JPS5918088B2 - Method for purifying valuable substances in liquid - Google Patents

Method for purifying valuable substances in liquid

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Publication number
JPS5918088B2
JPS5918088B2 JP51154704A JP15470476A JPS5918088B2 JP S5918088 B2 JPS5918088 B2 JP S5918088B2 JP 51154704 A JP51154704 A JP 51154704A JP 15470476 A JP15470476 A JP 15470476A JP S5918088 B2 JPS5918088 B2 JP S5918088B2
Authority
JP
Japan
Prior art keywords
liquid
membrane
stage
cleaning medium
valuable substances
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
Application number
JP51154704A
Other languages
Japanese (ja)
Other versions
JPS5378665A (en
Inventor
輝嘉 塚本
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.)
Ebara Corp
Original Assignee
Ebara Infilco 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 Ebara Infilco Co Ltd filed Critical Ebara Infilco Co Ltd
Priority to JP51154704A priority Critical patent/JPS5918088B2/en
Publication of JPS5378665A publication Critical patent/JPS5378665A/en
Publication of JPS5918088B2 publication Critical patent/JPS5918088B2/en
Expired legal-status Critical Current

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Description

【発明の詳細な説明】 本発明は、醗酵工業、製薬工業、製糖工業、蛋白質アミ
ノ酸工業、食品工業、あるいは工場廃水などの有機性あ
るいは無機性物質含有液中の有価物を精製する方法に関
するものである。
DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for purifying valuable substances in liquids containing organic or inorganic substances such as fermentation industry, pharmaceutical industry, sugar refining industry, protein and amino acid industry, food industry, or factory wastewater. It is.

本発明は、液中の有価物を効率よく精製回収することを
目的とするもので、有機物、無機物を含有する液を原液
として、洗浄媒液を添加しつつマイクロポーラス膜乃至
限外沖過膜に通液することによって膜面残留液と膜透過
液とに分離し不純物を膜透過液中に移行させ、原液中の
有機、無機性有価物を精製回収することを特徴とするも
のである。
The purpose of the present invention is to efficiently purify and recover valuable substances in a liquid, and use a liquid containing organic and inorganic substances as a stock solution to form a microporous membrane or ultrafiltration membrane while adding a cleaning medium. The method is characterized in that it is separated into a membrane surface residual liquid and a membrane-permeated liquid by passing liquid through the membrane, and impurities are transferred to the membrane-permeated liquid to purify and recover organic and inorganic valuables in the raw liquid.

ずなわら、本発明は、有機性物質としては、例えば蛋白
質含有液、合成高分子物質や天然高分子物質の親水性液
、あるいはこれらの沈殿含有液、無機性物質としては、
金属水酸化物、酸化物、硫化物等の沈殿含有液、粘土鉱
物や結晶等の含有液に、適当な洗浄媒液を添加しつつマ
イクロポーラス膜乃至限外r過膜を装着したセルに通液
し、該液中の有機、無機物質を洗浄精製し、膜面残留液
として回収するものである。
In the present invention, organic substances include, for example, protein-containing liquids, hydrophilic liquids of synthetic polymeric substances and natural polymeric substances, or liquids containing precipitates thereof, and inorganic substances such as:
A suitable cleaning medium is added to a liquid containing precipitates such as metal hydroxides, oxides, and sulfides, and a liquid containing clay minerals and crystals, and the liquid is passed through a cell equipped with a microporous membrane or ultrafiltration membrane. The liquid is drained, the organic and inorganic substances in the liquid are washed and purified, and the liquid remaining on the membrane surface is recovered.

また、上記マイクロポーラス膜乃至限外沖過膜を装着し
たセルに通液する原液は、あらかじめ濃縮しておくとよ
く、その調整方法には特に制限はないが、例えば加圧下
に透過膜に通液するこきによって濃縮液と膜透過液とに
分離し、親水性物質あるいは懸濁、乳濁性物質を含む濃
縮液を調整してこれを原液としたり、あるいは透過膜に
よって濃縮している間に発生した懸濁物、乳濁物、異物
を含む濃縮液を原液としてもよく、あるいはこれらの濃
縮液を沈降、浮上、濾過(膜沖過を含む)、遠心分離、
吸着、捕集などの分離手段によって分離処理し、この分
離された濃縮液を原液としてもよく、また上記膜処理前
の液あるいは膜処理後の濃縮液を加熱処理、pH調整、
凝集剤の注入、高分子化合物や無機塩などの添加剤を添
加して沈殿物を生成させるもよい。
In addition, the stock solution to be passed through the cell equipped with the above-mentioned microporous membrane or ultra-permeable membrane should be concentrated in advance, and there are no particular restrictions on the method of preparation, but for example, the stock solution is passed through the permeable membrane under pressure. The concentrated liquid and the membrane-permeated liquid are separated by pouring, and a concentrated liquid containing hydrophilic substances, suspended or emulsified substances is prepared and used as a stock solution, or during concentration through the permeable membrane. The concentrated liquid containing the generated suspended matter, emulsion, and foreign matter may be used as a stock solution, or the concentrated liquid may be subjected to sedimentation, flotation, filtration (including membrane filtration), centrifugation,
Separation treatment may be performed by a separation means such as adsorption or collection, and the separated concentrated liquid may be used as a stock solution, or the liquid before membrane treatment or the concentrated liquid after membrane treatment may be subjected to heat treatment, pH adjustment,
A precipitate may be generated by injecting a flocculant or adding additives such as a polymer compound or an inorganic salt.

さらに、有機、無機性物質含有液の濃縮手段としては、
上記各方法以外に蒸発法、冷凍法、イオン交換法、通常
の沈殿析出法による沈殿分離濃縮でもよく、濃度によっ
ては上記各濃縮手段を省略してもよい。
Furthermore, as a means of concentrating liquids containing organic and inorganic substances,
In addition to the above-mentioned methods, precipitation separation and concentration by evaporation, freezing, ion exchange, and ordinary precipitation methods may be used, and depending on the concentration, the above-mentioned concentration means may be omitted.

本発明において使用されるマイクロポーラス膜乃至限外
沖過膜としては、ポリエステル、アセチルセルローズ、
エチルセルローズ、アセチルブチルセルローズなどのセ
ルローズ系膜をはじめ、ポリアクリルアミド系膜、ポリ
アクリロニトリル膜、ポリビニレンカーボネート膜、ポ
リスルフォン膜などの有機性膜、グラファイト系化合物
よりなる膜のような金属酸化物、炭素化合物を含む無機
性膜、あるいはダイナミンク膜等の無機性膜も使用され
る。
The microporous membrane or ultrafilament membrane used in the present invention includes polyester, acetyl cellulose,
In addition to cellulose-based films such as ethyl cellulose and acetyl butyl cellulose, organic films such as polyacrylamide-based films, polyacrylonitrile films, polyvinylene carbonate films, and polysulfone films, metal oxide films such as films made of graphite-based compounds, An inorganic film containing a carbon compound or an inorganic film such as a Dynamink film may also be used.

なお、マイクロポーラス膜乃至限外沖過膜を使用するに
当っては、微生物の活動の予測されるときには60〜9
0℃における高温処理あるいは10℃以下の低温処理を
行なえば、微生物による成分分解に対する影響あるいは
膜自体に対する微生物による支障を阻市することができ
、これらの膜装置は性能の維持管理上管型膜装置、平板
膜装置が効果的で、圧力は1〜100 kgf/crt
lが通常利用される。
In addition, when using a microporous membrane or a microporous membrane, when microbial activity is expected, the
High-temperature treatment at 0°C or low-temperature treatment at 10°C or lower can prevent the effects of microorganisms on decomposition of components or the interference of microorganisms with the membrane itself. A flat plate membrane device is effective, and the pressure is 1 to 100 kgf/crt.
l is usually used.

また、本発明におけるマイクロポーラス膜乃至限外沖過
膜に対する通液は、直列多段に行なうことができ、その
場合の洗浄媒液の添加は最終段への供給液に対して行な
い、さらに多段の場合に初段以外の膜透過液を各その直
前段の供給液に添加することによって洗浄媒液の効果的
利用をはかるもよく、このように多段に行なう場合には
同一特性の膜を使用することも、分割分子量の大きい膜
を初段にし、その後順次分割分子量の小さい膜を使用す
ることもできる。
In addition, in the present invention, the liquid can be passed through the microporous membrane or the ultraviolet filtration membrane in multiple stages in series, and in that case, the cleaning medium is added to the liquid supplied to the final stage, and In some cases, effective use of the cleaning medium may be achieved by adding the membrane permeate from the membranes other than the first stage to the feed liquid from the immediately preceding stage, and when carrying out multiple stages like this, membranes with the same characteristics should be used. Alternatively, it is also possible to use a membrane with a large split molecular weight as the first stage, and then sequentially use membranes with a small split molecular weight.

本発明において使用する洗浄媒液としては、被洗浄物質
の特性、洗浄目的等によって選択するが、各種の有機性
、無機性の洗浄媒液を利用できるが、多くは淡水、アル
コール、酸、アルカリ液であり、また、これら洗浄媒液
に安定剤、凝集剤、pH調整剤、分散剤、あるいは品質
改良のための漂白剤、脱色剤等の酸化還元剤を併用する
もよい。
The cleaning medium used in the present invention is selected depending on the characteristics of the substance to be cleaned, the purpose of cleaning, etc. Various organic and inorganic cleaning mediums can be used, but most include fresh water, alcohol, acid, and alkali. In addition, stabilizers, flocculants, pH adjusters, dispersants, or redox agents such as bleaches and decolorizers for quality improvement may be used in combination with these cleaning media.

さらに本発明の実施態様を図面を参照しつつ説明すると
、第1図示例において、まず、被処理液1を前濃縮のた
めの膜装置Aに導入して膜面残留濃縮液2と膜透過液3
とに分離する。
Further, an embodiment of the present invention will be described with reference to the drawings. In the first illustrated example, first, the liquid to be treated 1 is introduced into the membrane device A for pre-concentration, and the concentrated liquid remaining on the membrane surface 2 and the membrane permeated liquid are 3
Separate into two parts.

この膜装置Aにおいては、膜特性によって要する圧力は
異なるも、マイクロポーラス膜乃至限外沖過膜を使用す
るときは1〜10に9f/fflであり、逆浸透膜にあ
っては15〜100 kgf/crA程度がよい。
In this membrane device A, the pressure required differs depending on the membrane characteristics, but when using a microporous membrane or ultrafiltration membrane, it is 9 f/ffl from 1 to 10, and when using a reverse osmosis membrane, it is 15 to 100 f/ffl. About kgf/crA is good.

また、膜装置Aを二段さし、前段に距浸透膜装置を配し
てその濃縮液を後段に配したマイクロポーラス膜乃至限
外0−コ過膜装置でさらに膜分離による濃縮を行なって
もよい。
In addition, further concentration by membrane separation is carried out using a microporous membrane or ultra-zero filtration membrane device in which the membrane device A is installed in two stages, a distance permeation membrane device is placed in the first stage, and the concentrated liquid is placed in the second stage. Good too.

かくして得られた濃縮液2を洗浄精製するためのマイク
ロポーラス膜乃至限外濾過膜装置Bへ供給するが、この
場合、供給される濃縮液2中へ洗浄媒液4また必要に応
じて上記安定剤等を添加し、マイクロポーラス膜乃至限
外濾過膜装置Bにおいて膜分離することによって、洗浄
精製された液中の有価物を含む膜面残留液5を回収し、
不純物は膜透過液(洗浄後液)6中に移行され、系外へ
排出される。
The concentrate 2 thus obtained is supplied to a microporous membrane or ultrafiltration membrane device B for washing and purification. In this case, the cleaning medium 4 is added to the supplied concentrate 2 and, if necessary, A residual liquid 5 on the membrane surface containing valuable substances in the washed and purified liquid is collected by adding a reagent, etc., and performing membrane separation in a microporous membrane or ultrafiltration membrane device B.
The impurities are transferred into the membrane permeate liquid (washed liquid) 6 and discharged to the outside of the system.

第2図示例は、上記第1図示例における前濃縮のための
膜装置Aを沈降分゛膜装置、浮上分離装置、遠心分離機
、イオン交換装置、吸着分離装置等の濃縮装置Cに代え
たもので、沈降分前によ−〕で濃縮されたスラッジ2′
を対象とし、その他は第1図示例と同様である。
In the second illustrated example, the membrane device A for pre-concentration in the first illustrated example is replaced with a concentrator C such as a sedimentation membrane device, flotation separation device, centrifugal separator, ion exchange device, adsorption separation device, etc. The sludge 2' was concentrated before settling.
The other aspects are the same as the first illustrated example.

第3図示例は、本発明を多段にした例であって、さらに
洗浄媒液を反復利用しようとするものである。
The third illustrated example is an example in which the present invention is multi-staged, and the cleaning medium is further used repeatedly.

すなわち、上記各図示例における洗浄精製するためのマ
イクロポーラス膜乃至限外濾過膜装置Bを例えばB−1
、B−2、B−3、B−4と4段に設置し、必要に応じ
て濃縮あるいは調整された供給液2を第1段装置B−1
へ供給するに当って、第2段装置H−2の膜透過液6“
を洗浄媒液として添加し、ここで膜面残留液5“′と膜
透過液6″に分離、膜透過液6′7を系外へ排出する。
That is, the microporous membrane or ultrafiltration membrane device B for cleaning and purification in each of the above illustrated examples is, for example, B-1.
, B-2, B-3, and B-4, and supply liquid 2, which has been concentrated or adjusted as necessary, to the first stage device B-1.
In supplying the membrane permeate liquid 6'' of the second stage device H-2 to
is added as a cleaning medium, and here it is separated into a membrane surface residual liquid 5'' and a membrane permeate liquid 6'', and the membrane permeate liquid 6'7 is discharged to the outside of the system.

次いでこの膜面残留液5″を第2段装置B−2へ供給す
るに当って、第3段装置B−3の膜透過液6′を洗浄媒
液として添加し、ここで膜面残留液5“と膜透過液6“
とに分離し、膜透過液6“を前記のように第1段装置B
−1での洗浄媒液上して利用する。
Next, when this membrane surface residual liquid 5'' is supplied to the second stage apparatus B-2, the membrane permeate liquid 6' from the third stage apparatus B-3 is added as a cleaning medium, and here the membrane surface residual liquid is 5" and membrane permeate 6"
and the membrane permeate 6'' is transferred to the first stage device B as described above.
-Use the cleaning medium in step 1 above.

第2段装置B−2において洗浄精製をうけた膜面残留液
5“は、次の第3段装置B−3へ供給されるが、ここで
第4段装置B−4の膜透過液6を洗浄媒液上して添加し
、膜面残留液5′と膜透過液6′とに分離し、膜透過液
6′を前記のように第2段装置B−2での洗浄媒液とし
て利用し、膜面残留液5′は新たな洗浄媒液4が添加さ
れて第4段装置B−4に供給され、膜面残留液5は洗浄
された精製品として回収され、膜透過液6は第3段装置
B−3の洗浄媒液として利用される。
The membrane surface residual liquid 5" that has been washed and purified in the second stage apparatus B-2 is supplied to the next third stage apparatus B-3, where the membrane permeated liquid 6" of the fourth stage apparatus B-4 is supplied to the third stage apparatus B-3. is added above the cleaning medium solution, separated into membrane surface residual liquid 5' and membrane permeate liquid 6', and membrane permeate liquid 6' is used as the cleaning medium liquid in the second stage device B-2 as described above. The residual liquid 5' on the membrane surface is added with a new cleaning medium 4 and supplied to the fourth stage device B-4, the residual liquid 5 on the membrane surface is recovered as a purified product, and the membrane permeated liquid 6 is is used as a cleaning medium in the third stage device B-3.

以上述べたように本発明によれば、有機、無機物質を含
(iする液中の有機、無機物質は勿論、有機、無機性の
懸濁液、乳濁液の洗浄、精製を極めて効率よく行ない、
精製された有価物を回収することができ、蛋白質、薬剤
、高分子化合物などの精製や結晶の精製なども効果的に
行なうことができるものである。
As described above, according to the present invention, not only organic and inorganic substances in liquids containing organic and inorganic substances, but also organic and inorganic suspensions and emulsions can be washed and purified extremely efficiently. conduct,
Purified valuable substances can be recovered, and proteins, drugs, polymer compounds, etc., and crystals can be purified effectively.

次に本発明の実施例を示す。Next, examples of the present invention will be shown.

実施例 1 蛋白質1.8%含有する廃液をpa+ 4.5〜5.0
に調整し、80〜90℃にて30分間加熱したのち、凝
集沈殿により蛋白質・を凝集沈殿濃縮し、固形分3%を
含む蛋白質含有スラリを得た。
Example 1 Waste liquid containing 1.8% protein was adjusted to pa+ 4.5-5.0
After heating at 80 to 90° C. for 30 minutes, the protein was concentrated by coagulation and precipitation to obtain a protein-containing slurry containing 3% solid content.

次にこのスラグ51/分に対して70℃に加熱した淡水
を151/分の流量比で添加しつつ、5インチの管型限
外沖過膜装置に通液した。
Next, fresh water heated to 70° C. was added to the slag at a flow rate of 51/min at a flow rate of 151/min, and the slag was passed through a 5-inch tube-type ultrafilter membrane device.

この場合、入口圧力は5kgf/cnfで液温は70〜
80 ”C:であり、固形分7,5%の精製蛋白スラリ
を211分で回収し?また。
In this case, the inlet pressure is 5 kgf/cnf and the liquid temperature is 70~
80"C:, and a purified protein slurry with a solid content of 7.5% was collected in 211 minutes.

かくて蛋白質と共存する無機成分を約%〜%程度に減少
させることができた。
In this way, the amount of inorganic components coexisting with protein could be reduced to approximately % to %.

実施例 2 .5インチの管型限外沢過膜装置を2段に配置し、固形
分として3%の蛋白質含有液31/分と第2段限外沖過
膜装置の膜透過液を171j/分の流量比で共に第1段
限外沖過膜装置に圧力5に9f/i、液温s o ’c
において通液し膜面残留液211分を得た。
Example 2. A 5-inch tube-type ultrafiltration membrane device is arranged in two stages, and a liquid containing 3% protein as a solid content is 31/min and a membrane permeate liquid from the second stage ultrafiltration membrane device is flowed at a flow rate of 171j/min. At a ratio of 5 to 9f/i and a liquid temperature of 5 to 9 f/i to the first stage ultra-fine filtration device.
A liquid was passed through the membrane to obtain a residual liquid of 211 minutes on the membrane surface.

この膜面残留液に171!/分の流に比で80℃に加熱
したえん酸によりpH4,5〜5.0に調整した淡水を
添加し、第2段限外沖過膜装置に圧力5 kg f/c
r/l、液温80℃で通液し、固形分として4:5%の
蛋白質を含有する膜面残留液21/分を得た。
171 to this residual liquid on the membrane surface! Fresh water adjusted to pH 4.5 to 5.0 with citric acid heated to 80°C was added to the flow per minute, and the pressure was set at 5 kg f/c to the second stage ultrafiltration membrane device.
The solution was passed through the solution at a temperature of 80° C., and a residual liquid on the membrane surface containing 4:5% protein as a solid content was obtained at 21/min.

かくて蛋白質と共存する無機塩分を約75 〜協程度に減少させることができた。In this way, the inorganic salts that coexist with protein are reduced to about 75%. - We were able to reduce it to a level of cooperation.

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

第1図は本発明の一実施態様を示す系統説明図、第2図
は他の実施態様を示す系統説明図、第3図は他の実が(
j態様を示す系統説明図である。 A−・・・・・膜装置、B・・・・・・マイクロポーラ
ス膜乃至限外濾過膜装置、C・・・・・・濃縮装置、1
・・・・・・被処理液、4・・・・・・洗浄媒液。
Fig. 1 is a system explanatory diagram showing one embodiment of the present invention, Fig. 2 is a system explanatory diagram showing another embodiment, and Fig. 3 is a system explanatory diagram showing another embodiment of the present invention.
FIG. A-...Membrane device, B...Microporous membrane or ultrafiltration membrane device, C...Concentration device, 1
...Liquid to be treated, 4...Cleaning medium liquid.

Claims (1)

【特許請求の範囲】 1 有機物、無機物を含有する液に淡水、アルコール、
酸、およびアルカリ液のいづれかを洗浄媒液として添加
しつつマイクロポーラス膜乃至限外濾過膜に通液し、膜
面残留液と膜透過液とに分離する液中の有価物の精製方
法において、前記マイクロポーラス膜乃至限外濾過膜に
対する通液を直列多段に行ない、かつ最終段への供給液
に洗浄媒液を添加し、該最終段の膜透過液をその前段の
供給液に添加することを特徴とする液中の有価物の精製
方法。 2 前記初段以外の膜透過液をそれぞれの前段の供給液
に添加する特許請求の範囲第1項記載の液中の有価物の
精製方法。
[Claims] 1. Fresh water, alcohol,
In a method for purifying valuable substances in a liquid, the liquid is passed through a microporous membrane or an ultrafiltration membrane while adding either an acid or an alkaline liquid as a cleaning medium, and separated into a membrane surface residual liquid and a membrane permeated liquid, Passing liquid through the microporous membrane or ultrafiltration membrane in series in multiple stages, adding a cleaning medium solution to the liquid supplied to the final stage, and adding the membrane permeate liquid from the final stage to the liquid supplied from the preceding stage. A method for purifying valuable substances in a liquid, characterized by: 2. The method for purifying valuable substances in a liquid according to claim 1, wherein the membrane permeate liquid other than the first stage is added to the feed liquid of each previous stage.
JP51154704A 1976-12-21 1976-12-21 Method for purifying valuable substances in liquid Expired JPS5918088B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP51154704A JPS5918088B2 (en) 1976-12-21 1976-12-21 Method for purifying valuable substances in liquid

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP51154704A JPS5918088B2 (en) 1976-12-21 1976-12-21 Method for purifying valuable substances in liquid

Publications (2)

Publication Number Publication Date
JPS5378665A JPS5378665A (en) 1978-07-12
JPS5918088B2 true JPS5918088B2 (en) 1984-04-25

Family

ID=15590120

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JP51154704A Expired JPS5918088B2 (en) 1976-12-21 1976-12-21 Method for purifying valuable substances in liquid

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Country Link
JP (1) JPS5918088B2 (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59140188A (en) * 1983-01-28 1984-08-11 ヤマハ発動機株式会社 Support structure of pivot shaft of motorcycle
CN106731851A (en) * 2017-01-04 2017-05-31 北京化工大学 A kind of method of anhydrous solvent in utilization infiltrating and vaporizing membrane separation and fermentation liquid

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3694871B2 (en) * 1996-10-18 2005-09-14 日鉄化工機株式会社 Separation and recovery method of target components
JP4485738B2 (en) * 2002-06-12 2010-06-23 月島環境エンジニアリング株式会社 Method for separating and recovering target substances
JP5398577B2 (en) * 2010-02-23 2014-01-29 月島環境エンジニアリング株式会社 Method and apparatus for separation and recovery of target substances

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5246127Y2 (en) * 1972-02-24 1977-10-20

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS59140188A (en) * 1983-01-28 1984-08-11 ヤマハ発動機株式会社 Support structure of pivot shaft of motorcycle
CN106731851A (en) * 2017-01-04 2017-05-31 北京化工大学 A kind of method of anhydrous solvent in utilization infiltrating and vaporizing membrane separation and fermentation liquid

Also Published As

Publication number Publication date
JPS5378665A (en) 1978-07-12

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