CN104084086A - Surfactant for automotive urea solution and preparation method and application thereof - Google Patents
Surfactant for automotive urea solution and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a surfactant for an automotive urea solution, and a preparation method and an application thereof. The surfactant for the automotive urea solution is an aliphatic amine polyoxypropylene polyoxyethylene ether non-ionic surfactant. The preparation method of the surfactant comprises the following steps: (1) putting aliphatic amine or aliphatic diamine or a mixture of aliphatic amine and aliphatic diamine and a catalyst I into a reaction kettle, displacing air in the kettle with nitrogen, vacuumizing, heating, and slowly feeding propylene oxide for reaction so as to prepare a propoxy polyether compound; (2) putting the propoxy polyether compound and a catalyst II into a kettle under conditions similar to those of the kettle in the step (1), slowly feeding ethylene oxide, adjusting liquid in the kettle till the liquid is neutral after reaction, moving out the feed liquid, and centrifuging so as to obtain the aliphatic amine polyoxypropylene polyoxyethylene ether non-ionic surfactant. The method has the advantages of simplicity in operation and easiness in large-scale production. The prepared surfactant is directly fed into the automotive urea solution to improve the urea dispersion and atomization effects, increase the NH3 conversion efficiency and prevent an SCR (selected catalytic reduction) system from being blocked.
Description
Technical field
The present invention relates to automobile-used urea liquid, particularly relate to a kind of surfactant for automobile-used urea liquid and its production and use.
Background technology
Automobile, especially diesel vehicle, exhaust emissions has become one of main source of atmospheric pollution, NO
xit is the Main Ingredients and Appearance of vehicle exhaust.NO
xneed exhaust gas processing device to control, as: thin nitrogen oxide trapping technique (LNT), SCR (SCR) technology, oxidation catalysis conversion (DOC) technology, EGR+particle trapper (EGR+DPF) technology etc., SCR technology is widely used in the vent gas treatment of heavy-duty diesel oil locomotive.
SCR technology is to reduce the generation of particle (PM) by burning in reinforcing stimulus machine, then utilizes urea liquid to NO
xon SCR catalyst converter, carry out catalytic reduction.SCR selective catalytic reduction system operating has comprised 3 parts such as urea liquid supply system, urea solution jet and control system, SCR selective catalysis restoring system.Urea liquid is deposited in vehicle-mounted special holding vessel, with pump by the motor exhaust of urea solution jet thermotropism, (approximately 300～500 DEG C, meet reduction reaction conditions).At high temperature, after urea liquid gasification, decompose and produce NH
3, under catalyst action, NH
3with the NO in tail gas
xreaction, generates harmless H
2o and N
2.
But due to urea bad dispersibility, decompose not exclusively, urea decomposition is NH
3intermediate product isocyanic acid (HNCO) in process is easy to urea or biuret reaction in solution, generates and is difficult to decompose cyanuric acid, and under higher temperature, cyanuric acid is further condensed into melamine.The deposits such as undecomposed urea, cyanuric acid and melamine are attached on exhaust pipe, blender and SCR catalyst, have changed original gas flowfield, cause again sedimental further gathering, cause SCR system jams.SCR system jams can directly cause automobile fuel consumption to increase, and exhaust emissions worsens, and can cause engine to damage when serious.
Summary of the invention
The first object of the present invention is: a kind of fatty amine polyoxyethylene polyoxypropylene ether non-ionic surface active agent for automobile-used urea liquid is provided, this surfactant can solve that urea bad dispersibility in urea liquid, spray effect are poor, the unequal problem of atomized drop distribution of sizes, can effectively prevent SCR system jams.
The second object of the present invention is: the preparation method of the above-mentioned fatty amine polyoxyethylene polyoxypropylene ether non-ionic surface active agent for automobile-used urea liquid is provided, and the method is simple, is easy to realize large-scale production.
The 3rd object of the present invention is: a kind of automobile-used urea liquid that contains above-mentioned surfactant is provided, and the urea good dispersion of this automobile-used urea liquid, atomizing effect are good, NH
3transformation efficiency is high, effectively prevents the sedimental generations such as biuret, cyanuric acid and melamine, avoids SCR system jams.
For this reason, technical scheme of the present invention is:
For a surfactant for automobile-used urea liquid, this surfactant is fatty amine polyoxyethylene polyoxypropylene ether non-ionic surface active agent, and its structural formula is:
Wherein: wherein R
1, R
2=H or CH
3; N=2～18, preferably 6～12; M=2～12, preferably 4～8; X=1～10, preferably 1～6; Y=3～20, preferably 5～15.
The preparation method of described fatty amine polyoxyethylene polyoxypropylene ether non-ionic surface active agent, comprises the steps:
1) by fatty amine or aliphatic diamine or both mixtures and catalyst I input reactor with any mass ratio mixing, with air in nitrogen replacement still, be ﹣ 0.05～﹣ 0.095MPa to being evacuated to pressure in still, and be warming up to 90～140 DEG C, and then in still, slowly adding expoxy propane, still internal pressure rises, controlled pressure is at 0.2～0.4MPa, reaction 1～6h, question response still internal pressure stops reaction while being down to below 0, and discharging obtains propoxyl group polyether compound;
2) by step 1) the propoxyl group polyether compound that obtains and catalyst I I drop in reactor, with air in nitrogen replacement still, be ﹣ 0.05～﹣ 0.095MPa to being evacuated to pressure in still, and be warming up to 90～140 DEG C, then in still, slowly add oxirane, still internal pressure rises, controlled pressure is at 0.2～0.4MPa, reaction 1～6h, question response still internal pressure stops reaction while being down to below 0, regulate liquid in still to be after neutrality, method for optimizing for to drip phosphoric acid in reactor, feed liquid is shifted out and obtain described fatty amine polyoxyethylene polyoxypropylene ether non-ionic surface active agent through centrifugal after removing insoluble matter,
Described catalyst I, II be respectively in NaOH, potassium hydroxide, caustic alcohol or sodium methoxide one or more with arbitrarily than mix mixture;
Step 1) described in the quality of catalyst I be 0.5%～2% of fatty amine or aliphatic diamine or mixture that both mix with any mass ratio and expoxy propane quality sum;
The mixture that described fatty amine or aliphatic diamine or both mix with any mass ratio and ratio=1:1～10 of the amount of expoxy propane;
Step 2) described in propoxyl group polyether compound be 1:3～20 with the ratio of the amount of substance of oxirane;
The quality of described catalyst I I be described propoxyl group polyether compound and oxirane quality and 0.5%～2%.
The structural formula of described fatty amine or aliphatic diamine is
Wherein: R
1, R
2=H or CH
3; N=2～18, preferably 6～12; M=2～12, preferably 4～8;
Described fatty amine is the mixture of different fatty amines; Described aliphatic diamine is the mixture of different aliphatic diamines.
An automobile-used urea liquid that contains described fatty amine polyoxyethylene polyoxypropylene ether non-ionic surface active agent, in this automobile-used urea liquid, comprising concentration is the described fatty amine polyoxyethylene polyoxypropylene ether non-ionic surface active agent of 10～5000ppm.
In this automobile-used urea liquid, comprising concentration is the described fatty amine polyoxyethylene polyoxypropylene ether non-ionic surface active agent of 10～5000ppm and the anti-foaming agent that concentration is 0.1～20wt.%.
Described anti-foaming agent is the mixture of one or more alcohol in methyl-silicone oil or the carbon number alcohol that is 2～8.
This is used for the fatty amine polyoxyethylene polyoxypropylene ether non-ionic surface active agent of automobile-used urea liquid, this surfactant can solve that urea bad dispersibility in urea liquid, spray effect are poor, the unequal problem of atomized drop distribution of sizes, effectively prevent the sedimental generations such as biuret, cyanuric acid and melamine, effect prevents SCR system jams.Its preparation method is simple, is easy to realize large-scale production.Coordinate anti-foaming agent to add in automobile-used urea liquid fat amine polyoxyethylene polyoxypropylene ether non-ionic surface active agent of the present invention, meeting on the basis of ISO22241-1 and GB29518 standard-required, its urea good dispersion, atomizing effect are good, NH
3transformation efficiency is high, can effectively prevent the sedimental generations such as biuret, cyanuric acid and melamine, avoids SCR system jams.
Brief description of the drawings
Surfactant S prepared by Fig. 1 embodiment of the present invention 1
1surface tension with concentration curve.
Surfactant S prepared by Fig. 2 embodiment of the present invention 2
2surface tension with concentration curve.
Surfactant S prepared by Fig. 3 embodiment of the present invention 3
3surface tension with concentration curve.
Detailed description of the invention
Below in conjunction with drawings and Examples, the present invention is described further, and its object is only better to understand content of the present invention but not limits the scope of the invention.
Embodiment 1
1) 24.1g cetylamine and 0.5g potassium hydroxide are dropped in autoclave, with air in nitrogen replacement still, to be evacuated in still-0.09Mpa, be warming up to 120 DEG C of reaction temperatures, then slowly in still, pass into 23.2g expoxy propane by conduit, still internal pressure constantly rises, controlled pressure is below 0.4Mpa, reaction 4h, expoxy propane complete reaction, discharging makes cetylamine polyethenoxy ether;
2) 23.6g cetylamine polyethenoxy ether and 0.5g caustic alcohol are dropped in autoclave, with air in nitrogen replacement still, to be evacuated in still-0.09Mpa, be warming up to 120 DEG C of reaction temperatures, then slowly pass into 22g oxirane by conduit, still internal pressure constantly rises, controlled pressure is below 0.4Mpa, reaction time is 4h, to oxirane complete reaction, be after neutrality to dripping phosphoric acid to liquid in still in reactor, feed liquid in still is moved to and in centrifuge tube, carries out centrifugally, remove insoluble matter and obtain cetylamine polyoxyethylene polyoxypropylene ether (S
1) product, its theoretical construct formula is as follows:
3) in the aqueous solution that is 32.5% to urea quality concentration, add the cetylamine polyoxyethylene polyoxypropylene ether surface active agent of variable concentrations, the surface tension of test different surfaces surfactant concentration solution, and mapping, as shown in Figure 1.The critical micelle concentration of cetylamine polyoxyethylene polyoxypropylene ether is 4.1 × 10
-5g/mL, the surface tension at critical micelle concentration place is 29.5mN/m.Add as seen from the figure S
1after, the surface tension of urea liquid declines, and energy barrier while disperseing for the lower solution's solute of surface tension is lower, so, add S
1be conducive to improve the dispersiveness of urea liquid.
4) use the automobile-used urea liquid that laser-Doppler dynamic particles analyzer (PDA) is 32.5% to urea quality concentration and add S
1automobile-used urea liquid (the S of additive
1addition is 1 × 10
-4g/mL, urea quality concentration is 32.5%) carry out testing spraying characteristic.In spray axis, choose five cross sections, 5 measurement points of each section selection, the average diameter of calculating drop, experimental result is in Table I.The visible S that adds
1after, the mean drop diameter on cross section obviously diminishes.
Table I cetylamine polyoxyethylene polyoxypropylene ether (S
1) spray characteristics is affected
5) by 3) in added the composite methyl-silicone oil that enters to account for its gross mass 1% in the automobile-used urea liquid of cetylamine polyoxyethylene polyoxypropylene ether surface active agent, be applied to the platform experiment of engine, experimental temperature is between 250 DEG C～280 DEG C, the impact that the addition of mensuration surfactant reduces SCR system sediment yield, the results are shown in table II.
Table II cetylamine polyoxyethylene polyoxypropylene ether (S
1) impact of addition on sediment yield minimizing
Embodiment 2
(1) 18.5g bis-n-hexylamines and 0.6g caustic alcohol are dropped in autoclave, with air in nitrogen replacement still, to be evacuated in still-0.07Mpa, be warming up to 100 DEG C of reaction temperatures, then slowly pass into 34.8g expoxy propane by conduit, still internal pressure constantly rises, controlled pressure is below 0.4Mpa, reaction 4h, to expoxy propane complete reaction, discharging makes two n-hexylamine polyethenoxy ethers;
(2) 26.6g bis-n-hexylamine polyethenoxy ethers and 0.89g NaOH are dropped in autoclave, with air in nitrogen replacement still, to be evacuated in still-0.07Mpa, be warming up to 100 DEG C of reaction temperatures, then slowly pass into 33g oxirane by conduit, still internal pressure constantly rises, controlled pressure is below 0.4Mpa, reaction time is 6h, to oxirane complete reaction, to dripping phosphoric acid in reaction system to neutral, feed liquid is moved to and in centrifuge tube, carries out centrifugally, remove insoluble matter and obtain two n-hexylamine polyoxyethylene polyoxypropylene ether (S
2) product, its theoretical construct formula is as follows:
(3) in the automobile-used urea liquid that is 32.5% to urea quality concentration, add two n-hexylamine polyoxyethylene polyoxypropylene ether (S of variable concentrations
2) surfactant, the surface tension of test different surfaces surfactant concentration solution, and mapping, as shown in Figure 2.The critical micelle concentration of two n-hexylamine polyoxyethylene polyoxypropylene ethers is 1.5 × 10
-5g/mL, the surface tension at critical micelle concentration place is 27.7mN/m.
(4) use laser-Doppler dynamic particles analyzer (PDA) to the automobile-used urea liquid of blank (urea quality concentration is 32.5%) and add S
2automobile-used urea (the S of additive
2addition is 1 × 10
-4g/mL, urea quality concentration is 32.5%) carry out testing spraying characteristic.In spray axis, choose five cross sections, 5 measurement points of each section selection, the average diameter of calculating drop, experimental result is in Table III.Add S
2after, the mean drop diameter on cross section obviously diminishes.
Table III two n-hexylamine polyoxyethylene polyoxypropylene ether (S
2) spray characteristics is affected
(5) by 3) in added the composite butanols that enters to account for its gross mass 2% in the automobile-used urea liquid of two n-hexylamine polyoxyethylene polyoxypropylene ether surface active agents, be applied to the platform experiment of engine, experimental temperature is 300 DEG C, the impact that the addition of mensuration surfactant reduces SCR system sediment yield, the results are shown in table IV.
Table IV two n-hexylamine polyoxyethylene polyoxypropylene ether (S
2) impact of addition on sediment yield minimizing
Embodiment 3
(1) 17.2g decamethylene diamine and 2g sodium methoxide are dropped in autoclave, with air in nitrogen replacement still, to be evacuated in still-0.05Mpa, be warming up to 120 DEG C of reaction temperatures, then slowly pass into 116g expoxy propane by conduit, still internal pressure constantly rises, controlled pressure is below 0.4Mpa, reaction 4h, to expoxy propane complete reaction, discharging makes decamethylene diamine polyethenoxy ether;
(2) 66.6g decamethylene diamine polyethenoxy ether and 2.5g sodium methoxide are dropped in autoclave, with air in nitrogen replacement still, to be evacuated in still-0.05Mpa, be warming up to 120 DEG C of reaction temperatures, then slowly pass into 88g oxirane by conduit, still internal pressure constantly rises, controlled pressure is below 0.4Mpa, reaction time is 6h, to oxirane complete reaction, to dripping phosphoric acid in reaction system to neutral, feed liquid is transferred to and in centrifuge tube, carries out centrifugally, remove insoluble matter and obtain decamethylene diamine polyoxyethylene polyoxypropylene ether (S
3) product, its theoretical construct formula is as follows:
(3) in the automobile-used urea liquid that is 32.5% to urea quality concentration, add the decamethylene diamine polyoxyethylene polyoxypropylene ether (S of variable concentrations
3) surfactant, the surface tension of test different surfaces surfactant concentration solution, and mapping, as shown in Figure 3.The critical micelle concentration of decamethylene diamine polyoxyethylene polyoxypropylene ether is 1.0 × 10
-4g/mL, the surface tension at critical micelle concentration place is 34.8mN/m.
(4) use laser-Doppler dynamic particles analyzer (PDA) to the automobile-used urea liquid of blank (urea quality concentration is 32.5%) and add S
3automobile-used urea (the S of additive
3addition is 1 × 10
-4g/mL, urea quality concentration is 32.5%) carry out testing spraying characteristic.In spray axis, choose five cross sections, 5 measurement points of each section selection, the average diameter of calculating drop, experimental result is in Table V.Add S
3after, the mean drop diameter on cross section obviously diminishes.
Table V decamethylene diamine polyoxyethylene polyoxypropylene ether (S
3) spray characteristics is affected
(5) by 3) in added the composite octanol that enters to account for its gross mass 2% in the automobile-used urea liquid of decamethylene diamine polyoxyethylene polyoxypropylene ether surface active agent, be applied to the platform experiment of engine, experimental temperature is 300 DEG C, the impact that the addition of mensuration surfactant reduces SCR system sediment yield, the results are shown in table VI.
Table VI decamethylene diamine polyoxyethylene polyoxypropylene ether (S
3) impact of addition on sediment yield minimizing
Claims (10)
1. for a surfactant for automobile-used urea liquid, it is characterized in that: this surfactant is fatty amine polyoxyethylene polyoxypropylene ether non-ionic surface active agent, and its structural formula is:
Wherein: wherein R
1, R
2=H or CH
3; N=2～18; M=2～12; X=1～10; Y=3～20.
2. surfactant as claimed in claim 1, is characterized in that: n=6～12 in the structural formula of surfactant; M=4～8; X=1～6; Y=5～15.
3. the preparation method of surfactant as claimed in claim 1 or 2, is characterized in that comprising the steps:
1) by fatty amine or aliphatic diamine or both mixtures and catalyst I input reactor with any mass ratio mixing, with air in nitrogen replacement still, be ﹣ 0.05～﹣ 0.095MPa to being evacuated to pressure in still, and be warming up to 90～140 DEG C, and then in still, slowly adding expoxy propane, still internal pressure rises, controlled pressure is at 0.2～0.4MPa, reaction 1～6h, question response still internal pressure stops reaction while being down to below 0, and discharging obtains propoxyl group polyether compound;
2) by step 1) the propoxyl group polyether compound that obtains and catalyst I I drop in reactor, with air in nitrogen replacement still, be ﹣ 0.05～﹣ 0.095MPa to being evacuated to pressure in still, and be warming up to 90～140 DEG C, then in still, slowly add oxirane, still internal pressure rises, controlled pressure is at 0.2～0.4MPa, reaction 1～6h, question response still internal pressure stops reaction while being down to below 0, regulate liquid in still to be after neutrality, feed liquid is shifted out and obtain described fatty amine polyoxyethylene polyoxypropylene ether non-ionic surface active agent through centrifugal after removing insoluble matter,
Described catalyst I, II be respectively in NaOH, potassium hydroxide, caustic alcohol or sodium methoxide one or more with arbitrarily than mix mixture;
Step 1) described in the quality of catalyst I be 0.5%～2% of fatty amine or aliphatic diamine or mixture that both mix with any mass ratio and expoxy propane quality sum;
The mixture that described fatty amine or aliphatic diamine or both mix with any mass ratio and ratio=1:1～10 of the amount of expoxy propane;
Step 2) described in propoxyl group polyether compound be 1:3～20 with the ratio of the amount of substance of oxirane;
The quality of described catalyst I I be described propoxyl group polyether compound and oxirane quality and 0.5%～2%.
4. preparation method as claimed in claim 3, is characterized in that: step 2) in to regulate liquid in still be that neutral method is to drip phosphoric acid.
5. preparation method as claimed in claim 3, is characterized in that: the structural formula of described fatty amine or aliphatic diamine is
Wherein: R
1, R
2=H or CH
3; N=2～18; M=2～12.
6. preparation method as claimed in claim 5, is characterized in that: n=6～12 in the structural formula of described fatty amine or aliphatic diamine; M=4～8.
7. preparation method as claimed in claim 5, is characterized in that: the mixture that described fatty amine is different fatty amines; Described aliphatic diamine is the mixture of different aliphatic diamines.
8. contain an automobile-used urea liquid for surfactant as claimed in claim 1 or 2, it is characterized in that: in this automobile-used urea liquid, comprising concentration is the described fatty amine polyoxyethylene polyoxypropylene ether non-ionic surface active agent of 10～5000ppm.
9. contain an automobile-used urea liquid for surfactant as claimed in claim 1 or 2, it is characterized in that: in this automobile-used urea liquid, comprising concentration is the described fatty amine polyoxyethylene polyoxypropylene ether non-ionic surface active agent of 10～5000ppm and the anti-foaming agent that concentration is 0.1～20wt.%.
10. automobile-used urea liquid as claimed in claim 9, is characterized in that: described anti-foaming agent is the mixture of one or more alcohol in methyl-silicone oil or the carbon number alcohol that is 2～8.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410341548.2A CN104084086B (en) | 2014-07-17 | 2014-07-17 | For the surfactant and its production and use of urea for vehicle solution |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410341548.2A CN104084086B (en) | 2014-07-17 | 2014-07-17 | For the surfactant and its production and use of urea for vehicle solution |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105032172A (en) * | 2014-11-17 | 2015-11-11 | 刘德龙 | High-efficient cleaning and maintenance liquid of diesel engine SCR system |
| CN106039996A (en) * | 2016-06-28 | 2016-10-26 | 许江煌 | Adblue and preparation method thereof |
| CN106064020A (en) * | 2016-06-28 | 2016-11-02 | 许江煌 | A kind of preparation method of urea for vehicle |
| CN107433123A (en) * | 2017-08-29 | 2017-12-05 | 东莞市升佳净水材料有限公司 | A kind of SNCR flue-gas denitration process denitrfying agent |
| CN108409957A (en) * | 2017-12-07 | 2018-08-17 | 天津工业大学 | A kind of urea for vehicle solution fluorocarbon surfactant |
| CN108499360A (en) * | 2018-04-14 | 2018-09-07 | 长沙小新新能源科技有限公司 | A kind of urea for vehicle and preparation method thereof containing catalyst |
| 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 |
| CN112791587A (en) * | 2020-12-31 | 2021-05-14 | 温州君怡化工贸易有限公司 | High-atomization automotive urea solution and preparation method thereof |
| CN114534487A (en) * | 2022-03-19 | 2022-05-27 | 北京盛鑫和谐润滑油脂有限公司 | Low-temperature-resistant anti-crystallization urea and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112791587A (en) * | 2020-12-31 | 2021-05-14 | 温州君怡化工贸易有限公司 | High-atomization automotive urea solution and preparation method thereof |
| CN114534487A (en) * | 2022-03-19 | 2022-05-27 | 北京盛鑫和谐润滑油脂有限公司 | Low-temperature-resistant anti-crystallization urea and preparation method and application thereof |
| CN114534487B (en) * | 2022-03-19 | 2024-06-04 | 北京盛鑫和谐润滑油脂有限公司 | Low-temperature-resistant crystallization-resistant urea and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104084086B (en) | 2016-01-13 |
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