Non-combustible fluorescent penetrant flaw detection agent composition and preparation method thereof

Abstract

The invention relates to the technical field of nondestructive testing, and discloses a non-combustible fluorescent penetrant flaw detection agent composition which comprises the following components in parts by weight: 8-10 parts of a solvent system; 0.1 to 0.2 part of a tetramethyl benzidine derivative; 0.1 to 0.2 part of polyoxyethylene octyl phenyl ether; the invention also provides a preparation method of the non-combustible fluorescent penetrant flaw detection agent composition, and the preparation method comprises the following steps: mixing the solvent matrix to form a solvent system; adding a fluorescent dye, wherein the fluorescent dye is dispersed in a solvent system; the surfactant is introduced to regulate the wettability of the composition; integration of the additive system is used to enhance thermal stability and dispersion stability. According to the invention, the solvent matrix ratio is optimized, and the thermal stability reinforcing agent and the dispersing agent are introduced to achieve a synergistic effect, so that the stability of the flaw detection agent in a high-temperature environment, the fluorescence signal uniformity of crack detection and the long-term storage performance are improved.

Description

Technical Field

[0001] The invention relates to the technical field of nondestructive testing, in particular to a non-flammable fluorescent penetrant flaw detection agent composition and a preparation method thereof. Background Art

[0002] In industrial production and maintenance, surface crack detection of metal components is a vital task, especially in high-risk fields such as aerospace, petrochemicals, etc. The accuracy of crack detection is directly related to the safety and service life of the equipment. As a non-destructive testing technology, fluorescent penetrant testing is widely used in the detection of microcracks and surface defects due to its high sensitivity and intuitive display effect.

[0003] In the existing technology, the research and development of fluorescent penetrant flaw detection agents has made some progress, mainly focusing on the selection of solvents and dyes. Some technologies improve the permeability of flaw detection agents by optimizing the ratio of organic solvents, enabling them to quickly enter microcracks and complete the appearance of surface defects. At the same time, some studies have used high-efficiency fluorescent dyes that can produce strong fluorescent signals under ultraviolet light, which is convenient for crack detection. These flaw detection agents are suitable for crack detection under normal working conditions, showing high sensitivity and ease of operation, and have been widely used.

[0004] However, the existing technology shows obvious deficiencies in high temperature environment, long-term storage and complex crack detection; first, traditional flaw detection agents mostly use volatile organic solvents, which suffer serious solvent loss under high temperature conditions and insufficient crack filling, resulting in unstable detection effect; secondly, the dispersion and light stability of fluorescent dyes are poor, making the signal susceptible to ultraviolet light irradiation and rapidly attenuating, and the inside of the crack displays unevenness; in addition, during long-term storage, the flaw detection agent is prone to stratification or precipitation, resulting in performance degradation. Summary of the invention

[0005] In view of the deficiencies of the prior art, the present invention provides a non-flammable fluorescent penetrant flaw detector composition and a preparation method thereof, which solves the problems of severe solvent volatilization and insufficient crack filling of fluorescent penetrant flaw detectors in the prior art under high temperature conditions.

[0006] To achieve the above object, the present invention is implemented by the following technical scheme: a non-flammable fluorescent penetrant flaw detection agent composition, the composition comprising the following components in parts by weight: Solvent system: 8-10 parts; Fluorescent dye: 0.1-0.2 parts; Tetramethylbenzidine derivatives have strong fluorescence emission capabilities and can produce high-intensity fluorescence signals under ultraviolet light excitation. Through nano-encapsulation technology, the dye molecules are protected inside the nanoparticles, avoiding light attenuation caused by long-term ultraviolet light exposure. At the same time, the high specific surface area of ​​the coated particles helps the fluorescent dye to be distributed on the surface and deep inside the cracks, enhancing the light reflection and fluorescence signal intensity inside the cracks; Polyoxyethylene octylphenyl ether: 0.1-0.2 parts; As a nonionic surfactant, polyoxyethylene octyl phenyl ether is used to reduce the interfacial tension of the penetrant and enhance the wettability of the liquid on the crack surface. At the same time, the balanced design of the hydrophilic and hydrophobic chains of polyoxyethylene octyl phenyl ether enables it to be stably distributed on the complex fractal surface of the crack, ensuring the continuity and uniformity of the liquid flow inside the crack. Additive system: 1-1.5 parts.

[0007] Preferably, the solvent system comprises: Diethylene glycol: 4-5 parts; Diethylene glycol is a small molecule solvent with low volatility. Its main function in the present invention is to reduce the overall viscosity of the solvent system and improve the diffusion performance of the penetrant. As one of the main components, diethylene glycol works synergistically with other solvents to form a matrix with excellent diffusivity and permeability. Polyethylene glycol ether: 4-5 parts; The high molecular weight of polyethylene glycol ether determines its adhesion ability on the crack wall. Through van der Waals forces and hydrogen bonding, it can delay the loss of solvent molecules. This retention effect not only ensures the full infiltration of the penetrant into the crack, but also improves the distribution stability of the fluorescent dye. In addition, the polymer chain structure of polyethylene glycol ether further enhances the filling capacity of the penetrant by occupying more effective volume in the crack. Functional solvent diethanolamine: 0.1-0.5 parts; Diethanolamine optimizes the interaction between the solvent system and the crack wall by forming hydrogen bonds and weak polar intermolecular forces.

[0008] Preferably, the additive system comprises: Thermal stability enhancer silica aerogel: 0.5-0.8 parts; The porous structure of silica aerogel temporarily captures solvent molecules through physical adsorption and gradually releases them under high temperature conditions, which plays a role in regulating the solvent evaporation rate; Dispersant block copolymer: 0.5-0.7 parts; The block copolymer forms hydrogen bonds with the solvent system through its hydrophilic end, increasing the dispersion stability of aerogel particles and fluorescent dyes in the liquid phase, while the hydrophobic end interacts with the weak polar regions on the surface of aerogel and fluorescent dyes to form a stable adsorption layer, inhibiting particle agglomeration.

[0009] The present invention also provides a method for preparing a non-flammable fluorescent penetrant flaw detection agent composition, comprising the following steps: mixing of solvent matrices to form a solvent system; The small molecular characteristics of diethylene glycol reduce the viscosity η of the system, increase the diffusion coefficient D, and contribute to the permeability of the solvent system; polyethylene glycol ether provides stronger intermolecular forces and high viscosity through its long-chain molecules, prolonging the residence time of the solvent in the crack; diethanolamine enhances the affinity between the solvent and the crack surface through polarity and improves the wettability of the solvent; The addition of fluorescent dye is used to disperse the fluorescent dye in the solvent system; The stability and dispersion performance of tetramethylbenzidine derivatives are improved through nano-encapsulation technology; the cavitation effect of ultrasonic dispersion destroys the aggregation state between dye molecules, further improving its dispersion uniformity; The introduction of surfactants is used to adjust the wetting properties of the composition; The addition of surfactant effectively reduces the discontinuity of liquid on the crack surface, ensuring uniform distribution and deep penetration of the penetrant; Integration of additive systems to enhance thermal and dispersion stability; The porous structure of silica aerogel reduces the volatilization rate of the solvent through adsorption and slow release, maintaining the stability of the composition under high temperature conditions; the block copolymer interacts with the solvent molecules and the surface of the nanoparticles through its hydrophilic and hydrophobic segments, respectively, to form a stable adsorption layer to prevent aerogel particles from agglomerating; Cooling and filtering, for cooling the composition to room temperature and removing impurities; The filtration process ensures that all particles in the composition have uniform particle sizes, eliminates large particle impurities that may affect the permeability, and forms a physically stable dispersion system after cooling, avoiding the precipitation or precipitation of components caused by temperature changes during storage; filling and sealing are used to complete the final preparation of the composition; Sealed storage conditions limit the volatilization of solvents and the degradation of fluorescent dyes, ensuring stable performance of the product during long-term storage. Through low-temperature storage and light-proof conditions, the degradation of polymer components and dyes due to photothermal oxidation is reduced.

[0010] Preferably, the solvent matrix mixture comprises: Mix diethylene glycol and polyethylene glycol ether in a weight ratio of 4-5; Stir at 300-500 rpm at 50-70°C; Stirring at 50-70°C can reduce the viscosity of the polyethylene glycol ether, making it more fully miscible with diethylene glycol. Too low a temperature may result in uneven mixing, while too high a temperature may cause the volatilization of the solvent components; Add functional solvent diethanolamine at a weight ratio of 0.1-0.5 and continue stirring for 15-30 minutes; The stirring speed is controlled within the range of 300-500rpm to form a uniform shear force field, avoid the mixing of bubbles due to excessive speed, and ensure the uniformity and stability of the solvent system.

[0011] Preferably, the addition of the fluorescent dye comprises: Rhodamine B or tetramethylbenzidine derivatives were selected as fluorescent dyes; Rhodamine B and tetramethylbenzidine derivatives have a wide UV absorption range and high quantum yield, ensuring the formation of strong fluorescent reflection signals in cracks, which helps to improve the sensitivity of defect detection. The aromatic rings and substituents in the molecular structure of these dyes enhance their solubility in the solvent matrix and avoid precipitation or stratification problems; at the same time, their high temperature resistance and UV resistance reduce the risk of light attenuation during crack detection. Add the fluorescent dye to the solvent matrix at a weight ratio of 0.1-0.2; The weight ratio of the fluorescent dye is controlled at 0.1-0.2, which can ensure the saturated distribution state in the solvent matrix and avoid the oversaturated precipitation phenomenon caused by excessive dye; Stir at 40-60°C for 30-60 minutes; This temperature range can reduce the viscosity of the solvent matrix and increase the solubility of the dye; and this stirring time can ensure the uniform distribution of the fluorescent dye molecules in the matrix and form a stable dissolved state to avoid precipitation during subsequent storage; The mixture was treated with ultrasonic dispersion equipment for 5-10 minutes at a frequency of 20-25 kHz; Ultrasonic dispersion equipment generates tiny bubbles in liquid through cavitation effect. The formation and rupture of these bubbles will cause local high pressure and high temperature environment, thereby breaking the aggregation state between dye molecules and further dispersing dye particles; frequency control in the range of 20-25kHz can achieve a balance between efficiency and safety. Low frequency may not effectively disperse dyes, while high frequency may cause degradation of solvent matrix or destruction of dye molecules.

[0012] Preferably, the introduction of the surfactant comprises: Adding nonionic surfactant polyoxyethylene octyl phenyl ether; Polyoxyethylene octylphenyl ether has a unique molecular structure, consisting of hydrophilic polyoxyethylene segments and hydrophobic octylphenyl segments. The hydrophilic end interacts with the aqueous solvent through hydrogen bonds, while the hydrophobic end adsorbs on the crack wall or the surface of the non-polar component through hydrophobic interaction; The weight ratio of surfactant is 0.1-0.2; The weight ratio of surfactant is 0.1-0.2, which can ensure good wetting performance while avoiding the generation of foam or abnormal increase in system viscosity caused by excessive concentration; Mix at a stirring speed of 400-600 rpm for 15-20 minutes; This stirring speed can provide sufficient shear force to promote the dispersion of the surfactant in the solvent, while avoiding solvent foaming or dye molecule agglomeration caused by too high a speed. This mixing time is sufficient to complete the dispersion process of the surfactant, while avoiding increased energy consumption or overheating and volatilization of the solvent caused by long-term stirring.

[0013] Preferably, the integration of the additive system includes: Adding thermal stability enhancer silica aerogel, the weight ratio is 0.5-0.8; Silica aerogel has a high specific surface area and a porous network structure. These properties enable it to adsorb solvent molecules and form a dynamic slow-release mechanism, thereby effectively reducing the volatilization rate of the solvent. In a high-temperature environment, the microporous structure of silica aerogel restrains the movement of solvent molecules, inhibits the large-scale volatilization of the solvent, and ensures the stability of the flaw detection agent under extreme conditions. Add dispersant block copolymer at a weight ratio of 0.5-0.7; The block copolymer is composed of hydrophilic and hydrophobic segments. The hydrophilic segments are bound to the solvent molecules through hydrogen bonds, while the hydrophobic segments are adsorbed on the aerogel surface to form a stable adsorption layer to prevent aerogel particles from agglomerating. The block copolymer reduces the interfacial energy γ between the aerogel particles and the solvent. sl , reduce the driving force for particle agglomeration and ensure uniform distribution of the additive system; Stir at 60-70°C for 30-60 minutes; Stirring at 60-70°C can reduce the viscosity of the solvent matrix, enhance the interaction between the additive and the solvent, and promote the uniform dispersion of the aerogel and the block copolymer. This stirring time is conducive to the formation and collapse of cavitation bubbles, generating local high pressure and high temperature in the liquid. The components are evenly distributed by combining mechanical dispersion with ultrasonic dispersion. This process can break the aggregation of aerogel particles and further disperse the fluorescent dye and dispersant molecules.

[0014] Preferably, the cooling and filtering include: Cool the mixture to 20-25°C; This cooling temperature can effectively reduce the vapor pressure of the solvent and avoid the rapid volatilization of the solvent under high temperature conditions, thereby maintaining the effective concentration of the flaw detection agent; Filter through a microporous membrane with a pore size of 0.2-0.5 μm; This pore size design can intercept tiny particles that may affect crack penetration, while ensuring a balance between filtration efficiency and flow rate. Too small a pore size may cause blockage, while too large a pore size may leak unstable particles; Filter out large particle impurities to ensure the uniformity of the final composition; After filtration, only evenly dispersed micron or nanometer particles are retained in the solution. These particles are stably distributed in the solvent system, which can effectively avoid inconsistent performance due to local concentration differences. Removing large particle impurities can prevent the detection agent from clogging inside the crack and improve the fluidity and penetration depth of the solvent system.

[0015] Preferably, the filling and sealing comprises: Place the cooled and filtered mixture into airtight containers; Sealed containers can effectively isolate the outside air, prevent the volatilization of solvent components, and ensure that the flaw detection agent maintains the stability of the active ingredients during storage; for compositions containing volatile components (such as diethylene glycol and polyethylene glycol ether), sealing can significantly reduce volatilization losses and extend their service life; Store at 5-25℃, avoid direct sunlight and high humidity; Storing within this temperature range can reduce the chemical reaction rate of the solvent matrix and avoid component degradation or solvent volatilization caused by high temperature environment. Temperature control can also prevent the fluorescence intensity of fluorescent dyes from decreasing due to thermal oxidation, thereby maintaining their detection performance.

[0016] The present invention provides a non-flammable fluorescent penetrant flaw detection agent composition and a preparation method thereof. It has the following beneficial effects: 1. The present invention optimizes the design of the solvent matrix, adopts the synergistic effect of diethylene glycol and polyethylene glycol ether, and combines the functional improvement of diethanolamine to enhance the diffusion ability and wetting performance of the penetrant flaw detection agent. Compared with the solution of using a single solvent in the prior art that leads to insufficient penetration depth, the present invention effectively solves the problem of uneven distribution of penetrants in crack detection and achieves higher-precision microcrack detection.

[0017] 2. The present invention introduces silica aerogel as a thermal stability enhancer and combines it with the dynamic dispersion performance of the dispersant block copolymer to construct a flaw detection agent system that can work stably in a high-temperature environment. Compared with the shortcomings of the prior art that the solvent volatilizes severely under high temperature conditions and the flaw detection agent performance decays rapidly, the present invention still maintains stable performance under conditions as high as 150°C, thereby expanding the scope of application.

[0018] 3. The present invention adopts rhodamine B or tetramethylbenzidine derivatives as fluorescent dyes, and realizes their uniform distribution in the solvent matrix through ultrasonic dispersion technology, thereby improving the intensity and stability of the fluorescent signal. The problem of discontinuous detection signal or decreased intensity due to uneven dispersion of fluorescent dyes or significant light attenuation in the prior art is effectively solved in the present invention, providing a guarantee for high-sensitivity crack detection.

[0019] 4. The present invention effectively prevents performance degradation caused by solvent volatilization, dye photochemical degradation and humidity through filling and sealing processes combined with a low-temperature storage environment. Compared with the prior art in which the flaw detection agent is prone to stratification or performance degradation during storage, the present invention achieves long-term stable performance maintenance and improves the reliability and applicability of the product. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 The figure is a flow chart of the method of the present invention. DETAILED DESCRIPTION

[0021] The following will be combined with the drawings in the specification of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0022] Please see attached Figure 1 : Example 1: Preparation of high permeability flaw detection agent for microcrack detection Raw material preparation Weigh diethylene glycol (4 parts), polyethylene glycol ether (molecular weight 500, 5 parts), and diethanolamine (0.3 parts) for use.

[0023] Rhodamine B fluorescent dye (0.2 parts) and surfactant polyoxyethylene octylphenyl ether (0.15 parts) were prepared.

[0024] Thermal stability enhancer silica aerogel (0.6 parts), dispersant block copolymer (0.5 parts).

[0025] Solvent Matrix Mixing Add diethylene glycol and polyethylene glycol ether into the reaction kettle, control the temperature at 55°C, set the stirring speed at 400 rpm, and mix for 20 minutes.

[0026] Slowly add diethanolamine and continue stirring for 15 minutes to ensure a uniform solvent system.

[0027] Fluorescent dye dispersion Add Rhodamine B to the mixture, maintain 50°C, and stir for 30 minutes.

[0028] Ultrasonic dispersion equipment was used for 5 min at a frequency of 20 kHz to further ensure uniform distribution of the fluorescent dye.

[0029] Additive Integration Silica aerogel and block copolymer were added, and the temperature of the mixture was raised to 60° C. The stirring speed was increased to 500 rpm and mixed for 40 minutes.

[0030] At the same time, ultrasonic dispersion (25kHz) was used for 8 minutes to ensure that the additives were evenly distributed without agglomeration.

[0031] Cooling and filtration The mixed solution was naturally cooled to 22°C and filtered through a microporous filter membrane with a pore size of 0.3 μm to remove undispersed particle impurities.

[0032] Filling and sealing The filtered flaw detection agent is placed in a clean sealed container and stored at low temperature (10°C) away from light.

[0033] Example 2: Preparation of flaw detection agent suitable for high temperature working conditions Raw material preparation Weigh diethylene glycol (5 parts), polyethylene glycol ether (molecular weight 600, 4 parts), and diethanolamine (0.2 parts).

[0034] A tetramethylbenzidine derivative (0.15 parts) and a surfactant polyoxyethylene octylphenyl ether (0.2 parts) were prepared.

[0035] Thermal stability enhancer silica aerogel (0.8 parts), dispersant block copolymer (0.7 parts).

[0036] Solvent Matrix Mixing Diethylene glycol and polyethylene glycol ether were added into a mixing kettle at a ratio of 5:4, the temperature was controlled at 60°C, the stirring speed was 500 rpm, and mixing was performed for 25 minutes.

[0037] Diethanolamine was added and mixing was continued for 20 minutes, maintaining temperature and stirring speed.

[0038] Fluorescent dye dispersion The tetramethylbenzidine derivative was added to the solvent base, the temperature was lowered to 50°C, and stirred for 40 minutes.

[0039] Ultrasonic dispersion equipment was used with a frequency of 25 kHz for 6 minutes to ensure uniform distribution of the fluorescent dye particles.

[0040] Additive Integration Silica aerogel and block copolymer were added sequentially, the mixing temperature was set at 65°C, the stirring speed was 550 rpm, and the mixing was performed for 50 minutes.

[0041] The ultrasonic dispersion frequency was set to 22 kHz and the time was 8 minutes.

[0042] Cooling and filtration The mixed solution was cooled to 20°C and filtered through a 0.2 μm filter membrane to remove undispersed particles and large impurities.

[0043] Filling and sealing Fill the filtered flaw detection agent into pre-treated sealed containers and store at a temperature of 5-20°C, away from direct sunlight.

[0044] Example 3: Preparation of long-lasting storage type flaw detection agent Raw material preparation Diethylene glycol (4.5 parts), polyethylene glycol ether (molecular weight 550, 4.5 parts), diethanolamine (0.3 parts).

[0045] Rhodamine B fluorescent dye (0.2 parts), polyoxyethylene octylphenyl ether (0.1 parts).

[0046] Silica aerogel (0.7 parts), block copolymer (0.6 parts).

[0047] Solvent Matrix Mixing Diethylene glycol and polyethylene glycol ether were added into a mixing kettle, the temperature was controlled at 55°C, the stirring speed was 450 rpm, and the mixture was mixed for 30 minutes.

[0048] Diethanolamine was added and stirring was continued for 20 minutes to ensure complete homogeneity.

[0049] Fluorescent dye dispersion Rhodamine B fluorescent dye was added to the solvent matrix and maintained at 50 °C with stirring for 35 min.

[0050] The ultrasonic dispersion frequency was set at 23 kHz and the treatment was performed for 5 minutes.

[0051] Additive Integration The silica aerogel and the block copolymer were added simultaneously, the mixing temperature was set at 60°C, the stirring speed was 500 rpm, and the time was 40 minutes.

[0052] Ultrasonic dispersion equipment was used with a frequency of 25 kHz for 7 minutes.

[0053] Cooling and filtration The mixed solution was cooled to 22°C and filtered using a 0.4 μm filter membrane to ensure uniform particle distribution.

[0054] Filling and sealing The filtrate was placed in a sealed container and stored at 10°C in a dark place.

[0055] Comparative Example 1: Solvent matrix design of Comparative Example 1 Preparation process: Solvent Base: Diethylene glycol (3 parts), polyethylene glycol ether (molecular weight 400, 6 parts), diethanolamine (0.5 parts).

[0056] Stir at 300 rpm at 50°C for 15 minutes.

[0057] Fluorescent dyes: Rhodamine B (0.3 parts) was added and stirred for 25 minutes without ultrasonic dispersion.

[0058] Additive system: Silica aerogel (0.6 parts), dispersant block copolymer (0.3 parts).

[0059] The mixture was stirred for 30 minutes with the temperature controlled at 50°C. No ultrasonic dispersion treatment was performed.

[0060] Cooling and Filtration: The mixture was cooled to 25°C and filtered through a filter membrane with a pore size of 0.5 μm.

[0061] Filling and sealing: Put it into a sealed container and store it at 25℃ without special light protection conditions.

[0062] the difference: The proportion of diethylene glycol was reduced, the molecular weight of polyethylene glycol ether was reduced, and ultrasonic dispersion treatment was not performed.

[0063] The proportion of dispersant block copolymer is reduced, and the stirring time and temperature are slightly lower than those in Example 1.

[0064] Comparative Example 2: High temperature stability design of comparative example 2 Preparation process: Solvent Base: Diethylene glycol (5.5 parts), polyethylene glycol ether (molecular weight 600, 3.5 parts), diethanolamine (0.1 parts).

[0065] Stir at 400 rpm at 65°C for 20 minutes.

[0066] Fluorescent dyes: Tetramethylbenzidine derivative (0.2 parts) was added, stirred for 30 minutes, and the ultrasonic dispersion time was shortened to 3 minutes (frequency 20 kHz).

[0067] Additive system: Silica aerogel (0.3 parts), dispersant block copolymer (0.5 parts).

[0068] The stirring temperature was reduced to 50°C and the time was reduced to 20 minutes without ultrasonic dispersion.

[0069] Cooling and Filtration: The mixture was cooled to 22°C and filtered using a 0.4 μm filter membrane.

[0070] Filling and sealing: Put it into a sealed container and store it at 25℃, away from light.

[0071] the difference: The proportion of silica aerogel in the additive system was significantly reduced, and ultrasonic dispersion was not performed.

[0072] The proportion of diethylene glycol in the solvent matrix is ​​slightly higher, and the proportion of diethanolamine is reduced.

[0073] Comparative Example 3: Storage stability design of comparative example 3 Preparation process: Solvent Base: Diethylene glycol (4 parts), polyethylene glycol ether (molecular weight 550, 5 parts), diethanolamine (0.2 parts).

[0074] Stir at 400 rpm at 50°C for 25 minutes.

[0075] Fluorescent dyes: Rhodamine B (0.15 parts) was added, the stirring time was shortened to 20 minutes, and ultrasonic dispersion was not used.

[0076] Additive system: Silica aerogel (0.5 parts), dispersant block copolymer (0.5 parts).

[0077] The stirring temperature was controlled at 55°C for 30 minutes, and no ultrasonic dispersion treatment was performed.

[0078] Cooling and Filtration: The mixture was cooled to 20°C and filtered through a 0.5 μm filter membrane.

[0079] Filling and sealing: Store in sealed containers at 15°C with no humidity restrictions.

[0080] the difference: The proportion of fluorescent dye was reduced and ultrasonic dispersion was not performed.

[0081] The stirring temperature and time of the additives were slightly low, and ultrasonic dispersion treatment was not combined.

[0082] Comparative Example 4: Comparison of the fluorescence display capability designs of Examples 2 and 3 Preparation process: Solvent Base: Diethylene glycol (4.5 parts), polyethylene glycol ether (molecular weight 500, 4.5 parts), diethanolamine (0.3 parts).

[0083] Stir at 300 rpm and 55°C for 30 minutes.

[0084] Fluorescent dyes: A tetramethylbenzidine derivative (0.1 parts) was added and stirred for 25 minutes.

[0085] The ultrasonic dispersion treatment was extended to 15 minutes (frequency 30 kHz).

[0086] Additive system: Silica aerogel (0.7 parts), dispersant block copolymer (0.4 parts).

[0087] The mixture was stirred at 65°C for 50 minutes and ultrasonically dispersed for 8 minutes.

[0088] Cooling and Filtration: The mixture was cooled to 22°C and filtered through a 0.3 μm filter membrane.

[0089] Filling and sealing: Place in a sealed container and store in a dark place (10°C).

[0090] the difference: The ultrasonic dispersion frequency and time were significantly extended.

[0091] The proportion of fluorescent dyes decreased and the proportion of dispersant block copolymers decreased.

[0092] Experiment 1: Penetration performance comparison test Experimental Description Experimental objectives By comparing the penetration performance of the flaw detection agent of Example 1 with that of Comparative Example 1, the advantage of the optimized design of the present invention in crack detection is verified.

[0093] Experimental procedures Sample preparation According to Example 1 and Comparative Example 1, flaw detection agent samples were prepared and marked as Sample A (Example 1) and Sample B (Comparative Example 1), respectively.

[0094] Workpiece preparation Aviation alloy plates were selected, and 10 artificial cracks were prepared on the surface by laser etching. The depth was 100 μm, the width was 20 μm, the crack spacing was 2 cm, and the cracks were distributed radially.

[0095] Experimental operation Spray sample A and sample B evenly on the surfaces of the two plates respectively to ensure that the cracks are completely covered.

[0096] Let it stand for 5 minutes and observe the penetration and filling status of the flaw detection agent in the crack.

[0097] A UV light source with a wavelength of 365 nm was used to excite the fluorescence signal inside the crack.

[0098] The penetration depth of each crack was measured (using a microscope, with an accuracy of ±5 μm).

[0099] Record the fluorescence signal intensity (using a fluorescence spectrometer, the unit is relative light intensity).

[0100] Repeat the test Each group of samples was tested 3 times and the average value was taken for comparison.

[0101] Experimental data on permeability comparison between Example 1 and Comparative Example 1 The penetration depth of sample A in the crack is significantly higher than that of sample B, which directly indicates that the optimized solvent matrix design plays a positive role. The synergistic ratio of diethylene glycol and polyethylene glycol ether in Example 1 is optimized, so that the diffusion performance and wetting ability of the solvent are enhanced. Combined with the introduction of diethanolamine, the interfacial wetting effect of the crack wall is significantly improved, and the penetration depth is more uniform, with almost no obvious deviation; The penetration performance of sample B fluctuates, and the depth is lower than that of sample A. In comparative example 1, ultrasonic dispersion treatment was not performed, and the distribution of fluorescent dye and additives in the solvent matrix may be uneven. This unevenness will lead to unstable penetration performance of the flaw detection agent, forming insufficiently filled gaps deep in the cracks. At the same time, the low proportion of diethylene glycol further reduces the diffusion coefficient of the solvent, making it difficult for the flaw detection agent to quickly fill the fine cracks; The intensity difference of the fluorescence signal is also significant. The fluorescence intensity of sample A is stable and uniform, while sample B is more discrete. Obviously, the ultrasonic dispersion step in the process of Example 1 effectively improves the uniformity of the dispersion of the fluorescent dye in the solvent matrix. The distribution of the dye deep in the crack is more complete, and the optical reflection effect inside the crack is enhanced. In contrast, in Comparative Example 1, because the dye is not fully dispersed, the fluorescence signal inside the crack is uneven, and even the signal at the bottom of some cracks is weak.

[0102] Experiment 2: Thermal stability performance comparison test Experimental Description Experimental objectives The thermal stability of Example 2 under high temperature conditions was verified, and compared with Comparative Example 2 to examine the volatilization of the solvent matrix and the ability to maintain the fluorescence signal.

[0103] Experimental procedures Sample preparation The flaw detection agent samples prepared using Example 2 and Comparative Example 2 are marked as Sample A (Example 2) and Sample B (Comparative Example 2), respectively.

[0104] Experimental setup Two aviation alloy plates of the same specifications were used, and 10 artificial cracks were prepared on the surface with a depth of 80 μm and a width of 15 μm.

[0105] Apply sample A and sample B to the crack area respectively to ensure uniform coverage of the flaw detection agent.

[0106] Heat treatment The sample was placed in a thermostat, the temperature was set to 150°C, and the heating time was 1 hour.

[0107] The intensity change of the fluorescence signal inside the crack (relative light intensity) was recorded every 20 minutes, and the total mass of the sample was weighed at the same time to calculate the solvent volatilization rate (%).

[0108] Testing Tools The changes in the intensity of the fluorescence signal within the crack were recorded using a fluorescence spectrometer.

[0109] The mass change was measured using a high-precision electronic balance (accuracy ±0.1 mg).

[0110] Repeat the experiment Three independent experiments were performed for each sample, and the average value was recorded.

[0111] Comparative experimental data of thermal stability performance of Example 2 and Comparative Example 2 Under high temperature environment, the fluorescence signal of sample A remains more stable. Although the intensity decreases slightly, the range of change is small. Silica aerogel plays a key role in Example 2. Its porous structure effectively adsorbs solvent molecules and slows down the volatilization of solvent at high temperature through sustained release. In contrast, the fluorescence signal of sample B decreases significantly, and the signal intensity at the bottom of the crack is particularly weak. This shows that the proportion of aerogel in comparative example 2 is insufficient and fails to provide sufficient thermal stability support, resulting in rapid volatilization of the solvent, affecting the performance of the flaw detection agent; The solvent volatilization rate of sample A is also significantly lower than that of sample B. In the experiment, the high aerogel ratio in Example 2 formed a denser adsorption network, which effectively reduced the diffusion rate of solvent molecules. At the same time, the dynamic stability of the dispersant block copolymer formed an adhesion layer on the surface of the aerogel, further reducing the solvent loss under high temperature conditions. In sample B, this synergistic effect was not reflected, the solvent evaporated faster, and the residual flaw detection agent in the crack area was insufficient to provide a stable detection signal; with the increase of heating time, the crack fluorescence signal of sample B fluctuated more violently, and some crack signals almost disappeared. The flaw detection agent of Example 2 has a more uniform filling effect in the crack, which is due to the combined process of stirring and ultrasonic dispersion. The uniform distribution of aerogel particles in the flaw detection agent enables it to form a continuous solvent release compensation mechanism deep in the crack. In contrast, due to the uneven distribution of aerogel in Comparative Example 2, the flaw detection agent is prone to detachment or incomplete distribution at the bottom of the crack, and the signal attenuation is significant. Overall, sample A exhibits superior stability and adaptability under high temperature conditions.

[0112] Experiment 3: Fluorescence display performance comparison test Experimental Description Experimental objectives The advantages of Example 3 in terms of fluorescence signal display intensity and stability were verified, and compared with Comparative Example 3 to evaluate its display effect in crack detection.

[0113] Experimental procedures Sample preparation The flaw detection agents were prepared according to the processes of Example 3 and Comparative Example 3, respectively. Sample A is Example 3, and sample B is Comparative Example 3.

[0114] Test Artifacts A steel plate workpiece was selected, and three groups of cracks were prefabricated on the surface, each group containing five cracks, with a crack depth of 80 μm and a width of 25 μm. The crack spacing was controlled to be 3 cm.

[0115] Experimental operation Evenly apply sample A and sample B on the surface of each group of cracks. After standing for 3 minutes, wipe off the excess flaw detection agent on the surface with a clean cloth and retain the flaw detection agent inside the cracks.

[0116] A UV light source with a wavelength of 365 nm was used to excite the fluorescence signal inside the crack.

[0117] The fluorescence intensity (relative light intensity, in units of measurement) of each crack was recorded, and the signal intensity changes were recorded every 30 seconds over 3 minutes.

[0118] Compare the crack signal distribution uniformity and signal intensity attenuation.

[0119] Repeat the experiment Each test was repeated 3 times and the average value was recorded.

[0120] Experimental data comparing the fluorescence display performance of Example 3 and Comparative Example 3 The fluorescence display of sample A is more uniform, and the signal variation of each crack in the crack is small. From a mechanistic point of view, the ultrasonic dispersion process in Example 3 makes the fluorescent dye particles evenly distributed in the flaw detection agent. The dye concentration distribution inside the crack is more consistent, avoiding the phenomenon of weak signals at the bottom of the crack. In contrast, because ultrasonic dispersion treatment was not used in sample B, the dye particles were unevenly deposited in the crack, resulting in large fluctuations in signal distribution. The fluorescence signal at the bottom of some cracks is weak, and the fluorescence at the edge of the crack is too concentrated, affecting the detection accuracy; In terms of signal stability, sample A showed better retention ability, and the signal attenuation within 90 seconds was only 5%-7% of the initial intensity. This is closely related to the nano-encapsulation treatment of the dye particles. Nano-encapsulation technology protects the dye molecules and prevents them from rapid photochemical degradation under long-term irradiation of ultraviolet light. In sample B, due to poor dispersion and unencapsulation of the dye particles, decomposition reactions are easily produced under ultraviolet light excitation, resulting in a rapid drop in the signal, and the attenuation after 60 seconds is even as high as 10%-15%; the signal intensity of sample B is lower than that of Example 3, and the initial light intensity is more discrete. This directly reflects the problem of low dye addition ratio in comparative example 3. The insufficient concentration of fluorescent dye and the uneven distribution of particles significantly limit the reflection effect at the bottom of the crack. In contrast, by optimizing the dye ratio and dispersion process in Example 3, not only the dye filling amount inside the crack is increased, but also the uniformity and brightness of the fluorescent signal are enhanced, fully demonstrating the technical advantages.

[0121] Experiment 4: Long-term storage stability comparison test Experimental Description Experimental objectives The physical stability and fluorescence performance retention ability of Example 3 during long-term storage were verified, and compared with Comparative Example 3 to evaluate the performance changes of the flaw detection agent during storage.

[0122] Experimental procedures Sample preparation The flaw detection agent samples were prepared according to the processes of Example 3 and Comparative Example 3, respectively, sample A was Example 3, and sample B was Comparative Example 3.

[0123] Storage conditions: Sample A and Sample B were placed in sealed containers, Sample A was stored at 10°C in a dark environment, and Sample B was stored at 25°C in a dark environment.

[0124] The storage period was 6 months, and the physical state and fluorescence properties of the samples were recorded every month.

[0125] Test content Observe the samples' color changes, stratification, and sedimentation every month.

[0126] After the storage, the sample was evenly coated on the surface of a cracked plate (crack depth 100 μm, width 20 μm), and after standing for 3 minutes, ultraviolet light (365 nm) was used to excite the crack signal.

[0127] Measure the intensity (unit: relative light intensity) and uniformity of the crack fluorescence signal.

[0128] Repeat the experiment Each group of samples was tested 3 times, and the average value was recorded to analyze the effect of storage on the performance of the flaw detection agent.

[0129] Comparative experimental data of long-term storage stability performance of Example 3 and Comparative Example 3 Sample A showed no obvious stratification and precipitation problems during the 6-month storage period. The reasonable additive ratio and ultrasonic dispersion process in Example 3 are the key reasons. The porous network structure of the silica aerogel stabilizes the interaction between the solvent and other components, and the dispersant block copolymer further enhances the dispersion uniformity through dynamic interface regulation. In contrast, the storage performance of sample B is poor, and obvious stratification began to occur from the third month. In Comparative Example 3, the proportion of dispersant is insufficient, and ultrasonic dispersion is not performed, resulting in aggregation and sedimentation of the fluorescent dye and aerogel during storage; The ability to maintain the intensity of the fluorescence signal also highlights the difference between the two samples. The fluorescence signal of sample A decays relatively slowly, with the intensity only decreasing by about 3% after 6 months. This is due to the nano-encapsulated fluorescent dye structure, which reduces the rate of photochemical degradation. In comparative example 3, the dye was not encapsulated and protected, unevenly distributed, and the storage environment was improper, resulting in a fluorescence signal drop of more than 10% after 6 months. The dye concentration inside the crack was significantly reduced, and the fluorescence display effect was affected; In terms of signal uniformity, sample A showed higher stability. The experiment showed that Example 3 filled the crack more completely, which is closely related to the dispersion uniformity. Ultrasonic dispersion treatment ensures that each component in the flaw detection agent maintains a stable distribution during storage, while in Comparative Example 3, due to insufficient dispersion, the crack edge signal is high and the center signal is weak, and the uniformity difference reaches 12%. It can be seen that the optimized design of Example 3 not only improves the instant performance of the flaw detection agent in use, but also significantly improves its overall stability during storage.

[0130] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A non-flammable fluorescent penetrant flaw detection agent composition, characterized in that: The composition comprises the following components in parts by weight: Solvent system: 8-10 parts; Tetramethylbenzidine derivative: 0.1-0.2 parts; Polyoxyethylene octylphenyl ether: 0.1-0.2 parts; Additive system: 1-1.5 parts.

2. A non-combustible fluorescent penetrant flaw detection agent composition according to claim 1, characterized in that: The solvent system comprises: Diethylene glycol: 4-5 parts; Polyethylene glycol ether: 4-5 parts; Functional solvent diethanolamine: 0.1-0.5 parts.

3. The non-combustible fluorescent penetrant flaw detection agent composition according to claim 1, characterized in that: The additive system comprises: Thermal stability enhancer silica aerogel: 0.5-0.8 parts; Dispersant block copolymer: 0.5-0.7 parts.

4. A method for preparing a non-flammable fluorescent penetrant flaw detection agent composition, characterized in that: The use of a non-flammable fluorescent penetrant flaw detection agent composition as described in any one of claims 1 to 3 comprises the following steps: mixing of solvent matrices to form a solvent system; The addition of fluorescent dye is used to disperse the fluorescent dye in the solvent system; The introduction of surfactants is used to adjust the wetting properties of the composition; Integration of additive systems to enhance thermal and dispersion stability; Cooling and filtering, for cooling the composition to room temperature and removing impurities; Filling and sealing are used to complete the final preparation of the composition.

5. The method for preparing a non-flammable fluorescent penetrant flaw detection agent composition according to claim 4, characterized in that: The solvent matrix mixture includes: Mix diethylene glycol and polyethylene glycol ether in a weight ratio of 4-5; Stir at 300-500 rpm at 50-70°C; Add the functional solvent diethanolamine at a weight ratio of 0.1-0.5 and continue stirring for 15-30 minutes.

6. The method for preparing a non-flammable fluorescent penetrant flaw detection agent composition according to claim 4, characterized in that: The addition of the fluorescent dye comprises: Rhodamine B or tetramethylbenzidine derivatives were selected as fluorescent dyes; Add the fluorescent dye to the solvent matrix at a weight ratio of 0.1-0.2; Stir at 40-60°C for 30-60 minutes; The mixture was treated with ultrasonic dispersion equipment for 5-10 minutes at a frequency of 20-25 kHz.

7. The method for preparing a non-flammable fluorescent penetrant flaw detection agent composition according to claim 4, characterized in that: The introduction of the surfactant comprises: Adding nonionic surfactant polyoxyethylene octyl phenyl ether; The weight ratio of surfactant is 0.1-0.2; Mix at a stirring speed of 400-600 rpm for 15-20 minutes.

8. The method for preparing a non-flammable fluorescent penetrant flaw detection agent composition according to claim 4, characterized in that: The integration of the additive system includes: Adding thermal stability enhancer silica aerogel, the weight ratio is 0.5-0.8; Add dispersant block copolymer at a weight ratio of 0.5-0.7; Stir at 60-70°C for 30-60 minutes; The components are evenly distributed by combining mechanical dispersion with ultrasonic dispersion.

9. The method for preparing a non-flammable fluorescent penetrant flaw detection agent composition according to claim 4, characterized in that: The cooling and filtering include: Cool the mixture to 20-25°C; Filter through a microporous membrane with a pore size of 0.2-0.5 μm; Filter out large particles of impurities to ensure the homogeneity of the final composition.

10. The method for preparing a non-flammable fluorescent penetrant flaw detection agent composition according to claim 4, characterized in that: The filling and sealing comprises: Place the cooled and filtered mixture into airtight containers; Store at 5-25℃, avoid direct sunlight and high humidity.

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