JPS59147618A - Process for regenerating adsorbent in high degree purification apparatus for gas - Google Patents

Process for regenerating adsorbent in high degree purification apparatus for gas

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Publication number
JPS59147618A
JPS59147618A JP58021818A JP2181883A JPS59147618A JP S59147618 A JPS59147618 A JP S59147618A JP 58021818 A JP58021818 A JP 58021818A JP 2181883 A JP2181883 A JP 2181883A JP S59147618 A JPS59147618 A JP S59147618A
Authority
JP
Japan
Prior art keywords
gas
adsorbent
temp
regeneration
low
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
JP58021818A
Other languages
Japanese (ja)
Other versions
JPH0372327B2 (en
Inventor
Masahiro Nakao
中尾 正博
Norio Moriya
則雄 守屋
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.)
Resonac Holdings Corp
Original Assignee
Showa Denko KK
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 Showa Denko KK filed Critical Showa Denko KK
Priority to JP58021818A priority Critical patent/JPS59147618A/en
Publication of JPS59147618A publication Critical patent/JPS59147618A/en
Publication of JPH0372327B2 publication Critical patent/JPH0372327B2/ja
Granted legal-status Critical Current

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  • Separation Of Gases By Adsorption (AREA)

Abstract

PURPOSE:To perform reasonably the regeneration of a low temp. adsorbent in a low temp. adsorption column of a high degree purification apparatus of gas by specifying the compsn. of the gas to be purified in the low temp. adsorption column and simultaneously by regulating the regeneration temp. to the ordinary temp. CONSTITUTION:For the purification of gas such as H2, He, Ar, etc. to a very high purity, the concn. of impurities contained in the gas is reduced by passing the gas through an ordinary temp. adsorption cylinder, and purified further by passing through a low temp. adsorption column packed with a low temp. adsorbent such as zeolite and cooled to deep temp. by liquefied N2 etc. The regeneration of the low temp. adsorbent is performed by passing purified gas heated to the room temp., but the regeneration may be performed more efficiently with less consumption of purified gas for the regeneration and heating energy if the content of moisture and CO2 in the feed gas to be purified in the low temp. adsorption column are both <=1ppm.

Description

【発明の詳細な説明】 本発明は、ガスの高純度精製全行なう場合に使用される
低温吸着筒内の吸着剤の再生方決に関するものである。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for regenerating an adsorbent in a low-temperature adsorption column used for high-purity purification of gas.

一般にH2、Hθ、Ar等のガスを高純度(例えば99
.9999%以上)に精製する場合には、通常モレキュ
ラシーブ等が充填さねた常温吸着筒を通してガス中に含
まれる不純物の濃度を減少させた後、こねを低温吸着筒
の原料ガスとして合成ゼオライト等(例えばモレキュラ
シーブ、活性炭或いは両者の混1合物)か充填され、液
体窒素(T、 −N2+等によって深冷(例えば−19
6°C)さねている低温吸着筒に箭してさらに不純分を
吸着除去して高純度ガスにiQ Illしている。
Generally, gases such as H2, Hθ, Ar, etc. are used with high purity (e.g. 99%
.. 9999% or more), the concentration of impurities contained in the gas is reduced by passing it through a room-temperature adsorption column filled with molecular sieves, etc., and then using synthetic zeolite, etc. as the raw material gas for the low-temperature adsorption column. For example, it is filled with molecular sieves, activated carbon, or a mixture of both, and deep cooled (for example, -19
The gas is placed in a low-temperature adsorption cylinder that is suspended at 6°C, and further adsorbs and removes impurities to produce high-purity gas.

上記常温、低温吸着筒内の吸着剤は、一定期間精側を行
なった後再生される。
The adsorbent in the normal-temperature and low-temperature adsorption column is regenerated after performing the refinement for a certain period of time.

上記常温、低温吸着筒はそれぞれ2基設けらね交互に再
生使用きね、るが、常温吸着筒は周知の加熱およびパー
ジガスの流通によって再生される。
Two of the above-mentioned room temperature and low temperature adsorption columns are provided and are alternately regenerated and used, but the room temperature adsorption column is regenerated by well-known heating and purge gas circulation.

また、低温吸着筒の吸着剤は一般に精製したガスを20
0〜650°Cに加熱して低温吸着筒に流通せしめ、吸
着剤の温度?150〜′500°Cに昇温して吸着物を
除去することにより再生されている。
In addition, the adsorbent in the low-temperature adsorption cylinder generally uses purified gas at 20%
The temperature of the adsorbent is increased by heating it to 0 to 650°C and passing it through a low temperature adsorption cylinder. It is regenerated by raising the temperature to 150-500°C and removing adsorbed substances.

ところで、上記低湿吸着筒の吸着剤は、−190°C以
下に冷eされているので、これを150〜乙00°Cに
加熱することは、吸着V″JJ製時生時との温度差が3
50〜500’Cと大きくなる。このため、 ■ 加熱エネルギーの損失プ、s大きく又ネ/j製ガス
を加熱する装置が必要々なる。
By the way, the adsorbent in the low-humidity adsorption column is cooled to below -190°C, so heating it to 150 to 00°C will reduce the temperature difference between the adsorption V''JJ production time and the temperature difference. is 3
The temperature increases from 50 to 500'C. For this reason, (1) there is a large loss of heating energy, and a device for heating the gas is required.

■ 加熱に精製ガスを使用するため精′叩ガスの4”0
失が大きい。
■ Because purified gas is used for heating, 4”0 of purified gas is used for heating.
It's a big loss.

■ 低温吸着装置のサーマルストレスが大きいので使用
材料が制限され又加工技術も高度なものが要求され、装
[i′ltの特殊什によるコスト了ツブが大きい。
(2) Since the thermal stress of the low-temperature adsorption device is large, the materials that can be used are limited, and advanced processing techniques are required, and the cost increase due to special supplies for the equipment is large.

等の欠点かあった。There were some drawbacks.

本発明者は、上記の間頴を解決すべく鏝、慧6斤究を行
なった結果、低温吸着剤を通過させて不純物を吸着除去
し高純度ガスとする原料ガス中のH20およびCO,の
含有量をそれぞり、 1 p(by以下とすると、破過
状態となった低温吸着剤(オ、こf]を苓温とすること
によって吸着されているN2や02 佑の不純1分が容
易に除去されて再生さねることを見出した。
As a result of conducting extensive research to solve the above-mentioned problem, the present inventor has discovered that H20 and CO in the raw material gas can be passed through a low-temperature adsorbent to adsorb and remove impurities to obtain a high-purity gas. If the content is less than 1 p (by), the impurities of N2 and It has been found that it can be easily removed and regenerated.

本発明は上記の知見に基すいて完成さねたものでその要
旨(ま、ガスの昼純度精製装置Nにおける低温吸着筒内
の吸着剤再生方法において、低温吸着筒に導入し、不純
物を吸着除去して高純(9)ガスとする原料ガス中の水
分および炭酸ガスの含有量をそねぞね11正以下とし、
再生時には上記低温吸着剤を至温に保持することを特徴
としたガスの高純度ネi’J 脚装置における吸着剤再
生方法にある。
The present invention was not completed based on the above knowledge, and its gist (well, in the method of regenerating an adsorbent in a low temperature adsorption column in a gas daytime purification device The content of moisture and carbon dioxide in the raw material gas to be removed to obtain high purity (9) gas is set to be less than 11 positive,
The present invention provides a method for regenerating an adsorbent in a gas high-purity gas equipment, characterized in that the low-temperature adsorbent is maintained at the lowest temperature during regeneration.

以下本発明の方法をH2ガスの高純、度1fi9製装置
における低温吸着筒の吸着剤再生2例として具体的に説
明する。
The method of the present invention will be specifically explained below as two examples of regenerating the adsorbent in a low-temperature adsorption cylinder in a high-purity H2 gas production device with a degree of 1fi9.

低温吸着筒の再生試験における吸着破過および再生後の
吸着量の油)定は次のようにして行なった。
The adsorption breakthrough in the regeneration test of the low-temperature adsorption column and the determination of the amount of adsorption after regeneration were carried out as follows.

吸着破過:吸着剤6gを20〜24メツシユに粉砕し、
内径10.5mfiの円筒の吸着筒に充填した。
Adsorption breakthrough: pulverize 6g of adsorbent into 20-24 meshes,
It was filled into a cylindrical adsorption tube with an inner diameter of 10.5 mfi.

充填高さく、ま約181で、粉砕し、た吸着剤を充填し
た吸着筒は液体窒素により一196°Cに保持した。
The adsorption column, which had a filling height of about 181 cm and was filled with crushed adsorbent, was maintained at -196°C with liquid nitrogen.

この状態で後述する実唯例に示す原料H2ガス(入口ガ
ス)を吸着剤に導入し、出口の窒素ガスの濃度が入口の
窒素ガスの濃度と同じとなった時を吸着破過とした。
In this state, the raw material H2 gas (inlet gas) shown in the actual example described below was introduced into the adsorbent, and adsorption breakthrough was defined as the time when the concentration of nitrogen gas at the outlet became the same as the concentration of nitrogen gas at the inlet.

再生後の吸着量:吸着破過と同じ装置に再生した吸着剤
を充填し液体窒素により一196°Cに保、持L、ソコ
ヘN、 : 50ppm、02:2ppm、N20 <
i pnm % CO2< 1ppIlを含むH2ガス
?導入し、吸着剤の入口と出口の窒素ガスの濃度変化を
4川定し、出口窒素濃度が25p所となった時の窒素ガ
スの吸着量を求めた。
Adsorption amount after regeneration: The same device as used for adsorption breakthrough was filled with the regenerated adsorbent and maintained at -196°C with liquid nitrogen.
i pnm % CO2 < H2 gas containing 1ppIl? The changes in the concentration of nitrogen gas at the inlet and outlet of the adsorbent were determined for four rivers, and the amount of nitrogen gas adsorbed when the outlet nitrogen concentration reached 25p was determined.

実j也例1 吸着剤としてモレキュラシーブ5Al市販品、ユニオン
昭和KK製)を用い原料ガス中の水分り度を種々変えて
精′M?行ない吸着破過させた。この破過した吸着剤を
種々な温度で再生させ、再生後の吸着量を測定した。結
果を第1表に示す〇実呼例2 実施例1と同じ吸着剤を用い、原料水素ガス中のCO2
濃度を変えて吸着破過させ、この破過した吸3′今剤を
温度シ変えて再生し、再生後の吸着量を測定した。結果
を第2表に示す。
Practical Example 1 Molecular Sieve 5Al (commercially available product, manufactured by Union Showa KK) was used as an adsorbent, and the degree of water content in the raw material gas was varied. This resulted in adsorption breakthrough. This breakthrough adsorbent was regenerated at various temperatures, and the amount of adsorption after regeneration was measured. The results are shown in Table 1. Actual Example 2 Using the same adsorbent as in Example 1, CO2 in the raw hydrogen gas was
The adsorption breakthrough was achieved by changing the concentration, and the adsorption agent that had broken through was regenerated by changing the temperature, and the amount of adsorption after regeneration was measured. The results are shown in Table 2.

第   2   表 実権例1および2より明がなように原料としてN20 
、CO2が1 ppm以下のHtガスヲ用いると、この
原料ガスによって破過した吸着剤は室温で完全に再生す
ることがわかる。
As is clear from Actual Examples 1 and 2 in Table 2, N20 is used as a raw material.
, it can be seen that when Ht gas containing 1 ppm or less of CO2 is used, the adsorbent that has broken through with this raw material gas is completely regenerated at room temperature.

実施例3 実施例1と同じ吸着剤?用い、原料1.7丁、ガス中7
7)N2・02の4度を変えて吸着破過すしぬ、これら
吸着破過した吸着剤を下記の条件で再生し、これら再生
した]!l!着剤の再生後の[段着指を測定した。結果
を第3表に示す。
Example 3 Same adsorbent as Example 1? Used, 1.7 raw materials, 7 in gas
7) The adsorption breakthrough was achieved by varying the N2/02 concentration by 4 degrees, and the adsorbents that had adsorption breakthrough were regenerated under the following conditions]! l! After regenerating the adhesive, the number of layers attached was measured. The results are shown in Table 3.

第   3   表 N20、CO2がそねぞれi pp+i以下の原料水素
ガスを用いて吸着破過せしめた吸着剤は、吸着剤σ)温
度を室温とすると、再生時の通過ガスの創にがかわりな
くほぼ再生されることがわかる。
Table 3 Adsorbents that have undergone adsorption breakthrough using raw material hydrogen gas with N20 and CO2 of less than ipp+i, respectively, have the following characteristics: When the temperature of the adsorbent σ is set to room temperature, the gas passing through during regeneration replaces the wound. You can see that it is played almost without any problem.

実施例4 吸着剤として活性1匁を用い、下表の不純物を含有する
原料H2カスにより吸不破過ぜしぬ、この原料カス′f
再生ガスとして再生温度および再生ガスの流す時間?変
えて上記破過した吸着剤を再生し、再生した(p6着剤
の吸着用を測定した。結果な第4表に示す。
Example 4 Using an active 1 momme as an adsorbent, this raw material scum'f which does not adsorb or break through with the raw material H2 scum containing the impurities shown in the table below.
What is the regeneration temperature and flow time of the regeneration gas? The adsorption capacity of the regenerated (P6 adhesion) was measured by regenerating the above-mentioned breakthrough adsorbent.The results are shown in Table 4.

なお上記実施例は、いずれも胚純度[2ガス精製装置Y
iの低温吸着剤の再生方法について述べたが、1−10
、Ar等の低温吸着剤の再生においても同様な結果が得
られた。
In addition, in the above examples, all embryo purity [2 gas purification equipment Y
I have described the regeneration method of low-temperature adsorbent in 1-10.
Similar results were obtained in the regeneration of low-temperature adsorbents such as , Ar, etc.

以上述べたように本発明に係る高純度ガス精製製型の吸
着剤の再生方法は、低温吸着剤を通1.て高純度ガスに
精製する原料ガス中のN20およびの原料ガスP再生ガ
スとして通すことにより、はぼ完全に再生出来る。した
がって再生に伴う加熱エネルギーの損失がヒく、また再
生ガスを加熱するj]0熱装凶も不要で、さらに吸着i
tJと再生時との温度差が少ないのでサーマルストレス
も小きく、装置の拐質、加工等のグレードを高める必要
がないなど、多くの一所を有する方法である。
As described above, the method for regenerating a high-purity gas purification type adsorbent according to the present invention involves passing a low-temperature adsorbent through 1. By passing N20 and P in the raw material gas to be purified into high-purity gas as regeneration gas, almost complete regeneration can be achieved. Therefore, the loss of heating energy accompanying regeneration is reduced, there is no need for heat equipment to heat the regenerated gas, and there is no need for adsorption.
This method has many advantages, such as there is little difference in temperature between tJ and the temperature during regeneration, so thermal stress is small, and there is no need to improve the quality of the equipment or the grade of processing.

Claims (1)

【特許請求の範囲】[Claims] ガスの高純度精製装置における低温吸着筒内の吸着剤再
生方法において、水分および炭酸ガスの含有量がそれぞ
れI 11111n以下の原料ガスを低温吸着筒に導入
して高純度ガスを生成せしめ、再生時には上記低温吸着
剤を塞流に保持することを特徴としたガスの高純度精製
装置における吸着剤再生方法。
In a method for regenerating an adsorbent in a low-temperature adsorption column in a high-purity gas purification device, a raw material gas having a moisture content and a carbon dioxide content of less than I1111n, respectively, is introduced into a low-temperature adsorption column to generate high-purity gas, and during regeneration, A method for regenerating an adsorbent in a high-purity gas purification device, the method comprising retaining the low-temperature adsorbent in a blockage state.
JP58021818A 1983-02-12 1983-02-12 Process for regenerating adsorbent in high degree purification apparatus for gas Granted JPS59147618A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP58021818A JPS59147618A (en) 1983-02-12 1983-02-12 Process for regenerating adsorbent in high degree purification apparatus for gas

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP58021818A JPS59147618A (en) 1983-02-12 1983-02-12 Process for regenerating adsorbent in high degree purification apparatus for gas

Publications (2)

Publication Number Publication Date
JPS59147618A true JPS59147618A (en) 1984-08-24
JPH0372327B2 JPH0372327B2 (en) 1991-11-18

Family

ID=12065636

Family Applications (1)

Application Number Title Priority Date Filing Date
JP58021818A Granted JPS59147618A (en) 1983-02-12 1983-02-12 Process for regenerating adsorbent in high degree purification apparatus for gas

Country Status (1)

Country Link
JP (1) JPS59147618A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115055026A (en) * 2022-05-25 2022-09-16 云南通威高纯晶硅有限公司 Method for purifying mixed gas by using tube array adsorption column

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115055026A (en) * 2022-05-25 2022-09-16 云南通威高纯晶硅有限公司 Method for purifying mixed gas by using tube array adsorption column

Also Published As

Publication number Publication date
JPH0372327B2 (en) 1991-11-18

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