JP2003128594A - Method for recovering organic solvent - Google Patents
Method for recovering organic solventInfo
- Publication number
- JP2003128594A JP2003128594A JP2001326079A JP2001326079A JP2003128594A JP 2003128594 A JP2003128594 A JP 2003128594A JP 2001326079 A JP2001326079 A JP 2001326079A JP 2001326079 A JP2001326079 A JP 2001326079A JP 2003128594 A JP2003128594 A JP 2003128594A
- Authority
- JP
- Japan
- Prior art keywords
- organic solvent
- titanium chloride
- recovering
- solution containing
- liquid
- 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.)
- Withdrawn
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、有機溶媒の回収方
法に関するものである。更に詳しくは、本発明は、チタ
ン塩化物を含有する有機溶媒溶液から有機溶媒を分離し
て回収する方法であって、装置の腐食を防止し、かつ作
業上の安全性及び容易性を有するという優れた特徴を有
する有機溶媒の回収方法に関するものである。TECHNICAL FIELD The present invention relates to a method for recovering an organic solvent. More specifically, the present invention is a method for separating and recovering an organic solvent from an organic solvent solution containing titanium chloride, which prevents corrosion of the device and has safety and ease of operation. The present invention relates to a method for recovering an organic solvent having excellent characteristics.
【０００２】[0002]
【従来の技術】たとえば、オレフィンを重合させるため
の触媒を製造する過程において、チタン塩化物を含有す
る有機溶媒溶液からなる廃溶液が発生する。そして、コ
スト節減の観点から、該廃溶液からは有機溶媒を分離し
て回収する必要がある。該分離・回収の手段として、廃
溶液を蒸留することにより有機溶媒を回収する方法があ
る。ところが、従来の方法によると、蒸留時にチタン塩
化物が濃縮された液が得られ、該液は水と接触すること
により塩酸を発生する。塩酸は装置の材質を腐食し、ま
た作業上の安全性と容易性に大きな問題をもたらし、極
めて不都合であった。2. Description of the Related Art For example, in the process of producing a catalyst for polymerizing an olefin, a waste solution consisting of an organic solvent solution containing titanium chloride is generated. Then, from the viewpoint of cost reduction, it is necessary to separate and recover the organic solvent from the waste solution. As a means for the separation and recovery, there is a method of recovering an organic solvent by distilling a waste solution. However, according to the conventional method, a liquid in which titanium chloride is concentrated is obtained at the time of distillation, and the liquid generates hydrochloric acid when contacting with water. Hydrochloric acid corrodes the material of the apparatus and poses a serious problem in safety and easiness in work, which is extremely inconvenient.
【０００３】[0003]
【発明が解決しようとする課題】かかる現状において、
本発明が解決しようとする課題は、チタン塩化物を含有
する有機溶媒溶液から有機溶媒を分離して回収する方法
であって、装置の腐食を防止し、かつ作業上の安全性及
び容易性を有するという優れた特徴を有する有機溶媒の
回収方法を提供する点にある。Under the present circumstances,
The problem to be solved by the present invention is a method of separating and recovering an organic solvent from an organic solvent solution containing titanium chloride, which prevents corrosion of the device, and improves work safety and easiness. The point is to provide a method for recovering an organic solvent having the excellent feature of having.
【０００４】[0004]
【課題を解決するための手段】すなわち、本発明は、チ
タン塩化物を含有する有機溶媒溶液から有機溶媒を分離
して回収する方法であって、下記の工程を有する有機溶
媒の回収方法に係るものである。
分解工程：チタン塩化物を含有する有機溶媒溶液に水酸
化ナトリウム水溶液を添加して混合し、チタン塩化物を
分解する工程
分離工程：分解工程で得られた液を蒸留に付し、有機溶
媒を分離して回収する工程That is, the present invention relates to a method for separating and recovering an organic solvent from an organic solvent solution containing titanium chloride, which method has the following steps: It is a thing. Decomposition step: A sodium hydroxide aqueous solution is added to an organic solvent solution containing titanium chloride and mixed to decompose titanium chloride Separation step: The liquid obtained in the decomposition step is subjected to distillation to remove an organic solvent. Separation and recovery process
【０００５】[0005]
【発明の実施の形態】本発明は、チタン塩化物を含有す
る有機溶媒溶液から有機溶媒を分離して回収する方法で
ある。チタン塩化物としては、Ｔｉ（ＯＲ）mＣｌ
4-m（ｍは０〜３の整数を表し、Ｒは炭素数１〜４のア
ルキル基を表す。）をあげることができ、具体的には四
塩化チタンを例示することができる。有機溶媒として
は、トルエン及びヘキサンを例示することができる。有
機溶媒中のチタン塩化物の濃度としては、５．０〜１
０．０容量％をあげることができる。チタン塩化物を含
有する有機溶媒溶液の例として、オレフィンを重合させ
るための触媒を製造する過程で発生する廃溶液をあげる
ことができる。BEST MODE FOR CARRYING OUT THE INVENTION The present invention is a method for separating and recovering an organic solvent from an organic solvent solution containing titanium chloride. As titanium chloride, Ti (OR) mCl
4-m (m represents an integer of 0 to 3 and R represents an alkyl group having 1 to 4 carbon atoms) can be given, and specific examples thereof include titanium tetrachloride. As the organic solvent, toluene and hexane can be exemplified. The concentration of titanium chloride in the organic solvent is 5.0 to 1
It is possible to increase 0.0% by volume. As an example of the organic solvent solution containing titanium chloride, a waste solution generated in the process of producing a catalyst for polymerizing an olefin can be mentioned.
【０００６】本発明の分解工程は、チタン塩化物を含有
する有機溶媒溶液に水酸化ナトリウム水溶液を添加して
混合し、チタン塩化物を分解する工程である。水酸化ナ
トリウム水溶液の濃度としては、１．０〜６．０重量％
をあげることができる。また、該水溶液の添加量として
は、有機溶剤溶液との重量比で１．０〜２．５倍をあげ
ることができる。本工程の具体的な方法及び条件の例と
しては、次のものをあげることができる。The decomposition step of the present invention is a step of decomposing titanium chloride by adding an aqueous sodium hydroxide solution to an organic solvent solution containing titanium chloride and mixing them. The concentration of the aqueous sodium hydroxide solution is 1.0 to 6.0% by weight.
Can be raised. The amount of the aqueous solution added can be 1.0 to 2.5 times the weight ratio of the organic solvent solution. The following can be mentioned as an example of a specific method and conditions of this step.
【０００７】高速で回転する攪拌翼を内蔵し、連続的に
液を配管で供給、排出が可能な密閉されたミキサーに、
チタン塩化物を含む有機溶剤溶液と１〜６重量％水酸化
ナトリウム水溶液を流量調節弁を介し連続的に供給す
る。供給するチタン塩化物を含む有機溶剤溶液と１〜６
重量％水酸化ナトリウム水溶液の流量は、重量比でチタ
ン塩化物を含む有機溶剤溶液 １に対して１〜６重量％
水酸化ナトリウム水溶液１〜２．５である。供給する有
機溶剤溶液、該水酸化ナトリウム水溶液、ミキサー本
体、ミキサーからの排出液は特に加温、冷却はしなくて
も問題はない。また、ミキサーの出口には、PH計を設置
し、排出液のＰＨが９．０〜１１．０の範囲となるよう
に、水酸化ナトリウムの供給量を流量調整弁で調整を行
い、有機溶媒溶液中のチタン塩化物濃度の変化に追従し
た反応が行なえるようにする。In a closed mixer, which has a stirring blade that rotates at high speed and can continuously supply and discharge the liquid through a pipe,
An organic solvent solution containing titanium chloride and a 1 to 6 wt% sodium hydroxide aqueous solution are continuously supplied through a flow control valve. Organic solvent solution containing titanium chloride to be supplied and 1 to 6
The flow rate of the weight% sodium hydroxide aqueous solution is 1 to 6% by weight with respect to the organic solvent solution 1 containing titanium chloride in a weight ratio.
Aqueous sodium hydroxide solution 1 to 2.5. The organic solvent solution to be supplied, the aqueous sodium hydroxide solution, the mixer body, and the liquid discharged from the mixer may be heated or cooled without any problem. In addition, a PH meter is installed at the outlet of the mixer, and the supply amount of sodium hydroxide is adjusted with a flow rate adjusting valve so that the pH of the discharged liquid is in the range of 9.0 to 11.0. Allow the reaction to follow the changes in titanium chloride concentration in the solution.
【０００８】本工程により、チタン塩化物は分解され、
分解生成物ＮａＣlとチタン酸化物が発生し、ＮａＣｌ
は 溶解し、チタン酸化物は 懸濁物質として、水層に含
まれる。By this step, titanium chloride is decomposed,
Decomposition products NaCl and titanium oxide are generated,
Are dissolved and titanium oxide is contained in the aqueous layer as a suspended substance.
【０００９】本発明の分離工程は、分解工程で得られた
液を蒸留に付し、有機溶媒を分離して回収する工程であ
る。本工程の具体的な方法及び条件の例としては、次の
ものをあげることができる。The separation step of the present invention is a step in which the liquid obtained in the decomposition step is subjected to distillation to separate and recover the organic solvent. The following can be mentioned as an example of a specific method and conditions of this step.
【００１０】ミキサーからの排出液と加圧された水蒸気
を、水蒸気蒸留塔の底部の液保有部に連続的に供給し、
水蒸気蒸留を行なう。水蒸気蒸留塔の底部の液温は設置
された温度計により測定され、約９６〜９８℃となるよ
うに供給する水蒸気の量を、流量調整弁で制御する。
また、水蒸気蒸留塔底部の液保有部の混合を向上する目
的で、水蒸気は分散機を介して、水蒸気蒸留塔底部に供
給する。水蒸気蒸留塔の塔頂からは、有機溶媒溶液中の
有機溶媒と水蒸気の混合蒸気が留出する。留出した混合
蒸気には、チタン塩素化合物は含まれていない。The liquid discharged from the mixer and the pressurized steam are continuously supplied to the liquid holding section at the bottom of the steam distillation column,
Perform steam distillation. The liquid temperature at the bottom of the steam distillation column is measured by a thermometer installed, and the amount of steam supplied so as to be about 96 to 98 ° C. is controlled by a flow rate adjusting valve.
Further, steam is supplied to the bottom of the steam distillation column through a disperser for the purpose of improving the mixing of the liquid holding part at the bottom of the steam distillation column. From the top of the steam distillation column, a mixed vapor of the organic solvent in the organic solvent solution and steam is distilled. The distilled mixed vapor does not contain a titanium chlorine compound.
【００１１】水蒸気蒸留塔底部の液保有部には液の保有
量を測定する目的で、レベル計を設置する。A level meter is installed in the liquid holding part at the bottom of the steam distillation column for the purpose of measuring the amount of liquid held.
【００１２】分解によって生じたＮａＣｌと チタン酸
化物は、水蒸気蒸留塔の底部より、ＮａＣｌを溶解した
チタン酸化物の懸濁液となり、缶出液として、水蒸気蒸
留塔の底部液保有量が一定となるように回収する。The NaCl and titanium oxide generated by the decomposition become a suspension of titanium oxide in which NaCl is dissolved from the bottom of the steam distillation column, and the bottom liquid of the steam distillation column is kept constant as a bottom product. To be collected.
【００１３】本発明により、有機溶媒は蒸留塔の塔頂成
分として得られ、ＮａＣｌとチタン酸化物を含む水層は
蒸留塔の缶出液として得られる。According to the present invention, the organic solvent is obtained as the top component of the distillation column, and the aqueous layer containing NaCl and titanium oxide is obtained as the bottom liquid of the distillation column.
【００１４】[0014]
【実施例】実施例１
回転数９５０ｒｐｍで内蔵した攪拌翼が回転しているサ
タケＤ型トップミキサー（ＭＳ３６−ＭＭＲ-７．５
Ｌ）に、四塩化チタンを約７重量％を含むトルエン溶液
３６０Ｋｇ／Ｈと、２５重量％水酸化ナトリウム水溶液
８７Ｋｇ／Ｈと工業用純水４８０Ｋｇ／Ｈの割合で混合
した約３．８重量％の水酸化ナトリウム水溶液とを 流
量流量調整弁を介し連続的に供給し、混合し、チタン塩
化物の分解中和処理を行い、排出させた。投入液体の温
度、ミキサー、排出液には特に加温、冷却は行なわなか
った。また、ミキサーの排出液のＰＨが９．０〜１１．
０の範囲となるように、ミキサーの出口には、PH計を設
置した。水酸化ナトリウム水溶液の供給量は、上記供給
量を初期値とし、ミキサーの排出液のＰＨが９．０〜１
１．０となるように調整した。続いて、ミキサー排出液
と約１ＭｐａＧに加圧した水蒸気を水蒸気蒸留塔に供給
し、水蒸気蒸留を行なった。水蒸気の供給量は、水蒸気
蒸留塔の底部液温が約９６〜９８℃となるように流量調
整弁で制御した。ミキサーの排出液を該水蒸気蒸留塔に
供給し、水蒸気蒸留塔 底部の液温を約９６〜９８℃と
するには、約８２０Ｋｇ／Ｈの約１ＭｐａＧの水蒸気を
必要とした。水蒸気蒸留塔の塔頂より、水蒸気とトルエ
ンの混合蒸気が留出した。留出した混合蒸気にはチタン
塩素化合物は含まれていなかった。塔頂より留出する蒸
気は、凝縮器で凝縮、液化され、水とトルエンの比重差
を利用した分離装置によって分離した。分離した水とト
ルエンの合計量は、約１０００Ｋｇ/Ｈで、その割合は
重量比で、トルエン：水＝１：１．８であった。分離さ
れたトルエンのみが、有機溶媒精製の蒸留塔へ送られ、
精製され回収された。水蒸気蒸留塔の底部のＮａＣｌ溶
解した酸化チタン懸濁水は、底部の液保有量が一定とな
る様にレベル制御しながら、缶出液として、約７５０Ｋ
ｇ/Ｈで回収された。EXAMPLES Example 1 A Satake D-type top mixer (MS36-MMR-7.5) in which a stirring blade incorporated at a rotation speed of 950 rpm is rotating.
L), a toluene solution containing about 7% by weight of titanium tetrachloride (360 kg / H), a 25% by weight sodium hydroxide aqueous solution (87 kg / H) and industrial pure water (480 kg / H) mixed at a ratio of about 3.8% by weight. The aqueous sodium hydroxide solution was continuously supplied through a flow rate control valve, mixed, decomposed and neutralized with titanium chloride, and then discharged. The temperature of the input liquid, the mixer, and the discharge liquid were not heated or cooled. The pH of the liquid discharged from the mixer is 9.0 to 11.
A PH meter was installed at the outlet of the mixer so that the range was 0. The supply amount of the sodium hydroxide aqueous solution is set to the above-mentioned supply amount as an initial value, and the pH of the liquid discharged from the mixer is 9.0 to 1
It was adjusted to be 1.0. Subsequently, the liquid discharged from the mixer and steam pressurized to about 1 MpaG were supplied to a steam distillation column to carry out steam distillation. The amount of steam supplied was controlled by a flow rate adjusting valve so that the liquid temperature at the bottom of the steam distillation column was about 96 to 98 ° C. In order to supply the liquid discharged from the mixer to the steam distillation column and bring the liquid temperature at the bottom of the steam distillation column to about 96 to 98 ° C., about 820 Kg / H of about 1 MpaG of steam was required. A mixed vapor of steam and toluene was distilled from the top of the steam distillation column. The distilled mixed vapor contained no titanium chlorine compound. The vapor distilled from the top of the column was condensed and liquefied by a condenser, and separated by a separator utilizing the difference in specific gravity between water and toluene. The total amount of separated water and toluene was about 1000 Kg / H, and the ratio by weight was toluene: water = 1: 1.8. Only the separated toluene is sent to the distillation column for organic solvent purification,
Purified and recovered. The NaCl-dissolved titanium oxide suspension water at the bottom of the steam distillation column was controlled at a level of about 750K as a bottom liquid while controlling the level so that the amount of liquid held at the bottom was constant.
Recovered at g / H.
【００１５】[0015]
【発明の効果】以上説明したとおり、本発明により、チ
タン塩化物を含有する有機溶媒溶液から有機溶媒を分離
して回収する方法であって、装置の腐食を防止し、かつ
作業上の安全性及び容易性を有するという優れた特徴を
有する有機溶媒の回収方法を提供することができた。As described above, according to the present invention, there is provided a method for separating and recovering an organic solvent from an organic solvent solution containing titanium chloride, which prevents corrosion of the device and is safe in operation. Further, it was possible to provide a method for recovering an organic solvent, which has an excellent feature that it has easiness.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 神長 康則 千葉県市原市姉崎海岸５の１ 住友化学工 業株式会社内 Ｆターム(参考） 4H006 AA02 AD14 BE10 ─────────────────────────────────────────────────── ─── Continued front page (72) Inventor Yasunori Kanaga Sumitomo Chemical Co., Ltd. 1-5 Anezaki Kaigan, Ichihara City, Chiba Prefecture Business F-term (reference) 4H006 AA02 AD14 BE10
Claims (4)
ら有機溶媒を分離して回収する方法であって、下記の工
程を有する有機溶媒の回収方法。 分解工程：チタン塩化物を含有する有機溶媒溶液に水酸
化ナトリウム水溶液を添加して混合し、チタン塩化物を
分解する工程 分離工程：分解工程で得られた液を蒸留に付し、有機溶
媒を分離して回収する工程1. A method for separating and recovering an organic solvent from an organic solvent solution containing titanium chloride, which comprises the following steps. Decomposition step: A sodium hydroxide aqueous solution is added to an organic solvent solution containing titanium chloride and mixed to decompose titanium chloride Separation step: The liquid obtained in the decomposition step is subjected to distillation to remove an organic solvent. Separation and recovery process
4-m（ｍは０〜３の整数を表し、Ｒは炭素数１〜４のア
ルキル基を表す。）である請求項１記載の方法。2. Titanium chloride is Ti (OR) mCl
The method according to claim 1, which is 4-m (m represents an integer of 0 to 3, and R represents an alkyl group having 1 to 4 carbon atoms).
請求項１記載の方法。3. The method according to claim 1, wherein the organic solvent is toluene or hexane.
が、オレフィンを重合させるための触媒を製造する過程
で発生する廃溶液である請求項１記載の方法。4. The method according to claim 1, wherein the organic solvent solution containing titanium chloride is a waste solution generated in the process of producing a catalyst for polymerizing an olefin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001326079A JP2003128594A (en) | 2001-10-24 | 2001-10-24 | Method for recovering organic solvent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001326079A JP2003128594A (en) | 2001-10-24 | 2001-10-24 | Method for recovering organic solvent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2003128594A true JP2003128594A (en) | 2003-05-08 |
Family
ID=19142526
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2001326079A Withdrawn JP2003128594A (en) | 2001-10-24 | 2001-10-24 | Method for recovering organic solvent |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2003128594A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8058328B2 (en) | 2003-11-05 | 2011-11-15 | Nippon Shokubai Co., Ltd. | Cement admixture |
-
2001
- 2001-10-24 JP JP2001326079A patent/JP2003128594A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US8058328B2 (en) | 2003-11-05 | 2011-11-15 | Nippon Shokubai Co., Ltd. | Cement admixture |
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