WO2014208825A1 - Manufacturing method for compound for detecting acid, alkali and toxic gas leaks, and use thereof - Google Patents

Manufacturing method for compound for detecting acid, alkali and toxic gas leaks, and use thereof Download PDF

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Publication number
WO2014208825A1
WO2014208825A1 PCT/KR2013/009374 KR2013009374W WO2014208825A1 WO 2014208825 A1 WO2014208825 A1 WO 2014208825A1 KR 2013009374 W KR2013009374 W KR 2013009374W WO 2014208825 A1 WO2014208825 A1 WO 2014208825A1
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Prior art keywords
acid
base
compound
preparing
mixture
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PCT/KR2013/009374
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French (fr)
Korean (ko)
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이석구
이종구
성대동
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Lee Seoggoo
Lee Jonggu
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Application filed by Lee Seoggoo, Lee Jonggu filed Critical Lee Seoggoo
Priority to JP2015524201A priority Critical patent/JP5951898B2/en
Publication of WO2014208825A1 publication Critical patent/WO2014208825A1/en

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/22Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
    • G01N31/221Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators for investigating pH value
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems 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
    • G01N21/78Systems 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
    • G01N21/783Systems 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 for analysing gases
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems 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
    • G01N21/78Systems 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
    • G01N21/80Indicating pH value
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N31/00Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
    • G01N31/22Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
    • G01N31/223Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators for investigating presence of specific gases or aerosols
    • G01N31/224Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators for investigating presence of specific gases or aerosols for investigating presence of dangerous gases
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/75Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
    • G01N21/77Systems 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
    • G01N2021/7756Sensor type

Definitions

  • the present invention relates to a method for producing a compound having an automatic detection function in the visible region in the case of acid, base and toxic gas leakage, and more particularly, the use thereof, and more particularly, through a pipeline in the production process It relates to a method for producing an environmentally friendly compound for visually detecting the leakage of acid, base and toxic gases in liquid and gaseous state and its use.
  • acids such as hydrochloric acid, sulfuric acid, hydrofluoric acid, nitric acid and acetic acid, which are frequently used in industrial manufacturing processes
  • bases such as ammonia, sodium hydroxide, potassium hydroxide and barium hydroxide, manganese oxide and sodium oxide
  • metal oxides that quickly turn into strong alkalis when contacted with moisture can cause fatal damage to humans and processes when leaked even in small amounts.
  • the present invention is to provide a method for producing a compound for the detection of environmentally friendly acid, base and toxic gas leakage that is safe for the applicator and minimizes the impact on the safety of the equipment after application and excellent in acid, base leakage, and its use Its purpose is.
  • Another object of the present invention is to safeguard the applicator and to minimize the impact on the safety of the equipment after application, and to detect the environmentally friendly acid, base and toxic gas leakage that can be quickly detected in the visible light area when acid, base leakage It provides a method for preparing the compound and its use.
  • the present invention is characterized in that it comprises the process of preparing a first mixture by dissolving Methylene blue in distilled water and dissolved in sorbitol and the second mixture by adding this solution to a solution dissolved in sorbitol.
  • FIG. 1 is a view showing a process for preparing a compound that automatically detects and reacts with acid leakage according to an embodiment of the present invention.
  • Figure 2 is a view showing a process for preparing a compound that automatically detects and reacts to the base (base) leak according to another embodiment of the present invention.
  • the present invention is characterized in that it comprises the process of preparing a first mixture by dissolving Methylene blue in distilled water and dissolved in sorbitol and the second mixture by adding this solution to a solution dissolved in sorbitol.
  • the invention of the production line as well as acid Compounds for detecting acid, base and toxic gas leaks, which can detect leaks from storage of bases and leaks when transporting tanks of acids and bases, protecting production facilities that can lead to large accidents and preventing human damage, And it is characterized in that the compound is blended paint and the tape coated with the compound, it is harmless to the human body when the paint is applied or the tape is attached to protect the production facility.
  • the present invention is a trace acid, base value valve, pump, flange, tank, precision measuring instrument, reagent field, pipe connection point, hose connection point, acid, base that can be harmful to the human body at the same time to damage the industrial facilities at the production site
  • Compounds of the present invention are automatically detected and harmless to the human body when leaking in the transport vehicle or during the dispersion, storage and processing of acids and bases. At the same time, it is a clear visual indication that protects precision facilities while providing quick indication of leak points.
  • the present invention produces an environmentally friendly compound that does not cause secondary pollution when the compound is applied and at the same time the color change that is expressed in the visible light region reacts quickly and quickly, so that the first detector can easily respond to safety.
  • a method for preparing a compound for detecting acid, base and toxic gas leakage and its use are presented.
  • a method of preparing a compound for detecting gas leakage and its use, specifically, a paint in which the compound is blended and a tape coated with the compound are provided.
  • the human body in order to manufacture a special compound that does not cause secondary contamination among the compounds reacting with acid and base, the human body using a compound that is recognized by the World Health Organization and suitable for the German Merck Index and the material safety data sheet It is a technology to increase safety.
  • compounds that prevent secondary contamination compounds that can react as quickly as possible to detect the detection of acid and base were prepared.
  • the technology employed in the present invention production line and acid.
  • the production of special functional paints and tapes for coating sensors that protect leaks from base storage facilities and leaks when transporting tanks of acids and bases protect production facilities that can lead to large accidents and prevent human damage.
  • In order to completely remove the secondary pollution source of the conventional product is to manufacture a product that is harmless to the human body when applied and protects the production facilities.
  • the technology to be solved in the present invention is a trace acid, base value valve, pump, flange, tank, precision measuring instrument, reagent field, pipe connection point, hose connection point,
  • the paint containing the compound of the present invention or the tape coated with the compound is automatically detected to protect human body and at the same time protect the precision facility. Visually and vividly to indicate where the leak is, accurately and quickly.
  • the present invention is a method for producing a product that is safe for the applicator and minimizes the effect on the safety of the equipment after application and has excellent visual effect upon acid and base leakage.
  • the present invention is the first to invent a technology for manufacturing an environmentally friendly product that is safe for the applicator and minimizes the effect on the safety of the equipment after application and can be quickly detected in the visible light region when acid and base leak.
  • the logarithm of the concentration ratio of the indicator reacting to the compound, the concentration of Hind, the acid participating in the reaction, and the concentration of Ind - generated by the base reacting with Hind is determined. It reacts quickly in the visible range of 500 ⁇ 780nm to maximize the visual effect and the compound itself should be an environment-friendly molecule that is harmless to the human body.
  • Methyl Orange Methylene Blue
  • Methyl Yellow Sorbitol
  • Ethyl Alcohol Methyl Ethyl Ketone
  • Alizarin Yellow which are harmless human body detection indicators
  • Thymol Blue Phenolphthalein, Sorbitol
  • Use Ethyl Alcohol Cresol Red, 1,3-Dimethyl Aniline.
  • a method for preparing a compound for acid leakage detection is as shown in FIG. 1, and the dispersion process of the pigment expression dye molecule having a leak acid detection function is described below.
  • the six mixtures were heated under vacuum distillation for 10 minutes under a reduced pressure of 10 mmHg to remove the distillation residue.
  • the 6 mixture solution from which the distillation residue was removed was added to a mixed solvent of 30 parts by weight of butyl acetate and 70 parts by weight of xylene, and stirred at -780C for 2 hours using a magnetic stirrer at 780 rpm. Slowly raise the temperature and blow nitrogen gas at 30 °C while stirring with magnetic stirrer at 520rpm for 2 hours.
  • the environmentally friendly sensor compound prepared above is reacted with the binder material as follows so that it can be clearly expressed in the eyes in the visible wavelength range of 570 ⁇ 590nm. Disperse 8 parts by weight of triethylamine in distilled water and stir vigorously with a magnetic stirrer at 880 rpm (7 mixtures).
  • titanium dioxide nano powder: 25-70nm (xrd): BET surface area-20-25m 2 / g
  • the above three mixtures (specifically, 1 + 2 + 3 mixture) are mixed one by one and heated by stirring with a magnetic stirrer at 70 ° C. for 38 hours for 1 hour (4 mixtures).
  • the six mixtures were heated under vacuum distillation for 10 minutes under a reduced pressure of 10 mmHg to remove the distillation residue.
  • the 6 mixture solution from which the distillation residue was removed was added to a mixed solvent of butyl acetate and 70 parts by weight of xylene, and stirred at a magnetic stirrer at 1120 rpm for 2 hours at -2 ° C. Slowly raise the temperature and stir with magnetic stirrer for 2 hours while blowing nitrogen gas at 30 °C. Slowly add 2 g of 1,3-dimethyl aniline as a stabilizer to the 6 mixture from which the distillation residue was removed and stir at a speed of 370 rpm with a magnetic stirrer.
  • a solution of 0.00071 parts by weight of triethylamine dispersed in distilled water is strongly stirred with a magnetic stirrer at a speed of 1830 rpm (7 mixtures).
  • the compound prepared by the method as described above can be used for a variety of uses, the most preferred among them can be used by blending the compound in the paint, and then applying it to the above-mentioned pipeline. In addition, after applying the compound to a conventional tape, it can be used by winding the pipeline or the like.
  • the compounds for detecting acid, base and toxic gas leaks prepared by the method according to the present invention are preferably used for the use of the above-described paints and tapes. However, the compounds of the present invention may be used in various forms. .
  • the compounds for detecting acid, base and toxic gas leakage according to the present invention can obtain the following technical features.
  • the present invention shows an excellent sensor effect in the acid, base leaking part as a method of manufacturing a product that can quickly detect acid, base leakage while preventing secondary contamination of the existing product.
  • the result of applying the sensor compound prepared by the present invention is as follows.
  • reaction discoloration range of the sensor compound in the case of acid and base leakage can be used in all processes using acid and base.
  • pH range 7-14 (without acid leakage): Yellow (570-590 nm visible wavelength light region)
  • pH range 1 to 3 (acid leak): Red (620 to 750 nm visible wavelength light region)
  • pH range 10 ⁇ 13 Red (625 ⁇ 760nm visible wavelength light region)
  • the function of the reaction sensor to detect acid and base leakage is excellent. It detects 10 ⁇ 150 times faster than existing products.
  • reaction time of the sensor produced in the present invention upon acid leakage is as follows.
  • the product of the present invention which reacts rapidly when acid and base leaks to show the function of the sensor, is used for valves, pumps, flanges, tanks, precision measuring instruments, reagent stations, pipe connection points, hose connection points, acids, and base transports.
  • the applicability was excellent when applied to detect leaks detected during vehicle, acid and base dispersion, storage and processing.
  • the acid and base leak sensor compounds prepared in the present invention were applied, the applicability was tested, and as shown in the following Table 3, Table 4, Table 5, Table 6 and Table 7, the performance of the product was superior to the existing sensor compounds. It was.
  • Table 4 Results of typical scratch test, shear test, and bend test on sensor paint of acid leakage with and without sputter cleaning after coating deposition on PVC pipe after scratching treatment corresponding for three month period.
  • the experimental results were obtained by Ergonic Workstation and 550 Shear / Scratch Tester, TABER.
  • Test method Substratetreatment NoSputterCleaning 5 minSputter Cleaning 10 minSputter Cleaning Scratch testLc (N) 5.2 27 64 Shear testFc (MNm -2 ) 2.3 6.5 7.3 Bend test, Mechanical notch (MNm -3/2 ) 1.6 6.3 9.2 Bend test, Copper notch (MNm -3/2 ) 0.81 4.7 8.0
  • the above results show the sensor paints are adequate for use of iron pipe or PVC pipe at least three months period.
  • the experimental results were obtained by Ergonic Workstation and 550 Shear / Scratch Tester, TABER.
  • the above results show the sensor paints are adequate for use of iron pipe or PVC pipe at least three months period.
  • the experimental results were obtained by Ergonic Workstation and 550 Shear / Scratch Tester, TABER.
  • the acid and base leak sensor compounds prepared in the present invention are chemically stable when applied to the process. In other words, it reacts with other molecules in the air until the acid and base are leaked, and the sensor itself does not lose its function and does not harm the human body.
  • the high stability of the sensor molecules makes them suitable for all industrial production processes.
  • the acid base leak sensor compound prepared in the present invention is manufactured in an environmentally friendly manner, it does not cause secondary pollution to the applicator or the person working in the post-application process.
  • the present invention produces an environmentally friendly compound that does not cause secondary pollution when the compound is applied and simultaneously changes the color that is expressed in the visible region in a quick and quick response, so that the first detector can easily respond to safety. There is this.
  • it has the advantage of blocking the secondary pollutant of the compound itself, and the compound reacts to the fast time within the microsecond time to implement the function of discoloring the vivid color so that the first detector can respond quickly.
  • the present invention is completely harmless to the human body in order to completely block the secondary pollutant in order to overcome the limitations of the conventional products and to produce environmentally friendly, it is possible to quickly and accurately detect the change of color visually when reacting with acid, base and Using thermodynamically tested molecules that have a stable molecular structure that is not easily oxidized or reduced in air, it has a synergistic effect with excellent chemical stability and no human toxicity.

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Abstract

The present invention relates to a compound that changes colour in response to acids, alkali liquid chemicals and toxic gases, and the use thereof. The colours of acids, alkali liquid chemicals and toxic gases are mostly transparent like water (H2O), and thus it is difficult for a person to immediately sense the danger thereof. For this reason, the risk of accidents is high, and a number of accidents associated with liquid chemicals and toxic gases occur at industrial sites. To solve this problem, the present invention provides a manufacturing method for a compound for detecting acid, liquid chemical and toxic gas leaks, and the use of the compound, wherein a paint is applied or a tape is wrapped on areas that have the potential for liquid chemical and gas leaks, the paint or tape containing a special reaction compound for detection that changes colour from yellow to red or from white to red if there is a liquid chemical or gas leak. Thus, the first person who finds the colour change can take quick action.

Description

산, 염기 및 독성가스 누출 감지를 위한 화합물의 제조방법 및 그 용도Method for preparing a compound for detecting acid, base and toxic gas leakage and its use
본 발명은 산(acid), 염기(base) 및 독성가스 누출 시 가시광선 영역에서 자동 감지 기능을 갖는 화합물을 제조하는 방법 및 그 용도에 관한 것으로서, 더욱 상세하게는 생산공정에서 파이프 라인을 통해 이동하는 액체 및 기체 상태의 산, 염기 및 독성가스의 누출을 시각적으로 감지하는 친환경적 화합물을 제조하는 방법 및 그 용도에 관한 것이다.The present invention relates to a method for producing a compound having an automatic detection function in the visible region in the case of acid, base and toxic gas leakage, and more particularly, the use thereof, and more particularly, through a pipeline in the production process It relates to a method for producing an environmentally friendly compound for visually detecting the leakage of acid, base and toxic gases in liquid and gaseous state and its use.
일반적으로 통용되고 있는 산, 염기의 누출을 감지하는 종래의 페인트는 산, 염기 누출을 감지하기 위하여 파이프 라인 등에 도포하였을 때 도포하는 사람이 화학분자의 독성에 노출되고 산업용 기자재의 보호기능도 저하되는 단점이 있다.Conventional paints for detecting acid and base leaks, which are commonly used, are applied to pipelines to detect acid and base leaks. There are disadvantages.
즉, 산업 현장의 제조 공정에서 많이 사용하고 있는 염산, 황산, 플루오르화수소산, 질산, 아세트산 등의 산과, 암모니아, 수산화나트륨, 수산화칼륨, 수산화바륨과 같은 염기 (알칼리)와 산화망간, 산화나트륨과 같이 수분에 접촉 시 곧바로 강알칼리로 변하는 금속산화물 등은 미량이라도 누출될 때 인체와 공정에 치명적인 손상을 준다. That is, acids such as hydrochloric acid, sulfuric acid, hydrofluoric acid, nitric acid and acetic acid, which are frequently used in industrial manufacturing processes, bases (alkali) such as ammonia, sodium hydroxide, potassium hydroxide and barium hydroxide, manganese oxide and sodium oxide, Likewise, metal oxides that quickly turn into strong alkalis when contacted with moisture can cause fatal damage to humans and processes when leaked even in small amounts.
현재 시판되는 제품은 영국 Basildon Essex에 소재하는 Allison Engineering 사의 On Guard Acid Detecting Paint와 미국 뉴저지 주에 있는 RAMCO 사의 Acid Leakage Detection Paint가 주를 이루고 있다. 이들 제품은 야외에 노출된 파이프 라인에서 산, 염기가 유출될 때의 파이프 라인에는 적용하기 쉬우나 실내 공정에 있는 파이프 라인이나 정밀시설에 적용했을 때 도포 화학물질이 인체에 유해하고 정밀 기자재에 부분적으로 손상을 가져올 수 있는 단점이 있다.Current products include On Guard Acid Detecting Paint of Allison Engineering, Basildon Essex, UK, and Acid Leakage Detection Paint of RAMCO, NJ, USA. These products are easy to apply to pipelines where acid and base are leaked from outdoor exposed pipelines, but when applied to pipelines or precision facilities in indoor processes, the applied chemicals are harmful to humans and partially applied to precision equipment. It has the disadvantage of being damaged.
이러한 단점을 보완하기 위하여 그동안 새로운 많은 발명이 시도되어왔다. 안전한 형태의 산 누출 센서로는 Spring G. Everett 등이 발명(발명자: Spring G. Everett, Keller, Jr. Douglas V., 및 etection with non-Toxic Liquids 미국특허번호: 08/281,854, 출원일: July 26, 1994) 한 것이 있다.Many new inventions have been tried in the meantime to compensate for these drawbacks. Safe type acid leak sensors are invented by Spring G. Everett et al. (Inventor: Spring G. Everett, Keller, Jr. Douglas V., and etection with non-Toxic Liquids US Patent No. 08 / 281,854, Filed July 26 , 1994).
또한 최근에 산, 염기 누출을 자동적으로 감지할 수 있는 개선된 제품으로는 Joseph C. Farmer의 발명(발명자: Joseph C. Farmer, Paint for Detection of Corrosion and Warning of Chemical and Radiological Attack 미국특허번호: 7,780,913 B2, 출원일: August 24, 2010)이 있다.In addition, recently improved products that can automatically detect acid and base leaks include the invention of Joseph C. Farmer (inventor: Joseph C. Farmer, Paint for Detection of Corrosion and Warning of Chemical and Radiological Attack US Pat. No. 7,780,913 B2, filing date: August 24, 2010).
그러나 이들 제품은 안전에 기준을 두었기 때문에 화합물 자체의 효율성이 떨어지는 단점이 있다. 특히 산. 염기가 누출되는 산업현장에서는 짧은 시간 내에 인체에 치명적인 영향을 줄 수 있기 때문에 빠른시간 내에 누출 현장을 바로 확인할 수 있어야 한다. 그리고 산. 염기가 누출될 때 화합물의 반응이 마이크로 시간 내에 바로 눈에 띌 수 있어야 한다. 즉, 마이크로 초 이내의 빠른시간 대와 가시광선 영역에서 바로 확인 가능하여야 함에도 불구하고 종래의 제품들은 반응 시간이 길고 누출부위가 선명하지 않은 단점이 있어왔다.However, these products have a disadvantage in that the efficiency of the compound itself is reduced because of safety standards. Especially mountains. In industrial sites where base leaks, it can have a fatal effect on the human body in a short time, so it must be possible to immediately identify the leak site. And mountains. When the base leaks, the reaction of the compound should be immediately visible within micro time. That is, despite the fact that it should be immediately visible in the visible region and the fast time within the microseconds, the conventional products have a disadvantage that the reaction time is long and the leakage is not clear.
따라서 산업현장에서 산. 염기가 누출될 때 마이크로 시간 내의 빠른시간에 화합물이 감응하여 즉시 발현될 수 있어야 한다. 상기 화합물이 누출된 산 혹은 염기와 반응하여 발현하는 빛의 파장이 570~590nm 영역에서와 625~760nm 영역에서 반응할 수 있는 화합물질이 요구되어 왔다.Therefore, live in the industrial field. When the base leaks, the compound should be able to respond and express immediately in a micro time. There has been a demand for compounds that can react in the wavelength range of 570-590 nm and in the range of 625-760 nm when the compound reacts with the leaked acid or base.
본 발명에서는 도포 자에게 안전하며 도포 후 기자재의 안전에 미치는 영향을 최소화하고 산, 염기 누출 시 시각적 효과가 뛰어난 친환경적인 산, 염기 및 독성가스 누출 감지를 위한 화합물의 제조방법 및 그 용도를 제공하는데 그 목적이 있다.The present invention is to provide a method for producing a compound for the detection of environmentally friendly acid, base and toxic gas leakage that is safe for the applicator and minimizes the impact on the safety of the equipment after application and excellent in acid, base leakage, and its use Its purpose is.
또한, 본 발명의 다른 목적은 도포 자에게 안전하며 도포 후 기자재의 안전에 미치는 영향을 최소화하고 산, 염기 누출 시 가시광선영역에서 빠르게 감지할 수 있는 친환경적인 산, 염기 및 독성가스 누출 감지를 위한 화합물의 제조방법 및 그 용도를 제공함에 있다.In addition, another object of the present invention is to safeguard the applicator and to minimize the impact on the safety of the equipment after application, and to detect the environmentally friendly acid, base and toxic gas leakage that can be quickly detected in the visible light area when acid, base leakage It provides a method for preparing the compound and its use.
본 발명은 Methylene blue를 증류수에 녹이고 sorbitol에 녹인 용액에 가하여 제 1 혼합액을 만드는 과정과 이 용액을 sorbitol에 녹인 용액 에 가하여 제 2혼합액을 제조하는 과정으로 이루어짐을 특징으로 한다.The present invention is characterized in that it comprises the process of preparing a first mixture by dissolving Methylene blue in distilled water and dissolved in sorbitol and the second mixture by adding this solution to a solution dissolved in sorbitol.
도 1은 본 발명의 바람직한 일 실시 예에 따른 산(acid) 누출을 자동으로 감지하여 반응하는 화합물을 제조하는 과정을 보여주고 있는 도면.1 is a view showing a process for preparing a compound that automatically detects and reacts with acid leakage according to an embodiment of the present invention.
도 2는 본 발명의 바람직한 다른 실시 예에 따른 염기(base) 누출을 자동으로 감지하여 반응하는 화합물을 제조하는 과정을 보여주고 있는 도면.Figure 2 is a view showing a process for preparing a compound that automatically detects and reacts to the base (base) leak according to another embodiment of the present invention.
본 발명은 Methylene blue를 증류수에 녹이고 sorbitol에 녹인 용액에 가하여 제 1 혼합액을 만드는 과정과 이 용액을 sorbitol에 녹인 용액 에 가하여 제 2혼합액을 제조하는 과정으로 이루어짐을 특징으로 한다.The present invention is characterized in that it comprises the process of preparing a first mixture by dissolving Methylene blue in distilled water and dissolved in sorbitol and the second mixture by adding this solution to a solution dissolved in sorbitol.
이하 본 발명의 실시 예를 첨부된 도면을 참조하여 설명하면 다음과 같다. 후술 될 상세한 설명에서는 상술한 기술적 과제를 이루기 위해 본 발명에 있어 대표적인 실시 예를 제시할 것이다. 그리고 본 발명으로 제시될 수 있는 다른 실시 예들은 본 발명의 구성에서 설명으로 대체한다.Hereinafter, an embodiment of the present invention will be described with reference to the accompanying drawings. In the following description will be presented a representative embodiment in the present invention to achieve the above technical problem. And other embodiments that can be presented with the present invention are replaced by the description in the configuration of the present invention.
본 발명은 생산라인은 물론 산. 염기의 저장 시설에서의 누출과 산, 염기의 탱크 운반 시 누출을 사전에 감지하여 대형 사고로 이어질 수 있는 생산시설을 보호하고 인체 손상을 예방할 수 있는 산, 염기 및 독성가스 누출 감지를 위한 화합물, 그리고 상기 화합물이 배합된 페인트 및 상기 화합물이 도포된 테이프로서, 상기 페인트를 도포하거나 테이프를 부착 시 인체에 무해하고 생산시설을 보호할 수 있는 특징으로 하고 있다.The invention of the production line as well as acid. Compounds for detecting acid, base and toxic gas leaks, which can detect leaks from storage of bases and leaks when transporting tanks of acids and bases, protecting production facilities that can lead to large accidents and preventing human damage, And it is characterized in that the compound is blended paint and the tape coated with the compound, it is harmless to the human body when the paint is applied or the tape is attached to protect the production facility.
또한, 본 발명은 생산현장에서 인체에 유해하고 동시에 산업 시설을 훼손할 수 있는 미량의 산, 염기가 밸브, 펌프, 플렌지, 탱크, 정밀계측기, 시약장, 파이프 연결지점, 호스 연결지점, 산, 염기 운반용 차량, 혹은 산, 염기의 분산, 저장 및 가공단계에서 누출될 때 자동적으로 본 발명의 화합물(구체적으로는, 상기 화합물이 배합된 페인트 또는 상기 화합물이 도포된 테이프)가 감지하여 인체에 무해하고 동시에 정밀 시설을 보호하면서 시각적으로 선명하게 발색하여 누출 지점을 신속하게 알려주는 데 있다.In addition, the present invention is a trace acid, base value valve, pump, flange, tank, precision measuring instrument, reagent field, pipe connection point, hose connection point, acid, base that can be harmful to the human body at the same time to damage the industrial facilities at the production site Compounds of the present invention (specifically, paints incorporating the compound or tape coated with the compound) are automatically detected and harmless to the human body when leaking in the transport vehicle or during the dispersion, storage and processing of acids and bases. At the same time, it is a clear visual indication that protects precision facilities while providing quick indication of leak points.
그리고 본 발명은 화합물을 도포하였을 때 2차 오염을 일으키지 않는 친환경적 화합물을 제조하고 동시에 발현하는 색깔의 변화가 가시광선영역에서 선명하게 빠른 시간 내에 반응하여 최초 발견자가 쉽게 대응하여 안전을 도모할 수 있는 산, 염기 및 독성가스 누출 감지를 위한 화합물의 제조방법 및 그 용도를 제시한다.In addition, the present invention produces an environmentally friendly compound that does not cause secondary pollution when the compound is applied and at the same time the color change that is expressed in the visible light region reacts quickly and quickly, so that the first detector can easily respond to safety. A method for preparing a compound for detecting acid, base and toxic gas leakage and its use are presented.
특히, 본 발명에서는 화합물질 자체가 갖는 2차 오염원을 차단하고 화합물질이 마이크로 초 시간 이내의 빠른시간에 반응하여 최초 발견자가 신속하게 대응할 수 있도록 선명한 색깔로 변색하는 기능을 갖는 산, 염기 및 독성가스 누출 감지를 위한 화합물의 제조방법 및 그 용도, 구체적으로는 상기 화합물이 배합된 페인트 및 상기 화합물이 도포된 테이프를 구현하고자 한다.Particularly, in the present invention, acids, bases, and toxicities having a function of blocking secondary pollutants of the compound itself and discoloring in vivid colors so that the compound reacts quickly in a microsecond time can be quickly responded by the first discoverer. A method of preparing a compound for detecting gas leakage and its use, specifically, a paint in which the compound is blended and a tape coated with the compound are provided.
본 발명에서는 종래의 제품이 갖는 한계를 극복하기 위하여 2차 오염원을 완전히 차단하여 친환경적으로 제조하기 위하여 인체에 전혀 무해하며 산, 염기와 반응 시 시각적으로 색깔의 변화를 빠르고 정확하게 감지할 수 있고, 또한 공기 중에서 자동 산화, 환원이 용이하지 않은 안정된 분자 구조를 열역학적으로 테스트한 분자를 사용하여 화학안정성이 뛰어나고 인체 독성이 전무한 분자를 택하여 제조하였다.In the present invention, in order to overcome the limitations of the conventional products to completely eco-friendly manufacturing by blocking the secondary pollution source completely harmless to the human body can visually detect the color change quickly and accurately when reacting with acid, base, Using a molecule that has been thermodynamically tested for a stable molecular structure that is not easily oxidized or reduced in air, a molecule having excellent chemical stability and no human toxicity was prepared.
특히, 본 발명에서는 산, 염기에 반응하는 화합물 중 2차 오염을 야기하지 않는 특수 화합물을 제조하기 위하여 세계보건기구에서 인정하고 독일 Merck Index와 화합물 안정도(material safety data sheet)에 적합한 화합물을 이용하여 인체안전성을 높이는 기술이다. 또한 2차 오염을 방지하는 화합물 중에서도 산, 염기 누출 시 감지 기능을 최대한 빠르게 반응할 수 있는 화합물을 제조하였다.In particular, in the present invention, in order to manufacture a special compound that does not cause secondary contamination among the compounds reacting with acid and base, the human body using a compound that is recognized by the World Health Organization and suitable for the German Merck Index and the material safety data sheet It is a technology to increase safety. In addition, among compounds that prevent secondary contamination, compounds that can react as quickly as possible to detect the detection of acid and base were prepared.
한편, 본 발명에서 채용한 기술은 생산라인과 산. 염기의 저장 시설에서의 누출과 산, 염기의 탱크 운반 시 누출을 사전에 감지하여 대형 사고로 이어질 수 있는 생산시설을 보호하고 인체 손상을 예방하는 도포 센서용 특수 기능성 페인트 및 테이프를 제조하는 것이다. 종래의 제품이 갖는 2차 오염원을 완전히 제거하기 위하여 도포 시 인체에 무해하고 생산시설을 보호할 수 있는 제품을 제조하는 것이다.On the other hand, the technology employed in the present invention production line and acid. The production of special functional paints and tapes for coating sensors that protect leaks from base storage facilities and leaks when transporting tanks of acids and bases protect production facilities that can lead to large accidents and prevent human damage. In order to completely remove the secondary pollution source of the conventional product is to manufacture a product that is harmless to the human body when applied and protects the production facilities.
본 발명에서 해결하고자 하는 기술은 생산현장에서 인체에 유해하고 동시에 산업 시설을 훼손할 수 있는 미량의 산, 염기가 밸브, 펌프, 플렌지, 탱크, 정밀 계측기, 시약장, 파이프 연결지점, 호스 연결지점, 산, 염기 운반용 차량, 혹은 산, 염기의 분산, 저장 및 가공단계에서 누출될 때 본 발명의 화합물이 배합된 페인트 또는 상기 화합물이 도포된 테이프가 자동으로 감지하여 인체에 무해하고 동시에 정밀 시설을 보호하면서 시각적으로 선명하게 발색하여 누출 지점을 정확하고 신속하게 알려주는 데 있다.The technology to be solved in the present invention is a trace acid, base value valve, pump, flange, tank, precision measuring instrument, reagent field, pipe connection point, hose connection point, When leaking in the acid, base transport vehicle or acid, base dispersing, storage and processing step, the paint containing the compound of the present invention or the tape coated with the compound is automatically detected to protect human body and at the same time protect the precision facility. Visually and vividly to indicate where the leak is, accurately and quickly.
따라서 본 발명에서는 도포 자에게 안전하며 도포 후 기자재의 안전에 미치는 영향을 최소화하고 산, 염기 누출 시 시각적 효과가 뛰어난 제품을 제조하는 방법이다. 그리고 본 발명에서는 도포 자에게 안전하며 도포 후 기자재의 안전에 미치는 영향을 최소화하고 산, 염기 누출 시 가시광선영역에서 빠르게 감지할 수 있는 친환경적 제품을 제조하는 기술을 최초로 발명한 것이다.Therefore, the present invention is a method for producing a product that is safe for the applicator and minimizes the effect on the safety of the equipment after application and has excellent visual effect upon acid and base leakage. In addition, the present invention is the first to invent a technology for manufacturing an environmentally friendly product that is safe for the applicator and minimizes the effect on the safety of the equipment after application and can be quickly detected in the visible light region when acid and base leak.
이하, 본 발명의 바람직한 실시 예에 의거 상세히 설명하겠는 바, 상기 본 발명이 실시 예에 의해 한정되는 것은 아니다.Hereinafter, the present invention will be described in detail based on the preferred embodiment of the present invention, but the present invention is not limited to the embodiment.
{실시 예 1}{Example 1}
(1) 산, 염기가 누출될 때 자동적으로 감지할 수 있는 화합물 중 인체에 무해하며 생산 공정 라인에 2차 오염을 방지하는 분자는 다음과 같이 반응한다.(1) Among the compounds that can be detected automatically when an acid or base leaks, the molecules that are harmless to the human body and prevent secondary pollution in the production process line react as follows.
즉, 산, 혹은 염기의 미량 누출을 자동적으로 감지하여 가시광선 영역에서 빠르게 반응하는 화합물은 다음의 Henderson-Hasselbalch 식(화학식 1)에서 pH 값에 따라 변색범위가 정해진다.That is, a compound that automatically detects a small leak of an acid or a base and reacts quickly in the visible range is discolored according to the pH value in the following Henderson-Hasselbalch equation (Formula 1).
화학식 1
Figure PCTKR2013009374-appb-C000001
Formula 1
Figure PCTKR2013009374-appb-C000001
변색 반응이 빠르게 진행되기 위해서는 화합물에 반응하는 지시약, Hind의 농도와 반응에 참여한 산, 염기가 Hind와 반응하여 생성한 Ind-의 농도 비의 대수 값이 결정한다. 500~780nm의 가시광선영역에서 빠르게 반응하여 시각적 효과를 극대화하고 화합물 자체가 인체에 무해한 친환경적 분자이어야 한다.In order to accelerate the discoloration reaction, the logarithm of the concentration ratio of the indicator reacting to the compound, the concentration of Hind, the acid participating in the reaction, and the concentration of Ind - generated by the base reacting with Hind is determined. It reacts quickly in the visible range of 500 ~ 780nm to maximize the visual effect and the compound itself should be an environment-friendly molecule that is harmless to the human body.
이러한 조건을 만족하며 인체에 무해한 산 누출 자동감지 지시약인 Methyl Orange, Methylene Blue, Methyl Yellow, Sorbitol, Ethyl Alcohol, Methyl Ethyl Ketone, Alizarin Yellow 를 사용하고 알칼리 누출 자동감지 지시약인 Thymol Blue, Phenolphthalein, Sorbitol, Ethyl Alcohol, Cresol Red, 1,3-Dimethyl Aniline을 사용한다.It satisfies these conditions and uses Methyl Orange, Methylene Blue, Methyl Yellow, Sorbitol, Ethyl Alcohol, Methyl Ethyl Ketone, Alizarin Yellow, which are harmless human body detection indicators, and Thymol Blue, Phenolphthalein, Sorbitol, Use Ethyl Alcohol, Cresol Red, 1,3-Dimethyl Aniline.
(2) 산, 염기 누출 감지 화합물 1 L를 제조하기 위하여 다음과 같은 과정으로 반응 혼합한다.(2) To prepare 1 L of acid and base leak detection compound, the reaction mixture is carried out as follows.
산 누출 감지를 위한 화합물의 제조방법은 도 1에서 도시하고 있는 바와 같으며, 누출 산 검지 기능을 갖는 색소발현염료분자의 분산과정은 아래에서 설명하는 바와 같다.A method for preparing a compound for acid leakage detection is as shown in FIG. 1, and the dispersion process of the pigment expression dye molecule having a leak acid detection function is described below.
즉, 유출된 산에 반응할 수 있는 색소발현염료분자 methylene blue 0.00046 중량부를 화학천칭에 달아둔다. 26중량부의 증류수에 110중량부의 sorbitol을 녹인 용액에 앞서 저울에 달아둔 0,00046중량부의 methylene blue를 가하고 50℃의 온도에서 25분간 가열하면서 magnetic stirrer로 저어 준다(1혼합액).That is, 0.00046 parts by weight of a pigment-expressing dye molecule methylene blue capable of reacting with the spilled acid is placed on a chemical balance. Prior to the solution of 110 parts by weight of sorbitol in 26 parts by weight of distilled water, 0,00046 parts by weight of methylene blue attached to the balance is added and stirred with a magnetic stirrer while heating at a temperature of 50 ° C. for 25 minutes (1 mixture).
4.78중량부의 methyl yellow를 증류수에 magnetic stirrer로 저어주면서 분산시킨다. 충분히 분산시킨 다음, 28중량부의 sorbitol을 증류수에 녹인 용액에 가하고 30분간 80℃의 온도에서 가열하면서 700 rpm의 속도의 magnetic stirrer로 저어준다(2혼합액).4.78 parts by weight of methyl yellow is dispersed in distilled water with magnetic stirr. After sufficient dispersion, 28 parts by weight of sorbitol is added to a solution dissolved in distilled water, and stirred at a magnetic stirrer at a speed of 700 rpm while heating at a temperature of 80 ° C. for 30 minutes (2 mixtures).
0.00027중량부의 alizarin yellow를 증류수에 분산시키고 magnetic stirrer로 저어준 다음 31중량부의 sorbitol을 증류수에 녹인 용액에 가하고 95℃의 온도에서 55분간 850rpm의 속도의 magnetic stirrer로 저어준다(3혼합액).Dissolve 0.00027 parts by weight of alizarin yellow in distilled water, stir with magnetic stirrer, add 31 parts by weight of sorbitol to the solution dissolved in distilled water, and stir with magnetic stirrer at 850 rpm for 55 minutes at 95 ° C (3 mixtures).
이상의 세 혼합액(구체적으로는, 위에서 제시한 1+2+3혼합액)을 한데 혼합하여 2시간 동안 95℃에서 2시간 동안 600rpm 속도의 magnetic stirrer로 저어주면서 가열한다(4혼합액).The above three mixtures (specifically, 1 + 2 + 3 mixtures presented above) are mixed together and heated while stirring with a magnetic stirrer at 600 rpm for 2 hours at 95 ° C. for 2 hours (4 mixtures).
18중량부의 palm oil을 무수ethyl alcohol을 용해시킨 후 100℃로 1시간 동안 590rpm의 속도의 magnetic stirrer로 저어주면서 가열한다(5혼합액).18 parts by weight of palm oil is dissolved in anhydrous ethyl alcohol and heated at 100 ° C with stirring with a magnetic stirrer at a speed of 590 rpm for 1 hour (5 mixtures).
상기 5혼합액에 4혼합액을 가하고 5시간 동안 80℃에서 3시간 동안 300rpm의 속도의 magnetic stirrer로 저어준다(6혼합액). Four mixtures were added to the five mixtures and stirred at a magnetic stirrer at 300 rpm for three hours at 80 ° C. for five hours (6 mixtures).
상기 6혼합액을 가열하면서 10mmHg의 감압 하에서 10분 동안 진공 증류하여 증류잔류물을 제거한다. 상기 증류잔류물을 제거한 6혼합액을 30중량부의 butyl acetate와 70중량부의 xylene을 혼합한 혼합용매에 가하고 -2℃에서 2시간 동안 780rpm 속도의 magnetic stirrer로 저어준다. 온도를 서서히 올려 30℃에서 질소기체를 불어 넣어 주면서 2시간 동안 520rpm속도의 magnetic stirrer로 저어준다.The six mixtures were heated under vacuum distillation for 10 minutes under a reduced pressure of 10 mmHg to remove the distillation residue. The 6 mixture solution from which the distillation residue was removed was added to a mixed solvent of 30 parts by weight of butyl acetate and 70 parts by weight of xylene, and stirred at -780C for 2 hours using a magnetic stirrer at 780 rpm. Slowly raise the temperature and blow nitrogen gas at 30 ℃ while stirring with magnetic stirrer at 520rpm for 2 hours.
다음으로, 친환경 누출 산 감지 센서화합물과 도포 성 Binder 재료 혼입과정은 아래에서 설명하는 바와 같다.Next, the process of mixing the environment-friendly leak acid sensor compound and the coatable binder material is as described below.
이상에서 제조한 친환경적인 센서화합물이 가시광선 파장 영역인 570~590nm에서 눈에 선명하게 발현될 수 있도록 binder물질에 다음과 같이 반응시킨다. 8중량부의 triethylamine을 증류수에 분산시킨 후 880 rpm속도의 magnetic stirrer로 강하게 저어준다(7혼합액).The environmentally friendly sensor compound prepared above is reacted with the binder material as follows so that it can be clearly expressed in the eyes in the visible wavelength range of 570 ~ 590nm. Disperse 8 parts by weight of triethylamine in distilled water and stir vigorously with a magnetic stirrer at 880 rpm (7 mixtures).
상기 7혼합액에 28중량부의 titanium dioxide (nano powder: 25~70nm(xrd): BET surface area-20-25m2/g)를 분액깔대기를 통해 가하고 magnetic stirrer로 500 rpm의 속도로 저어준다(8혼합액).28 parts by weight of titanium dioxide (nano powder: 25-70nm (xrd): BET surface area-20-25m 2 / g) is added to the seven mixtures through a funnel and stirred at a speed of 500 rpm with a magnetic stirrer (8 mixtures). ).
7.5중량부의 ammonium hydroxide (28% in H2O, 99.99+%)를 propoxy propanol에 서서히 넣고 530rpm속도의 magnetic stirrer로 저어준다.Add 7.5 parts by weight of ammonium hydroxide (28% in H 2 O, 99.99 +%) slowly to propoxy propanol and stir with a magnetic stirrer at 530 rpm.
3.23중량부의 iron(II) oxide (Fe2O3, 10mesh)를 증류수에 분산시킨 용액을 4,000rpm으로 저어준다(9혼합액).3.23 parts by weight of iron (II) oxide (Fe 2 O 3 , 10mesh) is dispersed in distilled water and stirred at 4,000 rpm (9 mixtures).
상기 8혼합액과 9혼합액을 섞은 다음 유도관을 통하여 0.017중량부의 n-butyl alcohol과 0.456중량부의 calcium carbonate (CaCO3, 10μm, 98%)와 0.528중량부의 barium carbonate (BaCO3, 26μm, 99%)를 서서히 가하고 5,000 rpm으로 저어준다(10혼합액). 상기 10혼합액에 앞서 증류잔류물을 제거한 6혼합물을 가한 후 57℃에서 3시간 동안 magnetic stirrer로 6,700 rpm으로 저어준다.After mixing the 8 mixture and the 9 mixture, 0.017 parts by weight of n-butyl alcohol, 0.456 parts by weight of calcium carbonate (CaCO 3, 10 μm, 98%) and 0.528 parts by weight of barium carbonate (BaCO 3 , 26 μm, 99%) were added. Add slowly and stir at 5,000 rpm (10 mixtures). After adding the six mixtures from which the distillation residues were removed prior to the ten mixtures, the mixture was stirred at 57 ° C. with a magnetic stirrer for 6 hours at 6,700 rpm.
다음으로, 염기 누출 감지를 위한 화합물의 제조방법은 도 2에서 도시하고 있는 바와 같으며, 염기 누출 자동 감지 기능을 갖는 색소발현염료분자의 분산과정은 아래에서 설명하는 바와 같다.Next, a method for preparing a compound for detecting base leakage is as shown in FIG. 2, and the process of dispersing a pigment-expressing dye molecule having an automatic base leakage detection function is described below.
0.018중량부의 thymol blue를 30.6중량부의 sorbitol을 증류수에 녹인 용액에 가하고 80℃의 온도에서 25분간 가열하면서 1200rpm속도의 magnetic stirrer로 저어 주면서 별도의 관으로 98% ethyl alcohol 10mL를 가한다(1혼합액).Add 0.018 parts by weight of thymol blue to a solution of 30.6 parts by weight of sorbitol in distilled water, and add 10 mL of 98% ethyl alcohol in a separate tube while stirring with a magnetic stirrer at 1200 rpm while heating at 80 ° C for 25 minutes (1 mixture). .
0.039중량부의 phenolphthalein을 증류수를 29.2중량부의 sorbitol을 증류수에 녹인 용액에 가하고 여기에 7.28중량부의 무수 ethyl alcohol(100%C2H5OH)을 가한 후 2시간 동안 55℃의 온도에서 가열하면서 690rpm속도의 magnetic stirrer로 저어준다(2혼합액).0.039 parts by weight of phenolphthalein was added to a solution of 29.2 parts by weight of sorbitol in distilled water, and 7.28 parts by weight of anhydrous ethyl alcohol (100% C 2 H 5 OH) was added thereto, followed by heating at a temperature of 55 ° C. for 2 hours at 690 rpm. Stir with a magnetic stirrer (2 mixtures).
0.0062중량부의 cresol red를 29.1중량부의 sorbitol을 증류수에 녹인 용액에 가하고 85℃의 온도에서 30분 동안 870rpm 속도의 magnetic stirrer로 저어준다(3혼합액).Add 0.0062 parts of cresol red to a solution of 29.1 parts of sorbitol in distilled water, and stir with a magnetic stirrer at 870 rpm for 30 minutes at a temperature of 85 ° C (3 mixtures).
이상의 세 혼합액(구체적으로는, 1+2+3혼합액)을 한 섞고 1시간 동안 70℃에서 38시간 동안 magnetic stirrer로 저어주면서 가열한다(4혼합액).The above three mixtures (specifically, 1 + 2 + 3 mixture) are mixed one by one and heated by stirring with a magnetic stirrer at 70 ° C. for 38 hours for 1 hour (4 mixtures).
18.8중량부의 palm oil을 220mL의 무수ethyl alcohol에 용해시킨 후 15mmHg로 유지된 감압 하에서 질소기체를 불어 넣어주면서 90℃로 20분 동안 570rpm속도의 magnetic stirrer로 저어준다(5혼합액). Dissolve 18.8 parts of palm oil in 220 mL of anhydrous ethyl alcohol and stir with a magnetic stirrer at 570 rpm for 20 minutes at 90 ° C. while blowing nitrogen gas under reduced pressure maintained at 15 mmHg (5 mixtures).
상기 5혼합액에 4혼합액을 가하고 6시간 동안 60℃에서 1시간 동안 930rpm속도의 magnetic stirrer로 저어준다(6혼합액).4 mixtures were added to the 5 mixtures and stirred for 6 hours at 60 ° C. with a magnetic stirrer at a speed of 930 rpm for 6 hours (6 mixtures).
상기 6혼합액을 가열하면서 10mmHg의 감압 하에서 10분 동안 진공 증류하여 증류잔류물을 제거한다. 상기 증류잔류물을 제거한 6혼합액을 중량부의 butyl acetate와 70중량부의 xylene을 혼합한 혼합용매에 가하고 -2℃에서 2시간 동안 1120rpm속도의 magnetic stirrer로 저어준다. 온도를 서서히 올려 30℃에서 질소기체를 불어 넣어 주면서 2시간 동안 magnetic stirrer로 저어준다. 증류잔류물을 제거한 6혼합액에 안정제인 1,3-dimethyl aniline 2g을 서서히 가하고 magnetic stirrer로 370rpm의 속도로 저어준다. 0.00071중량부의 triethylamine을 증류수에 분산시킨 용액을 1830rpm의 속도의 magnetic stirrer로 강하게 저어준다(7혼합액).The six mixtures were heated under vacuum distillation for 10 minutes under a reduced pressure of 10 mmHg to remove the distillation residue. The 6 mixture solution from which the distillation residue was removed was added to a mixed solvent of butyl acetate and 70 parts by weight of xylene, and stirred at a magnetic stirrer at 1120 rpm for 2 hours at -2 ° C. Slowly raise the temperature and stir with magnetic stirrer for 2 hours while blowing nitrogen gas at 30 ℃. Slowly add 2 g of 1,3-dimethyl aniline as a stabilizer to the 6 mixture from which the distillation residue was removed and stir at a speed of 370 rpm with a magnetic stirrer. A solution of 0.00071 parts by weight of triethylamine dispersed in distilled water is strongly stirred with a magnetic stirrer at a speed of 1830 rpm (7 mixtures).
다음으로, 친환경 누출 염기 감지 센서화합물과 도포성 Binder 재료 혼입과정은 아래에서 설명하는 바와 같다. Next, the process of incorporating the environmentally friendly leak base sensor compound and the coatable binder material is as described below.
상기 7혼합액에 8.18중량부의 titanium dioxide (nano powder: 25~70nm(xrd): BET surface area-20-25m2/g)를 가하고 5,500 rpm속도의 magnetic stirrer로 저어준다(8혼합액).8.18 parts by weight of titanium dioxide (nano powder: 25-70 nm (xrd): BET surface area-20-25 m 2 / g) was added to the seven mixtures, and stirred with a magnetic stirrer at a speed of 5,500 rpm (8 mixtures).
0.0021중량부의 ammonium hydroxide (27% in H2O, 99.99+%)를 propoxy propanol에 넣고 840rpm속도의 magnetic stirrer로 저어준다(9혼합액).Add 0.0021 parts of ammonium hydroxide (27% in H 2 O, 99.99 +%) to propoxy propanol and stir with a magnetic stirrer at 840 rpm (9 mixtures).
0.0192중량부의 iron(II) oxide (Fe2O3, 10mesh)를 증류수에 분산시킨 용액을 6,000rpm 속도의 magnetic stirrer로 저어준다(9혼합액). A solution in which 0.0192 parts by weight of iron (II) oxide (Fe 2 O 3 , 10mesh) is dispersed in distilled water is stirred with a magnetic stirrer at 6,000 rpm (9 mixtures).
상기 8혼합액과 9혼합액을 섞은 다음 유도관을 통하여 0.013중량부의 n-butyl alcohol과 43.2중량부의 calcium carbonate (CaCO3, 10μm, 98%)와 46.9중량부의 barium carbonate (BaCO3, 26μm, 99%)를 서서히 가하고 6,000 rpm의 속도로 magnetic stirrer로 저어준다(10혼합액).After mixing the 8 mixture and the 9 mixture, 0.013 parts by weight of n-butyl alcohol, 43.2 parts by weight of calcium carbonate (CaCO3, 10μm, 98%) and 46.9 parts by weight of barium carbonate (BaCO3, 26μm, 99%) were gradually added through the induction tube. And stir with a magnetic stirrer at a speed of 6,000 rpm (10 mixtures).
상기 10혼합액에 앞서 증류잔류물을 제거한 6혼합물을 가한 후 85℃에서 4시간 동안 7800 rpm의 속도의 magnetic stirrer로 저어준다.6 mixtures from which the distillation residues were removed prior to the 10 mixtures were added and then stirred with a magnetic stirrer at a speed of 7800 rpm for 4 hours at 85 ° C.
한편, 상기한 바와 같은 방법으로 제조된 화합물은 다양한 용도로 사용할 수 있는데, 그 중에서 가장 바람직한 예는 상기 화합물을 페인트에 배합한 다음, 이를 위에서 언급한 파이프 라인 등에 도포하여 사용할 수 있다. 또한 상기 화합물을 통상적인 테이프에 도포한 후, 이를 파이프 라인 등에 감아서 사용할 수 있다. 이와 같이 본 발명에 따른 방법으로 제조된 산, 염기 및 독성가스 누출 감지를 위한 화합물은 위에서 제시한 페인트나 테이프의 용도로 사용하는 것이 바람직하지만, 그 이외에 다양한 형태로 본 발명의 화합물을 사용할 수 있다.On the other hand, the compound prepared by the method as described above can be used for a variety of uses, the most preferred among them can be used by blending the compound in the paint, and then applying it to the above-mentioned pipeline. In addition, after applying the compound to a conventional tape, it can be used by winding the pipeline or the like. As described above, the compounds for detecting acid, base and toxic gas leaks prepared by the method according to the present invention are preferably used for the use of the above-described paints and tapes. However, the compounds of the present invention may be used in various forms. .
이상에서 살펴본 바와 같이, 본 발명에 따른 산, 염기 및 독성가스 누출 감지를 위한 화합물은 다음과 같은 기술적 특징을 얻을 수 있다.As described above, the compounds for detecting acid, base and toxic gas leakage according to the present invention can obtain the following technical features.
첫째, 본 발명은 기존 제품이 갖는 2차 오염을 방지하면서 산, 염기 누출을 신속하게 감지할 수 있는 제품을 제조하는 방법으로 산, 염기가 누출되는 부분에 탁월한 센서 효과를 보인다. First, the present invention shows an excellent sensor effect in the acid, base leaking part as a method of manufacturing a product that can quickly detect acid, base leakage while preventing secondary contamination of the existing product.
본 발명으로 제조한 센서화합물을 적용한 결과는 다음과 같다.The result of applying the sensor compound prepared by the present invention is as follows.
산업현장에서 사용하는 거의 모든 산, HCl, HNO3, H2SO4, HF, H3PO4, CH3COOH, HCOOH, HBr, HI, C6H5COOH, C6H4(COOH)2, C2H5COOH, HClO4, HClO3, H3BO3에 반응하여 pale yellowish 에서 red로 변색하였고, 거의 모든 염기(알칼리), KOH, NaOH, NH3, NH4OH, Ba(OH)2, Ca(OH)2, C6H5NH2, LiOH, CsOH, Mg(OH)2, Be(OH)2, Sr(OH)2, Ra(OH)2, FeO, CaO, Na2O, CoO, NiO, CuO, Mn(OH)2, RhO에 반응하여 무색에서 붉은 색으로 변하였다.Almost all acids used in industrial sites, HCl, HNO 3 , H 2 SO 4 , HF, H 3 PO 4 , CH 3 COOH, HCOOH, HBr, HI, C 6 H 5 COOH, C 6 H 4 (COOH) 2 , Pale yellowish to red in response to C 2 H 5 COOH, HClO 4 , HClO 3 , H 3 BO 3 , almost all bases (alkali), KOH, NaOH, NH 3 , NH 4 OH, Ba (OH) 2 , Ca (OH) 2 , C 6 H 5 NH 2 , LiOH, CsOH, Mg (OH) 2 , Be (OH) 2 , Sr (OH) 2 , Ra (OH) 2 , FeO, CaO, Na 2 O , Colorless to red in response to CoO, NiO, CuO, Mn (OH) 2 , RhO.
둘째, 산, 염기 누출 시 센서화합물의 반응하는 변색범위가 넓어 산, 염기를 사용하는 모든 공정에 사용할 수 있다.Second, the reaction discoloration range of the sensor compound in the case of acid and base leakage can be used in all processes using acid and base.
(1) Visible Detection Range(Acid Leakage Detection Sensor)(1) Visible Detection Range (Acid Leakage Detection Sensor)
pH range 7~14(산 누출이 없는 경우) : Yellow(570~590nm visible wavelength light region)pH range 7-14 (without acid leakage): Yellow (570-590 nm visible wavelength light region)
pH range 1~3(산 누출 시) : Red(620~750nm visible wavelength light region)pH range 1 to 3 (acid leak): Red (620 to 750 nm visible wavelength light region)
(2) Visible Detection Range(Base Leakage Detection Sensor)(2) Visible Detection Range (Base Leakage Detection Sensor)
pH range 1~7(염기(알칼리)누출이 없는 경우) : White pH range 1 ~ 7 (No base (alkali) leak): White
pH range 10~13 : Red(625~760nm visible wavelength light region)pH range 10 ~ 13: Red (625 ~ 760nm visible wavelength light region)
셋째, 산, 염기 누출 시 감지하는 반응센서의 기능이 탁월하다. 기존 제품보다 10~150배 이상 빠르게 감지한다.Third, the function of the reaction sensor to detect acid and base leakage is excellent. It detects 10 ~ 150 times faster than existing products.
(1) 본 발명에서 제조한 센서가 산 누출 시 반응하는 시간은 다음과 같다.(1) The reaction time of the sensor produced in the present invention upon acid leakage is as follows.
표 1 Detected Reaction Time* for Sensor Paint Coated on the Iron Pipe with Various Acids
Experimental Number Acid Reaction Time
1 HF 1 x 10-5 second
2 HCI 1 x 10-4 second
3 HBr 1 x 10-6 second
4 H2SO4 1 x 10-5 second
5 (COOH)2 1 x 10-6 second
6 TFA 1 x 10-5 second
7 HNO3 1 x 10-6 second
8 H3PO4 1 x 10-6 second
Table 1 Detected Reaction Time <sup> * </ sup> for Sensor Paint Coated on the Iron Pipe with Various Acids
Experimental Number Acid Reaction time
One HF 1 x 10 -5 second
2 HCI 1 x 10 -4 second
3 HBr 1 x 10 -6 second
4 H 2 SO 4 1 x 10 -5 second
5 (COOH) 2 1 x 10 -6 second
6 TFA 1 x 10 -5 second
7 HNO 3 1 x 10 -6 second
8 H 3 PO 4 1 x 10 -6 second
*The reaction times were recorded by the laser flash photolysis method. * The reaction times were recorded by the laser flash photolysis method.
(2) 본 발명에서 제조한 센서가 염기 누출 시 반응하는 시간은 다음 표 2와 같다.(2) The reaction time of the sensor prepared in the present invention during base leakage is shown in Table 2 below.
표 2 Detected Reaction Time* for Sensor Paint Coated on the Iron Pipe with Various Acids
Experimental Number Base Reaction Time
1 KOH 1 x 10-3 second
2 NaOH 1 x 10-5 second
3 NH3 1 x 10-4 second
4 NH4OH 1 x 10-5 second
5 Ba(OH)2 1 x 10-3 second
6 Ca(OH)2 1 x 10-5 second
7 C6H2NH2 1 x 10-4 second
8 LiOH 1 x 10-5 second
9 CsOH 1 x 10-4 second
10 Mg(OH)2 1 x 10-5 second
11 Be(OH)2 1 x 10-3 second
12 Sr(OH)2 1 x 10-5 second
13 Ra(OH)2 1 x 10-3 second
14 FeO 1 x 10-5 second
15 CaO 1 x 10-4 second
16 Na2O 1 x 10-5 second
TABLE 2 Detected Reaction Time <sup> * </ sup> for Sensor Paint Coated on the Iron Pipe with Various Acids
Experimental Number Base Reaction time
One KOH 1 x 10 -3 second
2 NaOH 1 x 10 -5 second
3 NH 3 1 x 10 -4 second
4 NH 4 OH 1 x 10 -5 second
5 Ba (OH) 2 1 x 10 -3 second
6 Ca (OH) 2 1 x 10 -5 second
7 C 6 H 2 NH 2 1 x 10 -4 second
8 LiOH 1 x 10 -5 second
9 CsOH 1 x 10 -4 second
10 Mg (OH) 2 1 x 10 -5 second
11 Be (OH) 2 1 x 10 -3 second
12 Sr (OH) 2 1 x 10 -5 second
13 Ra (OH) 2 1 x 10 -3 second
14 FeO 1 x 10 -5 second
15 CaO 1 x 10 -4 second
16 Na 2 O 1 x 10 -5 second
*The reaction times were recorded by the laser flash photolysis method. * The reaction times were recorded by the laser flash photolysis method.
넷째, 산, 염기 누출 시 빠르게 반응하여 센서의 기능을 나타내는 본 발명제품을 산, 염기가 누출되는 밸브, 펌프, 플렌지, 탱크, 정밀계측기, 시약장, 파이프연결지점, 호스연결지점, 산, 염기 운반용 차량과 산, 염기의 분산, 저장 및 가공단계에서 누출될 때 감지되는 것을 감지하기 위하여 도포할 때 도포 성이 뛰어났다. 본 발명에서 제조한 산, 염기 누출 센서 화합물을 도포하였을 때 도포 성 안정성을 시험하였더니 다음 표 3, 표 4, 표 5, 표 6 및 표 7에서 보는 바와 같이 기존 센서화합물보다 제품의 성능이 탁월하였다.Fourth, the product of the present invention, which reacts rapidly when acid and base leaks to show the function of the sensor, is used for valves, pumps, flanges, tanks, precision measuring instruments, reagent stations, pipe connection points, hose connection points, acids, and base transports. The applicability was excellent when applied to detect leaks detected during vehicle, acid and base dispersion, storage and processing. When the acid and base leak sensor compounds prepared in the present invention were applied, the applicability was tested, and as shown in the following Table 3, Table 4, Table 5, Table 6 and Table 7, the performance of the product was superior to the existing sensor compounds. It was.
표 3 Results of typical scratch test, shear test, and bend test on sensor paint for acid leakage with and without sputter cleaning after coating deposition on iron pipe after scratching treatment corresponding for three month period
Test method Substratetreatment
NoSputterCleaning 5 minSputter Cleaning 10 minSputter Cleaning
Scratch testLc (N) 6.6 29 68
Shear testFc (MNm-2) 2.4 5.2 8.3
Bend test,Mechanicalnotch (MNm-3/2) 1.3 5.6 8.4
Bend test,Copper Notch(MNm-3/2) 0.78 3.5 7.1
TABLE 3 Results of typical scratch test, shear test, and bend test on sensor paint for acid leakage with and without sputter cleaning after coating deposition on iron pipe after scratching treatment corresponding for three month period
Test method Substratetreatment
NoSputterCleaning 5 minSputter Cleaning 10 minSputter Cleaning
Scratch testLc (N) 6.6 29 68
Shear testFc (MNm -2 ) 2.4 5.2 8.3
Bend test, Mechanical notch (MNm -3/2 ) 1.3 5.6 8.4
Bend test, Copper Notch (MNm -3/2 ) 0.78 3.5 7.1
표 4 Results of typical scratch test, shear test, and bend test on sensor paint of acid leakage with and without sputter cleaning after coating deposition on PVC pipe after scratching treatment corresponding for three month period. The experimental results were obtained by Ergonic Workstation and 550 Shear/Scratch Tester, TABER.
Test method Substratetreatment
NoSputterCleaning 5 minSputter Cleaning 10 minSputter Cleaning
Scratch testLc (N) 5.2 27 64
Shear testFc (MNm-2) 2.3 6.5 7.3
Bend test,Mechanicalnotch (MNm-3/2) 1.6 6.3 9.2
Bend test,Copper notch(MNm-3/2) 0.81 4.7 8.0
Table 4 Results of typical scratch test, shear test, and bend test on sensor paint of acid leakage with and without sputter cleaning after coating deposition on PVC pipe after scratching treatment corresponding for three month period. The experimental results were obtained by Ergonic Workstation and 550 Shear / Scratch Tester, TABER.
Test method Substratetreatment
NoSputterCleaning 5 minSputter Cleaning 10 minSputter Cleaning
Scratch testLc (N) 5.2 27 64
Shear testFc (MNm -2 ) 2.3 6.5 7.3
Bend test, Mechanical notch (MNm -3/2 ) 1.6 6.3 9.2
Bend test, Copper notch (MNm -3/2 ) 0.81 4.7 8.0
표 5 Results of typical scratch test, shear test, and bend test on sensor paint for base leakage with and without sputter cleaning after coating deposition on iron pipe after scratching treatment corresponding for three month period. The experimental results were obtained by Ergonic Workstation and 550 Shear/Scratch Tester, TABER.
Test method Substratetreatment
NoSputterCleaning 5 minSputter Cleaning 10 minSputter Cleaning
Scratch testLc (N) 6.5 31 69
Shear testFc (MNm-2) 2.6 5.4 8.1
Bend test,Mechanicalnotch (MNm-3/2) 1.7 5.6 8.7
Bend test,Copper notch(MNm-3/2) 0.83 3.7 7.4
Table 5 Results of typical scratch test, shear test, and bend test on sensor paint for base leakage with and without sputter cleaning after coating deposition on iron pipe after scratching treatment corresponding for three month period. The experimental results were obtained by Ergonic Workstation and 550 Shear / Scratch Tester, TABER.
Test method Substratetreatment
NoSputterCleaning 5 minSputter Cleaning 10 minSputter Cleaning
Scratch testLc (N) 6.5 31 69
Shear testFc (MNm -2 ) 2.6 5.4 8.1
Bend test, Mechanical notch (MNm -3/2 ) 1.7 5.6 8.7
Bend test, Copper notch (MNm -3/2 ) 0.83 3.7 7.4
표 6 Results of typical scratch test, shear test, and bend test on sensor paint of base leakage with and without sputter cleaning after coating deposition on PVC pipe after scratching treatment corresponding for three month period. The experimental results were obtained by Ergonic Workstation and 550 Shear/Scratch Tester, TABER.
Test method Substratetreatment
NoSputterCleaning 5 minSputter Cleaning 10 minSputter Cleaning
Scratch testLc (N) 5.6 28 65
Shear testFc (MNm-2) 2.8 6.7 7.4
Bend test,Mechanicalnotch (MNm-3/2) 1.6 6.4 9.8
Bend test,Copper notch(MNm-3/2) 0.84 4.9 8.2
Table 6 Results of typical scratch test, shear test, and bend test on sensor paint of base leakage with and without sputter cleaning after coating deposition on PVC pipe after scratching treatment corresponding for three month period. The experimental results were obtained by Ergonic Workstation and 550 Shear / Scratch Tester, TABER.
Test method Substratetreatment
NoSputterCleaning 5 minSputter Cleaning 10 minSputter Cleaning
Scratch testLc (N) 5.6 28 65
Shear testFc (MNm -2 ) 2.8 6.7 7.4
Bend test, Mechanical notch (MNm -3/2 ) 1.6 6.4 9.8
Bend test, Copper notch (MNm -3/2 ) 0.84 4.9 8.2
표 7 Relationship between porocity and thickness of sensor paints of acid leakage (A) and base leakage (B) after scratching treatment corresponding for three month period under the condition of each adhesive interlayer on the critical load of 120 Lc grams. The experimental results were obtained by Ergonic Workstation and 550 Shear/Scratch Tester, TABER.
Thickness (μm) Porocity (dots/in2)
(A) (B)
Iron plate PVC plate Iron plate PVC plate
10.0 2760.0 1876 2459.9 1657
20.0 4832.7 2145 4873.2 1986
30.0 7843.2 3547 7682.5 2876
40.0 10982 4587 9834.3 3652
50.0 15680 5490 13722 4898
TABLE 7 Relationship between porocity and thickness of sensor paints of acid leakage (A) and base leakage (B) after scratching treatment corresponding for three month period under the condition of each adhesive interlayer on the critical load of 120 Lc grams. The experimental results were obtained by Ergonic Workstation and 550 Shear / Scratch Tester, TABER.
Thickness (μm) Porocity (dots / in 2 )
(A) (B)
Iron plate PVC plate Iron plate PVC plate
10.0 2760.0 1876 2459.9 1657
20.0 4832.7 2145 4873.2 1986
30.0 7843.2 3547 7682.5 2876
40.0 10982 4587 9834.3 3652
50.0 15680 5490 13722 4898
The above results show the sensor paints are adequate for use of iron pipe or PVC pipe at least three months period. The experimental results were obtained by Ergonic Workstation and 550 Shear/Scratch Tester, TABER. The above results show the sensor paints are adequate for use of iron pipe or PVC pipe at least three months period. The experimental results were obtained by Ergonic Workstation and 550 Shear/Scratch Tester, TABER.The above results show the sensor paints are adequate for use of iron pipe or PVC pipe at least three months period. The experimental results were obtained by Ergonic Workstation and 550 Shear / Scratch Tester, TABER. The above results show the sensor paints are adequate for use of iron pipe or PVC pipe at least three months period. The experimental results were obtained by Ergonic Workstation and 550 Shear / Scratch Tester, TABER.
상기 표 3~7에서 보는 바와 같이 본 발명에서 제조한 산, 염기 누출 센서 화합물을 철관 표면에 도포한 후 표면을 극한 상태의 조건에서의 반응결과는 일반 페인트를 표면에 도포하였을 때 보다 본 발명에서 제조한 것이 21~38 %이상 안정함을 알 수 있다.As shown in Tables 3 to 7, after the acid and base leak sensor compounds prepared in the present invention were applied to the surface of the steel pipe, the reaction result in the condition of the extreme condition was that in the present invention, when general paint was applied to the surface. It can be seen that the prepared is more than 21 ~ 38%.
또한 극한 조건이 아닌 일반 산업현장에서 산 및 염기가 누출될 때 본 발명에서 제조한 산. 염기누출센서 화합물의 도포성 안정성을 알아보기 위하여 철관과 PVC관에 도포한 다음 누출 된 산. 염기와 반응하기 전까지의 지속과정을 테스트한 결과는 다음 표 8, 표 9, 표 10, 표 11에서 보는 바와 같다.In addition, the acid produced in the present invention when the acid and base leakage in general industrial sites, not extreme conditions. Acid leaked after application to iron and PVC pipes to check the coating stability of base leak sensor compound. The results of the test until the reaction with the base are shown in Table 8, Table 9, Table 10, and Table 11 below.
표 8 ASTM Standard Test for Acid Sensor Paint Coated on the Steel Pipes by the Spot Methods (Triple-Spot Test (TST) and Single-Spot Test (SST)) after coated 18 months
TST TST SST TST
Coating Total Both Sides One Side Total Both Sides One Side
Designation (oz/ft2) (oz/ft2) (oz/ft2) (oz/ft2)
G01 no detection no detection no detection no detection
G30 0.28 0.08 0.26 0.06
G40 0.41 0.10 0.28 0.09
G60 0.61 0.17 0.34 0.13
G90 0.92 0.366 0.46 0.17
G100 1.02 0.37 0.73 0.18
G115 1.14 0.41 1.25 0.46
G140 1.47 0.52 1.43 0.67
G165 1.68 0.62 1.65 0.73
G185 1.84 0.63 1.74 0.89
G210 2.17 0.75 1.95 0.97
G235 2.36 0.89 2.01 1.25
G300 2.98 1.03 2.35 1.42
G360 3.62 1.30 3.03 1.52
Table 8 ASTM Standard Test for Acid Sensor Paint Coated on the Steel Pipes by the Spot Methods (Triple-Spot Test (TST) and Single-Spot Test (SST)) after coated 18 months
TST TST SST TST
Coating Total both sides One Side Total Both Sides One side
Designation (oz / ft 2 ) (oz / ft 2 ) (oz / ft 2 ) (oz / ft 2 )
G01 no detection no detection no detection no detection
G30 0.28 0.08 0.26 0.06
G40 0.41 0.10 0.28 0.09
G60 0.61 0.17 0.34 0.13
G90 0.92 0.366 0.46 0.17
G100 1.02 0.37 0.73 0.18
G115 1.14 0.41 1.25 0.46
G140 1.47 0.52 1.43 0.67
G165 1.68 0.62 1.65 0.73
G185 1.84 0.63 1.74 0.89
G210 2.17 0.75 1.95 0.97
G235 2.36 0.89 2.01 1.25
G300 2.98 1.03 2.35 1.42
G360 3.62 1.30 3.03 1.52
*The data show the preservation period of the acid sensor paint after coated on the steel pipe is 18 months. The experimental results were obtained by Ergonic Workstation and 550 Shear/Scratch Tester, TABER.* The data show the preservation period of the acid sensor paint after coated on the steel pipe is 18 months. The experimental results were obtained by Ergonic Workstation and 550 Shear / Scratch Tester, TABER.
표 9 ASTM Standard Test for Base Sensor Paint Coated on the Steel Pipes by the Spot Methods (Triple-Spot Test (TST) and Single-Spot Test (SST)) after Coated 17 Months
TST TST SST TST
Coating Total Both Sides One Side Total Both Sides One Side
Designation (oz/ft2) (oz/ft2) (oz/ft2) (oz/ft2)
G01 no detection no detection no detection no detection
G30 0.25 0.07 0.24 0.03
G40 0.39 0.07 0.25 0.07
G60 0.59 0.15 0.31 0.11
G90 0.87 0.33 0.44 0.15
G100 1.01 0.35 0.70 0.17
G115 1.12 0.39 1.22 0.42
G140 1.39 0.48 1.41 0.64
G165 1.63 0.56 1.63 0.69
G185 1.82 0.61 1.69 0.78
G210 2.14 0.72 1.91 0.95
G235 2.33 0.84 1.99 1.22
G300 2.94 0.09 2.31 1.39
G360 3.60 1.28 3.02 1.48
Table 9 ASTM Standard Test for Base Sensor Paint Coated on the Steel Pipes by the Spot Methods (Triple-Spot Test (TST) and Single-Spot Test (SST)) after Coated 17 Months
TST TST SST TST
Coating Total both sides One Side Total Both Sides One side
Designation (oz / ft 2 ) (oz / ft 2 ) (oz / ft 2 ) (oz / ft 2 )
G01 no detection no detection no detection no detection
G30 0.25 0.07 0.24 0.03
G40 0.39 0.07 0.25 0.07
G60 0.59 0.15 0.31 0.11
G90 0.87 0.33 0.44 0.15
G100 1.01 0.35 0.70 0.17
G115 1.12 0.39 1.22 0.42
G140 1.39 0.48 1.41 0.64
G165 1.63 0.56 1.63 0.69
G185 1.82 0.61 1.69 0.78
G210 2.14 0.72 1.91 0.95
G235 2.33 0.84 1.99 1.22
G300 2.94 0.09 2.31 1.39
G360 3.60 1.28 3.02 1.48
*The data show the preservation period of the base sensor paint after coated on the steel pipe is 17 months. The experimental results were obtained by Ergonic Workstation and 550 Shear/Scratch Tester, TABER.* The data show the preservation period of the base sensor paint after coated on the steel pipe is 17 months. The experimental results were obtained by Ergonic Workstation and 550 Shear / Scratch Tester, TABER.
표 10 ASTM Standard Test for Acid Sensor Paint Coated on the PVC Pipes by the Spot Methods (Triple-Spot Test (TST) and Single-Spot Test (SST)) after Coated 19 months
TST TST SST TST
Coating Total Both Sides One Side Total Both Sides One Side
Designation (oz/ft2) (oz/ft2) (oz/ft2) (oz/ft2)
G01 no detection no detection no detection no detection
G30 0.31 0.12 0.29 0.08
G40 0.43 0.15 0.31 0.12
G60 0.65 0.20 0.37 0.16
G90 0.94 0.39 0.49 0.19
G100 1.08 0.41 0.77 0.21
G115 1.17 0.46 1.29 0.49
G140 1.51 0.57 1.46 0.71
G165 1.72 0.65 1.68 0.76
G185 1.88 0.69 1.77 0.92
G210 2.21 0.78 1.99 1.02
G235 2.39 0.92 2.06 1.28
G300 3.02 1.06 2.42 1.46
G360 3.67 1.35 3.12 1.57
Table 10 ASTM Standard Test for Acid Sensor Paint Coated on the PVC Pipes by the Spot Methods (Triple-Spot Test (TST) and Single-Spot Test (SST)) after Coated 19 months
TST TST SST TST
Coating Total both sides One Side Total Both Sides One side
Designation (oz / ft 2 ) (oz / ft 2 ) (oz / ft 2 ) (oz / ft 2 )
G01 no detection no detection no detection no detection
G30 0.31 0.12 0.29 0.08
G40 0.43 0.15 0.31 0.12
G60 0.65 0.20 0.37 0.16
G90 0.94 0.39 0.49 0.19
G100 1.08 0.41 0.77 0.21
G115 1.17 0.46 1.29 0.49
G140 1.51 0.57 1.46 0.71
G165 1.72 0.65 1.68 0.76
G185 1.88 0.69 1.77 0.92
G210 2.21 0.78 1.99 1.02
G235 2.39 0.92 2.06 1.28
G300 3.02 1.06 2.42 1.46
G360 3.67 1.35 3.12 1.57
*The data show the preservation period of the acid sensor paint after coated on the steel pipe is 19 months. The experimental results were obtained by Ergonic Workstation and 550 Shear/Scratch Tester, TABER.* The data show the preservation period of the acid sensor paint after coated on the steel pipe is 19 months. The experimental results were obtained by Ergonic Workstation and 550 Shear / Scratch Tester, TABER.
표 11 ASTM Standard Test for Base Sensor Paint Coated on the PVC Pipe by the Spot Methods (Triple-Spot Test (TST) and Single-Spot Test (SST)) after Coated 18 months
TST TST SST TST
Coating Total Both Sides One Side Total Both Sides One Side
Designation (oz/ft2) (oz/ft2) (oz/ft2) (oz/ft2)
G01 no detection no detection no detection no detection
G30 0.28 0.10 0.27 0.04
G40 0.41 0.14 0.29 0.09
G60 0.62 0.17 0.35 0.13
G90 0.91 0.37 0.47 0.17
G100 1.04 0.39 0.72 0.19
G115 1.15 0.42 1.25 0.45
G140 1.41 0.52 1.44 0.66
G165 1.66 0.61 1.66 0.72
G185 1.85 0.65 1.69 0.80
G210 2.19 0.77 1.94 0.97
G235 2.37 0.86 2.02 1.26
G300 2.98 0.92 2.34 1.43
G360 3.66 1.33 3.05 1.50
Table 11 ASTM Standard Test for Base Sensor Paint Coated on the PVC Pipe by the Spot Methods (Triple-Spot Test (TST) and Single-Spot Test (SST)) after Coated 18 months
TST TST SST TST
Coating Total both sides One Side Total Both Sides One side
Designation (oz / ft 2 ) (oz / ft 2 ) (oz / ft 2 ) (oz / ft 2 )
G01 no detection no detection no detection no detection
G30 0.28 0.10 0.27 0.04
G40 0.41 0.14 0.29 0.09
G60 0.62 0.17 0.35 0.13
G90 0.91 0.37 0.47 0.17
G100 1.04 0.39 0.72 0.19
G115 1.15 0.42 1.25 0.45
G140 1.41 0.52 1.44 0.66
G165 1.66 0.61 1.66 0.72
G185 1.85 0.65 1.69 0.80
G210 2.19 0.77 1.94 0.97
G235 2.37 0.86 2.02 1.26
G300 2.98 0.92 2.34 1.43
G360 3.66 1.33 3.05 1.50
*The data show the preservation period of the base sensor paint after coated on the PVC pipe is 18 months. The experimental results were obtained by Ergonic Workstation and 550 Shear/Scratch Tester, TABER.* The data show the preservation period of the base sensor paint after coated on the PVC pipe is 18 months. The experimental results were obtained by Ergonic Workstation and 550 Shear / Scratch Tester, TABER.
또한 상기 표 8, 9, 10, 11에서 보는 바와 같이 본 발명에서 제조한 산, 염기 누출 화합물을 철관 표면에 도포한 후 표면을 일반 제조업 현장의 온화한 자연 상태의 조건에서의 반응결과도 일반 페인트를 표면에 도포하였을 때 보다 본 발명에서 제조한 것이 22~34 %이상 안정함을 알 수 있다.In addition, as shown in Tables 8, 9, 10, and 11, after the acid and base leaking compounds prepared in the present invention were applied to the surface of the steel pipe, the surface of the reaction resulted in the conditions of mild natural conditions in general manufacturing sites. When applied to the surface it can be seen that 22 to 34% or more is prepared in the present invention more stable.
다섯째, 본 발명에서 제조한 산, 염기 누출 센서 화합물을 공정에 적용하였을 때 화학적으로 안정하다. 즉, 산, 염기가 누출되기 직전까지 공기 중의 다른 분자와 반응하여 센서 자체의 기능을 상실하지 않고 인체에 해를 미치지 않는다. 센서분자자체의 안정도가 크기 때문에 모든 산업 생산 공정에 적용할 수 있다.Fifth, the acid and base leak sensor compounds prepared in the present invention are chemically stable when applied to the process. In other words, it reacts with other molecules in the air until the acid and base are leaked, and the sensor itself does not lose its function and does not harm the human body. The high stability of the sensor molecules makes them suitable for all industrial production processes.
여섯째, 본 발명에서 제조한 산 염기 누출센서화합물은 친환경적으로 제조되었기 때문에 도포 자나 도포 후 공정에서 작업하는 사람에게 2차 오염을 야기시키지 않는다.Sixth, since the acid base leak sensor compound prepared in the present invention is manufactured in an environmentally friendly manner, it does not cause secondary pollution to the applicator or the person working in the post-application process.
본 발명은 화합물을 도포하였을 때 2차 오염을 일으키지 않는 친환경적 화합물을 제조하고 동시에 발현하는 색깔의 변화가 가시광선영역에서 선명하게 빠른 시간 내에 반응하여 최초 발견자가 쉽게 대응하여 안전을 도모할 수 있는 장점이 있다. 뿐만 아니라 화합물질 자체가 갖는 2차 오염원을 차단하고 화합물질이 마이크로 초 시간 이내의 빠른시간에 반응하여 최초 발견자가 신속하게 대응할 수 있도록 선명한 색깔로 변색하는 기능을 구현할 수 있는 이점이 있다.The present invention produces an environmentally friendly compound that does not cause secondary pollution when the compound is applied and simultaneously changes the color that is expressed in the visible region in a quick and quick response, so that the first detector can easily respond to safety. There is this. In addition, it has the advantage of blocking the secondary pollutant of the compound itself, and the compound reacts to the fast time within the microsecond time to implement the function of discoloring the vivid color so that the first detector can respond quickly.
또한, 본 발명은 종래의 제품이 갖는 한계를 극복하기 위하여 2차 오염원을 완전히 차단하여 친환경적으로 제조하기 위하여 인체에 전혀 무해하며 산, 염기와 반응 시 시각적으로 색깔의 변화를 빠르고 정확하게 감지할 수 있고, 공기 중에서 자동 산화, 환원이 용이하지 않은 안정된 분자 구조를 열역학적으로 테스트한 분자를 사용하여 화학 안정성이 뛰어나고 인체 독성이 전혀없는 상승적인 효과가 있다.In addition, the present invention is completely harmless to the human body in order to completely block the secondary pollutant in order to overcome the limitations of the conventional products and to produce environmentally friendly, it is possible to quickly and accurately detect the change of color visually when reacting with acid, base and Using thermodynamically tested molecules that have a stable molecular structure that is not easily oxidized or reduced in air, it has a synergistic effect with excellent chemical stability and no human toxicity.

Claims (9)

  1. Methylene blue를 증류수에 녹이고 sorbitol에 녹인 용액에 가하여 제 1 혼합액을 만드는 과정과 이 용액을 sorbitol에 녹인 용액 에 가하여 제 2혼합액을 제조하는 과정으로 이루어짐을 특징으로 하는 산, 염기 및 독성가스 누출 감지를 위한 화합물의 제조방법.Detecting acid, base, and toxic gas leaks by dissolving methylene blue in distilled water and adding it to a solution dissolved in sorbitol to make a first mixed solution and adding this solution to a solution dissolved in sorbitol. Method for preparing the compound for.
  2. 제1항에 있어서,The method of claim 1,
    Alizarin yellow를 증류수를 sorbitol에 녹인 용액에 가하여 제 3 혼합액을 만드는 과정과 ethyl alcohol과 palm oil을 가하여 제 5 혼합액을 제조하는 과정으로 이루어짐을 특징으로 하는 산, 염기 및 독성가스 누출 감지를 위한 화합물의 제조방법.Alizarin yellow is added to a solution of distilled water in sorbitol to form a third mixture, and a fifth mixture is prepared by adding ethyl alcohol and palm oil to detect acid, base, and toxic gas leaks. Manufacturing method.
  3. Thymol blue를 증류수에 sorbitol에 녹인 용액에 가하고 ethyl alcohol을 가하여 제 1 혼합액을 제조하는 과정. phenolphthalein을 증류수를 sorbitol에 녹인 용액에 가하고 무수 ethyl alcohol을 가하여 제 2 혼합액을 제조하는 과정으로 이루어짐을 특징으로 하는 산, 염기 및 독성가스 누출 감지를 위한 화합물의 제조방법.A process of preparing a first mixed solution by adding thymol blue to a solution of sorbitol in distilled water and adding ethyl alcohol. A process for preparing an acid, base and toxic gas leak, characterized in that the phenolphthalein is added to a solution of distilled water in sorbitol and anhydrous ethyl alcohol is added to prepare a second mixture.
  4. 제3항에 있어서,The method of claim 3,
    Cresol red를 증류수를 sorbitol에 녹인 용액에 가하여 제 3 혼합액을 제조하는 과정과 palm oil을 ethyl alcohol을 용해시켜 제 5 혼합액을 제조하는 과정으로 이루어짐을 특징으로 하는 산, 염기 및 독성가스 누출 감지를 위한 화합물의 제조방법.For the detection of acid, base and toxic gas leakage, the process consists of preparing a third mixture by adding Cresol red to a solution of distilled water in sorbitol and preparing a fifth mixture by dissolving ethyl alcohol in palm oil. Method for preparing the compound.
  5. 제1항 내지 제3항 중 어느 하나의 항에 있어서,The method according to any one of claims 1 to 3,
    혼합액을 감압 하에서 진공 증류하여 증류잔류물을 제거하는 과정과 증류잔물을 제거한 혼합액에 안정제인 1,3-dimethyl aniline을 가하는 과정으로 이루어짐을 특징으로 하는 산, 염기 및 독성가스 누출 감지를 위한 화합물의 제조방법.Vacuum distillation of the mixture under reduced pressure to remove distillation residues and a process for adding 1,3-dimethyl aniline as a stabilizer to the mixture solution from which the distillation residues were removed. Manufacturing method.
  6. 제1항 내지 제3항 중 어느 하나의 항에 있어서,The method according to any one of claims 1 to 3,
    2차 증류수에 triethylamine을 넣어 제7 혼합액을 제조하는 과정과 titanium dioxide를 가하여 제 8 혼합액을 제조하는 과정으로 이루어짐을 특징으로 하는 산, 염기 및 독성가스 누출 감지를 위한 화합물의 제조방법.A process for preparing a compound for acid, base and toxic gas leakage detection comprising the process of preparing a seventh mixed solution by adding triethylamine to secondary distilled water and preparing an eighth mixed solution by adding titanium dioxide.
  7. 제1항 내지 제3항 중 어느 하나의 항에 있어서,The method according to any one of claims 1 to 3,
    Ammonium hydroxide를 propoxy propanol에 넣어 제 9 혼합액을 제조하는 과정과 제 9 혼합액에 n-butyl alcohol과 calcium carbonate를 가하여 제 10 혼합액을 제조하는 과정으로 이루어짐을 특징으로 하는 산, 염기 및 독성가스 누출 감지를 위한 화합물의 제조방법.The detection of acid, base, and toxic gas leaks consists of preparing a ninth mixture by adding ammonium hydroxide to propoxy propanol and preparing a tenth mixture by adding n-butyl alcohol and calcium carbonate to the ninth mixture. Method for preparing a compound for
  8. 산, 염기 및 독성가스 누출 감지를 위한 화합물이 배합된 페인트.Paint formulated with compounds for acid, base and toxic gas leak detection.
  9. 산, 염기 및 독성가스 누출 감지를 위한 화합물이 도포된 테이프.Tape coated with compounds for acid, base and toxic gas leak detection.
PCT/KR2013/009374 2013-06-28 2013-10-21 Manufacturing method for compound for detecting acid, alkali and toxic gas leaks, and use thereof WO2014208825A1 (en)

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KR101832412B1 (en) 2016-04-18 2018-02-26 주식회사 아바오 Acid detection sensor fabricated by conductive polymer and conductive carbon
KR20200012783A (en) * 2018-07-27 2020-02-05 한양대학교 산학협력단 Paint for detection of hydrogen ion concentration and fabricating method of the same

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