JPH0894598A - Measuring device for readily evaluating separative power of ceramic to separate nitrogen from carbon dioxide - Google Patents

Measuring device for readily evaluating separative power of ceramic to separate nitrogen from carbon dioxide

Info

Publication number
JPH0894598A
JPH0894598A JP30593193A JP30593193A JPH0894598A JP H0894598 A JPH0894598 A JP H0894598A JP 30593193 A JP30593193 A JP 30593193A JP 30593193 A JP30593193 A JP 30593193A JP H0894598 A JPH0894598 A JP H0894598A
Authority
JP
Japan
Prior art keywords
carbon dioxide
nitrogen
sample
measuring device
gas
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.)
Granted
Application number
JP30593193A
Other languages
Japanese (ja)
Other versions
JP2642856B2 (en
Inventor
Masakazu Horio
正和 堀尾
Kenji Suzuki
憲司 鈴木
Toshiaki Mori
聰明 森
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
National Institute of Advanced Industrial Science and Technology AIST
Original Assignee
Agency of Industrial Science and Technology
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Agency of Industrial Science and Technology filed Critical Agency of Industrial Science and Technology
Priority to JP5305931A priority Critical patent/JP2642856B2/en
Publication of JPH0894598A publication Critical patent/JPH0894598A/en
Application granted granted Critical
Publication of JP2642856B2 publication Critical patent/JP2642856B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Abstract

PURPOSE: To enable readily evaluating the separative power of ceramics to separate nitrogen from carbon dioxide by providing a sample-packed portion, a sample heating portion, an analytical portion, a recording portion, and a nitrogen/carbon dioxide injecting portion. CONSTITUTION: A sample-packed portion 1 is a stainless steel or glass pipe about 3mmϕ in bore and about 1m long and filled with a ceramics sample. A sample heating portion 2 is an electric furnace having a temperature controller 3 for keeping temperature constant. An analytical portion 4 is a TCD-equipped gas chromatograph and its data are recorded by a recording portion 5. Lines are connected together by a stainless steel or glass pipe, through which helium is circulated as a carrier gas by about 20ml/min. A nitrogen/carbon dioxide injecting portion 6 having a rubber plug mounted in a lateral hole bored in the pipe is provided in front of the packed portion 1, and mixed gases of nitrogen and carbon dioxide are introduced from the portion 6 to start measurements. Evaluation of separative power can be made quickly and easily since it can be achieved by simply checking the retention times of the nitrogen and the carbon dioxide, which are described at the recording portion 5.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】今日、地球規模の温暖化が大きな
社会問題となりつつあり、その主要原因物質のひとつは
工場等から排出される二酸化炭素であると言われてい
る。地球温暖化を解決するには、既に排出された二酸化
炭素を回収して固定したり、排ガス発生源での高濃度か
つ高温二酸化炭素の分離・回収等の技術開発が急務であ
る。高温二酸化炭素の分離・回収には有機系分離材料で
は耐熱性に問題があり、使用することができない。した
がって、熱的に安定なセラミックスが分離材料の有力候
補に挙がるが、その二酸化炭素分離能評価は出来る限り
簡便かつ迅速に行えることが望まれる。しかるに、本発
明は、窒素と二酸化炭素の分離能を簡便かつ迅速に評価
する装置を提供するものである。
[Industrial application] Today, global warming is becoming a major social problem, and one of the main causative substances is carbon dioxide emitted from factories and the like. In order to solve global warming, there is an urgent need for technological development such as collecting and fixing already emitted carbon dioxide, and separating and recovering high-concentration and high-temperature carbon dioxide at an exhaust gas source. Organic separation materials cannot be used for separation / recovery of high-temperature carbon dioxide because of problems with heat resistance. Therefore, thermally stable ceramics are listed as a strong candidate for the separation material, but it is desired that the carbon dioxide separation ability can be evaluated as easily and quickly as possible. Therefore, the present invention provides a device for easily and quickly evaluating the separation ability of nitrogen and carbon dioxide.

【0002】[0002]

【従来の技術】従来、セラミックスの窒素と二酸化炭素
の分離能は、ガス吸着量測定装置によりそれぞれの吸着
等温線を測定して評価している。ガス吸着量測定装置に
よる吸着等温線の測定は、定圧定容のガスを試料に1パ
ルス毎に導入し、各パルス毎に吸着平衡に達するまで放
置する。1パルス毎の吸着平衡に達するまでの時間は、
短くて数分間、長いと1時間程度にもなる。したがっ
て、吸着等温線を測定する時間は非常に長く、1試料を
測定するのに24時間を費やすこともよくある。また、
ガス吸着量測定装置は非常に高価な物である。
2. Description of the Related Art Conventionally, the ability of ceramics to separate nitrogen and carbon dioxide has been evaluated by measuring the respective adsorption isotherms of a gas adsorption amount measuring device. In the measurement of the adsorption isotherm by the gas adsorption amount measuring device, a gas at a constant pressure and a constant volume is introduced into the sample for each pulse, and the sample is left until the equilibrium is reached for each pulse. The time to reach adsorption equilibrium for each pulse is
It can be as short as a few minutes and as long as an hour. Therefore, the time to measure the adsorption isotherm is very long, and it often takes 24 hours to measure one sample. Also,
The gas adsorption amount measuring device is very expensive.

【0003】[0003]

【発明が解決しようとする課題】工場等の固定発生源か
ら排出される高温状態の窒素と二酸化炭素を分離するセ
ラミックス分離材を開発する場合、評価に多大な経費や
時間を費やすことなく、簡便かつ迅速に行えることが求
められている。本発明は、セラミックスの窒素と二酸化
炭素の分離能を簡便かつ迅速に測定する装置を提供する
ものである。
SUMMARY OF THE INVENTION When developing a ceramic separation material for separating nitrogen and carbon dioxide in a high-temperature state discharged from a fixed source such as a factory, it is simple to use without much expenditure and time for evaluation. It is required to be able to do it quickly. The present invention provides a device for simply and quickly measuring the ability of ceramics to separate nitrogen and carbon dioxide.

【0004】[0004]

【課題を解決するための手段】本発明は、セラミックス
の窒素と二酸化炭素の分離能を簡便かつ迅速に測定する
装置を提供するものである。
SUMMARY OF THE INVENTION The present invention provides an apparatus for simply and quickly measuring the ability of ceramics to separate nitrogen and carbon dioxide.

【0005】セラミックスにガスを接触させるとガスは
セラミックスの表面に吸着し、しばらくしてから脱離す
る。ガス吸着はセラミックスの温度の低いときは物理吸
着と化学吸着の両方が生じるが、温度が高くなると化学
吸着のみが生じることになる。これを換言すれば、物理
吸着は弱い吸着であり、化学吸着は強い吸着である。ガ
スがセラミックス表面に吸着してから脱離するまでの時
間をリテンションタイムと定義すると、リテンションタ
イムはガスの吸着能あるいは脱離能の強さに相当する。
すなわち、リテンションタイムが長い場合はガスがセラ
ミックス表面に強く吸着しており、容易に脱離しない状
態であることを示唆している。一方、リテンションタイ
ムが短い場合はガスとセラミックス表面との相互作用は
弱く、ガスは容易にセラミックス表面から脱離すること
を示唆している。したがって、セラミックスに対する窒
素と二酸化炭素のそれぞれのリテンションタイムを測定
し、それらの差を求め、その差が大きいほど窒素と二酸
化炭素の分離能は優れていることになる。
When a gas is brought into contact with ceramics, the gas is adsorbed on the surface of the ceramics and desorbed after a while. In gas adsorption, when the temperature of the ceramics is low, both physical adsorption and chemical adsorption occur, but when the temperature is high, only chemical adsorption occurs. In other words, physical adsorption is weak adsorption and chemical adsorption is strong adsorption. If the retention time is defined as the time from when the gas is adsorbed on the ceramic surface to when it is desorbed, the retention time corresponds to the strength of gas adsorption or desorption.
That is, it is suggested that when the retention time is long, the gas is strongly adsorbed on the ceramic surface and is not easily desorbed. On the other hand, when the retention time is short, the interaction between the gas and the ceramic surface is weak, suggesting that the gas is easily desorbed from the ceramic surface. Therefore, the retention times of nitrogen and carbon dioxide with respect to the ceramics are measured, the difference between them is determined, and the larger the difference, the better the separability of nitrogen and carbon dioxide.

【0006】以上の原理を利用して作成した本発明の測
定装置を図1に示す。装置は試料充填部(1)、試料加
熱部(2)、分析部(4)、記録部(5)、窒素/二酸
化炭素注入部(6)から成る。試料充填部はセラミック
ス試料を充填する部分であり、内径3mmφ、長さ1m
程度のステンレス製あるいはガラス製のパイプである。
パイプの材質および規格は、測定する試料の種類あるい
は測定条件により適当に選べばよい。直管でもU字管で
も形状は構わない。試料加熱部は電気炉であり、試料温
度を一定に保持する温度制御装置(3)の付いているこ
とが望ましい。また、電気炉の規格は測定する温度によ
り適当に選べばよい。分析部はTCD付ガスクロマトグ
ラフイ であり、デ−タはペンレコ−ダに記録させる。ガ
スクロマトグラフイ の検出器にはFIDとTCDの2種
類があるが、前者は無機ガスに対して全く感知しないこ
とから、後者の検出器を有するガスクロマトグラフイ を
用いる。ラインはステンレス製あるいはガラス製のパイ
プでつながれており、キャリア−ガスとしてヘリウムを
20ml/min程度流す。試料充填部の前にパイプに
横穴を開けてゴム栓を取り付けた窒素/二酸化炭素注入
部がある。ここからマイクロシリンジに採った窒素と二
酸化炭素の混合ガスを打ち込み、測定を開始する。窒素
/二酸化炭素注入部にガスサンプラ−を取り付ければガ
スの注入はより容易になる。
FIG. 1 shows a measuring device of the present invention produced by utilizing the above principle. The device comprises a sample filling section (1), a sample heating section (2), an analysis section (4), a recording section (5) and a nitrogen / carbon dioxide injection section (6). The sample filling part is a part for filling the ceramics sample, and the inner diameter is 3 mmφ and the length is 1 m.
It is a pipe made of stainless steel or glass.
The material and standard of the pipe may be appropriately selected according to the type of sample to be measured or the measurement conditions. The shape may be a straight pipe or a U-shaped pipe. The sample heating unit is an electric furnace, and is desirably provided with a temperature control device (3) for keeping the sample temperature constant. The specification of the electric furnace may be appropriately selected depending on the temperature to be measured. The analyzer is a gas chromatograph with a TCD, and the data is recorded on a pen recorder. There are two types of gas chromatograph detectors, FID and TCD, but since the former does not sense inorganic gas at all, gas chromatographs with the latter detector are used. The lines are connected by stainless steel or glass pipes, and helium flows at a flow rate of about 20 ml / min as a carrier gas. There is a nitrogen / carbon dioxide injection unit in which a horizontal hole is made in the pipe and a rubber stopper is attached in front of the sample filling unit. From here, a mixed gas of nitrogen and carbon dioxide taken into the micro syringe is injected to start the measurement. If a gas sampler is attached to the nitrogen / carbon dioxide injection part, gas injection becomes easier.

【0007】本発明の測定装置を用いれば測定時間は、
1試料当たり短い場合で5分、長い場合でも10分程度
で終了する。また、分離能はペンレコ−ダに描かれた窒
素と二酸化炭素のそれぞれのリテンションタイムを調べ
るだけでよいので評価も非常に早く、簡単である。
With the measuring device of the present invention, the measuring time is
The processing is completed in about 5 minutes for a short sample and about 10 minutes for a long sample. Further, the resolution is very quick and simple because the retention time of each of nitrogen and carbon dioxide drawn on the pen recorder needs to be examined.

【0008】本発明の窒素/二酸化炭素分離能測定装置
を用いて測定した実例を以下の実施例にて示す。
[0008] An example of measurement using the apparatus for measuring nitrogen / carbon dioxide separation ability of the present invention is shown in the following examples.

【0009】[0009]

【実施例】【Example】

【0010】実施例 1 セラミックス試料にシリカゲルの5.0gを選び、内径
3mmφ、長さ1mのステンレス製カラムに充填し、1
00℃に加熱した。キャリア−ガスを20ml/min
流し、窒素と二酸化炭素の1mlづつをマイクロシリン
ジに採り、窒素/二酸化炭素注入部より試料中に打ち込
んだ。打ち込んだ時間を0分とし、シリカゲルから脱離
してくる窒素および二酸化炭素をガスクロマトグラフイ
で測定し、リテンションタイムを調べた。得られたチャ
−トを図2に示すが、窒素(7)と二酸化炭素(8)の
リテンションタイムは、前者が0.54分、後者が1.
29分であり、この結果シリカゲルは100℃において
両者のガスを分離することが可能であることが判明し
た。測定時間は2分程度である。
Example 1 5.0 g of silica gel was selected as a ceramic sample and packed in a stainless steel column having an inner diameter of 3 mm and a length of 1 m.
Heated to 00 ° C. Carrier gas 20ml / min
The mixture was poured, and 1 ml each of nitrogen and carbon dioxide was taken in a microsyringe and injected into the sample from a nitrogen / carbon dioxide injection part. The nitrogen and carbon dioxide desorbed from the silica gel are gas chromatographed with the time of implantation set to 0 minutes.
And retention time was examined. The resulting chart is shown in FIG. 2. The retention times of nitrogen (7) and carbon dioxide (8) were 0.54 minutes for the former and 1.0 for the latter.
It was 29 minutes, and as a result, it was found that the silica gel can separate both gases at 100 ° C. The measurement time is about 2 minutes.

【0011】実施例 2 セラミックス試料にモレキュラ−シ−ブ13Xの4.0
gを選び、内径3mmφ、長さ1mのステンレス製カラ
ムに充填し、300℃に加熱した。キャリア−ガスを2
0ml/min流し、窒素と二酸化炭素の1mlづつを
マイクロシリンジに採り、窒素/二酸化炭素注入部より
試料中に打ち込んだ。打ち込んだ時間を0分とし、シリ
カゲルから脱離してくる窒素および二酸化炭素をガスク
ロマトグラフイ で測定し、リテンションタイムを調べ
た。得られたチャ−トを図3に示すが、窒素(7)と二
酸化炭素(8)のリテンションタイムは、前者が0.8
5分、後者が3.00分であり、この結果モレキュラ−
シ−ブ13Xは300℃において両者のガスを分離する
ことが可能であることが判明した。測定時間は4分程度
である。
Example 2 A ceramic sample having a molecular sieve 13X of 4.0 was used.
g was selected, packed in a stainless steel column having an inner diameter of 3 mmφ and a length of 1 m, and heated to 300 ° C. Carrier-gas 2
Flowing at 0 ml / min, 1 ml each of nitrogen and carbon dioxide was collected in a microsyringe, and was injected into the sample from the nitrogen / carbon dioxide injection part. The retention time was examined by measuring the nitrogen and carbon dioxide desorbed from the silica gel by gas chromatography with the time of implantation being 0 minute. The chart obtained is shown in Fig. 3. The retention time of nitrogen (7) and carbon dioxide (8) was 0.8 for the former.
5 minutes, the latter being 3.00 minutes, resulting in molecular
It was found that the sheave 13X can separate both gases at 300 ° C. The measurement time is about 4 minutes.

【0012】[0012]

【発明の効果】本発明は、窒素/二酸化炭素分離材を開
発するときに必要な性能評価を簡便かつ迅速に測定する
ことのできる装置を提供するものであり、セラミックス
分離材の製品開発に多大な貢献を及ぼすものと考えられ
る。
The present invention provides an apparatus which can easily and quickly measure the performance evaluation required for developing a nitrogen / carbon dioxide separating material, and is very useful for developing a ceramic separating material. It is considered to make a significant contribution.

【図面の簡単な説明】[Brief description of drawings]

【図1】本発明の構成図。FIG. 1 is a configuration diagram of the present invention.

【図2】100℃に加熱したシリカゲルの窒素と二酸化
炭素のクロマトグラフ。
FIG. 2 is a chromatogram of nitrogen and carbon dioxide on silica gel heated to 100 ° C.

【図3】300℃に加熱したモレキュラ−シ−ブ13X
の窒素と二酸化炭素のクロマトグラフ。
FIG. 3 Molecular sieve 13X heated to 300 ° C.
Nitrogen and carbon dioxide chromatograph.

【符号の説明】[Explanation of symbols]

1 試料充填部 2 試料加熱部 3 温度制御装置 4 分析部 5 記録部 6 窒素/二酸化炭素注入部 7 窒素のクロマトグラフ 8 二酸化炭素のクロマトグラフ DESCRIPTION OF SYMBOLS 1 Sample filling part 2 Sample heating part 3 Temperature control device 4 Analysis part 5 Recording part 6 Nitrogen / carbon dioxide injection part 7 Chromatograph of nitrogen 8 Chromatograph of carbon dioxide

Claims (2)

【特許請求の範囲】[Claims] 【請求項1】 セラミックスの窒素と二酸化炭素の分離
能を簡便に評価する測定装置。
1. A measuring device for easily evaluating the ability of ceramics to separate nitrogen and carbon dioxide.
【請求項2】 該測定装置は試料充填部、試料加熱部、
分析部、記録部、窒素/二酸化炭素注入部から成る、請
求項1に記載の分離能を簡便に評価する測定装置。
2. The measuring device comprises a sample filling section, a sample heating section,
The measuring device according to claim 1, which comprises an analysis unit, a recording unit, and a nitrogen / carbon dioxide injection unit, for easily evaluating the separability.
JP5305931A 1993-11-10 1993-11-10 Measuring device for easily evaluating the separation ability of ceramics for nitrogen and carbon dioxide Expired - Lifetime JP2642856B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP5305931A JP2642856B2 (en) 1993-11-10 1993-11-10 Measuring device for easily evaluating the separation ability of ceramics for nitrogen and carbon dioxide

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP5305931A JP2642856B2 (en) 1993-11-10 1993-11-10 Measuring device for easily evaluating the separation ability of ceramics for nitrogen and carbon dioxide

Publications (2)

Publication Number Publication Date
JPH0894598A true JPH0894598A (en) 1996-04-12
JP2642856B2 JP2642856B2 (en) 1997-08-20

Family

ID=17951026

Family Applications (1)

Application Number Title Priority Date Filing Date
JP5305931A Expired - Lifetime JP2642856B2 (en) 1993-11-10 1993-11-10 Measuring device for easily evaluating the separation ability of ceramics for nitrogen and carbon dioxide

Country Status (1)

Country Link
JP (1) JP2642856B2 (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115728123A (en) * 2022-11-15 2023-03-03 中海石油(中国)有限公司 Evaluation experiment method for simulating hydrogen sulfide output in thermal recovery process

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03110444A (en) * 1989-09-25 1991-05-10 Mitsubishi Kasei Corp Method and device for measuring adsorption performance of solid adsorbent
JPH04166763A (en) * 1990-10-30 1992-06-12 Nippon Carbon Co Ltd Adsorbing type gas chromatography packing agent and preparation thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03110444A (en) * 1989-09-25 1991-05-10 Mitsubishi Kasei Corp Method and device for measuring adsorption performance of solid adsorbent
JPH04166763A (en) * 1990-10-30 1992-06-12 Nippon Carbon Co Ltd Adsorbing type gas chromatography packing agent and preparation thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115728123A (en) * 2022-11-15 2023-03-03 中海石油(中国)有限公司 Evaluation experiment method for simulating hydrogen sulfide output in thermal recovery process

Also Published As

Publication number Publication date
JP2642856B2 (en) 1997-08-20

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