KR101766861B1 - A Complex Adsorbent To Treat Ethyanolamine And Preparation Method Of The Same - Google Patents

A Complex Adsorbent To Treat Ethyanolamine And Preparation Method Of The Same Download PDF

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KR101766861B1
KR101766861B1 KR1020160026397A KR20160026397A KR101766861B1 KR 101766861 B1 KR101766861 B1 KR 101766861B1 KR 1020160026397 A KR1020160026397 A KR 1020160026397A KR 20160026397 A KR20160026397 A KR 20160026397A KR 101766861 B1 KR101766861 B1 KR 101766861B1
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mixture
mixing
slag
zeolite
composite adsorbent
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KR1020160026397A
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Korean (ko)
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이민희
김종규
김병렬
황영길
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주식회사 에스비이앤이
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/16Alumino-silicates
    • B01J20/18Synthetic zeolitic molecular sieves
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28004Sorbent size or size distribution, e.g. particle size
    • B01J20/28007Sorbent size or size distribution, e.g. particle size with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28014Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
    • B01J20/28016Particle form
    • B01J20/28019Spherical, ellipsoidal or cylindrical
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/3007Moulding, shaping or extruding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/3021Milling, crushing or grinding
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/30Processes for preparing, regenerating, or reactivating
    • B01J20/3042Use of binding agents; addition of materials ameliorating the mechanical properties of the produced sorbent
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/28Treatment of water, waste water, or sewage by sorption
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/38Organic compounds containing nitrogen

Abstract

A composite adsorbent for treating ethanolamine and a process for producing the same are provided. The complex adsorbent for treating ethanolamine and the method for its preparation are composed of a mixture obtained by mixing a certain percentage of active ingredients, such as post mortem slag, slag slag and low slag, and the specific production method thereof is a method in which slag, Mixing step; A pulverization step of processing the mixture made of waste rubber, steel slag, and low-temperature circuit so as to have a particle size of 5 mm or less; An acid purification step of processing the mixture to remove heavy metals and harmful components contained in the mixture; A dehydrating step for removing moisture contained in the mixture; A zeolite-forming step of processing the dehydrated mixture to proceed with zeolitization; And a drying step of drying the zeolite-developed mixture, thereby efficiently treating ethanolamine at low cost, and a process for producing the same.

Description

Technical Field [0001] The present invention relates to a complex adsorbent for treating ethanolamine,

The present invention relates to a complex adsorbent for ethanolamine treatment and a method for producing the same. More specifically, the present invention relates to a method for producing ethanolamine, which is a toxic substance that induces respiratory diseases upon contact with eyes, skin, respiratory or lungs, To a complex adsorbent for the treatment of ethanolamine for effective treatment and a process for producing the same.

Ethanolamine is widely used as a corrosion inhibitor that suppresses sludge deposition, an absorbent used to remove CO 2 or H 2 S from the refinery, and a secondary system pH adjuster for nuclear power plants.

Ethanolamine is a substance obtained by replacing the hydrogen atom of ammonia with a hydroxyethyl radical, and there are three kinds such as monoethanolamine, diethanolamine and triethanolamine. These organic chemicals are mainly used as absorbents for absorbing acidic components in the oil and gas industry, and they are also used as emulsifiers for household products and industrial products, such as salt compounds and fatty acid-bonded compounds.

Especially recently, it has a higher basicity than ammonia, and its pH can be controlled by a small amount. It has proved to be excellent in corrosion control and is used as an alternative to ammonia.

However, the increase of chemical oxygen demand (COD) and total nitrogen (TN) of effluent water produced by wastewater after ethanolamine application causes serious environmental problems.

Nuclear power plants are diluted in place of ethanolamine (ETA) to reduce COD and TN concentrations in effluent. Therefore, much research has been conducted to satisfy the COD and TN effluent standards in the Water Environment Protection Law.

The currently used ethanolamine treatment methods include resin regeneration, adsorption, biological treatment, and electrolytic treatment, but they are unsatisfactory in terms of effective and economical treatment of high concentration of ethanolamine.

Korean Patent No. 10-0670629 entitled " Electrolytic Treatment Apparatus and Treatment Method for Removing Organic Substances and Nitrogen in a Multiple Desalting Plant Reforming Waste Water "discloses that organic substances in regenerated wastewater containing ethanolamine discharged from a multiple desalination plant and nitrogen Which is an effective method for treating ethanolamine regeneration wastewater by electrolysis with improved electrolysis operation conditions and types such as the shape and installation method of electrode plates and the use of catalysts.

However, Korean Patent Registration No. 10-0670629 has a problem in that excessive processing cost, difficult maintenance, and aged deterioration of the equipment occur.

In order to effectively treat wastewater containing high concentration of ethanolamine, a treatment technique employing an adsorbent or a catalyst such as activated carbon or natural zeolite having a high specific surface area and an active region and an ion exchange function is used. In particular, natural zeolites with high cation exchange capacity (CEC) are very effective to treat ethanolamine present in cationic form when pH is below 9.4.

However, adsorbing catalysts such as activated carbon and natural zeolite have a high production cost and are economically disadvantageous for completely treating ethanolamine.

In addition, in Korean Patent No. 10-0383362 entitled " Method for producing artificial zeolite "and Korean Patent No. 10-0541776 entitled" Method for producing artificial zeolite from fly ash ", fly ash is used as a main raw material and artificial zeolite Discloses a technique relating to a method for manufacturing a semiconductor device. However, the artificial zeolite prepared through Korean Patent No. 10-0383362 and Korean Patent No. 10-0541776 has not been produced for the purpose of treating a refractory material having high COD and TN concentration such as ethanolamine, There is a problem that the treatment efficiency is not high.

Korean Patent No. 10-0670629 Korean Patent No. 10-0383362 Korean Patent No. 10-0541776

SUMMARY OF THE INVENTION The present invention has been made in view of the above-mentioned conventional problems, and an object of the present invention is to provide a composite adsorbent for effectively treating ethanolamine, which is a toxic substance, by treating ethanolamine treatment for making pesticide, steel slag and bottom ash And a method for producing the same.

Another object of the present invention is to provide a coal-fired power plant using a coal-fired coal as an active ingredient of a composite adsorbent, a waste slurry used as a waste in a coal mine, a blast furnace slag generated when a pig iron is made in a steel mill, And to provide a composite adsorbent for ethanolamine treatment capable of obtaining a high efficiency treatment effect at a low cost by producing industrial waste such as bottom ash that is generated and a method for producing the same.

The composite adsorbent for the treatment of ethanolamine of the present invention for solving the above-mentioned problems is composed of a mixture obtained by mixing mortar, steel slag and undercook as an active ingredient at a certain ratio.

In the present invention, the mixture may be mixed at a ratio of 60 wt% to 75 wt% of post-treated gypsum, 20 wt% to 30 wt% of low-temperature slag, and 5 wt% to 10 wt% of steel slag.

In the present invention, the particle size of the mixture composed of the calcined stone, the undercook, and the steel making slag may be 5 mm or less.

In the present invention, the mixture may purify heavy metals and harmful components through an acid purification process.

In the present invention, the acid refining step may be performed by mixing an alkaline aqueous solution with the mixture, heating the mixture to 75 to 95 DEG C, adding hydrochloric acid to adjust the pH to 4 or less, and further heating the mixture for 150 to 180 minutes have.

In the present invention, the mixture may be subjected to a zeolitization process.

In the present invention, the zeolitization is performed by mixing an alkaline aqueous solution and hydrochloric acid to the mixture to adjust the pH to 11 to 13, and stirring the mixture at 90 to 120 ° C for 2 to 5 hours .

In the present invention, the alkaline aqueous solution may be a solution of any one of sodium hydroxide (NaOH), potassium hydroxide (KOH) and calcium hydroxide (CaOH 2 ).

According to another aspect of the present invention, there is provided a method of preparing a composite adsorbent for ethanolamine treatment, comprising: mixing a slag, a slag, and a slag; A pulverization step of processing the mixture made of waste rubber, steel slag, and low-temperature circuit so as to have a particle size of 5 mm or less; An acid purification step of processing the mixture to remove heavy metals and harmful components contained in the mixture; A dehydrating step for removing moisture contained in the mixture; A zeolite-forming step of processing the dehydrated mixture to proceed with zeolitization; And a drying step of drying the zeolite-developed mixture.

In the present invention, in the mixing step, the mixing ratio of the post mortem slurry, the under slurry and the steel slug is comprised of 60 wt% to 75 wt% of low molecular weight slurry: 20 wt% to 30 wt% of low slag and 5 wt% to 10 wt% .

In the present invention, the acid-refining step may be performed by mixing an alkaline aqueous solution with the mixture, heating the mixture to 75 to 95 DEG C, and then adding hydrochloric acid to adjust the pH to 4 or less and further heating for 150 to 180 minutes .

In the present invention, the zeolite-forming step may be performed by mixing an alkaline aqueous solution and hydrochloric acid to the mixture, adjusting the pH to 11 to 13, and stirring the mixture at 90 to 120 ° C for 2 to 5 hours.

In the present invention, the alkaline aqueous solution may be a solution of any one of sodium hydroxide (NaOH), potassium hydroxide (KOH) and calcium hydroxide (CaOH 2 ).

In the present invention, the drying may be performed by heating the mixture to 40 to 50 ° C.

In the present invention, the composite adsorbent prepared through the drying step is mixed with 2 to 5% by weight of bentonite (inorganic binder) and 3 to 7% by weight of cellulosic (organic binder And a pelletizing step of mixing and molding the remainder with water and a composite adsorbent.

Industrial Applicability According to the present invention, it is possible to reduce the environmental pollutant load by recycling wastes by producing a composite adsorbent that efficiently treats ethanolamine as an effective ingredient, such as waste lime, steel slag, and infertile, which are waste industrial wastes, It is possible to realize a high-efficiency processing effect.

In addition, the composite adsorbent produced by the present invention can effectively treat ethanolamine causing high concentrations of COD and TN, thereby preventing water pollution when discharged water is released into an aquatic ecosystem.

FIG. 1 is an XRD (X Ray Diffraction) graph for comparing crystal phases according to hydrothermal reaction conditions in a zeolite-forming process according to an embodiment of the present invention.
2 is a photographic image for comparing the appearance of a composite adsorbent and a natural zeolite according to an embodiment of the present invention.
3 is an XRD graph for comparing the crystalline phases of composite adsorbent and natural zeolite according to one embodiment of the present invention.
4 is a graph for comparing ethanolamine treatment efficiency between a complex adsorbent and another adsorbent according to an embodiment of the present invention.
FIG. 5 is a flowchart illustrating a process for producing a composite adsorbent according to an embodiment of the present invention.
Figure 6 is a schematic diagram illustrating the principle of composite adsorbent production according to one embodiment of the present invention.

The composite adsorbent for the treatment of ethanolamine according to the present invention contains an active ingredient such as post mortem, steel slag and underfill.

Silicone and aluminum are a basic constituent of zeolite and contain a large amount of inorganic substances having a wide specific surface area and porous property.

The steelmaking slag contains at least 20% of silicic acid and aluminum as a by-product in the production of pig iron in a steel mill, and particularly contains ammonia (MgO) and phosphoric acid (P 2 O 5 ) Helps to remove.

It is a by-product from a coal-fired thermal power plant. It is a material produced in a furnace with a high calcination temperature of 800 ° C or higher. Therefore, it has a high carbon content and a homogeneous inorganic component, Do.

The composite adsorbent for the treatment of ethanolamine according to the present invention is composed of a mixture of 60 wt% to 75 wt% of pumice stone, 20 wt% to 30 wt% of low-temperature slag, and 5 wt% to 10 wt% of steel slag.

Here, the active ingredients of the composite adsorbent, such as pumice stone, steel slug, and inferiority, have a uniform particle size. In the mixing ratio of the mixture, at least 60% by weight should be mixed in the case of waste slag, and at least 5% by weight should be maintained in case of steel slag, so that the ammonia component contained in the waste water can be easily removed. In addition, the final particle size of the mixture must be shrunk to 5 mm or less before the zeolitization process is properly performed.

When menopause seat at least 60 wt% are mixed to be sure, because the 20~35wt% menopause seats alumina (Al 2 O 3) components that are configured to most shale, silica (SiO 2) component is 40~60wt%, The amount of the iron oxide (Fe 2 O 3 ) component is 2 to 10 wt%, K 2 O + Na 2 O 3 to 5 wt%, CaO + MgO 3 to 5 wt% It is composed of non-crystalline aluminosilicate. Therefore, when heated in an alkaline state, it is transformed into a zeolite type having excellent cation exchange capacity (CEC), and thus has the ability to easily adsorb ammonia in the water, and the ammonia component in the water has the highest removal efficiency , At least 60 wt% should be mixed with steel slag and low slag.

In the case of steelmaking slug, it is used as a crystal of struvite crystallization reaction to remove the remaining ammonia component in the alkaline state. It shows the highest ammonia removal rate when the mixed injection amount is 5 ~ 10wt%, and it shows similar result to 5wt% even when injecting more than 10wt%, so that high treatment efficiency can not be expected even when a large amount of ammonia is mixed. On the other hand, the crystallization does not occur at all when injected at 5 wt% or less.

At least 20 to 30% by weight should be maintained in the case of low boiling water because it is produced in a furnace with a high calcination temperature of 800 ° C or higher. Therefore, it has porosity due to high carbon content and homogeneous mineral content. Other substances have the ability to adsorb easily. Therefore, the composite adsorbent prepared at the ratio of mixed composition ratio: low-slung: steel slug = 60~75 wt%: 20~30 wt%: 5~10 wt% shows the highest efficiency for removing ethanolamine in water.

The mixture of the active ingredients of the present invention is purified through acid purification to purify heavy metals and harmful components. In the acid purification process, the mixture is mixed with an alkaline aqueous solution, heated at 75 to 95 ° C, Adjusting the concentration to 4 or less, and heating it for 150 to 180 minutes.

Further, the mixture comprising the active ingredient of the present invention is subjected to a zeolitization process. The zeolitization is carried out by mixing the mixture with an alkaline aqueous solution and hydrochloric acid to adjust the pH to 11 to 13 and heating the mixture at 90 to 120 ° C for 2 to 5 hours while stirring. it is possible to produce composite adsorbents having cation exchange ability only when they are prepared in a high alkali state as in the case of pH 11 to 13. The hydrothermal reaction at 90 to 120 캜, Zeolite formation is possible using saturated steam. The agitation time of 2 to 5 hours is the most suitable reaction time for the mixed constituents to be zeolitized.

In the acid purification process and the zeolite formation process, all the alkaline aqueous solutions can be applied. In the embodiment of the present invention, any one of sodium hydroxide (NaOH), potassium hydroxide (KOH) and calcium hydroxide (CaOH 2 ) .

FIG. 1 is an XRD (X Ray Diffraction) graph for comparing crystal phases according to hydrothermal reaction conditions in a zeolite-forming process according to an embodiment of the present invention.

Referring to FIG. 1, hydrothermal reaction should be performed for at least 2 hours in the zeolitization process. Otherwise, the produced composite adsorbent exhibits a non-crystal form such as a graph of XRD (see FIG. 1A) and does not exhibit functions such as adsorption or ion exchange. When a hydrothermal reaction of 2 hours or more is carried out, a peak close to the standard sample (Bragg pattern appearing in the crystalline material) as shown in the graph of XRD (see FIG. 1B) is displayed and has a function as an adsorption or ion exchange catalyst .

2 is a photographic image for comparing the appearance of a composite adsorbent and a natural zeolite according to an embodiment of the present invention. The composite adsorbent according to the embodiment of the present invention was prepared by mixing at least 60 wt% of slag and at least 5 wt% of steel slag.

Referring to Fig. 2, the appearance of the composite adsorbent (a) of the present invention shows a color and a shape similar to the appearance of the natural zeolite (b).

3 is an XRD graph for comparing the crystalline phases of composite adsorbent and natural zeolite according to one embodiment of the present invention. The composite adsorbent according to the embodiment of the present invention was prepared by mixing at least 60 wt% of slag and at least 5 wt% of steel slag.

Referring to FIG. 3, it can be seen that the XRD pattern of the composite adsorbent (a) of the present invention is similar to the XRD pattern of natural zeolite (b).

Comparative Example  One

In order to evaluate the efficiency of ethanolamine treatment in water, the composite adsorbent according to the present invention and the currently marketed natural zeolite, artificial zeolite and powder activated carbon were injected into raw water in which ethanolamine was dissolved to compare and evaluate respective treatment efficiencies .

At this time, the initial COD concentration of raw water is 1200 mg / L and the initial TN concentration is 350 mg / L.

4 is a graph for comparing ethanolamine treatment efficiency between the composite adsorbent of the present invention and other adsorbents.

Referring to FIG. 4, when the natural zeolite, the artificial zeolite and the powder activated carbon were respectively injected, the COD showed a good treatment efficiency of about 75 to 85%, but the TN showed a very low treatment efficiency of about 35 to 55% . However, when the composite adsorbent of the present invention was injected, the COD provided a treatment efficiency of 90% or more, and the TN provided a treatment efficiency of 80% or more.

According to the present invention, the composite adsorbent using the slag and the slurry of the present invention can effectively treat TN as well as COD of high concentration of ethanolamine due to high adsorption power and ion exchange ability, and is applied to waste water containing ethanolamine It is used as adsorbent with high treatment efficiency.

FIG. 5 is a flow chart showing a process for producing a composite adsorbent according to an embodiment of the present invention, and FIG. 6 is a schematic view showing a principle of producing a composite adsorbent according to an embodiment of the present invention.

5 and 6, a method for producing a complex adsorbent for treating ethanolamine according to the present invention comprises: a mixing step (S10) of mixing a slag of manure, a slurry, and a steel slag at a predetermined ratio; A pulverization step (S20) of processing the mixture made of waste rubber, steel slag, and low-temperature circuit to have a particle size of 5 mm; An acid purification step (S30) of processing the mixture to remove heavy metals and harmful components contained in the mixture; A dehydrating step (S40) for removing water contained in the mixture; A zeolite-forming step (S50) of processing the dehydrated mixture to proceed with zeolitization; And a drying step (S60) of drying the mixture in which zeolite formation has proceeded.

In order to produce the composite adsorbent of the present invention, a roll mill is used to crush the pellets so as to have a diameter of 10 to 30 mm in order to obtain uniform and uniform powdered powder. The reason why the particle size is 10 ~ 20mm is the most suitable size for zeolite formation by hydrothermal reaction at 90 ~ 120 ℃.

Subsequently, the slurry of the calcined stone and the lower particles crushed by a roll mill is mixed with a steel sludge composed of a particle size of 10 to 20 mm.

In the mixing step (S10), the menstruum, the undercooking and the steelmaking slag are mixed at a certain ratio. The specific mixing ratio is 60% by weight to 75% by weight of the above gypsum: 20% by weight to 30% by weight of the lower phase and 5% by weight to 10% by weight of the steel slag.

In the mixing step (S10), the blended slag, undercooked slag, and steel slag mixed is processed to have a particle size of 5 mm or less through a pulverization step (S20). Processing such that the mixture has a particle size of 5 mm or less is implemented through a rotary impact shredder. Here, when the particle size of the mixture is larger than 5 mm, the zeolite formation step (S50) for proceeding the zeolitization of the mixture is not smoothly performed.

The mixture having a particle size of 5 mm or less through the decoloration step (20) removes the heavy metals and harmful components contained therein through the acid purification step (S30). The acid refining step (S30) is performed by mixing an alkaline aqueous solution to the mixture, heating the mixture to 75 to 95 DEG C, and then adding hydrochloric acid to adjust the pH to 4 or less and further heating the mixture for 150 to 180 minutes.

The mixture in which the heavy metal and harmful components contained in the mixture are removed through the acid cleaning step (S30) removes the moisture contained in the mixture in the acid cleaning step (S30) through the dehydration step (S40). At this time, the dehydration step (S40) is performed through a filter press dehydrator.

The water-removed mixture through the dewatering step (S40) is converted into a zeolite by proceeding zeolitization through a zeolite-forming step (S50). The zeolite-forming step (S50) is performed by mixing an alkaline aqueous solution and hydrochloric acid to the mixture, adjusting the pH to 11 to 13, and stirring the mixture at 90 to 120 ° C for 2 to 5 hours.

In the present invention, sodium hydroxide (NaOH), potassium hydroxide (KOH) and calcium hydroxide (CaOH 2 ) can be used in the acid cleaning step (S30) and the zeolite formation step (S50) It is preferable to apply any one of the solutions.

The mixture in which the zeolite has been formed through the zeolite-forming step (S50) is in the form of a fine powder having a pale grayish color. The mixture is heated to 40 to 50 ° C. through a drying step (S60) to be a composite adsorbent. The heating of the mixture in the drying step (S60) is implemented through an electric oven.

Meanwhile, the composite adsorbent produced through the drying step (S60) may be further subjected to a pelletizing step (S70) to produce a composite adsorbent in a spherical shape or a pellet shape.

The pelletizing step S70 may be carried out by mixing 2 to 5% by weight of bentonite (inorganic binder) and 3 to 7% by weight of cellulose (organic binder) with respect to the total weight of water and a composite adsorbent Molding process.

Thus, the composite adsorbent for the treatment of ethanolamine of the present invention and the method for producing the same can produce a composite adsorbent that efficiently treats ethanolamine as an effective ingredient, such as waste lime, slag and slag, which are industrial waste, So that a high-efficiency processing effect can be realized.

S10: mixing step S20: pulverization step;
S30: acid purification step S40: dehydration step;
S50: zeolite-forming step S60: drying step

Claims (11)

delete delete delete delete A mixing step of mixing the post mortem slurry, the low slurry and the steel slag;
A pulverization step of processing the mixture made of the above-mentioned post mortem slurry, steel slug, and lower slurry to have a particle size of 5 mm or less;
An acid purification step of processing the mixture to remove heavy metals and harmful components contained in the mixture;
A dehydrating step of removing moisture contained in the mixture;
A zeolite-forming step of processing the dehydrated mixture to proceed with zeolitization; And
And drying the mixture in which zeolite formation has proceeded. ≪ RTI ID = 0.0 > 11. < / RTI >
6. The method of claim 5,
The composite adsorbent for treating ethanolamine according to claim 1, wherein the mixing ratio of the gypsum, the underfill and the steel slag in the mixing step is 60 to 75% by weight of pumped gypsum, 20 to 30% by weight of low gypsum and 5 to 10% Manufacturing method
6. The method of claim 5,
The acid-
Mixing the above mixture with an alkaline aqueous solution, heating the mixture to 75 to 95 캜, and then adding hydrochloric acid to adjust the pH to 4 or less and further heating the mixture for 150 to 180 minutes. .
6. The method of claim 5,
The zeolite-
Mixing the aqueous mixture with an alkaline aqueous solution and hydrochloric acid to adjust the pH to 11 to 13 and stirring the mixture at 90 to 120 ° C for 2 to 5 hours while heating.
9. The method according to any one of claims 7 to 8,
Wherein the alkaline aqueous solution is a solution of any one of sodium hydroxide (NaOH), potassium hydroxide (KOH) and calcium hydroxide (CaOH 2 ).
6. The method of claim 5,
The drying step comprises:
Lt; RTI ID = 0.0 > 40 C < / RTI > to < RTI ID = 0.0 > 50 C. < / RTI >
6. The method of claim 5,
Wherein the composite adsorbent produced through the drying step further comprises a pelletizing step of mixing and molding a binder to produce the composite adsorbent in the form of spheres or pellets. .
KR1020160026397A 2016-03-04 2016-03-04 A Complex Adsorbent To Treat Ethyanolamine And Preparation Method Of The Same KR101766861B1 (en)

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EP4079721A1 (en) * 2021-04-21 2022-10-26 Givaudan SA Process for the isolation of amines

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4079721A1 (en) * 2021-04-21 2022-10-26 Givaudan SA Process for the isolation of amines
WO2022223659A1 (en) * 2021-04-21 2022-10-27 Givaudan Sa Process for the isolation of amines

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