KR20150123512A - Reformed recycled industrial by-products manufacturing system using liquid accelerated carbonation method and method thereof - Google Patents

Reformed recycled industrial by-products manufacturing system using liquid accelerated carbonation method and method thereof Download PDF

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KR20150123512A
KR20150123512A KR1020140049944A KR20140049944A KR20150123512A KR 20150123512 A KR20150123512 A KR 20150123512A KR 1020140049944 A KR1020140049944 A KR 1020140049944A KR 20140049944 A KR20140049944 A KR 20140049944A KR 20150123512 A KR20150123512 A KR 20150123512A
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carbonate
carbon dioxide
industrial
solution
liquid
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최창식
홍범의
장은석
이은실
한기보
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고등기술연구원연구조합
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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
    • B01D53/62—Carbon oxides
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone

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  • Oil, Petroleum & Natural Gas (AREA)
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  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
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Abstract

The present invention relates to a modified industrial by-product manufacturing system and a manufacturing method using the liquid-phase accelerated carbonation method, more specifically, to an industrial by-product which can be economically modified, Can reduce carbon dioxide and can reduce the environmental problems of industrial by-product recycled concrete products.
The present invention relates to a modified industrial by-product manufacturing system and a manufacturing method using the liquid-phase promoting carbonation method.
The modified industrial by-product manufacturing system and the manufacturing method using the liquid-phase accelerated carbonation method according to the present invention include: an inorganic ion elution for eluting inorganic ions in industrial by-products; A carbonate reaction tank for producing gaseous carbon dioxide as a liquid carbonate; And a transfer pump for transferring the carbonate of the carbonate reaction tank to the inorganic ion leaching tank, wherein carbonate transported by the transfer pump to the inorganic ion leaching tank reacts with a solution of inorganic ions in the inorganic ion leaching tank and a liquid- There is provided a modified industrial by-product manufacturing system using a liquid-phase promoted carbonation process that causes a carbonation reaction.

Description

BACKGROUND OF THE INVENTION 1. Field of the Invention [0001] The present invention relates to a modified by-product manufacturing system and a manufacturing method thereof,

The present invention relates to the production of industrial by-products modified by liquid phase catalytic carbonation, and more particularly, to industrial by-products generated as a by-product of coal-fired power plants, And a method of manufacturing the same.

Conventional Carbon Capture Storage (CCS) technologies are mainly used for storage of carbon dioxide, and the developed countries such as the United States, Canada and Australia have sufficient space. In Korea, however, And the storage of carbon dioxide through bedding or seabed storage causes problems such as leaks in the presence of physical changes in the storage area.

In order to overcome these drawbacks, there are stable storage and utilization methods through carbon dioxide immobilization. Direct gas-solid carbonation and indirect gas / solid carbonation Indirect gas-solid carbonation, for example. The direct gas / solid carbonation method requires a high temperature (185 to 500 ° C) and a high pressure (20 to 340 bar) in order to obtain a yield of a predetermined amount or more. In the indirect gas / solid carbonation method, , And high pressure (45 ~ 340bar), it is difficult to obtain economical efficiency compared with the conventional CO 2 capture and storage process.

In Korea, CO2 capture and storage technologies have reached a certain level, but it is difficult to secure and commercialize underground and offshore areas that can be stored in large quantities. In the case of industrial by-products and pretreatment technologies using carbon dioxide, The level of technology was low.

Industrial byproducts including construction waste such as fly ash, bottom ash, slag, and recycled aggregate can be used as construction materials and contain calcium oxide (CaO) due to the effect of burnt lime added incidentally in the generation process. This is a fundamental cause of environmental pollution by generating alkaline leachate by the formation of calcium hydroxide (Ca (OH) 2 ) upon reaction with water.

In order to solve these problems, mineral carbonation technology using carbon dioxide has been actively carried out in Korea, but it has not reached to practical use level, and most of them require high temperature and pressure as direct gas / solid carbonation technology, And the reaction time is prolonged, which is an uneconomical method. Therefore, efficient and economical minerals carbonation technology is urgently required to utilize industrial by-products and construction wastes, reduce accelerated global warming index, and use stable aggregates free from environmental problems.

Korean Patent Publication No. 10-2007-0024193 (published on Mar. 2, 2007); Method and apparatus for removing lime components from recycled aggregate using liquefied carbon dioxide gas and recycled aggregate produced thereby

DISCLOSURE Technical Problem The present invention has been made to solve the above-mentioned problems of the prior art, and it is an object of the present invention to provide a method of efficiently restoring industrial byproducts and, at the same time, fixing carbon dioxide which accelerates global warming, efficiently and stably, It is an object of the present invention to provide a modified industrial by-product manufacturing system and a manufacturing method using a modified low-temperature and low-pressure modified liquid-phase promoting carbonation method.

According to an aspect of the present invention, there is provided a method of manufacturing a semiconductor device, A carbonate reaction tank for producing gaseous carbon dioxide as a liquid carbonate; And a transfer pump for transferring the carbonate of the carbonate reaction tank to the inorganic ion leaching tank, wherein carbonate transported by the transfer pump to the inorganic ion leaching tank reacts with a solution of inorganic ions in the inorganic ion leaching tank and a liquid- There is provided a modified industrial by-product manufacturing system using a liquid-phase promoted carbonation process that causes a carbonation reaction.

In the inorganic salt introduction step, 0.1 to 1.0 M hydrochloric acid aqueous solution is added to a suspension solution containing 15 to 20% by weight of industrial by-products in terms of weight with respect to water, and stirred at a stirring speed of 300 to 1,000 rpm The inorganic ions may be eluted by stirring for 4 to 24 hours.

The carbonate reaction tank is prepared by stirring an aqueous amine solution of 20 to 30 wt% in terms of the weight of the amine with water and a gaseous carbon dioxide of 10 to 30 wt% in terms of the weight of nitrogen, .

The carbonate reaction tank may be provided with a sparger for supplying carbon dioxide to the inner side and a magnetic stirrer for stirring the aqueous amine solution and carbon dioxide on the bottom surface.

And a carbon dioxide measuring device installed to measure the concentration of carbon dioxide in the carbonate reaction tank in real time.

The transfer pump may be a metering pump for transferring the carbonate in the carbonate reaction tank to the inorganic ion leaching tank at a flow rate of 1 to 5 ml / min.

According to another aspect of the present invention, there is provided a process for producing inorganic ions, comprising: And a carbonate reaction tank for producing gaseous carbon dioxide as a liquid carbonate, wherein a solution of inorganic ions eluted from the inorganic ion leaching solution and a liquid carbonate produced in the carbonate reaction tank cause a liquid phase catalytic carbonation reaction A modified industrial by-product manufacturing system using accelerated carbonation is provided.

According to another aspect of the present invention, there is provided a method for producing an aqueous solution, comprising: preparing an aqueous solution of inorganic by-products of an industrial by-product using an aqueous hydrochloric acid solution; Preparing a conversion solution in which carbon dioxide is converted to carbonate at room temperature and atmospheric pressure using an amine aqueous solution; Preparing a modified industrial by-product by reacting the conversion solution with an aqueous solution from which the inorganic ion is eluted; And recovering the solid by dehydrating and drying the modified industrial by-product. The present invention also provides a process for producing a modified industrial by-product using the liquid-phase promoted carbonation process.

The step of preparing the aqueous solution from which the inorganic ions have been eluted is carried out by introducing 0.1 to 1.0 M hydrochloric acid aqueous solution into a suspension solution containing 15 to 20% by weight of industrial by-products in terms of weight with respect to water, The inorganic ion may be eluted by stirring at a stirring speed of 1,000 rpm for 4 to 24 hours.

The step of preparing the conversion solution comprises stirring an aqueous ammonia solution having an amine value of 20 to 30 wt% in terms of weight with respect to water and 10 to 30 wt% of gaseous carbon dioxide in terms of a weight converted to nitrogen, Carbonate can be produced.

The step of preparing the conversion solution may be determined to be a conversion solution in which the carbon dioxide is completely saturated when the initial concentration is maintained after the concentration of carbon dioxide is gradually increased.

The step of preparing the modified industrial by-products may include reacting the conversion solution and the aqueous solution from which the inorganic ions are eluted in a weight ratio of 1: 2 to 5.

According to the present invention, it is possible to economically modify industrial by-products, recycle modified industrial by-products, reduce carbon dioxide that accelerates global warming, reduce industrial waste by reducing the environmental problems of recycled concrete products .

FIG. 1 is a view showing a modified industrial by-product manufacturing system using a liquid-phase promoting carbonation method according to an embodiment of the present invention.
Figure 2 is a flow chart illustrating a method of manufacturing a modified industrial by-product using a liquid-phase enhanced carbonation process in accordance with one embodiment of the present invention.
FIG. 3 is a graph showing a result of concentration change according to supply of carbon dioxide for preparing a saturated carbonate solution in an amine aqueous solution in a modified industrial by-product manufacturing method using the liquid phase promoted carbonation method according to an embodiment of the present invention.

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. In addition, the following embodiments can be modified into various other forms, and the scope of the present invention is not limited to the following embodiments.

FIG. 1 is a block diagram showing a modified industrial by-product manufacturing system using a liquid-phase promoting carbonation process according to an embodiment of the present invention.

1, a modified industrial by-product manufacturing system 100 using a liquid-phase-enhanced carbonation process according to an embodiment of the present invention includes an inorganic-ion fork 110 for eluting inorganic ions in industrial by-products, And a carbonate solution tank 120 for producing carbon dioxide of liquid carbonate as a liquid carbonate. The solution of inorganic ions eluted from the inorganic ion application tank 110 and the liquid carbonate produced in the carbonate reaction tank 120 may be subjected to liquid- Let the reaction occur.

Here, industrial by-products are meant to include all industrial wastes such as fly ash, bottom ash and slag, as well as by-products and recycled aggregates.

The modified industrial by-product manufacturing system 100 using the liquid phase enhanced carbonation process according to an embodiment of the present invention further includes a transfer pump 130 for transferring the carbonate of the carbonate reaction tank 120 to the inorganic ion source tank 110 The carbonate transported by the transfer pump 130 to the inorganic ion leaching tank 110 can cause a liquid phase catalytic carbonation reaction with the inorganic ion solution in the inorganic ion leaching tank 110. [

The inorganic ion application tank 110 may be equipped with an agitator 111 having an impeller 112 located inside and a by-product of industrial by-products converted to weight in terms of water by 15 to 20% More specifically 0.1 to 0.5 M hydrochloric acid aqueous solution is added thereto and stirred at a stirring speed of 300 to 1,000 rpm, more specifically 300 to 500 rpm, for 4 to 24 hours, more specifically, for 6 to 8 hours by a stirrer So that the inorganic ions can be eluted.

The carbonic acid reaction tank 120 is supplied with carbon dioxide from a carbon dioxide supply unit such as a carbon dioxide gas bomb 200 through a supply line 210 and is transported through a transfer line 131 provided with a transfer pump 130, (110). In addition, a sparger 121 for supplying carbon dioxide to the inner side of the carbonate reaction tank 120 may be installed, and a magnetic stirrer 122 for stirring the aqueous amine solution and carbon dioxide, which will be described later, And a condenser 123 may be installed on the upper part.

 In the carbonate reaction tank 120, an amine aqueous solution of 20 to 30 wt% in terms of the weight of the amine converted to water, and 10 to 30 wt%, for example, 15 wt% of gaseous carbon dioxide Can be stirred to produce a carbonate. The amine may be, for example, monoethanolamine (MEA). Nitrogen can also mean nitrogen contained in the amine. In addition, the carbonic acid reaction tank 120 may be provided with a carbon dioxide measuring device 140 connected to the measuring line 141 to measure the concentration of carbon dioxide inside the tank 120 in real time.

The transfer pump 130 may be installed on the transfer line 131 extending from the carbonate reaction tank 120 to the lower portion of the inorganic ion application tank 110 and the carbonate of the carbonate reaction tank 120 may be placed in an amount of 1 to 5 ml / min, more specifically, at a flow rate of 3 to 4 ml / min to the inorganic ion application tank 110.

Figure 2 is a flow chart illustrating a method of manufacturing a modified industrial by-product using a liquid-phase enhanced carbonation process in accordance with one embodiment of the present invention.

As shown in FIG. 2, the modified industrial by-product manufacturing method using the liquid-phase promoted carbonation method according to an embodiment of the present invention includes a step (S11) of producing an aqueous solution in which inorganic ions are eluted from industrial by-products using an aqueous hydrochloric acid solution, (S12) preparing a conversion solution in which carbon dioxide is converted into carbonic acid at room temperature and atmospheric pressure using an amine aqueous solution, and preparing a modified industrial by-product by reacting the conversion solution with an aqueous solution from which inorganic ions have been eluted , And recovering the solids by dehydrating and drying the modified industrial by-products (S14).

Thus, the modified industrial by-product manufacturing method using the liquid-phase accelerated carbonation process according to an embodiment of the present invention can be applied to a process for dissolving inorganic ions in industrial by-products, a process for dissolving gaseous carbon dioxide In order to convert to the carbonate form, it is necessary to carry out a conversion reaction process using amine, and a process for reforming industrial by - product through carbonation reaction using eluted inorganic ion aqueous solution and conversion solution.

According to the step S11 of producing the aqueous solution from which the inorganic ions are eluted, the industrial byproducts are pulverized to an appropriate particle size for elution of inorganic ions such as calcium and magnesium from the industrial by-products, ), A suitable amount of water and a hydrochloric acid solution for dissolving inorganic ions are added, and the mixture is stirred at an appropriate rate for a certain period of time. Here, an aqueous hydrochloric acid solution of 0.1 to 1.0 M, for example, 0.1 to 0.5 M, is added to the suspension 110 for inorganic ions in a suspension solution containing 15 to 20% by weight of industrial by-products in terms of weight with respect to water, 111) at a stirring speed of 300 to 1,000 rpm, for example, 300 to 500 rpm for 4 to 24 hours, such as 6 to 8 hours, to elute inorganic ions.

According to the step of producing the conversion solution (S12), the amine may be a monoethanolamine (MEA) which is a primary amine for the production of the carbonate conversion solution, and the amine may be 20 to 30 wt% Carbonate can be produced by stirring gaseous carbon dioxide in an amount of 10 to 30% by weight, for example 15% by weight, in terms of the weight of the amine aqueous solution and nitrogen. The reaction in which the amine aqueous solution absorbs carbon dioxide is shown in the following reaction formula 1.

[Reaction Scheme 1]

Figure pat00001

Through the above reaction formula 1, it can be seen that the amine aqueous solution fixes the ionized carbon dioxide by chemical absorption, and the absorption of carbon dioxide by the amine aqueous solution takes place at room temperature and normal pressure. At this time, the amine aqueous solution is introduced into the carbonate reaction tank 120, and carbon dioxide is supplied to the lower part through the sparger 121 inside the carbonate reaction tank 120 and stirred using a magnetic stirrer 122 to produce carbonate do. The production time of the carbonate depends on the flow rate of the carbon dioxide, for example, it may be 10 to 15 minutes.

The degree of the reaction in the carbonate reaction tank 120 is measured through a carbon dioxide measuring device 140 capable of measuring the 0 to 100% carbon dioxide concentration at the downstream of the carbonate reaction tank 120, and the carbon dioxide concentration is measured according to the degree of the reaction. When the conversion solution is prepared, carbon dioxide is absorbed in the amine aqueous solution at the initial stage of the reaction so that the reaction proceeds, and when the exhausted concentration starts from 0 and reaches the fully saturated state according to the progress of the reaction of the amine aqueous solution, It is gradually increased to be maintained at the initially introduced concentration, which is considered to be a fully saturated carbon dioxide conversion solution, and the change of the carbon dioxide concentration in this reaction process is shown in FIG.

In this way, the fully saturated carbonate solution is transferred to the inorganic ion leaching solution 110 in which the inorganic ions of the industrial byproduct are eluted using the transfer pump 130 at a rate of 1 to 5 ml / min, more specifically 3 to 4 ml / min And the introduced carbonate solution is discharged to the lower part of the inorganic ion application tank 110 to optimize the carbonation reaction by stirring (S13). Here, the conversion solution and the aqueous solution from which the inorganic ions are eluted can be reacted at a weight ratio of 1: 2 to 5. Also, the carbonation reaction proceeds with agitation at an agitation speed of 100 to 600 rpm, more specifically 200 to 500 rpm, using an agitator 111 installed at the center of the inorganic ion application tank 110, and the degree of reaction is induced by high frequency induction Coupled plasma (ICP) and ion chromatography (IC). More specifically, a sample in the inside of the inorganic ion eluting tank 110 from which inorganic ions were eluted immediately before the introduction of the carbonate was collected, and a sample according to the reaction time was sampled to obtain calcium carbonate (CaCO 3 ) and calcium hydroxide The reaction level is analyzed by analyzing the rock side (Ca (OH) 2 ).

The modified industrial by-products can be used as an appropriately stabilized aggregate through analysis of basic aggregate evaluation items such as absorption rate, wear rate, and strength after leaching and drying (S14).

As described above, the present invention promotes the carbonation reaction by converting carbon dioxide into a carbonate form using an amine aqueous solution to proceed the carbonation reaction which has been carried out at a high temperature and a high pressure at an ordinary temperature and an atmospheric pressure, To provide modified industrial by-products.

It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit and scope of the invention. It is.

110: Induction of inorganic ions 111: Stirrer
112: Impeller 120: Carbonate Reactor
121: sparger 122: magnetic stirrer
123: condenser 130: transfer pump
131: transfer line 140: carbon dioxide measuring instrument
141: measurement line 200: carbon dioxide bombardment
210: supply line

Claims (12)

For inorganic ions to elute inorganic ions in industrial byproducts;
A carbonate reaction tank for producing gaseous carbon dioxide as a liquid carbonate; And
And a transfer pump for transferring the carbonate of the carbonate reaction tank to the inorganic ion application tank,
And a liquid phase accelerated carbonation process in which the carbonate transferred to the inorganic ion leaching tank by the transfer pump causes a liquid phase accelerated carbonation reaction with a solution of inorganic ions in the inorganic ion leaching tank. The method according to claim 1,
In the inorganic ion application,
0.1 to 1.0 M hydrochloric acid aqueous solution was added to a suspension solution containing 15 to 20% by weight of industrial by-products in terms of weight with respect to water, stirred for 4 to 24 hours at a stirring rate of 300 to 1,000 rpm by a stirrer Modified organic by-product manufacturing system using a liquid phase promoting carbonation method for eluting the inorganic ions. The method according to claim 1,
In the carbonate reaction tank,
An amine aqueous solution in which the amine is 20 to 30 wt% in terms of weight with respect to water, and a liquid phase accelerated carbonation method in which carbon dioxide is produced by stirring gaseous carbon dioxide in a concentration of 10 to 30 wt% Modified by - product manufacturing system. The method of claim 3,
In the carbonate reaction tank,
A modified sparger for supplying carbon dioxide to the inside and a magnetic stirrer for stirring an aqueous amine solution and carbon dioxide are installed on the bottom surface of the reformer. The method of claim 3,
Further comprising a carbon dioxide measuring device installed to measure the concentration of carbon dioxide in the carbonic acid reaction tank in real time. The method according to claim 1,
The transfer pump
And a metering pump for transferring the carbonate of the carbonate reaction tank to the inorganic ion leaching tank at a flow rate of 1 to 5 ml / min. For inorganic ions to elute inorganic ions in industrial byproducts; And
And a carbonate reaction tank for producing gaseous carbon dioxide as a liquid carbonate,
Wherein the solution of inorganic ions eluted from the inorganic ion leaching solution and the liquid carbonate produced in the carbonate reaction tank cause a liquid phase accelerated carbonation reaction. Preparing an aqueous solution in which inorganic ions of an industrial by-product are eluted using an aqueous hydrochloric acid solution;
Preparing a conversion solution in which carbon dioxide is converted to carbonate at room temperature and atmospheric pressure using an amine aqueous solution;
Preparing a modified industrial by-product by reacting the conversion solution with an aqueous solution from which the inorganic ion is eluted; And
Recovering the solids by dewatering and drying the modified industrial by-products;
≪ / RTI > wherein the method comprises the steps of: The method of claim 8,
The step of preparing an aqueous solution from which the inorganic ions are eluted,
0.1 to 1.0 M hydrochloric acid aqueous solution was added to a suspension solution containing 15 to 20% by weight of industrial by-products in terms of weight with respect to water, stirred for 4 to 24 hours at a stirring rate of 300 to 1,000 rpm by a stirrer Wherein the inorganic ion is eluted by a liquid phase catalytic carbonation process. The method of claim 8,
The step of preparing the conversion solution comprises:
An amine aqueous solution in which the amine is 20 to 30 wt% in terms of weight with respect to water, and a liquid phase accelerated carbonation method in which carbon dioxide is produced by stirring gaseous carbon dioxide in a concentration of 10 to 30 wt% Modified industrial by-products. The method according to claim 8 or 10,
The step of preparing the conversion solution comprises:
A method for producing a modified industrial by-product using a liquid-phase promoting carbonation method, wherein the carbon dioxide is determined to be a completely saturated conversion solution when the initial concentration of carbon dioxide is gradually increased after the increase. The method of claim 8,
The step of producing the modified industrial by-
Wherein the conversion solution and the aqueous solution from which the inorganic ion is eluted are reacted at a weight ratio of 1: 2 to 5, by the liquid-phase promoting carbonation method.
KR1020140049944A 2014-04-25 2014-04-25 Reformed recycled industrial by-products manufacturing system using liquid accelerated carbonation method and method thereof KR20150123512A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20210088954A (en) * 2020-01-07 2021-07-15 (주)유오티 An apparatus for manufacturing eco-friendly trace-element fertilizer
KR102617930B1 (en) * 2022-12-14 2023-12-26 김성중 Infiltration type rainwater reservoir system having eco-friendly water permeable concrete composition with recycled aggregates

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20210088954A (en) * 2020-01-07 2021-07-15 (주)유오티 An apparatus for manufacturing eco-friendly trace-element fertilizer
KR102617930B1 (en) * 2022-12-14 2023-12-26 김성중 Infiltration type rainwater reservoir system having eco-friendly water permeable concrete composition with recycled aggregates

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