WO2011077117A1 - Perfectionnements apportés ou relatifs à la capture de dioxyde de carbone - Google Patents

Perfectionnements apportés ou relatifs à la capture de dioxyde de carbone Download PDF

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WO2011077117A1
WO2011077117A1 PCT/GB2010/052118 GB2010052118W WO2011077117A1 WO 2011077117 A1 WO2011077117 A1 WO 2011077117A1 GB 2010052118 W GB2010052118 W GB 2010052118W WO 2011077117 A1 WO2011077117 A1 WO 2011077117A1
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mineral
serpentine
ions
solution
ammonium salt
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PCT/GB2010/052118
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WO2011077117A8 (fr
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Xialong Wang
Mercedes Maroto-Valer
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The University Of Nottingham
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Priority to EP10803472A priority Critical patent/EP2516042A1/fr
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Publication of WO2011077117A8 publication Critical patent/WO2011077117A8/fr
Priority to US13/847,381 priority patent/US20130287673A1/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
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/62—Carbon oxides
    • 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
    • B01D53/73—After-treatment of removed components
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/60—Preparation of carbonates or bicarbonates in general
    • 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
    • C01F5/00—Compounds of magnesium
    • C01F5/24—Magnesium carbonates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/20—Reductants
    • B01D2251/206—Ammonium compounds
    • B01D2251/2062—Ammonia
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2251/00—Reactants
    • B01D2251/40—Alkaline earth metal or magnesium compounds
    • B01D2251/402—Alkaline earth metal or magnesium compounds of magnesium
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • 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
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/151—Reduction of greenhouse gas [GHG] emissions, e.g. CO2

Definitions

  • the present invention relates to the capture of carbon dioxide.
  • CO 2 geological storage is thought to be one of the most important strategies for carbon mitigation and to progress from demonstration scale to large industrial scale technologies.
  • geological storage is a very !ocation-dependent technology.
  • Many countries cannot find appropriate geological formations, such as Finland [1 ], Or, the distances from storage site to the CO 2 producer site can be thousands of kilometres, which causes high pipeline construction cost. For example, in China, the optimum storage site in the eastern sea area is far from its majority of power plants in the Huabei area.
  • C0 2 mineralization is another potential option for long-term storage of C0 2 .
  • Mineral sequestration is a promising strategy to permanently and safely to store anthropogenic generated carbon dioxide (C0 2 ) in solid Mg- and Ca- carbonates. Advantages of mineral carbonation include vast storage capacity, permanent storage, less leakage risk, and the fact that mineralization is an exothermal reaction.
  • mineral sequestration also faces many problems such as low efficiency, slow kinetics, and energy intensive pre- treatment processes [2]. Although, some barriers like low efficiency and slow kinetics have been solved by using pH ⁇ swing process, the need to add large amounts of acid and base limit the development of mineral sequestration.
  • Calcium and magnesium are generally selected as feedstock for C0 2 mineralization. For reactivity, carbonation of calcium is easier, but the magnesium minerals, mostly serpentine, are abundantly available worldwide. Mineral carbonation have vast storage capacity, for instance, a deposit in Oman of 30,000 km 3 magnesium silicates which alone would be able to store most of the CO 2 generated by combustion of the world's coal reserves [3].
  • [29] proposed a process of production of Mg(OH) 2 from serpentine using (NH 4 ) 2 S0 4 .
  • Solid-solid reaction of serpentine with (NH 4 ) 2 S0 4 was carried out at 440 °C to generate MgS0 4l that was put into ammonia water to precipitate Mg(OH) 2 and regenerate (NH 4 ) 2 S0 4 , Mg(OH) 2 was then carbonated with C0 2 directly at a pressurized fluidized bed (PFB) reactor at 470-550 °C and 20 bar.
  • PFB pressurized fluidized bed
  • the present invention provides a method for capturing carbon dioxide comprising the steps of: extracting mineral ions from a mineral source material to a mineral solution by reaction with a first ammonium salt; reacting the mineral solution with a C0 2 source to precipitate a carbonate of the mineral and to produce a second ammonium salt; and recovering the first ammonium salt from the second ammonium salt.
  • the invention provides an apparatus for capturing carbon dioxide comprising means for extracting mineral ions from a mineral source material to a mineral solution by reaction with a first ammonium salt; means for reacting the mineral solution with a C0 2 source to precipitate a carbonate of the mineral and to produce a second ammonium salt; and means for recovering the first ammonium salt from the second ammonium salt.
  • the mineral ions may be magnesium or calcium ions.
  • the mineral ions may be derived from a magnesium silicate or a calcium silicate, preferably serpentine or olivine.
  • the mineral source material is serpentine or olivine or another suitable magnesium or calcium silicate.
  • the mineral source is in a substantially pure form although it may equally contain impurities.
  • the mineral source materia! is a mineral waste material.
  • the mineral source is used in its naturally occurring form.
  • the mineral tons may be extracted by reaction with ammonium bisu!phate.
  • the mineral solution may be regulated to neutral pH before reacting with the CO2 source.
  • the pH is regulated using ammonia.
  • the CO2 source may be an intermediate product, preferably an intermediate product obtained by capturing CO2 from a waste stream.
  • the C0 2 may be captured by reaction with ammonia.
  • the intermediate product may be ammonium bicarbonate.
  • the recovery step may include the production of ammonia.
  • the recovered ammonia may be used for capturing C0 2 .
  • the first ammonium sait may be recovered by a process which includes evaporation and/or heating; preferably heating to a temperature of from 250 °C to 350 °C, more preferably to a temperature of between 300 °C and 350 °C, even more preferably to a temperature between 320 °C and 335 °C, more preferably to a temperature at or below 330 °C, preferably the first ammonium saft should not decompose as a result of said heating.
  • the recovered first ammonium salts may be used for further extraction of mineral ions from the mineral source material.
  • the invention provides a method comprising: capturing C0 2 by reacting CO2 with ammonia to produce an intermediate product; and using the intermediate product as a CO2 source in a mineral carbonation process.
  • the invention provides an apparatus for capturing carbon dioxide comprising means for reacting C0 2 with ammonia to produce an intermediate product and using the intermediate product as a CO2 source in a mineral carbonation process.
  • the C0 2 is from a waste stream, preferably a gas waste stream, preferably a gas waste stream from the burning of fuel.
  • Waste stream is understood to mean a source of C0 2 wherein the C0 2 is a by-product of another process, preferably a by-product of burning fuel.
  • the intermediate product may be ammonium bicarbonate.
  • the ammonium bicarbonate is placed into solution at a temperature above 50 °C, preferably above 60 °C, preferably at a temperature from 60 °C to 90 °C.
  • the mineral carbonation process may include reacting the intermediate product with a mineral solution.
  • the reaction between the intermediate product and the mineral solution is carried out in the presence of ammonia.
  • the mineral solution may be obtained by extracting mineral ions from a mineral source material to a mineral solution by reaction with an ammonium salt
  • the mineral ions may be magnesium.
  • the mineral ions may be derived from serpentine.
  • the mineral ions may be extracted by reaction with ammonium bisulphate.
  • the intermediate product is NH 4 HC03 and the mineral ions are magnesium ions and they are reacted in the presence of ammonia in a mass ratio of Mg:NH4HC0 3 :NH3 of from 1 :3:1 to 1 :5:3, preferably 1 :3: 1 to 1 :4:2, most preferably 1 :4:2.
  • the invention provides a process for producing power comprising the steps of producing C0 2 by burning a fuel and capturing the CO2 using a method or apparatus as described above.
  • Table 8 Summary from XRF analyses of solids used and produced in the experiment (units: wt%), the C0 2 contain from TGA analysis.
  • Fig. 1 Schematic process route of pH-swing C02 mineral sequestration with recyclable ammonium salts
  • Fig.2 Experimental setup for dissolution experiments
  • Fig. 3 Schematic constant size particles dissolution model
  • Fig. 4 XRD pattern of serpentine sample
  • Fig. 5 TGA graph of serpentine sample
  • Fig. 6 Selection of ammonium salts for serpentine dissolution (20 grams serpentine in 400ml 2M solvent solution at 70°C for 3 hours)
  • Fig. 7 Mg extraction from serpentine (20 grams) in 1 .4 M NH4HS04 solution (400ml) at 70, 90 and 1 10°C for 3 hours (tested by ICP-AES)
  • Fig. 8 Fe extraction from serpentine (20 grams) in 1 .4 M NH4HS04 solution (400ml) at 70, 90 and 1 10°C for 3 hours (tested by ICP-AES)
  • Fig. 9 Si extraction from serpentine (20 grams) in 1 .4 M NH4HS04 solution (400ml) at 70, 90 and 1 10°C for 3 hours (tested by !CP-AES)
  • Fig. 10 1 -3(1 -XMg)2/3+2(1 -XMg) vs. reaction temperature for extraction of Mg from serpentine in 1.4 M NH4HS04
  • Fig. 11 Arrhenius plot for extraction of Mg from serpentine in 1 .4 M NH4HS04 including trend line equation
  • Fig. 12 Modified process route of pH-swing C0 2 mineral sequestration with recyclable ammonium salts
  • Fig. 13 Comparison of the process steps and net power generation percentages between carbon capture and geological storage and integrated carbon capture and mineral carbonation
  • Fig. 14 Dissolution efficiency of different elements after serpentine dissolution by NH 4 HS0 4 (Experiment 3, 100 °C, 2 h)
  • Fig. 15 XRD pattern of product 2 of experiment 7.
  • Fig. 16 Temperature, time, pH and concentration of Mg in solution during the course of a typical carbonation experiment (Experiment 7)
  • Fig. 17 XRD pattern of product 3 of experiment 7
  • Fig. 18 TGA profiles of product 3 and product 4 from experiment 7, NH 4 HS0 4 and (NH4) 2 S0 4
  • Fig. 19 Temperature, time, pH and concentration of Mg in solution during the course of a carbonation experiment when double ammonium carbonate precipitate (Experiment 4)
  • Fig. 20 Plotted data of carbonation efficiency vs. molar ratio of Mg-NH 4 HC0 3 -
  • Examples will be described of a new pH-swing C0 2 mineral sequestration process using recyclable ammonium salts.
  • magnesium ions were extracted from serpentine in ammonium salts solution.
  • the Mg-rich leaching solution reacts with intermediate product (in some embodiments ammonium bicarbonate) of a C0 2 capture step to precipitate hydromagnesite at miid heating conditions, preferably greater than 70°C, preferably at about 70°C.
  • intermediate product instead of C0 2 could remove the need to perform CO 2 compression, which consumes extensive energy.
  • at the end of carbonation preferably greater than 70% , more preferably greater than 80%, and most preferably all ammonium salts and ammonia used could be regenerated by thermal decomposition.
  • the new pH-swing mineral sequestration process using recyclable ammonium salts is described as follows.
  • the process preferably consists of five main steps, where reactions occur, listed in Table 1 .
  • ammonia will be used to capture C0 2 from a power plant's flue gas and produce ammonium bicarbonate (NH4HCO3) in the capture step.
  • C0 2 is captured from a waste stream by reaction with ammonia to produce an intermediate product.
  • the ammonium bisu!phate (NH 4 HS0 4 ) is used to extract magnesium (Mg) ions from serpentine at mild heating conditions in the mineral dissolution step.
  • Mg magnesium
  • the Mg-rich solution produced from mineral dissolution is regulated to neutral pH by adding ammonia water; then, the impurities in the leaching solution are removed by adding ammonia water. After that, the solution is reacted with the intermediate product (ammonium bicarbonate (NH4HCO3)) from the C0 2 capture step to precipitate carbonates at mild temperature.
  • the minerai solution is reacted with a C0 2 source to precipitate a carbonate of the minera! and to produce a second ammonium salt.
  • the intermediate product is used as a C0 2 source in a mineral carbonation process.
  • the nesquehonite (MgCO 3 o3H 2 O) will transfer to hydromagnesite (4MgC0 3o Mg(OH) 2 o4H 2 0) above 70°C.
  • the final solution mainly contains ammonium sulphate.
  • the ammonium sulphate could be collected (e.g. by evaporation) and subsequently heated up to regenerate ammonia which goes back to the capture step and ammonium bisuiphate which is reused in mineral dissolution.
  • the first ammonium salt is recovered from the second ammonium salt.
  • Magnesium hydroxide may react with magnesium bicarbonate:
  • the process routes are indicated in Fig. 1 . It can be seen that there are 3 products from this process.
  • the first product from the mineral dissolution mainly contains amorphous silica (quartz) and minor residua! serpentine. If the dissolution step is conducted at high temperature (above 100°C), the reaction will proceed completely so that high purity amorphous silica can be obtained from dissolution.
  • the amorphous silica produced from serpentine dissolution had a purity of 82-88% by weight, but it can be refined into 99% by weight pure silica using ultrasonic and electromagnetic separation as well as calcination. Pure silica is widely used in electronic, automotive, chemical, and ceramic industries [6]. Thus the silica by-product can be used in other industries.
  • the second product results from the removal of impurities and is rich in Fe, such as mohrite ((NH4) 2 Fe(S0 4 ) 2 ) and goethite (FeO(OH)).
  • This Fe-rich product could possibly be suitable for the iron industry and the manufacture of pigments.
  • the third product results from the carbonation step and is hydromagnesite with a very high purity (for example over 90% or over 95% or over 99%). Therefore, this product could be sold as a valuable product.
  • the application of hydromagnesite is quite wide in the paper industry, cement industry, civil engineering and production of fire retardant [7].
  • the C0 2 capture and mineral sequestration are considered as two separate processes.
  • the C0 2 is first absorbed or adsorbed by different kinds of chemicals, such as MEA, amine and ammonia
  • the C0 2 is then desorbed by heating or some other methods to recover the sorbents and release C0 2 .
  • the C0 2 is then compressed in order to be transferred to the storage site.
  • compression consumes a iot of energy, which nearly accounts for 25% of the total energy consumption of the whole CCS process [9].
  • the intermediate product in the capture step for example NH 4 HC0 3 in the ammonia method, has the potential to be used in mineral carbonation directly. In this case there is no need for desorption and compression of C0 2 any more, and thus the cost of the whole CCS process would be significant reduced.
  • the new pH-swing mineral carbonation process is proposed to combine capture and storage together to save C0 2 compression and transportation steps.
  • serpentine sample from Cedar Hills quarry in southeast Pennsylvania and supplied by Albany Research Center (U.S.), was selected for experimental study. A batch of 10 kg serpentine rocks was ground and sieved, from which a particle size fraction of 75-150 ⁇ was selected for the experiments. Samples of the sieved 75-150 ⁇ fraction was analyzed using X-Ray Diffraction (XRD). For measurement of the contents of elements in the serpentine, samples of the sieved fraction were completely dissolved using HF solutions in microwave digestion.
  • XRD X-Ray Diffraction
  • the solutions were analyzed with Inductively Coupled Plasma-Atomic Emission Spectrometry (iCP-AES) using two different wave lengths to give a more exact reference number for the concentrations of Mg, Si, Fe, Ca, Al, Ni, Mn, Cr, Cu, Ai, Sr, Na, Ti and 8a in serpentine.
  • the carbonate (CO3) content of serpentine was determined using a thermal gravimetric analyzer (TGA 500) by heating up to 950°C.
  • the loss on ignition (LOI) was determined by drying the sample at 950 °C for 1 h in argon.
  • ammonium chloride (NH4) 2 S0 4 )
  • ammonium bisulfate (NH4HSO4)
  • H 2 S0 4 traditional solvent sulphuric acid
  • the solutions were stirred at 800 rpm at a temperature of 70 °C.
  • the solutions were immediately filtered with 0.7 pm Pail syringe filters after 3 hours dissolution.
  • the concentrations of Mg, Fe, and Si in the filtered solutions were measured with ICP-AES.
  • Extraction experiments were carried out in a 600mi 3 necks glass flask reactor, which is heated by a temperature-controlled silicon oil bath and equipped with a water-cooled condenser to minimize solution losses due to evaporation (Fig. 2).
  • the solutions were well mixed by using a magnetic stirrer setting to 800 rpm.
  • a pH probe with digital meter was set up to in-situ measure the pH change during the course of experiment.
  • 400 ml of desired solution was added to the flask, a charge 20 grams of serpentine with a particle size fraction of 75-150 Mm was added into a certain concentration of solution until reaching the pre-determined temperature.
  • liquid samples would be extracted with a syringe at interval time, such as 5 min, 15 min, 30 min, 1 h, 2 h, and 3 h.
  • the samples are then immediately filtered with 0.45 pm syringe filter unit.
  • the Mg, Fe and Si concentrations of the samples are measured using ICP-AES.
  • the pH values are measured on-line and recorded, the compensation of pH at different temperature is automatically done by the digital pH meter.
  • solution will be cooled down to ambient temperature and filtered with glass microfibre 0.7pm syringe filter. The solid will be dried in the oven at 75°C for overnight as product 1.
  • C y is the concentration of element x in the solution sampled at y time
  • V is the volume of the solution in the reactor (each sampling will extract 1 ml solution, but this minor volume is ignored)
  • m batch is the mass of serpentine sample added.
  • w x is the weight percentage of mass of element x over the total mass of solid (this result report from the elemental analysis of raw serpentine).
  • the reaction rate is generally controlled by the following sequential steps: diffusion through the fluid film, diffusion through the layer on the particle surface, or the chemical reaction at the surface.
  • the rate of the reaction is controlled by the slowest of these steps [1 1 ].
  • the elemental composition result from the serpentine dissolution analyses is shown in Table 2.
  • Major elements were Mg, Si and Fe, minor elements were Mn, Ca, Al and Ni (concentrations of 0.1-0.3 wt.%).
  • the XRD pattern (Fig. 4) of the serpentine reveals that the rock contained serpentine, (Mg3Si20 5 (OH) 4 ; antigorite and chrysotile), forsterite (Mg 2 Si0 4 ) and magnetite (Fe 3 0 4 ). According to the TGA analysis (Fig.
  • serpentine contained trace carbonate (1.12 wt.%), the loss on ignition at 950 °C was 13.6 wt.%, the moisture content was 0.6 wt.% and chemical-bound water was 1 1.88 wt.%.
  • a summary of the results from serpentine characterization indicate that this serpentine sample is representative and suitable for CO2 mineralization.
  • NH 4 HS0 4 was selected for further studies.
  • the dissolution rate of serpentine with a particle size fraction of 75-150 pm was tested in 1 .4 M (which is 40% excess of stochiometric amount of NH 4 HS0 4 , was used to result in a more complete reaction ) concentrations of NH 4 HS0 4 using solution temperatures of 70 °C, 90 °C, and 1 10 °C respectively.
  • concentrations of NH 4 HS0 4 using solution temperatures of 70 °C, 90 °C, and 1 10 °C respectively.
  • the effect of temperature upon the dissolution of serpentine is shown in Figs. 7-9. As can be seen from the figures, higher temperatures yield higher extraction efficiencies for each element tested.
  • the heat released from reaction can promote rapid dissolution of serpentine.
  • it may be due to a decreasing additive concentration at high dissolution levels.
  • roughly 50% of NH4HSO4 is consumed after a 80% extraction of magnesium from serpentine.
  • they might due to variation in serpentine composition or the mass loss during the sample feed or the evaporation of solution. A larger scale the experiment could reduce those errors.
  • the apparent rate constant (k) was determined from the slope of the lines in Figs. 10.
  • the apparent rate constant can be used for determining the activation energy (E) by Arrhenius' law:
  • serpentine Pre-treatment of serpentine could further enhance the dissolution rate.
  • the serpentine, or other mineral source material could be broken into smaller pieces.
  • Physical activation such as concurrent grinding could effectively remove the silica layer from the particles [16].
  • heat-treatment at 650°C increase reactivity greatly [1 7].
  • thermal activation of the mineral increases considerably the energy demand of the process.
  • C0 2 mineralization is an interesting option for long-term storage of C0 2 .
  • Our new pH-swing mineral carbonation process by using ammonium salts could remove the barrier of recycling of all chemicals involved. And this process could combine capture and storage together to save CO 2 compression and transportation steps, if the by-products from this process reach high purity, it would compensate the cost of CO2 sequestration.
  • a modified process diagram can be seen in the Figure 12.
  • aqueous NH4HSO 4 was used to extract Mg from serpentine. Then the pH of the solution is swung by adding ammonia water, resulting in Fe and Si precipitating from solution.
  • NH4HCO3 and NH 3 were then added into solution to react with Mg and produce carbonates and (NH 4 ) 2 S0 4 , that was recycled from the solution by evaporation and then decomposed back into NH 3 and NH 4 HS0 4 .
  • ammonia water The reason for using ammonia water is because the above reaction produces ammonium sulphate, which can be converted to NH 3 and NH 4 HSO4 in the regeneration step to enable the recycling of the additives. If high value product (e.g. pure magnesium carbonate) is wanted, some impurities, such as Fe, Al, Cr, Zn, Cu and Mn, need to be precipitated out from the system by increasing pH. in order to optimize the removal of impurities, extra ammonia water was added into filtrate 1 after pH regulation.
  • the reactions for impurity removal are:
  • ammonia water 35 wt. %) was added into filtrate 1 until the pH value was neutral. During this process, the solution was stirred and an in-situ pH probe was used to measure the pH value. The solution was filtered with 0.7 pm Pall syringe filters. This filtrate is referred to as filtrate 2 and was used for the carbonation experiments. The solid residue was dried at 105 °C overnight and is referred to as product 2.
  • the filtrate 2 was analyzed by ICP-AES to quantify the concentration of different elements, including Mg, Si, Fe, Mn, Zn, Cu, A! and Cr.
  • the product 2 was analyzed by XRF and XRD to quantify its composition and identify the mineral phases present.
  • the filtrate 2 was put in a 500 ml 3 necks glass vessel and heated up to 60 °C using a silicon oil bath.
  • the experimental setup was as reported in the previous paper [32], The time, temperature and pH values were recorded every 5 mins during the whole experiments.
  • ammonia water 35 wt. %) was added into filtrate 2.
  • NH 4 HC0 3 (as CO2 source) was added and the solution was heated to 90 °C. 2 ml a!iquots were sampled using a needle syringe at 5, 10, 15, 30, 45 and 60 mins.
  • the liquid samples were filtered by a mini filter unit and acidified with HN0 3 .
  • the liquid samples were analyzed by iCP-AES to measure the change of magnesium concentration. After the solution was stabilised at 90 "C, the solution was kept at that temperature for 30 mins. After that, the solution was cooled down and filtered with 0.7 ⁇ » Pail syringe filters and the filtrate is referred to as filtrate 3. The solid residue was dried at 105 °C overnight and is referred to as product 3. The composition of the product 3 was analyzed using XRF and the mineral phases were identified by XRD. The carbon content of the product 3 was measured by TGA.
  • the carbonation efficiency is defined as follows:
  • C0 2 content (wt. %) is the weight loss of product 3 during the temperature range from 300 °C to 500 °C corresponding to carbonate decomposition from the TGA studies [33].
  • m 3 is the mass (grams) of product 3 from carbonation experiment
  • c 2 is the magnesium concentration in filtrate 2 from ICP-AES
  • V 2 is the volume of filtrate 2
  • 24 and 44 is the molecular weight of Mg and C0 2 .
  • the thermal decomposition of product 4 was performed on a thermal gravimetric analyzer (TGA Q500) in the temperature range of 30-530 °C with a constant heating rate of 10 °C/min under nitrogen atmosphere.
  • the temperature programme was as follows: from 30 °C to 230 °C at rate of 10 °C/min, hold for 10 mins at 230 °C, up to 330 °C at rate of 10 °C/min, hold for 10 mins at 330 °C and finally up to 530 °C at rate of 10 X/min.
  • the application of three steps heating can help to find the clear thermal decomposition temperature range and avoid the mixture decomposition of products.
  • the XRD pattern of product 2 ( Figure 15) identified double ammonium salts, (NH 4 ) 2 Fe 2 (S0 4 ) 2 o6H 2 0, (NH 4 ) 2 Mg 2 (S0 4 ) 2 o6H 2 0 and (NH 4 ) 2 Zn 2 (S0 4 ) 2 °6H 2 0, to be the major phases.
  • the presence of these double ammonium salts results from the excess of ammonia water. Hot water flashing can decompose these double ammonium salts into ammonium sulphate and insoluble hydroxide salts [34].
  • Table 7 clearly shows that the concentration of Fe in filtrate 2 decreased significantly compared to filtrate 1 . This decrease of Fe concentration indicates that Fe precipitates.
  • Figure 16 shows the Mg concentration changes with time and temperature in experiment 7.
  • the starting time is when heating is started, the pH of filtrate 2 decreased from 8.5 to 7.3 when the temperature was increased during the first 20 mins.
  • NH4HCO3 was added the filtrate 2 solutions at 60 °C as labelled in Figure 16, the pH increased slightly to 7.6. No precipitate was formed before adding NH 4 HC0 3 .
  • the concentration of magnesium started to drop when the temperature went up to 70°C at the 25 th minute, in the following 5 mins, half of the Mg ions precipitated at a very high rate of 33.3 mmol/min.
  • the carbon content of product 3 could be calculated from the TGA profiles ( Figure 18(a)), All samples contained only one carbonate phase according to XRD studies. Therefore, the mass of the identified carbonate phase was estimated based on the corresponding weight loss from the TGA studies.
  • Figure 18 (a) shows two peaks, where the first peak below 250 °C is about 12 wt. % and corresponds to the release of crystal water [33]. The second peak is due to the release of C0 2 and accounts for 37 wt. % [33]. It can be seen from the TGA graph that the hydromagnesite does not decompose unti! 300 °C. Finally, based on the CO2 content (Table 8) and the Mg concentration in filtrate 2 (Table 7), it can be calculated that the carbonation efficiency of experiment 7 is 90 %.
  • the Mg ions firstly react with HC0 3 - to form Mg(HC0 3 ) 2 .
  • Mg(HC0 3 )2 then thermal decomposes into insoluble MgC0 3 at elevated temperature.
  • 1 mole of magnesium bicarbonate ion can convert into 1 mole of magnesium carbonate and 1 mole of C0 2 .
  • the maximum stoichiometry carbonation efficiency is only 50 %.
  • the carbonation efficiency was only 25.5 %.
  • the joint use of ammonia water and NH 4 HC0 3 can improve the carbonation, as explained by the following reaction equations:
  • Ammonia captures C0 2 to regenerate NH 4 HC0 3 , where this reaction is already used in C0 2 capture technology [28].
  • Ammonia can convert NH 4 HC0 3 into (NH 4 ) 2 C03, which can directly produce MgCOs.
  • Ammonia can also react with MgS0 4 to form insoluble Mg(OH) 2 when the pH value is above 10 [26].
  • Mg(OH) 2 can react with CO 2 to form Mg(HCO 3 ) 2 .
  • the Mg(OH) 2 can also react with Mg(HCO 3 ) 2 directly to precipitate MgCO 3 . Therefore, the carbonation efficiency can be improved by addition of ammonia water to the high Mg concentration solution.
  • MgC03o(NH 4 )2C03o4H 2 0 magnesium ammonium carbonate
  • MgC03o(NH 4 )2C03'4H 2 0 is generated from the reaction where NH 3 and NH 4 HC0 3 react with Mg ions at iow temperature.
  • MgC03"(NH 4 )2C03o4H 2 0 can quickly precipitate by adding the NH 4 HC0 3 below 60 °C.
  • MgC0 3 o(NH4)2C03o4H 2 O decomposes quickly to produce MgHC0 3 , and NH 3 gas when temperature goes above 60 °C.
  • the reactions of production and decomposition of magnesium ammonium carbonate are presented here:
  • the carbonation efficiency of experiment 4 is as low as 53.4 % due to the shortage of NH 3 gas which escaped from the reaction system during the thermai decomposition of MgC0 3 o(NH4) 2 C0 3 o4H 2 0. Comparing experiments 4 and 9 using the same mass ratio of Mg-NH 4 HC0 3 -NH 3 and same experimental conditions, the carbonation efficiency decreased from 91.5 % to 53.4 % when there was precipitation of MgC0 3 o(NH4)2C03o4H 2 0 (Table 6). Therefore, in order to prevent the iow carbonation efficiency caused by precipitation of magnesium ammonium carbonate, NH 4 HC0 3 should preferably be added into solution above 60°C.
  • the second weight loss is 75.8 wt. % and is due to further decomposition of NH4HSO4 between 350 °C and 500 °C [37] [38] [39].
  • the weight loss of product 4 is 97.5 wt. %, and the residual 2.5 wt % is due to the presence of MgS0 4 which did not react during carbonation.
  • the similar TGA profile of pure (NH 4 ) 2 S0 4 (purchased from Fisher Scientific) is presented in Figure 18 (c), where two peaks appear at the same temperature range as those for the TGA profiie of product 4 ( Figure 18 (b)).
  • the TGA curve of NH 4 HS0 4 is presented in Figure 18 (d) and shows only one peak between 330 °C and 500 °C due to decomposition into NH 3 , H 2 0 and S0 3 .
  • the NH 4 HS0 4 and NH 3 regeneration efficiency from (NH 4 ) 2 S0 4 has been reported to be nearly 97 % [37] [38] [39]. In this work, the regeneration efficiency of NH 4 HS0 4 and NH 3 from product 4 is 95 %..
  • the mass ratio of Mg : NH 4 HC0 3 : NH 3 is the key factor to control carbonation efficiency as discussed here.
  • the stoichiometric molar ratio of Mg : NH 4 HC0 3 is 1 :2, but the results of experiment 5 show that when the ratio is 1 :2, the carbonation efficiency is only 41 .5 % (Table 6).
  • the increase of NH 4 HC0 3 can improve the carbonation efficiency, as presented in Table 6, where the carbonation efficiency increase to 71.6 %, 77.9 % and 89.9 % when the ratio of Mg : NH 4 HC0 3 is 1 :3, 1 :4 and 1 :5, respectively.
  • the dissolution efficiency can achieve 90 % at 100 °C and 2 h and that the carbonation efficiency is 95.9 % when the molar ratio of Mg:NH 4 HCO 3 :NH 3 is 1 :4:2, the net conversion of serpentine to hydromagnesite is 86.3 %.
  • the mass balance based on these efficiencies, about 2.63 t of serpentine, 8.48 1 of NH4HSO4, 2.31 t of NH 4 HCO 3 and 0.5 t of NH 3 are required to sequester 1 t CO 2 , and 2.95 t of hydromagnesite is produced.
  • pure hydromagnesite can be produced from serpentine with regenerated ammonium salts with a net conversion of 86.3 %.
  • Amorphous silica can be obtained from the dissolution step.
  • By-products with maximum 27.5 wt. % Fe content were obtained from the pH regulation and removal of impurities step.
  • the additives used, NH 4 HS0 4 and NH 3 can be regenerated by thermal decomposition of (NH 4 )2S0 4 preferably at 330 °C.
  • the addition of ammonia water before carbonation could significantly improve the carbonation efficiency.
  • NH4HCO3 should preferably be added into solution after 60 °C to prevent the production of magnesium ammonium carbonate.
  • the mass ratio of Mg:NH 4 HC0 3 :NH3 is a key factor to control the carbonation efficiency, and it was found that when the mass ratio of Mg:NH 4 HC0 3 :NH 3 was 1 :4:2, the carbonation efficiency achieved 95.9 %. From the TGA studies, the regeneration efficiency of NH 4 HS0 4 in this process was found to be 95 %. According to the mass balance, about 2.63 t of serpentine, 0.12 t of NH 4 HS0 4, 6.82 t of NH 4 HC0 3 and 0.025 t of NH 3 is required to sequester 1 t CO2, and 2.95 1 of hydromagnesite is produced.
  • IPCC IPCC special report on carbon dioxide capture and storage. Prepared by Working Group III of the Intergovernmental Pane! on climate Change (Metz, B. , O. Davidson, H. C. de Coninck, M. Loos, and L. A. Meyer (eds.)), Cambridge University Press, Cambridge, United Kingdom and New York, NY, USA, 2005 [10] Maroto-Valer, M. M., D. J, Fauth, M.E. Kuchta, Y. Zhang, J.M. Andresen. Activation of magnesium rich minerals as carbonation feedstock materials for C0 2 sequestration. Fuel Processing Technology 2005; 86(14-15): 1627-1645.

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Abstract

L'invention concerne un procédé de capture de dioxyde de carbone, qui comprend les étapes consistant à : extraire des ions minéraux provenant d'une matière source de minéraux dans une solution de minéraux par réaction avec un premier sel d'ammonium; faire réagir la solution de minéraux avec une source de CO2 pour précipiter un carbonate du minéral et produire un deuxième sel d'ammonium; et récupérer le premier sel d'ammonium à partir du deuxième sel d'ammonium.
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CN102794093A (zh) * 2012-08-14 2012-11-28 中国华能集团清洁能源技术研究院有限公司 一种二氧化碳捕集与矿化一体化工艺
CN103274551A (zh) * 2013-06-26 2013-09-04 瓮福（集团）有限责任公司 一种二氧化碳矿化技术处理高硬度水净化回用方法
EP2695661A1 (fr) * 2012-08-08 2014-02-12 Omya International AG Matériau d'échange d'ions pouvant être régénéré pour réduire la quantité de CO2
WO2014177857A1 (fr) * 2013-04-30 2014-11-06 Gulf Organisation For Research And Development Procédé de séquestration de dioxyde de carbone
CN106430264A (zh) * 2016-07-19 2017-02-22 四川大学 一种用炼铁高炉渣矿化co2联产氧化铝的方法
CN106830037A (zh) * 2017-02-17 2017-06-13 四川大学 一种利用高炉渣矿化co2联产铵明矾的方法
WO2017106923A1 (fr) * 2015-12-22 2017-06-29 Richard Hunwick Procédé et système de capture de dioxyde de carbone à partir de courant gazeux
EP3038737A4 (fr) * 2013-10-07 2017-08-23 Reid Systems (Australia) Pty Ltd. Procédé et appareil de retrait du dioxyde de carbone dans des gaz de carneau

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