JP2009007208A - Method for calcining calcium carbonate - Google Patents

Method for calcining calcium carbonate Download PDF

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JP2009007208A
JP2009007208A JP2007171323A JP2007171323A JP2009007208A JP 2009007208 A JP2009007208 A JP 2009007208A JP 2007171323 A JP2007171323 A JP 2007171323A JP 2007171323 A JP2007171323 A JP 2007171323A JP 2009007208 A JP2009007208 A JP 2009007208A
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calcining
caco
calcium carbonate
cao
carbon dioxide
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Sekiei Hayashi
石英 林
Hisashi Kiga
気駕尚志
Yin Wang
印 汪
Zenzo Suzuki
鈴木善三
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SEKITAN ENERGY CENTER
SEKITAN ENERGY CT
National Institute of Advanced Industrial Science and Technology AIST
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SEKITAN ENERGY CENTER
SEKITAN ENERGY CT
National Institute of Advanced Industrial Science and Technology AIST
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Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for calcining calcium carbonate (CaCO<SB>3</SB>) which exhibits high energy efficiency in calcining calcium carbonate (CaCO<SB>3</SB>) and can reproduce calcium oxide (CaO) excellent as a CO<SB>2</SB>absorbent in the HyPr-RING method. <P>SOLUTION: Provided is a method for preparing calcium oxide (CaO) and carbon dioxide (CO<SB>2</SB>) by calcining calcium carbonate (CaCO<SB>3</SB>), which is characterized by calcining in an atmosphere having a steam partial pressure of 50-80% and a carbon dioxide partial pressure of 20-50% (total pressure of 0.05-0.15 Mpa) at 750-1,000°C. <P>COPYRIGHT: (C)2009,JPO&INPIT

Description

本発明は、炭酸カルシウム（CaCO3）のカ焼方法に関し、より詳しくは、炭素を含有する物質をCaOと水の存在下、反応させ、炭素を含有する物質を熱化学的に分解しつつ、水を還元して水素を生成させる方法において（HyPr-RING法）、生成した炭酸カルシウムCaCO３をカ焼することにより再度CaOに再生して再利用するためのカ焼方法に関する。 The present invention relates to a method for calcining calcium carbonate (CaCO 3 ), and more specifically, reacting a carbon-containing substance in the presence of CaO and water, and thermally decomposing the carbon-containing substance, In the method of reducing hydrogen to generate hydrogen (HyPr-RING method), the present invention relates to a calcining method for regenerating and reusing CaO3 that has been generated to CaO.

有機物中の炭素を酸化する際に発生する熱を利用し、高温高圧の水を熱化学的に分解し水素を選択的に製造する方法（HyPr-RING法）は、すでに知られている（特許文献１〜特許文献７参照）。
二酸化炭素吸収剤としては、CaO が最も推奨される物質である。
主反応は
C + H２O = CO + H２ （吸熱反応）31.4 kcal (１)
H２O + CO = CO２ + H２（発熱反応）-9.9 kcal (２)
CaO + CO２ = CaCO３ （発熱反応）-42.5 kcal (３)
従って総括の反応は、
C + 2H２O + CaO = CaCO３ + 2H２(発熱反応）-21.0 kcal (４)
と示すことが出来る。 A method of selectively producing hydrogen (HyPr-RING method) using the heat generated when carbon in organic substances is oxidized and thermochemically decomposing high-temperature and high-pressure water is already known (patented) Reference 1 to Patent Document 7).
As a carbon dioxide absorbent, CaO is the most recommended substance.
The main reaction is
C + H 2 O = CO + H 2 (endothermic reaction) 31.4 kcal (1)
H 2 O + CO = CO 2 + H 2 (exothermic reaction) -9.9 kcal (2)
CaO + CO 2 = CaCO 3 (exothermic reaction) -42.5 kcal (3)
So the overall response is
C + 2H 2 O + CaO = CaCO 3 + 2H 2 (exothermic reaction) -21.0 kcal (4)
Can be shown.

炭素を含有する固体燃料と超臨界水とを反応させ、酸化カルシウム に二酸化炭素を炭酸カルシウム として固定することで水素及びメタンを製造する装置に、超臨界水及び熱を供給するシステムにおいて、超臨界圧水を加熱して供給する高温超臨界水供給装置と、炭酸カルシウム をカ焼 して酸化カルシウム に再生するのに必要な熱を供給する熱供給装置とを備えてなることを特徴とする超臨界水及び熱供給システムが知られている（特許文献８）。ここでは、炭酸カルシウム のカ焼 用の熱２８は、ＣａＯ再生器１４の形式や規模により、それに適した形で供給される。例えば、大容量のＣａＯ再生器の場合は、一般に高温（好ましくは５００℃以上）の気体（代表的には空気）の中に炭酸カルシウム を分散・散布して、高温の気体との直接接触によりカ焼 を行なう。その後、高温の気体はボイラの燃焼用空気の一部として活用されることが記載されている。   In a system that supplies supercritical water and heat to an apparatus that produces hydrogen and methane by reacting carbon-containing solid fuel with supercritical water and fixing carbon dioxide as calcium carbonate to calcium oxide. An ultra-high temperature supercritical water supply device that heats and supplies pressurized water, and a heat supply device that supplies heat necessary for calcining calcium carbonate to regenerate it into calcium oxide. A critical water and heat supply system is known (Patent Document 8). Here, the heat 28 for calcining calcium carbonate is supplied in a form suitable for the type and scale of the CaO regenerator 14. For example, in the case of a large-capacity CaO regenerator, calcium carbonate is generally dispersed and dispersed in a high-temperature (preferably 500 ° C. or higher) gas (typically air), and direct contact with the high-temperature gas. Perform calcination. Thereafter, it is described that the high-temperature gas is used as a part of boiler combustion air.

また、HyPr-RING法は水素製造と共にカルシウムベース吸収剤（CaO）を使ってガス化炉内でCO2を吸収分離する。使用済みの吸収剤(CaCO3炭酸塩）をカ焼してCO2の回収と共に、吸収剤（CaO）が再生される。
高濃度のCO2を回収するため、従来の考えはCO2とO2との混合ガスで燃料を燃やしてカ焼のための熱を提供し、排ガスから高濃度のCO2を回収することが提案されていた。しかし、この方法はカ焼炉内のCO2分圧を高くするため、CaCO3のカ焼温度を1000℃以上に高くしなければならず、エネルギーロスが増大するが、生石灰(CaO)の焼結が促進され、HyPr-RING法におけるCO2吸収率が低下し、吸収剤の活性低下が起きる。
The HyPr-RING method absorbs and separates CO 2 in a gasifier using a calcium-based absorbent (CaO) together with hydrogen production. The used absorbent (CaCO 3 carbonate) is calcined to recover the CO 2 and to regenerate the absorbent (CaO).
In order to recover high concentration of CO 2 , the conventional idea is to burn the fuel with a mixed gas of CO 2 and O 2 to provide heat for calcination, and to recover high concentration of CO 2 from the exhaust gas. It was proposed. However, since this method increases the CO 2 partial pressure in the calciner, the CaCO 3 calcining temperature has to be raised to 1000 ° C or more, which increases energy loss, but burns quick lime (CaO). Sedimentation is promoted, the CO 2 absorption rate in the HyPr-RING method decreases, and the activity of the absorbent decreases.

特許第２９７９１４９号明細書Japanese Patent No. 2979149 特許第３０５７２５０号明細書Japanese Patent No. 3057250 特開２００１−０１９４０２号公報JP 2001-019402 A 特許第３９１５０１０号明細書Japanese Patent No. 3915010 特開２００３−０８２３６１号公報Japanese Patent Laid-Open No. 2003-083361 特開２００４−０５９８１６号公報JP 2004-059816 A 特開２００５−１０４５９５号公報JP 2005-104595 A 特開２０００−２７３４７２号公報JP 2000-273472 A

本発明は、炭酸カルシウム(CaCO3）をカ焼するに際して、エネルギー効率が高く、HyPr-RING法におけるCO2吸収剤として優れた酸化カルシウム（CaO）を再生できる炭酸カルシウム(CaCO3）のカ焼方法を提供する。
The present invention, when calcined calcium carbonate (CaCO 3), high energy efficiency, calcination of calcium carbonate (CaCO 3) capable of reproducing an excellent calcium oxide as a CO 2 absorbent (CaO) in HyPr-RING method Provide a method.

本発明者は、炭酸カルシウム（CaCO3）を特定条件の水蒸気と炭酸ガス（CO2）を用いて、１０００℃以下で炭酸カルシウム（CaCO3）のカ焼を行うこと若しくは、場合により炭酸カルシウム（CaCO3）と炭素燃料を混合し、特定条件の水蒸気と酸素（O2）を用いて燃焼し、1000℃以下で炭酸カルシウム（CaCO3）のカ焼を行うと、エネルギーロスが少なく、焼結生石灰(CaO)の生成割合が小さく
吸収効率（炭酸ガス吸収剤として効率が良い）が高い酸化カルシウム（CaO）を得ることを見出し、本発明を完成させるに至った。
すなわち、本発明は、炭酸カルシウム（CaCO3）をカ焼して酸化カルシウム（CaO）と炭酸ガス（CO２）を得る方法において、水蒸気分圧５０〜８０％、炭酸ガス分圧２０〜５０％（全圧0.05−0.15Mpa）の雰囲気下、温度７５０〜１０００℃以下の条件でカ焼することを特徴とする炭酸カルシウム（CaCO3）カ焼方法である。
また、本発明は、雰囲気を、水蒸気分圧６０％、炭酸ガス分圧４０％、温度９５０とすることが望ましい。
さらに、本発明は、炭酸カルシウム（CaCO3）をカ焼して酸化カルシウム（CaO）と炭酸ガス（CO２）を得る方法において、炭酸カルシウム（CaCO3）と炭素燃料との混合物を水蒸気濃度５０〜８０％、酸素（O２）濃度２０〜５０％のガスで燃焼し、温度７５０〜１０００℃以下の条件でカ焼することを特徴とする炭酸カルシウム（CaCO3）カ焼方法である。
The present inventors, using calcium carbonate (CaCO 3) the specific condition of the water vapor and carbon dioxide (CO 2), 1000 ° C. or that perform calcination of calcium carbonate (CaCO 3) below, when the calcium carbonate ( When CaCO 3 ) and carbon fuel are mixed, burned with water vapor and oxygen (O 2 ) under specific conditions, calcining of calcium carbonate (CaCO 3 ) at 1000 ° C or less causes less energy loss and sintering The inventors have found that calcium oxide (CaO) having a low production rate of quick lime (CaO) and high absorption efficiency (high efficiency as a carbon dioxide absorbent) is obtained, and the present invention has been completed.
That is, the present invention relates to a method for calcining calcium carbonate (CaCO 3 ) to obtain calcium oxide (CaO) and carbon dioxide (CO 2 ), in which water vapor partial pressure is 50 to 80% and carbon dioxide partial pressure is 20 to 50%. It is a calcium carbonate (CaCO 3 ) calcining method characterized by calcining under a temperature of 750 to 1000 ° C. under an atmosphere of (total pressure 0.05-0.15 Mpa).
Further, in the present invention, it is desirable that the atmosphere has a water vapor partial pressure of 60%, a carbon dioxide partial pressure of 40%, and a temperature of 950.
Furthermore, the present invention relates to a method of calcining calcium carbonate (CaCO 3 ) to obtain calcium oxide (CaO) and carbon dioxide gas (CO 2 ), wherein a mixture of calcium carbonate (CaCO 3 ) and carbon fuel has a water vapor concentration of 50 It is a calcium carbonate (CaCO 3 ) calcining method characterized in that it is burned with a gas of ˜80% and oxygen (O 2 ) concentration of 20-50% and calcined at a temperature of 750-1000 ° C. or less.

本発明のカ焼方法は、CaCO3から活性の高いCaOを製造しつつCO2を回収することができる。従来法のCO2のみの雰囲気下では、カ焼率90%以上にカ焼するためにカ焼温度が1020℃以上必要することに対し、本発明のカ焼方法の水蒸気希釈CO2/steam雰囲気下でのカ焼温度が低く、約900℃であった。 The calcination method of the present invention can recover CO 2 while producing highly active CaO from CaCO 3 . In an atmosphere of only CO 2 of the conventional method, a calcination temperature of 1020 ° C or more is required to calcine to a calcining rate of 90% or more, whereas the steam-diluted CO 2 / steam atmosphere of the calcination method of the present invention The lower calcination temperature was about 900 ° C.

図１には従来法のCO2のみの雰囲気でカ焼を行ったものである。
比較のために、本発明のCO2/steam雰囲気下での温度とカ焼率の関係を示す。同様な温度条件ではCO2雰囲気下でのカ焼率は低く、水蒸気希釈CO2/steam雰囲気下でのカ焼率は高いことがわかる。
90%以上にカ焼するためにCO2雰囲気下でのカ焼温度が1020℃以上必要することに対し、水蒸気希釈CO2/steam雰囲気下でのカ焼温度が低く、約900℃であることが判る。
図２には従来法と本件からほぼ同じカ焼率の95-97%を得た試料のCO2吸収反応性を示す。従来法でカ焼した試料のCO2吸収率は約40%に対して、本件のCO2/steam雰囲気下でカ焼した試料のCO2吸収率はかなり高く約65%に達した。 FIG. 1 shows the calcination performed in a conventional CO 2 atmosphere.
For comparison, the relationship between the temperature and the calcination rate in the CO 2 / steam atmosphere of the present invention is shown. It can be seen that under similar temperature conditions, the calcination rate under a CO 2 atmosphere is low and the calcination rate under a steam diluted CO 2 / steam atmosphere is high.
The calcining temperature in the CO 2 atmosphere needs to be 1020 ° C or higher in order to calcine to 90% or higher, whereas the calcining temperature in the steam diluted CO 2 / steam atmosphere is low, about 900 ° C. I understand.
FIG. 2 shows the CO 2 absorption reactivity of a sample that obtained 95-97% of the calcining rate almost the same as that of the conventional method. The calcined the CO 2 absorption rate of the sample by the conventional method with respect to about 40%, CO 2 absorption rate of the calcined samples in CO 2 /? Steam atmosphere of matter reached much higher about 65%.

本発明のカ焼方法おいて、用いる炭酸カルシウム（CaCO3）は、どのような炭酸カルシウムでも良いが、HyPr-RING法の使用済み生成物としての吸収剤(CaCO3炭酸塩）がとくに望ましい。本発明のカ焼方法を具体化したカ焼装置は、HyPr-RINGの水素発生装置と連結させて用いることができる。
本発明で用いる炭素燃料は、炭素を含有するものであれば何でも良い。代表的には石炭であり、粉末状ないし顆粒状の石炭として用いることができる。石炭に代えてオイルサンドやタールや油等も用いることができる。 In the calcination method of the present invention, any calcium carbonate (CaCO 3 ) may be used, but an absorbent (CaCO 3 carbonate) as a used product of the HyPr-RING method is particularly desirable. The calcination apparatus embodying the calcination method of the present invention can be used in connection with a hydrogen generator of HyPr-RING.
The carbon fuel used in the present invention may be anything as long as it contains carbon. Typically, it is coal, and can be used as powdery or granular coal. Oil sand, tar, oil or the like can be used instead of coal.

本発明の実施の形態は以下のとおりである。
（１）炭酸カルシウム（CaCO3）をカ焼して酸化カルシウム（CaO）と炭酸ガス（CO２）を得る方法において、水蒸気分圧５０〜８０％、炭酸ガス分圧２０〜５０％（全圧０．０５−０．１５Mpa）の雰囲気下、温度７５０〜１０００℃以下の条件でカ焼することを特徴とする炭酸カルシウム（CaCO3）カ焼方法。
（２）雰囲気が、水蒸気分圧６０％、炭酸ガス分圧４０％、温度９５０である上記（１）に記載した炭酸カルシウム（CaCO3）カ焼方法。
（３）炭酸カルシウム（CaCO3）をカ焼して酸化カルシウム（CaO）と炭酸ガス（CO２）を得る方法において、炭酸カルシウム（CaCO3）と炭素燃料との混合物を水蒸気分圧５０〜８０％、酸素（O２）を分圧２０〜５０％の雰囲気下、温度７５０〜１０００℃以下の条件でカ焼することを特徴とする炭酸カルシウム（CaCO3）カ焼方法。 Embodiments of the present invention are as follows.
(1) In a method of calcining calcium carbonate (CaCO 3 ) to obtain calcium oxide (CaO) and carbon dioxide (CO 2 ), water vapor partial pressure 50 to 80%, carbon dioxide partial pressure 20 to 50% (total pressure) A calcium carbonate (CaCO 3 ) calcining method characterized by calcining under a temperature of 750 to 1000 ° C. under an atmosphere of 0.05 to 0.15 MPa.
(2) The calcium carbonate (CaCO 3 ) calcining method described in (1) above, wherein the atmosphere is a water vapor partial pressure of 60%, a carbon dioxide partial pressure of 40%, and a temperature of 950.
(3) In a method of calcining calcium carbonate (CaCO 3 ) to obtain calcium oxide (CaO) and carbon dioxide (CO 2 ), a mixture of calcium carbonate (CaCO 3 ) and carbon fuel is converted to a water vapor partial pressure of 50 to 80 %, Oxygen (O 2 ) is calcined under a temperature of 750 to 1000 ° C. in an atmosphere having a partial pressure of 20 to 50%, and the calcium carbonate (CaCO 3 ) calcining method.

炭酸カルシウム（CaCO3）（石灰石）１０ｋｇを、水蒸気分圧６０％、炭酸ガス分圧４０％、（全圧0.1Mpa）の雰囲気下、温度９１０〜９５０℃の条件でカ焼した。
酸化カルシウム（CaO）約5.6Ｋｇ、炭酸ガス（CO２）4.4Ｋｇが得られた。得られた酸化カルシウム（CaO）は、炭酸ガス（CO２）の吸収性を図２に示す。図２は、従来法と本件からほぼ同じカ焼率の95-97%を得た試料のCO2吸収反応性である。従来法でカ焼した試料のCO2吸収率は約40%に対して、本件のCO2/steam雰囲気下でカ焼した試料のCO2吸収率はかなり高く約65%に達したことが判る。
10 kg of calcium carbonate (CaCO 3 ) (limestone) was calcined under the conditions of a temperature of 910 to 950 ° C. in an atmosphere of a water vapor partial pressure of 60%, a carbon dioxide partial pressure of 40%, and a total pressure of 0.1 Mpa.
About 5.6 kg of calcium oxide (CaO) and 4.4 kg of carbon dioxide (CO 2 ) were obtained. The obtained calcium oxide (CaO) has carbon dioxide (CO 2 ) absorbability shown in FIG. FIG. 2 shows the CO 2 absorption reactivity of a sample that obtained 95-97% of the same calcining rate from the conventional method and this case. Respect calcined was CO 2 absorption rate of about 40% of the samples by the conventional method, CO 2 absorption rate of the calcined samples under CO 2 /? Steam atmosphere this matter it can be seen that reaching much higher about 65% .

炭酸カルシウム（CaCO3）＜水分含有率1％＞1０ｋｇと石炭粉末3Ｋｇを、酸素濃度4０％水蒸気濃度6０％（全圧0.1Mpa）で燃焼し、温度９１０〜９５０℃の条件でカ焼した。
酸化カルシウム（CaO）5.6Ｋｇ、炭酸ガス（CO２）6.4Ｋｇが得られた。得られた酸化カルシウム（CaO）の炭酸ガス（CO２）の吸収性は、実施例１とほぼ同じであった。
本実施例の概要を図３に示す。 10 kg of calcium carbonate (CaCO 3 ) <water content 1%> and 3 kg of coal powder were burned at an oxygen concentration of 40% and a water vapor concentration of 60% (total pressure 0.1 Mpa), and calcined at a temperature of 910 to 950 ° C.
5.6 kg of calcium oxide (CaO) and 6.4 kg of carbon dioxide (CO 2 ) were obtained. The absorbability of carbon dioxide (CO 2 ) of the obtained calcium oxide (CaO) was almost the same as in Example 1.
An outline of the present embodiment is shown in FIG.

本発明のカ焼方法は、生成したCO2と水蒸気は、後流で分離、回収が容易であるので、従来のカ焼方法に直接適用できる。また、低温で効率良く炭酸カルシウム（CaCO3）のカ焼を行うことができるため、環境に優しい手法であり、産業上の利用可能性が高いものである。 The calcining method of the present invention can be directly applied to the conventional calcining method because the produced CO2 and water vapor are easily separated and recovered in the downstream. In addition, since calcium carbonate (CaCO 3 ) can be calcined efficiently at low temperature, it is an environmentally friendly method and has high industrial applicability.

CO2のみの雰囲気下（従来技術）と、本件発明のCO2/steam雰囲気下のカ焼率Calcination rate under CO 2 only atmosphere (conventional technology) and CO 2 / steam atmosphere of the present invention 従来法と本件からほぼ同じカ焼率の95-97%を得た試料のCO2吸収反応性CO 2 absorption reactivity of samples with 95-97% calcination rate almost the same as the conventional method and this case 実施例２の概念図Conceptual diagram of Example 2

Claims (3)

炭酸カルシウム（CaCO3）をカ焼して酸化カルシウム（CaO）と炭酸ガス（CO２）を得る方法において、水蒸気分圧５０〜8０％、炭酸ガス分圧２０〜５０％（全圧0.05−0.15Mpa）の雰囲気下、温度７５０〜１０００℃以下の条件でカ焼することを特徴とする炭酸カルシウム（CaCO3）カ焼方法。 In a method of calcining calcium carbonate (CaCO 3 ) to obtain calcium oxide (CaO) and carbon dioxide gas (CO 2 ), water vapor partial pressure 50 to 80%, carbon dioxide partial pressure 20 to 50% (total pressure 0.05-0.15) Calcium carbonate (CaCO 3 ) calcining method, characterized in that calcining is performed under a temperature of 750 to 1000 ° C. in an atmosphere of Mpa). 雰囲気が、水蒸気分圧６０％、炭酸ガス分圧４０％、温度９５０である請求１に記載した炭酸カルシウム（CaCO3）カ焼方法。 The calcium carbonate (CaCO 3 ) calcining method according to claim 1, wherein the atmosphere is a water vapor partial pressure of 60%, a carbon dioxide partial pressure of 40%, and a temperature of 950. 炭酸カルシウム（CaCO3）をカ焼して酸化カルシウム（CaO）と炭酸ガス（CO２）を得る方法において、炭酸カルシウム（CaCO3）と炭素燃料との混合物を水蒸気濃度５０〜８０％、酸素（O２）濃度２０〜５０％のガスで燃焼し、温度７５０〜１０００℃以下の条件でカ焼することを特徴とする炭酸カルシウム（CaCO3）カ焼方法。

In a method of calcining calcium carbonate (CaCO 3 ) to obtain calcium oxide (CaO) and carbon dioxide gas (CO 2 ), a mixture of calcium carbonate (CaCO 3 ) and carbon fuel has a water vapor concentration of 50 to 80%, oxygen ( A calcium carbonate (CaCO 3 ) calcining method characterized by burning with a gas having a concentration of O 2 ) of 20 to 50% and calcining at a temperature of 750 to 1000 ° C. or less.

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CN114349037A (en) * 2022-01-02 2022-04-15 广西师范大学 Preparation method and application of black calcium carbonate

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CN114349037A (en) * 2022-01-02 2022-04-15 广西师范大学 Preparation method and application of black calcium carbonate
CN114349037B (en) * 2022-01-02 2023-09-15 广西师范大学 Preparation method and application of black calcium carbonate

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