JPH11216344A - Manufacture of polyamide-imide separation membrane - Google Patents
Manufacture of polyamide-imide separation membraneInfo
- Publication number
- JPH11216344A JPH11216344A JP3545198A JP3545198A JPH11216344A JP H11216344 A JPH11216344 A JP H11216344A JP 3545198 A JP3545198 A JP 3545198A JP 3545198 A JP3545198 A JP 3545198A JP H11216344 A JPH11216344 A JP H11216344A
- Authority
- JP
- Japan
- Prior art keywords
- solvent
- water
- separation membrane
- polyamideimide
- polyetherimide
- 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
Links
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、ポリアミドイミド
分離膜の製造方法に関する。更に詳しくは分離膜の表面
開口率を所定の範囲で設定可能とする製造方法である。The present invention relates to a method for producing a polyamideimide separation membrane. More specifically, it is a manufacturing method in which the surface aperture ratio of the separation membrane can be set within a predetermined range.
【０００２】[0002]
【従来の技術】ポリアミドイミドをその良溶媒に溶解さ
せて得られる均一溶液を基盤上に流延し、これを凝固浴
中に浸漬することによって得られる膜は、精密濾過膜、
限外濾過膜などの分離膜としての性能を有する。2. Description of the Related Art A uniform solution obtained by dissolving polyamideimide in a good solvent is cast on a substrate, and the resulting solution is immersed in a coagulation bath.
It has performance as a separation membrane such as an ultrafiltration membrane.
【０００３】さらにこの分離膜に対して加熱処理を施す
ことにより、著しく耐溶剤性能および膜強度が向上す
る。しかしこの時の膜は、水透過性の点では全く満足さ
れないものしか得られない。Further, by subjecting this separation membrane to a heat treatment, the solvent resistance and the membrane strength are remarkably improved. However, at this time, only a film which is not completely satisfied in terms of water permeability can be obtained.
【０００４】そこで、水透過性にすぐれた耐溶剤性分離
膜の製造方法として、ポリアミドイミドおよびそれと相
溶性を有する非水溶性添加剤が溶解した均一溶液から調
製した膜状物を熱処理した後、非水溶性添加剤の可溶性
溶剤でそれの抽出を行って分離膜を得る方法が提案され
ている（本発明と同じ出願人による特願平８−２１７９
８６号、特願平９−１９４９２３号参照）。[0004] Therefore, as a method for producing a solvent-resistant separation membrane having excellent water permeability, a membrane-like material prepared from a homogeneous solution in which polyamideimide and a water-insoluble additive compatible therewith are dissolved is heat-treated. There has been proposed a method of obtaining a separation membrane by extracting the same with a soluble solvent of a water-insoluble additive (Japanese Patent Application No. Hei 8-2179 by the same applicant as the present invention).
No. 86, Japanese Patent Application No. 9-194923).
【０００５】[0005]
【発明が解決しようとする課題】上記の方法により得ら
れた水透過性にすぐれた耐溶剤性分離膜において、さら
にこの分離膜の応用／適用範囲を広げることを可能とす
るために、膜表面の平均孔径ならびに開孔率を所望の値
に設定し、分画性能を向上させることが要求されてい
た。In the solvent-resistant separation membrane having excellent water permeability obtained by the above-mentioned method, the surface of the membrane is intended to be able to further expand the application / application range of the separation membrane. It has been required that the average pore diameter and the opening ratio be set to desired values to improve the fractionation performance.
【０００６】本発明は上記従来技術における問題を解決
するためになされたもので、その目的とするところは、
耐溶剤性及び高い水透過性を維持しつつ膜表面の平均孔
径及び開孔率を自由に設定可能とすることにより、優れ
た分画性能を有するポリアミドイミド分離膜の製造方法
を提供することにある。SUMMARY OF THE INVENTION The present invention has been made to solve the above-mentioned problems in the prior art.
To provide a method for producing a polyamideimide separation membrane having excellent fractionation performance by freely setting the average pore size and porosity of the membrane surface while maintaining solvent resistance and high water permeability. is there.
【０００７】[0007]
【課題を解決するための手段】上記目的を達成するため
に本発明にあっては、ポリアミドイミド及びポリアミド
イミドと相溶性を有する非水溶性添加剤をそれらの良溶
媒に溶解させ、さらに貧溶媒を相分離の生じない範囲で
添加した均一溶液から膜状物を成膜し、前記膜状物を約
３００〜４８０℃の温度条件下で熱処理した後、非水溶
性添加剤の可溶性溶剤で非水溶性添加剤の抽出を行なう
ことを特徴とする。According to the present invention, in order to achieve the above object, a polyamideimide and a water-insoluble additive compatible with the polyamideimide are dissolved in a good solvent thereof, and the poor solvent is further dissolved. Is formed from a uniform solution in which is added within a range that does not cause phase separation, and the film is heat-treated at a temperature of about 300 to 480 ° C. It is characterized in that the water-soluble additive is extracted.
【０００８】また、ポリアミドイミド及びポリエーテル
イミドをそれらの良溶媒に溶解させ、さらに貧溶媒を相
分離の生じない範囲で添加した均一溶液から膜状物を成
膜し、前記膜状物を約３００〜３４０℃の温度条件下で
熱処理した後、ポリエーテルイミドの可溶性溶剤でポリ
エーテルイミドの抽出を行なうことを特徴とする。Further, a film is formed from a homogeneous solution in which polyamideimide and polyetherimide are dissolved in a good solvent thereof, and a poor solvent is added within a range that does not cause phase separation. After heat treatment at a temperature of 300 to 340 ° C., extraction of the polyetherimide with a soluble solvent for the polyetherimide is performed.
【０００９】また、ポリアミドイミド５〜８重量％及び
ポリエーテルイミド８〜１２重量％となるようにそれら
の良溶媒に溶解させ、さらに貧溶媒を０．０１〜０．８
重量％で添加した均一溶液から膜状物を成膜し、前記膜
状物を約３００〜３４０℃の温度条件下で熱処理した
後、ポリエーテルイミドの可溶性溶剤でポリエーテルイ
ミドの抽出を行なうことを特徴とする。Further, the polyamideimide is dissolved in a good solvent so as to be 5 to 8% by weight and the polyetherimide to be 8 to 12% by weight.
Forming a film from a uniform solution added at a weight%, heat-treating the film under a temperature condition of about 300 to 340 ° C., and extracting polyetherimide with a soluble solvent of polyetherimide. It is characterized by.
【００１０】さらに、分離膜の平均孔径及び表面開口率
を前記貧溶媒の添加量に応じて設定することを特徴とす
ることも好適である。Further, it is preferable that the average pore diameter and the surface aperture ratio of the separation membrane are set according to the amount of the poor solvent added.
【００１１】このような製造法により、耐溶剤性及び高
い水透過性を維持しつつ膜表面の平均孔径及び開孔率を
自由に設定可能とすることにより、優れた分画性能を有
するポリアミドイミド分離膜が得られる。According to such a production method, a polyamideimide having excellent fractionation performance can be obtained by freely setting an average pore diameter and a pore ratio of a membrane surface while maintaining solvent resistance and high water permeability. A separation membrane is obtained.
【００１２】[0012]
【発明の実施の形態】（実施の形態１）本発明を適用し
た第１の実施の形態におけるポリアミドイミド分離膜の
製造方法を以下に説明する。(Embodiment 1) A method for manufacturing a polyamideimide separation membrane according to a first embodiment of the present invention will be described below.
【００１３】まず、ポリアミドイミド分離膜を成膜する
ための溶液の組成から説明する。First, the composition of a solution for forming a polyamideimide separation membrane will be described.
【００１４】ポリアミドイミドとしては、アモコ・ジャ
パン製品トーロン４０００Ｔ（製品名）等の市販品をそ
のまま用いることができる。As the polyamideimide, a commercially available product such as Amolco Japan's Tolon 4000T (product name) can be used as it is.
【００１５】また、ポリアミドイミドと相溶性を有する
非水溶性添加剤としては、溶解度パラメーターδ（ｃａ
ｌ1/2 ・ｃｍ-3/2）が１０〜１７の範囲内のもの、例え
ばポリエーテルスルホン、ポリエーテルイミド、ポリア
リレート等が用いられる。The non-water-soluble additive compatible with polyamideimide includes a solubility parameter δ (ca).
l 1/2 · cm -3/2 ) in the range of 10 to 17, for example, polyethersulfone, polyetherimide, polyarylate and the like are used.
【００１６】以上の各成分は、これらの共通の良溶媒で
あるジメチルホルムアミド、ジメチルアセトアミド、ジ
エチルホルムアミド、ジエチルアセトアミド、Ｎ−メチ
ルピロリドン、モルホリン、ジオキサン等の有機溶媒、
好ましくは非プロトン性極性溶媒中に均一に溶解させた
均一溶液に調整される。Each of the above-mentioned components is an organic solvent such as dimethylformamide, dimethylacetamide, diethylformamide, diethylacetamide, N-methylpyrrolidone, morpholine and dioxane, which are common good solvents.
It is preferably adjusted to a homogeneous solution uniformly dissolved in an aprotic polar solvent.
【００１７】さらに、この均一溶液に少なくとも１種の
貧溶媒を相分離を生じない範囲で添加させる。Further, at least one poor solvent is added to the homogeneous solution as long as phase separation does not occur.
【００１８】貧溶媒としては、水、メタノール、エタノ
ール、プロパノール、ブタノール、アセトン、ポリビニ
ルピロリドン等が、好ましくは水、メタノール、エタノ
ールが挙げられる。この貧溶媒を、均一溶液の重量に対
して０．０１％から均一溶液が相分離を生じない範囲で
添加する。Examples of the poor solvent include water, methanol, ethanol, propanol, butanol, acetone, polyvinylpyrrolidone and the like, preferably water, methanol and ethanol. The poor solvent is added within a range from 0.01% to the weight of the homogeneous solution so that the homogeneous solution does not cause phase separation.
【００１９】このように調整した均一溶液を基盤上に流
延し、これを凝固浴中に浸漬（及び乾燥）することによ
って成膜する。基盤としては、ガラス板、金属板等が用
いられ、また凝固浴としては一般に水が用いられるが、
そこに水溶性物質あるいは水溶性溶媒を加えた水溶液で
あってもよい。The uniform solution thus prepared is cast on a substrate, and immersed (and dried) in a coagulation bath to form a film. A glass plate, a metal plate, or the like is used as a base, and water is generally used as a coagulation bath.
It may be an aqueous solution to which a water-soluble substance or a water-soluble solvent is added.
【００２０】尚、この成膜工程は上記された方法に限定
されるものではなく、遠心流延や中空糸膜を形成するた
めの二重管吐出法等その他の成膜工程を採用することも
適宜行なうことができる。This film forming step is not limited to the above-mentioned method, and other film forming steps such as a centrifugal casting method and a double tube discharging method for forming a hollow fiber membrane may be employed. It can be performed appropriately.
【００２１】そして、この膜を約３００〜４８０℃、非
水溶性添加剤としてポリエーテルイミドを採用した場合
には約３００〜３４０℃の温度条件で熱処理した後、非
水溶性添加剤の可溶性溶剤でそれの抽出を行って耐溶剤
性を備えたポリアミドイミド分離膜を製造する。Then, this film is heat-treated at a temperature of about 300 to 480 ° C. and about 300 to 340 ° C. when polyetherimide is used as the water-insoluble additive, and then the soluble solvent of the water-insoluble additive is added. To produce a polyamideimide separation membrane having solvent resistance.
【００２２】可溶性溶剤としては、例えば非水溶性添加
剤としてポリエーテルイミドやポリエーテルスルホンが
用いられた場合には、クロロホルム、塩化メチレン等に
よる抽出が行なわれる。As a soluble solvent, for example, when polyetherimide or polyethersulfone is used as a water-insoluble additive, extraction with chloroform, methylene chloride, or the like is performed.
【００２３】この他に可溶性溶剤としては、Ｎ−メチル
−２−ピロリドン、ジメチルホルムアミド、ジメチルア
セトアミド等も用いられる。抽出は、約２０〜５０℃の
温度で２〜１００時間程度膜を可溶性溶剤中に浸漬する
ことにより行なわれる。In addition, N-methyl-2-pyrrolidone, dimethylformamide, dimethylacetamide and the like can be used as the soluble solvent. The extraction is performed by immersing the membrane in a soluble solvent at a temperature of about 20 to 50 ° C. for about 2 to 100 hours.
【００２４】このような方法により、ポリアミドイミド
分離膜が得られる。そして、上記したような均一溶液に
相分離を生じない範囲で添加される貧溶媒の種類や添加
量に応じて、分離膜の平均孔径及び表面開口率を所定範
囲で設定することが可能となり、優れた分画性能を有す
るポリアミドイミド分離膜が得られる。By such a method, a polyamideimide separation membrane is obtained. Then, depending on the type and amount of the poor solvent added in a range that does not cause phase separation in the uniform solution as described above, it becomes possible to set the average pore diameter and the surface aperture ratio of the separation membrane in a predetermined range, A polyamideimide separation membrane having excellent fractionation performance can be obtained.
【００２５】（実施の形態２）次に、第２の実施の形態
としてより具体的な実施の形態を以下に説明する。(Embodiment 2) Next, a more specific embodiment will be described as a second embodiment.
【００２６】ポリアミドイミド（アモコ・ジャパン製品
トーロン４０００Ｔ）とポリエーテルイミド（ＧＥプラ
スチック・ジャパン製品ウルテム１０００）とジメチル
アセトアミドを重量比率がポリアミドイミド／ポリエー
テルイミド／ジメチルアセトイミド＝６．４重量％／
９．６重量％／８４．０重量％となるように混合し、均
一溶液とした。Polyamideimide (Toron 4000T manufactured by Amoco Japan), polyetherimide (Ultem 1000 manufactured by GE Plastics Japan), and dimethylacetamide were used in a weight ratio of polyamideimide / polyetherimide / dimethylacetimide = 6.4% by weight /
The mixture was mixed so as to be 9.6% by weight / 84.0% by weight to obtain a uniform solution.
【００２７】その後、貧溶媒として水を均一溶液の重量
に対して、０．０〜０．８重量％となるように加えた。
ちなみに、水添加量が０．８５重量％では、均一溶液が
白濁化し相分離を生じていることが確認された。Thereafter, water was added as a poor solvent in an amount of 0.0 to 0.8% by weight based on the weight of the homogeneous solution.
Incidentally, when the amount of water added was 0.85% by weight, it was confirmed that the homogeneous solution became cloudy and phase separation occurred.
【００２８】得られた均一溶液を室温条件下でガラス基
板上に流延し、これを水中に浸漬して凝固させ、膜厚約
６０μｍのポリアミドイミドとポリエーテルイミドの混
合膜を得た。The obtained homogeneous solution was cast on a glass substrate at room temperature, immersed in water and solidified to obtain a mixed film of polyamideimide and polyetherimide having a thickness of about 60 μm.
【００２９】この混合膜を３２０℃で３時間熱処理した
後、クロロホルム中に５時間浸漬することによりポリエ
ーテルイミドを抽出し、膜厚４０μｍのポリアミドイミ
ド分離膜を得た。After heat treating the mixed film at 320 ° C. for 3 hours, the polyetherimide was extracted by immersing it in chloroform for 5 hours to obtain a polyamideimide separation film having a thickness of 40 μm.
【００３０】各水添加量において得られたポリアミドイ
ミド分離膜の表面平均孔径、表面の開孔率、ならびに印
加圧１ｋｇ／ｃｍ2 の条件下での全量透過方式によって
測定した純水透過係数を表１に示す。The average pore diameter of the surface of the polyamide-imide separation membrane obtained at each amount of water added, the porosity of the surface, and the permeability coefficient of pure water measured by the total amount permeation method under the conditions of an applied pressure of 1 kg / cm 2 are shown in Table 1. It is shown in FIG.
【００３１】[0031]
【表１】 この表によると、膜表面の平均孔径は、貧溶媒としての
水の添加量が０では０．１６（μｍ）であり、水の添加
量の増加に応じて平均孔径も増加し、水の添加量が０／
８では０．３５（μｍ）となっている。[Table 1] According to this table, the average pore size on the membrane surface is 0.16 (μm) when the amount of water as a poor solvent is 0, and the average pore size increases with an increase in the amount of water added. 0 /
8 is 0.35 (μm).
【００３２】また、同様に表面開孔率も４．５から８．
５（％）へと水の添加量の増加に応じて増加している。Similarly, the surface porosity is 4.5 to 8.
It increased to 5 (%) with an increase in the amount of water added.
【００３３】従って、水の添加量を０、０．２、０．
４、０．６、０．８と適宜変化させることにより、目的
とする膜表面の平均孔径及び表面開孔率を備えたポリア
ミドイミド分離膜を得ることが可能となる。Therefore, the added amount of water is set to 0, 0.2, 0.
By appropriately changing it to 4, 0.6, and 0.8, it becomes possible to obtain a polyamide-imide separation membrane having an intended average pore diameter and surface porosity on the membrane surface.
【００３４】尚、得られたポリアミドイミド分離膜を室
温条件下のジメチルホルムアミド中に１００ｈ時間浸漬
したが、水添加量に依らず膜形状に全く変化は見られ
ず、引張り試験における破断応力は浸漬前と同様に１．
０ｋｇｆ／ｃｍ2 であった。The obtained polyamideimide separation membrane was immersed in dimethylformamide at room temperature for 100 hours, but no change was observed in the membrane shape regardless of the amount of water added. As before 1.
It was 0 kgf / cm 2 .
【００３５】これに対して、貧溶媒の添加されていない
均一溶液から調製した未加熱状態の混合膜は室温条件下
のジメチルホルムアミドに可溶であった。また、この混
合膜を３２０℃で３時間熱処理した膜は、室温条件下の
ジメチルホルムアミド中に１００時間の浸漬を行ったと
ころ浸漬前後において膜形状ならびに破断応力に変化は
見られなかったが、純水を全く透過することがなかっ
た。On the other hand, the unheated mixed film prepared from the homogeneous solution to which the poor solvent was not added was soluble in dimethylformamide at room temperature. When the mixed film was heat-treated at 320 ° C. for 3 hours, it was immersed in dimethylformamide at room temperature for 100 hours. No water was permeated.
【００３６】[0036]
【発明の効果】上記発明の実施の形態に説明されたよう
に、耐溶剤性及び高い水透過性を維持しつつ膜表面の平
均孔径及び開孔率を所定の範囲で自由に設定可能とする
ことができ、優れた分画性能を有するポリアミドイミド
分離膜が得られる。As described in the embodiments of the present invention, it is possible to freely set the average pore diameter and the porosity of the membrane surface within a predetermined range while maintaining solvent resistance and high water permeability. As a result, a polyamideimide separation membrane having excellent fractionation performance can be obtained.
Claims (4)
と相溶性を有する非水溶性添加剤をそれらの良溶媒に溶
解させ、さらに貧溶媒を相分離の生じない範囲で添加し
た均一溶液から膜状物を成膜し、 前記膜状物を約３００〜４８０℃の温度条件下で熱処理
した後、非水溶性添加剤の可溶性溶剤で非水溶性添加剤
の抽出を行なうことを特徴とするポリアミドイミド分離
膜の製造方法。1. A film-like substance is formed from a homogeneous solution in which a polyamideimide and a water-insoluble additive compatible with the polyamideimide are dissolved in a good solvent thereof, and a poor solvent is added to such an extent that phase separation does not occur. A polyamide-imide separation membrane, wherein the membrane-like material is heat-treated at a temperature of about 300 to 480 ° C., and then the water-insoluble additive is extracted with a soluble solvent of the water-insoluble additive. Production method.
ドをそれらの良溶媒に溶解させ、さらに貧溶媒を相分離
の生じない範囲で添加した均一溶液から膜状物を成膜
し、 前記膜状物を約３００〜３４０℃の温度条件下で熱処理
した後、ポリエーテルイミドの可溶性溶剤でポリエーテ
ルイミドの抽出を行なうことを特徴とするポリアミドイ
ミド分離膜の製造方法。2. A film-like substance is formed from a uniform solution in which polyamideimide and polyetherimide are dissolved in a good solvent thereof, and a poor solvent is added within a range that does not cause phase separation. A method for producing a polyamideimide separation membrane, comprising heat-treating at a temperature of 300 to 340 ° C and extracting polyetherimide with a soluble solvent of polyetherimide.
エーテルイミド８〜１２重量％となるようにそれらの良
溶媒に溶解させ、さらに貧溶媒を０．０１〜０．８重量
％で添加した均一溶液から膜状物を成膜し、 前記膜状物を約３００〜３４０℃の温度条件下で熱処理
した後、ポリエーテルイミドの可溶性溶剤でポリエーテ
ルイミドの抽出を行なうことを特徴とするポリアミドイ
ミド分離膜の製造方法。3. A homogeneous solution prepared by dissolving a polyamideimide in 5 to 8% by weight and a polyetherimide in 8 to 12% by weight in a good solvent and further adding a poor solvent in 0.01 to 0.8% by weight. Forming a film from a solution; heat treating the film under a temperature condition of about 300 to 340 ° C .; and extracting polyetherimide with a soluble solvent of polyetherimide. A method for producing a separation membrane.
貧溶媒の添加量に応じて設定することを特徴とする請求
項１乃至３のいずれか１項に記載のポリアミドイミド分
離膜の製造方法。4. The production of a polyamide-imide separation membrane according to claim 1, wherein the average pore diameter and the surface opening ratio of the separation membrane are set according to the amount of the poor solvent added. Method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP03545198A JP3369950B2 (en) | 1998-02-02 | 1998-02-02 | Method for producing polyamide-imide separation membrane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP03545198A JP3369950B2 (en) | 1998-02-02 | 1998-02-02 | Method for producing polyamide-imide separation membrane |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH11216344A true JPH11216344A (en) | 1999-08-10 |
| JP3369950B2 JP3369950B2 (en) | 2003-01-20 |
Family
ID=12442183
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP03545198A Expired - Fee Related JP3369950B2 (en) | 1998-02-02 | 1998-02-02 | Method for producing polyamide-imide separation membrane |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3369950B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101317641B1 (en) * | 2010-12-29 | 2013-10-15 | 웅진케미칼 주식회사 | Manufacturing method of polyamideimide-based porous membrane |
| CN110548422A (en) * | 2019-08-27 | 2019-12-10 | 武汉艾科滤膜技术有限公司 | Organic solvent-resistant ultrafiltration membrane and preparation method and application thereof |
-
1998
- 1998-02-02 JP JP03545198A patent/JP3369950B2/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR101317641B1 (en) * | 2010-12-29 | 2013-10-15 | 웅진케미칼 주식회사 | Manufacturing method of polyamideimide-based porous membrane |
| CN110548422A (en) * | 2019-08-27 | 2019-12-10 | 武汉艾科滤膜技术有限公司 | Organic solvent-resistant ultrafiltration membrane and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3369950B2 (en) | 2003-01-20 |
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