JPH01274801A - Method for purifying organic solvent - Google Patents
Method for purifying organic solventInfo
- Publication number
- JPH01274801A JPH01274801A JP10589188A JP10589188A JPH01274801A JP H01274801 A JPH01274801 A JP H01274801A JP 10589188 A JP10589188 A JP 10589188A JP 10589188 A JP10589188 A JP 10589188A JP H01274801 A JPH01274801 A JP H01274801A
- Authority
- JP
- Japan
- Prior art keywords
- solvent
- organic solvent
- filter
- org
- tank
- 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.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000003960 organic solvent Substances 0.000 title claims description 70
- 239000012535 impurity Substances 0.000 claims abstract description 18
- 239000010419 fine particle Substances 0.000 claims abstract description 17
- 238000001704 evaporation Methods 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 abstract description 10
- 238000001223 reverse osmosis Methods 0.000 abstract description 7
- 239000002245 particle Substances 0.000 abstract description 5
- 230000001172 regenerating effect Effects 0.000 abstract description 5
- 238000009849 vacuum degassing Methods 0.000 abstract description 5
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 239000011347 resin Substances 0.000 abstract description 2
- 229920005989 resin Polymers 0.000 abstract description 2
- 239000003595 mist Substances 0.000 abstract 2
- 244000005700 microbiome Species 0.000 abstract 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 11
- 238000004519 manufacturing process Methods 0.000 description 10
- 239000000126 substance Substances 0.000 description 10
- 239000002994 raw material Substances 0.000 description 8
- 238000000746 purification Methods 0.000 description 6
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 5
- -1 KCI Chemical class 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000003456 ion exchange resin Substances 0.000 description 5
- 229920003303 ion-exchange polymer Polymers 0.000 description 5
- 239000012528 membrane Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 description 3
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 2
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 2
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- IVSZLXZYQVIEFR-UHFFFAOYSA-N m-xylene Chemical group CC1=CC=CC(C)=C1 IVSZLXZYQVIEFR-UHFFFAOYSA-N 0.000 description 2
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 description 2
- 238000011045 prefiltration Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 description 1
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- SBZXBUIDTXKZTM-UHFFFAOYSA-N diglyme Chemical compound COCCOCCOC SBZXBUIDTXKZTM-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 235000011187 glycerol Nutrition 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002828 nitro derivatives Chemical class 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- LYGJENNIWJXYER-UHFFFAOYSA-N nitromethane Chemical compound C[N+]([O-])=O LYGJENNIWJXYER-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- IWZKICVEHNUQTL-UHFFFAOYSA-M potassium hydrogen phthalate Chemical compound [K+].OC(=O)C1=CC=CC=C1C([O-])=O IWZKICVEHNUQTL-UHFFFAOYSA-M 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000011121 sodium hydroxide Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
Landscapes
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
この発明は、純度の極めて高い有機溶剤を得る方法に関
する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] This invention relates to a method for obtaining an organic solvent with extremely high purity.
有機溶剤は、物品の溶解、洗浄等に多く用いられる。そ
の際、用いる有機溶剤が不純なものであれば、溶解、洗
浄等の目的を達しがたいことがあるので、精製したもの
が用いられるのが一般であるが、最近、純度の極めて高
いものが次第に求められるようになってきた。なかには
、理論的に完全純粋に近い有機溶剤が要求されることも
ある。Organic solvents are often used for dissolving and cleaning articles. At that time, if the organic solvent used is impure, it may be difficult to achieve the objectives of dissolution, cleaning, etc., so purified organic solvents are generally used, but recently extremely pure organic solvents are being used. It has become increasingly sought after. In some cases, an organic solvent that is theoretically close to completely pure is required.
しかしながら、現状においては、空気の清浄化技術や超
純水の製造技術は進んで来ているが、有機溶剤の高度の
純粋化に関しては、殆ど改良が進んでいない。However, at present, although air purification technology and ultrapure water production technology have advanced, there has been little progress in the high degree of purification of organic solvents.
大抵の場合、有機溶剤中には、微粒子以外に不揮発性不
純物も含まれるが、これの含有量も満足した値以下には
達していないのが現状である。In most cases, organic solvents contain non-volatile impurities in addition to fine particles, but at present the content of these has not reached a satisfactory level.
このような事情から、極めて純度の高い有機溶剤を得る
ための精製法が要望されていた。Under these circumstances, there has been a demand for a purification method for obtaining extremely pure organic solvents.
以上の事情に濫みて、この発明は、極めて純度の高い有
機溶剤を得させるを機溶剤の精製法を提供することを課
題としている。In view of the above circumstances, it is an object of the present invention to provide a method for purifying organic solvents by which organic solvents with extremely high purity can be obtained.
前記課題を解決するため、発明者は、種々検討を重ねた
。従来、有機溶剤中の微粒子や不揮発性不純物を十分に
除去できなかったのは、有機溶剤が粘性を有するからで
ある。そこで、発明者は、原料有機溶剤を蒸発させて、
その蒸気をフィルタに通すようにすれば、微粒子や不揮
発性不純物の含有数が極めて少ない純粋有機溶剤が得ら
れるということを見出し、この発明を完成した。In order to solve the above problem, the inventor has conducted various studies. Conventionally, fine particles and nonvolatile impurities in organic solvents have not been sufficiently removed because organic solvents have viscosity. Therefore, the inventor evaporated the raw material organic solvent,
They discovered that by passing the vapor through a filter, they could obtain a pure organic solvent containing extremely few particulates and non-volatile impurities, and completed this invention.
すなわち、この発明は、原料有機溶剤を蒸発させて、そ
の蒸気をフィルタに通すことにより、原料有機溶剤中に
含まれていた微粒子および原料有機溶剤中に溶存してい
た不揮発性不純物を前記フィルタで除去して、純度の極
めて高い有機溶剤を得るようにするのである。That is, the present invention evaporates the raw organic solvent and passes the vapor through a filter, thereby removing fine particles contained in the raw organic solvent and non-volatile impurities dissolved in the raw organic solvent using the filter. The organic solvent is removed to obtain an extremely pure organic solvent.
有機溶剤を蒸発させて過熱蒸気または飽和蒸気などとす
ると、液体状態に比し粘度が極めて低下する。そのため
、この蒸気をフィルタに通すようにすれば、微粒子や不
揮発性不純物が確実にフィルタに捕捉され、純度の極め
て高い有機溶剤が得られる。When an organic solvent is evaporated into superheated steam or saturated steam, the viscosity is significantly lower than that in a liquid state. Therefore, by passing this vapor through a filter, fine particles and non-volatile impurities are reliably captured by the filter, and an extremely highly pure organic solvent can be obtained.
〔実 施 例〕
以下に、この発明を、その一実施例をあられす図面を参
照しながら詳しく説明する。[Embodiment] Hereinafter, one embodiment of the present invention will be described in detail with reference to the accompanying drawings.
第１図は、この発明にかかる有機溶剤の精製法の一実施
例を簡略化してあられしている。FIG. 1 shows a simplified embodiment of the organic solvent purification method according to the present invention.
図にみるように、この実施例にかかる有機溶剤の精製法
は、粗製有機溶剤から原料有機溶剤をつくる第１次製造
プロセスｌと、その原料有機溶剤から純粋有機溶剤をつ
（る第２次製造プロセス２とで構成されている。しかし
、この第１次製造プロセス１は、必ずしも必要ない。As shown in the figure, the organic solvent purification method according to this example consists of a first production process l of producing a raw organic solvent from a crude organic solvent, and a second production process l of producing a pure organic solvent from the raw organic solvent. This first manufacturing process 1 is not necessarily required.
第１次製造プロセス１では、つぎのようにして原料有機
溶剤がつくられる。タンク１１に蓄えられた粗製有機溶
剤は、熱交換器１２に送られ、ここで逆浸透装置１３の
運転に適した温度に温められる。さらに、５μｍ程度の
プレフィルタで濾過され、ｐＨを弱酸性に調節された後
、逆浸透装置１３に送られて処理される。粗製有機溶剤
に対しては、必要に応じ、タンク１１に蓄えられる前に
、前処理装置１４によって凝縮沈澱、濾過、活性炭吸着
などの処理を行っておく。この前処理は、粗製有機溶剤
の質、すなわち、懸濁性物質、他の有機物や無機物の含
有程度に応じて適宜必要な処理を選択して行うようにす
る。逆浸透装置１３では、イオン分が９０％以上除去さ
れるようになっている。それとともに、他の有機物や無
機物、コロイド状物質も分離除去されるようになってい
るので、後に行われるイオン交換樹脂処理を有利にする
ことができる。ただし、この逆浸透装置１３では、酸素
等の溶存ガスを分離することができないので、逆浸透装
置で処理された粗製有機溶剤は、真空脱気塔１５に送ら
れ、溶存ガスの除去が十分になされる。真空脱気塔１５
で処理された粗製有機溶剤は、いったんタンク１６に貯
蔵され、続いて再生式イオン交換樹脂塔１７で脱イオン
され、０．２μｍ程度のメンブレンフィルタ１８で濾過
された後、原料有機溶剤となってタンク１９に蓄えられ
る。なお、２０は塩酸タンクであり、２１は苛性ソーダ
タンクである。In the first manufacturing process 1, a raw organic solvent is produced as follows. The crude organic solvent stored in the tank 11 is sent to the heat exchanger 12, where it is heated to a temperature suitable for operating the reverse osmosis device 13. Furthermore, after being filtered through a pre-filter of about 5 μm and having its pH adjusted to be slightly acidic, it is sent to a reverse osmosis device 13 for processing. The crude organic solvent is subjected to treatments such as condensation and precipitation, filtration, and activated carbon adsorption in the pretreatment device 14, if necessary, before being stored in the tank 11. This pretreatment is carried out by selecting an appropriate treatment depending on the quality of the crude organic solvent, that is, the degree of content of suspended substances, other organic substances, and inorganic substances. The reverse osmosis device 13 is designed to remove 90% or more of ions. At the same time, other organic substances, inorganic substances, and colloidal substances are also separated and removed, making the subsequent ion exchange resin treatment advantageous. However, since this reverse osmosis device 13 cannot separate dissolved gases such as oxygen, the crude organic solvent treated with the reverse osmosis device is sent to the vacuum degassing tower 15 to ensure that dissolved gases are not sufficiently removed. It will be done. Vacuum degassing tower 15
The treated crude organic solvent is temporarily stored in a tank 16, then deionized in a regenerative ion exchange resin column 17, and filtered with a membrane filter 18 of about 0.2 μm, and then becomes a raw material organic solvent. It is stored in tank 19. Note that 20 is a hydrochloric acid tank, and 21 is a caustic soda tank.
このようにして得られた原料有機溶剤は、電気比抵抗が
非常に高く、微粒子や不揮発性不純物がおおむね除去さ
れている。また、溶存ガスもほとんど除去されているが
、空気と接触すると、ふたたび溶存ガスが増加するので
、真空脱気した後のタンク中の空気は窒素と置換される
ようになっている。The raw organic solvent obtained in this manner has a very high electrical resistivity, and is largely free of fine particles and non-volatile impurities. Also, most of the dissolved gas has been removed, but when it comes into contact with air, the amount of dissolved gas increases again, so the air in the tank after vacuum degassing is replaced with nitrogen.
第１次製造プロセス１の終了後、第２次製造プロセス２
が行われる。これが、この発明の製造プロセスである。After the completion of the first manufacturing process 1, the second manufacturing process 2
will be held. This is the manufacturing process of this invention.
そこで、つぎに、この第２次製造プロセス２について詳
しく説明する。Therefore, next, this second manufacturing process 2 will be explained in detail.
タンク１９に蓄えられた原料有機溶剤は、蒸発装置２２
に送られる。蒸発装置２２は、加熱手段であるヒータ２
３を備えている。このヒータ２３で装置内を加熱すると
原料有機溶剤２４の蒸発が起き、原料有機溶剤２４の液
滴２５が飛び出してくる。その液滴２５のキャリーオー
バーが装置２２の出口部へ移動する。液滴２５には、原
料有機溶剤２４中に含まれていた固体の粒子（微粒子）
と、原料有機溶剤２４中に溶存していた不揮発性不純物
が含まれている。液滴２５のキャリーオーバーから液体
を機溶剤が蒸発すると、溶存していた不揮発性不純物が
析出して粒子となるとともに、前記微粒子が残る。装置
２２の出口部にはフィルタ２６が配備されている。その
ため、前記析出粒子および微粒子がこのフィルタ２６で
捕捉されて除去されるのである。他方、蒸発により蒸気
となった有機溶剤は、フィルタ２６を通過する。フィル
タ２６を通った有機溶剤の蒸気を液化すれば、純度の極
めて高い有機溶剤が得られる。得られた純粋有機溶剤は
、タンク２７に蓄えられる。タンク２７に蓄えられた純
粋有機溶剤は、純度の劣化を防ぐため、タンク１９に還
流される。この循環は、連Ｍ して行うようにすること
が、純度の劣化を防止するうえて重要なことである。前
記フィルタ２６としては、たとえば、超精密フィルタが
用いられる。The raw organic solvent stored in the tank 19 is transferred to the evaporator 22.
sent to. The evaporator 22 includes a heater 2 which is a heating means.
It has 3. When the inside of the apparatus is heated by this heater 23, the raw organic solvent 24 evaporates, and droplets 25 of the raw organic solvent 24 fly out. The carryover of the droplet 25 moves to the outlet of the device 22. The droplets 25 contain solid particles (fine particles) contained in the raw organic solvent 24.
and nonvolatile impurities dissolved in the raw material organic solvent 24. When the organic solvent evaporates the liquid from the carryover of the droplets 25, the dissolved nonvolatile impurities precipitate and become particles, and the fine particles remain. A filter 26 is provided at the outlet of the device 22. Therefore, the precipitated particles and fine particles are captured and removed by this filter 26. On the other hand, the organic solvent that has become vapor due to evaporation passes through the filter 26. By liquefying the organic solvent vapor that has passed through the filter 26, an organic solvent with extremely high purity can be obtained. The pure organic solvent obtained is stored in tank 27. The pure organic solvent stored in tank 27 is refluxed to tank 19 to prevent deterioration of purity. It is important to perform this circulation continuously in order to prevent deterioration of purity. As the filter 26, for example, an ultra-precision filter is used.
以上にみてきたように、この有ａ溶剤の精製法は、原料
有機溶剤２４を蒸発させて、その蒸気をフィルタ２６に
通すことにより、原料有機溶剤中に分散した状態で含ま
れていた微粒子や、溶解し７た状態で含まれていた不揮
発性不純物を除去するようにしている。この際、−に記
実施例のように、フィルタとして超精密フィルタを用い
るようにすれば、超精密フィルタは微粒子および不運発
性不純物の捕捉効果が高いため、より純度の高い有機溶
剤を得ることができる。As we have seen above, the method for purifying this aqueous solvent involves evaporating the raw material organic solvent 24 and passing the vapor through the filter 26 to eliminate fine particles contained in the dispersed state in the raw material organic solvent. This is to remove non-volatile impurities contained in the dissolved state. In this case, if an ultra-precision filter is used as the filter as in the example described in -, the organic solvent with higher purity can be obtained since the ultra-precision filter has a high effect of trapping particulates and accidental impurities. I can do it.
なお、この発明で除去の対象とする微粒子は、求められ
る純度のレベルに応じて種々異なるため、特に限定され
ず、たとえば、粒径０゜２μｍ以上のものである。また
、除去の対象とする不揮発性不純物も、限定されること
はなく、Ｋ ＣＩなどの溶存無機塩類、フタル酸水素カ
リウムなどの溶存有機金属塩、溶存有機物などである。The fine particles to be removed in the present invention are not particularly limited, as they vary depending on the desired level of purity, and are, for example, those having a particle diameter of 0°2 μm or more. Furthermore, the nonvolatile impurities to be removed are not limited, and include dissolved inorganic salts such as KCI, dissolved organic metal salts such as potassium hydrogen phthalate, dissolved organic substances, and the like.
この発明において、処理の対象とする有機溶剤としては
、下記のものが例示される。In this invention, the following are exemplified as the organic solvent to be treated.
ヘキサン、ヘプタンなどの脂肪族炭化水素、シクロヘキ
ーリンなどの脂環式炭化水素、ベンゼン。Aliphatic hydrocarbons such as hexane and heptane, alicyclic hydrocarbons such as cyclohekyline, and benzene.
ｍ−キシレン、トルエンなどの芳香族炭化水素、ｌ・４
−ジオキサン、テトラヒドロフラン、ピリジンなどの複
素環式化合物、四塩化炭素、トリクロロエチレン、クロ
ロホルム、ジクロロメタンなどのハロゲン化炭化水素、
メタノール、エタノール、イソプロピルアルコール、ブ
タノール、グリセリンなどのアルコール、フェノールな
どのフェノール類、アセトンなどのケトン、酢酸、酢酸
無水物、酢酸エチル、ホルムアミド、Ｎ、Ｎ−ジメチル
ホルムアミドなどのカルボン酸とその誘導体、ニトロベ
ンゼン、ニトロメタンなどのニトロ化合物、エチルエー
テル、１・２−ジメトキシエタン、ジエチレングリコー
ルジメチルエーテル、エチレングリコールモノメチルエ
ーテルなどのエーテルのほか、ジメチルスルホキシドな
ど。Aromatic hydrocarbons such as m-xylene and toluene, l.4
- Heterocyclic compounds such as dioxane, tetrahydrofuran, pyridine, halogenated hydrocarbons such as carbon tetrachloride, trichloroethylene, chloroform, dichloromethane,
Alcohols such as methanol, ethanol, isopropyl alcohol, butanol, glycerin, phenols such as phenol, ketones such as acetone, carboxylic acids and their derivatives such as acetic acid, acetic anhydride, ethyl acetate, formamide, N,N-dimethylformamide, Nitro compounds such as nitrobenzene and nitromethane, ethers such as ethyl ether, 1,2-dimethoxyethane, diethylene glycol dimethyl ether, and ethylene glycol monomethyl ether, as well as dimethyl sulfoxide.
この発明において、純度の極めて高い有機溶剤を得るに
は、つぎのようにしてもよい。すなわち、まず、前記実
施例において、メンブレンフィルタ部分を蒸発装置に置
き換えて、再生式イオン交換樹脂塔で処理された水を直
ちに蒸発させ、その蒸気をフィルタに通すことにより、
純度の極めて高い有機溶剤を得るようにする方法があげ
られる。他に、前処理された粗製有機溶剤をまず蒸発さ
せ、その蒸気をフィルタに通してから、真空脱気を行い
、再生式イオン交換樹脂塔で処理した後、再度蒸発させ
て、その蒸気をフィルタに通すことにより、純度の極め
て高い有機溶剤を得るようにする方法があげられる。In this invention, the following method may be used to obtain an organic solvent with extremely high purity. That is, first, in the above embodiment, the membrane filter part is replaced with an evaporator, the water treated in the regenerative ion exchange resin column is immediately evaporated, and the vapor is passed through the filter.
One example is a method of obtaining an organic solvent with extremely high purity. Another method is to first evaporate the pretreated crude organic solvent, pass the vapor through a filter, perform vacuum degassing, treat it in a regenerative ion exchange resin tower, evaporate it again, and pass the vapor through a filter. An example of a method is to obtain an organic solvent of extremely high purity by passing the organic solvent through the solvent.
この発明に用いられるフィルタとと２では、耐熱性が高
く、しかも、微粒子も捕捉することができるフィルタ、
例えば、ＨＥ Ｐ Ａ （Ｈｉｇｈ Ｅｆｆｉｃｉｅｎ
ｃｙ Ｐａｒｔｉｃｕｌａｔｅ Ａｉｒ）フィルり、Ｕ
Ｌ Ｐ Ａ （ＵｌｔｒａＬｏｗ Ｐｅｎｅｔｒａ
ｔｉｏｎ Ａｉｒ）フィルタ、メンブレンフィルタ、静
電式フィルタなどの超精密フィルタ等が好ましい。これ
らのフィルタの材質は、耐熱性が高い、不純物の溶出が
ないなどの点から、たとえば、四フッ化エチレン樹脂（
デュポン社のテフロンなど）、シリカファイバなどが、
好ましい。The filter used in this invention is a filter that has high heat resistance and can also capture fine particles.
For example, H.E.P.A.
cy Particulate Air) Fill, U
L P A (UltraLow Penetra
Ultra-precision filters such as tion air filters, membrane filters, and electrostatic filters are preferable. The materials used for these filters are, for example, tetrafluoroethylene resin (
DuPont's Teflon, etc.), silica fiber, etc.
preferable.
以下に、実施例と比較例を示す。Examples and comparative examples are shown below.
一実施例−
前処理されたエタノールを熱交換器で２５℃に温め、５
μｍのプレフィルタで濾過して、ｐＨを弱酸性に調節し
た後、逆浸透装置に送って、イオン分の除去および他の
有機物や無機物、コロイド状物質の分離除去を行い、真
空脱器塔で溶存ガスの除去を行った。つぎに、再生式イ
オン交換樹脂塔で脱イオンして、０．２μｍのメンブレ
ンフィルタで濾過した後、蒸発装置で蒸発させて、その
蒸気をＵＬＰＡフィルタに通し、精製エタノールを得た
。One example - Pretreated ethanol was warmed to 25 °C in a heat exchanger and heated to 5 °C.
After filtering with a μm pre-filter and adjusting the pH to slightly acidic, it is sent to a reverse osmosis device to remove ions and other organic substances, inorganic substances, and colloidal substances. Dissolved gas was removed. Next, it was deionized using a regenerative ion exchange resin column, filtered using a 0.2 μm membrane filter, evaporated using an evaporator, and the vapor was passed through a ULPA filter to obtain purified ethanol.
一比較例一
上記実施例において、蒸発装置で蒸発させてその蒸気を
ＵＬＰＡフィルタに通す工程を省略した。それ以外は、
上記実施例と同様にして、エタノールを精製した。Comparative Example 1 In the above example, the step of evaporating with an evaporator and passing the vapor through a ULPA filter was omitted. Other than that,
Ethanol was purified in the same manner as in the above example.
以上のようにして得られた精製エタノールについて、微
粒子の含有数および不揮発性不純物の含有量の測定を行
った。その結果は第１表のとおりである。Regarding the purified ethanol obtained as described above, the number of fine particles contained and the content of non-volatile impurities were measured. The results are shown in Table 1.
第 １ 表
第１表をみてわかるように、実施例は、比較例より微粒
子の含有数および不揮発性不純物の含有量が極めて少な
くなっている。Table 1 As can be seen from Table 1, the number of fine particles and the content of non-volatile impurities in the Examples are significantly lower than in the Comparative Examples.
この発明にかかる有機溶剤の精製法は、前記実施例に限
定されない。原料有機溶剤としては、前記実施例のよう
に、種々の工程を経て精製されたものが好ましいが、粗
製有機溶剤をそのまま用いるようにしてもよく、とくに
限定されない。The organic solvent purification method according to the present invention is not limited to the above embodiments. As the raw organic solvent, it is preferable to use one purified through various steps as in the above examples, but a crude organic solvent may be used as it is, and is not particularly limited.
なお、前記実施例では、原料有機溶剤中に微粒子および
不揮発性不純物が共に含まれている場合を示したが、微
粒子および不揮発性不純物のどちらか一方が原料水中に
含まれていないか、含まれていてもごく僅かの場合もあ
る。このような場合には、微粒子および不揮発性不純物
のどちらか一方のみが除去されることになる。In addition, in the above example, a case was shown in which both fine particles and non-volatile impurities were contained in the raw material organic solvent, but either one of the fine particles and non-volatile impurities was not contained in the raw material water, or it was not included. In some cases, it may be very small. In such a case, only either the particulates or the non-volatile impurities will be removed.
Ｃ発明の効果〕
この発明にかかる有機溶剤の精製法は、以上のように構
成されているため、極めて純度の高い有機溶剤を得るこ
とができる。C Effects of the Invention] Since the method for purifying an organic solvent according to the present invention is configured as described above, it is possible to obtain an organic solvent with extremely high purity.
第１図はこの発明にかかる有機溶剤の精製法の一実施例
をあられす説明図である。
２４・・・原料有機溶剤 ２６・・・フィルタ代理人
弁理士 松 本 武 彦FIG. 1 is an explanatory diagram illustrating an embodiment of the organic solvent purification method according to the present invention. 24... Raw material organic solvent 26... Filter agent
Patent attorney Takehiko Matsumoto
Claims (1)
通すことにより、原料有機溶剤中に含まれていた微粒子
および原料有機溶剤中に溶存していた不揮発性不純物を
前記フィルタで除去して、純度の極めて高い有機溶剤を
得るようにする有機溶剤の精製法。1 By evaporating the raw organic solvent and passing the vapor through a filter, the fine particles contained in the raw organic solvent and the non-volatile impurities dissolved in the raw organic solvent are removed by the filter, and the purity is improved. A method for purifying organic solvents that allows obtaining extremely high organic solvents.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10589188A JPH01274801A (en) | 1988-04-27 | 1988-04-27 | Method for purifying organic solvent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP10589188A JPH01274801A (en) | 1988-04-27 | 1988-04-27 | Method for purifying organic solvent |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01274801A true JPH01274801A (en) | 1989-11-02 |
Family
ID=14419539
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP10589188A Pending JPH01274801A (en) | 1988-04-27 | 1988-04-27 | Method for purifying organic solvent |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01274801A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108091496A (en) * | 2018-01-09 | 2018-05-29 | 东莞市天丰电源材料有限公司 | A kind of electrolytic solution for super capacitor production system |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57140602A (en) * | 1981-02-26 | 1982-08-31 | Yoshimi Oshitari | Apparatus for distilling liquid |
| JPS62225204A (en) * | 1986-03-26 | 1987-10-03 | Hitachi Ltd | Distilling purifying device |
| JPH01119301A (en) * | 1987-10-31 | 1989-05-11 | Yoshimi Oshitari | Distillatory concentration apparatus |
-
1988
- 1988-04-27 JP JP10589188A patent/JPH01274801A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57140602A (en) * | 1981-02-26 | 1982-08-31 | Yoshimi Oshitari | Apparatus for distilling liquid |
| JPS62225204A (en) * | 1986-03-26 | 1987-10-03 | Hitachi Ltd | Distilling purifying device |
| JPH01119301A (en) * | 1987-10-31 | 1989-05-11 | Yoshimi Oshitari | Distillatory concentration apparatus |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108091496A (en) * | 2018-01-09 | 2018-05-29 | 东莞市天丰电源材料有限公司 | A kind of electrolytic solution for super capacitor production system |
| CN108091496B (en) * | 2018-01-09 | 2024-02-23 | 东莞市天丰电源材料有限公司 | Supercapacitor electrolyte production system |
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