High-sensitivity visual hydrogen detection slurry, mixed matrix membrane and preparation method

Abstract

The invention relates to the technical field of hydrogen detection, in particular to high-sensitivity visual hydrogen detection slurry, a mixed matrix membrane and a preparation method of the high-sensitivity visual hydrogen detection slurry and the mixed matrix membrane. The hydrogen detection slurry and the mixed matrix membrane prepared through the method can detect hydrogen leakage at the initial stage of hydrogen leakage of a device under the working conditions of low H2 concentration and low flow speed through obvious color conversion; in addition, the coated slurry can be stably applied to indoor and outdoor complex environments of hydrogen-related scenes.

Description

Technical Field

[0001] The present invention relates to the technical field of hydrogen detection, and specifically relates to a highly sensitive visual hydrogen detection slurry, a mixed matrix membrane and a preparation method thereof. Background Art

[0002] With the popularization and application of hydrogen energy as an energy carrier globally, the safety during the use of hydrogen energy and the early warning and prevention of safety issues have become the focus of attention. Due to the characteristics of hydrogen such as low ignition energy, wide explosion limit range, flammability and explosiveness, once leaked, it will bring serious hidden dangers to safety production, storage and use; in addition, hydrogen is a low-molecular-weight gas, which is very easy to leak and is prone to hydrogen embrittlement. Once leaked in a closed environment, it is extremely easy to cause fire or explosion (volume concentration between 4 - 75 vol%); and H 2 gas is odorless, colorless, and tasteless, so it is not easily detected by humans through the senses.

[0003] In addition, hydrogen has a relatively high diffusion coefficient compared to other combustible gases, further increasing the risk of rapid diffusion after leakage. Therefore, to ensure the safety during the use of hydrogen, it is urgent to develop a safe, efficient, real-time feedback, fast and highly sensitive trace hydrogen detection method for timely early warning at the initial stage of leakage.

[0004] So far, the hydrogen detection technology in actual application scenarios mainly uses fixed electrical signal hydrogen sensors. However, this sensor needs to reach the temperature threshold and be powered on during use, which is likely to generate electric sparks and has the risk of triggering hydrogen explosion; and the escape speed of hydrogen is extremely fast, and it is difficult to enrich in outdoor application scenarios, resulting in the risk of difficult sensor alarm triggering.

[0005] Currently, visual hydrogen-induced color change recovery powder materials have become the focus of attention. After contacting with H 2 it can undergo a color change distinguishable by the naked eye, thus quickly, intuitively, effectively and safely reflecting the hydrogen leakage situation. However, the powder materials are very inconvenient in actual application and are easily contaminated due to long-term outdoor placement. Summary of the Invention

[0006] The purpose of the present invention is to provide a highly sensitive visual hydrogen detection slurry, a mixed matrix membrane and a preparation method thereof for the defects existing in the prior art, which can detect hydrogen leakage under low H 2 concentration and low flow rate hydrogen leakage conditions through an obvious color change, can be reused, with low production cost and use cost. In addition, the coated slurry can be stably applied to the complex indoor and outdoor environments involving hydrogen.

[0007] The technical solution of the present invention is: a preparation method of a highly sensitive visual hydrogen detection slurry, characterized by comprising the following steps: Step 1, select a noble metal compound, and deposit noble metal nanoparticles on the surface of a material with hydrogenochromic function by chemical reduction method or physical sputtering method to obtain material A; Step 2, dissolve a chemical coupling agent in a solvent to obtain solution B; Step 3, fully mix material A and solution B to obtain suspension C; Step 4, add a polymerization monomer to the suspension and stir until evenly mixed; Step 5, add a polymerization initiator and a stabilizer, stir evenly, and obtain a highly sensitive visual hydrogen detection slurry.

[0008] Preferably, the noble metal in the noble metal compound in step 1 is one or more of gold, silver, palladium, platinum, rhodium, and iridium, and the mass loading of the noble metal is 0.05-3 wt%; The material with hydrogenochromic function is WO 3 , MoO 3 , SnO 2 , V 2 O 5 One or more of them.

[0009] Preferably, the chemical reduction method adopted in step 1 is atomic layer deposition method, chemical reduction deposition method, ultraviolet light reduction deposition method, and the physical sputtering method adopted is magnetron sputtering method.

[0010] Preferably, the chemical coupling agent in step 2 is one or more of cinnamic acid, lauric acid, stearic acid, oleic acid, myristic acid, and palmitic acid; The solvent is one or more of deionized water, methanol, ethanol, tert-butanol, isopropanol, n-pentanol, and 2-pentanol.

[0011] Preferably, the polymerization monomer in step 4 is one or more of ethylene glycol acrylate, ethylene glycol methyl ether acrylate, ethylene glycol methacrylate, ethylene glycol methyl ether methacrylate, ethylene glycol dimethacrylate, α,ω-dihydroxy polydimethylsiloxane, hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane, and decamethylcyclopentasiloxane.

[0012] Preferably, the mass ratio of material A, chemical coupling agent and polymerization monomer in suspension C is 0.005-0.1:0.005-0.5:1.

[0013] A highly sensitive visual hydrogen detection slurry is prepared by using the preparation method of a highly sensitive visual hydrogen detection slurry according to any one of claims 1-6.

[0014] A preparation method of a highly sensitive visual hydrogen detection mixed matrix membrane, comprising the following steps: First, a highly sensitive visual hydrogen detection slurry is prepared by using the preparation method of a highly sensitive visual hydrogen detection slurry described in any one of claims 1-6, and a highly sensitive visual hydrogen detection slurry is obtained; Then, the highly sensitive visual hydrogen detection slurry is uniformly coated by a flat film scraping machine, and then degassed, and finally a highly sensitive visual hydrogen detection mixed matrix membrane is obtained after curing.

[0015] Preferably, after the highly sensitive visual hydrogen detection slurry is selected, a polymerization initiator and a stabilizer are first added and stirred evenly, and then a flat film scraping machine is used to form a film. The mass ratio of the added polymerization initiator, stabilizer to the polymerization monomer is 0.01~0.3:0.01~0.3:1; The polymerization initiator is one or more of tetramethylammonium hydroxide, dibutyltin dilaurate, and dioctyltin dilaurate.

[0016] The stabilizer is one or more of benzotriazoles, benzophenones, carbodiimides, titanium oxide, zinc oxide, and silicon dioxide.

[0017] A highly sensitive visual hydrogen detection mixed matrix membrane is prepared by using the preparation method of a highly sensitive visual hydrogen detection mixed matrix membrane described in claim 9.

[0018] Compared with the prior art, the present invention has the following advantages: by means of in-situ chemical crosslinking, the present invention solves the problem of interfacial compatibility between inorganic materials and organic polymers, improves the dispersion degree and utilization efficiency of inorganic materials, and further improves the stability of the mixed matrix membrane and reduces the dosage of inorganic materials; And the addition of inorganic materials can provide channels for hydrogen diffusion, improve the mass transfer rate, and enhance the sensitivity to hydrogen; In addition, the materials are uniformly dispersed and encapsulated in the organic polymer film, which can effectively isolate the influence of the complex outdoor environment on the materials under actual outdoor use conditions, and the discolored mixed matrix membrane can be restored to the initial color when placed in a hydrogen-free air atmosphere and can be recycled multiple times, so the service life is long.

[0019] The highly sensitive visual hydrogen detection slurry and the mixed matrix membrane prepared by this method can both produce a rapid response visible to the naked eye to hydrogen within a short time at low H 2 concentration and low flow rate, and the preparation process conditions are relatively simple and easy to operate in large batches. The highly sensitive visual hydrogen detection slurry can be directly coated on the surface of the workpiece to form a coating to detect hydrogen, or can be made into a flexible mixed matrix membrane for adhering to the workpiece to detect hydrogen. Description of the Drawings

[0020] Figure 1 The mixed matrix membrane prepared in Example 1 and its flexibility and metal adhesion; Figure 2 Color change diagrams of the mixed matrix membrane prepared in Example 1 upon exposure to hydrogen for 1 min and 5 min; Figure 3 Color change diagrams of the mixed matrix membrane prepared in Example 1 after changing color upon exposure to hydrogen and then placed in air for 50 min and 2 h; Figure 4 Color change diagrams of the mixed matrix membrane prepared in Example 1 after the hydrogen exposure - air recovery process and then exposed to hydrogen again for 1 min and 5 min; Figure 5 Effect diagram of the mixed matrix membrane in the actual application scenario; Figure 6 Reflection spectra diagrams of the mixed matrix membrane before and after color change. Detailed implementation manners

[0021] The following further describes the present invention in conjunction with the accompanying drawings and examples. Example 1

[0022] A preparation method of a visual hydrogen detection mixed matrix membrane realized by in - situ cross - linking described in this example is as follows: Step 1, Weigh 1 g of WO 3 Disperse it in 100 mL of deionized water. After stirring and ultrasonic treatment to form a suspension, dropwise add 27.2 mL of a chloroplatinic acid solution with a concentration of 1 g / L; dropwise add 12 mL of an aqueous solution of NaBH 4 to the suspension, continue stirring for 0.5 h, let it stand for half an hour, then filter by suction, wash with deionized water, and dry to obtain material A.

[0023] Step 2, Dissolve 1.4 g of stearic acid, a chemical coupling agent, in 35 mL of ethanol to obtain solution B; Step 3, Weigh 0.8 g of material A, grind it, add it to solution B, and stir and mix at high speed to obtain suspension C; Step 4, Weigh 20 g of ethylene glycol and methacrylic acid polymerization monomers, slowly add suspension C to the polymerization monomers, and stir evenly at high speed to obtain a high - sensitivity visual hydrogen detection slurry; Step 5, Use a flat film - scraping machine to evenly coat the high - sensitivity visual hydrogen detection slurry with a film thickness of 150 μm. Place the film in a vacuum drying oven to remove bubbles, and then heat it to 80 °C for curing for 30 min to obtain a high - sensitivity visual hydrogen detection mixed matrix membrane.

[0024] The obtained mixed matrix membrane is as Figure 1 shown, and is composed of Figure 1It can be seen that the prepared mixed matrix membrane is uniformly light gray, has excellent flexibility, can be bent at will, and the prepared mixed matrix membrane has strong adhesion on the metal surface and is not easy to fall off.

[0025] Figure 2 For the color change of the mixed matrix membrane after contacting hydrogen for 1 minute and 5 minutes at a concentration of 1% H 2 Concentration and a flow rate of 30 mL / min. It can be seen by comparison that when the mixed matrix membrane contacts hydrogen at a low concentration and low flow rate for 1 min, the mixed matrix membrane changes from grayish white to light blue, and can become dark blue after 5 minutes, showing a visible color change to the naked eye. This proves that the mixed matrix membrane can realize the function of monitoring hydrogen leakage through visual color change.

[0026] Figure 3 It can be seen that when the hydrogen-sensitive mixed matrix membrane is placed in an air atmosphere and left standing for 50 minutes, it can basically return to the initial color, and can return to the initial state after being placed for 2 h. This shows that the mixed matrix membrane has good recoverability.

[0027] Figure 4 For the effect diagram of the hydrogen-discolored mixed matrix membrane after being restored to the initial state after being placed for 2 h and then passing hydrogen again. From Figure 4 It can be seen that it shows the same discoloration trend as the initial state after passing hydrogen for 1 min and 5 min under the same conditions, indicating that the prepared mixed matrix membrane has reusability.

[0028] Figure 5 This is the effect diagram of this mixed matrix membrane in the actual application scenario. It can be seen from the figure that the part of the mixed matrix membrane in contact with hydrogen can indeed undergo a visible color change to the naked eye, which can accurately indicate the leakage site and help to timely detect and solve the problem of hydrogen micro-leakage at the application site. Example 2

[0029] A preparation method of a visual hydrogen detection mixed matrix membrane realized by in-situ crosslinking described in this example is as follows: Step 1, Weigh 1 g of WO 3 Disperse it in 100 mL of deionized water, stir and ultrasonically form a suspension, and then dropwise add 25 mL of a palladium chloride solution with a concentration of 1 g / L; Add 18 mL of NaBH 4 Aqueous solution dropwise to the suspension, continue to stir for 0.5 h, stand for half an hour, then filter, wash with deionized water, and dry to obtain material A.

[0030] Step 2, Dissolve 1.5 g of lauric acid, a chemical coupling agent, in 20 mL of isopropanol to obtain solution B; Step 3, Weigh 0.75 g of material A, grind it, add it to solution B and mix by ball milling to obtain suspension C; Step 4: Weigh 25 g of ethylene glycol methacrylate polymerization monomer, slowly add suspension C to the polymerization monomer, stir evenly at high speed, add 0.8 g of zinc oxide and stir evenly to obtain a highly sensitive visual hydrogen detection slurry; Step 5: Use a flat film squeegee to evenly coat the highly sensitive visual hydrogen detection slurry with a film thickness of 150 μm. Place the film in a vacuum drying oven to remove bubbles, and then heat it to 100 °C for curing for 30 min to obtain a highly sensitive visual hydrogen detection mixed matrix membrane. Example 3

[0031] A preparation method of a visual hydrogen detection mixed matrix membrane realized by in-situ crosslinking according to this example is as follows: Step 1: Weigh 0.5 g of MO 3 Disperse it in a mixed solution of 48 mL of ethylene glycol and water (V 乙二醇 : V 水 = 5:1), stir for 30 min; dropwise add 14 mL of a chloroplatinic acid solution with a concentration of 1 g / L to the above suspension, stir for 2 h, then transfer it to a high-pressure crystallization kettle with a polytetrafluoroethylene inner lining, react at 120 °C for 3 h, filter the product by suction, wash it three times with deionized water, and dry it to obtain material A.

[0032] Step 2: Dissolve 0.75 g of oleic acid, a chemical coupling agent, in a mixed solvent of 10 mL of ethanol and tert-butanol (volume ratio 1:1) to obtain solution B; Step 3: Weigh 0.3 g of material A, grind it and add it to solution B, and mix it ultrasonically to obtain suspension C; Step 4: Weigh 10 g of α,ω-dihydroxypolydimethylsiloxane polymerization monomer, slowly add suspension C to the polymerization monomer, stir evenly at high speed, add 0.05 g of dibutyltin dilaurate, and continue to stir until evenly mixed to obtain a highly sensitive visual hydrogen detection slurry; Step 5: Use a flat film squeegee to evenly coat the highly sensitive visual hydrogen detection slurry with a film thickness of 200 μm. Place the film in a vacuum drying oven to remove bubbles, and then heat it to 80 °C for curing for 20 min to obtain a highly sensitive visual hydrogen detection mixed matrix membrane. Example 4

[0033] A preparation method of a visual hydrogen detection mixed matrix membrane realized by in-situ crosslinking according to this example is as follows: Step 1: Disperse a certain amount of WO 3, a deposition reaction is carried out in a deposition reactor of an atomic layer deposition (ALD) system. The precursor for depositing Pt nanoparticles by ALD is trimethylmethylcyclopentadienyl platinum, and precursor ozone is used as an oxidant. After depositing for 5 cycles, a hydrogenochromic material with fast response - recovery can be obtained.

[0034] Step 2: Dissolve 1.7 g of myristic acid, a chemical coupling agent, in 30 mL of tert - butanol to obtain solution B. Step 3: Weigh 0.9 g of material A, grind it, add it to solution B, and mix by ball - milling to obtain suspension C. Step 4: Weigh 14 g of ethylene glycol methyl ether acrylic polymerization monomer and 6 g of dimethylsiloxane monomer, and mix them evenly. Slowly add suspension C to the polymerization monomer. After stirring evenly at high speed, add tetramethylammonium hydroxide, a dimethylsiloxane polymerization initiator, and benzotriazole. After stirring evenly, a highly sensitive visual hydrogen - detection slurry is obtained. Step 5: Use a flat - blade coater to evenly coat the highly sensitive visual hydrogen - detection slurry. The film thickness is 150 μm. Place the film in a vacuum drying oven to remove bubbles, and then heat it to 110 °C and cure for 30 min to obtain a highly sensitive visual hydrogen - detection mixed - matrix membrane. Example 5

[0035] A preparation method of a visual hydrogen - detection mixed - matrix membrane achieved by in - situ cross - linking described in this example is as follows: Step 1: Weigh 1.0 g of SnO 2 Disperse it in 40 mL of deionized water and stir for 30 min; dropwise add 17 mL of a palladium chloride solution with a concentration of 1 g / L to the above suspension; expose the above suspension under an ultraviolet lamp for 7 h, perform suction filtration, wash three times with deionized water, and dry to obtain a hydrogenochromic material with fast response - recovery.

[0036] Step 2: Dissolve 2 g of cinnamic acid, a chemical coupling agent, in 15 mL of isopropanol to obtain solution B. Step 3: Weigh 1 g of material A, grind it, add it to solution B, and stir - mix at high speed to obtain suspension C. Step 4: Weigh 20 g of ethylene glycol methacrylate polymerization monomer, slowly add suspension C to the polymerization monomer, and stir evenly at high speed to obtain a highly sensitive visual hydrogen - detection slurry. Step 5: Use a flat - blade coater to evenly coat the highly sensitive visual hydrogen - detection slurry. The film thickness is 100 μm. Place the film in a vacuum drying oven to remove bubbles, and then heat it to 100 °C and cure for 50 min to obtain a highly sensitive visual hydrogen - detection mixed - matrix membrane. Example 6

[0037] A method for preparing a visual hydrogen detection mixed matrix membrane achieved by in-situ crosslinking according to this embodiment is as follows: Step 1: Weigh 0.500 g of WO 3 and disperse it in 60 mL of deionized water, and stir for 30 min; dropwise add 13.6 mL of a chloroplatinic acid solution with a concentration of 1 g / L to the above suspension; under an ice bath, dropwise add 6.5 mL of an NaBH 4 aqueous solution to the suspension, continue to stir for 0.5 h, let it stand for half an hour, filter by suction, wash three times with deionized water, and dry to obtain a hydrogenochromic material that can respond and recover quickly.

[0038] Step 2: Dissolve 0.9 g of stearic acid, a chemical coupling agent, in a mixed solution of 20 mL of ethanol and isopropanol (volume ratio 1:1) to obtain solution B; Step 3: Weigh 0.35 g of material A, grind it and add it to solution B, and stir and mix at high speed to obtain suspension C; Step 4: Weigh 10 g of octamethylcyclotetrasiloxane polymerization monomer, slowly add suspension C to the polymerization monomer, stir evenly at high speed, add the polymerization initiator tetramethylammonium hydroxide, and stir evenly to obtain a highly sensitive visual hydrogen detection slurry; Step 5: Use a flat film scraping machine to evenly coat the highly sensitive visual hydrogen detection slurry with a film thickness of 150 μm, place the film in a vacuum drying oven to remove bubbles, and then heat it to 100 °C and cure for 30 min to obtain a highly sensitive visual hydrogen detection mixed matrix membrane. Example 7

[0039] A method for preparing a visual hydrogen detection mixed matrix membrane achieved by in-situ crosslinking according to this embodiment is as follows: Step 1: Weigh 1 g of V 2 O 5 and disperse it in 100 mL of deionized water. After stirring and ultrasonicating to form a suspension, dropwise add 27.2 mL of a chloroplatinic acid solution with a concentration of 1 g / L; dropwise add 15 mL of an NaBH 4 aqueous solution to the suspension, continue to stir for 0.5 h, let it stand for half an hour, then filter by suction, wash with deionized water, and dry to obtain material A.

[0040] Step 2: Dissolve 2.1 g of lauric acid, a chemical coupling agent, in 25 mL of isopropanol to obtain solution B; Step 3: Weigh 1 g of material A, grind it and add it to solution B, and stir and mix at high speed to obtain suspension C; Step 4: Weigh 15 g of ethylene glycol acrylate polymerization monomer and mix it evenly with 5 g of decamethylpentasiloxane monomer. Slowly add suspension C to the polymerization monomer, stir evenly at high speed, add 0.5 g of dimethylsiloxane polymerization initiator tetramethylammonium hydroxide and stir for 5 min to obtain a highly sensitive visual hydrogen detection slurry. Step 5: Use a flat film applicator to evenly coat the highly sensitive visual hydrogen detection slurry with a film thickness of 200 μm. Place the film in a vacuum drying oven to remove air bubbles, and then heat it to 80 °C and cure for 30 min to obtain a highly sensitive visual hydrogen detection mixed matrix membrane.

[0041] Experimental Example 1: (1) To further accurately verify the detection performance of the highly sensitive visual hydrogen detection slurry, a color development test was carried out on it, and the steps are as follows: First, the highly sensitive visual hydrogen detection slurries prepared in Examples 1 to 7 were coated on the same sample card at intervals. Next, place the sample card inside an opaque gas chamber. The gas chamber is connected to an inlet pipe and an exhaust pipe, and then a 1% H 2 / Ar mixed gas is introduced through the inlet pipe at a flow rate of 30 mL / min. Next, take out the sample card. It was observed that the colors of the 7 coated slurries on the sample card had all changed significantly at the moment of opening the gas chamber, and then gradually returned to their original colors.

[0042] Experimental Example 2: To further accurately verify the visual hydrogen detection performance and rate of the highly sensitive visual hydrogen detection mixed matrix membrane, its spectral changes under test conditions were measured, and the steps are as follows: First, place the highly sensitive visual hydrogen detection mixed matrix membrane prepared in Example 1 on the sample stage and precisely fit it to the surface of the sample stage.

[0043] Next, seal the sample stage inside an opaque gas chamber and make it airtight.

[0044] Next, vertically irradiate the light source of the fiber optic spectrometer onto the surface of the sample, and then collect the reflection spectrum of the sample surface from the signal collector at the center of the probe.

[0045] To simulate the characteristics of low hydrogen concentration and low flow rate at the initial stage of hydrogen leakage in the actual application scenario, after the spectrum is stable, introduce a 1% H 2 / Ar mixed gas at a flow rate of 30 mL / min. Observe the change of the sample reflection spectrum after the mixed gas contacts the mixed matrix membrane, and record the change curve of the reflectance at 750 nm over time. The spectral comparison of the highly sensitive visual hydrogen detection mixed matrix membrane prepared in this example before and after hydrogen exposure is asFigure 6 as shown

[0046] As can be seen from the above results, the reflectivity of the slurry in the red light band decreases significantly before and after color change, while the change in the blue light band is relatively small. This indicates that the absorption ability of the hybrid matrix film for red light increases significantly after hydrogen-induced color change, and the absorption rate in the blue light region changes less. This is the physical factor for the color change of the slurry and the hybrid matrix film. From a chemical perspective, after hydrogen contacts the hydrogen-sensitive material, its band gap structure changes, and the color change rate is relatively fast at the initial stage of contact. The time for the reflectivity at 750 nm to decrease by 10% is only 2 minutes.

[0047] Then, according to the above experimental methods, the hydrogen-sensing performance of the highly sensitive visual hydrogen detection hybrid matrix films prepared in Examples 2 to 7 was tested respectively, and the data were statistically analyzed and plotted in Table 1 below. 。

[0048] The above results show that the hybrid matrix film can exhibit rapid and sensitive response in a short time at low concentration and low flow rate in the initial stage of hydrogen leakage, and is suitable for timely early warning, investigation and positioning when hydrogen sensors and alarm devices cannot be triggered in the initial stage of hydrogen leakage. It is especially suitable for hydrogen-related scenarios with high-density pipeline and joint layouts outdoors, such as refineries, hydrogen production and storage facilities, and hydrogen refueling stations.

[0049] The present invention is not limited to the above embodiments. Within the scope of knowledge possessed by those skilled in the art, various changes can be made without departing from the purpose of the present invention, and the changed content still falls within the protection scope of the present invention.

Claims

1. A method for preparing a highly sensitive visual hydrogen detection slurry, characterized in that: The following steps are involved: Step 1, selecting a noble metal compound, and depositing noble metal nanoparticles onto the surface of a material having a hydrogen-induced color-changing function by chemical reduction or physical sputtering to obtain material A; Step 2, dissolving the chemical coupling agent in a solvent to obtain solution B; Step 3, fully mixing material A and solution B to obtain suspension C; Step 4, adding the polymerization monomer into the suspension and stirring until it is evenly stirred; Step 5, adding a polymerization initiator and a stabilizer, stirring evenly, and obtaining a high-sensitivity visual hydrogen detection slurry.

2. The method for preparing a highly sensitive visual hydrogen detection slurry according to claim 1, characterized in that: Step 1: the precious metal in the precious metal compound is one or more of gold, silver, palladium, platinum, rhodium and iridium, and the mass loading of the precious metal is 0.05-3wt%; The material with hydrogen-induced color-changing function is one or more of WO3, MoO3, SnO2, and V2O5.

3. The method for preparing a highly sensitive visual hydrogen detection slurry according to claim 1, characterized in that: The chemical reduction method used in step 1 is atomic layer deposition, chemical reduction deposition, and ultraviolet light reduction deposition, and the physical sputtering method used is magnetron sputtering.

4. The method for preparing a highly sensitive visual hydrogen detection slurry according to claim 1, characterized in that: Step 2: the chemical coupling agent is one or more of cinnamic acid, lauric acid, stearic acid, oleic acid, myristic acid, and palmitic acid; The solvent is one or more of deionized water, methanol, ethanol, tert-butanol, isopropanol, n-pentanol, and 2-pentanol.

5. The method for preparing a highly sensitive visual hydrogen detection slurry according to claim 1, characterized in that: The polymerization monomer in step 4 is one or more of ethylene glycol acrylate, ethylene glycol methyl ether acrylate, ethylene glycol methacrylate, ethylene glycol methyl ether methacrylate, ethylene glycol dimethacrylate, α, ω-dihydroxy polydimethylsiloxane, hexamethylcyclotrisiloxane, octamethylcyclotetrasiloxane, and decamethylcyclopentasiloxane.

6. The method for preparing a highly sensitive visual hydrogen detection slurry according to claim 1, characterized in that: The mass ratio of material A, chemical coupling agent and polymerization monomer in suspension C is 0.005-0.1:0.005-0.5:

1.

7. A highly sensitive visual hydrogen detection slurry, characterized in that: The method for preparing a high-sensitivity visual hydrogen detection slurry is used as described in any one of claims 1 to 6.

8. A method for preparing a mixed matrix membrane for high-sensitivity visual hydrogen detection, characterized in that: The following steps are involved: First, a high-sensitivity visual hydrogen detection slurry is prepared by using a preparation method of a high-sensitivity visual hydrogen detection slurry according to any one of claims 1 to 6; Then, the high-sensitivity visual hydrogen detection slurry is evenly coated by a flat-plate scraper, and then degassing treatment is performed. Finally, after curing, a high-sensitivity visual hydrogen detection mixed matrix membrane is obtained.

9. The method for preparing a high-sensitivity visual hydrogen detection mixed matrix membrane according to claim 8, characterized in that: After selecting a high-sensitivity visual hydrogen detection slurry, first add a polymerization initiator and a stabilizer and stir evenly, then pour it into a flat scraping film machine to form a film. The mass ratio of the added polymerization initiator, stabilizer and polymerization monomer is 0.01~0.3:0.01~0.3:1; The polymerization initiator is one or more of tetramethylammonium hydroxide, dibutyltin dilaurate, and di-n-octyltin dilaurate; The stabilizer is one or more of benzotriazoles, benzophenones, carbodiimides, titanium oxide, zinc oxide, and silicon dioxide.

10. A high-sensitivity visual hydrogen detection mixed matrix membrane, characterized in that: The membrane is prepared by the method for preparing a high-sensitivity visual hydrogen detection mixed matrix membrane as described in claim 9.

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