving and dispersing for 19min, adding activated carbon, heating and refluxing for 36min, filtering while hot, and collecting filtrate;
s2, pumping the filtrate obtained in the step S1 into a second crystallization kettle, naturally cooling to room temperature, slowly stirring in the natural cooling process, continuously separating out urea crystals in the slow stirring process, cooling to room temperature, cooling to-6 ℃, and performing suction filtration to obtain second-stage urea coarse crystals and second-stage urine;
S3, adding the second-stage urea coarse crystals into a third crystallization kettle, adding an ethanol-dichloromethane solvent system, properly dissolving and dispersing, heating to reflux, carrying out reflux reaction for 50min, cooling and crystallizing to obtain wet urea products and third-stage urine products, and drying the wet urea products to obtain pure urea products;
s4, purifying the industrial water to obtain purified water with the resistivity of 20 omega cm;
S5, dissolving the pure urea product obtained in the step S3 into the purified water obtained in the step S4 to prepare a crude vehicle urea solution with the mass fraction of 36.5%;
s6, filtering the crude automobile urea solution in the step S5 by an ultrafiltration membrane to obtain an automobile urea solution finished product.
example 5:
The preparation method of the urea reagent for the vehicle comprises the following steps:
s1, pumping the urine after primary concentration into a first crystallization kettle, cooling and crystallizing, adding urea crystal seeds in the crystallization process, obtaining a section of urea coarse crystals and a section of urine after crystallization is finished, filtering to obtain the section of urea coarse crystals and the section of urine, adding the section of urea coarse crystals into a reaction kettle, adding absolute ethyl alcohol with the mass 5 times that of the urea crystals, dissolving and dispersing for 18min, adding activated carbon, heating and refluxing for 38min, filtering while hot, and collecting filtrate;
s2, pumping the filtrate obtained in the step S1 into a second crystallization kettle, naturally cooling to room temperature, slowly stirring in the natural cooling process, continuously separating out urea crystals in the slow stirring process, cooling to room temperature, cooling to-7 ℃, and performing suction filtration to obtain second-stage urea coarse crystals and second-stage urine;
S3, adding the second-stage urea coarse crystals into a third crystallization kettle, adding an ethanol-dichloromethane solvent system, properly dissolving and dispersing, heating to reflux, carrying out reflux reaction for 48min, cooling and crystallizing to obtain wet urea products and third-stage urine products, and drying the wet urea products to obtain pure urea products;
S4, purifying the industrial water to obtain purified water with the resistivity of 18 omega cm;
S5, dissolving the pure urea product obtained in the step S3 into the purified water obtained in the step S4 to prepare a vehicle urea solution crude product with the mass fraction of 37%;
S6, filtering the crude automobile urea solution in the step S5 by an ultrafiltration membrane to obtain an automobile urea solution finished product.
And (3) performance testing:
the physical and chemical properties of the vehicle urea prepared in the embodiment 1 of the invention are tested, and the test results are shown in table 1:
TABLE 1
| test items | detection method | The result of the detection |
| Urea/%) | GB29158-2013 | 36.8 |
| refractive index | GB/T614-2006 | 1.3724 |
| Alkali degree/%) | GB/T29518-2013 | <0.06 |
| Biuret/% | GB/T29518-2013 | <0.07 |
| Aluminum ion/mg.kg-1 | GB/T29518-2013 | <0.05 |
| calcium ion/mg.kg-1 | GB/T29518-2013 | <0.04 |
| chromium ion/mg.kg-1 | GB/T29518-2013 | <0.08 |
as can be seen from Table 1: the urea reagent solution for vehicles prepared by the technical scheme disclosed by the invention has the advantages of high purity and low impurity content.
Although the present invention has been described in detail with reference to the foregoing embodiments, it should be understood by those skilled in the art that various changes and modifications may be made, and equivalents may be substituted for elements thereof without departing from the scope of the present invention; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (6)
1. the urea reagent for the vehicle is characterized by comprising a pure urea product and high-purity water for dissolving the pure urea product, and the preparation method of the urea reagent for the vehicle comprises the following steps:
s1, pumping the urine after primary concentration into a first crystallization kettle, cooling and crystallizing, adding urea seed crystals in the crystallization process, obtaining a section of urea coarse crystals and a section of urine after crystallization, adding the section of urea coarse crystals into a reaction kettle, adding absolute ethyl alcohol with the mass of 3-5 times of that of the urea crystals, dissolving and dispersing for 15-20min, adding activated carbon, heating and refluxing for 35-40min, filtering while hot, and collecting filtrate;
S2, pumping the filtrate obtained in the step S1 into a second crystallization kettle, naturally cooling to room temperature, slowly stirring in the natural cooling process, continuously separating out urea crystals in the slow stirring process, cooling to room temperature, cooling to-5 to-10 ℃, and performing suction filtration to obtain second-stage urea coarse crystals and second-stage urine;
S3, adding the two-stage urea coarse crystals into a third crystallization kettle, adding an ethanol-dichloromethane solvent system, properly dissolving and dispersing, heating to reflux, carrying out reflux reaction for 45-55min, cooling and crystallizing to obtain a wet urea product and three-stage urine, and drying the wet urea product to obtain a pure urea product;
s4, purifying the industrial water to obtain purified water with the resistivity of 17-20 omega cm;
S5, dissolving the pure urea product obtained in the step S3 into the purified water obtained in the step S4 to prepare a vehicle urea solution crude product with the mass fraction of 35-38%;
s6, filtering the crude automobile urea solution in the step S5 by an ultrafiltration membrane to obtain an automobile urea solution finished product.
2. The urea reagent for vehicle according to claim 1, wherein the first-stage urine, the second-stage urine and the third-stage urine are concentrated to be used as a raw material for urine crystallization in step S1.
3. the vehicular urea reagent according to claim 1, wherein in step S1, the urine is primarily concentrated and pumped into a first crystallization kettle, then cooled and crystallized, urea seed crystals are added during crystallization, after crystallization is completed, a section of urea coarse crystals and a section of urine are obtained after filtration, the section of urea coarse crystals are added into a reaction kettle, absolute ethyl alcohol with 4 times of the mass of the urea crystals is added for dissolution and dispersion for 18min, activated carbon is added, after heating and refluxing for 40min, hot filtration is performed, and a filtrate is collected.
4. the vehicular urea reagent according to claim 1, wherein in the step S2, the filtrate obtained in the step S1 is pumped into a second crystallization kettle, and is naturally cooled to room temperature, and slowly stirred in the natural cooling process, wherein urea crystals are continuously separated out in the slow stirring process, and are cooled to room temperature, then cooled to-8 ℃, and subjected to suction filtration to obtain second-stage urea coarse crystals and second-stage urine.
5. the vehicular urea reagent according to claim 1, wherein the second-stage urea coarse crystals are added to a third crystallization kettle in step S3, an ethanol-dichloromethane solvent system is added, after proper dissolution and dispersion, the temperature is raised to reflux, after a reflux reaction is performed for 50min, cooling crystallization is performed to obtain wet urea and third-stage urine, and the wet urea is dried to obtain a pure urea product.
6. the vehicle urea reagent according to claim 1, wherein the pure urea in step S3 is dissolved in the purified water in step S4 in step S5 to prepare a crude vehicle urea solution with a mass fraction of 36.5%.
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| CN201810595422.6A CN110575751A (en) | 2018-06-11 | 2018-06-11 | automobile urea reagent and preparation method thereof |
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| CN201810595422.6A CN110575751A (en) | 2018-06-11 | 2018-06-11 | automobile urea reagent and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112094207A (en) * | 2020-09-30 | 2020-12-18 | 河南弘康环保科技有限公司 | Preparation method of low-formaldehyde automobile urea solution |
| CN115400493A (en) * | 2022-09-13 | 2022-11-29 | 江苏可兰素环保科技有限公司 | Purification process of urea solution for vehicle |
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| CN104289106A (en) * | 2014-09-23 | 2015-01-21 | 河南弘康环保科技有限公司 | Method for preparing vehicle urea solution |
| CN106621867A (en) * | 2015-10-30 | 2017-05-10 | 青岛鹏通瑞德电气科技有限公司 | A preparing method of a urea solution used for vehicles |
| CN107051204A (en) * | 2017-05-09 | 2017-08-18 | 东莞蔚蓝环保科技有限公司 | A kind of preparation technology of urea for vehicle solution |
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2018
- 2018-06-11 CN CN201810595422.6A patent/CN110575751A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO1994013630A1 (en) * | 1992-12-09 | 1994-06-23 | Sankt-Peterburgsky Gosudarstvenny Universitet | Process for obtaining carbamide |
| CN104289106A (en) * | 2014-09-23 | 2015-01-21 | 河南弘康环保科技有限公司 | Method for preparing vehicle urea solution |
| CN106621867A (en) * | 2015-10-30 | 2017-05-10 | 青岛鹏通瑞德电气科技有限公司 | A preparing method of a urea solution used for vehicles |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112094207A (en) * | 2020-09-30 | 2020-12-18 | 河南弘康环保科技有限公司 | Preparation method of low-formaldehyde automobile urea solution |
| CN115400493A (en) * | 2022-09-13 | 2022-11-29 | 江苏可兰素环保科技有限公司 | Purification process of urea solution for vehicle |
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