CN115521727B - Color-changing adhesive tape for ammonia gas leakage detection and preparation method thereof - Google Patents

Color-changing adhesive tape for ammonia gas leakage detection and preparation method thereof Download PDF

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CN115521727B
CN115521727B CN202211121109.1A CN202211121109A CN115521727B CN 115521727 B CN115521727 B CN 115521727B CN 202211121109 A CN202211121109 A CN 202211121109A CN 115521727 B CN115521727 B CN 115521727B
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adhesive tape
ammonia gas
color
changing
tetrahydrofuran
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CN115521727A (en
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樊宝峰
张宪国
黄毅杰
项冲
陈升山
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Beijing Zhongneng Hangke Technology Co ltd
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00—Adhesives in the form of films or foils
    • C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04—Polysiloxanes
    • 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
    • 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
    • G01N21/783—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 for analysing gases
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J2423/00—Presence of polyolefin
    • C09J2423/10—Presence of homo or copolymers of propene
    • C09J2423/105—Presence of homo or copolymers of propene in the release coating
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters

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  • Physics & Mathematics (AREA)
  • Organic Chemistry (AREA)
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  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The invention discloses a color-changing adhesive tape for ammonia gas leakage detection and a preparation method thereof, wherein the color-changing adhesive tape comprises the following components: 107 silicon rubber, a reinforcing agent, a cross-linking catalyst, a metal oxide and metal nano particles; the adhesive tape prepared by the invention can avoid the problem that curing failure is easy to occur in the process of preparing the adhesive tape by using titanate as a catalyst in the prior art, and the special molecular structure of the adhesive tape can generate higher functionality and more crosslinking points in the curing process of the adhesive tape, so that stronger limitation is formed on a molecular chain, the crosslinking depth of the adhesive tape is deepened, and the curing of the adhesive tape can be promoted; the color-changing adhesive tape provided by the invention is simple and direct in ammonia gas detection, can quickly perform color-changing early warning, is high in sensitivity and wide in application range, and can be widely applied to ammonia gas storage containers, pipelines and equipment; when in use, the color-changing adhesive tape is only needed to be pasted at the position where ammonia gas leakage is easy to occur, and the method is economical, practical, simple to operate and high in accuracy.

Description

Color-changing adhesive tape for ammonia gas leakage detection and preparation method thereof
Technical Field
The invention relates to the technical field of ammonia gas leakage detection, in particular to a color-changing adhesive tape for ammonia gas leakage detection and a preparation method thereof.
Background
Ammonia gas is an important chemical raw material, has lower density than air, and is widely applied to the industries of fertilizer production, petrochemical industry, biological pharmacy and the like. Ammonia mainly comes from production sites of various chemicals, the most important is the production of synthetic ammonia and the production of nitrogen fertilizers, for example, the production of ammonium bicarbonate, urea and ammonium chloride takes ammonia as raw materials; production of nitric acid, ammoxidation to generate nitric acid, dye production and ammonia for synthesis of indigo; ammonia is used in the production of plastics, synthetic fibers, synthetic rubber, plexiglass, polyacrylonitrile fibers, nitrile rubber, and the like.
For convenience of use, a pressurized method is usually adopted to convert ammonia gas into liquid ammonia for storage in industrial production, and the vaporization of the liquid ammonia can absorb a large amount of heat, so that the liquid ammonia is a green refrigerant. The domestic refrigeration industry generally adopts two refrigerants: freon and liquid ammonia; freon is used for refrigerator, air conditioner more, and is costly, and freon can cause irreversible destruction to the ozone layer moreover, and the liquid ammonia system contains the high pressure, through pipeline and valve interconnect, needs the manual work to operate, when the valve junction leakproofness is not good, takes place the leakage accident very easily. After leakage, the liquid ammonia can be quickly vaporized into ammonia cloud, and a large-area contamination area is formed.
People are exposed to ammonia gas in excess of 500ppm to cause acute poisoning, and excessive ammonia gas inhalation can cause serious effects on the human body, such as damage to the central nervous system, brain, lungs and eyes, causing acute bronchitis, cyanosis, chest pain, headache, throat inflammation, vomiting, loss of consciousness, and fever. In addition, exhaled ammonia gas is one of the key biomarkers for diagnosing diseases such as lung or kidney, and for people suffering from the diseases, monitoring ammonia gas by a breath analyzer is a very important detection means in clinical practice. It is necessary to accurately measure ammonia gas and, at the same time, diagnose diseases associated with high ammonia gas exhaled from the human body, prevent fatal accidents caused by excessive exposure to high ammonia gas and environmental pollution problems caused by excessive discharge of ammonia gas into the atmosphere. Therefore, in recent years, ammonia gas detection has attracted much attention.
CN201510372140.6 discloses an ammonia gas detection reagent and a preparation method thereof, wherein the reagent comprises the following components in parts by mass: 5-12 parts of sodium nitrite, 5-10 parts of indophenol blue, 4-8 parts of potassium iodide, 5-12 parts of polyethylene glycol, 2-7 parts of oxalic acid, 2-5 parts of potassium hydroxide, 2-7 parts of phosphorus trichloride and 25-40 parts of deionized water. A preparation method of an ammonia gas detection reagent comprises the following preparation steps: preparing a premixed solution; (2) obtaining a clear mixed solution; (3) And standing for 4-8h in vacuum, and sealing to obtain the ammonia gas detection reagent. The ammonia gas detection reagent provided by the invention combines the advantages of a Nashi reagent colorimetric method and an indophenol blue colorimetric method, has the characteristics of high sensitivity, accurate measurement result and simple operation method, and is suitable for measuring the ammonia gas content in a home or office place and a breeding industry environment. The reagent has the characteristics of convenience, rapidness and the like, but is not suitable for detecting ammonia gas leakage in ammonia gas storage containers, ammonia gas transportation pipelines or equipment.
CN111662650A discloses a hydrogen-sensitive color-changing detection tape, a preparation method and an application thereof, in particular to a self-adhesive tape which can change color under the contact of hydrogen, and also relates to a preparation method and a use method of the self-adhesive tape. The invention has the advantages of intrinsic safety, simple and convenient fixation and simple and visual representation mode, can indicate the position of the leakage point through local color change, makes up the defects of limited positioning capability of the pressure loss hydrogen leakage detection leakage point and difficulty in finding tiny leakage, makes up the defect of high layout cost of electronic hydrogen detection equipment, is a supplement of a common hydrogen leakage detection method, greatly reduces the time cost for searching the leakage position after leakage occurs, promotes emergency response and has extremely high popularization and use values. However, the method has the problems that the adhesive tape is small in adhesive force and peeling force, cannot be well adhered to equipment to be detected, and is easy to cause accuracy reduction.
Disclosure of Invention
In view of the above defects in the prior art, the technical problem to be solved by the present invention is to provide a color-changing adhesive tape for ammonia gas leakage detection with high accuracy and low cost, and a preparation method thereof.
In order to achieve the purpose, the invention provides the color-changing adhesive tape for ammonia gas leakage detection, which has the advantages of low economic cost, high accuracy and sensitive reaction, the liquid 107 silicon rubber is modified by the special modifier, so that a plurality of active group carboxyl groups are introduced into the modifier molecules, the liquid 107 silicon rubber molecules can have more crosslinking points, a more complex and compact crosslinking structure can be generated under the action of the crosslinking agent, the flowing of a colloid can be inhibited, and the solidification is accelerated.
In order to achieve the purpose of the invention, the invention adopts the following technical scheme:
a color-changing adhesive tape for ammonia gas leakage detection comprises the following components: 107 silicon rubber, a reinforcing agent, a cross-linking catalyst, a metal oxide and metal nano particles.
Preferably, the color-changing adhesive tape for ammonia gas leakage detection comprises the following components in parts by weight: 80-120 parts of 107 silicon rubber, 20-50 parts of reinforcing agent, 5-10 parts of cross-linking agent, 0.5-1.5 parts of cross-linking catalyst, 0.1-0.3 part of anti-aging agent, 1-5 parts of metal oxide and 0.01-1 part of metal nano-particles.
Preferably, the color-changing adhesive tape for detecting ammonia gas leakage can also comprise dyes, preservatives, mildewproof agents and flame retardants commonly used in the field.
Preferably, the 107 silicone rubber is a modified 107 silicone rubber, and the preparation method comprises the following steps:
uniformly stirring and mixing 60-100g of 107 silicone rubber, 2-3g of modifier and 200-300mL of 20-40wt% sodium methoxide methanol solution, heating to 40-60 ℃, adding 5-10g of 3-aminopropyltrimethoxysilane at the temperature, stirring for 30-50min at 2000-3000rpm, adding 4-7g of n-octylamine, and stirring for 10-15min to obtain the modified 107 silicone rubber.
Preferably, the preparation method of the modifier comprises the following steps:
1) Dissolving 30-50g of methallyl alcohol in 500-1000mL of tetrahydrofuran at 0-5 ℃, adding 20-25g of metal sodium, stirring at room temperature for reaction for 10-12h, heating to 60-70 ℃, and continuing to react at the temperature for 10-12h to obtain a sodium alkoxide solution;
2) Dissolving 40-60g of hexachlorocyclotriphosphazene in 200-300mL of tetrahydrofuran to obtain tetrahydrofuran solution of hexachlorocyclotriphosphazene, then dropwise adding the tetrahydrofuran solution of hexachlorocyclotriphosphazene into sodium alkoxide solution at the speed of 1-2 drops/second, and reacting at 60-70 ℃ for 40-48h; after the reaction is finished, cooling to room temperature, concentrating under reduced pressure to 20-30% of the original volume, and adding 60-100mL of 50-70wt% ethanol water solution into the residue; stirring for 20-30min, filtering, collecting precipitate, washing the precipitate with water and anhydrous ethanol for 2-3 times, and drying at 50-60 deg.C for 6-8 hr to obtain the modifier.
Further preferably, the preparation method of the modifier comprises the following steps:
1) Dissolving 30-50g of methallyl alcohol in 500-1000mL of tetrahydrofuran at 0-5 ℃, adding 20-25g of metal sodium, stirring at room temperature for reaction for 10-12h, heating to 60-70 ℃, and continuing to react at the temperature for 10-12h to obtain a sodium alkoxide solution;
2) Dissolving 40-60g of hexachlorocyclotriphosphazene in 200-300mL of tetrahydrofuran to obtain tetrahydrofuran solution of hexachlorocyclotriphosphazene, then dropwise adding the tetrahydrofuran solution of hexachlorocyclotriphosphazene into sodium alkoxide solution at the speed of 1-2 drops/second, and reacting for 40-48h at 60-70 ℃; after the reaction is finished, cooling to room temperature, concentrating under reduced pressure to 20-30% of the original volume, and adding 60-100mL of 50-70wt% ethanol water solution into the residue; stirring for 20-30min, filtering, collecting precipitate, washing the precipitate with water and anhydrous ethanol for 2-3 times, drying at 50-60 deg.C for 6-8 hr, and marking as M 1 ；
3) 3 to 6g of dithiodibenzoic acid and 8 to 15g of M in the step 2) 1 Mixing and stirring 6-10g of benzoin dimethyl ether and 100-200mL of tetrahydrofuran, irradiating the mixture for 10-15min by using ultraviolet light at normal temperature after the raw materials are completely dissolved, adding 50-100mL of 50-75wt% ethanol aqueous solution for precipitation, filtering the mixture after 30-50min, collecting precipitates, washing the precipitates for 2-3 times by using water and absolute ethyl alcohol respectively, and drying the precipitates for 6-8h at 50-60 ℃ to obtain the modifier.
The adhesive tape prepared by the invention is a three-dimensional reticular elastomer formed by crosslinking a linear structure through 107 silicon rubber, metal oxide and metal nano particles under the action of substances such as a crosslinking agent, a crosslinking catalyst and the like. In the prior art, an organic tin compound or titanate is mostly used as a catalyst, and the action of the catalyst remained in a matrix can break Si-O bonds in a silicon rubber structure, so that the matrix becomes soft, the strength is reduced, and the problem of curing failure is easy to occur. The adhesive tape prepared by the inventor has good storage stability and adhesive property by modifying 107 silicone rubber and obviously enhancing the adhesive activity of the 107 silicone rubber. The modifier used in the invention is a molecular skeleton composed of inorganic phosphorus and nitrogen elements, and the side chain is an inorganic-organic compound composed of organic groups, the inventor finds that when the modified 107 silicone rubber is used for preparing the adhesive tape, the problem that the adhesive tape is easy to cure and lose efficacy in the process of preparing the adhesive tape by using titanate as a catalyst in the prior art can be avoided, and the special molecular structure of the modified 107 silicone rubber can generate higher functionality and more crosslinking points in the curing process of the adhesive tape, so that stronger limitation is formed on the molecular chain, the crosslinking depth of the adhesive tape can be deepened, and the curing of the adhesive tape can be promoted; the modifier is further modified, so that a plurality of active groups of carboxyl are introduced into molecules of the modifier, liquid 107 silicon rubber molecules can have more crosslinking points, and a more complex and compact crosslinking structure is generated under the action of the crosslinking agent, so that colloid flow can be inhibited, curing is accelerated, surface drying time is shortened, and the bonding effect is further improved; and the modifier endows the adhesive tape with good flame retardant property.
Preferably, the reinforcing agent is one or a mixture of two or more of nano calcium carbonate, white carbon black, quartz powder, titanium dioxide, kaolin, carbon black and carbon nano tubes.
Preferably, the cross-linking agent is one or more of methyl tributyrinoxime silane, vinyl tributyrinoxime silane, methyl trimethoxy silane, ethyl trimethoxy silane and methyl triacetoxy silane.
Preferably, the crosslinking catalyst is one or a mixture of two or more of dibutyltin dilaurate, dihexyltin dilaurate, dibutyltin diacetate, dihexyltin diacetate, isopropyl titanate and butyl titanate.
Preferably, the anti-aging agent is one selected from 2- (2H) -benzotriazol-2-yl) -6-dodecyl-4-methylphenol, 2-cyano-3, 3-diphenyl-2-ethylhexyl acrylate, pentaerythritol tetrakis [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] and n-octadecyl 3- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate.
Preferably, the metal oxide is one or more of tungsten oxide, molybdenum oxide, tungstic acid and molybdic acid.
Preferably, the metal nanoparticles are one or more of platinum, palladium and nickel; the particle size of the metal nano particles is less than or equal to 20nm; the metal nano-ions can break chemical bonds of ammonia molecules to form active hydrogen atoms, so that the reaction between hydrogen and metal oxide is catalyzed, and the metal oxide is reduced into a metal simple substance or a low-valence metal oxide which has color difference from the original metal oxide.
The preparation method of the color-changing adhesive tape for ammonia gas leakage detection comprises the following steps:
weighing the components according to the formula, and then placing the components in a kneading machine for mixing to obtain a mixture; and then preparing the mixture into a strip-shaped sheet, attaching lining paper to the strip-shaped sheet to prepare a semi-finished adhesive tape roll or a semi-finished adhesive tape strip, and standing at room temperature to obtain the color-changing adhesive tape for ammonia gas leakage detection.
Preferably, the lining paper is one of a polypropylene film and a PET film.
Preferably, the width of the color-changing adhesive tape for detecting ammonia gas leakage is 1-20cm, and the thickness is 0.2-2mm.
The adhesive tape adopts 107 silicone rubber, a reinforcing agent, a cross-linking agent and a catalyst as raw materials, can realize normal-temperature curing of the adhesive tape, can well retain the original appearance of metal oxide ions without heating, and achieves a good color-changing effect.
The use method of the color-changing adhesive tape for ammonia gas leakage detection comprises the following steps: and (4) tearing off the lining paper, and winding and bonding the lining paper on a storage container, a pipeline or equipment to be detected.
Compared with the prior art, the invention has the following beneficial effects: the color-changing adhesive tape provided by the invention is simple and direct in ammonia gas detection, can quickly perform color-changing early warning, is high in sensitivity and wide in application range, and can be widely applied to ammonia gas storage containers, pipelines and equipment; when the color-changing adhesive tape is used, the color-changing adhesive tape is only required to be adhered and wound on a part where ammonia gas leakage is easy to occur, the operation is simple, the ammonia gas leakage part can be accurately displayed through the color change of the adhesive tape after ammonia gas is adsorbed, the ammonia gas leakage part detection capability is higher, the hidden danger of ammonia gas leakage can be timely discovered, and the ammonia gas leakage can be prevented from happening in the bud; according to the invention, the raw material liquid 107 silicone rubber is modified, so that higher functionality can be generated in the curing process of the adhesive tape, more crosslinking points are generated, stronger limitation is formed on molecular chains, the crosslinking depth of the adhesive tape is deepened, the mechanical property of the adhesive tape is improved due to a complex and compact crosslinking structure, and the liquid 107 silicone rubber molecules have more crosslinking points by introducing a plurality of active group carboxyl groups on modifier molecules, so that the adhesive tape can inhibit colloid flow and accelerate curing, thereby shortening the surface drying time and further improving the bonding effect of the adhesive tape.
Detailed Description
For the sake of avoiding redundant description, the articles used in the following examples are all commercially available products unless otherwise specified, and the methods used are all conventional methods unless otherwise specified.
The sources of part of raw materials used by the invention are as follows:
97% of nano calcium carbonate, 80nm of particle size and 92% of whiteness, shijiazhuang Leitai science and technology Co.
Methyl tributyl ketoxime silane with content of 99% and density of 0.982g/cm 3 Guangzhou far from new materials, inc.
Tungsten oxide with particle size of 40nm, purity of 99.9%, and specific surface area of 74m 2 G, density 7.16g/cm 3 Nangong, plain alloy materials, inc.
Nanometer palladium powder with particle diameter of 50nm, melting point of 1554, mohs hardness at 4.75 deg.C, and density of 12.023g/cm 3 Beijing Zhongkoku science and technology Co., ltd.
99% of methallyl alcohol, having a density of 0.829g/cm 3 The boiling point is 116.3, DEG C, hubei Kowadd chemical Co., ltd.
Hexachlorocyclotriphosphazene with purity of 99%, melting point of 112-115, specific gravity at 1.98, and is available from general Biotech of Wuhan Hua.
Dithiodibenzoic acid, 99% in content, melting point 287-290, C Wuhan Carnoz Tech Ltd.
Benzoin dimethyl ether with purity of 99% and density of 1.2g/cm 3 The melting point is 67-70, and the temperature is manufactured by the company of Art health chemical (Hubei).
107 silicone rubber, viscosity of 20000cs, surface vulcanization time of 2h, shandong Jinnaite environmental protection science and technology Limited.
Example 1
A preparation method of a color-changing adhesive tape for ammonia gas leakage detection comprises the following steps:
100g of 107 silicon rubber, 40g of nano calcium carbonate, 8g of methyltributanone oxime silane, 1g of dibutyltin dilaurate, 0.2g of 2-cyano-3, 3-diphenyl-2-acrylic acid-2-ethylhexyl ester, 3g of tungsten oxide and 0.5g of nano palladium powder are placed in a kneader and mixed to obtain a mixture; and then preparing the mixture into a strip-shaped sheet, attaching a polypropylene film to the strip-shaped sheet to prepare a semi-finished adhesive tape, and standing at room temperature for 6 hours to obtain the color-changing adhesive tape for ammonia gas leakage detection.
The 107 silicone rubber is modified 107 silicone rubber, and the preparation method comprises the following steps:
100g of 107 silicon rubber, 3g of modifier and 250mL of 30wt% sodium methoxide methanol solution are stirred and mixed uniformly, then the mixture is heated to 50 ℃, 7.8g of 3-aminopropyltrimethoxysilane is added at the temperature, the mixture is stirred for 30min at the speed of 2200rpm, 5.6g of n-octylamine is added, and the mixture is stirred for 10min, so that the modified 107 silicon rubber is obtained.
The preparation method of the modifier comprises the following steps:
1) Dissolving 40g of methallyl alcohol in 800mL of tetrahydrofuran at 5 ℃, adding 22.5g of metallic sodium, stirring at room temperature for reaction for 12 hours, heating to 60 ℃, and continuing to react for 12 hours to obtain a sodium alkoxide solution;
2) Dissolving 45g of hexachlorocyclotriphosphazene in 280mL of tetrahydrofuran to obtain a tetrahydrofuran solution of hexachlorocyclotriphosphazene, then dropwise adding the tetrahydrofuran solution of hexachlorocyclotriphosphazene into a sodium alkoxide solution at the speed of 2 drops/second, and reacting for 48 hours at 70 ℃; after the reaction is finished, cooling to room temperature, concentrating under reduced pressure to 30% of the original volume, and adding 80mL of 50wt% ethanol water solution into the residue; stirring for 20min, filtering, collecting precipitate, washing the precipitate with water and anhydrous ethanol for 3 times, respectively, and drying at 60 deg.C for 8 hr, and marking as M 1 ；
3) 4.5g of dithiodibenzoic acid, 10.8g of M described in step 2) 1 Mixing 7.8g benzoin dimethyl ether and 150mL tetrahydrofuran, stirring, irradiating with 365nm ultraviolet light at room temperature for 10min after the raw materials are completely dissolved, adding 60mL 50wt% ethanol water solution for precipitation, filtering after 30min, collecting precipitate, washing the precipitate with water and absolute ethanol respectivelyAnd drying for 8 hours at 60 ℃ after 3 times to obtain the modifier.
Example 2
A preparation method of a color-changing adhesive tape for ammonia gas leakage detection comprises the following steps:
placing 100g of 107 silicon rubber, 40g of nano calcium carbonate, 8g of methyl tributyl ketoxime silane, 1g of dibutyltin dilaurate, 0.2g of 2-cyano-3, 3-diphenyl-2-acrylic acid-2-ethylhexyl ester, 3g of tungsten oxide and 0.5g of nano palladium powder in a kneader for mixing to obtain a mixture; and then preparing the mixture into a strip-shaped sheet, attaching a polypropylene film to the strip-shaped sheet to prepare a semi-finished adhesive tape, and standing at room temperature for 6 hours to obtain the color-changing adhesive tape for ammonia gas leakage detection.
The 107 silicone rubber is modified 107 silicone rubber, and the preparation method comprises the following steps:
100g of 107 silicon rubber, 3g of modifier and 250mL of 30wt% sodium methoxide methanol solution are stirred and mixed uniformly, then the mixture is heated to 50 ℃, 7.8g of 3-aminopropyltrimethoxysilane is added at the temperature, the mixture is stirred for 30min at the speed of 2200rpm, 5.6g of n-octylamine is added, and the mixture is stirred for 10min, so that the modified 107 silicon rubber is obtained.
The preparation method of the modifier comprises the following steps:
1) Dissolving 40g of methallyl alcohol in 800mL of tetrahydrofuran at 5 ℃, adding 22.5g of metal sodium, stirring at room temperature for reaction for 12 hours, heating to 60 ℃, and continuing to react at the temperature for 12 hours to obtain a sodium alkoxide solution;
2) Dissolving 45g of hexachlorocyclotriphosphazene in 280mL of tetrahydrofuran to obtain a tetrahydrofuran solution of hexachlorocyclotriphosphazene, then dropwise adding the tetrahydrofuran solution of hexachlorocyclotriphosphazene into a sodium alkoxide solution at the speed of 2 drops/second, and reacting for 48 hours at 70 ℃; after the reaction is finished, cooling to room temperature, concentrating under reduced pressure to 30% of the original volume, and adding 80mL of 50wt% ethanol water solution into the residue; stirring for 20min, filtering, collecting precipitate, washing the precipitate with water and absolute ethyl alcohol for 3 times respectively, and drying at 60 ℃ for 8h to obtain the modifier.
Comparative example 1
A preparation method of a color-changing adhesive tape for ammonia gas leakage detection comprises the following steps:
placing 100g of 107 silicon rubber, 40g of nano calcium carbonate, 8g of methyl tributyl ketoxime silane, 1g of dibutyltin dilaurate, 0.2g of 2-cyano-3, 3-diphenyl-2-acrylic acid-2-ethylhexyl ester, 3g of tungsten oxide and 0.5g of nano palladium powder in a kneader for mixing to obtain a mixture; and then preparing the mixture into a strip-shaped sheet, attaching a polypropylene film to the strip-shaped sheet to prepare a semi-finished adhesive tape, and standing the semi-finished adhesive tape at room temperature for 6 hours to obtain the color-changing adhesive tape for ammonia gas leakage detection.
The 107 silicone rubber is modified 107 silicone rubber, and the preparation method comprises the following steps:
100g of 107 silicone rubber, 3g of modifier and 250mL of a methanol solution of 30wt% sodium methoxide are stirred and mixed uniformly, then the mixture is heated to 50 ℃, 7.8g of 3-aminopropyltrimethoxysilane is added at the temperature, the mixture is stirred for 30min at the speed of 2200rpm, 5.6g of n-octylamine is added, and the mixture is stirred for 10min, so that the modified 107 silicone rubber is obtained.
The preparation method of the modifier comprises the following steps:
mixing and stirring 4.5g of dithiodibenzoic acid, 10.8g of hexachlorocyclotriphosphazene, 7.8g of benzoin dimethyl ether and 150mL of tetrahydrofuran, after the raw materials are completely dissolved, irradiating for 10min by using ultraviolet light with the wavelength of 365nm at normal temperature, adding 60mL of 50wt% ethanol water solution for precipitation, filtering after 30min, collecting precipitate, washing the precipitate for 3 times by using water and absolute ethyl alcohol respectively, and drying for 8h at 60 ℃ to obtain the modifier.
Comparative example 2
A preparation method of a color-changing adhesive tape for ammonia gas leakage detection comprises the following steps:
100g of 107 silicon rubber, 40g of nano calcium carbonate, 8g of methyltributanone oxime silane, 1g of dibutyltin dilaurate, 0.2g of 2-cyano-3, 3-diphenyl-2-acrylic acid-2-ethylhexyl ester, 3g of tungsten oxide and 0.5g of nano palladium powder are placed in a kneader and mixed to obtain a mixture; and then preparing the mixture into a strip-shaped sheet, attaching a polypropylene film to the strip-shaped sheet to prepare a semi-finished adhesive tape, and standing the semi-finished adhesive tape at room temperature for 6 hours to obtain the color-changing adhesive tape for ammonia gas leakage detection.
The 107 silicone rubber is modified 107 silicone rubber, and the preparation method comprises the following steps:
the modified 107 silicone rubber is prepared by uniformly mixing 100g of 107 silicone rubber and 250mL of a methanol solution of 30wt% sodium methoxide, heating to 50 ℃, adding 7.8g of 3-aminopropyltrimethoxysilane, stirring for 30min at 2200rpm, adding 5.6g of n-octylamine, and stirring for 10 min.
Comparative example 3
A preparation method of a color-changing adhesive tape for ammonia gas leakage detection comprises the following steps:
100g of 107 silicon rubber, 40g of nano calcium carbonate, 8g of methyltributanone oxime silane, 1g of dibutyltin dilaurate, 0.2g of 2-cyano-3, 3-diphenyl-2-acrylic acid-2-ethylhexyl ester, 3g of tungsten oxide and 0.5g of nano palladium powder are placed in a kneader and mixed to obtain a mixture; and then preparing the mixture into a strip-shaped sheet, attaching a polypropylene film to the strip-shaped sheet to prepare a semi-finished adhesive tape, and standing the semi-finished adhesive tape at room temperature for 6 hours to obtain the color-changing adhesive tape for ammonia gas leakage detection.
Test example 1
Testing the mechanical property of the color-changing adhesive tape: the color-changing adhesive tapes for ammonia gas leakage detection obtained in examples 1-2 and comparative examples 1-3 were peeled from the polypropylene films according to GB/T13477.8-2017 part 8 of test method for building sealing materials: measurement of tensile adhesion Property "measurement of tensile adhesion Property and elongation at break was carried out at a speed of 6mm/min; the test results are shown in table 1:
table 1 mechanical property test results of the color-changeable adhesive tape
Figure BDA0003846641930000121
As can be seen from the experimental results in Table 1, the discoloration adhesive tape for ammonia gas leakage detection prepared in example 1 has the best mechanical properties, and example 1 is different from other examples in that dithiodibenzoic acid and M are added 1 The modifier generated by the reaction of benzoin dimethyl ether can be probably caused by introducing a plurality of active group carboxyl groups on the molecules of the modifier, so that liquid 107 silicon rubber molecules can have more crosslinking points, and a more complex and compact crosslinking structure can be generated under the action of the crosslinking agent, thereby inhibiting the colloid flow and accelerating the solidificationThe bonding effect is improved.
Test example 2
Testing the ammonia gas sensitivity of the color-changing adhesive tape: the color-changing adhesive tape for ammonia gas leakage detection obtained in the embodiment 1 is wound outside a prepared pipeline leakage point after a polypropylene film is removed, the adhesive tape is fixed by utilizing the self-adhesion property of the adhesive tape, a mixed gas consisting of 3% ammonia gas and 97% nitrogen gas in volume fraction is passed through a pipeline with the leakage point at the speed of 1L/min, the color of the leakage point wrapped by the adhesive tape is changed into light brown after 8 minutes, and the color is gradually changed into dark brown along with the prolonging of time. The color-changing adhesive tape prepared by the invention is free from abnormity caused by uneven tension force, and the testing accuracy is high.

Claims (8)

1. The color-changing adhesive tape for ammonia gas leakage detection is characterized by comprising the following components: 107 silicon rubber, a reinforcing agent, a cross-linking catalyst, a metal oxide and metal nano particles;
the 107 silicone rubber is modified 107 silicone rubber, and the preparation method comprises the following steps:
uniformly stirring and mixing 60-100g of 107 silicon rubber, 2-3g of modifier and 200-300mL of 20-40wt% of methanol solution of sodium methoxide, heating to 40-60 ℃, adding 5-10g of 3-aminopropyltrimethoxysilane, stirring for 30-50min at 2000-3000rpm, adding 4-7g of n-octylamine, and stirring for 10-15min to obtain modified 107 silicon rubber;
the preparation method of the modifier comprises the following steps:
1) Dissolving 30-50g of methallyl alcohol in 500-1000mL of tetrahydrofuran at 0-5 ℃, adding 20-25g of metal sodium, stirring and reacting at room temperature for 10-12h, heating to 60-70 ℃, and continuing to react for 10-12h to obtain a sodium alkoxide solution;
2) Dissolving 40-60g of hexachlorocyclotriphosphazene in 200-300mL of tetrahydrofuran to obtain tetrahydrofuran solution of hexachlorocyclotriphosphazene, then dropwise adding the tetrahydrofuran solution of hexachlorocyclotriphosphazene into sodium alkoxide solution at the speed of 1-2 drops/second, and reacting for 40-48h at 60-70 ℃; after the reaction is finished, cooling to room temperature, concentrating under reduced pressure to 20-30% of the original volume, and adding 60-100mL of 50-70wt% ethanol water solution into the residue; stirring for 20-30min, filtering, collecting precipitate, washing the precipitate with water and anhydrous ethanol for 2-3 times, and drying at 50-60 deg.C for 6-8 hr to obtain the modifier.
2. A colour-changing tape for ammonia gas leakage detection according to claim 1, characterised in that it comprises the following components in parts by weight: 80-120 parts of 107 silicon rubber, 20-50 parts of reinforcing agent, 5-10 parts of cross-linking agent, 0.5-1.5 parts of cross-linking catalyst, 0.1-0.3 part of anti-aging agent, 1-5 parts of metal oxide and 0.01-1 part of metal nano-particles.
3. A color-changing adhesive tape for ammonia gas leak detection according to claim 1 or 2, characterized in that: also comprises dyes, preservatives, mildewcides and flame retardants commonly used in the field.
4. A color-changing adhesive tape for ammonia gas leakage detection according to claim 1, wherein the preparation method of the modifier comprises the following steps:
1) Dissolving 30-50g of methallyl alcohol in 500-1000mL of tetrahydrofuran at 0-5 ℃, adding 20-25g of metallic sodium, stirring and reacting at room temperature for 10-12h, heating to 60-70 ℃, and continuing to react for 10-12h to obtain a sodium alkoxide solution;
2) Dissolving 40-60g of hexachlorocyclotriphosphazene in 200-300mL of tetrahydrofuran to obtain tetrahydrofuran solution of hexachlorocyclotriphosphazene, then dropwise adding the tetrahydrofuran solution of hexachlorocyclotriphosphazene into sodium alkoxide solution at the speed of 1-2 drops/second, and reacting for 40-48h at 60-70 ℃; after the reaction is finished, cooling to room temperature, concentrating under reduced pressure to 20-30% of the original volume, and adding 60-100mL of 50-70wt% ethanol water solution into the residue; stirring for 20-30min, filtering, collecting precipitate, washing the precipitate with water and anhydrous ethanol for 2-3 times, drying at 50-60 deg.C for 6-8 hr, and marking as M1;
3) Mixing and stirring 3-6g of dithiodibenzoic acid, 8-15g of M1 described in the step 2), 6-10g of benzoin dimethyl ether and 100-200mL of tetrahydrofuran, after the raw materials are completely dissolved, irradiating for 10-15min by using ultraviolet light at normal temperature, adding 50-100mL of 50-75wt% ethanol aqueous solution for precipitation, filtering after 30-50min, collecting precipitates, washing the precipitates for 2-3 times by using water and absolute ethyl alcohol respectively, and drying for 6-8h at 50-60 ℃ to obtain the modifier.
5. A colour-changing tape for ammonia gas leak detection as defined in claim 1 or 2, wherein: the reinforcing agent is one or the mixture of two or more of nano calcium carbonate, white carbon black, quartz powder, titanium dioxide, kaolin, carbon black and carbon nano tubes.
6. A color-changing adhesive tape for ammonia gas leak detection according to claim 1 or 2, characterized in that: the cross-linking agent is one or more of methyl tributyrinoxime silane, vinyl tributyrinoxime silane, methyl trimethoxy silane, ethyl trimethoxy silane and methyl triacetoxy silane.
7. A colour-changing tape for ammonia gas leak detection as defined in claim 1 or 2, wherein: the crosslinking catalyst is one or the mixture of more than two of dibutyltin dilaurate, dihexyltin dilaurate, dibutyltin diacetate, dihexyltin diacetate, isopropyl titanate and butyl titanate.
8. A method of preparing a colour-changing adhesive tape for ammonia gas leak detection as defined in any one of claims 1 to 7, comprising the steps of: weighing the components, placing the components in a kneading machine, and mixing to obtain a mixture; and then preparing the mixture into a strip-shaped sheet, attaching lining paper to the strip-shaped sheet to prepare a semi-finished adhesive tape roll or a semi-finished adhesive tape strip, and standing at room temperature to obtain the color-changing adhesive tape for ammonia gas leakage detection.
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