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JP2001089438A - Method for recovering dimethylsulfoxide - Google Patents

Method for recovering dimethylsulfoxide

Info

Publication number
JP2001089438A
JP2001089438A JP27046999A JP27046999A JP2001089438A JP 2001089438 A JP2001089438 A JP 2001089438A JP 27046999 A JP27046999 A JP 27046999A JP 27046999 A JP27046999 A JP 27046999A JP 2001089438 A JP2001089438 A JP 2001089438A
Authority
JP
Japan
Prior art keywords
mixture
dmso
mea
recovering
monoethanolamine
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
JP27046999A
Other languages
Japanese (ja)
Other versions
JP3692497B2 (en
Inventor
Yoshiyuki Fukui
芳之 福井
Haruki Yamaguchi
春樹 山口
Hiroshi Takeuchi
宏 竹内
Katsuto Hirai
克仁 平居
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.)
Toray Fine Chemicals Co Ltd
Original Assignee
Toray Fine Chemicals Co Ltd
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 Toray Fine Chemicals Co Ltd filed Critical Toray Fine Chemicals Co Ltd
Priority to JP27046999A priority Critical patent/JP3692497B2/en
Priority to TW89112301A priority patent/TW553926B/en
Publication of JP2001089438A publication Critical patent/JP2001089438A/en
Application granted granted Critical
Publication of JP3692497B2 publication Critical patent/JP3692497B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

PROBLEM TO BE SOLVED: To provide a method for efficiently recovering DMSO at a low cost from a mixture of DMSO with MEA used in electronic materials and the like usually disposed as industrial wastes. By this method DMSO having high purity, capable of being reused especially as the electronic material and containing little metals is recovered. SOLUTION: In a method for recovering dimethylsulfoxide from a mixture of dimethylsulfoxide with monoethanolamine, this method for reccovering dimethylsulfoxide is to neutralize the mixture and distill the neutralized mixture at a reduced pressure by using sulfuric acid to neutralize the mixture and fixing monoethanolamine in the mixture in a salt form, then, distilling the mixture under the reduced pressure and removing monoethanolamine remaining in the distillate in a minute amount by treating the distillate with an ion exchanger.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は、ジメチルスルホキ
シド(以下、DMSOという)とモノエタノールアミン
(以下、MEAという)の混合物から、DMSOを回収
する方法に関するものである。
[0001] The present invention relates to a method for recovering DMSO from a mixture of dimethyl sulfoxide (hereinafter, referred to as DMSO) and monoethanolamine (hereinafter, referred to as MEA).

【0002】[0002]

【従来の技術】従来、DMSOは、医農薬中間体の反応
溶剤や電子材料の特殊洗浄剤等として工業的に幅広く使
用されている。特に、DMSOとMEAの混合物は、電
子材料用の優れた特殊剥離剤のひとつである。また、D
MSOは前記剥離剤を使用して剥離を行なった後のリン
ス工程でリンス液としても使用されており、近年、これ
らの使用量が著しく増加しており、そこで発生する使用
済み液の処理問題が新しい課題としてクローズアップさ
れている。このような用途に使用されたDMSOとME
Aの混合物は、通常の減圧蒸留だけではDMSOとME
Aを完全に分離し、DMSOのみを回収することは困難
である。また、晶析操作を繰り返してDMSOとMEA
を分離する方法(特開平7−118223号公報)もあ
るが、DMSOとMEAの混合物は、現状では、通常は
産業廃棄物として廃棄されている。
2. Description of the Related Art Heretofore, DMSO has been widely used industrially as a reaction solvent for intermediates of medical and agricultural chemicals and a special detergent for electronic materials. In particular, a mixture of DMSO and MEA is one of the excellent special release agents for electronic materials. Also, D
MSO is also used as a rinsing liquid in a rinsing step after stripping using the above-mentioned stripping agent. In recent years, the amount of these used has increased remarkably. It has been highlighted as a new issue. DMSO and ME used for such applications
A mixture of DMSO and ME
It is difficult to completely separate A and recover only DMSO. In addition, the crystallization operation was repeated to obtain DMSO and MEA.
There is also a method of separating the compound (JP-A-7-118223), but at present, a mixture of DMSO and MEA is usually discarded as industrial waste.

【0003】[0003]

【発明が解決しようとする課題】本発明の目的は、現状
では、通常は産業廃棄物として廃棄されている電子材料
用などに使用しているDMSOとMEAの混合物から、
DMSOを安価で効率よく回収する方法を提供するもの
であり、具体的には、非プロトン性極性有機溶媒で低毒
性であり、また、水と任意に混合する他、MEAなどの
有機溶媒とも任意の割合で混合する性質を有し、医農薬
中間体の反応溶剤や合成試薬、電子材料等の特殊洗浄
剤、剥離液として工業的に幅広く使用されているDMS
Oを含む混合物から安価で効率よくDMSOを回収する
方法、特に電子材料用として再使用が可能なほど高純度
かつ金属分の低いDMSOを回収する方法を提供するこ
とにある。
SUMMARY OF THE INVENTION The object of the present invention is to obtain a mixture of DMSO and MEA which is currently used for electronic materials which are usually discarded as industrial waste.
The present invention provides a method for recovering DMSO at low cost and efficiently. Specifically, it is an aprotic polar organic solvent and has low toxicity, and is optionally mixed with water and optionally with an organic solvent such as MEA. DMS, which is widely used industrially as a special solvent for chemicals and agrochemical intermediates as a reaction solvent and synthetic reagents, special cleaning agents for electronic materials, etc.
It is an object of the present invention to provide a method for recovering DMSO efficiently and inexpensively from a mixture containing O, particularly a method for recovering DMSO having a high purity and a low metal content so that it can be reused for electronic materials.

【0004】[0004]

【課題を解決するための手段】本発明は上記目的を達成
せんとするものであって、DMSOとMEAを含む混合
物からDMSOを分離回収する方法において、該混合物
を中和して減圧蒸留することを特徴とするDMSOの回
収方法であり、より具体的には、DMSOとMEAを含
み、DMSOの含有率がMEAの含有率よりも高い混合
物からDMSOを分離、回収する方法において、該混合
物を硫酸を用いて中和し、MEAを硫酸塩の形で該混合
物中に固定化しておき、減圧蒸留することによりDMS
Oを主成分とする液体を留出させ、次にイオン交換塔に
通液し、該液体中に微量残存しているMEAを除去し、
精留を行ない、DMSOを回収することを特徴とするD
MSOとMEA混合物からのDMSOの回収方法であ
る。
DISCLOSURE OF THE INVENTION The present invention has been made to achieve the above object, and in a method for separating and recovering DMSO from a mixture containing DMSO and MEA, the mixture is neutralized and distilled under reduced pressure. More specifically, in a method for separating and recovering DMSO from a mixture containing DMSO and MEA, wherein the content of DMSO is higher than the content of MEA, the method comprises the steps of: The MEA was fixed in the mixture in the form of sulfate in the form of a sulfate, and distilled under reduced pressure to obtain DMS.
Distill a liquid containing O as a main component, then pass the liquid through an ion exchange column to remove a small amount of MEA remaining in the liquid,
D is characterized by performing rectification and recovering DMSO
This is a method for recovering DMSO from a mixture of MSO and MEA.

【0005】そして、本発明のDMSOの回収方法によ
れば、DMSOは、電子材料処理用としてリサイクル使
用が可能なほど高純度でかつ金属分の低いものとして回
収される。すなわち、DMSOのみを高純度かつ金属分
を低くして蒸留回収することができる。
According to the method for recovering DMSO of the present invention, DMSO is recovered as a substance having a purity and a low metal content that can be recycled for electronic material processing. That is, only DMSO can be recovered by distillation with high purity and low metal content.

【0006】[0006]

【発明の実施の形態】本発明は、DMSOとMEAの混
合物からDMSOを回収する方法に関するもので、本発
明においては、該混合物からのDMSOの回収率、コス
ト等のため、以下に述べるようないくつかの好ましい条
件がある。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for recovering DMSO from a mixture of DMSO and MEA. In the present invention, the following methods are used for the recovery rate of DMSO from the mixture, the cost, and the like. There are several favorable conditions.

【0007】本発明におけるDMSOとMEA混合物の
組成は、DMSO含量がMEAのそれと同じかそれより
低くても良いが、DMSO含量がMEAのそれよりも高
い場合に好適に用いられる。具体的には、MEA含有量
が例えば30重量%以下のもので、より好ましくは10
重量%以下のものである。また、このような混合物に
は、含水しているもの、非含水のものの両方があり、こ
れらにはDMSOとMEA以外に若干量の有機物が含ま
れているものもある。
The composition of the mixture of DMSO and MEA in the present invention may be used when the DMSO content is the same or lower than that of MEA, but is higher when the DMSO content is higher than that of MEA. Specifically, the MEA content is, for example, 30% by weight or less, more preferably 10% by weight.
% By weight or less. In addition, such mixtures include both those containing water and those not containing water, and some of them contain a small amount of organic substances in addition to DMSO and MEA.

【0008】本発明におけるDMSOとMEAの混合物
の代表的な例として、電子材料等を処理した後の使用済
み剥離液が挙げられるが、本発明の混合物はこれに限定
されず、他用途に使用した混合物でもよい。また、本発
明は使用済み液と定義されないような混合物、つまりD
MSOとMEAのみの混合物にも適用できる。
[0008] A typical example of the mixture of DMSO and MEA in the present invention is a used stripper after treating an electronic material or the like. However, the mixture of the present invention is not limited to this, and may be used for other purposes. Mixtures may be used. The present invention also relates to mixtures which are not defined as spent liquids,
It can be applied to a mixture of only MSO and MEA.

【0009】この場合液組成は特に限定されないが、好
適には使用済み液中のMEA濃度と同じでMEAが30
重量%以下、さらに好ましくは10重量%以下で適用さ
れる。
In this case, the composition of the liquid is not particularly limited, but preferably the same as the MEA concentration in the used liquid and the MEA is 30%.
It is applied at not more than 10% by weight, more preferably at most 10% by weight.

【0010】本発明のDMSOの回収方法では、上記の
ような混合液中のMEAを中和し蒸留する。中和には、
硫酸、塩酸、リン酸等の無機酸(鉱酸)が用いられる
が、無機酸の不揮発性、中和蒸留後の缶残の産廃処理が
容易であること等の理由で、硫酸が好ましく用いられ
る。このときに添加し用いられる硫酸の量は、混合液中
に存在するMEAの0.8〜2.0倍当量が好ましく、
より好ましくは1.0〜1.5倍当量が適当である。こ
の場合、硫酸量が0.8倍当量未満では、MEAが十分
中和されず留出する。また、2.0倍当量より多い場合
は、硫酸が過剰となるため、コストアップにつながる。
In the method for recovering DMSO of the present invention, MEA in the above-mentioned mixed solution is neutralized and distilled. To neutralize,
Inorganic acids (mineral acids) such as sulfuric acid, hydrochloric acid, and phosphoric acid are used. However, sulfuric acid is preferably used because of the non-volatility of the inorganic acid and the ease of industrial waste treatment of the residue after neutralization distillation. . The amount of sulfuric acid added and used at this time is preferably 0.8 to 2.0 equivalents of MEA present in the mixed solution,
More preferably, a 1.0 to 1.5 equivalent is appropriate. In this case, if the amount of sulfuric acid is less than 0.8 equivalent, the MEA is not sufficiently neutralized and is distilled off. On the other hand, if it is more than 2.0 equivalents, the sulfuric acid becomes excessive, which leads to an increase in cost.

【0011】ここでいう中和とは、以下の反応式
(1)、(2)で表されるような反応である。
The neutralization referred to herein is a reaction represented by the following reaction formulas (1) and (2).

【0012】 HOCH2CH2NH2 + H2SO4 → HOCH2CH2NH3 +・HSO4 ~ ・・・(1) 2HOCH2CH2NH2 + H2SO4 → (HOCH2CH2NH3 +)2・SO4 2~・・・(2) 中和蒸留に際しては、缶温は通常は130℃以下、より
好適には110℃以下が好ましい。このときの缶内の圧
力としては、それぞれ14.2kPa以下、6.7kP
a以下が好ましい。温度または圧力が高くなりすぎると
DMSOの分解が著しく促進されるので、好ましくな
い。
HOCH 2 CH 2 NH 2 + H 2 SO 4 → HOCH 2 CH 2 NH 3 + · HSO 4 ~・ ・ ・ (1) 2HOCH 2 CH 2 NH 2 + H 2 SO 4 → (HOCH 2 CH 2 NH 3 + ) 2 · SO 4 2 ~ ... (2) In the neutralization distillation, the can temperature is usually 130 ° C or lower, more preferably 110 ° C or lower. At this time, the pressure in the can was 14.2 kPa or less and 6.7 kP, respectively.
a or less is preferable. If the temperature or pressure is too high, the decomposition of DMSO is remarkably promoted, which is not preferable.

【0013】本発明において、このようにして中和蒸留
して得られたDMSOを主成分とする液体は、次にイオ
ン交換処理、活性炭吸着処理、酸性白土処理、モレキュ
ラーシーブ吸着処理等に供されるが、MEAの除去が確
実であること、処理速度が比較的速いこと等の理由でイ
オン交換処理が最も好ましい。イオン交換処理は、好適
にはDMSOを主成分とする液体をイオン交換塔に通液
することにより行なわれるが、このとき、塔に充填する
イオン交換樹脂としては、MEAがカチオンになること
からカチオン交換樹脂を単独で使用するのが適当であ
る。カチオン交換樹脂とアニオン交換樹脂とを混合した
ものを使用しても処理能力は有るが、この場合、アニオ
ン交換樹脂はMEAの除去には寄与しておらず無意味で
ある。このことからもカチオン交換樹脂単独で使用する
のが適当である。
In the present invention, the liquid containing DMSO as a main component obtained by the neutralization distillation in this manner is then subjected to an ion exchange treatment, an activated carbon adsorption treatment, an acid clay treatment, a molecular sieve adsorption treatment and the like. However, the ion exchange treatment is most preferable because the removal of MEA is reliable and the treatment speed is relatively high. The ion exchange treatment is preferably performed by passing a liquid containing DMSO as a main component through an ion exchange column. At this time, the ion exchange resin to be filled in the column is a cation exchange agent because MEA is a cation. Suitably, the exchange resin is used alone. The use of a mixture of a cation exchange resin and an anion exchange resin has a processing ability, but in this case, the anion exchange resin does not contribute to the removal of MEA and is meaningless. From this, it is appropriate to use the cation exchange resin alone.

【0014】また、イオン交換は流動床式でも固定床式
でも良いが、固定床式が好ましい。処理温度は常温が好
ましい。
The ion exchange may be a fluidized bed type or a fixed bed type, but a fixed bed type is preferred. The processing temperature is preferably room temperature.

【0015】通液量はウエット樹脂の100〜150倍
量が目安であるが、この通液量は樹脂の交換容量と被処
理液中のMEA濃度に大きく依存する。処理前に被処理
液中のMEA濃度の分析をすることが重要である。
The amount of liquid passing is roughly 100 to 150 times that of the wet resin, but the amount of liquid passing largely depends on the exchange capacity of the resin and the MEA concentration in the liquid to be treated. It is important to analyze the MEA concentration in the liquid to be treated before the treatment.

【0016】さらに本発明では、イオン交換処理後の液
体を精留するが、このときの操作条件としては以下の様
なものがある。具体的には、例えば特開平9−2787
43号公報に記載のように、精留における缶温は通常1
30℃以下、より好適には110℃以下である。缶内の
圧力としては、それぞれ14.2kPa以下、6.7k
Pa以下が好ましい。温度または圧力が高くなりすぎる
とDMSOの分解が著しく促進されるので、好ましくな
い。
Further, in the present invention, the liquid after the ion exchange treatment is rectified. The operating conditions at this time are as follows. Specifically, for example, Japanese Patent Application Laid-Open No. 9-2787
As described in JP-A No. 43, the can temperature in rectification is usually 1 unit.
The temperature is 30 ° C or lower, more preferably 110 ° C or lower. The pressure in the can was 14.2 kPa or less and 6.7 k, respectively.
Pa or less is preferable. If the temperature or pressure is too high, the decomposition of DMSO is remarkably promoted, which is not preferable.

【0017】また、蒸留精製し、回収したDMSOを電
子材料処理用に使用可能なレベルにまでするためには、
接液部、特に気化部以降の設備の材質に耐食性材料を使
用することが好ましい。この様に耐食性材料を使用する
と、回収したDMSO中に含まれる鉄等の金属分を10
ppb以下にまで低く押さえることが出来る。
Further, in order to reduce the DMSO recovered by distillation and purification to a level usable for electronic material processing,
It is preferable to use a corrosion resistant material for the material of the equipment after the liquid contact part, especially the vaporization part. When the corrosion resistant material is used in this way, the metal content such as iron contained in the recovered DMSO can be reduced by 10%.
It can be held down to ppb or less.

【0018】さらに、蒸留時のDMSOの熱分解防止等
のため、蒸留に使用するDMSOを主成分とする粗液の
pHをアルカリ性に保つことが重要である。好ましいp
Hは8以上で、より好ましくはpH9〜12の範囲内で
好適なpHが選択される。
Further, in order to prevent the thermal decomposition of DMSO during the distillation, it is important to keep the pH of the crude liquid containing DMSO as a main component used in the distillation to be alkaline. Preferred p
H is 8 or more, and more preferably a suitable pH is selected within the range of pH 9 to 12.

【0019】粗液のpHをアルカリ性に調整する際に使
用する物質としてはアルカリ金属やアルカリ土類金属の
水酸化物または炭酸塩等が挙げられるが、特に水酸化ナ
トリウムが好ましく使用される。
Substances used for adjusting the pH of the crude liquid to alkaline include hydroxides or carbonates of alkali metals and alkaline earth metals, and sodium hydroxide is particularly preferably used.

【0020】本発明で回収されたDMSOは、電子材料
処理の他、医農薬中間体の反応溶剤や合成試薬に好適に
使用される。
The DMSO recovered in the present invention is suitably used as a reaction solvent or a synthetic reagent for a pharmaceutical or agricultural chemical intermediate in addition to electronic material processing.

【0021】[0021]

【実施例】以下、図面を参照して本発明の実施例につい
て詳細に説明するが、本発明はこれらの実施例に限定さ
れない。
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings, but the present invention is not limited to these embodiments.

【0022】図1は、図1は、本発明のDMSOの回収
において使用する回収装置の概要を説明するためのモデ
ル図である。
FIG. 1 is a model diagram for explaining the outline of the recovery apparatus used in the recovery of DMSO of the present invention.

【0023】図1において、配管5からDMSOを92
%、MEAを4.5%、水を3.5%含む混合液400
0gを配管7を経て蒸発缶1に供給し、別に配管6から
98%硫酸176gを配管7を経て蒸発缶1に供給して
蒸発缶1内で中和し、缶内圧を4.0kPaに保ち、缶
温が120℃に達するまで蒸留した。次いで、蒸留液を
配管8でコンデンサ2に導きコンデンサ2で凝縮して得
られた留分は3200gで、その内、DMSOは95.
6%であった。この留分を配管9からイオン交換塔3に
供給し、留分中にppmレベル残存しているMEAを除
去した後、配管10を通して蒸留塔4に供給し、缶内圧
4.0kPaで脱水精留を行なった。その結果、284
0gのDMSOが得られた。この回収されたDMSOの
品質は、pH7.0、Na含有量2ppb、Fe含有量
1ppbと金属不純物が少なく、合成したDMSOなみ
の品質で、電子材料処理用として再利用可能であった。
またこのときのDMSOの回収率は77%であった。
Referring to FIG. 1, 92
%, MEA 4.5%, water 3.5%
0 g is supplied to the evaporator 1 via the pipe 7, and 176 g of 98% sulfuric acid is separately supplied from the pipe 6 to the evaporator 1 via the pipe 7 and neutralized in the evaporator 1, and the internal pressure of the can is maintained at 4.0 kPa. , Until the can temperature reached 120 ° C. Next, the distillate was led to the condenser 2 through the pipe 8 and condensed by the condenser 2 to obtain 3200 g of a fraction, of which DMSO contained 95.
6%. This fraction is supplied from the pipe 9 to the ion exchange tower 3 to remove the MEA remaining at the ppm level in the fraction, and then supplied to the distillation tower 4 through the pipe 10, and subjected to dewatering and rectification at a vessel internal pressure of 4.0 kPa. Was performed. As a result, 284
0 g of DMSO was obtained. The quality of the recovered DMSO was pH 7.0, the content of Na was 2 ppb, and the content of Fe was 1 ppb, the content of metal impurities was small, and the quality was the same as that of the synthesized DMSO.
At this time, the recovery of DMSO was 77%.

【0024】[0024]

【発明の効果】DMSOとMEAの混合物は、通常は電
子材料処理使用後は廃棄されている。これに対し本発明
によれば、従来廃棄物として処理されていたDMSO/
MEA混合物から、簡便に効率よくDMSOを分離、回
収して有効に再利用することができる。例えば、本発明
により回収したDMSOは、そのまま電子材料用の剥離
液や洗浄剤として再利用することが可能であり、さらに
各種反応溶媒、染料用溶剤、防カビ剤等にも再利用可能
であることから、省資源化、コスト低減化に寄与できる
ものである。
The mixture of DMSO and MEA is usually discarded after use of electronic material processing. On the other hand, according to the present invention, DMSO /
DMSO can be simply and efficiently separated and recovered from the MEA mixture and efficiently reused. For example, DMSO recovered according to the present invention can be reused as it is as a stripping solution or cleaning agent for electronic materials, and can also be reused as various reaction solvents, dye solvents, fungicides, and the like. Therefore, it can contribute to resource saving and cost reduction.

【0025】本発明によれば、装置も簡単な構造のもの
で済み、処理コストも安価であることから、経済的にも
有利である。
According to the present invention, the apparatus has a simple structure and the processing cost is low, which is economically advantageous.

【図面の簡単な説明】[Brief description of the drawings]

【図1】 図1は、本発明のDMSOの回収において使
用する回収装置の概要を説明するためのモデル図であ
る。
FIG. 1 is a model diagram for explaining an outline of a recovery apparatus used in recovering DMSO of the present invention.

【符号の説明】[Explanation of symbols]

1・・・蒸発缶 2・・・コンデンサ 3・・・イオン交換塔 4・・・蒸留塔 5〜11・・・配管 DESCRIPTION OF SYMBOLS 1 ... Evaporator 2 ... Condenser 3 ... Ion exchange tower 4 ... Distillation tower 5-11 ... Piping

───────────────────────────────────────────────────── フロントページの続き (72)発明者 竹内 宏 滋賀県守山市勝部6丁目1番1号 東レ・ ファインケミカル株式会社内 (72)発明者 平居 克仁 滋賀県守山市勝部6丁目1番1号 東レ・ ファインケミカル株式会社内 Fターム(参考) 4H006 AA02 AD11 AD30 AD32 BB22 DA60 TA01  ────────────────────────────────────────────────── ─── Continuing on the front page (72) Hiroshi Takeuchi, Inventor, 6-1-1-1 Katsurbe, Moriyama-shi, Shiga Prefecture Toray Fine Chemical Co., Ltd. (72) Katsuhito Hirai 6-1-1, Katsurbe, Moriyama-shi, Shiga Toray・ F-term in Fine Chemical Co., Ltd. (reference) 4H006 AA02 AD11 AD30 AD32 BB22 DA60 TA01

Claims (4)

【特許請求の範囲】[Claims] 【請求項1】 ジメチルスルホキシドとモノエタノール
アミンを含む混合物からジメチルスルホキシドを分離回
収する方法において、該混合物を中和して減圧蒸留する
ことを特徴とするジメチルスルホキシドの回収方法。
1. A method for separating and recovering dimethyl sulfoxide from a mixture containing dimethyl sulfoxide and monoethanolamine, wherein the mixture is neutralized and distilled under reduced pressure.
【請求項2】 前記混合物を中和する際に硫酸を使用
し、該混合物中のモノエタノールアミンを塩の形で固定
化して減圧蒸留することを特徴とする請求項1記載のジ
メチルスルホキシドの回収方法。
2. The recovery of dimethyl sulfoxide according to claim 1, wherein sulfuric acid is used to neutralize the mixture, monoethanolamine in the mixture is immobilized in the form of a salt, and the mixture is distilled under reduced pressure. Method.
【請求項3】 減圧蒸留した後のジメチルスルホキシド
を主成分とする液体中に微量残存しているモノエタノー
ルアミンを、イオン交換して除去することを特徴とする
請求項1または2記載のジメチルスルホキシドの回収
法。
3. The dimethyl sulfoxide according to claim 1, wherein a trace amount of monoethanolamine remaining in the liquid containing dimethyl sulfoxide as a main component after vacuum distillation is removed by ion exchange. Collection method.
【請求項4】 回収されるジメチルスルホキシドが、電
子材料処理用としてリサイクル使用が可能なほど高純度
でかつ金属分の低いものであることを特徴とする請求項
1〜3いずれかに記載のジメチルスルホキシドの回収
法。
4. The dimethyl sulfoxide according to claim 1, wherein the recovered dimethyl sulfoxide has a high purity and a low metal content so that it can be recycled for treating electronic materials. Method for recovering sulfoxide.
JP27046999A 1999-09-24 1999-09-24 Method for recovering dimethyl sulfoxide Expired - Lifetime JP3692497B2 (en)

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JP27046999A JP3692497B2 (en) 1999-09-24 1999-09-24 Method for recovering dimethyl sulfoxide
TW89112301A TW553926B (en) 1999-09-24 2000-06-22 Method for recycling dimethylsulfoxide

Applications Claiming Priority (1)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1312124C (en) * 2002-05-13 2007-04-25 东丽精密化学株式会社 Process for purifying high purity dimethyl sulfoxide, and dimethyl sulfoxide and amine mixture
US9492213B2 (en) 2000-02-01 2016-11-15 Biomet C.V. Volar fixation system
CN108686397A (en) * 2017-04-12 2018-10-23 东丽精细化工株式会社 Distill the method and multisection type destilling tower of dimethyl sulfoxide
CN110713446A (en) * 2019-12-04 2020-01-21 河北美邦膜科技有限公司 Method for separating dimethyl sulfoxide from amlodipine resolution waste liquid
CN114989047A (en) * 2022-07-21 2022-09-02 无锡中天固废处置有限公司 Method for recovering dimethyl sulfoxide from waste organic solvent

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9492213B2 (en) 2000-02-01 2016-11-15 Biomet C.V. Volar fixation system
US9572609B2 (en) 2000-02-01 2017-02-21 Biomet C.V. Method of using a volar bone plate on a fracture
CN1312124C (en) * 2002-05-13 2007-04-25 东丽精密化学株式会社 Process for purifying high purity dimethyl sulfoxide, and dimethyl sulfoxide and amine mixture
CN108686397A (en) * 2017-04-12 2018-10-23 东丽精细化工株式会社 Distill the method and multisection type destilling tower of dimethyl sulfoxide
CN110713446A (en) * 2019-12-04 2020-01-21 河北美邦膜科技有限公司 Method for separating dimethyl sulfoxide from amlodipine resolution waste liquid
CN114989047A (en) * 2022-07-21 2022-09-02 无锡中天固废处置有限公司 Method for recovering dimethyl sulfoxide from waste organic solvent

Also Published As

Publication number Publication date
TW553926B (en) 2003-09-21
JP3692497B2 (en) 2005-09-07

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