JPS60197288A - Preparation of aseptic water - Google Patents

Preparation of aseptic water

Info

Publication number
JPS60197288A
JPS60197288A JP59053845A JP5384584A JPS60197288A JP S60197288 A JPS60197288 A JP S60197288A JP 59053845 A JP59053845 A JP 59053845A JP 5384584 A JP5384584 A JP 5384584A JP S60197288 A JPS60197288 A JP S60197288A
Authority
JP
Japan
Prior art keywords
water
hollow
ratio
hollow fiber
average pore
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
Application number
JP59053845A
Other languages
Japanese (ja)
Inventor
Matsuro Suzuki
鈴木 松郎
Takanori Anazawa
穴沢 孝典
Yoshiyuki Ono
善之 小野
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.)
Kawamura Institute of Chemical Research
DIC Corp
Original Assignee
Kawamura Institute of Chemical Research
Dainippon Ink and 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 Kawamura Institute of Chemical Research, Dainippon Ink and Chemicals Co Ltd filed Critical Kawamura Institute of Chemical Research
Priority to JP59053845A priority Critical patent/JPS60197288A/en
Publication of JPS60197288A publication Critical patent/JPS60197288A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/44Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • C02F1/444Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D71/00Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06Organic material
    • B01D71/66Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only

Abstract

PURPOSE:To obtain aseptic water sterilizable by a chemical agent, by treating water with a hollow fiber based on polyphenylene sulfide having fine piercing pores with a specific average pore size and a specific void ratio, specific membrane thickness, a hollow ratio and an outer diameter. CONSTITUTION:Water is filtered by using a hollow fiber, which has fine piercing pores with an average pore size of 0.01-0.1mum and a void ratio of 10-85% and of which the membrane thickness is 5-200mum, the hollow ratio is 8-85% and the outer diameter is 30mum-5mm., to remove bacteria in water. For example, well water is precisely filtered by using a module (an available area of 1.2m<2>) of a microporous hollow fiber comprising polyphenylene sulfide with an average pore size of 0.061mum, a void ratio of 35%, a membrane thickness of 19mum, a hollow ratio of 64% and an outer diameter of 192mum under a pressure of 3kg/ cm<2> toward the inside of the hollow fiber from the outside thereof. The amount of transmitted water after filtering over 5hr is 500l/m<2>.hr and a bacteria removal ratio measured by a direct microscopic examination method is 100%.

Description

【発明の詳細な説明】 廃水の再利用、医薬品や食品の製造、電子工業用水など
において無菌水の需要は枚挙にいとまがない。近年、こ
のような無菌水の製造に、膜濾過法が雀エネルギーでり
るなど様々な利点から適用されている。このような無菌
水製造用の分離膜には、セルロース系、ナイロン6.6
あるいはスルホン化ポリオレフィンなどが用いられてい
る。
DETAILED DESCRIPTION OF THE INVENTION The demand for sterile water is overwhelming for purposes such as wastewater reuse, pharmaceutical and food manufacturing, and electronic industry water. In recent years, membrane filtration has been applied to the production of sterile water due to its various advantages, including its use of energy. Separation membranes for producing sterile water include cellulose-based and nylon 6.6 membranes.
Alternatively, sulfonated polyolefins are used.

しかし、これらの膜は耐熱性、耐薬品性の満足できるも
のはなく、化学洗浄あるいはスチーム洗浄による滅閘処
理ができず、回生再使用が出来ない、j漠寿命が短かい
などの問題を有していた。
However, none of these membranes has satisfactory heat resistance or chemical resistance, cannot be sterilized by chemical or steam cleaning, cannot be reused, and has short service life. Was.

本発明者らは、かかる問題点を鑑み鋭意検討した結果、
化学薬剤または熱水あるいはスチームによる滅菌が可能
で、かつip過寿命が長い無菌水の製造方法を発明した
As a result of intensive study in view of such problems, the present inventors found that
We have invented a method for producing sterile water that can be sterilized by chemical agents, hot water, or steam, and has a long IP overlife.

すなわち、平均孔径0.01〜1μ、窒孔率10〜85
%の貫通した微多孔を有し、膜厚5〜200μm、中空
率8〜85%、外径30μrIL〜5趨のポリフェニレ
ンスルフィドを主成分とする中空繊維を用いることによ
シ目的が達成されることを見出した。
That is, the average pore diameter is 0.01 to 1μ, and the nitrogen porosity is 10 to 85.
This objective can be achieved by using hollow fibers mainly composed of polyphenylene sulfide, which have 5% penetrating microporosity, a membrane thickness of 5 to 200 μm, a hollow ratio of 8 to 85%, and an outer diameter of 30 μrIL to 5. I discovered that.

本発明で用いる中空繊維は外表面から内表面に貫通した
微多孔を有することが必要であり、このことは繊維の断
面を電子顕微鏡によシ観察して確認される。また平均孔
径は0.01〜1μ、空孔率は10〜85%であること
が必要である。平均孔径0.01μ以下、空孔率゛10
%以下の場合は透水量が少なく実用的ではない。平均孔
径が1μ以上の場合は透過水中に菌が漏洩し、空孔率8
5%以−ヒの場合は中空系の機械的強度が弱くなる。な
お、平均孔径は電子顕微鏡観察から次式によ請求めるこ
とができる。
The hollow fiber used in the present invention must have micropores that penetrate from the outer surface to the inner surface, and this is confirmed by observing the cross section of the fiber using an electron microscope. Further, it is necessary that the average pore diameter is 0.01 to 1 μm and the porosity is 10 to 85%. Average pore diameter 0.01μ or less, porosity ゛10
% or less, the amount of water permeation is so small that it is not practical. If the average pore diameter is 1μ or more, bacteria will leak into the permeated water, and the porosity will be 8.
If it is less than 5%, the mechanical strength of the hollow system becomes weak. Note that the average pore diameter can be calculated from electron microscopic observation using the following formula.

但しη=20〜100 また空孔率は、100個の孔が占める外表面の面&を測
定し、そnに基き外表面1cIL2当りの微多孔の個数
を4葬し、空孔率(%)=(外表面1cInF尚りの微
多孔の細動つ×(平均孔径(cm)X−戸X5.14X
100’(1″計算してめることができる。
However, η = 20 to 100 In addition, the porosity is determined by measuring the surface area of the outer surface occupied by 100 pores, and then calculating the number of micropores per 1 cIL2 of the outer surface by 4, and calculating the porosity (%). ) = (fibrillation of micropores of 1 cInF on the outer surface x (average pore diameter (cm) x - door x 5.14 x
It can be calculated by 100'(1'').

さらに、本発明に用いる中空欅維は、膜厚5〜200μ
m1中空率8〜85%、外径60μrrL〜5朋である
ことが必胃であめ。膜厚5μm以下、中空率85%以上
、あるいは外径60μm以下では中空繊維の伎械的強度
が低くなシ、膜厚200μrrL1中空率8%以下、外
径5罪以上ではffs過効率が低く実用的でない。なお
中空率は、顕微貌によりl@、計的に測定した平均外径
Doと平均内径り、から中空率=(Ds/Do)”X 
100 (s) として11掬ルてめらnる。
Furthermore, the hollow keyaki fiber used in the present invention has a film thickness of 5 to 200 μm.
It is essential that m1 has a hollow ratio of 8 to 85% and an outer diameter of 60 μrr to 5 mm. If the film thickness is 5μm or less, the hollowness ratio is 85% or more, or the outer diameter is less than 60μm, the mechanical strength of the hollow fiber is low, and if the film thickness is 200μrr, the hollowness ratio is 8% or less, and the outer diameter is 5 or more, the ffs overefficiency is low and practical. Not on point. The hollowness ratio is determined by the microscopic appearance, the mean outer diameter Do and the mean inner diameter measured mechanically, and the hollowness ratio = (Ds/Do)"X
100 (s) and 11 scoops.

本発明に用いる微多孔含有する中空繊維は、ポ’J(p
−フェニレンスルフィド)を主成分とするものでろゐ。
The microporous hollow fiber used in the present invention is po'J (p
-phenylene sulfide) as the main component.

このような中空繊維は本出願人らの先細である%細昭5
7〜168446号に記載さ牡た方法によp製造するこ
とができる。
Such hollow fibers are tapered by Applicants.
It can be produced by the method described in No. 7-168446.

本発明のポリフェニレンスルフィドとは、ポリマーの主
構成単位としてフェニレンスルフィド?l1−90モル
慟以上に/(有したポリマーをいう。他eこ10モル悌
未満で含有できる構成単位としては、例えば、3′1能
フエニルスルフイドルケトンスルフイド、ジフェニルス
ルホンスルフィド、と(R:フルキル、フェニル、アル
コキシ、ニトロ、ハロゲン基のいづnか)等を例示でき
る。
The polyphenylene sulfide of the present invention is phenylene sulfide as the main constituent unit of the polymer? This refers to a polymer having 1-90 mol or more of mol. Examples include (R: any one of furkyl, phenyl, alkoxy, nitro, and halogen group).

ポリフェニレンスルフィドにブレンドできる他のポリマ
ーの嵐は65%未満である。他のポリマーが35%以上
を占めると、微多孔の形成、耐熱性、側薬品性、カ宇的
特性等のいづlしたに欠点が生じてポリフェニレンスル
フィドの特質が消えてくる。ブレンドできる他のポリマ
ーとしては、ポリエチレンテレフタレート、ポリブチレ
ンテレフタレート、ナイロン−6、ナイロン−66、ポ
リヵー・jζネート、ポリオキシメチレン、ボリフェニ
レンメキシド、ポリ−4−メチルベンゾン−1、ポリグ
ロピレン、ポリテトラフロロエチレン、ポリエーテルエ
ーテルケトン等の結晶性ポリマーや、ポリサルホン、ポ
リエーテルサルホン赫の非晶性ポリマーt−例示できる
。また、この様な原I+偏脂は、酸化防止剤、帯電防止
剤、抗#A剤、M剤、表面活性剤等の添加剤を必敦に応
じて適i合有することができる。
Less than 65% of other polymers can be blended with polyphenylene sulfide. If other polymers account for 35% or more, defects such as the formation of microporous, heat resistance, side chemical properties, and anti-oxidant properties will occur, and the characteristics of polyphenylene sulfide will disappear. Other polymers that can be blended include polyethylene terephthalate, polybutylene terephthalate, nylon-6, nylon-66, polycarbonate, polyoxymethylene, polyphenylene mexide, poly-4-methylbenzone-1, polyglopylene, and polytetrafluoro. Examples include crystalline polymers such as ethylene and polyetheretherketone, and amorphous polymers such as polysulfone and polyethersulfone. In addition, such raw I+ biased fat may contain additives such as antioxidants, antistatic agents, anti-#A agents, M agents, and surfactants as necessary.

本発明の無凶水の製造においては、耐熱性、劇薬品性の
優nたポリ(フェニレンスルフィド)を特徴とする特許
繊維を用いるため、酸、アルカリ、酸化剤等の化学薬剤
に↓る滅菌あるいは、80℃以上の熱水まfcは100
〜150℃のスチームで洗浄した後、1過操作を繰り返
し行なうことが出来る。また、該中空繊維は、耐熱性お
よび機械的強度が従来の分#膜に比べ優nあfcの、8
0〜150℃の加熱下での#J過> 10w′clT−
’以上の加圧下での1過などの効率的な1過操作を行な
うことができる。
In producing the non-toxic water of the present invention, we use a patented fiber that is characterized by poly(phenylene sulfide), which has excellent heat resistance and strong chemical resistance, so it is sterilized by chemical agents such as acids, alkalis, and oxidizing agents. Alternatively, fc of hot water over 80℃ is 100
After washing with steam at ~150°C, one pass operation can be repeated. In addition, the hollow fibers have heat resistance and mechanical strength superior to that of conventional membranes.
#J filtration >10w'clT- under heating at 0-150℃
It is possible to carry out an efficient one-pass operation such as one-pass operation under a pressure higher than '.

本発明の無菌水の製造方法は、紙・パルグ工業、化学工
業等の膨水の処理、医薬品・食品製造あるいは電子工業
等の工業用水の処理tはじめ、各種の除菌、水買改善操
作に適用することができる。
The method for producing sterile water of the present invention can be used to treat swelling water in the paper/pulg industry, chemical industry, etc., industrial water treatment in the pharmaceutical/food manufacturing industry, electronic industry, etc., as well as various sterilization and water purchasing improvement operations. Can be applied.

以下に本発明について実施例を示すが、本発明はこれに
Lりて制約さ扛るものではない。
Examples of the present invention are shown below, but the present invention is not limited to these.

実施例 1 井水を平均孔径o、o6iμ町空孔率35%、換部19
μm、中空率64qh、外径192μ扉のポリフェニレ
ンスルフィドの微多孔中空繊維モジュール(有効膜面積
1,2が)會用い、中空繊維の外側から内側に向けて圧
力6騰ろがで祐密F5過した。C過5時間後の透過水量
は500 IIが・hrであ九直接検鋭法によ?)測定
した除fiA率は100%であった。
Example 1 Well water was used with an average pore diameter of o, o6iμ, porosity of 35%, and exchange part 19.
A polyphenylene sulfide microporous hollow fiber module (effective membrane area 1, 2) with a door diameter of 64 qh and an outer diameter of 192 μm is used, and the pressure is increased by 6 from the outside to the inside of the hollow fiber with a dense F5 filter. did. The amount of permeated water after 5 hours of C is 500 hr. According to the direct probe method? ) The measured anti-fiA rate was 100%.

実施例 2 実施例1で用いたポリフェニレンスルフィドの数多孔中
空繊維膜t3%過酸化水素水お工ひ120℃スチームで
滅菌処理を行なった後、再ひ井水を圧力511−y/c
rrL”で精密P遇した。e過5時間後の透過水*ts
、50017m” −hr、 除7率は100%であハ
f過性能は滅劇処坤前と例ら変化がなかりた。
Example 2 A multi-porous hollow fiber membrane of polyphenylene sulfide used in Example 1 was sterilized with 3% hydrogen peroxide solution and steam at 120°C, and then the well water was drained again at a pressure of 511-y/c.
Precise treatment with rrL''.e Permeated water after 5 hours *ts
, 50,017 m''-hr, the 7% rate was 100%, and the overperformance was unchanged from before.

実施例 3 実施例2で用いたポリフェニレンスルフィドの敵多孔中
空繊維Mt−3%ホルマリン水および120℃スチーム
で滅菌処理を行なった後、井水を圧力1「14−で梢曽
f過し丸。1過5時間後の透過水量は15001/m”
・hrで、かり除蘭率は100%でおり、高圧下におい
ても膜の損傷はなく秀f′L、fC濾過性能を保持して
いることがわかった。
Example 3 After sterilizing the polyphenylene sulfide porous hollow fiber Mt used in Example 2 with 3% formalin water and 120°C steam, the well water was sterilized at a pressure of 1 to 14 mm. The amount of permeated water after 1 hour and 5 hours is 15001/m”
・The filter removal rate was 100% in hours, and it was found that even under high pressure, there was no damage to the membrane and excellent f'L and fC filtration performance was maintained.

1c埋人 弁理士高橋勝利1c Buried Patent Attorney Katsutoshi Takahashi

Claims (1)

【特許請求の範囲】 t 水中の菌を除去するに際し、平均孔径0.01〜1
μ、空孔率10〜85%の貫通した微多孔を有し膜厚5
〜200μm1 中空率8〜85%、外径30μWL〜
5寵のポリフェニレンスルフィドを主成分とする中空繊
維を用いてP遇することを特徴とする無菌水の製造方法
。 2 中空繊維が、化を薬剤で洗浄滅菌されたものである
ことを特徴とする特許請求の範囲第1項記載の製造方法
。 3、中空数86F=が、80℃以上の熱水または100
〜150℃のスチームで洗浄されたものであることを特
徴とする特許請求の範囲第1項記載の製造方法。
[Claims] t When removing bacteria in water, an average pore diameter of 0.01 to 1
μ, has penetrating micropores with a porosity of 10 to 85%, and a film thickness of 5
~200μm1 Hollow rate 8~85%, outer diameter 30μWL~
A method for producing sterile water, which comprises using hollow fibers containing polyphenylene sulfide as a main component. 2. The manufacturing method according to claim 1, wherein the hollow fibers are those that have been washed and sterilized with a chemical. 3. Hollow number 86F = hot water of 80℃ or higher or 100
2. The manufacturing method according to claim 1, wherein the product is washed with steam at a temperature of ~150°C.
JP59053845A 1984-03-21 1984-03-21 Preparation of aseptic water Pending JPS60197288A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP59053845A JPS60197288A (en) 1984-03-21 1984-03-21 Preparation of aseptic water

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP59053845A JPS60197288A (en) 1984-03-21 1984-03-21 Preparation of aseptic water

Publications (1)

Publication Number Publication Date
JPS60197288A true JPS60197288A (en) 1985-10-05

Family

ID=12954108

Family Applications (1)

Application Number Title Priority Date Filing Date
JP59053845A Pending JPS60197288A (en) 1984-03-21 1984-03-21 Preparation of aseptic water

Country Status (1)

Country Link
JP (1) JPS60197288A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0441340A2 (en) * 1990-02-07 1991-08-14 House Food Industrial Co., Ltd. Method for preparing packaged sterilized mineral water and packaged sterilized mineral water
US5049276A (en) * 1988-10-13 1991-09-17 Fuji Photo Film Co., Ltd. Hollow fiber membrane
CN112609254A (en) * 2020-12-10 2021-04-06 广东宝泓新材料股份有限公司 Preparation method of polyphenylene sulfide pulp fiber

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS57159587A (en) * 1981-03-27 1982-10-01 Asahi Chem Ind Co Ltd Sterilization and purification of water
JPS57171403A (en) * 1981-04-15 1982-10-22 Mitsubishi Rayon Co Ltd Removal of pyrogen in water
JPS5867733A (en) * 1981-10-19 1983-04-22 Dainippon Ink & Chem Inc Microporous film and its preparation

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS57159587A (en) * 1981-03-27 1982-10-01 Asahi Chem Ind Co Ltd Sterilization and purification of water
JPS57171403A (en) * 1981-04-15 1982-10-22 Mitsubishi Rayon Co Ltd Removal of pyrogen in water
JPS5867733A (en) * 1981-10-19 1983-04-22 Dainippon Ink & Chem Inc Microporous film and its preparation

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5049276A (en) * 1988-10-13 1991-09-17 Fuji Photo Film Co., Ltd. Hollow fiber membrane
EP0441340A2 (en) * 1990-02-07 1991-08-14 House Food Industrial Co., Ltd. Method for preparing packaged sterilized mineral water and packaged sterilized mineral water
EP0441340A3 (en) * 1990-02-07 1991-11-27 House Food Industrial Co., Ltd. Method for preparing packaged sterilized mineral water, method for producing sterilized container for packaging the same and packaged sterilized mineral water
US5152900A (en) * 1990-02-07 1992-10-06 House Food Industrial Co., Ltd. Method for preparing packaged sterilized mineral water, method for producing sterilized container for packaging the same and packaged sterilized mineral water
CN112609254A (en) * 2020-12-10 2021-04-06 广东宝泓新材料股份有限公司 Preparation method of polyphenylene sulfide pulp fiber

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