WO2018074638A1 - Procédé de production de carbonate de calcium à haute pureté et de réutilisation de solvant au moyen de carbonatation indirecte de sous-produits industriels alcalins - Google Patents

Procédé de production de carbonate de calcium à haute pureté et de réutilisation de solvant au moyen de carbonatation indirecte de sous-produits industriels alcalins Download PDF

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WO2018074638A1
WO2018074638A1 PCT/KR2016/011896 KR2016011896W WO2018074638A1 WO 2018074638 A1 WO2018074638 A1 WO 2018074638A1 KR 2016011896 W KR2016011896 W KR 2016011896W WO 2018074638 A1 WO2018074638 A1 WO 2018074638A1
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solvent
calcium
calcium carbonate
carbon dioxide
salt
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Korean (ko)
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김명진
정성수
김다미
전준혁
조태연
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R&DB Foundation of Korea Maritime and Ocean University
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R&DB Foundation of Korea Maritime and Ocean University
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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
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/18—Carbonates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/18—Carbonates
    • C01F11/181—Preparation of calcium carbonate by carbonation of aqueous solutions and characterised by control of the carbonation conditions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/50—Carbon oxides
    • B01D2257/504—Carbon dioxide
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
    • Y02C20/00—Capture or disposal of greenhouse gases
    • Y02C20/40—Capture or disposal of greenhouse gases of CO2

Definitions

  • the present invention relates to carbon dioxide storage and high-purity calcium carbonate production using indirect carbonation of alkaline industrial by-products, and to a method for effectively reusing a solvent to elute calcium from industrial by-products and to improve calcium dissolution and carbonation efficiency.
  • Mineral carbonation one of the carbon dioxide storage technologies, is currently under research and is suitable for medium and small scale carbon dioxide storage, unlike underground storage and marine storage, which sequester large-scale carbon dioxide. Carbonate minerals produced after carbon dioxide storage are thermodynamically stable, allowing for long-term disposal and a safe way to avoid gas leakage into the atmosphere. Mineral carbonation research has been actively conducted in the United States, the United Kingdom, Finland and Japan since the first report of the concept of carbon dioxide treatment using minerals in 1990.
  • mineral carbonation can be classified into direct carbonation and indirect carbonation.
  • Direct carbonation is a single process in which carbon dioxide is directly carbonated by reacting with a raw material
  • indirect carbonation is a two or more step in which carbon or magnesium is eluted from a raw material using a solvent, and then carbon dioxide is reacted and carbonated with the eluate.
  • the present inventors use alkali industrial by-products as raw materials, reuse solvents, and produce high-purity particulate calcium carbonate in the process of storing carbon dioxide. And developed the present invention.
  • the present invention provides a method for producing calcium carbonate with high purity through carbonation reaction using alkali industrial by-products, and providing a method for reusing a solvent and storing carbon dioxide in an economical and environmentally friendly manner. do.
  • the present invention for solving the above technical problem
  • a first step of eluting calcium by adding a solvent to an alkali industrial by-product A second step of separating the calcium eluate and residual byproducts; Injecting carbon dioxide into the calcium eluate to produce calcium carbonate; A fourth step of separating the calcium eluate into calcium carbonate and a solvent after the carbonation reaction; And a fifth step of reusing the solvent of the fourth step as the solvent of the first step, wherein the solvent is a chelating reagent having a stabilization constant with calcium less than the stabilization constant of calcium carbonate.
  • the present invention for solving the other problem is the first step of eluting calcium by adding a solvent to the alkali industrial by-products; A second step of separating the calcium eluate and residual byproducts; Injecting carbon dioxide into the calcium eluate to produce calcium carbonate; A fourth step of separating the calcium eluate into calcium carbonate and a solvent after the carbonation reaction; And a fifth step of reusing the solvent of the fourth step as the solvent of the first step; wherein the solvent is an ammonium salt, the method of storing carbon dioxide through the production of high purity calcium carbonate.
  • Carbon dioxide storage method in the present invention has the advantage of generating high purity calcium carbonate can be used in the industry, minimizing waste emission by reusing the solvent, resource recycling is possible, there is an economic effect.
  • the present invention it is possible to improve the calcium dissolution efficiency by removing the surface layer of the industrial by-products by mixing the beads in the step of eluting calcium by mixing the alkali industrial by-products and the solvent, calcium using two solvents continuously
  • the dissolution reaction can improve the calcium dissolution efficiency.
  • Figure 1 shows a schematic representation of the resource recycling type carbon dioxide storage process according to the production of high-purity calcium carbonate and solvent reuse of the present invention.
  • Figure 2 shows the change in calcium concentration eluted from the PSA according to the concentration of the chelating agent according to an embodiment of the present invention.
  • Figure 3 shows the change in calcium concentration eluted from CKD according to the concentration of the chelating agent according to an embodiment of the present invention.
  • Figure 4 shows the change in calcium concentration eluted from PSA according to the concentration of ammonium salt according to an embodiment of the present invention.
  • Figure 5 shows the change in calcium concentration eluted from CKD according to the concentration of ammonium salt according to an embodiment of the present invention.
  • Figure 6 shows the XRD analysis results of calcium carbonate produced in the solvent-specific carbonation reaction according to an embodiment of the present invention.
  • the present invention relates to a high-purity calcium carbonate production and solvent reuse method using indirect carbonation of alkali industrial by-products.
  • the "high purity calcium carbonate” produced in the present invention refers to calcium carbonate having a purity of 99% or higher.
  • a first step of eluting calcium by adding a solvent to an alkali industrial by-product A second step of separating the calcium eluate and residual byproducts; Injecting carbon dioxide into the calcium eluate to produce calcium carbonate; A fourth step of separating the calcium eluate into calcium carbonate and a solvent after the carbonation reaction; And a fifth step of reusing the solvent of the fourth step as the solvent of the first step, wherein the solvent is a chelating reagent having a stabilization constant with calcium less than the stabilization constant of calcium carbonate.
  • the present invention is the first step of eluting calcium by adding a solvent to the alkali industrial by-products; A second step of separating the calcium eluate and residual byproducts; Injecting carbon dioxide into the calcium eluate to produce calcium carbonate; A fourth step of separating the calcium eluate into calcium carbonate and a solvent after the carbonation reaction; And a fifth step of reusing the solvent of the fourth step as the solvent of the first step; wherein the solvent is an ammonium salt, the method of storing carbon dioxide through the production of high purity calcium carbonate.
  • the method may further include a method of improving calcium elution efficiency by additionally adding beads to the first step to remove the surface layer of the industrial by-product.
  • the bead (bead) is characterized in that the ceramic series. Ceramic-based beads have high particle hardness and low chemical reactivity, making them suitable for physical surface activation of industrial by-products.
  • the beads used in the present invention may be zirconia beads. The zirconia beads have a hardness of 1200-1300 (Vickers hardness) and a density of 3.98 g / ml. The beads are characterized in that 30% by volume is added when the mixture of the first step is 100% by volume.
  • the beads are added, the entire surface layer of the alkali industrial byproduct is removed at least 10-30% or more to allow the surface of the industrial byproduct to be activated.
  • the beads are mixed and stirred with an alkali industrial by-product and a solvent to remove the surface layer of the industrial by-product, thereby making it more reactive. That is, the calcium elution efficiency is improved by adding beads to remove the surface layer.
  • Alkaline industrial by-products PSA and CKD are high in calcium, but not all calcium is eluted by the solvent. This is because the particle surface layer of the industrial by-products inhibits contact between the solvent and CaO in the by-products.
  • the physical surface activation process is applied as a method for increasing the reactivity of the solvent and the industrial by-product CaO by removing the surface layer of the industrial by-product.
  • the beads are mixed with an alkali industrial by-product and a solvent, and the calcium dissolution efficiency from the industrial by-product is improved by 20 to 70%.
  • the method may further include repeatedly performing the first step at least twice, and each solvent of the repeatedly performed steps may use the same or different types of solvents.
  • each solvent of the repeatedly performed steps may use the same or different types of solvents.
  • the calcium may be eluted once more with a solvent different from the solvent used during the calcium eluting (ammonium chloride).
  • the mineral carbonation reaction is one of the technologies for storing carbon dioxide, which is a technique of stably storing carbon dioxide with a metal oxide containing calcium and stably storing it as an insoluble carbonate mineral.
  • the higher the concentration of calcium, magnesium and the like and the pH of the slurry eluted from the raw material according to the reaction scheme can store a larger amount of carbon dioxide. Therefore, in mineral carbonation, it is important to use a large amount of metal oxide to react with carbon dioxide, and to create a condition in which carbon dioxide and metal oxide can sufficiently react.
  • the selection conditions of the industrial by-products applicable in the present invention include 1) high calcium content, 2) alkaline industrial by-products, 3) smaller particle size is advantageous for calcium elution and carbonation, and 4) in industrial by-products.
  • the simpler form of calcium, such as calcium oxide or calcium hydroxide, is more advantageous for calcium elution and carbonation, and should be continuously generated by industrial activities.
  • the industrial by-products shown in Table 1 may be used.
  • the present invention may use paper sludge ash (PSA) or cement kiln dust (CKD).
  • PSA paper sludge ash
  • CKD cement kiln dust
  • the alkali industrial by-product is characterized in that the calcium content of 15 to 70%.
  • PSA used in the present invention was supplied by domestic H paper company, CKD was supplied by domestic D cement manufacturer.
  • X-ray diffraction analysis XRD, X'Pert-MPD System, Philips
  • X-ray fluorescence analysis XRF, XRF-1700 X-ray Fluorescence, Shimadzu
  • particle size analysis LS 13320 Laser Diffraction Particle Size Analysis, Beckman Coulter was conducted to know the size of industrial by-products.
  • Table 2 below is a table showing the physicochemical properties of PSA and CKD used in the present invention.
  • PSA and CKD which are by-products of the alkaline industrial by-products, have a high calcium content and a small particle size, which is very advantageous for mineral carbonation.
  • the present invention selected a solvent that is high in calcium elution efficiency and reusable from industrial by-products.
  • Indirect carbonation solvents selected in the present invention can be largely divided into chelating reagents and ammonium salts, and both have excellent calcium elution efficiency and reusable carbonation reactors.
  • both the chelating reagent and ammonium salt are restored to the form of the initial solvent after the carbonation reaction.
  • the chelating reagent reacts with calcium to form a complex.
  • the calcium carbonate production reaction may not proceed. Therefore, the solubility constant of calcium chelate must be considered when selecting solvents.
  • a solvent that does not react with calcium to produce a solid compound should be used.
  • Calcium-ligand complexes must be present as a liquid.
  • the calcium-ligand complex is not an end product but an intermediate product for the carbonation reaction. If the complex is present as a solid, it is difficult to react with carbon dioxide to produce calcium carbonate.
  • the solvent is preferably in the form of a salt rather than an acid.
  • trisodium citrate should be used as a solvent instead of citric acid.
  • the pH of the calcium eluate is higher than 9, the injected carbon dioxide is present in the form of CO 3 2- and carbonation reaction occurs.
  • the acidic solvent is not preferable because the pH of the calcium eluate is 9 or less.
  • the concentration of the solvent should be properly adjusted. This is because excessive injection of solvents creates calcium-ligand complexes and the remaining free ligand can interfere with CaCO 3 production.
  • the reusable solvent used in the carbon dioxide storage method of the present invention from the selection criteria as described above is characterized in that the stabilization constant is less than the stabilization constant of calcium carbonate (chelating reagent) or ammonium salt (ammonium salt).
  • the solvent used in the present invention is characterized in that the calcium dissolution and carbonation efficiency is high and the solvent is reusable.
  • the chelating agent (citrate salt), malonate salt (malonate salt), adipate salt (adipate salt), maleate salt (maleate salt), fumarate salt (iminodiacetate salt) and nitrilotri It may be any one selected from the acetate salt (nitrilotriacetate salt).
  • the chelating agent may be one selected from trisodium citrate, malonic acid disodium salt, adipic acid disodium salt, disodium maleate, disodium fumarate, iminodiacetic acid disodium salt, and nitrilotriacetic acid trisodium salt.
  • the ammonium salt may be ammonium chloride, ammonium acetate, and ammonium nitrate.
  • the purity of the calcium carbonate produced by the carbonation reaction of the present invention is characterized in that 99.5 to 99.7%. As described above, there is an advantage that can be used industrially by producing high purity calcium carbonate.
  • the solvent used in the carbon dioxide storage method of the present invention is characterized in that it can be reused at least three times. Not only can the solvent of the present invention be reused repeatedly, the calcium dissolution efficiency is kept constant even when the calcium dissolution is repeatedly performed as described above.
  • FIGS. 2 and 3 show graphs of changes in calcium concentration eluted from industrial by-products according to the solvent concentration of Experimental Example 1-1.
  • the optimal concentration of calcium elution solvent for PSA and CKD was 0.1-0.3M for trisodium citrate, 0.1-0.3M for malonic acid disodium salt, 0.1-1.5M for adipic acid disodium salt and 0.1-1M, respectively.
  • Trisodium citrate is used as a solvent for PSA and CKD, and the industrial by-products and the solvent are mixed at a ratio of 1:50 (w / v) at a concentration of 0.1-0.3 M, at a pressure of 1 atm. Calcium was eluted by stirring at 250 rpm for 1 hour. When the reaction was completed, the industrial by-products and the solvent were filtered and separated to measure calcium concentration and pH of the filtered calcium eluate.
  • the obtained calcium eluate was placed in a carbonation reactor, and carbon dioxide was injected at a rate of 0.1 L / min (based on 1 L of solvent) while stirring at 250 rpm, and carbonized until the pH of the reaction solution reached 10-11.
  • the produced white solid (calcium carbonate) was separated by filtration and the calcium concentration and pH in the filtrate were measured.
  • the resulting solid was washed with 1 L of distilled water and dried, and then the mass was measured and its components and contents were confirmed by XRD and XRF analysis.
  • the remaining solution and industrial by-products are mixed at a ratio of 1:50 (w / v) to proceed with the calcium elution reaction, and then experimented under the same conditions and methods as the carbonation reaction. Was repeated. That is, the reuse of the solvent was repeated at least three times.
  • the experiment was carried out under the same conditions and methods as in Experimental Example 2-1, except that malonic acid disodium salt was used as the solvent. However, the concentration of malonic acid disodium salt was 0.2-0.3M, and the carbonation reaction was carried out by injecting carbon dioxide at a rate of 0.1L / min (based on 1L of solvent) until the pH of the reaction solution reached 11-12.
  • the experiment was conducted under the same conditions and methods as in Experimental Example 2-1, except that adipic acid disodium salt was used as the solvent. However, the concentration of adipic acid disodium salt was 0.2-0.3M, and the carbonation reaction was carried out by injecting carbon dioxide at a rate of 0.1L / min (based on 1L of solvent) until the pH of the reaction solution reached 11-12.
  • the experiment was conducted under the same conditions and methods as in Experimental Example 2-1, except that ammonium acetate was used as the solvent. However, the concentration of ammonium acetate was 0.3 M, and the carbonation reaction was performed until the pH of the reaction solution reached 8-8.5 by injecting carbon dioxide at a rate of 0.1 L / min (based on 1 L of solvent).
  • the result of using PSA as a raw material is as follows.
  • the highest calcium elution concentration was when trisodium citrate was used.
  • the calcium elution concentration was 3656 ppm
  • the calcium elution concentration was 4547 ppm
  • the calcium elution concentration was 4296 ppm.
  • the carbonation efficiency was highest when the ammonium acetate was used as the solvent, with an average of 80% three times.
  • the average carbon dioxide storage amount is trisodium citrate, ammonium chloride, when using ammonium acetate as a solvent, respectively 167, 165, 166 kg-CO 2 / showed relatively high in ton-waste, average CaCO 3 amount at this time is 380, 375, respectively 377 kg-CaCO 3 / ton-waste.
  • the result of using CKD as a raw material is as follows.
  • the highest calcium elution concentration was when ammonium chloride was used.
  • the calcium elution concentration was 5524 ppm
  • the calcium elution concentration was 5688 ppm when the solvent was used twice
  • the calcium elution concentration was 6094 ppm when the solvent was used three times.
  • the carbonation efficiency was highest when the trisodium citrate was used as solvent, with an average of 88% three times.
  • the average carbon dioxide storage amount is trisodium citrate, ammonium chloride, when using ammonium acetate as a solvent, respectively 210, 220, 225 kg-CO 2 / showed relatively high in ton-waste, average CaCO 3 amount at this time is 478, 499, respectively 512 kg-CaCO 3 / ton-waste.
  • the carbon dioxide storage method of the present invention can be confirmed that not only high efficiency, but also an economical and environmentally friendly way to reuse the solvent.
  • Figure 6 shows the XRD analysis of the solid obtained through the carbonation reaction for each solvent.
  • Figure 6 shows the results of XRD analysis of (a) calcite, (b) trisodium citrate, (c) malonic acid disodium salt, (d) adipic acid disodium salt, (e) ammonium chloride, and (f) ammonium acetate.
  • a) calcite (b) trisodium citrate, (c) malonic acid disodium salt, (d) adipic acid disodium salt, (e) ammonium chloride, and (f) ammonium acetate.
  • XRF analysis confirmed that the purity of calcium carbonate according to the reuse by solvent was very high, average 99%. However, only trisodium citrate showed about 88% purity.
  • the solvent was reused, the purity of calcium carbonate obtained in each round showed a difference within ⁇ 1%.
  • one of 0.1-0.3M chelating reagent (trisodium citrate, malonic acid disodium salt, adipic acid disodium salt) is mixed with industrial by-products at a ratio of 1:50 (w / v) for high liquid ratio, and then 250rpm for 1 hour Stirred at.
  • the industrial by-products and solvents were filtered and separated, and 0.3M ammonium chloride was continuously mixed with the filtered industrial by-products at a ratio of 1:50 (w / v) in a solid solution ratio and then stirred again at 250 rpm for 1 hour. It was.
  • the solvent was filtered and separated from the industrial by-products and the calcium concentration in the filtered solvent was measured.
  • the concentration of solvent used was 0.3M trisodium citrate, 0.2M malonic acid disodium salt, 0.2M adipic acid disodium salt, 0.3M ammonium chloride for PSA, 0.1M trisodium citrate, 0.3M malonic acid disodium salt, 0.3M for CKD adipic acid disodium salt, 0.3M ammonium chloride.
  • the carbon dioxide can be effectively stored and in the form of high purity calcium carbonate by the indirect carbonation method under optimal conditions in consideration of the type of solvent, concentration of solvent, solid solution ratio, carbon dioxide flow rate and reaction time. It can be confirmed.
  • the carbon dioxide storage method of the present invention is a relatively simple process and can be reused solvent is economical and environmentally friendly to store carbon dioxide, physical surface activation process or through the calcium elution process using two solvents in succession It can be seen that carbon dioxide storage efficiency can be further improved.

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Abstract

La présente invention concerne le stockage d'un dioxyde de carbone et la production d'un carbonate de calcium à haute pureté au moyen d'une carbonatation indirecte de sous-produits industriels alcalins. En particulier, la présente invention concerne un procédé de stockage d'un dioxyde de carbone par l'intermédiaire de la production de carbonate de calcium à haute pureté, le procédé comprenant une première étape d'ajout d'un solvant aux sous-produits industriels alcalins pour éluer ainsi le calcium ; une deuxième étape de séparation de l'éluat de calcium du sous-produit résiduel ; une troisième étape de réalisation d'une réaction de carbonatation dans laquelle du dioxyde de carbone est introduit dans l'éluat de calcium afin de produire un carbonate de calcium ; une quatrième étape de séparation de l'éluat de calcium dans le carbonate de calcium et d'un solvant après la réaction de carbonatation ; et une cinquième étape de réutilisation du solvant de la quatrième étape en tant que solvant de la première étape, le solvant étant un réactif de chélation dont la constante de stabilisation avec le calcium est inférieure à la constante de stabilisation du carbonate de calcium.
PCT/KR2016/011896 2016-10-21 2016-10-21 Procédé de production de carbonate de calcium à haute pureté et de réutilisation de solvant au moyen de carbonatation indirecte de sous-produits industriels alcalins Ceased WO2018074638A1 (fr)

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KR102800109B1 (ko) 2023-06-14 2025-04-28 연세대학교 산학협력단 시멘트 킬른 더스트를 활용한 칼슘 이온 추출 및 나노사이즈 탄산칼슘 제조방법
KR102762214B1 (ko) * 2024-04-26 2025-02-04 주식회사 엑스카본 Cbs 더스트를 이용한 탄산칼슘 제조 방법

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