KR101122569B1 - Gas separation membrane and coating method for increasing separation properties of gas separation membrane - Google Patents
Gas separation membrane and coating method for increasing separation properties of gas separation membrane Download PDFInfo
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- KR101122569B1 KR101122569B1 KR1020090114325A KR20090114325A KR101122569B1 KR 101122569 B1 KR101122569 B1 KR 101122569B1 KR 1020090114325 A KR1020090114325 A KR 1020090114325A KR 20090114325 A KR20090114325 A KR 20090114325A KR 101122569 B1 KR101122569 B1 KR 101122569B1
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- 239000012528 membrane Substances 0.000 title claims abstract description 100
- 238000000926 separation method Methods 0.000 title claims abstract description 73
- 238000000576 coating method Methods 0.000 title claims abstract description 41
- 239000011247 coating layer Substances 0.000 claims abstract description 50
- 239000011248 coating agent Substances 0.000 claims abstract description 41
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 24
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 238000010438 heat treatment Methods 0.000 claims abstract description 8
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 30
- 239000002904 solvent Substances 0.000 claims description 6
- -1 Increased Resolution Substances 0.000 abstract description 4
- 239000007789 gas Substances 0.000 description 50
- 230000000052 comparative effect Effects 0.000 description 14
- 239000000203 mixture Substances 0.000 description 8
- 230000007547 defect Effects 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 5
- 239000004205 dimethyl polysiloxane Substances 0.000 description 5
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 230000000704 physical effect Effects 0.000 description 5
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000012510 hollow fiber Substances 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000009987 spinning Methods 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 229920001187 thermosetting polymer Polymers 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000004848 polyfunctional curative Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004382 potting Methods 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 230000003313 weakening effect Effects 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
- B01D71/027—Silicium oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/22—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion
- B01D53/228—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by diffusion characterised by specific membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0083—Thermal after-treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/1213—Laminated layers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/02—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber
- B05D7/04—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to macromolecular substances, e.g. rubber to surfaces of films or sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/08—Specific temperatures applied
- B01D2323/081—Heating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/12—Specific ratios of components used
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/219—Specific solvent system
Abstract
본 발명은 기체분리막의 제조기술에 관한 것으로, 본 발명은 막 표면에 코팅층 갖는 기체분리막에 있어서, 상기 막 표면에 2액형 실리콘 엘라스토머와 상온경화용 일액형 실리콘이 1:1의 무게비 또는 부피비로 혼합된 코팅액으로 형성시킨 코팅층을 포함하여 이루어지는 기체분리막을 특징으로 한다.The present invention relates to a technology for producing a gas separation membrane, the present invention is a gas separation membrane having a coating layer on the membrane surface, the two-component silicone elastomer and the one-component silicone for room temperature curing on the membrane surface is mixed in a weight ratio or volume ratio of 1: 1 Characterized by a gas separation membrane comprising a coating layer formed of the coating solution.
또한, 본 발명은 제조되는 기체분리막의 막 표면에 행하는 코팅처리방법에 있어서, 2액형 실리콘 엘라스토머와 상온경화용 일액형 실리콘을 포함하는 코팅액을 막 표면에 코팅 처리하여 코팅층을 형성시킨 후, 50~80℃의 온도에서 1시간~2시간 30분 동안 열처리하여 코팅층을 경화시키는 기체분리막의 분리능 증대를 위한 코팅처리방법을 특징으로 한다.In addition, the present invention is a coating treatment method performed on the membrane surface of the gas separation membrane to be prepared, after the coating liquid containing a two-component silicone elastomer and a one-component silicone for room temperature curing to form a coating layer, 50 ~ Characterized by a coating treatment method for increasing the separation capacity of the gas separation membrane to cure the coating layer by heat treatment for 1 hour to 2 hours 30 minutes at a temperature of 80 ℃.
본 발명은 제조되는 기체분리막의 막 표면에 일정두께 이상의 코팅층을 용이하면서도 안정적으로 형성시킬 수 있을 뿐만 아니라 균일한 코팅층을 형성시킬 수 있으며, 이를 통해 내구성을 갖는 코팅층을 형성시킬 수 있고 기체분리막의 분리능을 증대시킬 수 있다.The present invention can not only easily and stably form a coating layer of a predetermined thickness or more on the membrane surface of the gas separation membrane to be manufactured, but also form a uniform coating layer, thereby forming a coating layer having durability and separation ability of the gas separation membrane. Can be increased.
기체분리막, 분리능 증대, 코팅층, 용이성, 안정성, 균일성, 내구성 Gas Separation Membrane, Increased Resolution, Coating Layer, Ease, Stability, Uniformity, Durability
Description
본 발명은 각종 기체를 분리하는데 사용되는 기체분리막의 제조기술에 관한 것으로, 더욱 상세하게는 개선된 분리능을 위한 코팅층을 갖는 기체분리막 및, 막 표면에 일정두께 이상의 코팅층을 용이하면서도 안정적으로 형성시킬 수 있도록 함은 물론 균일한 코팅층을 형성시킬 수 있도록 하며 제조되는 기체분리막의 분리능을 증대시킬 수 있도록 한 기체분리막의 분리능 증대를 위한 코팅처리방법에 관한 것이다.The present invention relates to a manufacturing technology of a gas separation membrane used to separate various gases, and more particularly, a gas separation membrane having a coating layer for improved resolution and a coating layer of a predetermined thickness or more on the membrane surface can be easily and stably formed. The present invention relates to a coating treatment method for increasing the separation capability of the gas separation membrane to allow the formation of a uniform coating layer and to increase the separation ability of the gas separation membrane to be manufactured.
일반적으로 기체분리막은 산소나 질소 등 기체를 분리하는데 사용되는 막으로서, 특수하게 제작된 막의 한쪽 면으로 기체가 접촉되어 막 반대편의 압력이 저압상태로 될 때 혼합기체중의 특정 기체가 막을 투과하는 현상을 이용하여 기체를 분리해내는 방식이 사용된다.In general, a gas separation membrane is a membrane used to separate gases such as oxygen and nitrogen, and when a gas is brought into contact with one side of a specially prepared membrane and the pressure on the opposite side of the membrane becomes a low pressure state, specific gas in the mixed gas penetrates the membrane. The method of separating gas by using is used.
이렇게 기체 분리에 사용되는 기체분리막은 막 표면의 치밀한 선택분리층과 막 하부에 최소의 투과저항을 갖는 다공성 지지체로 이루어지는 비대칭구조로 제조됨이 바람직한 것으로 보고되고 있으며, 기체분리를 위한 운전조건에 차이가 있으나 중공사막 모듈형태의 기체분리막이 많이 사용되고 있다.It is reported that the gas separation membrane used for gas separation is preferably made of an asymmetric structure consisting of a dense selective separation layer on the membrane surface and a porous support having a minimum permeation resistance at the bottom of the membrane, and the operating conditions for gas separation are different. However, gas separation membranes in the form of hollow fiber membrane modules are widely used.
종래 중공사막 모듈형태의 기체분리막 제조공정을 개략적으로 살펴보면, 중공사막 형성을 위한 고분자용액 및 내부응고액을 제조하는 도프 제조단계, 제조된 도프를 방사노즐을 통해 공기 중에 방사하는 방사단계, 방사된 도프를 외부응고액 속에 침지시켜 응고시키는 응고단계, 세정단계, 용매치환단계, 건조단계, 코팅단계, 중공사막의 다발을 형성하는 모듈 포팅단계를 포함하는 공정으로 이루어진다.Looking at the manufacturing process of the conventional gas separation membrane of the hollow fiber membrane module form, the dope manufacturing step of preparing the polymer solution and the internal coagulating solution for forming the hollow fiber membrane, the spinning step of spinning the prepared dope in the air through the spinning nozzle, It consists of a process including a coagulation step of immersing the dope in the external coagulation liquid to solidify, a washing step, a solvent replacement step, a drying step, a coating step, a module potting step of forming a bundle of hollow fiber membranes.
이때, 제조되는 기체분리막은 표면에 결함이 존재하지 않는 표면층으로 존재하여야 하나, 실제 상기의 방사단계에서 결함이 존재하지 않는 막 표면을 만드는데 상당한 어려움 및 한계상황이 발생되고 있어 상기의 건조단계 이후에 제조되는 막 표면의 결함을 커버 및 제거할 수 있도록 코팅작업을 수행하고 있으며, 종래 코팅단계의 수행시 코팅제로는 대부분이 폴리디메틸실록산(poly dimethyl siloxane; PDMS)을 사용하고 있다.At this time, the gas separation membrane to be prepared should be present as a surface layer that does not have a defect on the surface, but in fact, in the spinning step, significant difficulties and limitations have arisen in making the membrane surface free of defects. The coating process is performed to cover and remove defects on the surface of the film to be produced. In the conventional coating step, the coating agent is mostly polydimethyl siloxane (PDMS).
그런데, 종래 기체분리막의 제조시 막 표면의 결함을 커버하기 위해 코팅제로 사용되고 있는 폴리디메틸실록산은 코팅단계의 수행시 일정시간 이상 열원이 가해져야 경화되는 열경화형으로서 히팅존이 존재하게 되므로 이로 인해 유독한 유기용매가 발생하여 오염원이 생기는 단점 및 안정성이 떨어지는 문제점이 있었으며, 점도가 낮아 막 표면에 일정두께 이상의 코팅층을 형성하는데 어려움을 겪고 있음 은 물론 균일한 코팅층의 형성에도 어려움이 존재하고 있는 실정에 있다.However, polydimethylsiloxane, which is used as a coating agent to cover defects on the surface of the membrane during the production of a conventional gas separation membrane, has a heating zone as a thermosetting type that is cured only when a heat source is applied for a predetermined time or more during the coating step. One organic solvent was generated, and there was a problem in that a pollution source was generated and the stability was inferior. As a result of the low viscosity, it was difficult to form a coating layer having a predetermined thickness or more on the surface of the film, as well as a difficulty in forming a uniform coating layer. have.
본 발명은 상기와 같은 문제점 등을 감안하여 안출된 것으로서, 개선된 분리능을 위한 코팅층을 갖는 기체분리막 및, 막 표면에 일정두께 이상의 코팅층을 용이하면서도 안정적으로 형성시킬 수 있도록 함은 물론 균일한 코팅층을 형성시킬 수 있도록 하며 제조되는 기체분리막의 분리능을 증대시킬 수 있도록 한 기체분리막의 분리능 증대를 위한 코팅처리방법을 제공하는데 그 목적이 있다.The present invention has been made in view of the above problems, such as, gas separation membrane having a coating layer for improved resolution, and to facilitate and stably form a coating layer of a predetermined thickness or more on the surface of the membrane as well as a uniform coating layer It is an object of the present invention to provide a coating treatment method for increasing the separation ability of the gas separation membrane to be formed and to increase the separation ability of the gas separation membrane to be produced.
본 발명은 막 표면의 결함을 제거하면서도 기체분리에 따른 효율 및 효용성을 높일 수 있도록 한 기체분리막 및, 기체분리막의 분리능 증대를 위한 코팅처리방법을 제공하는데 있다.The present invention provides a gas separation membrane and a coating treatment method for increasing the separation ability of the gas separation membrane to remove the defects on the surface of the membrane and to improve the efficiency and effectiveness of the gas separation.
본 발명은 막 표면을 갖는 기체분리막에 있어서,The present invention is a gas separation membrane having a membrane surface,
상기 막 표면에 2액형 실리콘 엘라스토머와 상온경화용 일액형 실리콘이 1:1의 무게비 또는 부피비로 혼합된 코팅액으로 형성시킨 코팅층을 포함하여 이루어지는 기체분리막을 특징으로 한다.Characterized in that the gas separation membrane comprising a coating layer formed of a coating liquid mixed with a two-component silicone elastomer and a one-component silicone for room temperature curing in a weight ratio or volume ratio of 1: 1 on the membrane surface.
또한, 본 발명은 제조되는 기체분리막의 막 표면에 행하는 코팅처리방법에 있어서,In addition, the present invention is a coating treatment method performed on the membrane surface of the gas separation membrane to be produced,
2액형 실리콘 엘라스토머와 상온경화용 일액형 실리콘을 포함하는 코팅액을 막 표면에 코팅 처리하여 코팅층을 형성시킨 후, 50~80℃의 온도에서 1시간~2시간 30분 동안 열처리하여 코팅층을 경화시키는 기체분리막의 분리능 증대를 위한 코팅처리방법을 특징으로 한다.A coating liquid comprising a two-component silicone elastomer and a one-component silicone for room temperature curing is coated on a surface of a film to form a coating layer, and then heat-treated at a temperature of 50 to 80 ° C. for 1 hour to 2 hours 30 minutes to cure the coating layer. Characterized by a coating treatment method for increasing the separation ability of the membrane.
본 발명은 제조되는 기체분리막의 막 표면에 일정두께 이상의 코팅층을 용이하면서도 안정적으로 형성시킬 수 있을 뿐만 아니라 균일한 코팅층을 형성시킬 수 있고, 이를 통해 내구성을 갖는 코팅층을 형성시킬 수 있으면서 기체분리막의 분리능을 증대시킬 수 있으며, 기체분리막의 막 표면에 대한 결함을 제거하면서도 각종 기체의 분리에 따른 효율 및 효용성을 높일 수 있다.The present invention can not only easily and stably form a coating layer of a predetermined thickness or more on the membrane surface of the gas separation membrane to be manufactured, but also can form a uniform coating layer, thereby forming a durable coating layer, thereby separating the gas separation membrane. It is possible to increase the efficiency and efficiency of separation of various gases while removing defects on the membrane surface of the gas separation membrane.
본 발명의 실시예에 대해 상세히 설명하면 다음과 같다.Hereinafter, the embodiment of the present invention will be described in detail.
본 발명의 실시예에 의한 기체분리막은 제조공정의 순차적인 진행으로 막 표면을 갖게 되는 기체분리막에 있어서,Gas separation membrane according to an embodiment of the present invention in the gas separation membrane having a membrane surface by the sequential progress of the manufacturing process,
상기 막 표면에 2액형 실리콘 엘라스토머와 상온경화용 일액형 실리콘이 혼합된 코팅액을 코팅 처리함으로써 막 표면의 결함을 제거함과 아울러 분리능을 개선하기 위한 코팅층을 포함하여 이루어지게 한다.The coating solution is a coating solution containing a two-component silicone elastomer and a one-component silicone for room temperature curing on the surface of the membrane to remove defects on the surface of the membrane and to include a coating layer for improving resolution.
이때, 상기 코팅층의 형성에 사용되는 코팅액은 2액형 실리콘 엘라스토머와 상온경화용 일액형 실리콘을 1:1의 무게비 또는 부피비로 혼합한 것을 사용함이 바람직하다 할 것이다.At this time, the coating liquid used for the formation of the coating layer will be preferable to use a mixture of two-component silicone elastomer and one-component silicone for room temperature curing in a weight ratio or volume ratio of 1: 1.
여기서, 상기 코팅층을 위한 코팅액은 2액형 실리콘 엘라스토머와 상온경화용 일액형 실리콘을 혼합함에 있어 용매를 사용함이 바람직한데, 이때에는 용매로 헥산을 사용함이 바람직하며, 2액형 실리콘 엘라스토머 1~10중량%와 상온경화용 일액형 실리콘 1~10중량% 및 헥산 80~98중량%의 조성으로 이루어지게 한다.Here, the coating liquid for the coating layer is preferably a solvent in mixing the two-component silicone elastomer with a one-component silicone for room temperature curing, in this case, it is preferable to use hexane as a solvent, 1 to 10% by weight two-
한편, 본 발명에 의한 기체분리막의 분리능 증대를 위한 코팅처리방법은 제조되는 기체분리막의 막 표면에 코팅처리를 수행함에 있어서,On the other hand, the coating treatment method for increasing the separation ability of the gas separation membrane according to the present invention in the coating treatment on the membrane surface of the gas separation membrane to be prepared,
상기 막 표면에 2액형 실리콘 엘라스토머와 상온경화용 일액형 실리콘을 포함하는 코팅액을 코팅 처리함으로써 코팅층을 형성시킨다.The coating layer is formed on the surface of the film by coating a coating solution containing a two-component silicone elastomer and a one-component silicone for curing at room temperature.
이때, 상기 2액형 실리콘 엘라스트머는 주재와 경화재가 10:1의 배합비율로 이루어지는 열경화형 2액형 실리콘 재료로서 화학적으로 안정되고 점도가 낮은 것이며, 상기 상온경화형 일액형 실리콘은 상온(20~30℃)에서 공기중의 습기와 반응하여 자연 경화되는 상온경화형이고 내부식성의 특성 및 점도가 높은 것이다.In this case, the two-component silicone elastomer is a thermosetting two-component silicone material composed of a main material and a hardener in a blending ratio of 10: 1, which is chemically stable and low in viscosity, and the room temperature-curable one-component silicone is room temperature (20 to 30 ° C). ) Is a room temperature curing type that reacts with moisture in the air and hardens naturally, and has high corrosion resistance and viscosity.
상기 2액형 실리콘 엘라스토머와 상온경화용 일액형 실리콘은 1:1의 무게비 또는 부피비로 혼합하여 사용함이 바람직한데, 이는 어느 한쪽의 조성비가 다른 쪽에 비해 높게 되면 코팅품질에 악영향을 미쳐 막 표면에 코팅이 안정적으로 형성되지 않거나 균일한 코팅층의 형성을 어렵게 할 수 있다.The two-component silicone elastomer and the one-component silicone for curing at room temperature are preferably used by mixing in a weight ratio or volume ratio of 1: 1. If the composition ratio of one is higher than the other, the coating quality is adversely affected by coating quality. It may be difficult to form stably or to form a uniform coating layer.
부연하면, 상기 2액형 실리콘 엘라스토머의 조성이 많게 되면 낮은 점도의 형성으로 막 표면에 코팅 처리시 일정두께 이상의 코팅층을 형성하는데 어려움이 있을 뿐만 아니라 안정성이 떨어지게 되며, 상기 상온경화형 일액형 실리콘의 조성이 많게 되면 높은 점도의 형성으로 막 표면이 너무 끈적끈적해지고 이로 인해 모듈작업시 사용되는 접착제와의 접착력이 약화되어 접착부분에 리크(leak)가 발생할 가능성이 높아지게 되는 것으로, 상기 2액형 실리콘 엘라스토머와 상온경화용 일액형 실리콘은 동일한 배합비율로 적용함이 가장 바람직하다 할 것이다.In other words, when the composition of the two-component silicone elastomer is large, it is difficult to form a coating layer having a predetermined thickness or more during coating treatment on the surface of the membrane due to the formation of a low viscosity, and the stability is lowered, and the composition of the room temperature-curable one-component silicone is When the viscosity increases, the surface of the membrane becomes too sticky due to the formation of a high viscosity, thereby weakening the adhesive strength with the adhesive used in the module work, thereby increasing the likelihood of leaking in the adhesive portion, and the two-component silicone elastomer and room temperature. It is most preferable to apply the one-component silicone for curing in the same compounding ratio.
또한, 상기 코팅층의 형성을 위한 코팅액은 2액형 실리콘 엘라스토머와 상온경화용 일액형 실리콘의 혼합에 따른 용이성을 위해 용매를 사용함이 바람직한데, 이때에는 용매로 헥산을 사용함이 바람직하다 할 것이며, 2액형 실리콘 엘라스토머 1~10중량%와 상온경화용 일액형 실리콘 1~10중량% 및 헥산 80~98중량%의 조성으로 이루어지게 함이 바람직하다.In addition, the coating liquid for the formation of the coating layer is preferably a solvent for ease of mixing according to the two-component silicone elastomer and room temperature curing one-component silicone, in this case it is preferable to use hexane as a solvent, two-component It is preferable to make the composition of 1-10% by weight of silicone elastomer, 1-10% by weight of one-component silicone for curing at room temperature, and 80-98% by weight of hexane.
여기서, 상기 2액형 실리콘 엘라스토머와 상온경화용 일액형 실리콘을 포함하는 코팅액의 적용으로 코팅층의 두께를 1.00㎛ 이상으로 용이하게 형성시킬 수 있을 뿐만 아니라 적절한 점도 형성에 의해 코팅층을 균일하게 형성시킬 수 있게 되므로 기체분리막에 대한 분리능의 개선효과를 기대할 수 있게 된다.Here, by applying the coating liquid containing the two-component silicone elastomer and the one-component silicone for room temperature curing, the coating layer may be easily formed to a thickness of 1.00 μm or more, and the coating layer may be uniformly formed by appropriate viscosity. Therefore, it is possible to expect an effect of improving the resolution for the gas separation membrane.
이어, 상기 막 표면에 코팅층을 형성시킨 이후에는, 50~80℃의 온도에서 1시간~2시간 30분 동안 열처리하여 코팅층을 경화시킨다.Subsequently, after the coating layer is formed on the film surface, the coating layer is cured by heat treatment at a temperature of 50 to 80 ° C. for 1 hour to 2 hours and 30 minutes.
이때, 코팅층은 적절한 배합비율을 갖는 2액형 실리콘 엘라스토머와 상온경화형 일액형 실리콘의 물질특성에 의해 예전보다 비교적 빠른 시간에 경화가 이루어지도록 촉진되므로 긴 히팅존이 존재할 필요가 없게 되고 보다 용이하면서도 안정적으로 형성시킬 수 있게 된다.At this time, the coating layer is promoted to be cured in a relatively quick time by the material properties of the two-component silicone elastomer and the room temperature curing one-component silicone having an appropriate mixing ratio, so that a long heating zone does not need to exist and is easier and more stable. It can be formed.
이렇게 제조되는 기체분리막의 막 표면에 코팅층을 빠르면서도 안정적으로 형성시킬 수 있고 용이하면서도 균일하게 형성시킬 수 있음에 따라 기체분리막의 분리능에 대한 물성특성을 높일 수 있으면서 품질신뢰성 또한 향상시킬 수 있고 보다 우수한 특성을 발휘하는 기체분리막을 제조할 수 있게 되는 것이다.The coating layer can be quickly and stably formed on the membrane surface of the gas separation membrane thus prepared, and can be easily and uniformly formed, thereby improving the physical properties of the gas separation membrane and improving quality reliability. It will be possible to produce a gas separation membrane exhibiting characteristics.
[실시예 1]Example 1
기체분리막의 막 표면에 2액형 실리콘 엘라스토머 3중량%와 상온경화용 일액형 실리콘 3중량% 및 헥산 94중량%의 조성으로 이루어진 코팅액으로 코팅하여 코팅층을 형성시킨 후, 70℃에서 2시간 열처리하여 경화시켰다.A coating layer was formed on the membrane surface of the gas separation membrane with a composition consisting of 3% by weight of a two-component silicone elastomer, 3% by weight of a one-component silicone for room temperature curing and 94% by weight of hexane, and then formed by coating a heat treatment at 70 ° C. for 2 hours to cure. I was.
[실시예 2][Example 2]
기체분리막의 막 표면에 2액형 실리콘 엘라스토머 1중량%와 상온경화용 일액형 실리콘 1중량% 및 헥산 98중량%의 조성으로 이루어진 코팅액으로 코팅하여 코팅층을 형성시킨 후, 70℃에서 2시간 열처리하여 경화시켰다.A coating layer was formed on the membrane surface of the gas separation membrane with a composition consisting of 1% by weight of a two-component silicone elastomer, 1% by weight of a one-component silicone for room temperature curing, and 98% by weight of hexane to form a coating layer, followed by curing at 70 ° C. for 2 hours. I was.
[비교예 1]Comparative Example 1
기체분리막의 막 표면에 폴리디메틸실록산 5중량% 및 헥산 95중량%의 조성으로 이루어진 코팅액으로 코팅하여 코팅층을 형성시킨 후, 70℃에서 2시간 열처리하여 경화시켰다.After coating with a coating liquid consisting of 5% by weight of polydimethylsiloxane and 95% by weight of hexane on the membrane surface of the gas separation membrane to form a coating layer, it was cured by heat treatment at 70 ℃ for 2 hours.
[비교예 2]Comparative Example 2
기체분리막의 막 표면에 폴리디메틸실록산 10중량% 및 헥산 90중량%의 조성으로 이루어진 코팅액으로 코팅하여 코팅층을 형성시킨 후, 70℃에서 2시간 열처리하여 경화시켰다.After coating with a coating liquid consisting of a composition of 10% by weight of polydimethylsiloxane and 90% by weight of hexane on the membrane surface of the gas separation membrane to form a coating layer, it was cured by heat treatment at 70 ℃ for 2 hours.
이때, 상기한 실시예 1과 실시예 2, 비교예 1과 비교예 2에 사용된 기체분리막은 동일한 조건에 의해 막 표면이 형성된 것을 사용하였다.At this time, the gas separation membrane used in Example 1 and Example 2, Comparative Example 1 and Comparative Example 2 was used that the membrane surface was formed under the same conditions.
이러한 실시예 1과 실시예 2, 비교예 1과 비교예 2를 가지고 산소 분리능에 대한 물성테스트를 실시하되 모두 동일한 운전조건으로 실시하였으며, 이하의 표 1에 그 결과치를 나타내었다.Example 1 and Example 2, Comparative Example 1 and Comparative Example 2 having a physical property test for the oxygen separation performance was carried out under the same operating conditions, the results are shown in Table 1 below.
표 1. 산소 분리능 물성테스트 결과Table 1. Oxygen Resolution Property Test Results
표 1에서 보여주는 바와 같이, 본 발명에 의한 실시예 1 및 실시예 2가 종래기술에 의한 비교예 1 및 비교예 2에 비해 투과량은 줄여주면서 분리능은 높여주는 물성특성을 발휘함을 나타내고 있다.As shown in Table 1, Examples 1 and 2 according to the present invention exhibits physical properties that improve the resolution while reducing the permeation amount compared to Comparative Example 1 and Comparative Example 2 according to the prior art.
특히, 본 발명에 의한 실시예 1 및 실시예 2는 운전압력을 높이더라도 분리능이 저하되지 않는 물성을 갖게 하는 것인데 반하여, 종래기술에 의한 비교예 1 및 비교예 2는 운전압력을 높일 경우 분리능이 저하되는 물성을 나타내고 있어 본원발명이 분리능의 증대효과를 발생시킴을 확인할 수 있을 뿐만 아니라 기체분리막의 내구성 증대에도 일조함을 확인할 수 있다.In particular, Example 1 and Example 2 according to the present invention is to have a physical property that the resolution does not decrease even if the operating pressure is increased, whereas Comparative Example 1 and Comparative Example 2 according to the prior art has a resolution when the operating pressure is increased It can be confirmed that the present invention exhibits deteriorated physical properties, and thus, the present invention causes an effect of increasing the resolution, and also helps to increase the durability of the gas separation membrane.
한편, 도 1 및 도 2는 본 발명에 의한 실시예 1 및 실시예 2를 통해 기체분리막의 막 표면에 형성시킨 코팅층을 관찰한 주사전자현미경(SEM) 사진이고, 도 3 및 도 4는 종래기술에 의한 비교예 1 및 비교예 2를 통해 기체분리막의 막 표면에 형성시킨 코팅층을 관찰한 주사전자현미경(SEM) 사진이다.Meanwhile, FIGS. 1 and 2 are scanning electron microscope (SEM) photographs of the coating layer formed on the membrane surface of the gas separation membrane through Examples 1 and 2 according to the present invention, and FIGS. 3 and 4 are related arts. Scanning electron microscope (SEM) photographs of the coating layer formed on the membrane surface of the gas separation membrane through Comparative Example 1 and Comparative Example 2 by.
여기서, 본 발명에 의한 실시예 1 및 실시예 2를 통해 기체분리막의 막 표면에 형성시킨 코팅층은 도 1 및 도 2의 사진에서 보여주는 바와 같이 분리능의 기능을 발휘할 수 있는 정도의 코팅층이 일정 두께 이상으로 막 표면에 형성되어 있고 균일하게 형성되어 있음을 보여주고 있으며, 종래기술에 의한 비교예 1 및 비교예2에 있어서는 도 3 및 도 4의 사진에서 보여주는 바와 같이 코팅층이 막 표면에 너무 얇게 형성되어 있고 이로 인해 균일하게 형성되기 어려움을 보여주고 있다.Here, the coating layer formed on the membrane surface of the gas separation membrane through Example 1 and Example 2 according to the present invention is a coating layer of a degree that can exhibit the function of the resolution as shown in the picture of Figure 1 and 2 or more than a certain thickness As shown in the photographs of FIGS. 3 and 4, the coating layer is formed too thin on the surface of the film. It is difficult to form uniformly because of this.
도 1 및 도 2는 본 발명에 의한 실시예 1 및 실시예 2를 통해 기체분리막의 막 표면에 형성시킨 코팅층을 관찰한 주사전자현미경(SEM) 사진.1 and 2 are scanning electron microscope (SEM) photographs of the coating layer formed on the membrane surface of the gas separation membrane through Examples 1 and 2 according to the present invention.
도 3 및 도 4는 종래기술에 의한 비교예 1 및 비교예 2를 통해 기체분리막의 막 표면에 형성시킨 코팅층을 관찰한 주사전자현미경(SEM) 사진.3 and 4 are scanning electron microscope (SEM) photographs of the coating layer formed on the membrane surface of the gas separation membrane through Comparative Example 1 and Comparative Example 2 according to the prior art.
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