KR20200075347A - Hollow fiber type nanofiltration membrane module having high salt rejection and manufacturing method thereof - Google Patents
Hollow fiber type nanofiltration membrane module having high salt rejection and manufacturing method thereof Download PDFInfo
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Abstract
Description
본 발명은 다가의 음이온이나 유기물을 선택적으로 분리 효율이 우수한 특성을 갖는 중공사형 나노분리막 모듈에 관한 것이다. 보다 상세하게는 중공사형 한외여과막 모듈에 계면중합막을 균일하게 코팅함으로써 염배제율이 우수한 중공사형 나노여과막 모듈의 제조방법에 관한 것이다.The present invention relates to a hollow fiber-type nano-separation membrane module having a property of selectively separating polyvalent anions or organics and having excellent separation efficiency. More specifically, the present invention relates to a method for manufacturing a hollow fiber type nanofiltration membrane module having excellent salt rejection rate by uniformly coating an interfacial polymerization membrane on a hollow fiber type ultrafiltration membrane module.
분리하려는 대상물질의 상태에 따른 분류방법은 크게 정밀여과(Microfiltration), 한외여과(Ultrafiltration), 나노여과(Nanofiltration),역삼투(Reverse osmosis)가 있는데, 기공에 크기에 따라서 분리막을 통과하는 속도 차에 의해 부유물질, 박테리아를 제거하는 정밀여과, 현탁물질이나 단백질, 다당류, 고분자물질을 제거하는 한외여과, 다가이온이나 유기물을 선택적으로 분리하는 나노여과, 이온성 물질 또는 중금속 등을 분리하는 역삼투막이 있다.The classification method according to the state of the target material to be separated is largely classified into microfiltration, ultrafiltration, nanofiltration, and reverse osmosis. Microfiltration to remove suspended solids and bacteria, ultrafiltration to remove suspended substances, proteins, polysaccharides, and polymers, nanofiltration to selectively separate polyions or organics, reverse osmosis membranes to separate ionic or heavy metals have.
나노여과막은 역삼투(RO)와 한외여과(UF)막의 중간 특성을 갖는 영역으로 RO막과 구조, 제조방법, 사용법 등에서 유사한 특징을 가진다. The nanofiltration membrane is a region having an intermediate characteristic between a reverse osmosis (RO) and an ultrafiltration (UF) membrane and has similar characteristics in terms of the RO membrane, structure, manufacturing method, and usage.
통상 0.5∼2.0 nm 사이의 크기이며, 낮은 투자비와 낮은 운전압력, 높은 투과성능, 다가 음이온 염과 200∼1000 gmol- 1사이의 유기물에 대한 높은 제거율을 가진다.The normal size of between 0.5~2.0 nm, low investment cost and low operating pressure, a high permeability, polyvalent anion salts and 200~1000 gmol - has a high removal rate of the organic material between the first.
중공사형 모듈은 평막형, 나권형 모듈에 비하여 단위부피당 막 면적의 비율이 가장 높다는 장점이 있으며 어떤 형태의 모듈보다 장치 소형화에 유리하다.The hollow fiber type module has the advantage that the ratio of the membrane area per unit volume is the highest compared to the flat membrane type or the spiral type module, and is advantageous for miniaturization of the device over any type of module.
주된 분리대상은 용질의 크기가 10 Å보다 약간 큰 즉, 나노미터(nm)의 크기를 갖는 2가 이온, 각종 단당류와 저 분자량의 유기물로써, 오염도가 낮은 물 또는 우유 등의 낙농산업에서의 특수 가공, 항생물질 분리, 단당류 분리 등에서 탁월한 선택적 분리 능력을 보인다.The main separation targets are divalent ions having a size of nanometer (nm) slightly larger than 10 Å, various monosaccharides, and low molecular weight organic substances. Special in dairy industry such as low-contamination water or milk Excellent selective separation ability in processing, separation of antibiotics, separation of monosaccharides, etc.
나노여과막을 제조하기 위한 방법으로으로 상전이법으로 비대칭 단일막을 제조하거나 다공성지지체 위에 계면중합을 일으켜 얇은 활성층을 제조하는 복합막형태로 제조되고 있다. 이러한 계면중합법은 낮은 염배제율이 문제점으로 지적되고 있으며 향상시키기위한 연구들이 진행되고 있다. As a method for manufacturing a nanofiltration membrane, an asymmetric single membrane is prepared by a phase transfer method or an interfacial polymerization is performed on a porous support to produce a thin active layer. In the interfacial polymerization method, a low salt rejection rate has been pointed out as a problem, and studies are being conducted to improve it.
본 발명에서는 이러한 계면중합법을 이용한 나노여과막 모듈의 낮은 염배제율을 해결하기 위한 것으로 중공사형 모듈내의 중공섬유에 균일한 계면중합을 통하여 우수한 염배제율을 갖는 중공사형 나노여과막 모듈을 제조가 가능한 발명이다.In the present invention, to solve the low salt rejection rate of the nanofiltration membrane module using the interfacial polymerization method, it is possible to manufacture a hollow fiber nanofiltration membrane module having excellent salt rejection rate through uniform interfacial polymerization of hollow fibers in the hollow fiber module. It is an invention.
중공사형 한외여과막 모듈을 제조하고 아민 수용액을 함침 후 과량의 아민 수용액을 제거하는 방법에 있어서 건조된 공기로 한외여과막 내부와 외부에 블로윙 할 때 압력을 동일하게 유지시켜줌으로써 중공 내부의 기공에 균일하게 도포함으로써 계면중합막이 흠집(Defect)이 없어 염배제율이 우수한 중공사형 나노여과막 모듈이 제조가 가능한 방법을 제공한다.In the method of manufacturing a hollow fiber type ultrafiltration membrane module and impregnating the amine aqueous solution, and then removing the excess amine aqueous solution, the pressure in the inside and outside of the ultrafiltration membrane is maintained uniformly in the pores of the inside of the hollow by drying air. It provides a method capable of manufacturing a hollow fiber nanofiltration membrane module having an excellent salt rejection rate because the interfacial polymerization membrane is not defective by application.
본 발명은 중공사형 모듈 내부에 균일한 계면중합막을 코팅하여 염배제율이 우수한 중공사형 나노여과막이 제조가 가능하다.The present invention can manufacture a hollow fiber-type nanofiltration membrane having excellent salt rejection by coating a uniform interfacial polymerization membrane inside the hollow fiber-type module.
이하에 본 발명을 상세하게 설명하기에 앞서, 본 명세서에 사용된 용어는 특정의 실시예를 기술하기 위한 것일 뿐 첨부하는 특허청구의 범위에 의해서만 한정되는 본 발명의 범위를 한정하려는 것은 아님을 이해하여야 한다. 본 명세서에 사용되는 모든 기술용어 및 과학용어는 다른 언급이 없는 한은 기술적으로 통상의 기술을 가진 자에게 일반적으로 이해되는 것과 동일한 의미를 가진다.Before describing the present invention in detail below, it is understood that the terms used herein are only for describing specific embodiments and are not intended to limit the scope of the present invention, which is limited only by the scope of the appended claims. shall. All technical and scientific terms used in this specification have the same meaning as commonly understood by those skilled in the art unless otherwise stated.
본 명세서 및 청구범위의 전반에 걸쳐, 다른 언급이 없는 한 포함(comprise, comprises, comprising)이라는 용어는 언급된 물건, 단계 또는 일군의 물건, 및 단계를 포함하는 것을 의미하고, 임의의 어떤 다른 물건, 단계 또는 일군의 물건 또는 일군의 단계를 배제하는 의미로 사용된 것은 아니다.Throughout this specification and claims, unless otherwise stated, the terms comprise, comprises, comprising means referring to an article, step or group of articles, and steps, and any other article It is not meant to exclude a step or group of things or a group of steps.
한편, 본 발명의 여러 가지 실시예들은 명확한 반대의 지적이 없는 한 그 외의 어떤 다른 실시예들과 결합될 수 있다. 특히 바람직하거나 유리하다고 지시하는 어떤 특징도 바람직하거나 유리하다고 지시한 그 외의 어떤 특징 및 특징들과 결합될 수 있다.On the other hand, various embodiments of the present invention can be combined with any other embodiments, unless otherwise indicated. Any feature indicated as particularly preferred or advantageous may be combined with any other feature or features indicated as preferred or advantageous.
본 발명의 일측면은,One aspect of the present invention,
(1) 폴리아클리로니트릴를 포함하는 방사원액과 내부응고제를 포함하여 방사노즐을 통해 방사 한 후 외부응고제로 침지시켜 중공사형태의 다공성 한외여과막(UF) 지지체를 방사하여 중공사 모듈을 제조하는 단계;(1) A step of manufacturing a hollow fiber module by spinning a porous ultrafiltration membrane (UF) support in the form of a hollow fiber by spinning through a spinning nozzle, including a spinning stock solution containing polyacrylonitrile and an internal coagulant, and then immersing with an external coagulant. ;
(2) 상기 제조된 중공사 지지체에 포함된 용매 및 내부응고액을 세척하는 단계: 40℃, DI 48hr(2) washing the solvent and the internal coagulation solution contained in the prepared hollow fiber support: 40℃, DI 48hr
(3) 상기 제조된 중공사 지지체 내부에 다관능성 아민 수용액을 침지하는 단계: 정량펌프로 공급, 모듈상부에 아민 Gravity Force, (3) immersing the polyfunctional amine aqueous solution inside the prepared hollow fiber support: supplied with a metering pump, amine Gravity Force on the module top,
(4) 상기 중공사 지지체 내부에 주입된 과량의 다관능성 아민수용액을 제거하는 단계: 중공사 내부/외부에 동일압력으로 에어로 주입, 버블포인트 이하의 압력으로 제거, 장시간 제거시 기화됨(4) Step of removing the excess polyfunctional amine aqueous solution injected into the hollow fiber support: air injection at the same pressure inside/outside the hollow fiber, removal at a pressure below the bubble point, vaporization when removed for a long time
(5) 다관능성 산할로겐화합물을 포함하는 유기용액과 접촉하여 폴리아미드층을 형성시키는 단계: 접촉시간, 건조방법(5) Forming a polyamide layer by contacting with an organic solution containing a polyfunctional acid halide compound: contact time, drying method
(6) 상기 제조된 나노중공사 분리막 모듈은 유량이 28GFD, 93%염배제율을 갖는 중공사형 나노분리막 모듈의 제조방법을 제공한다. (6) The prepared nano hollow fiber separator module provides a method for manufacturing a hollow fiber type nano separator module having a flow rate of 28 GFD and a salt removal rate of 93%.
이 때, 상기 (1)단계는At this time, step (1) is
방사원액에 사용되는 고분자 물질은 폴리아크릴로니트릴(PAN), 폴리아크릴로니트릴 공중합체중 하나로 선택되고 유기성 용매 및 내부응고제로는 N-메틸-2-피롤리디온(NMP)인 것을 특징으로하는 고염배제율을 갖는다. The high molecular salt used in the spinning dope is selected from polyacrylonitrile (PAN) and polyacrylonitrile copolymers, and is an organic solvent and an internal coagulant characterized by N-methyl-2-pyrrolidion (NMP). Has an exclusion rate.
또한, 상기 (2)단계는, In addition, the step (2),
상기 중공사형태의 한외여과막(UF)에 잔류하고 있는 용매 및 내부응고제를 초순수로 30℃ ~ 40℃로 중공 내부와 외부를 48hr 동안 세척하는 단계이다. It is a step of washing the inside and the outside of the hollow with ultrapure water at 30°C to 40°C for 48hr with the solvent and internal coagulant remaining in the hollow fiber membrane ultrafiltration membrane (UF).
또한, 상기 (3)단계는 ,In addition, step (3) is,
상기 중공 내부에 다관능성 아민은 피페라진,메타페닐렌디아민, 디페닐디아민, 파라페닐렌디아민으로 이루어진 군으로부터 선택되는 1종 이상을 포함한다. The polyfunctional amine in the hollow contains at least one member selected from the group consisting of piperazine, metaphenylenediamine, diphenyldiamine, and paraphenylenediamine.
또한, 상기 (3)단계는, In addition, the step (3),
상기 중공 내부에 다관능성 아민을 침지시키는 방법으로는 모듈 내부에 중공사 내부 부피의 1.2배의 다관능성 아민을 수직방향으로 중력(Gravity Force)에 의해 지지체 기공에 함침시키는 것을 특징으로 한다. As a method of immersing the polyfunctional amine in the hollow, the polyfunctional amine of 1.2 times the volume of the hollow fiber inside the module is impregnated into the pores of the support by gravity in the vertical direction.
또한, 상기 (4)단계는, In addition, step (4),
상기 중공사 지지체 내부에 과량의 다관능성 아민 수용액을 제거하는 방법에 있어서 건조된 공기를 지지체 기공의 버블포인트(Bubble Point) 압력 이하로 수초내로 제거하는 것을 특징으로 한다. In the method of removing the excess polyfunctional amine aqueous solution inside the hollow fiber support, it is characterized in that the dried air is removed within a few seconds below the bubble point pressure of the pores of the support.
또한, 상기 중공사 지지체 내부에 과량의 다관능성 아민 수용액을 제거하는 방법에 있어서 지지체 내부와 외부에 동일한 압력으로 건조된 공기를 주입하는 것을 특징으로 한다. In addition, in the method of removing the excess polyfunctional amine aqueous solution inside the hollow fiber support, it is characterized by injecting dried air at the same pressure inside and outside the support.
또한, 상기 (5)단계는,In addition, step (5),
상기 다관능성 산할로겐화합물을 포함하는 유기용액과 접촉하여 폴리아미드층을 형성시켜 제조한다. It is prepared by contacting with an organic solution containing the polyfunctional acid halide compound to form a polyamide layer.
또한, 상기 폴리아미드층의 형성에 사용된 다관능성 아민수용액과 다관능성 산할로겐화화합물의 농도비는 10:1의 비율로 계면중합하여 형성된 폴리아미드층을 포함한다. In addition, the concentration ratio of the polyfunctional amine aqueous solution used for forming the polyamide layer and the polyfunctional acid halide compound includes a polyamide layer formed by interfacial polymerization in a ratio of 10:1.
또한, 상기 (6)단계는,In addition, step (6),
상기 나노분리막 모듈은 2가염 배제율이 93%이상, 1가염 배제율이 50%이상의 제거 성능을 갖고 순수 유량이 28GFD을 갖는다. The nano-membrane module has a removal performance of at least 93% of the divalent salt exclusion rate and at least 50% of the single salt exclusion rate, and has a pure flow rate of 28GFD.
또한, 계면중합을 위한 코팅액 제조는 피페라진 용액 0.5~5%, 트리에탄올아민 0.1~3%, 폴리비닐 알코올 5~20%, 증류수 중 어느 하나이상을 중량비로 포함하는 것을 특징으로 한다. In addition, the preparation of a coating solution for interfacial polymerization is characterized in that it contains at least one of piperazine solution 0.5 to 5%, triethanolamine 0.1 to 3%, polyvinyl alcohol 5 to 20%, and distilled water.
전술한 각 실시예에서 예시된 특징, 구조, 효과 등은 실시예들이 속하는 분야의 통상의 지식을 가지는 자에 의하여 다른 실시예들에 대해서도 조합 또는 변형되어 실시 가능하다. 따라서 이러한 조합과 변형에 관계된 내용들은 본 발명의 범위에 포함되는 것으로 해석되어야 할 것이다.The features, structures, effects, and the like exemplified in each of the above-described embodiments may be combined or modified for other embodiments by a person having ordinary knowledge in the field to which the embodiments belong. Therefore, the contents related to such combinations and modifications should be interpreted as being included in the scope of the present invention.
Claims (11)
(2) 상기 제조된 중공사 지지체에 포함된 용매 및 내부응고액을 세척하는 단계: 40℃, DI 48hr
(3) 상기 제조된 중공사 지지체 내부에 다관능성 아민 수용액을 침지하는 단계: 정량펌프로 공급, 모듈상부에 아민 Gravity Force,
(4) 상기 중공사 지지체 내부에 주입된 과량의 다관능성 아민수용액을 제거하는 단계: 중공사 내부/외부에 동일압력으로 에어로 주입, 버블포인트 이하의 압력으로 제거, 장시간 제거시 기화됨
(5) 다관능성 산할로겐화합물을 포함하는 유기용액과 접촉하여 폴리아미드층을 형성시키는 단계: 접촉시간, 건조방법
(6) 상기 제조된 나노중공사 분리막 모듈은 유량이 28GFD, 93%염배제율을 갖는 중공사형 나노분리막 모듈의 제조방법.(1) A step of manufacturing a hollow fiber module by spinning a porous ultrafiltration membrane (UF) support in the form of a hollow fiber by spinning through a spinning nozzle, including a spinning stock solution containing polyacrylonitrile and an internal coagulant, and then immersing with an external coagulant. ;
(2) washing the solvent and the internal coagulation solution contained in the prepared hollow fiber support: 40℃, DI 48hr
(3) immersing the polyfunctional amine aqueous solution inside the prepared hollow fiber support: supplied with a metering pump, amine Gravity Force on the module top,
(4) Step of removing the excess polyfunctional amine aqueous solution injected into the hollow fiber support: air injection at the same pressure inside/outside the hollow fiber, removal at a pressure below the bubble point, vaporization when removed for a long time
(5) Forming a polyamide layer by contacting with an organic solution containing a polyfunctional acid halide compound: contact time, drying method
(6) The prepared nano hollow fiber membrane module is a method of manufacturing a hollow fiber type nano membrane module having a flow rate of 28 GFD and a salt removal rate of 93%.
상기 (1)단계는
방사원액에 사용되는 고분자 물질은 폴리아크릴로니트릴(PAN), 폴리아크릴로니트릴 공중합체중 하나로 선택되고 유기성 용매 및 내부응고제로는 N-메틸-2-피롤리디온(NMP)인 것을 특징으로하는 고염배제율을 갖는 중공사형 나노분리막 모듈의 제조방법.The method of claim 1,
Step (1) above
The high molecular salt used in the spinning dope is selected from polyacrylonitrile (PAN) and polyacrylonitrile copolymers, and is an organic solvent and an internal coagulant characterized by N-methyl-2-pyrrolidion (NMP). Method of manufacturing a hollow fiber nano-separation membrane module having an exclusion rate.
상기 (2)단계는,
상기 중공사형태의 한외여과막(UF)에 잔류하고 있는 용매 및 내부응고제를 초순수로 30℃ ~ 40℃로 중공 내부와 외부를 48hr 동안 세척하는 단계인 중공사형 나노분리막 모듈의 제조방법.The method of claim 1,
Step (2) above,
A method of manufacturing a hollow fiber nano-membrane module which is a step of washing the inside and the outside of the hollow with ultrapure water at 30°C to 40°C for 48hr with the solvent and internal coagulant remaining in the hollow fiber membrane ultrafiltration membrane (UF).
상기 (3)단계는 ,
상기 중공 내부에 다관능성 아민은 피페라진,메타페닐렌디아민, 디페닐디아민, 파라페닐렌디아민으로 이루어진 군으로부터 선택되는 1종 이상을 포함하는 중공사형 나노분리막 모듈의 제조방법.The method of claim 1,
Step (3) above,
A polyfunctional amine in the hollow is a method of manufacturing a hollow fiber-type nano-separation membrane module comprising at least one member selected from the group consisting of piperazine, metaphenylenediamine, diphenyldiamine, and paraphenylenediamine.
상기 (3)단계는,
상기 중공 내부에 다관능성 아민을 침지시키는 방법으로는 모듈 내부에 중공사 내부 부피의 1.2배의 다관능성 아민을 수직방향으로 중력(Gravity Force)에 의해 지지체 기공에 함침시키는 것을 특징으로하는 중공사형 나노분리막 모듈의 제조방법.The method of claim 1,
Step (3) above,
As a method of immersing the polyfunctional amine in the hollow, a hollow fiber nano which is characterized in that a polyfunctional amine of 1.2 times the volume of the hollow fiber inside the module is impregnated into the pores of the support by gravity in the vertical direction. Method of manufacturing a separator module.
상기 (4)단계는,
상기 중공사 지지체 내부에 과량의 다관능성 아민 수용액을 제거하는 방법에 있어서 건조된 공기를 지지체 기공의 버블포인트(Bubble Point) 압력 이하로 수초내로 제거하는 것을 특징으로하는 중공사형 나노분리막 모듈의 제조방법.The method of claim 1,
Step (4) is,
Method for removing excess polyfunctional amine aqueous solution inside the hollow fiber support, wherein the dried air is removed within a few seconds below the bubble point pressure of the pores of the support. .
상기 중공사 지지체 내부에 과량의 다관능성 아민 수용액을 제거하는 방법에 있어서 지지체 내부와 외부에 동일한 압력으로 건조된 공기를 주입하는 것을 특징으로하는 중공사형 나노분리막 모듈의 제조방법.The method of claim 6,
In the method for removing excess polyfunctional amine aqueous solution inside the hollow fiber support, a method for manufacturing a hollow fiber nano-separation membrane module characterized by injecting dried air at the same pressure inside and outside the support.
상기 (5)단계는,
상기 다관능성 산할로겐화합물을 포함하는 유기용액과 접촉하여 폴리아미드층을 형성시시켜 중공사형 나노분리막 모듈의 제조방법.The method of claim 1,
Step (5) above,
A method of manufacturing a hollow fiber-type nano-separation membrane module by forming a polyamide layer in contact with an organic solution containing the polyfunctional acid halide compound.
상기 폴리아미드층의 형성에 사용된 다관능성 아민수용액과 다관능성 산할로겐화화합물의 농도비는 10:1의 비율로 계면중합하여 형성된 폴리아미드층을 포함하는 중공사형 나노분리막 모듈의 제조방법.The method of claim 8,
A method of manufacturing a hollow fiber nanoseparation membrane module comprising a polyamide layer formed by interfacial polymerization at a ratio of 10:1 in a concentration ratio of a polyfunctional amine aqueous solution and a polyfunctional acid halide compound used to form the polyamide layer.
상기 (6)단계는,
상기 나노분리막 모듈은 2가염 배제율이 93%이상, 1가염 배제율이 50%이상의 제거 성능을 갖고 순수 유량이 28GFD을 갖는 중공사형 나노분리막 모듈의 제조방법.The method of claim 1,
Step (6) is,
The nano-membrane module is a method of manufacturing a hollow fiber type nano-membrane module having a removal performance of at least 93% divalent salt exclusion rate, at least 50% a single salt exclusion rate, and a pure flow rate of 28 GFD.
계면중합을 위한 코팅액 제조는 피페라진 용액 0.5~5%, 트리에탄올아민 0.1~3%, 폴리비닐 알코올 5~20%, 증류수 중 어느 하나이상을 중량비로 포함하는 것을 특징으로 하는 중공사형 나노분리막 모듈의 제조방법.
The method of claim 10,
Preparation of the coating solution for the interfacial polymerization of the hollow fiber-type nano-separator module characterized in that it comprises at least one of piperazine solution 0.5 to 5%, triethanolamine 0.1 to 3%, polyvinyl alcohol 5 to 20%, distilled water Manufacturing method.
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| WO2022071123A1 (en) * | 2020-09-30 | 2022-04-07 | ユニチカ株式会社 | Nanofiltration membrane and manufacturing method therefor |
| CN116059852A (en) * | 2023-02-22 | 2023-05-05 | 泰州南潇新材料科技有限公司 | Method for facilitating interfacial polymerization of hollow fiber organic filter membrane into polyamide membrane |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2022071123A1 (en) * | 2020-09-30 | 2022-04-07 | ユニチカ株式会社 | Nanofiltration membrane and manufacturing method therefor |
| CN116059852A (en) * | 2023-02-22 | 2023-05-05 | 泰州南潇新材料科技有限公司 | Method for facilitating interfacial polymerization of hollow fiber organic filter membrane into polyamide membrane |
| CN116059852B (en) * | 2023-02-22 | 2023-09-19 | 泰州南潇新材料科技有限公司 | Method for facilitating interfacial polymerization of hollow fiber organic filter membrane into polyamide membrane |
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