WO2024010229A1 - Composition de capteur pour la détection de fuite d'hydrogène et ruban adhésif la contenant - Google Patents

Composition de capteur pour la détection de fuite d'hydrogène et ruban adhésif la contenant Download PDF

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Publication number
WO2024010229A1
WO2024010229A1 PCT/KR2023/007737 KR2023007737W WO2024010229A1 WO 2024010229 A1 WO2024010229 A1 WO 2024010229A1 KR 2023007737 W KR2023007737 W KR 2023007737W WO 2024010229 A1 WO2024010229 A1 WO 2024010229A1
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adhesive
hydrogen
polymer material
sample
discoloration
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PCT/KR2023/007737
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English (en)
Korean (ko)
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심춘택
엄주흥
황상일
고경훈
전재선
정진우
김남윤
정경민
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주식회사 대현에스티
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Publication of WO2024010229A1 publication Critical patent/WO2024010229A1/fr

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
    • G01M3/00—Investigating fluid-tightness of structures
    • G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
    • G01M3/04—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point
    • G01M3/20—Investigating fluid-tightness of structures by using fluid or vacuum by detecting the presence of fluid at the leakage point using special tracer materials, e.g. dye, fluorescent material, radioactive material
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
    • G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00

Definitions

  • the present invention relates to a sensor composition for detecting hydrogen leakage, and more specifically, to a sensor composition for detecting hydrogen leakage comprising a discoloring composite for detecting hydrogen leakage and an adhesive polymer material, and to an adhesive tape containing the same.
  • Hydrogen has the physical properties of low density (0.0899kg/m 3 ), low boiling point (20.39K), and high diffusion coefficient (0.61cm 2 /s in air), very low critical ignition energy (0.017mJ), and heat of combustion. It is a very high gas (142kJ/g H 2 ), has a wide explosion range (4 ⁇ 75%), has a very fast combustion rate, and has a low ignition temperature of 560°C.
  • hydrogen is a colorless, odorless, flammable gas that cannot be detected by human perception, and can be easily ignited by external factors (flame, electric shock, etc.), especially at concentrations above 4% in the air. Therefore, hydrogen is used as a warning system for this. Sensors for leak detection are essential, and above all, early detection of hydrogen leaks is very important.
  • Patent No. 10-1933313 which is a prior art, a hydrogen detection sensor using a discoloring composite made of palladium nanoparticles formed on the surface of two-dimensional tungsten oxide is disclosed.
  • a hydrogen detection sensor composed of a single adhesive layer including a discoloring composite and an adhesive component is disclosed. Not starting.
  • the senor's color-changing ability may weaken over time because the color-changing composite is directly exposed to oxygen or water vapor in the external environment.
  • the present invention provides a sensor composition for detecting hydrogen leakage, including a color change composite that reacts to hydrogen and an adhesive polymer material.
  • the discoloring composite is a discoloring composite in which palladium (Pd) particles are coated on tungsten oxide (WO 3 ) or molybdenum oxide (MoO 3 ), and the mixing ratio (weight ratio) of the discoloring composite and the adhesive polymer material is ) is characterized in that it is 1:100 to 60:100.
  • the adhesive polymer material includes a silicone adhesive, a resin, and rubber, and in addition to the polymer material, silica and a curing agent are included.
  • the silicone adhesive is polydimethylsiloxane, organopolysiloxane, polymethylphenylsiloxane, polyethylphenylsiloxane, polyalkylphenylsiloxane, vinyl It is characterized by using one type of polysiloxane (vinylpolysiloxane) or methylpolysiloxane (methylpolysiloxane) or a mixture of two or more types.
  • the resin uses one or two or more of organopolysiloxane, silsesquioxane, and tetra(trimethylsiloxy)silane. It is characterized by being used in combination.
  • a self-adhesive type tape for detecting hydrogen leakage in which a sensor composition for detecting hydrogen leakage is applied in a single layer with a thickness of 30 to 200 ⁇ m between release films to form a hydrogen detection sensor adhesive layer.
  • the base film is characterized in that it is a PET, PEN, PI, PP, PE, PO, or TPU film.
  • the adhesive polymer material used in the adhesive tape for hydrogen detection including the base film is characterized by being made by mixing an acrylic adhesive or a silicone adhesive with a curing agent.
  • the sensor composition for detecting hydrogen leakage according to the present invention and the adhesive tape containing the same are cheaper and easier to install than mechanical sensors, and do not require an electrical signal and do not require a special explosion-proof function, so they are easy to install and manage. .
  • the structure has an adhesive layer containing a discoloration complex for detecting hydrogen leaks, making it easy to attach to the desired part of the user, and the excellent hydrogen detection ability enables accurate hydrogen detection regardless of location and location, and can easily check for leaks with the naked eye. This is possible, and the polymer can prevent the sensing complex from being oxidized by moisture.
  • FIG. 1 is a schematic diagram of a self-adhesive tape for detecting hydrogen leakage according to an embodiment of the present invention.
  • Figure 2 is a diagram showing discoloration of a self-adhesive tape for hydrogen leak detection (sample 12) using WO 3 -Pd discoloration composite.
  • Figure 3 is a picture showing discoloration of self-adhesive tapes (a) sample 14, (b) sample 15, and (c) sample 16 for hydrogen leak detection using MoO 3 -Pd discoloration composite.
  • Figure 4 is a schematic diagram of an adhesive tape for detecting hydrogen leakage including a base film according to an embodiment of the present invention.
  • FIG. 1 is a schematic diagram of a self-adhesive tape for detecting hydrogen leakage according to an embodiment of the present invention.
  • a hydrogen sensing sensor adhesive layer 20 made of a sensor composition for detecting hydrogen leakage is located between the release films 10 and 30.
  • the sensor composition for detecting hydrogen leakage can be manufactured by mixing a color-changing composite that changes color when reacting with hydrogen and an adhesive polymer material that provides adhesion, and will be described in detail with reference to examples below.
  • the WO 3 -Pd color change complex which is one of the color change complexes for hydrogen sensing, is synthesized by the following sequence.
  • tungsten oxide hydrate (WO 3 ⁇ nH 2 O) powder separated from Na + is obtained through centrifugation.
  • the powder is annealed at 500°C for 2 hours to produce crystallized two-dimensional tungsten oxide (2D-WO 3 ).
  • the palladium (Pd) precursor solution was prepared by mixing 10 mL of methyl alcohol and 3 mg of 0.25mM palladium chloride (PdCl 2 ) as a solvent, then added 10 mg of polyvinylpyrrolidone (PVP, molecular weight 40,000) and incubated for 2 hours. Prepare the palladium precursor solution by sonicating for a while.
  • PVP polyvinylpyrrolidone
  • the MoO 3 -Pd discoloration composite for hydrogen sensing which is another embodiment of the present invention, is manufactured by the following sequence. First, add 1 g of molybdenum oxide (MoO 3 , Sigma-aldrich) to 600 mL of methyl alcohol and disperse it using an ultrasonicator. In the present invention, molybdenum oxide was purchased and used, but it can also be manufactured using hydrothermal synthesis, etc.
  • MoO 3 molybdenum oxide
  • a palladium precursor solution was prepared by mixing 10 mL of methyl alcohol as a solvent and 3 mg of 0.25mM palladium chloride (PdCl 2 ), then 10 mg of polyvinylpyrrolidone (PVP, molecular weight 40,000) was added and sonicated for 2 hours. Prepare a palladium precursor solution.
  • PdCl 2 0.25mM palladium chloride
  • PVP polyvinylpyrrolidone
  • the MoO 3 -Pd discoloration composite was prepared by mixing the molybdenum oxide (MoO 3 ) dispersed solution and the palladium precursor solution and irradiating them with ultraviolet rays for 2 minutes while stirring.
  • the hydrogen leak detection adhesive tape of the present invention can be divided into two types. First, we will explain the self-adhesive type tape. Self-adhesive tape has a certain level of elasticity (Young's Modulus) and is stretchable, so it can be easily attached by deforming in various ways depending on the area to which it is attached.
  • Young's Modulus Young's Modulus
  • a hydrogen detection sensor in order to be easy for users to use, maintain adhesive properties, and be usable for a long time, a hydrogen detection sensor must not only have good hydrogen gas permeability, but also exhibit elasticity (Young's Modulus) above a certain level.
  • the oxidation of the discoloration complex due to penetration of moisture in the atmosphere, thereby weakening the discoloration reaction must be suppressed as much as possible.
  • the present invention uses a general-purpose silicone adhesive as a base, and adds a resin that increases the hardness or hardness of the adhesive layer, a rubber that increases elasticity, and silica as a filler.
  • the adhesive polymer material composition was completed by adding a curing agent to cure the silicone adhesive used as a base.
  • the silicone adhesives to be used as a base include polydimethylsiloxane, organopolysiloxane, polymethylphenylsiloxane, methylpolysiloxane, polyethylphenylsiloxane, vinylpolysiloxane, and polysiloxane.
  • One type of alkylphenylsiloxane (polyalkylphenylsiloxane) was used or a mixture of two or more types was used.
  • silicone resin To secure the hardness or hardness of the adhesive layer, silicone resin was used.
  • the silicone resins include organopolysiloxane, tetra(trimethylsiloxy)silane, and silsesquioxane.
  • One type of (Silsesquioxane) was used or a mixture of two or more types was used.
  • Silicone rubber was additionally added to ensure the elasticity of the adhesive layer, and organopolysiloxane was used for this purpose.
  • Silica used as a filler can be used alone or in combination of amorphous silica and spherical silica.
  • crystalline silica When crystalline silica is used alone, a problem occurs in which the adhesive layer turns white, and when only amorphous silica is used, elasticity decreases because it cannot be used above a certain amount. Therefore, depending on the type of product, amorphous silica and spherical silica can be mixed and used with different ingredient ratios.
  • the amount of silica used is preferably 5 to 10 parts by weight based on a total of 100 parts by weight of the silicone adhesive, resin, and rubber. If silica is not included, the elastic modulus is lowered, and if silica is too much, dispersibility deteriorates.
  • the curing agent includes benzoyl peroxide, t-butyl peroxybenzoate, dicumyl peroxide, t-butylcumyl peroxide, di-t-butyl peroxide, 2,5-dimethyl-2,5-di(t-butyl) Peroxy)hexane, 2,4-dichlorobenzoyl peroxide, 1,1-bis(t-butylperoxy)-3,3,5-trimethylcyclohexane, 2,5-dimethyl2,5-di(t- Butyl peroxy)hexene-3, dibenzoyl peroxide, or any of its derivatives can be used.
  • the amount of curing agent used is preferably 2 to 10 parts by weight based on a total of 100 parts by weight of the silicone adhesive, resin, and rubber. If the curing agent is less than 2 parts by weight, curing is difficult or takes a long time, and the curing agent is used at 10 parts by weight. As it grows larger, crystallization occurs on the surface.
  • Table 1 below is a sample table prepared by varying the component ratio of the adhesive polymer material composition that provides the adhesive function to the self-adhesive tape.
  • the base adhesive polydimethylsiloxane
  • resin tetra(trimethylsiloxy)silane
  • rubber organopolysiloxane
  • each weight part of silica (non-crystalline silica) and curing agent (dibenzoyl peroxide) is calculated as phr (parts per hundred resin (here) Resin refers to the total polymer and is expressed as)).
  • the sample preparation method used a 50 ⁇ m thick fluorine-coated release film, and the adhesive layer was coated with a 100 ⁇ m thickness. By laminating the release film, sample production was completed to evaluate the characteristics of the composition forming the adhesive layer. .
  • Sample Result Young's Modulus (kgf/mm2) Release film peeling note Sample 1 0.18 delamination instability Sample 2 0.21 Good peeling Sample 3 0.34 Good peeling Sample 4 1.11 Good peeling When stretched, it turns white. Sample 5 0.09 delamination instability Sample 6 0.63 Good peeling When stretched, it turns white. Sample 7 0.47 delamination instability When stretched, it turns white.
  • Table 2 shows test results of adhesive polymer material compositions for self-adhesive type. As shown in Table 2, in the case of Samples 2 to 7 containing silica as a filler, Young's Modulus mostly increased slightly compared to Sample 1, which did not contain silica.
  • Table 3 below is a sample table prepared by mixing sample 6, which showed good results in peeling from the release film, while changing the content of the WO 3 -Pd complex.
  • the component ratio of the adhesive polymer material was applied based on Sample 6, and the content of the color change composite (WO 3 -Pd) was tested while varying from 0 to 20 parts by weight based on 100 parts by weight of the total adhesive polymer material. proceeded.
  • composition Sample 8 Sample 9 Sample 10 Sample 11 Sample 12 Sample 13 Sample 6 based adhesive polymer material (parts by weight) 100 100 100 100 100 100 100 Discoloration complex (parts by weight) One 2 5 10 20
  • Table 4 below is a table of results evaluating the discoloration ability of samples 8 to 13 by hydrogen concentration.
  • the degree of discoloration of the sample due to hydrogen reaction is determined by adding hydrogen gas at different concentrations (mixture of nitrogen gas and hydrogen gas) into the hydrogen chamber, reacting the sample and hydrogen for 5 minutes, and measuring the color change ( ⁇ E) of the sample as the color difference. It was confirmed through the system (Konica minolta, CM-3600d). At this time, the reference point for judging color change is the color of the sample before it is discolored by hydrogen.
  • Figure 2 is a picture showing the results of manufacturing a self-adhesive type tape based on Sample 12 and confirming the color change due to hydrogen leakage. As a result of the experiment, it was confirmed that the tape before reaction with hydrogen (left) changed to a dark color after reaction with hydrogen (right).
  • the appropriate mixing ratio of the color-changing composite and the adhesive polymer material is preferably 1 to 60 parts by weight of the color-changing composite relative to 100 parts by weight of the total adhesive polymer materials, and more preferably, the weight of the color-changing composite is 1 to 60 parts by weight relative to 100 parts by weight of the total polymer materials. 20 parts by weight is appropriate. If the discoloration composite exceeds 60 parts by weight, the elasticity of the tape decreases, making it difficult to use as a tape, and if the weight of the discoloration composite is less than 1 part by weight, it becomes difficult to confirm discoloration due to hydrogen leakage.
  • discoloration complex since the discoloration complex is not directly exposed to the outside, it is relatively less affected by moisture or oxygen compared to prior technologies, so it can be expected to be used for a longer period of time.
  • the composition ratio of the adhesive polymer material is applied based on the composition of Sample 6, as in the case of the previous WO 3 -Pd discoloring composite, and the content of the discoloring composite (MoO 3 -Pd) is 10 to 40 parts by weight compared to 100 parts by weight of the total adhesive polymer material.
  • the experiment was conducted with different parts.
  • composition Sample 14 Sample 15 Sample 16 Sample 17 Sample 6 based adhesive polymer material (parts by weight) 100 100 100 100 100 Discoloration complex (parts by weight) 10 20 30 40
  • the appropriate mixing ratio of the MoO 3 -Pd discoloring composite is 10 to 60 parts by weight based on 100 parts by weight of the total adhesive polymer material, and more preferably, 10 to 40 parts by weight of the discoloring composite is included.
  • the discoloration complex exceeds 60 parts by weight, the elasticity of the tape decreases, making it difficult to use as a tape, and if it is less than 1 part by weight, the degree of discoloration becomes weak, making it difficult to check whether hydrogen leaks.
  • Figure 3 is a diagram showing the degree of color change of the sample before reaction with hydrogen gas (top) and the sample after reaction (bottom). It can be seen that the greater the content of the discoloration complex compared to the adhesive polymer material, the darker the color.
  • (a) is an adhesive tape made of sample 14,
  • (b) is sample 15, and
  • (c) is sample 16.
  • Adhesive tape for hydrogen detection including base film
  • Film-type hydrogen sensors include a base film, so they have the advantage of being able to finely adjust physical properties according to consumer needs.
  • the film-type hydrogen sensor including the base film has a relatively simple manufacturing method compared to the self-adhesive type, can realize various physical properties, and is easy to attach to a large area.
  • the adhesive polymer material used in this type is manufactured using general-purpose adhesives such as acrylic, rubber, urethane, and silicone as a base, and adding only a curing agent to harden the adhesive.
  • the adhesive polymer material was mixed with the WO 3 -Pd or MoO 3 -Pd discoloration composite and used.
  • the curing agent includes benzoyl peroxide, t-butyl peroxybenzoate, dicumyl peroxide, t-butylcumyl peroxide, di-t-butyl peroxide, 2,5-dimethyl-2,5-di(t-butyl) Peroxy)hexane, 2,4-dichlorobenzoyl peroxide, 1,1-bis(t-butylperoxy)-3,3,5-trimethylcyclohexane, 2,5-dimethyl2,5-di(t- Butyl peroxy)hexene-3, dibenzoyl peroxide, or any of its derivatives can be used.
  • a sensor tape for detecting hydrogen leakage was manufactured by first synthesizing the WO 3 -Pd discoloration composite and then mixing it with the adhesive polymer material.
  • it will be described in detail in Example 1 below.
  • Sample 18 Sample 19 Sample 20 Sample 21 Sample 22 Sample 23 Film type PET PET P.O. P.O. TPU TPU Adhesive type acryl silicon acryl silicon acryl silicon acryl silicon
  • Table 7 below shows the results of the hydrogen reaction discoloration test conducted using the samples in Table 6.
  • mixed gas mixture of nitrogen gas and hydrogen gas
  • an adhesive polymer material based on an acrylic adhesive or a silicone adhesive was mixed with WO 3 -Pd discoloration composite at a weight ratio of 7:3, and then discoloration due to hydrogen leakage was checked. As a result, strong discoloration was confirmed. However, if the above ratio exceeds 7:3, the elasticity of the tape is expected to decrease, making it difficult to use it as a tape.

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Abstract

La présente invention concerne une composition de capteur pour détecter des fuites d'hydrogène et un ruban adhésif la contenant. Plus particulièrement, une composition de capteur est fabriquée par mélange d'un composite chromique constitué de WO3-Pd ou de MoO3-Pd avec un matériau polymère adhésif, puis par application de celui-ci entre des films de libération pour fournir un ruban auto-adhésif pour la détection de fuite d'hydrogène ou un ruban adhésif, comprenant un film de base, pour la détection de fuite d'hydrogène, fournissant ainsi un capteur de détection de fuite d'hydrogène qui peut être facilement installé et détecte visuellement des fuites d'hydrogène avec facilité.
PCT/KR2023/007737 2022-07-06 2023-06-07 Composition de capteur pour la détection de fuite d'hydrogène et ruban adhésif la contenant WO2024010229A1 (fr)

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KR1020220082885A KR102525775B1 (ko) 2022-07-06 2022-07-06 수소 누출 감지용 센서 조성물 및 이를 포함하는 점착 테이프
KR10-2022-0082885 2022-07-06

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KR102525775B1 (ko) * 2022-07-06 2023-04-26 주식회사 대현에스티 수소 누출 감지용 센서 조성물 및 이를 포함하는 점착 테이프

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KR102525775B1 (ko) * 2022-07-06 2023-04-26 주식회사 대현에스티 수소 누출 감지용 센서 조성물 및 이를 포함하는 점착 테이프

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JP2005345338A (ja) * 2004-06-04 2005-12-15 Matsushita Electric Ind Co Ltd 水素ガス検知用塗膜顔料、水素ガス検知用塗膜、及び水素ガス検知テープ
KR101734733B1 (ko) * 2015-12-30 2017-05-11 현대자동차주식회사 산화몰리브덴 기반 색가변 수소 검출센서 및 그 제조방법
JP2018004505A (ja) * 2016-07-05 2018-01-11 東京瓦斯株式会社 水素ガス検知テープ
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CN109825090A (zh) * 2019-02-20 2019-05-31 北京航天试验技术研究所 一种复合硅胶材料及其制备方法
KR102525775B1 (ko) * 2022-07-06 2023-04-26 주식회사 대현에스티 수소 누출 감지용 센서 조성물 및 이를 포함하는 점착 테이프

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