CN114375220B - Method for regenerating carbonic acid type layered double hydroxide and acid exhaust gas treatment equipment - Google Patents
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- B01D53/34—Chemical or biological purification of waste gases
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Abstract
The purpose of the present invention is to provide a method for regenerating a carbonic acid type layered double hydroxide (Mg-Al LDH) capable of efficiently regenerating a used anionic type Mg-Al type layered double hydroxide (Mg-Al LDH) in an acid exhaust gas treatment, and an acid exhaust gas treatment facility. The method for regenerating a carbonic acid type layered double hydroxide according to the present invention is a method for regenerating a carbonic acid type Mg-Al LDH by bringing a mixed gas containing water and carbon dioxide having a concentration of 5 vol.% or more at 70 ℃ or more into contact with an anionic Mg-Al LDH produced in an acidic exhaust gas treatment using a carbonic acid type Mg-Al LDH.
Description
Technical Field
The present invention relates to a method for regenerating a carbonic acid type layered double hydroxide used for treating an acidic exhaust gas generated from a combustion facility such as a thermal power plant or an incineration facility, and an acidic exhaust gas treatment apparatus including the regeneration unit.
Background
The combustion exhaust gas generated in thermal power generation, waste incineration, and the like contains harmful acidic substances such as hydrogen chloride, sulfur oxides, and nitrogen oxides. Accordingly, the acid exhaust gas containing the acid substances is treated by various methods for removing the acid substances.
In such a method for removing acidic substances, the present applicant has proposed a method for treating acidic exhaust gas and a treating agent using a carbonic acid type mg—al layered double hydroxide (hereinafter, also referred to as mg—al LDH (Layered Double Hydroxide)) as an effective treatment technique capable of simultaneously treating and removing a plurality of acidic substances (see patent document 1).
The Mg-Al LDH is a treatment agent that can be regenerated and reused, and conventionally, as described in patent document 1, when the carbonic acid type Mg-Al LDH is used for acid exhaust gas treatment and converted into an anionic Mg-Al LDH, the used layered double hydroxide is regenerated by mixing with an aqueous carbonic acid solution.
Prior art literature
Patent literature
Patent document 1: japanese patent laid-open publication 2016-190199
Disclosure of Invention
Problems to be solved by the invention
The method of mixing the used layered double hydroxide with the carbonic acid aqueous solution as described above may be carried out in a layered double hydroxide regeneration facility provided outside the waste incineration facility. However, the following problems are presented: the labor and cost burden for transporting the used layered double hydroxide and regenerating the layered double hydroxide between the waste incineration facility and the layered double hydroxide regeneration facility, or for installing an external facility separate from the waste incineration facility, etc. is great.
In addition, when the used layered double hydroxide regeneration facility is installed in a waste incineration facility, it is necessary to install and connect a storage tank, a mixing tank, or the like for the carbonic acid aqueous solution, and the facility as a whole has to be large-scale.
The present invention has been made to solve the above-described technical problems, and an object of the present invention is to provide a method for regenerating a carbonic acid type layered double hydroxide capable of efficiently regenerating a used anionic mg—al LDH in an acid exhaust gas treatment into a carbonic acid type mg—al LDH, and an acid exhaust gas treatment facility.
Solution for solving the problem
The invention is based on the following findings: by bringing the used layered double hydroxide in the acid exhaust gas treatment into contact with a gas containing water and a predetermined amount of carbon dioxide, particularly a treated gas in the acid exhaust gas treatment, the acid exhaust gas treatment can be efficiently regenerated into a carbonic acid layered double hydroxide.
That is, the present invention provides the following [1] to [4].
[1] A method for regenerating a carbonic acid type layered double hydroxide, wherein a mixed gas containing water and carbon dioxide having a concentration of 5 vol% or more and having a temperature of 70 ℃ or higher is brought into contact with an anionic Mg-Al type layered double hydroxide produced in an acidic exhaust gas treatment using a carbonic acid type Mg-Al type layered double hydroxide to regenerate the carbonic acid type Mg-Al type layered double hydroxide.
[2] The method for regenerating a carbonic acid type layered double hydroxide according to [1], wherein the amount of water in the mixed gas is 10% or more.
[3] The method for regenerating a carbonic acid type layered double hydroxide according to [1] or [2], wherein the acid exhaust gas treatment is a treatment of acid exhaust gas generated in a combustion facility, and a treated gas obtained by removing acid gas other than the treated carbon dioxide is used as the mixed gas.
[4] An acid exhaust gas treatment device comprising: a unit (1) for performing an acidic exhaust gas treatment using a carbonic acid type Mg-Al layered double hydroxide; and a unit (2) for regenerating a carbonic acid type Mg-Al layered double hydroxide by the regeneration method described in any one of [1] to [3 ].
ADVANTAGEOUS EFFECTS OF INVENTION
According to the present invention, the used layered double hydroxide in the acid exhaust gas treatment can be regenerated into the carbonic acid layered double hydroxide in the in-plant (onsite) without requiring a large-scale facility, and the present invention is advantageous from the viewpoints of facility, labor and cost burden as compared with the regeneration treatment in the regeneration facility outside the plant (offsite).
In addition, the acid exhaust gas treatment apparatus according to the present invention can also be used to efficiently regenerate carbonic acid type layered double hydroxide.
Drawings
FIG. 1 is a schematic flow chart of an acid exhaust treatment process using an acid exhaust apparatus according to an embodiment of the present invention.
Detailed Description
The method for regenerating a carbonic acid type layered double hydroxide and a part of an acidic exhaust gas treatment apparatus according to the present invention will be described below with reference to the drawings.
[ method for regenerating carbonic acid type layered double hydroxide ]
The method for regenerating a carbonic acid type layered double hydroxide of the present invention is characterized in that: the mixed gas containing water and carbon dioxide having a concentration of 5 vol% or more and having a temperature of 70 ℃ or higher is brought into contact with anionic Mg-LDH generated in an acidic exhaust gas treatment using carbonic acid Mg-LDH, thereby regenerating carbonic acid Mg-LDH.
As described above, the regeneration treatment of the anionic mg—al LDH after the acid exhaust gas treatment is performed by the contact with the gas containing water and a predetermined amount of carbon dioxide, whereby the regeneration into the carbonic acid mg—al LDH is efficiently performed.
< carbonic acid type Mg-Al LDH >)
The carbonic acid type Mg-Al LDH is a solid with hydroxide base layer ([ Mg) 2+ 1-x Al 3+ x (OH) 2 ]) And from interlayer carbonate ions and interlayer waterAn intermediate layer of composition ([ (CO) 3 2- ) x/2 ·yH 2 O]) Nanoparticles of an alternating layered structure. And is a non-integer ratio compound as follows: the hydroxide base layer has a positive charge of x equivalent, and carbonate ions are present in the intermediate layer as anions having a negative charge that compensates for the positive charge.
The carbonic acid type mg—al LDH can take acid gases such as hydrogen chloride, sulfur dioxide, nitrogen dioxide, etc. into the layers while maintaining the hydroxide base layer. Thus, it can be suitably used for acid exhaust gas treatment for removing the acid exhaust gas.
When the carbonic acid type mg—al LDH is used for the acid exhaust gas treatment, a layered double hydroxide other than the carbonic acid type mg—al LDH, or a chemical agent other than the layered double hydroxide such as calcium hydroxide (slaked lime), calcium oxide, sodium bicarbonate (Sodium bicarbonate), sodium carbonate, dolomite hydroxide, dolomite light burned, aluminum hydroxide, aluminum oxide, magnesium hydroxide, magnesium oxide, or the like may be used in combination. Among them, from the viewpoint of efficiently regenerating and reutilizing the carbonic acid type mg—al LDH, it is preferable that the carbonic acid type mg—al LDH is not mixed with other layered double hydroxides or chemicals.
As hydrotalcite, the carbonic acid type mg—al LDH also exists as a naturally occurring clay mineral, but synthetic powders are generally used. The synthesis method is not particularly limited, and a known method (for example, the method described in patent document 1) can be used.
For example, a carbonic acid type mg—al LDH can be obtained by: magnesium nitrate (Mg (NO) 3 ) 2 ) With aluminum nitrate (Al (NO) 3 ) 3 ) The aqueous solution mixed with Mg/al=2/1 (molar ratio) was kept at pH 10.5, while being added dropwise to sodium carbonate (Na 2 CO 3 ) In an aqueous solution.
When the acid gas is taken into the interlayer, the carbonic acid mg—al LDH used in the acid exhaust gas treatment becomes an anionic mg—al LDH in which interlayer carbonate ions are exchanged for other anions derived from the acid exhaust gas such as chloride ions, sulfate ions, nitrate ions, and the like. The anionic Mg-Al LDH produced in this way does not have the ability to further remove acidic off-gases. Thus, the anionic Mg-Al LDH is regenerated into a carbonic acid type Mg-Al LDH again by anion exchange and is provided for reuse.
< Mixed gas >
In the method for regenerating a carbonic acid type layered double hydroxide of the present invention, a mixed gas containing water and carbon dioxide having a concentration of 5 vol% or more and having a temperature of 70 ℃ or higher is used to perform anion exchange of an anionic mg—al LDH of the used layered double hydroxide as an acidic exhaust gas treatment, thereby regenerating the same into a carbonic acid type mg—al LDH.
Such a regeneration method using gas contact is effective as a regeneration method for mg—al LDH to carbonic acid, compared with a conventional regeneration method using a liquid carbonic acid aqueous solution.
The mixed gas contains water and carbon dioxide with a concentration of 5% by volume or more.
Such a mixed gas containing water and carbon dioxide is used for regenerating an interlayer anion in an anionic mg—al LDH, which is derived from acid exhaust gas, into carbonate ions, and a carbonate type mg—al LDH having interlayer carbonate ions and interlayer water in the interlayer.
Further, "water" as used herein refers to water of a gas, i.e., water vapor.
The content of carbon dioxide in the mixed gas is 5% by volume or more, preferably 10% by volume to 75% by volume, more preferably 10% by volume to 30% by volume.
If the content is 10 vol% or more, the interlayer anions of the anionic mg—al LDH are efficiently desorbed and exchanged to interlayer carbonate ions, whereby the regeneration of the carbonate mg—al LDH can be performed.
The moisture content in the mixed gas is preferably 10% or more, more preferably 15% to 30%, and still more preferably 20% to 25%.
If the amount of water is 10% or more, the interlayer anions of the anionic mg—al LDH are efficiently desorbed to regenerate the carbonaceous mg—al LDH having interlayer carbonate ions and interlayer water in the interlayer.
The "moisture content" in the present invention means a moisture content corresponding to japanese industrial standard (Japanese Industrial Standards, JIS) Z8808: the volume fraction [% ] of the water vapor contained in the exhaust gas in 2013 can be measured by a method according to a method using a moisture absorption tube described in the JIS standard.
The mixed gas may also contain water and a gas other than carbon dioxide, and preferably is free of an acid gas other than carbon dioxide. The mixed gas is preferably prepared by mixing air in terms of simplicity and cost in preparing the mixed gas containing a predetermined amount of water and a predetermined amount of carbon dioxide.
The temperature of the mixed gas is set to 70 ℃ or higher, preferably 75 ℃ to 100 ℃, more preferably 80 ℃ to 90 ℃.
If the temperature is 70 ℃ or higher, the regeneration from anionic mg—al LDH to carbonic acid mg—al LDH can be efficiently performed.
Among the mixed gases, it is preferable to use a treated gas obtained by removing acid gases other than treated carbon dioxide of acid exhaust gas generated in the combustion facility.
By using the treated gas, the gas generated by the self-combustion facility can be effectively utilized, and the regeneration from the anionic Mg-Al LDH to the carbonic acid Mg-Al LDH in the factory can be performed, thereby further realizing the efficiency of the regeneration treatment.
[ acid exhaust gas treatment device ]
The acid exhaust gas treatment apparatus of the present invention is characterized by comprising: a unit (1) for performing an acidic exhaust gas treatment using a carbonic acid type Mg-Al layered double hydroxide; and a unit (2) for regenerating the carbonic acid type Mg-Al layered double hydroxide by using the regeneration method of the present invention.
According to this acid exhaust gas treatment apparatus, the regeneration of the carbonic acid type layered double hydroxide used in the acid exhaust gas treatment can be performed in the factory while the acid exhaust gas treatment is being performed.
Fig. 1 shows a flow of an acid exhaust gas treatment process using an acid exhaust gas treatment apparatus according to an embodiment of the present invention. In the acid exhaust gas treatment process flow shown in fig. 1, first, the acid exhaust gas a discharged from the fuel burning facility 10 is introduced into a layered double hydroxide container 20 containing carbonic acid type mg—alldh. Then, in the layered double hydroxide container 20, the acid exhaust gas a is brought into contact with the carbonic acid mg—al LDH to perform an acid exhaust gas treatment, and the treated gas b is sent to the exhaust duct 50 by an induction fan or the like (not shown) and is released to the atmosphere.
Further, as the acid exhaust gas a, for example, in the case where the combustion facility 10 is a waste incinerator, the following gases can be suitably used: the high-temperature exhaust gas from the incinerator body is cooled by a heat exchanger such as a boiler, and the dust and other gases are removed by a dust collector.
As the acidic exhaust gas treatment proceeds, the carbonic acid type mg—al LDH is changed to the anionic type mg—al LDH, and when the acidic exhaust gas treatment capacity is lowered, the line is switched by the switching valve V1 so that the acidic exhaust gas a is introduced into the layered double hydroxide storage container 21 separately provided. The switching valve V2 is operated, and a part of the treated gas b is introduced into the layered double hydroxide container 20 through the bypass line 40 by a fan or the like. The treated gas b, that is, the mixed gas, is brought into contact with the anionic mg—al LDH in the above-described manner to perform a regeneration treatment into the carbonic acid type mg—al LDH.
In the regeneration treatment, anions desorbed from the anionic mg—al LDH are absorbed by water (liquid) condensed by the moisture in the acid exhaust gas a, and stored in the regeneration treatment drain recovery vessel 30 in the form of the regeneration treatment drain c.
When the regeneration process is completed, the switching valves V1 and V2 are restored, and the acid exhaust process in the layered double hydroxide storage container 20 is restarted. The determination of the end of the regeneration treatment of the carbonic acid type mg—al LDH can be performed based on the concentration analysis of the anion component contained in the regeneration treatment wastewater c.
Even if the layered double hydroxide container 21 is separately provided, if the same regeneration process is performed, the layered double hydroxide container 20 and the layered double hydroxide container 21 may be alternately used by switching the line by the switching valve V1, and the acid exhaust gas treatment may be continuously and efficiently performed without stopping the flow of the acid exhaust gas a.
Examples
Hereinafter, the present invention will be described in more detail based on examples, but the present invention is not limited by the following examples.
[ test for regeneration treatment of carbonic acid type layered double hydroxide ]
According to the following preparation example 1, a chlorine type mg—al LDH (anionic type mg—al LDH sample) in which interlayer carbonate ions were replaced with interlayer chloride ions was prepared by bringing hydrogen chloride gas as an acidic exhaust gas for test into contact with carbonic acid type mg—al LDH. 20g of the chlorine type Mg-Al LDH was packed in a column made of an acrylic resin having an inner diameter of 40mm, and a regeneration treatment test was performed under each of the following conditions of examples and comparative examples.
The regeneration efficiency of the carbonic acid type layered double hydroxide was evaluated by measuring the chlorine content in mg—al LDH before and after the regeneration treatment test by ion chromatography and obtaining the desorption rate of chloride ions. The higher the desorption rate of chloride ions, the higher the regeneration efficiency from chlorine type mg—al LDH to carbonic acid type mg—al LDH can be said to be.
Preparation example 1
A column made of an acrylic resin having an inner diameter of 40mm was filled with a carbonic acid type Mg-Al LDH ("Qiao Wode (KYOWARD) (registered trademark) 500PL", manufactured by Co., ltd., synthetic hydrotalcite), and hydrogen chloride gas was introduced into the air to circulate the hydrogen chloride-containing gas having a hydrogen chloride concentration of about 1000ppm at 100℃until hydrogen chloride was detected at the outlet of the column, thereby obtaining a chlorine type Mg-Al LDH.
Further, the formation of chlorine type mg—al LDH was confirmed by powder X-ray diffraction measurement and ion chromatography.
Example 1
The regeneration treatment test was performed by introducing water and carbon dioxide into air and allowing a mixed gas having been adjusted to a water content of 20%, a carbon dioxide concentration of 30% by volume, and a temperature of 80 ℃ to flow through the column filled with the chlorine type mg—alldh for 8 hours.
The desorption rate of chloride ions in the regeneration treatment test was 96%.
Comparative example 1
Carbon dioxide was introduced into the air, and a mixed gas at room temperature (25 ℃) adjusted to a carbon dioxide concentration of 30% by volume was circulated in the column filled with the chlorine type mg—alldh for 24 hours to conduct a regeneration treatment test.
The desorption rate of chloride ions in the regeneration treatment test was 6%.
Comparative example 2
Water was introduced into the air, and a mixed gas having a water content of 20% and a temperature of 80 ℃ was circulated in the column filled with the chlorine type mg—alldh for 8 hours to perform a regeneration treatment test.
The desorption rate of chloride ions in the regeneration treatment test was 37%.
Comparative example 3
Carbon dioxide was introduced into the air, and a mixed gas of 80 ℃ adjusted to a carbon dioxide concentration of 30% by volume was circulated in the column filled with the chlorine type mg—alldh for 8 hours to conduct a regeneration treatment test.
The desorption rate of chloride ions in the regeneration treatment test was 30%.
From the test results of the examples and comparative examples, it was confirmed that the anionic mg—al LDH was brought into contact with a gas containing water and a predetermined amount of carbon dioxide, thereby efficiently regenerating the anionic mg—al LDH.
Description of the reference numerals
10: combustion facility
20. 21: layered double hydroxide container
30: drainage recovery container for regeneration treatment
40: bypass line
50: exhaust duct
V1, V2: switching valve
a: acid bleed
b: post-treatment gas
c: regeneration treatment drain
Claims (3)
1. A method for regenerating a carbonic acid type layered double hydroxide, comprising bringing a mixed gas containing water and carbon dioxide having a concentration of 5 vol.% or more at 70 ℃ or more into contact with an anionic Mg-Al layered double hydroxide converted from the carbonic acid type Mg-Al layered double hydroxide in an acidic exhaust treatment using the carbonic acid type Mg-Al layered double hydroxide, and exchanging interlayer anions of the anionic Mg-Al layered double hydroxide for interlayer carbonate ions,
the acid exhaust gas treatment is a treatment of acid exhaust gas generated in a combustion facility, the treated gas is obtained by removing acid gas other than carbon dioxide, the treated gas is used as the mixed gas,
the water refers to water of gas, namely water vapor.
2. The method for regenerating a carbonic acid type layered double hydroxide according to claim 1, wherein the amount of water in the mixed gas is 10% or more.
3. An acid exhaust gas treatment device comprising means for: a unit (1) for performing an acidic exhaust gas treatment using a carbonic acid type Mg-Al layered double hydroxide; and a unit (2) for regenerating a carbonic acid type mg—al layered double hydroxide by the regeneration method according to claim 1 or 2.
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| JP2019223146A JP6898627B2 (en) | 2019-12-10 | 2019-12-10 | Carbonated layered double hydroxide regeneration method and acidic exhaust gas treatment equipment |
| JP2019-223146 | 2019-12-10 | ||
| PCT/JP2020/009329 WO2021117261A1 (en) | 2019-12-10 | 2020-03-05 | Method for regenerating carbonate-type layered double hydroxide and acidic exhaust gas treatment facility |
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| JP2017078014A (en) * | 2015-10-20 | 2017-04-27 | テイカ株式会社 | Layered double hydroxide in which hydrogen phosphate ion is intercalated, flame retardant containing layered double hydroxide, flame-retardant synthetic resin composition, and method for producing layered double hydroxide |
| CN107649093A (en) * | 2016-07-26 | 2018-02-02 | 中国石化扬子石油化工有限公司 | A kind of renovation process of aromatic hydrocarbon refining carclazyte |
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| KR20220104675A (en) | 2022-07-26 |
| JP2021090913A (en) | 2021-06-17 |
| CN114375220A (en) | 2022-04-19 |
| JP6898627B2 (en) | 2021-07-07 |
| TW202122349A (en) | 2021-06-16 |
| WO2021117261A1 (en) | 2021-06-17 |
| TWI809256B (en) | 2023-07-21 |
| KR102511218B1 (en) | 2023-03-16 |
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