KR101774254B1 - Selective non-catalytic reduction solution for nitrogen oxides removal - Google Patents
Selective non-catalytic reduction solution for nitrogen oxides removal Download PDFInfo
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- KR101774254B1 KR101774254B1 KR1020150179905A KR20150179905A KR101774254B1 KR 101774254 B1 KR101774254 B1 KR 101774254B1 KR 1020150179905 A KR1020150179905 A KR 1020150179905A KR 20150179905 A KR20150179905 A KR 20150179905A KR 101774254 B1 KR101774254 B1 KR 101774254B1
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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
- B01D53/46—Removing components of defined structure
- B01D53/54—Nitrogen compounds
- B01D53/56—Nitrogen oxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2257/00—Components to be removed
- B01D2257/40—Nitrogen compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2257/00—Components to be removed
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- B01D2257/404—Nitrogen oxides other than dinitrogen oxide
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Abstract
The present invention relates to a selective catalystless reducing agent for reducing nitrogen oxides, and more particularly, to a method for reducing nitrogen oxides by adding a certain amount of a surface tension improver to a hydrazine aqueous solution used in a selective non-catalytic reduction method for nitrogen oxides, The reducing agent of the hydrazine aqueous solution can be refined to reduce the nitrogen oxide at a high efficiency compared to the same amount of use and chemically accelerates the decomposition reaction of hydrazine even at a relatively low temperature of 800 ° C or lower, The present invention relates to a selective catalytic reduction agent which is very useful as a reducing agent for exhaust gas purification in various industrial facilities and automobiles.
Description
The present invention relates to a selective catalytic reduction agent for reducing nitrogen oxides, and more particularly, to a method for reducing nitrogen oxides by adding a certain amount of a surface tension improver to a hydrazine aqueous solution used in a selective non-catalytic reduction method for nitrogen oxides It is possible to reduce the nitrogen oxide at a high efficiency compared with the same amount of use and to chemically accelerate the decomposition reaction of hydrazine even at a relatively low temperature of 800 ° C or lower, Which can effectively reduce nitrogen oxides (NOx), and is very useful as a reducing agent for exhaust gas purification in various industrial facilities and automobiles.
Generally, nitrogen oxides (NOx) contained in exhaust gases refer to nitrogen monoxide (NO), nitrogen dioxide (NO 2 ), and nitrous oxide (N 2 O), which are examples of substances that cause environmental pollution such as carbon monoxide and sulfur compounds It is one.
And nitrous oxide is not toxic but it is the main cause of global warming together with carbon dioxide. Nitrous oxide is the main component of exhaust gas nitrogen oxide, and when it is discharged into the air, it reacts with oxygen even at room temperature and is easily converted into nitrogen dioxide.
In particular, nitrogen monoxide and nitrogen dioxide are highly toxic carcinogens that cause serious air pollution and cause acid rain as well as sulfur oxides.
Accordingly, a technique for reducing nitrogen oxides by combustion control and exhaust gas treatment has been developed.
Among them, the nitrogen oxide reduction technique by the exhaust gas treatment is roughly divided into a case of using a catalyst and a case of treating without using a catalyst.
The selective non-catalytic reduction process is performed by direct injection of ammonia (e.g., U.S. Patent No. 3,900,554) or urea aqueous solution (e.g., U.S. Patent No. 4,119,702, U.S. Patent No. 4,208,386) at high temperature to reduce NOx by nitrogen and water vapor The NOx reduction rate can be reduced to 60 ~ 80% by converting NO into N 2 and H 2 O through a multi-stage reaction process in a narrow temperature range of 930 ~ 980 ° C.
On the other hand, hydrazine (Hydrazine, N 2 H 4) is when the temperature rises as having a molecular structure of the H 2 N-NH 2 about the coupling between the HN than other NH bond, so may be first cut off, and thus N 2 H 4 2NH the reaction of 2 generate NH 2, and is end-digested with N 2 and H 2 O through the reaction of the NH 2 + NO.
Pure hydrazine has thermodynamic properties quite similar to water, but the reduction potential is very strong and toxic and explosive. However, a low concentration of hydrazine aqueous solution has been used as a nitrogen oxide reducing agent easily and safely.
Then, hydrazine hydrate (N 2 H 4. H 2 O) use of a nitrogen oxide reducing agent in the first, and so on Azuhata the N 2 H 4 -NO-O NO even in the second-low temperature range of 773 ~ 873K is N 2 And H 2 O (S, Azuhata, H. Akimoto, Y. Hishinuma, AICHE J., 1985, 31 (7), 1223-1225).
In addition, JB and Lee et al. (1998) reported that NOx reduction was effective at temperatures of 800 to 950 K, which is 300 ° C lower than ammonia, through pilot scale experiments (JBLee et al. 99-104).
As such, the selective non-catalytic reduction method has a lower reduction efficiency than the selective catalytic reduction (SCR) method using a catalyst, but the installation cost and the installation period are short and the additional facility is not required. Therefore, It is more effective.
However, in the selective non-catalytic reduction method, the NOx reduction efficiency is sensitive to the reaction parameters such as the reduction temperature range, the reducing liquid injection concentration, the injection amount, and the oxygen concentration, so optimization of the reducing liquid and the process parameters is required.
Therefore, as a conventional method for solving the above problems, a method of using a gas phase additive together with an urea aqueous solution injection (WO 91/17814), a method of injecting alcohol, sugar and ketone as a liquid phase additive / 17814), and a method using ammonium carbamate containing ammonium ion as a reducing agent (U.S. Patent No. 4,997,631).
Further, a solution of paraffin, olefin-based oxidized hydrocarbons (U.S. Patent No. 4,719,092) and a chemical solution containing an urea aqueous solution or ammonium ion is introduced at a temperature of 730 to 930 캜 , A method of mixing hydroxyaminohydrocarbons with aqueous hydrogen peroxide at a temperature lower than 760 ° C (U.S. Patent No. 4,777,024).
Other patents for additives include ammonia aqueous solution, ammonium carbonate, ammonium oxalate, etc. as a liquid additive in the aqueous solution, and hydrogen, carbon monoxide, and hydrocarbons as a vapor additive (U.S. Patent No. 3,900,554 number).
In addition, a method of using KOH or NaOH as an additive (U.S. Patent No. 5,543,123) as an additive and a method of preventing scale formation in a pipe by adding phosphate to improve the operability of the entire process (U.S. Patent No. 5,441,743) It has been suggested.
Nevertheless, in the conventional methods as described above, ammonia is used as a reducing agent, and a reducing temperature range is also applied to a high temperature range. In the case of an additive for injecting at a low temperature, the cost is high or the nitrogen oxide reduction performance is low There was a drawback and needed improvement.
On the other hand, in advanced countries, there is a tendency to strictly regulate various environmentally polluting exhaust gases, and the demand for exhaust gas purification technology is expected to increase greatly in the future.
Therefore, it is desired to develop a selective non-catalytic reducing agent which can maintain excellent nitrogen oxide reduction efficiency over a wide temperature range compared with the conventional one.
SUMMARY OF THE INVENTION Accordingly, the present invention has been made to solve the above-mentioned problems occurring in the prior art, and an object of the present invention is to provide a method for reducing nitrogen oxides by adding a specific amount of a surface tension improver to a nitrogen oxide reduction catalyst, And an object of the present invention is to provide a selective non-catalytic reducing agent for reducing nitrogen oxides.
The present invention provides a selective catalytic reduction agent for reducing nitrogen oxides in the form of a water-soluble reducing liquid in which hydrazine hydrate and distilled water are mixed and dissolved at a weight ratio of 1: 1-1: 9; 0.1 to 5.0 parts by weight of a surface tension improver composed of at least one of a polyether-modified polydimethylsiloxane and an alkyl-modified polymethylalkylsiloxane is added to 100 parts by weight of the water-soluble reducing liquid to adjust the surface tension of the water- To 30 dyn / cm or less, thereby reducing the droplet size of the spray liquid even at 800 ° C or lower, thereby enhancing the reducibility of hydrazine.
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Further, the water-soluble reducing liquid is characterized by further adding not more than 50 parts by weight of alcohols to 100 parts by weight of the water-soluble reducing liquid.
The alcohols are also characterized by being at least one selected from the group consisting of methyl alcohol, ethyl alcohol, isobutanol, butyl glycol, diethylene glycol, ethylene glycol, cyclohexanol, and triethylene glycol.
According to the present invention, the selective non-catalytic reduction liquid containing the surface tension improver reduces the size of the droplet of the reducing liquid in the process of reducing the nitrogen oxide in the exhaust gas to harmless nitrogen and water, thereby effectively improving the contact efficiency between the nitrogen oxide and the reducing material Thereby ultimately enhancing the reduction efficiency of nitrogen oxides.
Further, the present invention improves the contact efficiency between the nitrogen oxide and the reducing liquid, thereby making it possible to reduce the nitrogen oxide at a lower temperature, thereby lowering the cost of the nitrogen oxide removal process.
The selective non-catalytic reducing agent for reducing nitrogen oxides according to the present invention improves the performance of a hydrazine aqueous solution by using a predetermined amount of a surface tension improver so that a reducing agent capable of maintaining a high NOx reduction rate even at a low temperature, Nitrogen oxides can be effectively reduced even at a relatively low temperature, thereby contributing greatly to prevention of environmental pollution.
BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a graph showing the relationship between the reduction rate of nitrogen oxides using a reducing solution containing polyether-modified siloxane (BYK-348) as a reducing agent and the amount of nitrogen oxides Of the total amount of the waste water.
Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.
Before describing the present invention, the following specific structural or functional descriptions are merely illustrative for the purpose of describing an embodiment according to the concept of the present invention, and embodiments according to the concept of the present invention may be embodied in various forms, And should not be construed as limited to the embodiments described herein.
In addition, since the embodiments according to the concept of the present invention can make various changes and have various forms, specific embodiments are illustrated in the drawings and described in detail herein. However, it should be understood that the embodiments according to the concept of the present invention are not intended to limit the present invention to specific modes of operation, but include all modifications, equivalents and alternatives falling within the spirit and scope of the present invention.
As a result of efforts to develop a selective catalystless reducing agent that maintains a high NOx reduction rate in a lower and wider temperature range, the present inventors have found that when a certain amount of a surface tension improver is added as a liquid compound to a hydrazine aqueous solution used as a reducing agent, The formation of NH 2 radicals generated by the decomposition of hydrazine is made possible at a lower temperature and the reduction performance is rapidly improved even at a low temperature. Thus, the present invention has been completed.
Accordingly, unlike the prior art, the present invention provides an improved non-catalytic reducing agent having a nitrogen oxide reduction effect at a low temperature as well as a high temperature by adding a specific amount of a surface tension improver to increase the nitrogen oxide reduction efficiency.
The selective non-catalytic reducing agent for nitrogen oxide reduction according to the present invention constitutes a water-soluble, non-catalytic reducing liquid containing hydrazine.
At this time, the hydrazine is a strong reducing agent, as is well known.
In order to further improve the nitrogen oxide reduction effect, a surface tension improving agent capable of reducing the droplet size of the water-soluble reducing spray liquid as an additive to the aqueous non-catalytic reducing liquid, that is, .
In this case, the surface tension improver is added in an amount of 0.1-5 parts by weight based on 100 parts by weight of the water-soluble, non-catalytic reducing liquid.
In particular, the surface tension of the water-soluble, non-catalytic reducing liquid prepared by adding the surface tension improver should be kept at 30 dyn / cm or less.
When the amount of the surface tension improver is more than 5.0 parts by weight, there is a problem in that not only the economical efficiency of the reducing solution but also the contamination of the continuous residue of the contained silicon oxide occurs, and when the surface tension improver is less than 0.1 part by weight, It is difficult to obtain.
In addition, the reducing agent is a myriad deurajin (N 2 H 4) or hydrated hydrazine (N 2 H 4. H 2 O) may be used without distinction, in consideration of the ease of handling using the hydrazine hydrate is particularly preferred.
The addition amount of the hydrazine should be in the range of 10-50 parts by weight based on 100 parts by weight of the aqueous non-catalytic reducing solution. Therefore, distilled water is used for constituting the reducing liquid, and the hydrazine and distilled water are mixed at a weight ratio of 1: 1-1: 9.
If the hydrazine is added in an amount of less than 10 parts by weight, it is difficult to expect a reduction effect of nitrogen oxides. When the amount of the hydrazine is more than 50 parts by weight, the loss due to excessive spraying increases and economical efficiency is lowered. .
In addition, in order to further increase the reducing property of the water-soluble, non-catalytic reducing liquid, alcohols may be further added in an amount of 50 parts by weight or less based on 100 parts by weight of the aqueous non-catalytic reducing liquid.
Examples of the surface tension improver include polyether-modified polydimethylsiloxane, alkyl-modified polymethylalkylsiloxane, and specifically, BYK 306, 337, 341, 307, 333, 310, 344, 315, 320, 322, 323, 325, 340, 345, 347, 348, 349, 346, BYK-DYNWET 800, Shinetsu KP-341 and the like.
The alcohols added for improving the nitrogen oxide reduction efficiency include at least one selected from the group consisting of methyl alcohol, ethyl alcohol, isobutanol, butyl glycol, diethylene glycol, ethylene glycol, cyclohexanol, triethylene glycol, .
Hereinafter, examples will be described.
Hydrazine hydrate (N 2 H 4. H 2 O) slowly dissolved in 100g of distilled water of 900g and, where the polyether-modified siloxane (manufactured by BYK-348, BYK Gardner GmbH) for using the followed by the addition of 5g agitator 30 ℃ For 60 minutes to prepare a reducing aqueous solution for reducing nitrogen oxides, that is, a water-soluble reducing liquid.
The surface tension of the aqueous reducing solution was measured using an automatic force tensometer (KSV Model Sigma 702). The result was 25.2 dyn / cm at 25 ° C.
On the other hand, the effect of the present invention was tested by injecting the aqueous reducing solution into a reduction reactor having controlled nitrogen concentration and temperature.
At this time, the configuration of the used apparatus is as follows.
In a burner that burns liquefied petroleum gas (LPG), high temperature flue gas is generated. The flue gas is passed through a reduction reaction apparatus made of stainless steel material (SUS304) having an outer diameter of 62 mm and a length of 1.0 m, And then released into the atmosphere.
The reduction reactor is horizontally installed inside an electric furnace capable of controlling the temperature, and the temperature inside the steel pipe is controlled by controlling the amount of combustion of the LPG gas and the heat amount of the electric furnace.
The temperature was measured at three places on the side of the steel pipe, and several tubes having an outer diameter of 5.0 mm were installed for the purpose of sample collection and drug injection. The concentration of nitrogen oxide was measured in an LPG combustion burner And the NO supplied through the gas flow meter (MFC) is appropriately mixed with the supplied secondary air.
The hydrazine-containing reducing aqueous solution was supplied using a metering pump and injected into the reduction reactor together with the atomizing air.
The exhaust gas discharged from the reduction reaction apparatus is continuously collected in a sample tube installed before the absorption tower and the concentration is measured by a NOx analyzer. Here, the concentration of nitrogen oxide is adjusted to 500 ppm and the temperature is maintained at 800 ° C. And the prepared reducing agent was sprayed inside.
After spraying, the concentration of nitrogen oxides was measured to evaluate the reduction rate.
As a result of the evaluation, when the reducing solution of [Example 1] was used, it was measured at 85 ppm, and the reduction ratio was 83.0% when calculated proportionally.
[Comparative Example 1]
As in Example 1, a water-soluble reducing liquid from which only the surface tension improver was removed in the preparation of a reduced aqueous solution (aqueous reducing solution) using hydrazine was prepared. The surface tension of the aqueous reducing solution was 40.6 dyn / cm at 25 ° C.
The nitrogen oxide reduction rate was measured by the same method and the initial concentration of 503 ppm was measured at 146 ppm at the outlet.
From this, the nitrogen oxide reduction ratio of the reducing solution containing no surface tension improver was evaluated as 71.0%.
That is, it was confirmed that the reduction rate of nitrogen oxides was effectively improved when the surface tension improver was included in comparison with [Example 1], and it is shown in FIG. 1 as a graph to facilitate understanding.
Hydrazine hydrate (N 2 H 4. H 2 O) slowly dissolved in 100g of distilled water of 700g and, here, a surface tension modifier of a polyether-modified siloxane (BYK-348, manufactured by BYK Gardner GmbH) in 5g of methanol 120g of ethanol 80g Were mixed and homogeneously mixed at 30 ° C for 60 minutes using a stirrer to prepare a reducing aqueous solution (aqueous reducing solution) for reducing nitrogen oxides.
The surface tension of the aqueous alcohol-containing water reducing solution was 20.6 dyn / cm at 25 ° C. The nitrogen oxide reduction rate was measured in the same manner as in [Example 1], and the initial concentration of 501 ppm was measured at 76 ppm at the outlet.
As a result, it was confirmed that the reduction rate of nitrogen oxides in the aqueous reducing solution further containing alcohol was 84.8%, and the reduction rate of nitrogen oxides was further improved when the alcohol was contained.
Claims (5)
0.1 to 5.0 parts by weight of a surface tension improver composed of at least one of a polyether-modified polydimethylsiloxane and an alkyl-modified polymethylalkylsiloxane is added to 100 parts by weight of the water-soluble reducing liquid to adjust the surface tension of the water- To 30 dyn / cm or less, thereby reducing the droplet size of the spray liquid even at 800 ° C or lower, thereby enhancing the reducibility of hydrazine.
Wherein the water-soluble reducing liquid is further added with not more than 50 parts by weight of alcohols per 100 parts by weight of the water-soluble reducing liquid.
Wherein the alcohols are at least one selected from the group consisting of methyl alcohol, ethyl alcohol, isobutanol, butyl glycol, diethylene glycol, ethylene glycol, cyclohexanol, and triethylene glycol.
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| FR3130815A1 (en) * | 2021-12-21 | 2023-06-23 | Arkema France | METHOD FOR THE PREPARATION OF HYDRAZINE HYDRATE IN THE PRESENCE OF AN ANTI-FOAMING AGENT |
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| KR102079768B1 (en) * | 2018-05-08 | 2020-02-20 | 에스케이가스 주식회사 | A method for reducing nitrogen dioxide in the exhaust gas generated during an olefin production process |
| CN109758898A (en) * | 2019-02-21 | 2019-05-17 | 上海市机电设计研究院有限公司 | Based on ammonium hydroxide+hydrazine mixing denitrfying agent, denitration method for flue gas and preparation facilities |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR100393322B1 (en) * | 2003-03-28 | 2003-08-02 | Samjungenvis Co Ltd | Agent for removing nitrogen oxide in exhaust gas from waste incinerator |
| KR100402051B1 (en) * | 2000-10-18 | 2003-10-17 | 한국과학기술연구원 | Selective non-catalytic reducing agent for reducing nitric oxides in flue gases |
| JP4544996B2 (en) * | 2002-08-22 | 2010-09-15 | Ａｇｃセイミケミカル株式会社 | Fluorosurfactant |
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| KR100402051B1 (en) * | 2000-10-18 | 2003-10-17 | 한국과학기술연구원 | Selective non-catalytic reducing agent for reducing nitric oxides in flue gases |
| JP4544996B2 (en) * | 2002-08-22 | 2010-09-15 | Ａｇｃセイミケミカル株式会社 | Fluorosurfactant |
| KR100393322B1 (en) * | 2003-03-28 | 2003-08-02 | Samjungenvis Co Ltd | Agent for removing nitrogen oxide in exhaust gas from waste incinerator |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR3130815A1 (en) * | 2021-12-21 | 2023-06-23 | Arkema France | METHOD FOR THE PREPARATION OF HYDRAZINE HYDRATE IN THE PRESENCE OF AN ANTI-FOAMING AGENT |
| WO2023118739A1 (en) * | 2021-12-21 | 2023-06-29 | Arkema France | Process for preparing hydrazine hydrate in the presence of an anti-foaming agent |
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