JPS6232123B2 - - Google Patents
Info
- Publication number
- JPS6232123B2 JPS6232123B2 JP54092895A JP9289579A JPS6232123B2 JP S6232123 B2 JPS6232123 B2 JP S6232123B2 JP 54092895 A JP54092895 A JP 54092895A JP 9289579 A JP9289579 A JP 9289579A JP S6232123 B2 JPS6232123 B2 JP S6232123B2
- Authority
- JP
- Japan
- Prior art keywords
- gas
- component
- carbon material
- conversion
- acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 239000003575 carbonaceous material Substances 0.000 claims description 16
- 238000006243 chemical reaction Methods 0.000 claims description 14
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 4
- 230000003213 activating effect Effects 0.000 claims description 3
- 238000003672 processing method Methods 0.000 claims description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 239000011261 inert gas Substances 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 1
- 239000007789 gas Substances 0.000 description 30
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 238000001994 activation Methods 0.000 description 5
- 229910001873 dinitrogen Inorganic materials 0.000 description 5
- 239000003595 mist Substances 0.000 description 5
- 230000004913 activation Effects 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 3
- 229910001882 dioxygen Inorganic materials 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 230000009931 harmful effect Effects 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- AXDJCCTWPBKUKL-UHFFFAOYSA-N 4-[(4-aminophenyl)-(4-imino-3-methylcyclohexa-2,5-dien-1-ylidene)methyl]aniline;hydron;chloride Chemical compound Cl.C1=CC(=N)C(C)=CC1=C(C=1C=CC(N)=CC=1)C1=CC=C(N)C=C1 AXDJCCTWPBKUKL-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000012080 ambient air Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 206010022000 influenza Diseases 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 235000019362 perlite Nutrition 0.000 description 1
- 239000010451 perlite Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- XTQHKBHJIVJGKJ-UHFFFAOYSA-N sulfur monoxide Chemical class S=O XTQHKBHJIVJGKJ-UHFFFAOYSA-N 0.000 description 1
- 229910052815 sulfur oxide Inorganic materials 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Landscapes
- Exhaust Gas Treatment By Means Of Catalyst (AREA)
- Carbon And Carbon Compounds (AREA)
- Catalysts (AREA)
Description
本発明は環境大気、排気ガス等、種々の気体中
に含有されるSO3成分を選択的にSO2に変換する
際に還元触媒として使用されるSO3／SO2変換用
カーボン材料の活性化処理法に関する。
煙道からの燃焼排気カス、自動車排気ガス等の
各種排気ガスはSO2，SO3等のイオウ酸化物（以
下、これをSOxという。）、NO，NO2等の窒素酸
化物（以下、これをNOxという。）等、種々の有
害成分を多く含有するため、これを大気中に無制
限に排出したのでは環境大気は増々汚染されるこ
とになる。このため、前記排気ガスを大気中に排
出するに当り、現今では大気汚染防止の立場から
厳しい法規制を受けている。このため、前記排気
ガスは大気中に排出するに先立つてSO2測定器、
NO2測定器などの分析計を用いてこれら有害成分
量を測定して管理することが必要である。また、
環境大気も前述と同様、有害成分量を測定して常
に管理することが必要である。特にSO3成分は共
存する水分と反応して徴細な硫酸ミストを形成す
るが、この硫酸ミストは露点が高くしかも腐食性
を有するため、SO3成分を含有する気体を各種分
析計を用いて測定する際に、分析計における配管
の腐食および検出部の汚染による感度低下等、
種々の弊害をひき起こす。このため、環境大気、
排気ガス等、測定すべき各種気体からSO3成分を
除去すること、あるいは気体中のSOx成分ないし
はSO3成分を測定することは重要な問題である。
気体中のSO3成分の除去、すなわち硫酸ミスト
の除去に際して、従来、ガラス繊維ろ紙等のフイ
ルタあるいはパーライト等の吸着剤が利用されて
いるが、徴細な硫酸ミストの完全な除去は不可能
であり、また、除去効率を高めようとすると圧力
損失が大きくなり、実用的でなくなる等の欠点が
あつた。
また、気体、特に排気ガス中のSOx成分の測定
に際して、従来、赤外線式のSO2ガス分析計が用
いられているが、SOx成分のうち数パーセントを
占めるといわれているSO3（大部分は硫酸ミスト
として存在するものと思われる）の測定は行なう
ことができないという欠点がある。（なお、環境
大気中のSO2成分の測定に際しては赤外線分析法
は不適であり、ロザニリン・ホルマリン法等を用
いることになる。）
このような欠点を改良するため、本発明者は環
境大気、各種排気ガス等、気体中のSO3成分を選
択的にしかも高効率でSO2に変換して前記気体か
らSO3成分の除去、あるいはSOx成分ないしは
SO3成分の測定を行ないうるSO3／SO2変換法を
開発し、本件と同一出願人により特許出願中であ
る。（特開昭55―32758号）
この先願にかかる発明によれば、SO3成分を含
有する気体を320℃〜500℃の温度に加熱されたカ
ーボンを主成分とする材料に接触させて該気体中
のSO3成分を選択的に、しかも高効率でSO2に変
換し、これによつて前記気体からSO3成分の除
去、あるいはSOx成分ないしはSO3成分の測定を
行なうことを特徴とする。
本発明の目的は前述の先願にかかる発明におい
て使用するカーボンを主成分とする材料、すなわ
ち、カーボン材料を高活性化する処理方法を提供
することにある。いいかえれば、本発明の目的は
SO3／SO2変換活性の高いSO3／SO2変換用カーボ
ン触媒を得ることにある。
前述の目的を達成するため、本発明によれば、
SO3／SO2変換用カーボン材料に次の工程を施す
ことを特徴とする。
前記カーボン材料を酸化性を有する酸で処理し
た後、不活性ガス雰囲気中で300℃〜700℃の温度
で加熱処理を行なう工程。（活性化処理工程）
以下、本発明を具体的に詳述する。まず。カー
ボン材料を還元触媒として用いたSO3／SO2変換
法を第１図を用いて説明する。第１図は前述
SO3／SO2変換法を実施するための実験装置であ
る。本装置においてはまず、SO3成分を含有する
気体（試験ガス）を調製し、次いでこの試験ガス
中のSO3成分をSO2に変換する。
１はSO2／N2標準混合ガスボンベ、２は酸素ガ
スボンベ、３は窒素ガスボンベである。これらの
ボンベからそれぞれSO2／N2標準混合ガス、酸素
ガスおよび窒素ガスを取出して例えば表１に示す
試験ガスを調製し、これを酸化触媒６上に導く。
ガス流量は1.0l／分（０℃）である。窒素ガスは
加湿器４を通過させて加湿窒素ガスとする。５，
５′、５″はいずれも流量計である。酸化触媒６は
白金／アルミナ触媒（GHSV＝20000）であり、
電気炉７により650℃前後の温度に加熱されてい
る。８は熱電対である。このとき前記試験ガス中
のSO2成分の一部は式
SO2＋１／202→SO3 ……(1)
により酸化されてSO3に変化する。試験ガスの酸
化触媒通過前および通過後の組成を表に示す。
The present invention is aimed at activating a carbon material for SO 3 /SO 2 conversion, which is used as a reduction catalyst when selectively converting SO 3 components contained in various gases such as environmental air and exhaust gas into SO 2 . Regarding processing methods. Various exhaust gases such as combustion exhaust residue from flues and automobile exhaust gas contain sulfur oxides such as SO 2 and SO 3 (hereinafter referred to as SO x ), and nitrogen oxides such as NO and NO 2 (hereinafter referred to as SO x). This is called NOx . For this reason, the discharge of the exhaust gas into the atmosphere is currently subject to strict legal regulations from the standpoint of preventing air pollution. For this reason, before the exhaust gas is discharged into the atmosphere, an SO 2 measuring device is used,
It is necessary to measure and control the amount of these harmful components using an analyzer such as a NO 2 meter. Also,
As mentioned above, the environmental atmosphere also needs to be constantly managed by measuring the amount of harmful components. In particular, the SO 3 component reacts with coexisting moisture to form a fine sulfuric acid mist, but since this sulfuric acid mist has a high dew point and is corrosive, it is necessary to analyze the gas containing the SO 3 component using various analyzers. During measurement, there may be problems such as reduced sensitivity due to corrosion of the analyzer's piping and contamination of the detection part.
It causes various harmful effects. For this reason, the environmental atmosphere,
It is an important problem to remove the SO 3 component from various gases to be measured, such as exhaust gas, or to measure the SO x component or SO 3 component in the gas. Conventionally, filters such as glass fiber filter paper or adsorbents such as perlite have been used to remove the SO 3 component in the gas, that is, to remove sulfuric acid mist, but it is not possible to completely remove the fine sulfuric acid mist. In addition, when attempting to increase the removal efficiency, the pressure loss increases, making it impractical. In addition, infrared SO 2 gas analyzers have traditionally been used to measure SO x components in gases, especially exhaust gas, but SO 3 (large The disadvantage is that it is not possible to measure the amount of sulfuric acid that exists in the form of sulfuric acid mist. (In addition, when measuring SO2 components in the ambient air, infrared analysis is not suitable, and the rosaniline/formalin method etc. will be used.) In order to improve this drawback, the present inventors Selectively and highly efficiently converts the SO 3 component in gases such as various exhaust gases to SO 2 and removes the SO 3 component from the gas, or SO x component or
We have developed an SO 3 /SO 2 conversion method that can measure the three SO components, and are currently applying for a patent by the same applicant. (Japanese Unexamined Patent Publication No. 55-32758) According to the invention of this earlier application, a gas containing SO 3 is brought into contact with a carbon-based material heated to a temperature of 320°C to 500°C. It is characterized by selectively and highly efficiently converting the SO 3 component in the gas into SO 2 , thereby removing the SO 3 component from the gas or measuring the SO x component or SO 3 component. . An object of the present invention is to provide a treatment method for highly activating a material containing carbon as a main component, that is, a carbon material used in the invention according to the aforementioned prior application. In other words, the purpose of the present invention is
The object of the present invention is to obtain a carbon catalyst for SO 3 /SO 2 conversion that has high SO 3 /SO 2 conversion activity. In order to achieve the aforementioned object, according to the present invention:
It is characterized by subjecting the carbon material for SO 3 /SO 2 conversion to the following process. A step of treating the carbon material with an oxidizing acid and then performing a heat treatment at a temperature of 300°C to 700°C in an inert gas atmosphere. (Activation Treatment Step) The present invention will be specifically described in detail below. first. The SO 3 /SO 2 conversion method using a carbon material as a reduction catalyst will be explained using FIG. Figure 1 is mentioned above.
This is an experimental device for implementing the SO 3 /SO 2 conversion method. In this apparatus, first, a gas (test gas) containing an SO 3 component is prepared, and then the SO 3 component in this test gas is converted into SO 2 . 1 is an SO 2 /N 2 standard mixed gas cylinder, 2 is an oxygen gas cylinder, and 3 is a nitrogen gas cylinder. The SO 2 /N 2 standard mixed gas, oxygen gas and nitrogen gas are taken out from these cylinders to prepare, for example, the test gases shown in Table 1, which are introduced onto the oxidation catalyst 6.
The gas flow rate was 1.0 l/min (0°C). The nitrogen gas is passed through a humidifier 4 to become humidified nitrogen gas. 5,
5′ and 5″ are both flow meters.The oxidation catalyst 6 is a platinum/alumina catalyst (GHSV=20000),
It is heated to a temperature of around 650°C by an electric furnace 7. 8 is a thermocouple. At this time, a part of the SO 2 component in the test gas is oxidized and changed to SO 3 according to the formula SO 2 +1/20 2 →SO 3 (1). The composition of the test gas before and after passing through the oxidation catalyst is shown in the table.
まず、市販の試薬を用い、濃硝酸0.5lと濃硫酸
0.5lの混合液（混酸溶液）を調製する。次いでこ
の液中の前述のカーボン材料B1150ｇを撹拌しな
がら徐々に添加した後24時間静置する。次に該液
を口別後、純水を用いて充分に洗浄し、上澄液が
BaCl2溶液を添加してもBaSO4による白濁を呈さ
なくなるようにする。ろ過後該カーボン材料を電
気炉に入れ、窒素気流中150℃の温度で３時間乾
燥した後、さらに600℃に昇温し、３時間加熱処
理を行ない、活性化する。（B1〓）
前述のカーボン材料B1およびこれに活性化処
理の施されたカーボン材料B1〓について、それ
ぞれSO3／SO2変換活性を測定し、結果を第５図
に示した。試験条件は前掲のとおりである。第５
図からこの活性化処理を施こすことにより、かな
りの活性化効果が得られることがわかる。
なお、本発明の処理方法による実験例に関して
は、カーボン材料B1、B1〓について第５図で代
表的に説明したが、他のカーボン材料についても
同様の効果が得られている。
First, using commercially available reagents, add 0.5 liters of concentrated nitric acid and concentrated sulfuric acid.
Prepare 0.5l of mixed solution (mixed acid solution). Next, 150 g of the carbon material B 1 described above was gradually added to this liquid while stirring, and the mixture was allowed to stand for 24 hours. Next, after separating the liquid, wash thoroughly with pure water to remove the supernatant liquid.
Even if BaCl 2 solution is added, it should not become cloudy due to BaSO 4 . After filtration, the carbon material is placed in an electric furnace and dried at 150° C. for 3 hours in a nitrogen stream, then further heated to 600° C. and heat-treated for 3 hours for activation. (B 1 〓) The SO 3 /SO 2 conversion activity of the carbon material B 1 described above and the activated carbon material B 1 〓 was measured, and the results are shown in FIG. The test conditions are as described above. Fifth
It can be seen from the figure that a considerable activation effect can be obtained by performing this activation process. Regarding the experimental example using the treatment method of the present invention, carbon materials B 1 and B 1 〓 were representatively explained with reference to FIG. 5, but similar effects were obtained with other carbon materials.
第１図はSO3／SO2変換法を実施するための実
験装置であり、第２図〜第４図は各種カーボン材
料のSO3／SO2変換活性を示すグラフであり、第
５図は活性化処理の施された各種カーボン材料の
SO3／SO2変換活性を示すグラフである。
１……SO2／N2標準混合ガスボンベ、２……酸
素ガスボンベ、３……窒素ガスボンベ、６……酸
化触媒、７……電気炉、７′……電気炉（変換
器）、８……熱電体、９……活性炭、１１……
SO2検知管。
Figure 1 shows an experimental device for carrying out the SO 3 / SO 2 conversion method, Figures 2 to 4 are graphs showing the SO 3 /SO 2 conversion activity of various carbon materials, and Figure 5 is a graph showing the SO 3 /SO 2 conversion activity of various carbon materials. Various activated carbon materials
It is a graph showing SO 3 /SO 2 conversion activity. 1... SO 2 /N 2 standard mixed gas cylinder, 2... Oxygen gas cylinder, 3... Nitrogen gas cylinder, 6... Oxidation catalyst, 7... Electric furnace, 7'... Electric furnace (converter), 8... Thermoelectric body, 9...Activated carbon, 11...
SO 2 detection tube.
Claims (1)
する酸で処理した後、不活性ガス雰囲気中で300
℃〜700℃の温度で加熱処理を行なうことを特徴
とするSO3／SO2変換用カーボン材料の活性化処
理法。 ２ 特許請求の範囲第１項に記載の処理法におい
て、酸化性を有する酸は混酸、硝酸または熱濃硫
酸である処理法。 ３ 特許請求の範囲第１項に記載の処理法におい
て、加熱処理はカーボン材料を前記酸化性を有す
る酸で処理した後、洗浄し、次いで乾燥してから
行なうことを特徴とする処理法。 ４ 特許請求の範囲第３項に記載の処理法におい
て、前記乾燥は不活性ガス雰囲気中で加熱して行
なうことを特徴とする処理法。[Claims] 1. After treating the carbon material for SO 3 /SO 2 conversion with an oxidizing acid,
A method for activating a carbon material for SO 3 /SO 2 conversion, characterized by performing heat treatment at a temperature of ℃ to 700 ℃. 2. The treatment method according to claim 1, wherein the oxidizing acid is a mixed acid, nitric acid, or hot concentrated sulfuric acid. 3. The processing method according to claim 1, wherein the heat treatment is performed after the carbon material is treated with the oxidizing acid, washed, and then dried. 4. The processing method according to claim 3, wherein the drying is performed by heating in an inert gas atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9289579A JPS5617634A (en) | 1979-07-21 | 1979-07-21 | Activating treatment of carbon material for so3/so2 conversion |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9289579A JPS5617634A (en) | 1979-07-21 | 1979-07-21 | Activating treatment of carbon material for so3/so2 conversion |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5617634A JPS5617634A (en) | 1981-02-19 |
| JPS6232123B2 true JPS6232123B2 (en) | 1987-07-13 |
Family
ID=14067187
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9289579A Granted JPS5617634A (en) | 1979-07-21 | 1979-07-21 | Activating treatment of carbon material for so3/so2 conversion |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5617634A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4624937A (en) * | 1984-05-10 | 1986-11-25 | Monsanto Company | Process for removing surface oxides from activated carbon catalyst |
| JP2554689Y2 (en) * | 1992-02-14 | 1997-11-17 | アイワ株式会社 | Display of operation body in audio equipment, etc. |
| IT1301999B1 (en) * | 1998-08-05 | 2000-07-20 | Enichem Spa | CATALYST, PROCESS FOR THE PRODUCTION OF OXYGEN WATER AND ITS USE IN OXIDATION PROCESSES. |
-
1979
- 1979-07-21 JP JP9289579A patent/JPS5617634A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5617634A (en) | 1981-02-19 |
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