JPS6116370B2 - - Google Patents
Info
- Publication number
- JPS6116370B2 JPS6116370B2 JP3362182A JP3362182A JPS6116370B2 JP S6116370 B2 JPS6116370 B2 JP S6116370B2 JP 3362182 A JP3362182 A JP 3362182A JP 3362182 A JP3362182 A JP 3362182A JP S6116370 B2 JPS6116370 B2 JP S6116370B2
- Authority
- JP
- Japan
- Prior art keywords
- adsorbent
- heptane
- water
- adsorption
- adsorption tower
- 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
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 70
- 239000003463 adsorbent Substances 0.000 claims description 34
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000011148 porous material Substances 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 11
- 229910021536 Zeolite Inorganic materials 0.000 claims description 10
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims description 10
- 239000010457 zeolite Substances 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000001179 sorption measurement Methods 0.000 description 29
- 239000002808 molecular sieve Substances 0.000 description 4
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003034 coal gas Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000007327 hydrogenolysis reaction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 description 1
Description
本発明は、粗ベンゾールの精製方法に関し、更
に詳しくは、ｎ−ヘプタンと水とを含有する粗ベ
ンゾールの精製方法に関する。
例えば石炭ガスの製造に際し副生する粗ベンゾ
ールからのｎ−ヘプタンの除去は、通常、高温高
圧下での水添分解、或いはスルホラン等による抽
出により行なわれている。しかしながら、これ等
の方法には、エネルギーコストが高いという欠点
がある。本発明者は、従来法の欠点を解消すべく
種々研究を進めるうちに、吸着法によりｎ−ヘプ
タンの除去を行なうことを着想した。一般に吸着
除去法を採用する場合には、例えば、モレキユラ
ーシーブ（商標）として知られているゼオライト
系吸着剤を充填した吸着塔に粗ベンゾールを通
し、ｎ−ヘプタンを吸着除去することになる。し
かるに、粗ベンゾールは水分をも含有しており、
吸着剤には水分とｎ−ヘプタンとが吸着される。
従つて、吸着剤の再生時には、ｎ−ヘプタンのコ
ーキングを防止すべく、先ず120〜150℃の比較的
低温に吸着剤を加熱してｎ−ヘプタンの脱着を行
ない、次いで吸着剤を250℃程度の高温に加熱し
て水分の脱着を行なう必要がある。従つて、この
方法には、(イ)脱着操作を２段階で行なう為、煩雑
である。(ロ)150℃までの低温での加熱ではｎ−ヘ
プタンの脱着が完全に行なわれない為、250℃近
傍の加熱によつて残存するｎ−ヘプタン（常温平
衡吸着量の２〜３℃程度）のコーキングが発生す
ることは避け難い。この為、吸着と脱着とを繰返
すにしたがつて吸着能が次第に低下し、吸着剤の
寿命が短いものとなる等の欠点があり、公知の吸
着法をｎ−ヘプタンの除去にそのまま転用するこ
とは不可能となることが判明した。
本発明者は、上記の如き現状に鑑みて更に種々
実験及び研究を重ねるうちに、水とｎ−ヘプタン
の吸着除去を順次別個に行なう場合には、吸着剤
の寿命が飛躍的に延長されることを見出し、本発
明を完成するにいたつた。即ち、本発明は、ｎ−
ヘプタンと水とを含有する粗ベンゾールを精製す
るに際し、細孔径４Å程度の細孔から主としてな
るゼオライト系吸着剤により水分を吸着除去した
後、細孔径５〜13Å程度の細孔から主としてなる
ゼオライト系吸着剤及び活性炭の少なくとも１種
によりｎ−ヘプタンを吸着除去し、次いで上記の
両吸着剤を加熱して水分及びｎ−ヘプタンを夫々
脱着することを特徴とする粗ベンゾールの精製方
法に係る。
以下、図面に示す実施態様を参照しつつ、本発
明を更に詳細に説明する。
第１図において、水分及びｎ−ヘプタンを含有
する粗ベンゾールは、ライン１から、水分を選択
的に吸着する第１の吸着剤３を充填する第１の吸
着塔５に供給される。水分を選択的に吸着する吸
着剤としては、細孔径４Å程度の細孔から主とし
てなるゼオライト系吸着剤を使用する。吸着時の
条件は、温度10〜50℃程度、圧力常圧近傍、線速
度１〜20cm／分程度とすることが好ましい。水分
を除去された粗ベンゾールは、ライン７を経てｎ
−ヘプタンの吸着能を有する第２の吸着剤９を充
填された第２の吸着塔１１に送られ、ここでｎ−
ヘプタンが吸着除去される。第２の吸着剤として
は、ｎ−ヘプタンを選択的に吸着し得るものが好
ましいが、すでに粗ベンゾール中の水分が十分に
除去されているので、水分吸着能をも併有するも
のであつても使用可能である。第２の吸着剤とし
ては、細孔径５Å乃至13Å程度の細孔から主とし
てなる吸着剤、より具体的には、細孔５〜13Å程
度の細孔から主としてなるゼオライト系吸着剤及
び活性炭の少なくとも１種が使用される。第２の
吸着塔１１における吸着条件は、温度10〜50℃程
度、圧力常圧近傍、線速度１〜20cm／分程度とす
ることが好ましい。第２の吸着塔１１においてｎ
−ヘプタンの除去を終えたベンゾールは、ライン
１３から系外に取り出される。
所定時間の運転後に行なわれる吸着剤の再生処
理は、第１の吸着剤の場合には、200〜300℃程度
に加熱して水撫を脱着させ、又第２の吸着剤の場
合には、90〜150℃程度に加熱するとともに100〜
200mmHg（絶対圧）程度に吸着塔１１内を減圧す
ることにより、行なうのが好ましい。
尚、第１の吸着塔５と第２の吸着塔１１を１セ
ツトとし、同様のセツトを複数個設けて粗ベンゾ
ールの供給を順次切りかえる場合には、粗ベンゾ
ールの精製を連続的に行なうことが出来る。
本発明によれば、以下の如き効果が達成され
る。
(a) 水分とｎ−ヘプタンの吸着が別個に行なわれ
るので、再生間隔が延長される。
(b) 各吸着塔の再生が一段階で行なわれるので、
再生時間の短縮及び所要エネルギーの節減が可
能となる。
(c) 吸着剤の寿命が著るしく延長される。
(d) 吸着剤の使用量が減少する。
実施例 １
水800ppm及びｎ−ヘプタン1000ppmを含む粗
ベンゾールを、ゼオライト吸着剤（商標：モレキ
ユラーシーブ4A、米国リンデ社製）２m3を充填
させた内径1.2mの第１吸着塔に供給し水分の除
去を行なつた。吸着条件は、常温、常圧で線速度
８cm／minであつた。次いで、第１吸着塔を出た
粗ベンゾールを、ゼオライト吸着剤（商標モレキ
ユラーシーブ5A、米国リンデ社製）４m3を充填
させた内径1.2mの第２吸着塔に送り、ｎ−ヘプ
タンの吸着除去を行なつた。吸着条件は、常温、
常圧で線速度８cm／minであつた。
第１表に本実施例の結果を示す。
比較例 １
内径1.2mの単一の吸着塔にゼオライト吸着剤
（モレキユラーシーブ5A）10m3を充填し、実施例
１と同様の粗ベンゾールを常温、常圧下に線速度
８cm／minで吸着処理した。
結果は、第１表に示す通りである。
The present invention relates to a method for purifying crude benzole, and more particularly to a method for purifying crude benzole containing n-heptane and water. For example, n-heptane is usually removed from crude benzole, which is produced as a by-product during the production of coal gas, by hydrogenolysis under high temperature and pressure, or extraction using sulfolane or the like. However, these methods have the disadvantage of high energy costs. The inventor of the present invention came up with the idea of removing n-heptane by an adsorption method while proceeding with various studies to overcome the drawbacks of conventional methods. Generally, when an adsorption removal method is adopted, for example, crude benzole is passed through an adsorption column filled with a zeolite adsorbent known as Molecular Sieve (trademark) to adsorb and remove n-heptane. . However, crude benzol also contains water,
Moisture and n-heptane are adsorbed on the adsorbent.
Therefore, when regenerating the adsorbent, in order to prevent n-heptane coking, the adsorbent is first heated to a relatively low temperature of 120 to 150°C to desorb n-heptane, and then the adsorbent is heated to about 250°C. It is necessary to desorb moisture by heating it to a high temperature. Therefore, this method is complicated because (a) the attachment and detachment operations are performed in two steps. (b) Since n-heptane is not completely desorbed when heated at low temperatures up to 150°C, n-heptane remains when heated to around 250°C (about 2 to 3°C of the normal temperature equilibrium adsorption amount). It is unavoidable that caulking will occur. For this reason, as adsorption and desorption are repeated, the adsorption capacity gradually decreases and the life of the adsorbent becomes short.Therefore, known adsorption methods cannot be directly used for the removal of n-heptane. turned out to be impossible. In view of the above-mentioned current situation, the inventor of the present invention has conducted various experiments and researches, and has found that if water and n-heptane are adsorbed and removed sequentially and separately, the life of the adsorbent will be dramatically extended. This discovery led to the completion of the present invention. That is, the present invention provides n-
When purifying crude benzole containing heptane and water, water is adsorbed and removed using a zeolite-based adsorbent mainly composed of pores with a pore diameter of about 4 Å, and then water is adsorbed and removed using a zeolite-based adsorbent mainly composed of pores with a pore diameter of about 5 to 13 Å. The present invention relates to a method for purifying crude benzole, which comprises adsorbing and removing n-heptane using at least one of an adsorbent and activated carbon, and then heating both of the adsorbents to desorb water and n-heptane, respectively. Hereinafter, the present invention will be explained in more detail with reference to embodiments shown in the drawings. In FIG. 1, crude benzole containing water and n-heptane is fed from line 1 to a first adsorption tower 5 filled with a first adsorbent 3 that selectively adsorbs water. As the adsorbent that selectively adsorbs water, a zeolite adsorbent mainly consisting of pores with a pore diameter of about 4 Å is used. The conditions during adsorption are preferably a temperature of about 10 to 50°C, a pressure near normal pressure, and a linear velocity of about 1 to 20 cm/min. The crude benzol from which water has been removed passes through line 7 to n
- is sent to a second adsorption tower 11 filled with a second adsorbent 9 having an adsorption capacity for heptane, where n-
Heptane is adsorbed and removed. As the second adsorbent, it is preferable to use one that can selectively adsorb n-heptane, but since the water in the crude benzene has already been sufficiently removed, it is also possible to use a second adsorbent that also has water adsorption ability. Available for use. The second adsorbent is an adsorbent mainly composed of pores with a pore diameter of about 5 Å to 13 Å, more specifically, a zeolite-based adsorbent mainly composed of pores with a pore size of about 5 Å to 13 Å, and at least one of activated carbon. seeds are used. The adsorption conditions in the second adsorption tower 11 are preferably about a temperature of about 10 to 50°C, a pressure of about normal pressure, and a linear velocity of about 1 to 20 cm/min. In the second adsorption tower 11, n
- Benzol from which heptane has been removed is taken out of the system through line 13. In the case of the first adsorbent, the adsorbent is regenerated by heating it to about 200 to 300°C to desorb the water, and in the case of the second adsorbent, the adsorbent is regenerated after a predetermined period of operation. Heat to around 90~150℃ and heat to 100~
It is preferable to carry out this by reducing the pressure inside the adsorption tower 11 to about 200 mmHg (absolute pressure). In addition, when the first adsorption tower 5 and the second adsorption tower 11 are set as one set, and when a plurality of similar sets are provided and the supply of crude benzole is sequentially switched, it is possible to purify the crude benzol continuously. I can do it. According to the present invention, the following effects are achieved. (a) Since the adsorption of water and n-heptane takes place separately, the regeneration interval is extended. (b) Since the regeneration of each adsorption tower is carried out in one step,
It is possible to shorten the playback time and save the required energy. (c) The lifetime of the adsorbent is significantly extended. (d) The amount of adsorbent used is reduced. Example 1 Crude benzene containing 800 ppm of water and 1000 ppm of n-heptane was supplied to a first adsorption tower with an inner diameter of 1.2 m filled with 2 m 3 of zeolite adsorbent (trademark: Molecular Sieve 4A, manufactured by Linde, USA). Water was removed. The adsorption conditions were normal temperature, normal pressure, and a linear velocity of 8 cm/min. Next, the crude benzene that has come out of the first adsorption tower is sent to a second adsorption tower with an inner diameter of 1.2 m filled with 4 m 3 of zeolite adsorbent (trademark Molecular Sieve 5A, manufactured by Linde, Inc., USA) to remove n-heptane. Adsorption removal was performed. The adsorption conditions were room temperature,
The linear velocity was 8 cm/min at normal pressure. Table 1 shows the results of this example. Comparative Example 1 A single adsorption tower with an inner diameter of 1.2 m was filled with 10 m 3 of zeolite adsorbent (Molecular Sieve 5A), and the same crude benzol as in Example 1 was adsorbed at room temperature and pressure at a linear velocity of 8 cm/min. Processed. The results are shown in Table 1.
【表】
第１表に示す結果から、本発明方法の優れた効
果が明らかである。[Table] From the results shown in Table 1, the excellent effects of the method of the present invention are clear.
第１図は、本発明方法の一実施態様を示すフロ
ーチヤートである。
３……第１の吸着剤、５……第１の吸着塔、９
……第２の吸着剤、１１……第２の吸着塔。
FIG. 1 is a flowchart showing one embodiment of the method of the present invention. 3...First adsorbent, 5...First adsorption tower, 9
...Second adsorbent, 11...Second adsorption tower.
Claims (1)
を精製するに際し、細孔径４Å程度の細孔から主
としてなるゼオライト系吸着剤により水分を吸着
除去した後、細孔径５〜13Å程度の細孔から主と
してなるゼオライト系吸着剤及び活性炭の少なく
とも１種によりｎ−ヘプタンを吸着除去し、次い
で上記の両吸着剤を加熱して水分及びｎ−ヘプタ
ンを夫々脱着することを特徴とする粗ベンゾール
の精製方法。1. When purifying crude benzole containing n-heptane and water, water is adsorbed and removed using a zeolite adsorbent mainly from pores with a pore diameter of about 4 Å, and then water is removed mainly from pores with a pore diameter of about 5 to 13 Å. A method for purifying crude benzole, which comprises adsorbing and removing n-heptane using at least one of a zeolite adsorbent and activated carbon, and then heating both adsorbents to desorb water and n-heptane, respectively.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3362182A JPS58150522A (en) | 1982-03-02 | 1982-03-02 | Purification method of crude benzene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3362182A JPS58150522A (en) | 1982-03-02 | 1982-03-02 | Purification method of crude benzene |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS58150522A JPS58150522A (en) | 1983-09-07 |
| JPS6116370B2 true JPS6116370B2 (en) | 1986-04-30 |
Family
ID=12391515
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3362182A Granted JPS58150522A (en) | 1982-03-02 | 1982-03-02 | Purification method of crude benzene |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS58150522A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5210333A (en) * | 1992-09-30 | 1993-05-11 | Exxon Research And Engineering Company | Benzene removal from hydrocarbon streams |
| JP6346606B2 (en) * | 2012-05-31 | 2018-06-20 | ユーオーピー エルエルシー | Method and apparatus for treating hydrocarbon streams |
| WO2016094249A2 (en) * | 2014-12-12 | 2016-06-16 | Uop Llc | Processes for adsorptive separation of benzene |
-
1982
- 1982-03-02 JP JP3362182A patent/JPS58150522A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS58150522A (en) | 1983-09-07 |
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