JPH0411632B2 - - Google Patents
Info
- Publication number
- JPH0411632B2 JPH0411632B2 JP21444084A JP21444084A JPH0411632B2 JP H0411632 B2 JPH0411632 B2 JP H0411632B2 JP 21444084 A JP21444084 A JP 21444084A JP 21444084 A JP21444084 A JP 21444084A JP H0411632 B2 JPH0411632 B2 JP H0411632B2
- Authority
- JP
- Japan
- Prior art keywords
- nmp
- solvent
- sacrificial metal
- line
- extract
- 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
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 54
- 229910052751 metal Inorganic materials 0.000 claims description 23
- 239000002184 metal Substances 0.000 claims description 23
- 239000002904 solvent Substances 0.000 claims description 23
- 238000000034 method Methods 0.000 claims description 10
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 9
- 229910052749 magnesium Inorganic materials 0.000 claims description 9
- 239000011777 magnesium Substances 0.000 claims description 9
- 238000000638 solvent extraction Methods 0.000 claims description 6
- 238000005260 corrosion Methods 0.000 claims description 5
- 230000007797 corrosion Effects 0.000 claims description 5
- 150000002739 metals Chemical class 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052788 barium Inorganic materials 0.000 claims description 2
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 239000011575 calcium Substances 0.000 claims description 2
- 229910052712 strontium Inorganic materials 0.000 claims description 2
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 239000011701 zinc Substances 0.000 claims description 2
- 238000010276 construction Methods 0.000 claims 1
- 230000005764 inhibitory process Effects 0.000 claims 1
- 238000011084 recovery Methods 0.000 description 9
- 239000007788 liquid Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 239000013557 residual solvent Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 239000011449 brick Substances 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 235000012489 doughnuts Nutrition 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910001092 metal group alloy Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
Landscapes
- Extraction Or Liquid Replacement (AREA)
- Prevention Of Electric Corrosion (AREA)
Description
【発明の詳細な説明】
発明の分野
本発明は、選択的Ｎ−メチル−２−ピロリドン
（NMP）溶剤抽出プロセスにおける腐食を抑制
する方法に関する。DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a method for inhibiting corrosion in a selective N-methyl-2-pyrrolidone (NMP) solvent extraction process.
発明の概要
選択的Ｎ−メチル−２−ピロリドン（NMP）
溶剤抽出プロセスはプロセス設備の腐食問題に悩
まされている。この腐食は、反応／抽出容器、溶
剤回収容器、溶剤取扱い配管、冷却用容器等を含
めてプロセス設備の構成に使用された材料より高
い電気化学的ポテンシヤルを有する金属乃至金属
合金を含む接触帯域或いは床において犠牲金属と
NMP流れとを接触することにより著しく軽減さ
れうることが見出された。設備が炭素鋼或いはス
テンレス鋼から成るプラントにおいて使用するに
好ましい犠牲金属の例は、マグネシウム、亜鉛、
カルシウム、バリウム、ストロンチウムであり、
好ましいものはマグネシウムである。これら犠牲
金属は、バー、ロツド、リボン、ストリツプ、シ
エービング、スポンジ、フアイリング、チツプ、
ドーナツ、ビード、ノジユール、ブロツク、ブリ
ツク、シート等を含む任意の都合の良い形態にお
いて使用されうる。犠牲金属は、NMP回収流れ
中に任意の都合の良い位置において、好ましくは
回収流れ中の該流れが主にNMPであるような地
点において挿入されうる。犠牲金属は塔のフラツ
シユ帯域において一定の間隔で大きな中実ブロツ
ク或いはシートとして挿入さえなしうる。NMP
流れが犠牲金属と接触する或いはそれを貫いて若
しくは乗越えて通る条件に関しては特別な予備注
意は必要とされない。しかし、犠牲金属は溶剤回
収流れ中NMP回収流れの温度が約250〜600〓に
好ましくは約400〜600〓に昇温される地点に位置
づけられることが好ましい。その結果、犠牲金属
の配置の為の好ましい位置は流れの温度が約525
〓でありそしてNMP流れが好ましくは丁度凝縮
を開始せんとする蒸気の形態にあるようなNMP
回収オーバヘツド流れ中である。SUMMARY OF THE INVENTION Selective N-methyl-2-pyrrolidone (NMP)
Solvent extraction processes suffer from corrosion problems in process equipment. This corrosion may occur in contact zones or contact zones containing metals or metal alloys that have a higher electrochemical potential than the materials used to construct the process equipment, including reaction/extraction vessels, solvent recovery vessels, solvent handling piping, cooling vessels, etc. sacrificial metal on the floor
It has been found that it can be significantly alleviated by contacting with a NMP stream. Examples of preferred sacrificial metals for use in plants where equipment is constructed of carbon steel or stainless steel include magnesium, zinc,
Calcium, barium, strontium,
Preferred is magnesium. These sacrificial metals include bars, rods, ribbons, strips, shavings, sponges, firings, chips,
It can be used in any convenient form, including donuts, beads, nodules, blocks, bricks, sheets, and the like. The sacrificial metal may be inserted into the NMP recovery stream at any convenient location, preferably at a point in the recovery stream where the stream is predominantly NMP. The sacrificial metal may even be inserted as large solid blocks or sheets at regular intervals in the flash zone of the tower. NMP
No special precautions are required as to the conditions under which the flow will contact or pass through or over the sacrificial metal. However, it is preferred that the sacrificial metal be located in the solvent recovery stream at a point where the temperature of the NMP recovery stream is raised to about 250-600°C, preferably about 400-600°C. As a result, the preferred location for sacrificial metal placement is at a flow temperature of approximately 525°C.
〓 and the NMP stream is preferably in the form of a vapor just about to start condensing.
Recovery overhead is in flow.
発明の具体的説明
第１及び２図は代表的なNMP溶剤抽出プラン
トの系統図である。犠牲金属接触帯域或いは床が
有益に位置づけられうる位置は第１図にＡ〜Ｆそ
して第２図にＡ〜Ｃとして示されている。こうし
た帯域或いは床の１つ以上が必要に応じて使用さ
れうる。好ましくは、犠牲金属は第１図に表示Ａ
即ちフラツシユ塔オーバヘツド流れの地点に位置
づけられる。第２の選択は、乾燥塔或いは高圧フ
ラツシユ塔のフラツシユ帯域に犠牲金属のシート
を位置づけることである。DETAILED DESCRIPTION OF THE INVENTION Figures 1 and 2 are system diagrams of a typical NMP solvent extraction plant. Locations where sacrificial metal contact zones or beds may be advantageously located are shown as A-F in FIG. 1 and A-C in FIG. 2. One or more of these zones or floors may be used as desired. Preferably, the sacrificial metal is labeled A in FIG.
That is, it is located at the point of the flash tower overhead flow. A second option is to position a sheet of sacrificial metal in the flash zone of a drying tower or high pressure flash tower.
第１図は、スチームストリツピングプラントに
おいて抽出液からのNMP回収工程の概略図を表
す。抽出プロセスからの抽出液は、管路１を経由
して乾燥器２に送られる。抽出液は加熱器３にお
いて管路４における乾き溶剤との間接熱交換によ
り予熱ずみである。乾燥器２において、抽出液は
脱水されて、主に水から成るオーバヘツド部分
（これは最終的にNMPと再混合されて抽出帯域
（図示なし）で使用される）と抽出物／溶剤部分
とを生みだす。前者は管路５にそして後者は管路
６に通る。乾燥器２からの抽出物／溶剤は管路７
において管路４における乾き溶剤オーバヘツドと
のユニツト８での熱交換により加熱される。乾燥
器２からの抽出物／溶剤は、管路６を経て、加熱
器（炉９）を通つてフラツシユ塔１０に送られ
る。フラツシユ塔において、溶剤はオーバヘツド
として蒸発分離され（管路４）そして抽出物は管
路１１を経て回収されそしてストリツパー１２に
送られ、ここで残留する僅かの溶剤が管路１３か
らのスチームを使用して蒸発分離される。この残
留溶剤は管路１４を経てストリツパー１２から回
収されて溶剤回収プロセスへ再循環され、他方抽
出物は管路１５を経て回収される。 FIG. 1 represents a schematic diagram of the NMP recovery process from the extract in a steam stripping plant. The extract from the extraction process is sent to the dryer 2 via line 1. The extract liquid has been preheated in heater 3 by indirect heat exchange with the dry solvent in line 4. In dryer 2, the extract is dehydrated to separate an overhead part consisting mainly of water (which is ultimately remixed with NMP and used in the extraction zone (not shown)) and an extract/solvent part. produce. The former passes into line 5 and the latter into line 6. Extract/solvent from dryer 2 goes to line 7
It is heated by heat exchange in unit 8 with the dry solvent overhead in line 4. The extract/solvent from dryer 2 is sent via line 6 to flash column 10 through a heater (furnace 9). In the flash column, the solvent is evaporated off as overhead (line 4) and the extract is recovered via line 11 and sent to a stripper 12, where the remaining solvent is removed using steam from line 13. It is separated by evaporation. This residual solvent is recovered from the stripper 12 via line 14 and recycled to the solvent recovery process, while the extract is recovered via line 15.
このスチームストリツピング系統において、犠
牲金属接触帯域或いは床は多くの場所において位
置づけることが出来る。以下に呈示する実験にお
いて、犠牲金属はフラツシユ帯域からの乾き溶剤
オーバヘツド管路（図面における管路４）におけ
る位置Ａに位置づけられた。位置Ａにおいて、流
れは約525〓における蒸気の形態にある。また別
の位置は、乾燥器内の管路７に対する加熱された
抽出物／溶剤流れ導入口における位置Ｂであり、
ここでは流れは約450〓における蒸気／液体形態
にある。位置Ｃはフラツシユ塔内の溶剤導入口に
あり、ここでは流れ約600〓における蒸気／液体
形態にある。位置Ｄはストリツパーからのオーバ
ヘツド管路１４内にあり、ここでは流れは約400
〓における蒸気形態にある。位置Ｅは乾燥器から
のオーバヘツド管路５にあり、ここでは流れは約
250〓における水に富む蒸気形態にある。位置Ｆ
は抽出液供給管路１にあり、ここでは流れは約
390〓における液体の形態にある。 In this steam stripping system, the sacrificial metal contact zone or bed can be located in many locations. In the experiments presented below, the sacrificial metal was positioned at position A in the dry solvent overhead line (line 4 in the drawings) from the flash zone. At position A, the flow is in the form of steam at about 525°. Another location is location B at the heated extract/solvent stream inlet to line 7 in the dryer;
Here the flow is in vapor/liquid form at about 450°. Location C is at the solvent inlet in the flash column, here in vapor/liquid form at a flow of about 600 ml. Location D is in the overhead line 14 from the stripper, where the flow is approximately 400 m
It is in vapor form at 〓. Location E is in the overhead line 5 from the dryer, where the flow is approximately
250〓 in water-rich vapor form. Position F
is in extract supply line 1, where the flow is approximately
390〓 in liquid form.
第２図は気体ストリツピングプラントにおける
抽出液からのNMP回収系統を示す。抽出液／溶
剤は管路１において熱交換器２に通りここで流れ
は精留塔４から流れる管路３における乾き溶剤と
の間接熱交換により昇温される。熱交換器２から
の加熱された抽出液／溶剤は管路５を経て加熱炉
６に送られそして後管路７を経て精留塔４に送ら
れる。精留塔から、乾き溶剤は管路３を経て回収
されそして抽出液／溶剤流れは管路８を経て回収
されそしてストリツパー９に送られる。ストリツ
パー９において、残留溶剤を蒸発分離するのに管
路１０からのストリツピング気体流れが使用され
る。残留溶剤は管路１１を経て精留塔に戻して送
られる。気体ストリツピングプラントにおいて、
犠牲金属は好ましくは乾き溶剤オーバヘツド管路
（図面の管路３）における位置Ａに配置され、こ
こでは流れは約525〓における蒸気形態にある。
別様には、犠牲金属は精留塔内で高温抽出液／溶
剤導入口における位置Ｂに配置でき、ここでは流
れは約600〓における蒸気／液体形態にある。或
いは、犠牲金属は加熱炉に通じる抽出液／溶剤管
路５内の位置Ｃに配置でき、ここでは流れは約
480〓における液体状態にある。 Figure 2 shows the NMP recovery system from extract in a gas stripping plant. The extract/solvent passes in line 1 to heat exchanger 2 where the stream is heated by indirect heat exchange with dry solvent in line 3 flowing from rectification column 4. The heated extractant/solvent from the heat exchanger 2 is sent via line 5 to the heating furnace 6 and then via line 7 to the rectification column 4. From the rectification column, dry solvent is recovered via line 3 and the extract/solvent stream is recovered via line 8 and sent to stripper 9. In stripper 9, the stripping gas stream from line 10 is used to evaporate off residual solvent. The residual solvent is sent back to the rectification column via line 11. In a gas stripping plant,
The sacrificial metal is preferably placed at location A in the dry solvent overhead line (line 3 in the drawings), where the flow is in vapor form at about 525°.
Alternatively, the sacrificial metal can be placed in the rectification column at position B at the hot extract/solvent inlet, where the flow is in vapor/liquid form at about 600°C. Alternatively, the sacrificial metal can be placed at location C in the extractant/solvent line 5 leading to the furnace, where the flow is approximately
It is in a liquid state at 480〓.
例
NMP溶剤抽出プラントにおいて、冷却水熱交
換器はすべて漏洩水を排除する為補修若しくは交
換された。６インチ直径×２フイート長容器内の
マグネシウムチツプの試験床が溶剤フラツシユ塔
オーバヘツドから流れてくる高温NMP蒸気（約
525〓）の小さなスリツプ流れに据付けられた。
NMP蒸気は、マグネシウム床と接触して流れる
NMPの総容積が系統内のNMPの保蔵量の少く
とも２倍であるよう何日もにわたつてマグネシウ
ムチツプと接触せしめられた。その後、試験床は
開かれそして検査された。マグネシウムの大部分
が消尽されたことが観察された。マグネシウム床
が据付けられる前後での循回NMPのPHの測定
は、約１〜1.5PH単位の増加を示した。恐らく、
これは数ケ月にわたつて累積しそしてNMP流れ
中で循環していた強酸の除去から生じたものであ
ろう。生成したマグネシウム塩は恐らく抽出物と
一緒に系統から取出されそして循回されなかつた
ものと思われる。プラントを構成する容器及び管
路の腐食はとまつた。Example In an NMP solvent extraction plant, all cooling water heat exchangers were repaired or replaced to eliminate leakage water. A test bed of magnesium chips in a 6 inch diameter x 2 foot long vessel was exposed to hot NMP vapor (approx.
525〓) installed in a small slip stream.
NMP vapor flows in contact with the magnesium bed
The NMP was contacted with the magnesium chips over a number of days so that the total volume of NMP was at least twice the amount of NMP stored in the system. The test bed was then opened and inspected. It was observed that most of the magnesium was depleted. Measurements of the PH of circulating NMP before and after the magnesium bed was installed showed an increase of approximately 1-1.5 PH units. perhaps,
This may have resulted from the removal of strong acids that had accumulated over several months and were circulating in the NMP stream. The magnesium salts formed were probably removed from the system along with the extract and not recycled. Corrosion of the containers and pipes that make up the plant has stopped.
第１及び２図は、代表的なNMP溶剤抽出プラ
ントの流れ系統図である。
第１図の主要要素は次の通りである、１……抽
出液供給管路、３……熱交換器、２……乾燥器、
１０……フラツシユ塔、１２……ストリツパー、
第２図の主要要素は次の通りである、１……抽出
液供給管路、２……熱交換器、４……精留塔、９
……ストリツパー。
Figures 1 and 2 are flow diagrams of a typical NMP solvent extraction plant. The main elements in Figure 1 are as follows: 1...extract supply pipe, 3...heat exchanger, 2...dryer,
10... Flash tower, 12... Stripper,
The main elements in Figure 2 are as follows: 1...extract supply pipe, 2...heat exchanger, 4...rectification column, 9
...Stripper.
Claims (1)
（NMP）溶剤抽出プロセスプラントにおいて該
プラントの構成に使用された金属より高い電気化
学的ポテンシヤルを有する犠牲金属を使用し、
NMP溶剤流れを犠牲金属と接触せしめることを
特徴とする腐食抑制方法。 ２ 犠牲金属が、マグネシウム、亜鉛、カルシウ
ム、バリウム及びストロンチウムの群から選択さ
れる特許請求の範囲第１項記載の方法。 ３ 犠牲金属がマグネシウムである特許請求の範
囲第２項記載の方法。 ４ NMPが約250〜600〓の温度において犠牲金
属と接触される特許請求の範囲第１〜３項のうち
のいずれかの項記載の方法。Claims: 1. Using a sacrificial metal in a selective N-methyl-2-pyrrolidone (NMP) solvent extraction process plant that has a higher electrochemical potential than the metals used in the construction of the plant;
A corrosion inhibition method characterized by bringing an NMP solvent stream into contact with a sacrificial metal. 2. The method of claim 1, wherein the sacrificial metal is selected from the group of magnesium, zinc, calcium, barium and strontium. 3. The method according to claim 2, wherein the sacrificial metal is magnesium. 4. A method according to any one of claims 1 to 3, wherein the NMP is contacted with the sacrificial metal at a temperature of about 250-600°C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21444084A JPS6196090A (en) | 1984-10-15 | 1984-10-15 | Removal of corrosive substance from nmp solvent by contact with sacrifice metal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21444084A JPS6196090A (en) | 1984-10-15 | 1984-10-15 | Removal of corrosive substance from nmp solvent by contact with sacrifice metal |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS6196090A JPS6196090A (en) | 1986-05-14 |
| JPH0411632B2 true JPH0411632B2 (en) | 1992-03-02 |
Family
ID=16655807
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP21444084A Granted JPS6196090A (en) | 1984-10-15 | 1984-10-15 | Removal of corrosive substance from nmp solvent by contact with sacrifice metal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6196090A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2362205A1 (en) | 2010-02-19 | 2011-08-31 | Mitsubishi Heavy Industries, Ltd. | Tire inflation method for tire testing machine |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100371680B1 (en) * | 2000-08-18 | 2003-02-11 | 한국지질자원연구원 | Method for long term and continuos operation of supported liquid membrane by periodical supply of extraction reagent |
| KR20030043368A (en) * | 2001-11-28 | 2003-06-02 | 한국지질자원연구원 | Supply method of extraction reagent for prevent decreasing of extraction efficiency on the immobilized liquid membrane |
-
1984
- 1984-10-15 JP JP21444084A patent/JPS6196090A/en active Granted
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP2362205A1 (en) | 2010-02-19 | 2011-08-31 | Mitsubishi Heavy Industries, Ltd. | Tire inflation method for tire testing machine |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6196090A (en) | 1986-05-14 |
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