CN104533577A - Nitric oxide reducing agent with ultra-low freezing point and manufacturing method thereof - Google Patents
Nitric oxide reducing agent with ultra-low freezing point and manufacturing method thereof Download PDFInfo
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- CN104533577A CN104533577A CN201510017530.1A CN201510017530A CN104533577A CN 104533577 A CN104533577 A CN 104533577A CN 201510017530 A CN201510017530 A CN 201510017530A CN 104533577 A CN104533577 A CN 104533577A
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Abstract
The invention provides a nitric oxide reducing agent with an ultra-low freezing point and a manufacturing method thereof. The nitric oxide reducing agent comprises, by mass, 7-23% of urea, 5-10% of dimethyl sulfoxide, 42-55% of pure water, and one or more of 20-30% of amines, amides and alcohols. The manufacturing method includes the following methods: preparing the raw materials, and fully mixing the raw materials at the temperature of 10-30 DEG C until the raw materials are completely dissolved into aqueous solution, wherein the raw materials are evenly mixed; using a filter element with the filter precision of 0.5-5 micrometers, and under the pressure of 0.2-1Mpa, filtering the aqueous solution of the raw materials and obtaining the finished product. The nitric oxide reducing agent has the advantages that raw materials of an anti-freezing agent are safe, good in anti-freezing effect, easy to obtain, non-toxic and harmless, the freezing point of the reducing agent is greatly lowered, the problems of lower temperature crystallization and freezing are solved, the anti-freezing properties of the nitric oxide reducing agent are remarkably improved, and the freezing point can reach below minus 35 DEG C. Tests have shown that after engine exhaust gas is added to an SCR post-processing system adopting the nitric oxide reducing agent, exhaust gas emission can reach the national IV standard.
Description
Technical field
The present invention relates to diesel motor exhaust reprocessing field, specifically a kind of ultralow freezing point NOx reducing agent and preparation method thereof.
Background technique
In recent years, along with the frequent appearance of China's various places haze weather, increasingly sharpening of Chinese government's environmental protection pressure.The improvement making the motor vehicle discharged tail gas of main contributions for haze weather pollution sources is also accelerated, and after Beijing takes the lead in implementing state IV emission standard in March, 2008, Motor Vehicle state IV standards is implemented in the cities such as Shanghai, Shenzhen and Guangzhou, Xi'an in succession.The city of carrying out state four emission standard for nearly 2 years increases day by day, estimates that country in 2015 will enforce Motor Vehicle state IV emission standard comprehensively.
According to the production technology of diesel engines at present, diesel-oil vehicle wants to reach state IV emission standard, except improving the emission controls by improving combustion measure such as fuel injection system, Optimizing Combustion process, also must increase the outer after-treatment device of machine.On our times, the exhaust aftertreatment technology path of main flow is SCR route.Adopt the diesel engine of SCR technology first to optimize in-cylinder combustion, reduce the discharge of particulate matter, then pass through SCR technology to high NO
xthe tail gas of content carries out reprocessing.Due to adopt state IV Fuel Economy of SCR technology better, little to engine modification than EGR technology, to fuel oil and machine oil require lower, there is advantage, SCR catalyst good endurance and there is not the risk of catalyst converter blocking in technology upgrading continuity, therefore SCR technology is the large diesel engine energy-conserving and emission-cutting technology route of applicable China's national situation.And for SCR system, NOx reducing agent-urea for vehicle solution is then that its performance effect must be prepared, urea for vehicle solution deposits in special holding vessel, with pressurized air, urea liquid is sprayed the motor exhaust (about 300 DEG C ~ 500 DEG C of thermotropism, meet reduction reaction conditions), produce the ammonia that reduction efficiency is high after this vaporizer, under the effect of the NOx catalyzer in SCR catalyst in ammonia and tail gas, redox reaction occurs, be converted into harmless water vapor and N
2.
China has started to promote the diesel-oil vehicle meeting state four discharge adopting SCR technology, and supply, the sale of the urea for vehicle solution of the car needs of the type also begin to take shape.Traditional urea for vehicle solution is the aqueous solution containing urea 32.5%, and the freezing point of this product is ﹣ 11.5 DEG C, will crystallization lower than this temperature product, actual use in can go up completely when ﹣ 20 DEG C.Because China is vast in territory, in especially winter, various places temperature difference is larger.Freezing point be ﹣ 11.5 DEG C urea for vehicle solution the north or other extremely frigid zones, do not have corresponding measure to use.
At present, the method solving urea for vehicle crystallization condensation mainly takes Insulation to SCR system on the one hand, is then by adding antifreezing solution in urea for vehicle on the one hand, reduces freezing point, prevents solution crystallization coagulation to play.
Retrieval finds, the achievement in research improving reductant solution freezing point comprises the patent JP20090031713 " ANTIFREEZING UREA SOLUTION FOR UREA SCR SYSTEM AND UREA SCR SYSTEM USING THE SAME " of Japan, European product Denoxium-30 and China patent CN201110134706.3 " a kind of low-temperature urea reducing agent composition ", CN201110134698.2 " a kind of ultralow-temperature urea reducing agent composition ".What Japan Patent JP20090031713 adopted is that the alcohols of C1 ~ C7 is as freezing point improver, its adding quantity ratio of the adding quantity of the alcohols of (alcohols+urea of water+C1 ~ C7)/C1 ~ C7 limits, ratio is 7/1, calculate in theory, suppose that the density of ethanol is 0.789kg/L at 20 DEG C of temperature, calculate that the adding quantity of alcohols is less than 10%wt; If adopt methyl alcohol or ethanol to implement, actual detection shows the ﹣ 30 DEG C that its freezing point can not reach described, and supposition should be with the addition of isopropanol or ethylene glycol, or inventor has a mind to imply certain composition or addition; Inventor about this point JP20090031713 patent does not describe.The low-temperature urea reducing agent product Denoxium-30 in Europe adopts the aqueous solution of 20% urea and 26% ammonium formate as reducing agent, product freezing point is between ﹣ 26 DEG C ~ ﹣ 30 DEG C, use in the extremely cold north and still have certain narrow limitation, in addition, the relative this patent high cost of this product.
China patent CN 201110134706.3 and CN 201110134698.2 is all by adding the materials such as ammonium class, amide-type, alcohols to reach the object reducing freezing point in urea for vehicle.The relative this patent complicated component of this patent, increases production difficulty.In addition, alcohol reagent has volatility mostly, and the poorly sealed or long-time uncovered placement of product not only can affect quality of product, also can produce certain pollution to ambient air.
Summary of the invention
The object of the invention is to: provide a kind of for NOx reducing agent and preparation method thereof in diesel motor exhaust under low temperature.
The technical solution adopted in the present invention is:
A kind of ultralow freezing point NOx reducing agent, its component and mass percent are: the urea of 17% ~ 23%, the dimethyl sulfoxide (DMSO) of 5% ~ 10%, one or more compositions in the pure water of 42% ~ 55% and the ammonium class of 20% ~ 30%, amide-type and alcohols.
Described urea need meet the technical requirements of the special urea of AUS 32 in GB 29518-2013 " diesel engine NOx reducing agent aqueous solution of urea (AUS 32) " standard.
Described pure water need meet the technical requirements to pure water in GB 29518-2013 " diesel engine NOx reducing agent aqueous solution of urea (AUS 32) " standard.
Described dimethyl sulfoxide (DMSO), ammonium class, amide-type and low molecule alcohols are the product analyzing pure above grade.
The preparation method of described ultralow freezing point NOx reducing agent, comprises following concrete steps:
(1) raw material is assorted by described component and mass percent, fully stir at the temperature of 10 ~ 30 DEG C, until all raw materials are dissolved as the aqueous solution completely, mix;
(2) filter precision is used to be the filter core of 0.5 ~ 5 μm, under the pressure of 0.2 ~ 1MPa, after being filtered by the aqueous solution of raw material that step (1) obtains, to obtain ultralow freezing point NOx reducing agent solution.
The beneficial effect that the present invention produces is:
The present invention improves component and the preparation method of existing NOx reducing agent, compared with the prior art, and the features such as this NOx reducing agent has antifreezing solution materials safety and is easy to get, good freezing protection effect, nontoxic; The present invention reduces reducing agent freezing point greatly, and solve low temperature crystallization and ice formation issues, can significantly improve NOx reducing agent resistance to frost, freezing point can reach ﹣ less than 35 DEG C; Product of the present invention carries out ETC, ESC working condition measurement on diesel engine machine frame, and motor exhaust is after the SCR aftertreatment system process of this product of annotating, and exhaust emissions can reach state four standard.
Embodiment
The invention discloses a kind of production method for NOx reducing agent in diesel motor exhaust under ultralow temperature, this ultralow freezing point NOx reducing agent composition, by one or more in acyl ammonium class, ammonium class, low molecule alcohols, urea, dimethyl sulfoxide (DMSO) and pure water composition.Wherein urea accounts for 17% ~ 23% of mixture gross mass, and dimethyl sulfoxide (DMSO) accounts for 5% ~ 10% of mixture gross mass, and ammonium class, amide-type and alcohols account for 20% ~ 30% of mixture gross mass, and water accounts for 42% ~ 55% of mixture gross mass.
In invention composition component:
The purity requirement of urea is higher, need meet the technical requirements of the special urea of AUS 32 in GB 29518-2013 " diesel engine NOx reducing agent aqueous solution of urea (AUS 32) " standard.
Dimethyl sulfoxide (DMSO) is the product analyzing pure above grade, and molecular formula is (CH
3)
2sO, decomposes, spontaneous combustion more than 300 DEG C under the high temperature of 140 ~ 150 DEG C, generates CO
2, H
2o and SO
2.
Ammonium class, amide-type and low molecule alcohols are the product analyzing pure above grade.If Some substitute urea decomposition is discharged ammonia by adding portion ammonium class, amide-type product, corresponding minimizing amount of urea.Ammonium class, amide-type final product are nitrogen, carbon dioxide.Ammonium class, amide-type and alcohols can be used alone one, also can multiple combination, select according to cost, character, effect; Generally can low molecular weight and the low carbon content material such as formic acid ammonium, formamide, methyl alcohol, ethylene glycol, diethylene glycol, ethanol, isopropanol, glycerine.
The purity requirement of component pure water is also higher, need reach or be better than the technical requirements to pure water in GB 29518-2013 " diesel engine NOx reducing agent aqueous solution of urea (AUS 32) " standard.
After each component is mixed in proportion, even if ultralow freezing point NOx reducing agent product of the present invention.The existence of dimethyl sulfoxide (DMSO), ammonium class, amide-type and alcohols additive does not affect the safety in utilization of nitrogen oxide aqueous solution of urea.
The preparation method of the ultralow freezing point NOx reducing agent of the present invention, comprises following concrete steps:
(1) raw material is assorted by described component and mass percent, fully stir at the temperature of 10 ~ 30 DEG C, until all raw materials are dissolved as the aqueous solution completely, and mix.Concrete: because acyl ammonium class, ammonium class, low molecule alcohols and dimethyl sulfoxide (DMSO) are liquid, soluble in water; Therefore, in actual fabrication process, after urea solid all dissolves, can stop stirring.
(2) filter precision is used to be the filter core of 0.5 ~ 5 μm, under the pressure of 0.2 ~ 1MPa, after being filtered by the aqueous solution of raw material that step (1) obtains, to obtain ultralow freezing point NOx reducing agent solution.
embodiment 1
With satisfactory urea component 170kg, analyze pure above rank dimethyl sulfoxide (DMSO) 100kg, ammonium class, acid amides and low molecule alcohols 250kg(be wherein: ammonium formate 100kg, formamide 150kg), pure water 480kg, each component is mixed, be stirred to urea to dissolve completely, the filter core with filter precision being 0.5 μm, after 0.2Mpa filtered under pressure, is composition solution of the present invention.
After measured, mixture solution freezing point ﹣ 35 DEG C, slightly ammonia taste, clear appearance is transparent.The indexs such as metal ion, biuret, aldehydes, phosphate, undissolved substance, basicity all meet the demands.Separate out without crystal under ﹣ more than 35 DEG C temperature environments, after room temperature lower seal stores 6 months, outward appearance, smell change without sensory perceptible, and reducing property meets the requirements.
Product is that 336 horsepowers of (discharge capacity 9.726L) diesel engine machine frames carry out ETC, ESC working condition measurement through power, and motor exhaust is after the SCR aftertreatment system process of this product of annotating, and exhaust emissions can reach state four standard.
embodiment 2
With satisfactory urea component 230kg, analyze pure above rank dimethyl sulfoxide (DMSO) 100kg, ammonium class, acid amides and low molecule alcohols 250kg(be wherein: methyl alcohol 100kg, formamide 150kg), pure water 420kg, each component being mixed, be stirred to urea and dissolve completely, is the filter core of 0.5 μm with filter precision, after 0.6Mpa filtered under pressure, be composition solution of the present invention.
After measured, mixture solution freezing point ﹣ 36 DEG C, slightly ammonia taste, clear appearance is transparent.The indexs such as metal ion, biuret, aldehydes, phosphate, undissolved substance, basicity all meet the demands.Separate out without crystal under ﹣ more than 35 DEG C temperature environments, after room temperature lower seal stores 6 months, outward appearance, smell change without sensory perceptible, and reducing property meets the requirements.
Product is that 336 horsepowers of (discharge capacity 9.726L) diesel engine machine frames carry out ETC, ESC working condition measurement through power, and motor exhaust is after the SCR aftertreatment system process of this product of annotating, and exhaust emissions can reach state four standard.
embodiment 3
With satisfactory urea component 190kg, analyze pure above rank dimethyl sulfoxide (DMSO) 80kg, ammonium class, acid amides and low molecule alcohols 300kg(be wherein: methyl alcohol 100kg, formamide 200kg), pure water 430kg, each component being mixed, be stirred to urea and dissolve completely, is the filter core of 1 μm with filter precision, after 1Mpa filtered under pressure, be composition solution of the present invention.
After measured, mixture solution freezing point ﹣ 38.7 DEG C, slightly ammonia taste, clear appearance is transparent.The indexs such as metal ion, biuret, aldehydes, phosphate, undissolved substance, basicity all meet the demands.Separate out without crystal under ﹣ more than 35 DEG C temperature environments, after room temperature lower seal stores 6 months, outward appearance, smell change without sensory perceptible, and reducing property meets the requirements.
Product is that 336 horsepowers of (discharge capacity 9.726L) diesel engine machine frames carry out ETC, ESC working condition measurement through power, and motor exhaust is after the SCR aftertreatment system process of this product of annotating, and exhaust emissions can reach state four standard.
embodiment 4
With satisfactory urea component 230kg, analyze pure above rank dimethyl sulfoxide (DMSO) 100kg, ammonium class, acid amides and low molecule alcohols 250kg(be wherein: ethylene glycol 100kg, formamide 150kg), pure water 420kg, each component being mixed, be stirred to urea and dissolve completely, is the filter core of 5 μm with filter precision, after 0.5Mpa filtered under pressure, be composition solution of the present invention.
After measured, mixture solution freezing point ﹣ 36 DEG C, slightly ammonia taste, clear appearance is transparent.The indexs such as metal ion, biuret, aldehydes, phosphate, undissolved substance, basicity all meet the demands.Separate out without crystal under ﹣ more than 35 DEG C temperature environments, after room temperature lower seal stores 6 months, outward appearance, smell change without sensory perceptible, and reducing property meets the requirements.
Product is that 336 horsepowers of (discharge capacity 9.726L) diesel engine machine frames carry out ETC, ESC working condition measurement through power, and motor exhaust is after the SCR aftertreatment system process of this product of annotating, and exhaust emissions can reach state four standard.
Claims (5)
1. a ultralow freezing point NOx reducing agent, it is characterized in that, its component and mass percent are: the urea of 17% ~ 23%, the dimethyl sulfoxide (DMSO) of 5% ~ 10%, one or more compositions in the pure water of 42% ~ 55% and the ammonium class of 20% ~ 30%, amide-type and alcohols.
2. ultralow freezing point NOx reducing agent according to claim 1, it is characterized in that, described urea need meet the technical requirements of the special urea of AUS 32 in GB 29518-2013 " diesel engine NOx reducing agent aqueous solution of urea (AUS 32) " standard.
3. ultralow freezing point NOx reducing agent according to claim 1, it is characterized in that, described pure water need meet the technical requirements to pure water in GB 29518-2013 " diesel engine NOx reducing agent aqueous solution of urea (AUS 32) " standard.
4. ultralow freezing point NOx reducing agent according to claim 1, it is characterized in that, described dimethyl sulfoxide (DMSO), ammonium class, amide-type and low molecule alcohols are the product analyzing pure above grade.
5. the preparation method of ultralow freezing point NOx reducing agent according to claim 1, is characterized in that, comprise following concrete steps:
(1) raw material is assorted by described component and mass percent, fully stir at the temperature of 10 ~ 30 DEG C, until all raw materials are dissolved as the aqueous solution completely, and mix;
(2) filter precision is used to be the filter core of 0.5 ~ 5 μm, under the pressure of 0.2 ~ 1MPa, after being filtered by the aqueous solution of raw material that step (1) obtains, to obtain ultralow freezing point NOx reducing agent solution.
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Cited By (8)
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| CN105498537A (en) * | 2015-11-30 | 2016-04-20 | 许昌学院 | Low-temperature diesel exhaust reducing agent and preparation method thereof |
| CN105536865A (en) * | 2015-11-30 | 2016-05-04 | 许昌学院 | Diesel oil tail gas reducing agent for improving low temperature performances, and preparation method thereof |
| CN105964143A (en) * | 2016-05-10 | 2016-09-28 | 南宁市夏阳化工科技有限责任公司 | Diesel engine tail gas treatment agent |
| CN107138044A (en) * | 2017-06-02 | 2017-09-08 | 许昌学院 | A kind of diesel vehicle urea liquid with cryogenic property and preparation method thereof |
| CN109908755A (en) * | 2019-04-11 | 2019-06-21 | 兰州梓苑环保科技有限公司 | A kind of vent gas treatment liquid and preparation method thereof suitable for -25 DEG C of environment |
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| CN111389208A (en) * | 2020-03-25 | 2020-07-10 | 山东骏逸环境科技有限公司 | Amino denitration agent and preparation method thereof |
| CN113731151A (en) * | 2021-09-13 | 2021-12-03 | 广东新翔星科技股份有限公司 | Composite denitration desulfurizer and preparation method and application thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105498537A (en) * | 2015-11-30 | 2016-04-20 | 许昌学院 | Low-temperature diesel exhaust reducing agent and preparation method thereof |
| CN105536865A (en) * | 2015-11-30 | 2016-05-04 | 许昌学院 | Diesel oil tail gas reducing agent for improving low temperature performances, and preparation method thereof |
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| CN109908755A (en) * | 2019-04-11 | 2019-06-21 | 兰州梓苑环保科技有限公司 | A kind of vent gas treatment liquid and preparation method thereof suitable for -25 DEG C of environment |
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| CN111389208A (en) * | 2020-03-25 | 2020-07-10 | 山东骏逸环境科技有限公司 | Amino denitration agent and preparation method thereof |
| CN113731151A (en) * | 2021-09-13 | 2021-12-03 | 广东新翔星科技股份有限公司 | Composite denitration desulfurizer and preparation method and application thereof |
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Application publication date: 20150422 |