JPS62168525A - Method for separating and purifying carbon monoxide by adsorption - Google Patents
Method for separating and purifying carbon monoxide by adsorptionInfo
- Publication number
- JPS62168525A JPS62168525A JP61009467A JP946786A JPS62168525A JP S62168525 A JPS62168525 A JP S62168525A JP 61009467 A JP61009467 A JP 61009467A JP 946786 A JP946786 A JP 946786A JP S62168525 A JPS62168525 A JP S62168525A
- Authority
- JP
- Japan
- Prior art keywords
- gas
- adsorption
- tower
- pressure
- carbon monoxide
- 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
Links
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 84
- 238000000034 method Methods 0.000 title claims abstract description 64
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 229910002091 carbon monoxide Inorganic materials 0.000 title claims abstract description 52
- 238000011084 recovery Methods 0.000 claims abstract description 13
- 238000010926 purge Methods 0.000 claims abstract description 7
- 239000007789 gas Substances 0.000 claims description 152
- 239000002994 raw material Substances 0.000 claims description 38
- 238000004140 cleaning Methods 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 239000003463 adsorbent Substances 0.000 claims description 13
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 230000006837 decompression Effects 0.000 claims description 2
- 238000007670 refining Methods 0.000 claims description 2
- 238000003795 desorption Methods 0.000 abstract description 10
- 239000000047 product Substances 0.000 description 22
- 238000000926 separation method Methods 0.000 description 12
- 238000010586 diagram Methods 0.000 description 7
- 239000002912 waste gas Substances 0.000 description 5
- 238000011027 product recovery Methods 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- JFMOYHBEGWPXBI-UHFFFAOYSA-N [C].[As] Chemical compound [C].[As] JFMOYHBEGWPXBI-UHFFFAOYSA-N 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000011403 purification operation Methods 0.000 description 2
- 239000010959 steel Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241001494479 Pecora Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- -1 blast furnace gas Chemical compound 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
- 238000013517 stratification Methods 0.000 description 1
Landscapes
- Separation Of Gases By Adsorption (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、一酸化炭素ガスに対して選択枝層性ケ有する
吸着剤を用いたＰ８Ａ法（圧力変動式吸着分離法）によ
って、転炉ガス及び高炉ガス等の、少なくとも一酸化炭
素ガス及び窒素ガスを含む原料ガスηλら高純度の一酸
化炭素ガスを高贋回収率で分離する方法に関する。Detailed Description of the Invention (Industrial Field of Application) The present invention is a method for converting carbon monoxide gas into converter furnaces using the P8A method (pressure fluctuation type adsorption separation method) using an adsorbent having selective layer properties for carbon monoxide gas. The present invention relates to a method for separating high-purity carbon monoxide gas from raw material gas ηλ containing at least carbon monoxide gas and nitrogen gas, such as gas and blast furnace gas, with a high recovery rate from counterfeiting.
（従来の技術）
製鉄所で副生される転炉ガス及び、高炉ガスは表ＩＶｃ
示す様な成分を含む。(Prior art) Converter gas and blast furnace gas by-produced in steel plants are shown in Table IVc.
Contains the ingredients shown.
表 １
一酸化炭素は、有機合成用原料として、また冶金反応等
に非常に有用である。一酸化炭素ガスを多（含む製鉄副
生ガスヲｒヒ学分野で有効利用する為には、上記成分の
ままでは用いることができず、一酸化炭素以外の成分を
除去する必要があることが多い。Table 1 Carbon monoxide is very useful as a raw material for organic synthesis and in metallurgical reactions. In order to effectively utilize carbon monoxide gas in the field of steel manufacturing by-product gas, it cannot be used as is, and it is often necessary to remove components other than carbon monoxide. .
転炉ガス及び高炉ガスのような混合ガスから、一酸化炭
素ガスを濃縮分離する方法には、深冷分離法と溶液吸収
法及び吸着分離法がある。Methods for concentrating and separating carbon monoxide gas from a mixed gas such as converter gas and blast furnace gas include a cryogenic separation method, a solution absorption method, and an adsorption separation method.
深冷分離法では一酸ｆヒ炭素の沸点と非常に近い沸点の
窒素が多く含捷れる場合は、一酸化炭素の分Ｓ精製が困
難であり、低温と高圧操作を必要として設備が高価にな
る。In the cryogenic separation method, it is difficult to purify carbon monoxide when it contains a large amount of nitrogen, which has a boiling point very close to that of carbon monoxide, and requires low-temperature and high-pressure operation, making equipment expensive. Become.
溶液吸収法の調液吸収法は２０℃％ １５０〜２００
ｋｇ／ｍ−Ｇの高い圧力が必要であり。Solution absorption method: 20℃% 150-200
A high pressure of kg/m-G is required.
Ｃ０８０ＲＢ 法は原料ガス中の水分ｋｌｐｐｍ以下に
する前処理工程が必要となり％装置が複雑で設備が高価
になる。The C080RB method requires a pretreatment step to reduce the water content in the raw material gas to less than klppm, making the equipment complex and expensive.
吸着による方法は、一酸化炭素ガス選択吸Ｎ注？示す吸
着剤を用いｆｃＰＳＡ法が知られている（特開昭５８−
１０４００９号、特開昭５９−２２６２５号、特開昭５
９−２６１２１号、特開昭５９−４９８１８号各公報等
）。Is there a method of adsorption using selective inhalation of carbon monoxide gas? The fcPSA method using the adsorbent shown is known (Japanese Unexamined Patent Publication No. 1983-1999).
No. 104009, JP-A-59-22625, JP-A-5
9-26121, Japanese Unexamined Patent Publication No. 59-49818, etc.).
（発明が解決しようとする問題点）
ＰＳＡ法による一酸化炭素ガスの分離は、装置が簡単で
あり運転コストも少なくて済むので、他の方法に比べて
非常に優れた方法である。し〃為し従来の方法では、廃
棄ガス中にかなりの一酸化炭素ガスが混入してしまうた
め、回収率が悪く、高純度の製品一酸化炭素ガス全回収
する場合はど、その傾向は顕著である。(Problems to be Solved by the Invention) The separation of carbon monoxide gas by the PSA method is an extremely superior method compared to other methods because the equipment is simple and the operating cost is low. However, in the conventional method, a considerable amount of carbon monoxide gas is mixed into the waste gas, resulting in a poor recovery rate. It is.
本発明は、高純度の製品一酸化炭素ガスを高い回収率で
得ることのできる分離精製法全提供するもので、しかも
新たな大規模な設備投資などケ行なうことな〈実施する
ことができる経済的な方法である。The present invention provides an entire separation and purification method that can obtain high-purity product carbon monoxide gas with a high recovery rate, and can be carried out economically without any new large-scale capital investment. This is a typical method.
（問題点全解決するための手段）
上記の工つな問題を解決するため鋭意検豹した結果、Ｐ
ＳＡ法に裏、る一酸化炭素ガス分離精製において、高純
度の一酸化炭素製品ガスを高回収率で分離する方法を発
明した。(Means for solving all the problems) As a result of intensive investigation to solve the above difficult problems, P.
In carbon monoxide gas separation and purification behind the SA method, we have invented a method for separating high-purity carbon monoxide product gas with a high recovery rate.
即ち１本発明は、一酸化炭素及び窒素を含む原料ガス中
の一酸化炭素全吸着法により分離精製する方法において
、該原料ガス中の一酸化炭素に対して選択吸Ｎ注？有す
る吸着剤を充填した２つ以上の吸着塔を使用して、
（（Ｉ）原料ガス？吸着塔に導入して所定の圧力まで昇
圧させた後、原料ガスを流通させて一酸化炭素を吸着さ
せる散層工程。Namely, the present invention provides a method for separating and purifying a raw material gas containing carbon monoxide and nitrogen by total adsorption of carbon monoxide, in which carbon monoxide in the raw material gas is selectively adsorbed with nitrogen. Using two or more adsorption towers filled with an adsorbent containing ((I) Raw material gas? After introducing the raw material gas into the adsorption tower and increasing the pressure to a predetermined pressure, the raw material gas is passed through to adsorb carbon monoxide. dispersion process.
（ｂｌ 吸着工程終了後、吸着塔内のガスを放出させ
て吸着塔の圧力を降下きせる減圧工程、ｆｃｌ 減圧
工程終了後、製品一酸化炭素ガスを吸着工程時の原料ガ
ス流通方向と同じ方向に導入して、難吸着成分全ノージ
する洗浄工程、ｆｄ） 洗浄工程終了後、吸着塔の原
料ガス入口側から大気圧以下に排気して吸着剤に吸着し
ている一酸化炭素を脱着させ、製品一酸化炭素ガスを回
収する製品ガス回収工程、
（ｅ） 製品ガス回収工程終了後の吸着塔へ、（ｃ）
の洗浄工程の吸着塔力１ら流出するガスを吸着工程時の
原料ガス流通方向と逆の方向に導入して、前者の吸着塔
内を昇圧する昇圧（Ｉ）工程。(bl) After the adsorption process is completed, the pressure reduction process is to release the gas in the adsorption tower to lower the pressure in the adsorption tower; (fd) After the cleaning process, the adsorption tower is evacuated to below atmospheric pressure from the raw gas inlet side to desorb carbon monoxide adsorbed on the adsorbent, and the product Product gas recovery process for recovering carbon monoxide gas, (e) To the adsorption tower after the product gas recovery process, (c)
A pressurization (I) step in which the gas flowing out from the adsorption tower 1 in the cleaning step is introduced in a direction opposite to the flow direction of the raw material gas in the adsorption step to raise the pressure inside the former adsorption tower.
（ｆ） 昇圧７１）工程終了後の吸着塔へ、（ｂ）の
減圧工程時の吸着塔からの放出ガスを吸着工程時の原料
ガス流通方向と逆の方向に導入して、前者の吸着塔内を
昇圧する昇圧ｆｌｕ）工程
たらなる操作ケ、定期的に吸着塔間の流れ全かえて繰り
返すこと’に％徴とする一酸化炭素ガスの分離精製法で
ある。(f) Pressurization 71) After the completion of the step, the gas released from the adsorption tower during the pressure reduction step of (b) is introduced into the adsorption tower in the opposite direction to the flow direction of the raw material gas during the adsorption step, and the former adsorption tower is This is a method for separating and purifying carbon monoxide gas, which consists of a step of increasing the pressure inside the adsorption column (flu), and periodically changing the flow between the adsorption towers and repeating the process.
本発明では、使用する原料ガスは一酸化炭素及び窒素を
含むガスであり、高炉ガス、転炉ガス、水性ガス、石炭
ガス化ガス等である。好ましくは、原料ガスは事前に二
酸化炭素、水を除去しておく、。In the present invention, the raw material gas used is a gas containing carbon monoxide and nitrogen, such as blast furnace gas, converter gas, water gas, coal gasification gas, etc. Preferably, carbon dioxide and water are removed from the raw material gas in advance.
水素ガス等の難吸着成分の存在は、一酸化炭素の精製と
いう面からは差し支えない。The presence of a component that is difficult to adsorb, such as hydrogen gas, does not pose a problem from the viewpoint of purifying carbon monoxide.
吸着剤は一酸化炭素に対して選択吸着注ケ有するもので
あって、窒素に対して吸着音の少ないものを使用する。The adsorbent used is one that selectively adsorbs carbon monoxide and produces less adsorption noise for nitrogen.
この様な吸着剤としては、モレキュラーシープタイプの
ゼオライト、活性炭等の他、前記各公報に例示されたも
のがある。Examples of such adsorbents include molecular sheep type zeolite, activated carbon, and the like, as well as those exemplified in the above-mentioned publications.
吸着剤は吸着塔に充填して使用する一吸Ｎ塔は複数本必
要であって、２塔でもよいが、３塔あれば原料ガスの連
続導入処理が可能であり、容易に効率良く操業すること
が出来る。４塔以上でもさしつかえはないが、バルブの
切り替えなどの操作が繁雑となり、捷た設備費が高くな
る傾向がある。The adsorbent is used by filling the adsorption tower with a plurality of N towers, and two towers may be sufficient, but three towers allow for continuous introduction of raw material gas and facilitate efficient operation. I can do it. There is no problem with four or more towers, but operations such as switching valves become complicated and equipment costs tend to increase.
２塔式でも後述する工うに本発明の方法を実施すること
はできるが、この場合には吸着塔以外にバッファタンク
が必要となる他、原料ガスを連続導入処理することが難
しくなるｉ１向がある。Although it is possible to carry out the method of the present invention in a two-column type as described later, in this case, a buffer tank is required in addition to the adsorption column, and it is difficult to continuously introduce and process the raw material gas. be.
（ａ）の吸着工程は、吸着塔に原料ガス全導入して吸着
塔の昇圧を行ない、所定の圧力で原料ガス全流通させて
一酸化炭素含南量の少ない廃棄ガスを流出させ、吸着剤
の破過点までまたは破過点に達する少し前まで原料ガス
の導入を行う。ここで破過点とは吸着剤の吸着量が飽和
に達して吸着が行なわれなくなり、塔の出口〃）ら原料
ガス組成と同じガスが流出して来ることをいう。本発明
では回収すべきガスは易吸着成分であるので高い圧力は
必要ではなく、１０ ｋｇ／ ｉ、Ｇ以下で充分であり
、好ましくは３ ｋｇ／ ｄ、Ｇ程度の吸着圧力、また
それより低い圧力であってもＬい。In the adsorption step (a), all of the raw material gas is introduced into the adsorption tower, the pressure of the adsorption tower is increased, and all of the raw material gas is circulated at a predetermined pressure to allow waste gas with a low carbon monoxide content to flow out. The raw material gas is introduced until the breakthrough point or slightly before reaching the breakthrough point. Here, the breakthrough point refers to the point where the amount of adsorption of the adsorbent reaches saturation and adsorption is no longer performed, and a gas having the same composition as the raw material gas flows out from the outlet of the column. In the present invention, since the gas to be recovered is an easily adsorbed component, a high pressure is not necessary, and an adsorption pressure of 10 kg/i, G or less is sufficient, and preferably an adsorption pressure of about 3 kg/d, G, or lower. Even pressure is low.
（ｂ）の減圧工程では、吸着の終わった吸着塔から。In the pressure reduction step (b), from the adsorption tower after adsorption.
塔内の吸着剤間の空隙中のガス（一酸化炭素濃度が原料
ガスと同じあるいは原料ガスより低いガス）が放出され
、昇圧（Ｉ）工程が終わった他の吸着塔に、両方の塔が
均圧になるまでもしくは近い圧力になるまで導入される
。Gas in the voids between the adsorbents in the tower (gas whose carbon monoxide concentration is the same as or lower than the raw material gas) is released, and both towers are transferred to the other adsorption tower that has completed the pressurization (I) step. The pressure is introduced until the pressure is equalized or close to it.
（ｃ）の洗浄工程では、減圧の終わった吸着塔に製品ガ
ス全原料ガス流通方向と同じ方向に導入して吸着塔内に
若干残っている難吸着成分をパージする。ノぐ−ジガス
は他塔の昇圧（Ｉ）工程に利用する。In the cleaning step (c), the product gas is introduced into the adsorption tower after depressurization in the same direction as the flow direction of all the raw material gases to purge the slightly remaining difficult-to-adsorb components in the adsorption tower. The nozzle gas is used for the pressurization (I) step in another column.
ｃｄ）の製品回収工程では、ノクージ工程の終わった塔
から真空ポンプ等を用いて真空度３００ Ｔｏｒｒ以下
に、好ましくは５０ Ｔｏｒｒ以下［まで排気して。cd) In the product recovery step, the column after the Nokoji step is evacuated to a vacuum of 300 Torr or less, preferably 50 Torr or less, using a vacuum pump or the like.
吸着剤に吸着されていた成分（一酸化炭素等）を脱Ｎ−
Ｊせ、製品ガスとして回収する。De-N- removes components (carbon monoxide, etc.) that have been adsorbed on the adsorbent.
It is recovered as a product gas.
（ｅ）の昇圧（１）工程では％製品回収が終わった塔に
、他塔のノクージ工程の一酸化炭素ケ多く含んだ流出ガ
スを吸着工程時の原料ガス流通方向と逆の方向に導入し
て塔内？昇圧するとともに、 −ｅ（ヒ炭素を塔内に吸
着させる。ここで逆の方向とけ、原料ガスを吸着塔の塔
底から導入する場合は、塔頂から導入すること全意味す
る。In step (e), pressurization (1), the effluent gas containing a large amount of carbon monoxide from the Nokuji process in another column is introduced into the column after % product recovery in the opposite direction to the feed gas flow direction during the adsorption step. Inside the tower? While raising the pressure, -e(arsenic carbon is adsorbed in the column.If the direction is reversed and the raw material gas is introduced from the bottom of the adsorption column, it means that it is introduced from the top of the column.
（ｆ）の昇圧（ＩＤ工程では、パージ工程の流出ガスを
導入して昇圧（ｆ）工程が終了した吸着塔に１吸着工程
が終わった吸着塔の波圧放圧ガスを吸着工程時の原料ガ
ス流通方向と逆の方向に導入する。この時に導入するガ
スの一酸化炭素ガス濃度はパージ工程の流出ガスよりも
低いため、吸着工程時の排ガス出口側は一酸化炭素ガス
濃度の低いガスで満たされ、塔内部に一酸化炭素が濃縮
される。昇圧ｆｌｌ）工程の終わった吸着塔はｆａｌの
吸着工程の吸着塔として使用される。(f) Pressurization (In the ID process, the effluent gas from the purge process is introduced and the wave pressure release gas from the adsorption tower that has completed one adsorption process is transferred to the adsorption tower where the pressure increase (f) process has been completed.) The carbon monoxide gas concentration of the gas introduced at this time is lower than the outflow gas of the purge process, so the exhaust gas outlet side during the adsorption process is a gas with a low carbon monoxide gas concentration. The adsorption tower after the pressurization fll) step is used as an adsorption tower for the fal adsorption step.
第２図に２本の吸着塔を用いて本発明の分離精製操作を
行う場合の装置の１例を示す。第１図にはその時のサイ
クルの１例を示す。FIG. 2 shows an example of an apparatus for carrying out the separation and purification operation of the present invention using two adsorption towers. FIG. 1 shows an example of the cycle at that time.
Ａ塔は１のバルブが開けられて原料供給による昇圧が行
われる。この時Ｂ塔は５のバルブが開けられ１１の真空
ポンプにより製品ガスの脱着が行われる。また、２ 、
３ 、４ 、６ 、７ 、８ 、９．１０のバルブは閉
である。In tower A, valve 1 is opened to increase the pressure by supplying raw materials. At this time, valve 5 in tower B is opened and product gas is desorbed by vacuum pump 11. Also, 2,
Valves 3, 4, 6, 7, 8, 9.10 are closed.
Ａ塔は所定の圧まで昇圧された後、７．１０のバルブを
開として原料ガスの流通による吸着工程全行い、流出ガ
スは廃棄される。破過点あるいはその前まで原料ガスを
流通させた後に、１．１０のバルブを閉％９のノ々ルブ
を開とし、Ａ基金減圧放圧させて１３のバッファタンク
にその流出ガスを取込む、、Ａ塔を所定の圧まで減圧し
た後、９のバルブを閉とする。又、Ｂ塔は５のノ々ルブ
を閉にして脱着を終了する。After the pressure in tower A is increased to a predetermined pressure, valve 7.10 is opened to perform the entire adsorption process by flowing the raw material gas, and the outflow gas is discarded. After flowing the raw material gas to or before the breakthrough point, close the valve 1.10 and open the nonoru valve %9 to depressurize the A fund and take the outflow gas into the buffer tank 13. ,, After reducing the pressure in tower A to a predetermined pressure, valve 9 is closed. Also, in tower B, the nodal valve 5 is closed to complete the desorption.
次に３．８のノ々ルブ全開にし、１２の製品ガス中間タ
ンクから製品ガスをＡ塔に導入してパージを行い、その
時の流出ガスをＢ塔へ導入する。ノクージ後、３，７の
バルブを閉にし１次に９のバルブｉ開にして先にノ々ツ
ファタンク１３に取込んだＡ塔の減圧放出ガスをＢ塔へ
導入する。均圧した後、９．８のバルブは閉とする。Next, the No. 3.8 nozzle is fully opened, and the product gas is introduced from the 12 product gas intermediate tanks into the A tower for purging, and the effluent gas at that time is introduced into the B tower. After the discharge, the valves 3 and 7 are closed, and the valve i, 9 is first opened to introduce the depressurized discharged gas from the A column, which was taken into the nototsufa tank 13, into the B column. After equalizing the pressure, valve 9.8 is closed.
次にＡ塔は上記Ｂ塔のように脱Ｎｖｈら昇圧まで行い、
Ｂ塔は上記Ａ塔のように原料ガスによる昇圧から洗浄工
程までを行い、これら操作？繰り返すことにより易吸着
成分である一酸化炭素ガスを分離精製する。Next, Column A performs de-Nvh and pressurization like the above-mentioned Column B.
Column B performs the steps from pressurization using raw material gas to cleaning process like the above-mentioned column A, and performs these operations. By repeating this process, carbon monoxide gas, which is an easily adsorbed component, is separated and purified.
第４図に３本の吸着塔を用いて本発明の分離精製操作全
行う場合の装置の１例を示す。第３図にはその時のサイ
クルの１例を示す、
Ａ塔は４１のバルブが開けられて原料供給による昇圧が
行われる。Ｃ塔は、４９．５５のバルブが開けられて製
品ガスｖＣＬる洗浄が行われ、Ｂ塔１ｌ−ｉＣ塔から流
出するガスを５５のバルブを通して導入し昇圧される。FIG. 4 shows an example of an apparatus in which all the separation and purification operations of the present invention are carried out using three adsorption towers. Figure 3 shows an example of the cycle at that time. In tower A, 41 valves are opened and the pressure is increased by supplying raw materials. In the C column, the valve 49.55 is opened to wash the product gas vCL, and the gas flowing out from the B column 1l-iC column is introduced through the valve 55 and the pressure is increased.
、４２，４３．４４．４５゜４６．４７．４８．５０，
５１．５２．５３゜５４のバルブは閉である。Ｃ塔の洗
浄工程が終了した後に、４９．５５のノ々ルブを閉とし
、Ｂ塔の昇圧（１）工程も終了する。Ｃ塔は直ちに４８
のノ々ルブを開として１１の真空ポンッにて製品ガスの
脱着が行われるーＡ塔は所定の圧まで昇圧された後、５
０のバルブを開として原料ガスの流通による吸着工程を
行り、流出ガスは廃棄される。破過点あるいはその前ま
で原料ガスを流通させた後に、４１．５０のノ々ルブを
閉とする。次にｂ５４のノ々ルブを開としてＡ塔は減圧
放圧を行い、その時の流出ガスを昇圧ｆＩ）がおわった
Ｂ塔に導入してＢ塔は昇圧（Ｉｆ）工程を行う。両方の
塔が均圧化された後に５４のバルブを閉としてＡ塔の減
圧工程およびＢ塔の昇圧（■）工程が終了する。同時に
４８のノ々ルブも閉としＣ塔の脱着工程が終了する。,42,43.44.45゜46.47.48.50,
The valves at 51, 52, 53 and 54 are closed. After the cleaning step of the C column is completed, the 49.55-hole valve is closed, and the pressurization (1) step of the B column is also completed. C tower immediately 48
The nozzle of the column A is opened, and the product gas is desorbed with 11 vacuum pumps.
The adsorption process is performed by opening the valve 0 and flowing the raw material gas, and the outflow gas is discarded. After flowing the raw material gas to or before the breakthrough point, the 41.50 nozzle valve is closed. Next, the nozzle of b54 is opened to perform depressurization of the A column, and the outflow gas at that time is introduced into the B column where the pressurization fI) has finished, and the B column performs the pressurization (If) step. After the pressures of both columns are equalized, valve 54 is closed, and the pressure reduction step of the A column and the pressure increase (■) step of the B column are completed. At the same time, No. 48 knob is also closed, and the desorption process of the C tower is completed.
次ｉｃＡ塔は洗浄、脱着工程を行い、Ｂ塔は原料ガスに
よる昇圧、吸着、及び減圧工程ｋｓｃ塔は昇圧（１）及
び（ＩＩ）’を行う。この時Ｃ塔はＡ塔からの流出ガス
に工り昇圧ｆｌｌｉ、ｔたＢ塔〃＼らの流出ガスにより
昇圧（■）？行う。Next, the icA column performs washing and desorption steps, the B column performs pressurization, adsorption, and depressurization using the raw material gas, and the ksc column performs pressurization (1) and (II)'. At this time, the C tower uses the outflow gas from the A tower to raise the pressure, and the B tower uses the outflow gas from the B tower to raise the pressure (■)? conduct.
次Ｋｋ塔は昇圧（Ｉ）及びｆＩＩｌ工程を行い％Ｂ塔は
洗＃１脱着工程ｉ Ｃ塔は原料ガスによる昇圧、吸着、
及び減圧工程全行う。この時Ａ塔はＢ塔からの流出ガス
により昇圧（１１ｋ 、またＣ塔７Ｏ３らの流出ガスに
より昇圧（ｍｌ 全行う。これら操作を繰り返すことに
より易吸着成分である一酸化炭素ガス全分離精製する。Next, the Kk column performs pressurization (I) and fIIl steps, the %B column performs washing #1 desorption step i, and the C column performs pressurization, adsorption, and
and perform the entire decompression process. At this time, the A tower is pressurized (11k) by the outflow gas from the B tower, and the pressure is increased (ml) by the outflow gas from the C tower 7O3. By repeating these operations, the carbon monoxide gas, which is an easily adsorbed component, is completely separated and purified. .
（作用）
本発明では、他塔の排出ガスを成層工程時の原料ガス流
通方向と逆の方向に、しかも洗浄工程時の流出ガス全最
初に、次に減圧放圧時の流出ガスの順に導入することに
エリ、−酸ｆヒ炭素の回収率を高めることができる、こ
れはこの操作にエリ吸着工程時の廃棄ガス中に含まれる
一酸ｆヒ炭素ガス量がおさえられたためと思われる。(Function) In the present invention, the exhaust gases from other towers are introduced in the opposite direction to the flow direction of the raw material gas during the stratification process, and moreover, all the outflow gas during the cleaning process is introduced first, and then the outflow gas during depressurization is introduced in this order. In particular, it is possible to increase the recovery rate of monoacid f arsenic carbon, which is thought to be because this operation suppresses the amount of monoacid f arsenic gas contained in the waste gas during the eli adsorption step.
（実施例）
一酸化炭素及び窒素ガスの混合ガス（ガス組成ＣＯ＝
７ （１，５％、Ｎ２＝ ２９．５％）〃＼ら一酸ｆヒ
炭素ガスの分離精製を行った。(Example) Mixed gas of carbon monoxide and nitrogen gas (gas composition CO=
7 (1.5%, N2 = 29.5%) Separation and purification of carbon gas was carried out.
第４図に示した７０−において吸着塔（２７６關φＸ８
００ｍ＋、３本）Ａ、Ｂ、Ｃにそれぞれ３５０℃で焼成
した合成ゼオライト（昭和ユニオン製モレキュラシーブ
５Ａｌｉ３３０９ずつ収納して連続運転を行った。運転
時の気温は２１℃であった。At 70- shown in Figure 4, the adsorption tower (276 mm φX8
Synthetic zeolite (Molecular Sieve 5Ali3309 manufactured by Showa Union Co., Ltd., manufactured by Showa Union) was stored in A, B, and C, respectively, and was operated continuously.The temperature during operation was 21°C.
Ａ塔における操作は、４１のバルブ全開にして混合ガス
ｋ ３．５ Ｎ＃／ｍｉｎで導入して塔内の圧力を３、
０ ｋｇ／ ｃｍ、Ｇまで昇圧した後に、更に混合ガス
を導入して塔内の圧力’ｋ ３．０ ｋｇ／７．０に保
つ様に５０のパルプ全開とする。この時に流出するガス
は廃棄する。破過する前に４１．５０のバルブを閉にし
て吸着工程？終了し％５４のバルブをＡ塔内圧力が１．
４ｋｇ／〜、Ｇになるまで開にして、昇圧（ｎ）工程の
終わったＢ塔へその流出ガス全導入させ一
減圧放置する。次に４３．５３のノ々ルブ會開にして製
品中間タンクから製品ガス金導入して洗浄を行か、その
流出ガスは製品回収工程の終わつｙｃｃ塔へ導入させる
。４３．５３の／々ルブを閉にして洗浄工程全終了させ
几後、４２のバルブを開にして真空ポンプ１１に工り−
酸ｒヒ炭素を脱着ζせて製品ガス２回収する。この脱着
操作はＡ塔内正方が１００ Ｔｏｒｒになる捷で行った
。脱着終了後、４２のバルブを閉にし、次に５４のバル
ブ全開にして、洗浄工程のＢ塔から洗浄時の流出ガス全
導入きせ（１，４ｋｇ／ ｃｒｄ、（）まで昇圧した後
５４のバルブ全開とする。次に５，３のバルブを開にし
てＣ塔の減圧放圧時の流出ガスを導入して１．６ ｋｑ
’／ ｃｎｆ、Ｇまで昇圧させる。この後、混合ガスを
前述と同様に吸着塔に導入して吸着工程以下の操作を繰
り返した。The operation in column A is to fully open valve 41 and introduce a mixed gas k at a rate of 3.5 N#/min to reduce the pressure inside the column to 3.5 N#/min.
After increasing the pressure to 0 kg/cm, G, a mixed gas is further introduced and the 50 pulp is fully opened to maintain the pressure inside the column at 3.0 kg/7.0. The gas that flows out at this time is discarded. Close the 41.50 valve before the breakthrough and adsorption process? When the valve at %54 was closed, the pressure inside the A column was 1.
It was opened until the pressure reached 4 kg/~G, and all of the effluent gas was introduced into the B column where the pressure increase (n) step had been completed, and the pressure was left to be reduced. Next, at the 43.53 nonorubu meeting, the product gas is introduced from the product intermediate tank for cleaning, and the effluent gas is introduced into the YCC tower at the end of the product recovery process. 43. After the entire cleaning process is completed by closing the 53/3 valve, open the 42 valve and start the vacuum pump 11.
The product gas 2 is recovered by desorbing the acid and arsenic carbon. This desorption operation was carried out at a pressure of 100 Torr inside the A tower. After the desorption is completed, the valve 42 is closed, then the valve 54 is fully opened, and all the effluent gas during cleaning is introduced from the B tower in the cleaning process (1.4 kg/crd, after increasing the pressure to Fully open.Next, open valves 5 and 3 to introduce the outflow gas from the C tower during depressurization and release to 1.6 kq.
'/cnf, raise the pressure to G. Thereafter, the mixed gas was introduced into the adsorption tower in the same manner as described above, and the operations following the adsorption step were repeated.
Ｂ塔及びＣ塔も同じ条件とがる様に、定期的に吸着塔１
１７）流れをかえて操作金繰り返した。１サイクル６分
で行い２時間運転した。Adsorption tower 1 is periodically removed so that the B tower and C tower are under the same conditions.
17) Changed the flow and repeated the operation. One cycle was performed for 6 minutes and the operation was for 2 hours.
運転開始後１時間３０分から２時間着での３０分間のガ
ス量は、混合ガスの供給量がＪＯ５Ｎ＃で、流出廃棄ガ
ス量は４．５ Ｍ％そのＣａ２度は３２．９％、捷た回
収ガス量は６０ Ｎ＃、 ＣＯ濃度は９９．０％であっ
た。この時００回収率は８０．０％であった。The amount of gas for 30 minutes from 1 hour and 30 minutes after the start of operation to 2 hours after the start of operation was JO5N#, the amount of waste gas flowing out was 4.5 M%, the Ca2 degree was 32.9%, and the amount of mixed gas was JO5N#. The amount of recovered gas was 60 N#, and the CO concentration was 99.0%. At this time, the 00 recovery rate was 80.0%.
（比較例）
従来の一酸化炭素分離ＰＳＡ法金用込て前述の実施例と
同じ混合ガスから一酸化炭素ガスの分離精製を行った。(Comparative Example) Using the conventional carbon monoxide separation PSA method, carbon monoxide gas was separated and purified from the same mixed gas as in the previous example.
吸着剤と吸着塔は実施例と同じ物を用いた。第６図に装
置図を、第５図にサイクルを示した。運転時の気温は２
１℃であった。The same adsorbent and adsorption tower as in the example were used. FIG. 6 shows an apparatus diagram, and FIG. 5 shows a cycle. The temperature when driving is 2
The temperature was 1°C.
Ａ塔における操作は、６１のバルブを開にして混合ガス
ｆ ３．５ Ｎ＃／ｍｉｎで導入して塔内の圧力を３、
０ ｋｙ ／ ｄ、Ｇまで昇圧した後に、更に混合ガス
を導入して塔内の圧力ｋ ３．０ ｋｚ／ ｃｍ、Ｇに
保つ様に７０のバルブを開とする。この時に流出するガ
スは廃棄する。破過する前［６１，７Ｑのバルブを閉に
して吸着工程を終了し、７３のバルブｌｒＡ塔内圧力が
（１，１吟／ ｃｒｌ、Ｇになるまで開にして、製品回
収工程の終わったＣ塔へその流出ガスを導入させ減圧放
圧する。次に６３のバルブを開にして製品中間タンク刀
＼ら製品ガス全導入して洗浄を行い、その流出ガスは昇
圧（Ｉ）工程の終わったＣ塔へひき続き導入させる。６
３．７３のバルブ全開にシテ洗浄工程を終了させた後％
６２のノ々ルブを開にして真空ポンプ１１に工り一酸
化炭素ゲ脱着させて製品ガスを回収する。この脱着操作
はＡ塔内圧力が］ ００ Ｔａｒｒになるまで行った。The operation in column A is to open the valve 61 and introduce a mixed gas f 3.5 N#/min to raise the pressure inside the column to 3.5 N#/min.
After increasing the pressure to 0 ky/d, G, the mixed gas is further introduced and valve 70 is opened so as to maintain the pressure in the column at k 3.0 kz/cm, G. The gas that flows out at this time is discarded. Before breakthrough [valve 61, 7Q was closed to complete the adsorption process, valve 73 was opened until the internal pressure of lrA reached (1,1 gin/crl, G), and the product recovery process was completed. The effluent gas is introduced into the C tower and depressurized.Next, valve 63 is opened and all the product gas is introduced from the product intermediate tank for cleaning. Continue to introduce it into C tower.6
3.73% after finishing the shite cleaning process with the valve fully open
The nozzle 62 is opened and the vacuum pump 11 is operated to desorb carbon monoxide and recover the product gas. This desorption operation was carried out until the pressure inside the A tower reached ] 00 Tarr.
脱着終了後６２のバルブを閉にし、次に７４のバルブ全
開にしてＢ塔の減圧放圧時の流出ガス全導入してｏｌｋ
ｐ ／ｆｆ１．Ｇまで昇圧し、次にＢ塔の洗浄工程時の
流出ガスをひき続き導入して１１．８ ｋｚ ／ （ｙ
ｄ、Ｇまで昇圧させる。この後、混合ガスを前述と同様
に吸着塔に導入して吸着工程以下の操作金繰り返した。After the desorption is completed, close the valve 62, then fully open the valve 74, and introduce all the effluent gas from the B column during depressurization and release.
p/ff1. The pressure was increased to 11.8 kz/(y
d, raise the pressure to G. Thereafter, the mixed gas was introduced into the adsorption tower in the same manner as described above, and the operations following the adsorption step were repeated.
Ｂ塔及びＣ塔も同じ条件となる様［、定期的に吸着塔間
の流れをたえて操作を繰り返した。１サイクル６分で行
い２時間運転した。The operation was repeated by periodically increasing the flow between the adsorption towers so that the conditions were the same for the B tower and the C tower. One cycle was performed for 6 minutes and the operation was for 2 hours.
運転開始後１時間３０分から２時間までの３０分間のガ
ス量は、混合ガスの供給量が１０５ Ｎ＃で、流出廃棄
ガス量は５１ＮＩ！／、そのＣＯ換度は４０．５％、ま
た回収ガス量は５５ Ｎ＃％ＣＯ洟度は９９．０％であ
ったが、この時００回収率は７２０％であった。The amount of gas supplied for 30 minutes from 1 hour 30 minutes to 2 hours after the start of operation was 105 N# of mixed gas, and the amount of waste gas flowing out was 51 NI! /, the CO exchange rate was 40.5%, the amount of recovered gas was 55 N#%, the CO concentration was 99.0%, and the 00 recovery rate was 720%.
（発明の効果）
本発明は、少な（とも−酸ｆヒ炭素及び窒業を含む原料
ガス〃１ら、純度９９％以上の一酸化炭素ガスを分離精
製する際に、従来の吸着法に比べて８０％と込う高い回
収率で製品一酸化炭素ガスを回収することができる。本
発明によるＰＳＡ法では、２本あるいは３本という少な
い吸着塔数で製品ガスの連続生産が可能であり、設備コ
ストがかからず、またバルブ等の操作が簡単であるため
容易に自動化することができる。それ換え従来のＰＳＡ
法による一酸化炭素分離精製法に比べより安価に高純Ｋ
Ｍ品ガスが得られる方法であり、転煩ガス及び高炉ガス
から有機合成用原料として、また冶金反応等に非常に有
用である一酸化炭素ガスを安価に供給する事が可能とな
る。(Effects of the Invention) The present invention is effective in separating and refining carbon monoxide gas with a purity of 99% or higher, compared to conventional adsorption methods. Product carbon monoxide gas can be recovered with a high recovery rate of 80%.The PSA method according to the present invention allows continuous production of product gas with as few as two or three adsorption towers. It can be easily automated because there is no equipment cost and the operation of valves etc. is simple.Instead, conventional PSA
Highly pure K at a lower cost than carbon monoxide separation and purification methods
This is a method for obtaining M-product gas, and it becomes possible to supply carbon monoxide gas, which is very useful as a raw material for organic synthesis and in metallurgical reactions, at a low cost from gas and blast furnace gas.
第１図は２塔弐ＰＥＡ装置において本発明を実施するサ
イクルタイムシステムの一例を示す図、第２図は本発明
を実施する友めの２塔式ＰＳＡ装置の一例を示す図。
第３図は３塔式ＰＳ＆装置において本発明を実施するサ
イクルタイムシステムの一例を示す図。
第４図は本発明を実施するための３塔式ＰＥＡ装誼の一
例を示す図、
第５図は従来の方法による３塔式ＰＳＡ装置のサイクル
タイムシステムの一例を示す図、第６図は従来の方法を
実施する３塔弐ＰＳＡ装置の一例を示す図である。
】〜１０・・・バルブ、１１・・−真空ポンプ、１２・
・・製品ガス中間タンク、１３・・・パン７アタンク、
４１〜５５．６］〜７５・・・バルブ。
代理人 弁理士 秋 沢 政 光
信２名
７ｉ２図
１／′）
井１図
肚過茜鼎FIG. 1 is a diagram showing an example of a cycle time system implementing the present invention in a two-column PEA device, and FIG. 2 is a diagram showing an example of a companion two-column PSA device implementing the present invention. FIG. 3 is a diagram showing an example of a cycle time system for implementing the present invention in a three-column PS& device. FIG. 4 is a diagram showing an example of a three-column type PEA equipment for carrying out the present invention, FIG. 5 is a diagram showing an example of a cycle time system of a three-column type PSA device using a conventional method, and FIG. FIG. 2 is a diagram showing an example of a three-tower PSA device implementing a conventional method. ] ~10...Valve, 11...-Vacuum pump, 12...
...Product gas intermediate tank, 13...Pan 7 tank,
41-55.6]-75...Valve. Agent Patent Attorney Masaaki Aki Sawa Mitsunobu 2 people 7i2 Figure 1/') Figure 1
Claims (1)
素を吸着法により分離精製する方法において、該原料ガ
ス中の一酸化炭素に対して選択吸着性を有する吸着剤を
充填した２つ以上の吸着塔を使用して、 （ａ）原料ガスを吸着塔に導入して所定の圧力まで昇圧
させた後、原料ガスを流通させて一酸化炭素を吸着させ
る吸着工程、 （ｂ）吸着工程終了後、吸着塔内のガスを放出させて吸
着塔の圧力を降下させる減圧工程。 （ｃ）減圧工程終了後、製品一酸化炭素ガスを吸着工程
時の原料ガス流通方向と同じ方向に導入して、難吸着成
分をパージする洗浄工程、 （ｄ）洗浄工程終了後、吸着塔の原料ガス入口側から大
気圧以下に排気して吸着剤に吸着している一酸化炭素を
脱着させ、製品一酸化炭素ガスを回収する製品ガス回収
工程、 （ｅ）製品ガス回収工程終了後の吸着塔へ、（ｃ）の洗
浄工程の吸着塔から流出するガスを吸着工程時の原料ガ
ス流通方向と逆の方向に導入して、前者の吸着塔内を昇
圧する昇圧（ I ）工程、 （ｆ）昇圧（ I ）工程終了後の吸着塔へ、（ｂ）の減
圧工程時の吸着塔からの放出ガスを吸着工程時の原料ガ
ス流通方向と逆の方向に導入して、前者の吸着塔内を昇
圧する昇圧（II）工程、 からなる操作を定期的に吸着塔間の流れをかえて繰り返
すことを特徴とする一酸化炭素ガスの分離精製法。(1) In a method for separating and refining carbon monoxide in a raw material gas containing carbon monoxide and nitrogen by an adsorption method, two types are filled with an adsorbent that has selective adsorption properties for carbon monoxide in the raw material gas. Using the above adsorption tower, (a) an adsorption step in which the raw material gas is introduced into the adsorption tower, the pressure is increased to a predetermined pressure, and then the raw material gas is circulated to adsorb carbon monoxide; (b) an adsorption step After completion of the depressurization process, the gas inside the adsorption tower is released to lower the pressure of the adsorption tower. (c) After the decompression process, a cleaning process in which the product carbon monoxide gas is introduced in the same direction as the flow direction of the raw material gas during the adsorption process to purge difficult-to-adsorb components; (d) After the cleaning process, the adsorption tower A product gas recovery process in which carbon monoxide adsorbed on an adsorbent is desorbed by exhausting the source gas to below atmospheric pressure from the inlet side and product carbon monoxide gas is recovered; (e) Adsorption after the product gas recovery process is completed; a pressurization (I) step in which the gas flowing out from the adsorption tower in the cleaning step of (c) is introduced into the tower in a direction opposite to the flow direction of the raw material gas during the adsorption step to raise the pressure inside the former adsorption tower; ) After the pressurization (I) step, the gas released from the adsorption tower during the pressure reduction step in (b) is introduced into the adsorption tower in the opposite direction to the flow direction of the raw material gas during the adsorption step, and the gas released into the adsorption tower is A method for separating and purifying carbon monoxide gas, which is characterized by repeating the following steps by periodically changing the flow between adsorption towers:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61009467A JPS62168525A (en) | 1986-01-20 | 1986-01-20 | Method for separating and purifying carbon monoxide by adsorption |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61009467A JPS62168525A (en) | 1986-01-20 | 1986-01-20 | Method for separating and purifying carbon monoxide by adsorption |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS62168525A true JPS62168525A (en) | 1987-07-24 |
| JPH0221285B2 JPH0221285B2 (en) | 1990-05-14 |
Family
ID=11721081
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61009467A Granted JPS62168525A (en) | 1986-01-20 | 1986-01-20 | Method for separating and purifying carbon monoxide by adsorption |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS62168525A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6397213A (en) * | 1986-10-15 | 1988-04-27 | Mitsui Eng & Shipbuild Co Ltd | Pressure-swinging adsorption and separation method |
| JP2008152383A (en) * | 2006-12-14 | 2008-07-03 | Fuji Electric Systems Co Ltd | Cleaning work allocation device, cleaning work allocation method, and cleaning work allocation program |
-
1986
- 1986-01-20 JP JP61009467A patent/JPS62168525A/en active Granted
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6397213A (en) * | 1986-10-15 | 1988-04-27 | Mitsui Eng & Shipbuild Co Ltd | Pressure-swinging adsorption and separation method |
| JPH0478324B2 (en) * | 1986-10-15 | 1992-12-10 | Mitsui Shipbuilding Eng | |
| JP2008152383A (en) * | 2006-12-14 | 2008-07-03 | Fuji Electric Systems Co Ltd | Cleaning work allocation device, cleaning work allocation method, and cleaning work allocation program |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0221285B2 (en) | 1990-05-14 |
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