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KR102770272B1 - Composition for hydrogen sensing tape, tape and manufacturing method thereof - Google Patents

Composition for hydrogen sensing tape, tape and manufacturing method thereof Download PDF

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KR102770272B1
KR102770272B1 KR1020210183010A KR20210183010A KR102770272B1 KR 102770272 B1 KR102770272 B1 KR 102770272B1 KR 1020210183010 A KR1020210183010 A KR 1020210183010A KR 20210183010 A KR20210183010 A KR 20210183010A KR 102770272 B1 KR102770272 B1 KR 102770272B1
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hydrogen gas
silicone tape
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tape
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KR20230094239A (en
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윤동신
김서영
이경훈
김상민
송희
조일희
어준
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주식회사 유니드
하이리움산업(주)
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Abstract

본 발명은 단순하게 접착 또는 점착성 테이프 형태로 제조될 수 있어 현장적용성이 뛰어나고, 인장강도 및 색변화 시인성도 우수한 수소가스 감지용 실리콘 테이프 조성물, 그 수소가스 감지 실리콘 테이프, 그 제조방법에 관한 것이다.
본 발명에 따른 수소가스 감지용 실리콘 테이프 조성물은 수소가스 감지제와, PDMS와, 백금촉매를 포함하여 이루어진다.
The present invention relates to a silicone tape composition for detecting hydrogen gas, which can be simply manufactured in the form of an adhesive or sticky tape and thus has excellent field applicability and excellent tensile strength and color change visibility, a hydrogen gas detecting silicone tape, and a manufacturing method therefor.
A silicone tape composition for detecting hydrogen gas according to the present invention comprises a hydrogen gas detecting agent, PDMS, and a platinum catalyst.

Description

수소가스 감지용 실리콘 테이프 조성물, 그 수소가스 감지 실리콘 테이프, 그 제조방법{COMPOSITION FOR HYDROGEN SENSING TAPE, TAPE AND MANUFACTURING METHOD THEREOF}Composition of silicone tape for hydrogen gas detection, and method for manufacturing the same {COMPOSITION FOR HYDROGEN SENSING TAPE, TAPE AND MANUFACTURING METHOD THEREOF}

본 발명은 수소가스 감지용 실리콘 테이프 조성물, 그 수소가스 감지 실리콘 테이프, 그 제조방법에 관한 것으로,The present invention relates to a silicon tape composition for detecting hydrogen gas, a silicon tape for detecting hydrogen gas, and a method for producing the same.

보다 상세하게는 단순하게 접착 또는 점착성 테이프 형태로 제조될 수 있어 현장적용성이 뛰어나고, 인장강도 및 색변화 시인성도 우수한 수소가스 감지용 실리콘 테이프 조성물, 그 수소가스 감지 실리콘 테이프, 그 제조방법에 관한 것이다.More specifically, the present invention relates to a silicone tape composition for detecting hydrogen gas, which can be simply manufactured in the form of an adhesive or sticky tape and thus has excellent field applicability, as well as excellent tensile strength and color change visibility, the hydrogen gas detecting silicone tape, and a method for manufacturing the same.

수소 연료 전지 에너지원이나 수소차, 다양한 산업분야에서 사용되는 수소가스를 감지하는 수소센서와 관련하여 특허등록 제10-1015088호(2011년02월09일) [초 고감도 수소 센서에 사용되는 환원된 PdO 박막과 그것을 제조하기 위한 방법]이 있는데,Regarding a hydrogen sensor that detects hydrogen gas used in hydrogen fuel cell energy sources, hydrogen cars, and various industrial fields, there is patent registration No. 10-1015088 (February 9, 2011) [Reduced PDHO thin film used in ultra-high sensitivity hydrogen sensor and method for manufacturing the same].

이 등록특허는 리액티브 스퍼터링 기법(reactive DC magnetron sputtering system)을 이용하여 인위적으로 PdO 박막을 제작하는 단계와, 상기 PdO 박막을 환원반응시켜 나노크랙이 형성된 Pd 박막을 얻는 단계를 포함하며, This registered patent includes a step of artificially producing a PdO thin film using a reactive sputtering technique (reactive DC magnetron sputtering system), and a step of obtaining a Pd thin film with nanocracks formed by subjecting the PdO thin film to a reduction reaction.

상기 나노크랙이 형성된 Pd 박막은 수소검지특성이 향상되어 수소검지 센서에 사용되기 적합한 기술을 제시하고 있다.The Pd thin film formed with the above nanocracks has improved hydrogen detection characteristics, suggesting a technology suitable for use in a hydrogen detection sensor.

또 특허등록 제10-1269510호(2013년05월24일) [수소 농도 측정이 가능한 수소 감지 센서]가 있는데,There is also a patent registration number 10-1269510 (May 24, 2013) [Hydrogen detection sensor capable of measuring hydrogen concentration].

이 등록특허는 수소 가스의 농도 변화에 상응하여 저항값이 변함으로써 연속적으로 수소 가스의 농도 변화를 측정할 수 있는 수소 감지 센서에 관한 것으로 This registered patent relates to a hydrogen detection sensor capable of continuously measuring changes in the concentration of hydrogen gas by changing the resistance value corresponding to changes in the concentration of hydrogen gas.

구체적으로 수소 가스와 접촉시 수소화되는 수소 감지부를 포함하되, 상기 수소 감지부가 수소화될 때, 상기 수소 감지부의 저항값이 변하고, 수소 가스의 제1농도에서 제1 저항값 변화율를 갖고, 상기 제1 농도와 다른 수소 가스의 제2 농도에서 상기 제1 저항값 변화율과 다른 제2 저항값 변화율을 갖는 것을 특징으로 한다.Specifically, it comprises a hydrogen detection unit that is hydrogenated when in contact with hydrogen gas, wherein when the hydrogen detection unit is hydrogenated, the resistance value of the hydrogen detection unit changes, has a first resistance value change rate at a first concentration of hydrogen gas, and has a second resistance value change rate that is different from the first resistance value change rate at a second concentration of hydrogen gas that is different from the first concentration.

그러나 이 두 특허를 비롯한 종래문헌은 즉자적인 현장적용성 부분이나 색변화 시인성을 향상하여 이상 상태를 즉각적으로 감지할 수 있도록 하는 기술과는 무관하다.However, these two patents and other prior literature are unrelated to the immediate field applicability or the technology that improves the visibility of color changes to enable immediate detection of abnormal conditions.

이에 본 발명은 단순하게 접착 또는 점착성 테이프 형태로 제조될 수 있어 현장적용성이 뛰어나고, 인장강도 및 색변화 시인성도 우수한 수소가스 감지용 실리콘 테이프 조성물, 그 수소가스 감지 실리콘 테이프, 그 제조방법을 제공하는 것을 목적으로 한다.Accordingly, the present invention aims to provide a silicone tape composition for detecting hydrogen gas, which can be simply manufactured in the form of an adhesive or sticky tape and thus has excellent field applicability and excellent tensile strength and color change visibility, the hydrogen gas detecting silicone tape, and a manufacturing method thereof.

상기와 같은 목적을 달성하기 위하여 본 발명에 따른 수소가스 감지용 실리콘 테이프 조성물은 In order to achieve the above purpose, the silicon tape composition for hydrogen gas detection according to the present invention

수소가스 감지제와, PDMS와, 백금촉매를 포함하여 이루어진다.It consists of a hydrogen gas detector, PDMS, and a platinum catalyst.

또 본 발명에 따른 수소가스 감지용 실리콘 테이프 조성물에서In addition, in the silicone tape composition for detecting hydrogen gas according to the present invention,

상기 수소가스 감지제 30 중량부에 대하여 PDMS 600~1200 중량부 및 백금촉매 0.5~3 중량부로 구성되고,It is composed of 600 to 1,200 parts by weight of PDMS and 0.5 to 3 parts by weight of platinum catalyst for 30 parts by weight of the above hydrogen gas detector.

테이프의 변색 시인성 향상제가 더 첨가되며,Additional discoloration visibility enhancer is added to the tape.

상기 변색 시인성 향상제는 알루미나이고,The above discoloration visibility improving agent is alumina,

경화지연제가 더 첨가되고,More hardening retarder is added,

상기 경화지연제는 메틸비닐시클로실록산(MVC)인 것을 특징으로 한다.The above curing retardant is characterized by being methylvinylcyclosiloxane (MVC).

나아가 본 발명에 따른 수소가스 감지 실리콘 테이프 및 그 제조방법은 상기 조성물을 이용하여 이루어진다.Furthermore, a hydrogen gas sensing silicone tape according to the present invention and a method for manufacturing the same are made using the composition.

본 발명은 현장적용성이 뛰어난 테이프 형태이면서도, 인장강도 및 색변화 시인성도 우수한 수소가스 감지용 실리콘 테이프 조성물, 그 수소가스 감지 실리콘 테이프, 그 제조방법을 제공할 수 있다.The present invention can provide a silicone tape composition for detecting hydrogen gas in a tape form with excellent field applicability and also excellent tensile strength and color change visibility, a silicone tape for detecting hydrogen gas, and a method for manufacturing the same.

도 1은 본 발명에 따른 수소가스 감지 실리콘 테이프의 수소가스 노출 전후 비교사진.Figure 1 is a comparative photograph of a hydrogen gas-detecting silicone tape according to the present invention before and after exposure to hydrogen gas.

이하 본 발명을 상세히 설명하도록 한다. The present invention will be described in detail below.

본 발명은 다양한 변경을 가할 수 있고 여러 가지 형태를 가질 수 있는 바, 구현예(態樣, aspect)(또는 실시예)들을 본문에 상세하게 설명하고자 한다. 그러나 이는 본 발명을 특정한 개시 형태에 대해 한정하려는 것이 아니며, 본 발명의 사상 및 기술범위에 포함되는 모든 변경, 균등물 내지 대체물을 포함하는 것으로 이해되어야 한다. The present invention can have various modifications and various forms, and thus, embodiments (aspects) (or examples) are described in detail in the text. However, this is not intended to limit the present invention to a specific disclosed form, and it should be understood that it includes all modifications, equivalents, or substitutes included in the spirit and technical scope of the present invention.

본 명세서에서 사용한 용어는 단지 특정한 구현예(태양, 態樣, aspect)(또는 실시예)를 설명하기 위해 사용된 것으로, 본 발명을 한정하려는 의도가 아니다. 단수의 표현은 문맥상 명백하게 다르게 뜻하지 않는 한, 복수의 표현을 포함한다. 본 출원에서, ~포함하다~ 또는 ~이루어진다~ 등의 용어는 명세서 상에 기재된 특징, 숫자, 단계, 동작, 구성요소, 부분품 또는 이들을 조합한 것이 존재함을 지정하려는 것이지, 하나 또는 그 이상의 다른 특징들이나 숫자, 단계, 동작, 구성요소, 부분품 또는 이들을 조합한 것들의 존재 또는 부가 가능성을 미리 배제하지 않는 것으로 이해되어야 한다.The terminology used herein is only used to describe particular implementations (modes, aspects) (or examples) and is not intended to be limiting of the present invention. The singular expressions include plural expressions unless the context clearly dictates otherwise. In this application, it should be understood that terms such as “comprises” or “consists of” are intended to specify the presence of a feature, number, step, operation, component, part or combination thereof described in the specification, but do not exclude in advance the possibility of the presence or addition of one or more other features, numbers, steps, operations, components, parts or combinations thereof.

다르게 정의되지 않는 한, 기술적이거나 과학적인 용어를 포함해서 여기서 사용되는 모든 용어들은 본 발명이 속하는 기술 분야에서 통상의 지식을 가진 자에 의해 일반적으로 이해되는 것과 동일한 의미를 가지고 있다. 일반적으로 사용되는 사전에 정의되어 있는 것과 같은 용어들은 관련 기술의 문맥 상 가지는 의미와 일치하는 의미를 가지는 것으로 해석되어야 하며, 본 출원에서 명백하게 정의하지 않는 한, 이상적이거나 과도하게 형식적인 의미로 해석되지 않는다.Unless otherwise defined, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Terms defined in commonly used dictionaries, such as those defined in common dictionaries, should be interpreted as having a meaning consistent with the meaning they have in the context of the relevant art, and will not be interpreted in an idealized or overly formal sense unless expressly defined in this application.

본 발명에 따른 수소가스 감지용 실리콘 테이프 조성물, 그 수소가스 감지 실리콘 테이프, 그 제조방법은 기본 조성물로 A silicon tape composition for detecting hydrogen gas according to the present invention, a silicon tape for detecting hydrogen gas, and a method for producing the same are as follows:

수소가스 감지제와, 폴리디메틸실록산(Polydimethylsiloxane(이하 'PDMS'로 함)와, 백금촉매를 포함하여 이루어진다.It is composed of a hydrogen gas detector, polydimethylsiloxane (hereinafter referred to as 'PDMS'), and a platinum catalyst.

구체적으로 수소가스 감지제 30 중량부에 대하여 PDMS 600~1200 중량부 및 백금촉매 0.5~3 중량부로 구성되는 것이 바람직하다.
상기 PDMS는 VTP(Vinyl Terminated Polydimethylsiloxane)와 함께
hTPS(Hydride Terminated Polydimethylsiloxane) 또는 HTPS(Hydroxyl Terminated Polydimethylsiloxane), 또는 hTPS 및 HTPS 둘 모두의 혼합으로 구성되는 것이 바람직하다.
상기 PDMS는 VTP 100 중량부에 대하여 hTPS 10~80 중량부, HTPS 0~120 중량부의 혼합으로 구성되는 것이 바람직하다.
Specifically, it is preferable to comprise 600 to 1,200 parts by weight of PDMS and 0.5 to 3 parts by weight of platinum catalyst per 30 parts by weight of hydrogen gas detector.
The above PDMS is used together with VTP (Vinyl Terminated Polydimethylsiloxane).
It is preferable that it be composed of hTPS (Hydride Terminated Polydimethylsiloxane) or HTPS (Hydroxyl Terminated Polydimethylsiloxane), or a mixture of both hTPS and HTPS.
It is preferable that the above PDMS is composed of a mixture of 10 to 80 parts by weight of hTPS and 0 to 120 parts by weight of HTPS with respect to 100 parts by weight of VTP.

또 테이프의 변색 시인성 향상제가 더 첨가되는 것이 바람직한데,It is also desirable to add a discoloration visibility enhancer to the tape.

이 변색 시인성 향상제는 알루미나인 것이 바람직하며, 이 경우 알루미나는 테이프의 인장강도 향상에도 일조한다.It is preferred that this discoloration visibility enhancer be alumina, in which case the alumina also helps to improve the tensile strength of the tape.

아울러 본 발명은 경화지연제가 더 첨가되는 것을 좋고, 이 경화지연제는 메틸비닐시클로실록산(MVC)일 수 있다.In addition, the present invention preferably further includes a curing retarder, and the curing retarder may be methylvinylcyclosiloxane (MVC).

기초적으로 수소가스 감지제는 PdO(Palladium Oxide)를 사용하는 것이 바람직하다.Basically, it is desirable to use PdO (Palladium Oxide) as a hydrogen gas detector.

또 수소가스 감지제는 조작 용이성, 물질 안정성, 보존성 등을 고려하여 담체에 수용된 것이 바람직하며, 그 담체의 예로는 제올라이트(Zeolite), TiO2, SiO2, ZnO, Al2O3 등의 다공성 물질(이 중 하나, 일부 또는 모두일 수 있다)을 활용할 수 있고, 이중 제올라이트가 적합하다.In addition, the hydrogen gas detector is preferably contained in a carrier considering ease of operation, material stability, and preservability. Examples of the carrier include porous materials such as zeolite, TiO 2 , SiO 2 , ZnO, and Al 2 O 3 (one, some, or all of these may be used), and among these, zeolite is suitable.

즉, PdCl2를 담체인 제올라이트에 혼합하여 담지한다.That is, PdCl 2 is mixed and supported on zeolite, which is a carrier.

나아가 수소가스 감지 원리는 아래와 같으며, 본 발명에 따른 테이프를 이용한 수소가스 감지 전후의 변색은 도 1의 비교 사진에서 확인할 수 있다.Furthermore, the principle of hydrogen gas detection is as follows, and the discoloration before and after hydrogen gas detection using the tape according to the present invention can be confirmed in the comparative photograph of Fig. 1.

PdO (Brown) + H2 → Pd (Gray)+ H2O PdO (Brown) + H 2 → Pd (Gray) + H 2 O

[조성물의 성분에 대한 설명][Description of the composition's ingredients]

본 발명에 따른 수소가스 감지 실리콘 테이프는 특히 다양한 분야에 안정적으로 적용되도록 실리콘 테이프를 채용하는 것이 바람직하며, 실리콘 테이프는 비닐(Vinyl)기, 수소(H)기, 수산(OH)기가 부여된 실리콘을 혼합 사용하여 기능성 향상을 도모하였다. 또 실리콘의 경화반응은 부가반응형으로 백금(Pt)촉매를 채용하는 것이 바람직하다.According to the present invention, it is preferable to adopt a silicone tape so that the hydrogen gas detection silicone tape can be stably applied to various fields, and the silicone tape is intended to improve functionality by mixing and using silicone to which a vinyl group, a hydrogen (H) group, and an hydroxyl (OH) group are assigned. In addition, it is preferable to adopt a platinum (Pt) catalyst as the curing reaction of the silicone is an addition reaction type.

○ 말단 비닐기를 갖는 폴리디메틸실록산(Vinyl terminated Polydimethylsiloxane(이하 'PDMS'로 함)○ Vinyl terminated polydimethylsiloxane (hereinafter referred to as 'PDMS') having a terminal vinyl group

실리콘의 기재(Back-bone) 역할을 한다.It serves as the backbone of silicon.

○ 말단 수소기를 갖는 PDMS(Hydride terminated PDMS)○ PDMS with terminal hydrogen groups (Hydride terminated PDMS)

가교제 (Cross-linker) 역할을 한다.It acts as a cross-linker.

○ 말단 수산기를 갖는 PDMS(Hydroxyl terminated PDMS)○ PDMS with terminal hydroxyl groups (Hydroxyl terminated PDMS)

수산기 특유의 점착 특성을 부여한다(부가경화에 참여하지 않는 -OH를 부여하여 피착물에 대한 점착력을 확보할 수 있다).It provides adhesive properties unique to hydroxyl groups (by providing -OH, which does not participate in additional curing, adhesive strength to the adherend can be secured).

○ Pt 촉매○ Pt catalyst

실리콘의 경화반응을 유도한다.Induces curing reaction of silicone.

<Silicone 반응 예><Silicone reaction example>

Hydride terminated PDMS + Vinyl terminated PDMS (Pt 촉매 사용) Hydride terminated PDMS + Vinyl terminated PDMS (using Pt catalyst)

{Source: Gelest社 카탈로그}{Source: Gelest catalog}

아울러 수소가스 감지를 위한 필러는 다음과 같다.In addition, the fillers for hydrogen gas detection are as follows.

○ PdO/담체○ PdO/Carrier

PdO는 수소가스와 반응하여 변색 특성을 나타내며, 제올라이트, TiO2, SiO2, ZnO, Al2O3는 PdO의 담체 역할을 하며, 제올라이트가 적합하다.PdO exhibits discoloration properties when reacted with hydrogen gas, and zeolite, TiO 2 , SiO 2 , ZnO, and Al 2 O 3 act as carriers for PdO, with zeolite being suitable.

○ 알루미나(Al22O3)○ Alumina (Al 2 2O 3 )

PdO의 색변화의 시인성(색 대비 효과)을 극대화하며(즉, 변색 시인성 향상제로 기능한다) 아울러 테이프의 인장강도 증가에도 일조한다.It maximizes the visibility of color change (color contrast effect) of PdO (i.e., functions as a color change visibility enhancer) and also helps increase the tensile strength of the tape.

○ 경화지연제(inhibitor)○ Curing inhibitor

경화지연제인 Inhibitor MVC(메틸비닐시클로실록산)를 사용한다.Inhibitor MVC (methylvinylcyclosiloxane), a curing retardant, is used.

이하 본 발명은 구체 실시예 및 비교예를 통하여 더 잘 이해될 수 있다.The present invention can be better understood through specific examples and comparative examples.

[실시예 및 비교예][Examples and Comparative Examples]

구 분(단위:중량%)Classification (unit: weight%) 실시예 ①Example ① 실시예 ②Example ② 실시예 ③Example ③ 실시예 ④Example ④ 실시예 ⑤Example ⑤ 실시예 ⑥Example ⑥ 실시예 ⑦Example ⑦ 실시예 ⑧Example ⑧ 실시예 ⑨Example ⑨ VTPVTP 21.1621.16 20.920.9 21.321.3 21.121.1 21.121.1 21.121.1 12.512.5 21.721.7 23.923.9 Silicone GUMSilicone GUM 55.755.7 53.153.1 51.751.7 49.649.6 51.651.6 49.249.2 62.462.4 5353 59.859.8 hTPS- 가교제 hTPS- crosslinker 5.15.1 66 4.74.7 5.15.1 55 55 4.24.2 2.72.7 2.92.9 HTPS- 50 cps HTPS- 50 cps 7.37.3 7.27.2 7.47.4 7.37.3 7.37.3 7.37.3 7.37.3 7.57.5 00 Catalyst- Pt 촉매 Catalyst- Pt catalyst 0.070.07 0.070.07 0.070.07 0.20.2 0.30.3 0.70.7 0.370.37 0.30.3 0.250.25 Filler- Al2O3 Filler- Al 2 O 3 77 88 99 1010 77 88 99 1010 77 Filler- SiO2 Filler- SiO 2 0.070.07 0.130.13 0.130.13 0.10.1 0.10.1 0.10.1 0.130.13 0.10.1 0.150.15 InhibitorInhibitor 11 22 33 44 55 66 11 22 33 수소가스감지제Hydrogen gas detector 2.62.6 2.62.6 2.72.7 2.62.6 2.62.6 2.62.6 3.13.1 2.72.7 33 MS-
adhesion promoter
MS-
adhesion promoter
2.62.6 2.62.6 2.72.7 2.62.6 2.62.6 2.62.6 3.13.1 2.72.7 33
수소가스 감지제 담체Hydrogen gas detector carrier 제올라이트Zeolite 제올라이트Zeolite 제올라이트Zeolite 제올라이트Zeolite 제올라이트Zeolite 제올라이트Zeolite 제올라이트Zeolite 제올라이트Zeolite 제올라이트Zeolite

구 분(단위:중량%)Classification (unit: weight%) 실시예 ⑩Example ⑩ 실시예 ⑪Example ⑪ 실시예 ⑫Example ⑫ 실시예 ⑬Example ⑬ 실시예 ⑭Example ⑭ 비교예①Comparative Example ① 비교예②Comparative Example ② 비교예③Comparative Example ③ 비교예④Comparative Example ④ 비교예⑤Comparative Example ⑤ VTPVTP 23.723.7 23.723.7 13.913.9 6.46.4 5.65.6 78.378.3 71.971.9 74.374.3 7272 25.825.8 Silicone GUMSilicone GUM 57.857.8 55.455.4 6464 78.578.5 69.169.1 00 00 00 00 35.335.3 hTPS- 가교제 hTPS- crosslinker 2.92.9 2.92.9 2.32.3 22 3.53.5 1.81.8 1.61.6 2.62.6 2.42.4 7.77.7 HTPS- 50 cps HTPS- 50 cps 00 00 00 00 7.57.5 7.87.8 14.514.5 11.111.1 14.414.4 6.16.1 Catalyst- Pt 촉매 Catalyst- Pt catalyst 0.410.41 0.820.82 0.20.2 0.40.4 0.750.75 0.20.2 0.10.1 0.10.1 0.10.1 0.10.1 Filler- Al2O3 Filler- Al 2 O 3 88 99 1010 88 99 8.88.8 8.88.8 8.88.8 00 8.88.8 Filler- SiO2 Filler- SiO 2 0.190.19 0.180.18 0.10.1 0.10.1 0.150.15 00 00 00 88 00 InhibitorInhibitor 44 55 66 33 33 0.10.1 0.10.1 0.10.1 0.10.1 0.10.1 수소가스감지제Hydrogen gas detector 33 33 3.53.5 1.61.6 1.41.4 33 33 33 33 33 MS-
adhesion promoter
MS-
adhesion promoter
33 33 3.53.5 1.61.6 1.41.4 00 00 00 00 13.113.1
수소가스 감지제 담체Hydrogen gas detector carrier 제올라이트Zeolite TiO₂TiO₂ SiO2 SiO 2 ZnOZnO Al2O3 Al 2 O 3 제올라이트Zeolite 제올라이트Zeolite 제올라이트Zeolite 제올라이트Zeolite 제올라이트Zeolite

*VTP = Vinyl Terminated Polydimethylsiloxane* VTP = Vinyl Terminated Polydimethylsiloxane

*hTPS = Hydride Terminated Polydimethylsiloxane* hTPS = Hydride Terminated Polydimethylsiloxane

*HTPS = Hydroxyl Terminated Polydimethylsiloxane* HTPS = Hydroxyl Terminated Polydimethylsiloxane

*MS = Methacylate Silane* MS = Methacylate Silane

[제조예 : 수소가스 감지 실리콘 테이프를 제조하기 위한 전체 조성물 제조][Manufacturing Example: Manufacturing of the entire composition for manufacturing a hydrogen gas detection silicone tape]

○ 수소가스 감지제 제조○ Manufacturing of hydrogen gas detector

1. Substrate(담체)(제올라이트(Zeolite), TiO2, SiO2 또는 ZnO)와 함께 PdCl2 및 물(H2O)을 혼합하여 제조한다.1. Prepare by mixing PdCl 2 and water (H 2 O) with a substrate (zeolite, TiO 2, SiO 2 or ZnO).

PdCl2는 담체 대비 2~4 phr로 투입한다. PdCl 2 is added at 2 to 4 phr relative to the carrier.

2. 10분간 교반하며, 반응온도는 상온(RT)~60 ℃이다.2. Stir for 10 minutes, and the reaction temperature is room temperature (RT) to 60 ℃.

3. pH Control; 묽은염산을 이용하여 용액의 pH를 7로 조절한다.3. pH Control; Adjust the pH of the solution to 7 using diluted hydrochloric acid.

4. 60분간 교반하며, 반응온도는 상온~60 ℃이다.4. Stir for 60 minutes, and the reaction temperature is room temperature to 60 ℃.

5. 필터를 이용하여 가압 필터링 한다.(0.2 ㎛ Membrane filter with washing).5. Pressure filter using a filter (0.2 ㎛ Membrane filter with washing).

6. 12시간 동안 건조하여(건조온도: 120 ℃) PdO/담체 분말 수득한다.6. Dry for 12 hours (drying temperature: 120 ℃) to obtain PdO/carrier powder.

○ 원료 배합비 ○ Raw material mixing ratio

수소가스 감지제인 PdO/Zeolite 100 중량부를 기준으로Based on 100 parts by weight of PdO/Zeolite, a hydrogen gas detector

각 실시예 및 비교예의 나머지 조성물을 2,000~4,000 중량부, 바람직하기로는 2,500~3,800 중량부, 보다 바람직하기로는 2,800~3,500 배합한다.The remaining composition of each example and comparative example is mixed in an amount of 2,000 to 4,000 parts by weight, preferably 2,500 to 3,800 parts by weight, more preferably 2,800 to 3,500 parts by weight.

또 상기 말단 비닐기를 갖는 PDMS(VTP)는 서로 다른 점도를 갖는 것을 혼합하여 사용하여 수소가스 감지제(Detector)인 PdO/담체에 대한 분산 특성을 확보하는 데 일조할 수 있다. 예를 들어 1000 cps 점도의 VTP 100 중량부에 대하여 20000 cps 점도의 VTP 90~120 중량부, 65000 cps 점도의 VTP 40~60 중량부를 혼합하여 사용하는 것이 적합하다.In addition, PDMS (VTP) having the terminal vinyl group can be used by mixing those having different viscosities to help secure dispersion characteristics for PdO/carrier, which is a hydrogen gas detector. For example, it is suitable to mix and use 90 to 120 parts by weight of VTP having a viscosity of 20,000 cps and 40 to 60 parts by weight of VTP having a viscosity of 65,000 cps for 100 parts by weight of VTP having a viscosity of 1,000 cps.

○ 혼합(Planetary Mixing)○ Mixing (Planetary Mixing)

실시예 및 비교예별 조성물을 믹서(Planetary Mixer) 장비를 이용하여 혼합하는데,The compositions for each example and comparative example are mixed using a mixer (planetary mixer).

공전 블레이드 기준 60 rpm으로 설정(자전 블레이드 120 rpm)하여 10분간 혼합한다.Set the idle blade speed to 60 rpm (rotating blade speed to 120 rpm) and mix for 10 minutes.

○ 밀링(Three Roll Milling)○ Milling (Three Roll Milling)

상기 혼합된 조성물내 존재하는 입자(필러)들을 분쇄/분산하는 공정으로,A process for crushing/dispersing particles (fillers) present in the above mixed composition.

실리콘 레진이 투입되는 롤의 갭을 20 ㎛, 토출되는 롤의 갭을 5 ㎛로 하여 밀링한다.Milling is performed with a gap of 20 ㎛ for the roll into which the silicone resin is injected and a gap of 5 ㎛ for the roll from which it is discharged.

○ 후공정; 필름화하여 수소가스 변색 관찰 ○ Post-processing; Filming and observing hydrogen gas discoloration

PET 기재에 300 ㎛ 습도막 두께로 코팅하여 120 ℃에서 10분간 경화하고, 경화된 필름은 수소가스에 노출하여 변색을 관찰한다.The PET substrate is coated with a moisture film thickness of 300 ㎛, cured at 120°C for 10 minutes, and the cured film is exposed to hydrogen gas to observe discoloration.

[실험예-변색 측정][Experimental Example - Discoloration Measurement]

경화된 필름은 수소가스에 노출하여 변색을 관찰한다.The cured film is exposed to hydrogen gas and discoloration is observed.

수소가스 노출 조건으로 4 % H2 가스에 1 mL/min의 유량으로 5분간 노출시켰다.(노출 전후 변색은 도 1 참조)Under hydrogen gas exposure conditions, it was exposed to 4% H2 gas at a flow rate of 1 mL/min for 5 minutes. (See Figure 1 for discoloration before and after exposure.)

본 발명의 실시예와 같이 수소가스 감지를 위한 필러로 알루미나(Al 2 O 3 )를 사용한 것이 아니라, 비교예와 같이 SiO 2 를 사용한 경우에는 아래 비교 사진에서 확인할 수 있는 바와 같이, 실시예(알루미나(Al 2 O 3 ))가 더 시인성이 더 뛰어남을 확인할 수 있다.In the case where SiO 2 was used as in the comparative example instead of alumina (Al 2 O 3 ) as a filler for detecting hydrogen gas as in the embodiment of the present invention, it can be confirmed that the embodiment (alumina (Al 2 O 3 )) has better visibility as can be confirmed in the comparative photo below.

[실시예들의 변색 사진][Discoloration photos of examples]

{좌측-브라운(변색 전), 우측-그레이(변색 후)}{Left - Brown (before discoloration), Right - Gray (after discoloration)}

[비교예 4의 변색 사진][Discoloration photo of Comparative Example 4]

{좌측-라이트 브라운 또는 아이보리(변색 전), 우측-라이트 그레이 (변색 후)}{Left - Light brown or ivory (before discoloration), Right - Light gray (after discoloration)}

[실험예-인장강도 측정][Experimental example - tensile strength measurement]

구 분 division 인장강도 (N/㎟)Tensile strength (N/㎟) 연신율 (%)Elongation (%) 실시예 1Example 1 3.463.46 372372 실시예 2Example 2 3.343.34 390390 실시예 3Example 3 3.423.42 390390 실시예 4Example 4 3.073.07 332332 실시예 5Example 5 4.044.04 338338 실시예 6Example 6 3.783.78 296296 실시예 7Example 7 2.872.87 364364 실시예 8Example 8 2.632.63 524524 실시예 9Example 9 2.962.96 532532 실시예 10Example 10 3.063.06 464464 실시예 11Example 11 3.173.17 441441 실시예 12Example 12 2.802.80 597597 실시예 13Example 13 2.922.92 543543 실시예 14Example 14 2.922.92 443443 비교예 1Comparative Example 1 0.62 0.62 340340 비교예 2Comparative Example 2 0.27 0.27 271271 비교예 3Comparative Example 3 0.48 0.48 204204 비교예 4Comparative Example 4 0.29 0.29 113113 비교예 5Comparative Example 5 0.92 0.92 168168

이상의 설명에서 수소가스 감지용 실리콘 테이프 조성물, 그 수소가스 감지 실리콘 테이프, 그 제조방법과 관련한 통상의 공지된 기술은 생략되어 있으나, 당업자라면 용이하게 이를 추측 및 추론하고 재현할 수 있다.In the above description, conventionally known techniques related to the silicon tape composition for detecting hydrogen gas, the silicon tape for detecting hydrogen gas, and the manufacturing method thereof have been omitted, but those skilled in the art can easily guess, infer, and reproduce them.

Claims (14)

수소가스 감지제와, PDMS(Polydimethylsiloxane)와, 백금촉매를 포함하고,
상기 PDMS는 VTP(Vinyl Terminated Polydimethylsiloxane)와 함께 hTPS(Hydride Terminated Polydimethylsiloxane) 및 HTPS(Hydroxyl Terminated Polydimethylsiloxane)의 혼합으로 구성되고,
상기 VTP는 1000 cps 점도의 VTP 100 중량부에 대하여 20000 cps 점도의 VTP 90~120 중량부, 65000 cps 점도의 VTP 40~60 중량부를 혼합하여 사용하는 것을 특징으로 하는 수소가스 감지용 실리콘 테이프 조성물.
Contains a hydrogen gas detector, PDMS (Polydimethylsiloxane), and a platinum catalyst.
The above PDMS is composed of a mixture of VTP (Vinyl Terminated Polydimethylsiloxane) and hTPS (Hydride Terminated Polydimethylsiloxane) and HTPS (Hydroxyl Terminated Polydimethylsiloxane).
The above VTP is a silicone tape composition for detecting hydrogen gas, characterized in that it is used by mixing 90 to 120 parts by weight of VTP having a viscosity of 20,000 cps and 40 to 60 parts by weight of VTP having a viscosity of 65,000 cps, per 100 parts by weight of VTP having a viscosity of 1,000 cps.
제 1 항에 있어서,
상기 수소가스 감지제는 PdO를 사용하고, 담체는 제올라이트, TiO2, SiO2, ZnO, Al2O3 중 일부 또는 모두인 것을 특징으로 하는 수소가스 감지용 실리콘 테이프 조성물.
In paragraph 1,
A silicone tape composition for detecting hydrogen gas, characterized in that the hydrogen gas detector uses PdO and the carrier is some or all of zeolite, TiO2, SiO2, ZnO, and Al2O3.
제 1 항에 있어서,
상기 수소가스 감지제 30 중량부에 대하여 PDMS 600~1200 중량부 및 백금촉매 0.5~3 중량부로 구성되는 것을 특징으로 하는 수소가스 감지용 실리콘 테이프 조성물.
In paragraph 1,
A silicone tape composition for hydrogen gas detection, characterized in that it comprises 600 to 1,200 parts by weight of PDMS and 0.5 to 3 parts by weight of a platinum catalyst with respect to 30 parts by weight of the hydrogen gas detector.
제 1 항 내지 제 3 항 중 어느 한 항에 있어서,
테이프의 변색 시인성 향상제가 더 첨가되는 것을 특징으로 하는 수소가스 감지용 실리콘 테이프 조성물.
In any one of claims 1 to 3,
A silicone tape composition for detecting hydrogen gas, characterized in that a discoloration visibility improving agent is further added to the tape.
제 4 항에 있어서,
상기 변색 시인성 향상제는 알루미나인 것을 특징으로 하는 수소가스 감지용 실리콘 테이프 조성물.
In paragraph 4,
A silicone tape composition for detecting hydrogen gas, characterized in that the discoloration visibility improving agent is alumina.
제 1 항 내지 제 3 항 중 어느 한 항에 있어서,
경화지연제가 더 첨가되는 것을 특징으로 하는 수소가스 감지용 실리콘 테이프 조성물.
In any one of claims 1 to 3,
A silicone tape composition for detecting hydrogen gas, characterized in that a curing retarder is further added.
제 6 항에 있어서,
상기 경화지연제는 메틸비닐시클로실록산(MVC)인 것을 특징으로 하는 수소가스 감지용 실리콘 테이프 조성물.
In paragraph 6,
A silicone tape composition for detecting hydrogen gas, characterized in that the curing retarder is methylvinylcyclosiloxane (MVC).
제 1 항 내지 제 3 항 중 어느 한 항에 있어서,
접착성 향상제(adhesion promoter)가 더 첨가되는 것을 특징으로 하는 수소가스 감지용 실리콘 테이프 조성물.
In any one of claims 1 to 3,
A silicone tape composition for hydrogen gas detection characterized in that an adhesion promoter is further added.
제 1 항 내지 제 3 항 중 어느 한 항에 있어서,
인장강도 향상제(Filler)가 더 첨가되는 것을 특징으로 하는 수소가스 감지용 실리콘 테이프 조성물.
In any one of claims 1 to 3,
A silicone tape composition for hydrogen gas detection characterized by further adding a tensile strength improving agent (filler).
삭제delete 삭제delete 삭제delete 삭제delete 청구항 1에 따른 조성물을 이용하여 제조되는 수소가스 감지용 실리콘 테이프.A silicone tape for detecting hydrogen gas, manufactured using the composition according to claim 1.
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