KR101833775B1 - Method for preparing porous sorbent for sewagne sludge incineration gas - Google Patents

Method for preparing porous sorbent for sewagne sludge incineration gas Download PDF

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KR101833775B1
KR101833775B1 KR1020150104630A KR20150104630A KR101833775B1 KR 101833775 B1 KR101833775 B1 KR 101833775B1 KR 1020150104630 A KR1020150104630 A KR 1020150104630A KR 20150104630 A KR20150104630 A KR 20150104630A KR 101833775 B1 KR101833775 B1 KR 101833775B1
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South Korea
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sewage sludge
absorbent
slurry
foaming
combustion gas
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KR1020150104630A
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Korean (ko)
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KR20170011659A (en
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한요셉
김현중
최시영
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전북대학교산학협력단
한국과학기술원
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Priority to KR1020150104630A priority Critical patent/KR101833775B1/en
Priority to PCT/KR2015/013818 priority patent/WO2017014376A1/en
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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
    • B01D53/14—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 by absorption
    • 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
    • B01D53/14—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 by absorption
    • B01D53/1456—Removing acid components
    • B01D53/1481—Removing sulfur dioxide or sulfur trioxide
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F11/00—Treatment of sludge; Devices therefor
    • C02F11/10—Treatment of sludge; Devices therefor by pyrolysis
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
    • F23G7/00—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals
    • F23G7/06—Incinerators or other apparatus for consuming industrial waste, e.g. chemicals of waste gases or noxious gases, e.g. exhaust gases
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2252/00—Absorbents, i.e. solvents and liquid materials for gas absorption
    • B01D2252/10—Inorganic absorbents
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F23—COMBUSTION APPARATUS; COMBUSTION PROCESSES
    • F23G—CREMATION FURNACES; CONSUMING WASTE PRODUCTS BY COMBUSTION
    • F23G2209/00—Specific waste
    • F23G2209/12—Sludge, slurries or mixtures of liquids

Abstract

Mixing the lime powder obtained from the slaked lime or limestone with water and then milling to prepare a slurry; Mixing and foaming the foaming agent in the slurry; Mixing the foamed solution with a gelation solution to induce gelation to form a spherical solid; And calcining the molded spherical solid body. The method of manufacturing a porous spherical absorbent for sewage sludge combustion gas according to claim 1,

Description

FIELD OF THE INVENTION [0001] The present invention relates to a porous sorbent for sewage sludge combustion gas,

The present invention relates to a porous spherical sorbent for manufacturing sewage sludge combustion gas, and more particularly, to a porous spherical sorbent preparation method capable of simultaneously removing sulfur oxide, fine dust and heavy metals from sewage sludge combustion gas.

The SO 2 removal method included in the combustion gas generated by the incineration of sewage sludge is divided into a dry method and a wet method. The wet method absorbs gaseous sulfur dioxide (SO 2 ) by using water, an alkaline solution or a slurry. The advantage of the wet method is that the reaction rate is high and it is possible to remove SO 2 and fine dust simultaneously. However, secondary pollutants are generated frequently, energy loss due to waste gas treatment is large, and further corrosion of the apparatus is severe, and the initial installation cost is relatively large compared to the dry method.

In the case of the dry method, there are few secondary pollutants, low initial installation cost and economical operation cost. However, a large amount of unreacted SO 2 is generated even when SO 2 is removed through the injection of a fine neutralizing agent into the incinerator. Install a dry processing facility on the front of the bag filter or install a cleaning tower at the back of the bag filter to remove residual SO 2 . That is, the SO 2 removal efficiency is relatively low. Further, the scattered particulate absorbent may be generated as an additional fine dust and become a secondary pollutant. Therefore, if the economical dry method is applied, it will be very suitable in the treatment of flue gas by incineration of sewage sludge if it is excellent in terms of removal efficiency.

On the other hand, the fine dust generated by the incineration of sewage sludge is generally generated as a fine fly ash because the sewage sludge has a uniform fine particle size. At this time, heavy metal and alkali metal particles generated at the same time are adsorbed on fly ash particles and are easily released into the atmosphere. Therefore, the concentrations of heavy metals and alkali metals are high in the generated dust. Therefore, the removal of dust generated by incineration can simultaneously remove heavy metals and alkali metals, which are secondary contaminants. Therefore, semi-dry processes (gas inflow in lime slurry or lime slurry spraying), which combine advantages of wet process and advantages of dry process, have been applied in many researches and fields. However, this semi-dry method also has some drawbacks of the wet method.

The 1996 London Convention has greatly strengthened marine emissions standards for wastes including sewage sludge, and the disposal of sewage sludge by recycling, reclamation and incineration is widely used. In Korea, about 27.18 million tons of sewage sludge was generated in 2006 and 36.53 million tons of sewage sludge was generated in 2012. Among them, incineration of sewage sludge is increasing from 16% in 2006 to 25.2% in 2012. The Ministry of Environment is expected to increase the incineration to 28% of the total sewage sludge production by 2015. Incineration has many advantages, for example, volume reduction, destruction of organic contaminants, and energy recovery. Despite the significant potential due to the incineration of sewage sludge, dioxins, SO 2 , NO x, fine dust (PM) and heavy metals are generated in the exhaust gas. Generally, SO 2 is generated during the incineration process due to high sulfur content in sewage sludge than in municipal waste. In addition, due to small particles of sewage sludge, many fine dusts are generated by incineration. Particularly, the fine dust generated by the incineration is discharged together with the adsorbed heavy metals and alkali metals. Therefore, removal of fine dust generated by incineration of sewage sludge is considered to be important from the viewpoint of removal of heavy metals and alkali metals released to the atmosphere. In addition, the sewage sludge incineration system is operated in a large number of fluidized bed incinerators because it has advantages over multiple incinerators and rotary Kiln incinerators for ease of use and fuel use. However, it has the disadvantage that fine dust is generated compared to other incineration methods. Therefore, it is necessary to treat not only SO 2 generated by incineration of sewage sludge but also fine dust effectively, and when sewage sludge can be removed simultaneously, it can have a great advantage in sewage sludge treatment from fluidized bed incineration.

The treatment methods of SO 2 and fine dust are divided into wet and dry methods. First, in the case of wet treatment, SO 2 and dust can be removed at the same time, and the reaction rate is very high. However, wastewater is generated, equipment corrosion is severe, and initial installation cost is relatively large compared to dry processing. On the other hand, dry treatment has been actively studied due to low generation of secondary pollutants and due to initial installation cost and economical operation cost. Particularly, in the dry treatment, a lime absorbent is most widely used, and waste materials such as coal fly ash and sewage sludge are mixed and used as an absorbent. In general, lime absorbents are most widely used for direct SO 2 removal in a fluidized bed furnace, and the lime and SO 2 removal reactions are as follows.

Figure 112015071873163-pat00001

Carbon dioxide is generated by the combustion reaction and occurs simultaneously with the SO 2 reaction. When limestone (CaCO 3 ) is used as an absorbent for SO 2 removal, the calcination reaction is associated with combustion and increases CO 2 production. At this time, limestone is limited in use as an absorbent for SO 2 capture. Because of the calcium sulfate (CaSO 4 ), the pores present on the surface of the sintered lime sorbent are clogged. Therefore, the activity is deteriorated due to no reaction of CaO and SO 2 present in the absorbent. As a result, the dry process using lime sorbents for SO 2 treatment at industrial sites has a disadvantage that it is less efficient than the other processes (wet process, semi-dry process). Therefore, for effective application of the lime sorbent to the sewage sludge incinerator, the SO 2 removal efficiency should be improved. Furthermore, the absorbent mainly used may be discharged in the form of particles as the unreacted absorbent itself, causing an increase in the fine dust concentration. In recent years, there have been a lot of studies on simultaneous removal of NOx and SO 2 by coating a catalyst on a bulk type porous filter, but there is insufficient research on materials capable of simultaneously removing SO 2 and fine dust and heavy metals.

SUMMARY OF THE INVENTION Accordingly, it is an object of the present invention to provide a new absorbent capable of simultaneously removing sulfur dioxide, fine dust, and heavy metals from a sewage sludge combustion gas and a method for producing the same.

In order to solve the above problems, the present invention provides a method for producing a slurry, comprising: mixing a lime powder obtained from a slaked lime or limestone with water and then milling to prepare a slurry; Mixing and foaming the foaming agent in the slurry; Mixing the foamed solution with a gelation solution to induce gelation to form a spherical solid; And calcining the molded spherical solid body. The present invention also provides a method for manufacturing a porous spherical absorbent for sewage sludge combustion gas.

In one embodiment of the present invention, in the step of producing the slurry, the lime powder is a calcium hydroxide powder, and the foaming ratio in the foaming step is 4. [

In one embodiment of the present invention, the foaming ratio is controlled through bubble concentration control in the foaming step.

The present invention also relates to a porous spherical absorbent for sewage sludge combustion gas produced by the method described above, wherein the absorbent is capable of simultaneously removing sulfur dioxide, fine dust and heavy metals from the sewage sludge. Thereby providing a spherical absorbent.

In the dry method for treating flue gas or incineration flue gas as reported previously, most of the alkaline sorbent is used as a powder state, and in particular, the dust collecting process is required in the second stage due to the powdery sorbent. Furthermore, the reaction at the solid phase has a low removal performance, and the unreacted powder can also be scattered, resulting in additional contaminants as fine dust. Accordingly, the present invention does not require an additional collection step by producing a spherical alkali absorbent having a fixed size with a high specific surface area. Moreover, it is easy to install and has low replacement cost and low operation cost, so that it has excellent price competitiveness. Lastly, not only maintaining the removal efficiency of 95% or more but also making it to have high gas permeability, it is possible to simultaneously remove fine dust and heavy metal generated by maintaining the filter performance. Accordingly, it can be used not only as a combustion gas generated in a sewage sludge incinerator, but also as an absorbent capable of simultaneously removing fine dust and heavy metals as well as effectively removing sulfur oxides contained in exhaust gas generated in an incineration plant. Therefore, it is possible to develop new absorbent which not only can not overcome the disadvantages of the previously reported alkali absorbent, but also has not been reported previously.

In addition, the most significant feature of this technology is that it has a high specific surface area and a high pore structure in producing a porous calcined sphere of several mm size, and has a new SO 2 removal performance and a new absorbent capable of simultaneously removing fine dust and heavy metals . Furthermore, in the present technology, SO 2 removal tests were conducted at actual site sewage sludge incineration sites and were maintained for more than 95% over 160 hours and achieved fine dust and heavy metal removal. In addition, it can be used as a competitive material because it has easy installation and cheap operation cost at the incinerator site due to the molding of several mm size.

1 is a view for explaining a method of producing spherical porous lime as an absorbent according to an embodiment of the present invention.
2 is a view showing an absorber and a removal scheme using an absorbent manufactured according to an embodiment of the present invention.
Figures 3 and 4 show the pore size distribution of the porous spherical calcium sorbent prepared according to the present invention and the gas permeability analysis results thereof.
FIG. 5 is a graph showing the removal performance of sulfur oxide according to the operation time by installing the developed absorbent in an actual large sewage sludge incineration plant.
Figure 6 is an analysis of the size of the dust hanging on the surface of the absorbent during the process in the incinerator plant.

Hereinafter, embodiments and examples of the present invention will be described in detail with reference to the accompanying drawings, which will be readily apparent to those skilled in the art to which the present invention pertains.

It should be understood, however, that the present invention may be embodied in many different forms and is not limited to the embodiments and examples described herein. In order to clearly illustrate the present invention, parts not related to the description are omitted, and similar parts are denoted by like reference characters throughout the specification.

Throughout this specification, when an element is referred to as "including " an element, it is understood that the element may include other elements as well, without departing from the other elements unless specifically stated otherwise.

As used herein, the terms "about," " substantially, "and the like are used herein to refer to or approximate the numerical value of manufacturing and material tolerances inherent in the stated sense, Accurate or absolute numbers are used to prevent unauthorized exploitation by unauthorized intruders of the mentioned disclosure. Also, throughout the present specification, the phrase " step "or" step "does not mean" step for.

Throughout this specification, the term "combination thereof" included in the expression of the machine form means one or more combinations or combinations selected from the group consisting of the constituents described in the expression of the machine form, And the like.

Throughout this specification, the description of "A and / or B" means "A or B, or A and B".

As described above, according to the related art, generally, in the method for removing sulfur oxide (SO2) in an exhaust gas, an alkaline removing agent is put into an exhaust gas to react and remove sulfur oxides in the exhaust gas with the alkaline removing agent. In the next step, the alkaline removing agent is collected by a dust collector Should be performed. Representative alkaline removers include limestone, quicklime, slaked lime and sodium bicarbonate. As shown in the prior art process, since the powder method is used for applying the dry method, it has a disadvantage of performing the collection at the dust collector stage and it is difficult to maintain the removal performance of 95% or more because the reaction rate is always lower than that of the wet method. Accordingly, since the present invention is manufactured to have a size of several millimeters having a certain size, it is easy to install in an existing incinerator site and recovery is also easy. Furthermore, by having a high specific surface area, the removal efficiency was improved by increasing the reaction rate between the combustion gas and the absorbent, and the gas permeability performance was improved by having a high porosity and 3-D pore structure . As a result, it is characterized as a material capable of simultaneously removing sulfur oxide generated by combustion of sewage sludge, fine dust, and heavy metals.

1 is a view for explaining a method of producing spherical porous lime as an absorbent according to an embodiment of the present invention.

Referring to FIG. 1, well-known slaked lime or limestone powder and water are mixed and then milled to prepare a slurry. Thereafter, a foaming agent is mixed into the slurry, followed by foaming, and then a gelling solution for inducing gelation in the foamed solution is mixed to form a spherical solid body. After that, it is dried and then calcined.

Example

Mix slaked lime or limestone powder with water to make slurry. At this time, the slurry concentration was 40%.

Then, the surfactant SLL (sodium lauryl sulfate) was added as a foaming agent to increase the critical micelle concentration to 4 times. In one embodiment of the present invention, the physical foaming method was used to increase the ratio of the foamed slurry to the slurry volume to 2, 3, and 4 times. Then, 6 wt% of gelated agar solution is added to the foamed slurry. Here, the gelled slurry is dropped into a 4 ° C paraffin column solution to form a spherical solid body. Thereafter, after the solid-liquid separation, the obtained spherical solid body is dried at room temperature for 24 hours. The final precipitate was calcined at 600 ° C for 1 hour to form a compact.

2 is a view showing an absorber and a removal scheme using an absorbent manufactured according to an embodiment of the present invention.

Referring to FIG. 2, it can be seen that the absorbent according to the present invention can be used in an absorption tower in an actual sewage sludge incinerator plant.

Experimental Example 1

Figures 3 and 4 show the pore size distribution of the porous spherical calcium sorbent prepared according to the present invention and the gas permeability analysis results thereof.

The results of the experiments of FIGS. 3 and 4 are summarized in Table 1 below.

Porosity, pore size, specific surface area and gas permeability of porous lime absorbent Name of material Porosity
(%) Pore size
(탆) Specific surface area
(m 2 / g) Gas permeability
(ㅧ 10 -10 m 2 ) SL-1 48 5 34.1 0.22 SL-2 55 9 45.3 0.27 SL-3 72 21 56.7 0.53 SL-4 80 130 68.5 1.12 LS-3 80 95 17.3 0.96

In the above experimental example, SL is a case where the raw material is a calcium hydroxide powder, and LS is a limestone. Also, 1, 2, 3, and 4 mean the expansion ratio, that is, the increased ratio. Here, the foaming ratio is controlled by the foaming agent concentration or the foaming time.

Referring to the above results, it was found that the gas permeability was also improved in the case of an absorbent having a large pore size.

Experimental Example 2

FIG. 5 is a graph showing the removal performance of sulfur oxide according to the operation time by installing the developed absorbent in an actual large sewage sludge incineration plant.

Referring to FIG. 5, it can be seen that the inventive SL-4 (sorbic-made sorbent) having a higher specific surface area than the LS-3 (limestone sorbent) sorbent having the same porosity has a very high It can be seen that the removal performance is maintained.

Experimental Example 3

Figure 6 is an analysis of the size of the dust hanging on the surface of the absorbent during the process in the incinerator plant.

Referring to FIG. 6, it was confirmed that the size of the initially introduced dust was less than 2 μm and accounted for more than 50% of the total volume. In particular, ultra fine dust (< 1 mu m) was confirmed to be considerably large. At this time, dust was caught on the surface of the absorbent in the absorption tower where the sulfuric acid removal was proceeding, and the size distribution was shown with time. During 60 hours, 8% or less of 2 ㎛ occupied the whole dust, but it was confirmed that fine dust was deposited more than 25% on the surface of the absorbent for 120 hours. Thus, it can be confirmed that the fine dust is removed during sulfur oxide removal.

Table 2 below shows the results of analyzing the components of the removed fine particles together with the heavy metal content present in the sewage sludge at the beginning.

Analysis of Heavy Metal Concentration Adsorbed on Surface of Developed Lime Absorbent over Time element dried sewage sludge
(mg / kg) PM collected
at 60 h (mg / kg) PM collected
at 120 h (mg / kg) As 2.0 1.1 1.3 CD 6.8 13.2 15.1 Cr 104 266 288 Cu 326 480 522 Hg 1.08 0.88 2.52 Pb 59.9 144 180 Zn 1600 2420 3245

Of particular interest from the results of Table 2 above, it has been found that heavy metals that are removed by deposition for 60 hours in addition to arsenic and mercury having properties that are not largely volatilized by heat increase, and even during 120 hours of removal, And it is confirmed that removal of heavy metals is also performed at the same time due to fine dust removal. Thus, it can be seen that the present absorbent can be removed at the same time as the removal of fine dust and the removal of heavy metals, together with the high sulfur oxide removal rate, by installing the absorbent in a simple absorber without major modification of the existing incinerator plant.

The foregoing description is merely illustrative of the technical idea of the present invention, and various changes and modifications may be made by those skilled in the art without departing from the essential characteristics of the present invention. Therefore, the embodiments disclosed in the present invention are intended to illustrate rather than limit the scope of the present invention, and the scope of the technical idea of the present invention is not limited by these embodiments. The scope of protection of the present invention should be construed according to the following claims, and all technical ideas within the scope of equivalents should be construed as falling within the scope of the present invention.

It is also to be understood that the terms such as " comprises, "" comprising," or "having ", as used herein, mean that a component can be implanted unless specifically stated to the contrary. But should be construed as including other elements. All terms, including technical and scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs, unless otherwise defined. Commonly used terms, such as predefined terms, should be interpreted to be consistent with the contextual meanings of the related art, and are not to be construed as ideal or overly formal, unless expressly defined to the contrary.

Claims (4)

Mixing the lime powder obtained from the slaked lime or limestone with water and then milling to prepare a slurry;
Mixing and foaming the foaming agent in the slurry;
Mixing the foamed solution with a gelation solution to induce gelation to form a spherical solid; And
And calcining the shaped spherical solid,
The gelation solution is an agar solution,
The ratio of foaming in the foaming step is 4 times by volume,
And a specific surface area of 68.5 m &lt; 2 &gt; / g. In the method for producing a porous spherical absorbent for combustion gas of sewage sludge,
Wherein the porous spherical absorbent for sewage sludge combustion gas produced by the method is capable of simultaneously removing sulfur dioxide, fine dust, and heavy metals from the combustion gas of the sewage sludge. delete delete A porous spherical absorbent for sewage sludge combustion gas produced by the process according to claim 1.
KR1020150104630A 2015-07-23 2015-07-23 Method for preparing porous sorbent for sewagne sludge incineration gas KR101833775B1 (en)

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KR20090083695A (en) * 2008-01-30 2009-08-04 케이씨코트렐 주식회사 Apparatus for removing sulfur oxides from exhaust gas using high reaction slaked lime for desulfurization process
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