CN102580531B - Low temperature-resistant tail gas catalytic reduction agent and preparation method thereof - Google Patents
Low temperature-resistant tail gas catalytic reduction agent and preparation method thereof Download PDFInfo
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- CN102580531B CN102580531B CN201210008070.2A CN201210008070A CN102580531B CN 102580531 B CN102580531 B CN 102580531B CN 201210008070 A CN201210008070 A CN 201210008070A CN 102580531 B CN102580531 B CN 102580531B
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- gas catalytic
- catalytic reducer
- tail gas
- low temperature
- exhaust gas
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- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 238000010531 catalytic reduction reaction Methods 0.000 title abstract 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 45
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 15
- 235000012501 ammonium carbonate Nutrition 0.000 claims abstract description 15
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 15
- 229910021642 ultra pure water Inorganic materials 0.000 claims abstract description 13
- 239000012498 ultrapure water Substances 0.000 claims abstract description 13
- 239000003638 chemical reducing agent Substances 0.000 claims description 63
- 230000003197 catalytic effect Effects 0.000 claims description 60
- 238000001914 filtration Methods 0.000 claims description 13
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 claims description 6
- 229910001424 calcium ion Inorganic materials 0.000 claims description 6
- 238000000746 purification Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 3
- 229910001415 sodium ion Inorganic materials 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract 6
- 239000004721 Polyphenylene oxide Substances 0.000 abstract 1
- 150000001412 amines Chemical class 0.000 abstract 1
- 229920000570 polyether Polymers 0.000 abstract 1
- 238000006722 reduction reaction Methods 0.000 abstract 1
- 230000008014 freezing Effects 0.000 description 13
- 238000007710 freezing Methods 0.000 description 13
- 239000000463 material Substances 0.000 description 9
- 238000006243 chemical reaction Methods 0.000 description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 7
- 239000004202 carbamide Substances 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 150000001298 alcohols Chemical class 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 4
- 150000003863 ammonium salts Chemical class 0.000 description 3
- 230000009931 harmful effect Effects 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 238000000108 ultra-filtration Methods 0.000 description 3
- 238000010792 warming Methods 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 238000000889 atomisation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229920002114 octoxynol-9 Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
Landscapes
- Exhaust Gas After Treatment (AREA)
- Exhaust Gas Treatment By Means Of Catalyst (AREA)
Abstract
The invention relates to a tail gas catalytic reduction agent and a preparation method thereof, and belongs to the technical field of chemical industry. Aiming at the characteristic that due to low-temperature performance, the conventional vehicular tail gas catalytic reduction agent only can be used at the temperature of -11 DEG C, a vehicular low temperature-resistant tail gas catalytic reduction agent which can be used at the low temperature of between -25 and -40 DEG C normally and accords with a selective catalytic reduction (SCR) system is compounded on the basis of the fundamental mechanism of a reduction agent. The tail gas catalytic reduction agent comprises the following components in percentage by weight: 30 to 60 percent of Adblue, 10 to 40 percent of ammonium carbonate, 10 to 40 percent of methanol, 0.02 to 0.2 percent of low-molecular weight polyether amine and 10 to 35 percent of ultrapure water. A blending process comprises the following steps of: dissolving, purifying and filling. The tail gas catalytic reduction agent is suitable to be used at the temperature of -11 DEG C and meets the requirement of the normal operation of the SCR system completely.
Description
Technical field
The present invention relates to a kind of tail gas catalytic reducer and preparation method thereof, belong to chemical technology field.
Background technology
At present, the freezing point of the tail gas catalytic reducer of applicable SCR technology-vehicle tail gas catalytic reducer (AUS32) is-11 ℃, so in the temperature in Northern Part of China winter generally all lower than-11 ℃, like this to using traditional AUS32 to cause freezing harmful effect as the vehicle tail gas catalytic reducer, vehicle must first heat by heating system, both increased the cost of SCR system, again owing to using heating system just can bring into use the SCR system, OBD to the SCR system has certain adverse effect, cause the rules of state's four discharges phenomenon in violation of rules and regulations to occur in fulfillment process.Abroad for the anti-low temperature of tail gas catalytic reducer, also study for a long time, the applicant recognizes that the formula of anti-low temperature exhaust gas catalytic reducer mainly passes through the composite of some ammonium class materials, prepare qualified anti-low temperature exhaust gas catalytic reducer by certain Blending, but the severe corrosive due to ammonium class material, corrosion of metal to exhaust system also receives publicity always, fails to promote the use of on a large scale.The emphasis that the low-carbon (LC) alcohols material is also research is added in employing in qualified Adblue, because low-carbon alcohols is all to reduce the ability of freezing point, so add the freezing point that appropriate low-carbon alcohols can reduce tail gas catalytic reducer, but the characteristic due to low-carbon alcohols, the transformation efficiency of its NOx will reduce, so also fail to promote on a large scale.At home because the SCR system just started to be paid close attention to by the people in recent years, tail gas catalytic reducer market for the SCR system is little, anti-low temperature exhaust gas catalytic reducer is not research especially, but, under the low temperature in winter of north of China zone, vehicle is badly in need of cryophylactic tail gas catalytic reducer and is reduced freezing harmful effect.
Summary of the invention
The present invention wants the technical solution problem to be: for domestic existing common tail gas, absorb reducing agent lower than-11 ℃ of icing defects, propose a kind of anti-low temperature exhaust gas catalytic reducer and preparation method thereof, tail gas catalytic reducer can be used under-25 ℃～-40 ℃ low temperature.
The present invention is the technical solution problem by the following technical programs: a kind of anti-low temperature exhaust gas catalytic reducer, by weight percentage, composed of the following components:
The Adblue 30%～60% that meets the ISO22241-1 standard
Ammonium carbonate 10%～40%
Methyl alcohol 10%～40%
Polyetheramine 0.02%～0.2%
Ultra-pure water 10%～35%.
Wherein, Adblue is translated into the diesel engine vent gas treatment fluid, domestic being commonly called as automobile urea, and automobile-used urea, automobile environment-protection urea, be the running stores that must use in the SCR technology.Its constituent is approximately high-purity urea of 32.5% and approximately 67.5% deionized water, meets the ISO22241-1 standard.
Described ammonium carbonate is pure for analyzing, its calcium ion≤0.5ppm.
Described methyl alcohol is pure for analyzing, its sodium ion, calcium ion all≤0.5ppm.
The molecular weight of described polyetheramine is M=1000-1500.
Described ultrapure resistivity of water is at 13～14M Ω * cm.
The said goods is obtained by following technical scheme: a kind of preparation method of tail gas catalytic reducer comprises the following steps:
Step 1, dissolving, add described Adblue, ammonium carbonate, methyl alcohol in dissolving tank, mixes, stirs, and makes the tail gas catalytic reducer first product,
Step 2, purification, purify described tail gas catalytic reducer first product by filtration, obtain the tail gas catalytic reducer filtered, then separate by film, obtains the tail gas catalytic reducer separated;
Step 3, make, described polyetheramine is added in the tail gas catalytic reducer of separation, and to adjust mass percentage concentration with ultra-pure water be 30%～50%, obtain cryophylactic tail gas catalytic reducer.
Wherein, in described step 1, solution temperature is 30 ℃～35 ℃.
In described step 2, bag filter, mechanical filter, the filtering accuracy that filters equipment for purifying and be filtering accuracy and be 10 microns is at least one in the precision Filter element filter of 0.45 micron, and filtration flow-rate is controlled at 2m
3/ H～3m
3/ H.
The present invention is directed to the shortcoming of prior art, in component proportion, adopted alcohols and ammonium class material to mix, reduce the freezing point of product, in the time of cost-saving, product quality meets standard, the NOx conversion ratio of the reducing agent system be composited also significantly increases than alcohols, by adding polyetheramine, rust-preventing characteristic, dissolubility stability, the atomization ability of product are strengthened.During preparation, adopt the continuous purifying technique of slot type and film process for separating and purifying, making whole production process is to carry out in airtight pipeline, avoided the possibility of polluting, multi-filtering is removed mechanical admixture, and metal ion is carried out to the film separation, makes anti-low temperature exhaust gas absorb reducing agent and is purified.Adopt online control, make whole production process that control point be arranged, guaranteed stability and the controllability of product.Its beneficial effect is: finished product can be used under-25 ℃～-40 ℃ low temperature, for the large-scale popularization of domestic northern area SCR system lays the foundation.
The specific embodiment
Raw material of the present invention all can be buied from market, and wherein Adblue meets the ISO22241-1 standard; Ammonium carbonate is pure for analyzing, the content≤0.5ppm of calcium ion wherein, methyl alcohol is pure for analyzing, wherein the content of sodium ion, calcium ion all≤0.5ppm; Below repeat no more.
Embodiment mono-
The component proportion of this example following (in % by weight):
| Component | Form % |
| Adblue | 55 |
| Ammonium carbonate | 14 |
| Methyl alcohol | 20 |
| Polyetheramine (molecular weight 1010) | 0.1 |
| Ultra-pure water | 10.9 |
Prepared in the steps below by the component of said ratio:
Step 1, dissolving, by automobile-used urea, ammonium carbonate, methyl alcohol, join mixing in dissolving tank, be warming up to 30 ℃, stirs 20min, makes the tail gas catalytic reducer first product;
Step 2, purification, filtered the tail gas catalytic reducer first product, and filter plant is comprised of 10 μ bag filters, activated carbon filtration tower and 0.45 μ precision Filter element filter (PP material), take flow velocity as 2.5m
3obtain the tail gas catalytic reducer filtered by filter plant, then by molecular weight at 100,000 ultrafiltration folded membrane, obtain the tail gas catalytic reducer separated;
Step 3, make, polyetheramine is added to the tail gas catalytic reducer of separation, pulse 10min, reconcile into ultra-pure water the anti-low temperature exhaust gas catalytic reducer that mass percentage concentration is 32%.
Embodiment bis-
The component proportion of this example following (in % by weight):
| Material | Form % |
| Adblue | 45 |
| Ammonium carbonate | 30 |
| Methyl alcohol | 10 |
| Polyetheramine (molecular weight 1200) | 0.15 |
| Ultra-pure water | 14.85 |
Prepared in the steps below by the component of said ratio:
Step 1, dissolving, by automobile-used urea, ammonium carbonate, methyl alcohol and ultra-pure water, join mixing in dissolving tank, be warming up to 32 ℃, stirs 20min, makes the tail gas catalytic reducer first product;
Step 2, purification, filtered the tail gas catalytic reducer first product, and wherein filter plant is comprised of 10 μ bag filters, activated carbon filtration tower and 0.45 μ precision Filter element filter (PP material), take flow velocity as 3.5m
3obtain the tail gas catalytic reducer filtered by filter plant, then by molecular weight the ultrafiltration folded membrane at 7-8 ten thousand, obtain the tail gas catalytic reducer separated;
Step 3, make, polyetheramine is added to the tail gas catalytic reducer after filtration, pulse 10min, reconcile into ultra-pure water the anti-low temperature exhaust gas catalytic reducer that mass percentage concentration is 44.6%.
Embodiment tri-
The component proportion of this example following (in % by weight):
| Material | Form % |
| Adblue | 35 |
| Ammonium carbonate | 35 |
| Methyl alcohol | 15 |
| Polyetheramine (molecular weight 1000) | 0.2 |
| Ultra-pure water | 14.8 |
Prepared in the steps below by the component of said ratio:
Step 1, dissolving, by automobile-used urea, ammonium carbonate, methyl alcohol and ultra-pure water, join mixing in dissolving tank, be warming up to 35 ℃, stirs 20min, makes the tail gas catalytic reducer first product;
Step 2, purification, filtered the tail gas catalytic reducer first product, and wherein filter plant is comprised of 10 μ bag filters, activated carbon filtration tower and 0.45 μ precision Filter element filter (PP material), take flow velocity as 2.5m
3obtain the tail gas catalytic reducer filtered by filter plant, then by molecular weight at 200,000 ultrafiltration folded membrane, obtain the tail gas catalytic reducer separated;
Step 3, make, polyetheramine is added to the tail gas catalytic reducer of separation, pulse 10min, reconcile into ultra-pure water the anti-low temperature exhaust gas catalytic reducer that mass percentage concentration is 46.4%.
The contrast experiment
The freezing point of the anti-low temperature exhaust gas catalytic reducer obtained according to conventional method detection above-described embodiment, refer to table 1:
| Embodiment | Freezing point |
| Embodiment mono- | -30℃ |
| Embodiment bis- | -35℃ |
| Embodiment tri- | -40℃ |
| Adblue | -11℃ |
Table 1
As shown in Table 1, the freezing point of anti-low temperature exhaust gas catalytic reducer of the present invention is far below Adblue,, the anti-low temperature exhaust gas catalytic reducer that above-described embodiment is made can be used under-25 ℃～-40 ℃ low temperature, be applicable to the vehicle under the low temperature in winter of north of China zone, reduce the freezing harmful effect that vehicle is caused.
With the tail gas catalytic reducer that only adds alcohols in Adblue as a comparison case, detect according to a conventional method NO
xconversion ratio, refer to table 2:
| NO XConversion ratio | Embodiment | Comparative Examples |
| The NO that freezing point is-30 ℃ XConversion ratio | 83% | 71% |
| The NO that freezing point is-35 ℃ XConversion ratio | 80% | 63% |
| Freezing point be-40 ℃ NO XConversion ratio | 77% | 57% |
Table 2
As shown in Table 2, the NO of anti-low temperature exhaust gas catalytic reducer of the present invention
xconversion ratio is compared to the NO of the tail gas catalytic reducer that only adds alcohols
xconversion ratio is significantly improved.
In addition to the implementation, the present invention can also have other embodiments.All employings are equal to the technical scheme of replacement or equivalent transformation formation, all drop on the protection domain of requirement of the present invention.
Claims (7)
1. an anti-low temperature exhaust gas catalytic reducer, by weight percentage, composed of the following components:
The diesel engine vent gas treatment fluid 30%～60% that meets the ISO22241-1 standard
Ammonium carbonate 10%～40%
Methyl alcohol 10%～40%
Polyetheramine 0.02%～0.2%
Ultra-pure water 10%～35%;
The preparation method of described anti-low temperature exhaust gas catalytic reducer comprises the following steps:
Step 1, dissolving, add described diesel engine vent gas treatment fluid, ammonium carbonate, methyl alcohol in dissolving tank, mixes, stirs, and makes the tail gas catalytic reducer first product;
Step 2, purification, purify described tail gas catalytic reducer first product by filtration, obtain the tail gas catalytic reducer filtered, then separate by film, obtains the tail gas catalytic reducer separated;
Step 3, make, described polyetheramine is added in the tail gas catalytic reducer of separation, and to adjust mass percentage concentration with ultra-pure water be 30%～50%, obtain cryophylactic tail gas catalytic reducer.
2. anti-low temperature exhaust gas catalytic reducer according to claim 1 is characterized in that: described ammonium carbonate is for analyzing pure ammonium carbonate, wherein calcium ion content≤0.5ppm.
3. anti-low temperature exhaust gas catalytic reducer according to claim 1 is characterized in that: described methyl alcohol is for analyzing pure methyl alcohol, wherein sodium ion, calcium ion content all≤0.5ppm.
4. anti-low temperature exhaust gas catalytic reducer according to claim 1, it is characterized in that: the molecular weight of described polyetheramine is M=1000-1500.
5. anti-low temperature exhaust gas catalytic reducer according to claim 1, it is characterized in that: described ultrapure resistivity of water is between 13～14M Ω cm.
6. anti-low temperature exhaust gas catalytic reducer according to claim 1, it is characterized in that: in described step 1, solution temperature is 30 ℃～35 ℃.
7. anti-low temperature exhaust gas catalytic reducer according to claim 1, it is characterized in that: in described step 2, bag filter, mechanical filter, the filtering accuracy that filters equipment for purifying and be filtering accuracy and be 10 microns is at least one in the precision Filter element filter of 0.45 micron, and filtration flow-rate is controlled at 2m
3/ H～3m
3/ H.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210008070.2A CN102580531B (en) | 2012-01-12 | 2012-01-12 | Low temperature-resistant tail gas catalytic reduction agent and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210008070.2A CN102580531B (en) | 2012-01-12 | 2012-01-12 | Low temperature-resistant tail gas catalytic reduction agent and preparation method thereof |
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| Publication Number | Publication Date |
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| CN102580531A CN102580531A (en) | 2012-07-18 |
| CN102580531B true CN102580531B (en) | 2014-01-08 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104265422B (en) * | 2014-08-03 | 2017-08-11 | 长春市永畅实业有限责任公司 | A kind of cryogenic conditions release ammonia reducing agent composition and preparation method thereof |
| CN104147926A (en) * | 2014-08-03 | 2014-11-19 | 长春市永畅实业有限责任公司 | Reducing agent mixture capable of releasing ammonia at low temperature |
| CN104128090A (en) * | 2014-08-03 | 2014-11-05 | 长春市永畅实业有限责任公司 | Reducing agent satisfying low temperature removal of nitrogen oxides of vehicles |
| CN104307366A (en) * | 2014-10-21 | 2015-01-28 | 张家港迪克汽车化学品有限公司 | Diesel vehicle tail gas catalyst reduction composition |
| CN105688669B (en) * | 2016-03-08 | 2018-03-09 | 江苏可兰素汽车环保科技有限公司 | Pectination polyacrylamide crystalloid increases agent interfering, the resistive connection crystal formation tail gas catalytic reducer prepared using the agent interfering and preparation method |
| CN105854603A (en) * | 2016-05-10 | 2016-08-17 | 南宁市夏阳化工科技有限责任公司 | Diesel tail gas treating agent production method |
| CN106745060A (en) * | 2016-12-14 | 2017-05-31 | 河南省化工研究所有限责任公司 | A kind of low form urea for vehicle solution and preparation method thereof |
| CN107198943A (en) * | 2017-05-02 | 2017-09-26 | 山西艾珂灵环境科技有限公司 | A kind of tail gas absorption liquid |
| CN108443000A (en) * | 2018-02-12 | 2018-08-24 | 新疆现代特油科技股份有限公司 | The automobile-used purified treatment liquid of low temperature |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102006059760A1 (en) * | 2006-12-18 | 2008-06-19 | Skw Stickstoffwerke Piesteritz Gmbh | Preparing pure urea solution, useful as reducing agent for selective catalytic reduction of nitrogen oxides, comprises rinsing urea solution in deaerator, separating urea crystals and re-circulating mother liquor enriched with biuret |
| CN101560422A (en) * | 2008-11-05 | 2009-10-21 | 戴伟平 | AdBlue composition as reducing agent for diesel engine with SCR technology |
| CN101811065A (en) * | 2010-04-20 | 2010-08-25 | 江苏可兰素汽车环保科技有限公司 | Production process for tail gas catalytic reducer |
-
2012
- 2012-01-12 CN CN201210008070.2A patent/CN102580531B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102006059760A1 (en) * | 2006-12-18 | 2008-06-19 | Skw Stickstoffwerke Piesteritz Gmbh | Preparing pure urea solution, useful as reducing agent for selective catalytic reduction of nitrogen oxides, comprises rinsing urea solution in deaerator, separating urea crystals and re-circulating mother liquor enriched with biuret |
| CN101560422A (en) * | 2008-11-05 | 2009-10-21 | 戴伟平 | AdBlue composition as reducing agent for diesel engine with SCR technology |
| CN101811065A (en) * | 2010-04-20 | 2010-08-25 | 江苏可兰素汽车环保科技有限公司 | Production process for tail gas catalytic reducer |
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Application publication date: 20120718 Assignee: JIANGSU LOPAL TECH. Co.,Ltd. Assignor: KELAS ENVIRONMENTAL PROTECTION TECHNOLOGY Co.,Ltd. Contract record no.: 2018320000050 Denomination of invention: Low temperature-resistant tail gas catalytic reduction agent and preparation method thereof Granted publication date: 20140108 License type: Exclusive License Record date: 20180309 |