A flexible sealant, its preparation method and GIS

Abstract

The present invention relates to the technical field of sealants, and specifically provides a flexible plugging agent, a preparation method thereof, and a GIS. The formula of the plugging agent is as follows: 60-80 parts of polydimethylsiloxane, 10-20 parts of modified epoxy POSS, 2-5 parts of silane coupling agent, 5-10 parts of plasticizer, and 0.1-0.5 part of catalyst, wherein the modified epoxy POSS is epoxy POSS grafted with a benzene ring. When the flexible plugging agent of the present invention is applied to high-pressure gas leakage scenarios, it can effectively resist the impact of high-pressure gas, perform good plugging on it, and avoid the occurrence of bubbling problems.

Description

Technical Field

[0001] The present invention relates to the technical field of sealants, and particularly to a flexible plugging agent, a preparation method thereof, and a GIS. Background Art

[0002] GIS (Gas Insulated Switchgear) is widely used in modern power systems due to its advantages of small floor area, excellent insulation performance, high reliability, etc. As the main insulation and arc-extinguishing medium in GIS, SF6 gas has excellent insulation performance and arc-extinguishing ability. However, during the long-term operation of GIS, due to factors such as installation technology, mechanical stress, and material aging, there may be a small amount of leakage of SF6 gas.

[0003] The leakage of SF6 gas will not only reduce the insulation performance and safety of the equipment, but also cause serious environmental impacts, because SF6 is a strong greenhouse gas, and its greenhouse effect potential is thousands of times that of carbon dioxide. Therefore, timely and effectively plugging the leakage of SF6 gas in GIS is an important task to ensure the safe operation of the power system and environmental protection.

[0004] Traditional methods for plugging the leakage of SF6 gas in GIS usually require power outage for treatment, resulting in the interruption of power supply and affecting the normal power consumption needs of users. At the same time, the power outage operation is complex and time-consuming, increasing the maintenance cost and workload. In order to avoid power outage, some pressure plugging methods have been proposed in the prior art, but in actual application, during the pressure plugging process, the sealant often produces bubbling phenomena due to the pressure or impact of the leaked gas, resulting in poor plugging effect and unable to effectively prevent the leakage of SF6 gas. Summary of the Invention

[0005] In view of this, the present invention proposes an improved plugging agent that can plug the leakage of SF6 gas in GIS under pressure.

[0006] In a first aspect, the present invention provides a flexible plugging agent. The raw material formula of the plugging agent is calculated by weight as follows:

[0007]

[0008] The modified epoxy POSS is epoxy POSS grafted with a benzene ring.

[0009] In some embodiments, the preparation method of the modified epoxy POSS includes: dissolving epoxy POSS in absolute ethanol, slowly dropping phenyltrimethoxysilane, then adding APTES, heating to 40 - 50 °C, keeping warm and stirring for 2 h, filtering and then drying to obtain the modified epoxy POSS. The mass ratio of epoxy POSS: absolute ethanol: phenyltrimethoxysilane: APTES is 1: (5 - 10): (0.4 - 0.6): (0.04 - 0.06).

[0010] In some embodiments, in the preparation method of the modified epoxy POSS, it is heated to 40 - 50 °C, kept warm and stirred for 1 - 3 h. After filtration and drying, it further includes adding toluene, poly(dicyclopentadiene) and a catalyst, stirring and heating to 60 - 70 °C, keeping warm and reacting for 5 - 7 h, cooling to 25 - 35 °C, filtering and drying to obtain the modified epoxy POSS, and the catalyst is boron trifluoride ethyl ether complex.

[0011] In some embodiments, it is heated to 40 - 50 °C, kept warm and stirred for 1 - 3 h, and the mass ratio of the solid material obtained after filtration and drying to poly(dicyclopentadiene) is 1:(1 - 3).

[0012] In some embodiments, the modified epoxy POSS also undergoes a composite treatment, and the steps of the composite treatment include: dissolving the modified epoxy POSS in absolute ethanol, adding PAMAM, stirring for 3 - 5 h, filtering and then drying to obtain the modified epoxy POSS after composite treatment.

[0013] In some embodiments, PAMAM is the third-generation polyamidoamine.

[0014] In some embodiments, the epoxy POSS is EP0408 produced by Hybrid Plastics.

[0015] In some embodiments, the silane coupling agent is methyltriethoxysilane, and / or; the plasticizer is silicone oil, and / or; the catalyst is dibutyltin dilaurate or a platinum catalyst.

[0016] In a second aspect, the present invention also provides a preparation method of the above flexible sealant, including the following steps:

[0017] Step 1: Mix polydimethylsiloxane, a silane coupling agent and a plasticizer, and slowly add the modified epoxy POSS under stirring, and mechanically stir evenly;

[0018] Step 2: Add a catalyst, and obtain a flexible sealant after stirring and dispersing.

[0019] In a third aspect, the present invention also provides a GIS device, and this GIS device is subjected to a plugging treatment using the above flexible sealant.

[0020] The present invention has the following beneficial effects compared with the prior art:

[0021] The present invention generally provides a technical solution for a flexible sealant, which is particularly suitable for applications in high-pressure gas leakage environments, especially for sealing SF6 gas leakage in GIS. By introducing modified epoxy POSS, the mechanical strength and impact resistance of the material are significantly improved, ensuring an efficient sealing effect in a high-pressure gas environment and reducing gas leakage and the problem of easy bubbling during sealing. Moreover, the low shrinkage and high mechanical properties of polydicyclopentadiene effectively reduce the bubbling phenomenon caused by pressure changes during the use of the sealant. The PAMAM high molecular weight structure and multifunctional groups in the composite treatment further enhance the adhesion and stability of the material, reducing the probability of bubbling. Detailed implementation manners

[0022] The following will describe clearly and completely the technical solutions in the embodiments of the present invention in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts belong to the scope of protection of the present invention.

[0023] Unless otherwise defined, all technical terms and scientific terms used herein have the same meaning as commonly understood by those of ordinary skill in the technical field to which the embodiments of the present invention belong. If the definitions stated in this part are contrary to or inconsistent with the definitions stated in the patents, patent applications, published patent applications and other publications incorporated herein by reference, the definitions listed in this part shall prevail over the definitions incorporated herein by reference.

[0024] Unless otherwise specified, the methods used in the following examples are all conventional methods. The materials, reagents and instruments used, unless otherwise specified, are all conventional materials, reagents and instruments in this field, and those skilled in the art can obtain them through commercial channels.

[0025] When an equivalent, concentration or other value or parameter is expressed as a range, a preferred range or a range defined by a series of upper limit preferred values and lower limit preferred values, it should be understood that all ranges formed by any pairing of any range upper limit or preferred value with any range lower limit or preferred value are specifically disclosed, regardless of whether the ranges are separately disclosed. For example, when the range "1 to 5" is disclosed, the described range should be interpreted to include the ranges "1 to 4", "1 to 3", "1 to 2", "1 to 2 and 4 to 5", "1 to 3 and 5", etc. When a numerical range is described herein, unless otherwise stated, the range is intended to include its end values and all integers and fractions within the range. In the specification and claims of this application, range limitations can be combined and / or interchanged, and if not otherwise stated, these ranges include all sub-ranges contained therein.

[0026] Before conventional flexible silicone adhesives are used for plugging, their mechanical strength is usually insufficient. This results in a situation where, when plugging a location with high-pressure leaking gas, the continuously ejected gas exerts pressure on the adhesive film, causing the adhesive film to be easily blown up and form bubbles. The main reason is that the main matrix materials in the flexible plugging adhesive have flexible molecular chains and lack a rigid structure, unable to provide high-strength support. For example, polydimethylsiloxane (PDMS). Moreover, generally, inorganic fillers are usually used in these plugging adhesives. After these fillers are unevenly dispersed, stress concentration points will be formed, making the plugging agent more likely to generate cracks or deform under high pressure. The adhesion of some adhesive films is insufficient or they cannot adhere tightly to the surface of the substrate. High-pressure gas is also likely to form a gap between the adhesive film and the substrate, causing the adhesive film to be blown up. The insufficient adhesion is mainly due to the large surface energy difference between the silicone adhesive matrix and the adhered substrate, resulting in weak chemical bond binding between the silicone adhesive matrix and the substrate surface. The mechanical strength and elasticity of some adhesive films are insufficient and they cannot resist the impact of high-pressure gas, being easily deformed or broken to form bubbles. This bubbling problem seriously affects the sealing effect of the plugging adhesive on the air leakage location.

[0027] In the technical solution of the present application, modified epoxy POSS grafted with a benzene ring is mainly used. By introducing a benzene ring, the modified epoxy POSS improves the mechanical strength and rigidity of the adhesive film, enabling it to better resist the impact of high-pressure gas. The epoxy group provides better adhesion performance, enabling the adhesive film to adhere tightly to the surface of the substrate and reducing the gap for high-pressure gas to enter between the adhesive film and the substrate.

[0028] After introducing the benzene ring structure, the rigidity and heat resistance of the modified POSS are enhanced. At the molecular level, the benzene ring provides rigidity, making the overall material have higher anti-deformation ability when subjected to the impact of high-pressure gas. And APTES containing amino groups forms stronger chemical bond connections through reaction with epoxy groups. These chemical bond connections increase the crosslinking density between molecules and improve the mechanical strength and adhesion performance of the material.

[0029] By introducing the modified epoxy POSS and making it evenly dispersed in the PDMS matrix, a strengthened composite material structure is formed, making the material not easily deformed or broken under high-pressure environments.

[0030] In some specific technical solutions of the present application, dicyclopentadiene is introduced into the modified epoxy POSS. Dicyclopentadiene has excellent mechanical strength and impact resistance, which enables the plugging adhesive film to withstand the impact of high-pressure gas without being blown up. At the same time, the low shrinkage and high chemical resistance of dicyclopentadiene further enhance the stability of the adhesive film and reduce the risk of deformation and rupture.

[0031] The polymer chains of dicyclopentadiene react with epoxy POSS, increasing the intermolecular forces inside the material and at the interface, and improving the overall adhesion performance.

[0032] In some other specific technical solutions of this application, the modified epoxy POSS is also compounded with PAMAM. PAMAM has a highly branched structure and multifunctional groups, which helps to further improve the adhesion and stability of the adhesive film. The multifunctional groups can combine with the modified POSS, making the adhesive film have better uniformity and consistency, avoiding local stress concentration, and helping to further enhance the ability to resist high-pressure gas impact.

[0033] Epoxy POSS has a relatively large molecular weight and a complex molecular structure. By reacting phenyltrimethoxysilane and APTES, functional groups such as benzene rings and amino groups are introduced. The amino group in APTES can undergo a ring-opening reaction with the epoxy group, further increasing the reactivity and adhesion performance of epoxy POSS. The silyl groups combine with the silicone network through hydrolysis and condensation, helping to improve the crosslinking density and stability of the material. Ultimately, the thermal stability, mechanical strength, and adhesion performance of epoxy POSS are improved, making the modified epoxy POSS perform better under high temperature and mechanical stress. After stirring and heating at 40 - 50 °C for 2 h, the reaction is ensured to proceed fully. After filtration and drying, relatively pure modified epoxy POSS is obtained.

[0034] The mixture of PDMS, silane coupling agent, and silicone oil provides basic flexibility and adhesion performance. The introduction of modified epoxy POSS enhances the mechanical properties and adhesion performance of the sealant, especially the sealing effect under high-pressure environments. The addition of the catalyst promotes the crosslinking reaction to form a stable network structure. Among them, the modified epoxy POSS provides enhanced mechanical strength and adhesion performance. By slowly adding and mechanically stirring, it is ensured that the modified epoxy POSS is uniformly dispersed in the PDMS matrix to form a stable composite material. This helps the sealant maintain the structural stability of the adhesive film under the impact of high-pressure gas, achieving the purpose of leak prevention and plugging.

[0035] In some further improved solutions, after catalytic reaction, PDCPD forms a three-dimensional network structure with a certain degree of crosslinking with the modified epoxy POSS grafted with phenyltrimethoxysilane. The crosslinking helps to improve the compactness and stability inside the material, reducing the pores inside the material. Thus, in a high-pressure gas environment, it effectively prevents the generation of bubbles. Moreover, PDCPD itself has relatively low shrinkage and will not shrink significantly during curing and crosslinking, reducing the generation of internal stress in the material, so that the sealant can still maintain the consistency of the internal structure during and after curing. At the same time, it can also improve the thermal stability of the material, enabling the sealant to maintain mechanical properties in high-temperature and chemical environments.

[0036] In some further improved solutions, PAMAM is compounded with modified epoxy POSS grafted with phenyltrimethoxysilane. Among them, PAMAM has a highly branched structure and multifunctional groups. By dissolving it in ethanol and stirring for a certain period of time, PAMAM and modified epoxy POSS are uniformly mixed to form a high-performance composite material. This composite material improves the adhesion performance and mechanical strength, provides good crosslinking density through the highly branched structure, reduces internal voids and micropores, helps prevent gas penetration and diffusion, reduces the bubbling phenomenon, and enables the material to perform better under high-pressure environments.

[0037] The performance of the flexible sealant of the present application is tested through specific examples below.

[0038] In the following examples and comparative examples, the epoxy POSS used is produced by Hybrid Plastics, with the model number EP0408.

[0039] Example 1

[0040] This example provides a preparation method of a flexible sealant, and its formula weight ratio is as follows:

[0041]

[0042]

[0043] Preparation of modified epoxy POSS:

[0044] Dissolve 10 g of epoxy POSS in 50 g of absolute ethanol, slowly dropwise add 5 g of phenyltrimethoxysilane. After the addition is completed, add 0.5 g of APTES, then stir and heat to 45 °C, keep stirring and reacting for 2 h, and then filter and dry to obtain modified epoxy POSS.

[0045] [[ID=Z7]]Preparation of flexible sealant:

[0046] Mix polydimethylsiloxane, methyltriethoxysilane, and silicone oil and stir evenly. Under stirring, slowly add modified epoxy POSS, mechanically stir evenly, and then add dibutyltin dilaurate and stir evenly to obtain a flexible sealant.

[0047] Example 2

[0048] This example provides a preparation method of a flexible sealant, and its formula weight ratio is as follows:

[0049]

[0050] Preparation of modified epoxy POSS:

[0051] Dissolve 10 g of epoxy POSS in 70 g of absolute ethanol, slowly add 4 g of phenyltrimethoxysilane dropwise. After the addition is complete, add 0.4 g of APTES, then stir and heat to 40 °C, keep stirring and reacting for 2 h, and then filter and dry to obtain modified epoxy POSS.

[0052] Preparation of flexible sealant:

[0053] Mix polydimethylsiloxane, methyltriethoxysilane, and silicone oil and stir evenly. Under stirring, slowly add modified epoxy POSS and mechanically stir evenly, then add dibutyltin dilaurate and stir evenly to obtain a flexible sealant.

[0054] Example 3

[0055] This example provides a preparation method of a flexible sealant, and its formula weight parts ratio is as follows:

[0056]

[0057] Preparation of modified epoxy POSS:

[0058] Dissolve 10 g of epoxy POSS in 100 g of absolute ethanol, slowly add 6 g of phenyltrimethoxysilane dropwise. After the addition is complete, add 0.6 g of APTES, then stir and heat to 50 °C, keep stirring and reacting for 2 h, and then filter and dry to obtain modified epoxy POSS.

[0059] Preparation of flexible sealant:

[0060] Mix polydimethylsiloxane, methyltriethoxysilane, and silicone oil and stir evenly. Under stirring, slowly add modified epoxy POSS and mechanically stir evenly, then add dibutyltin dilaurate and stir evenly to obtain a flexible sealant.

[0061] Example 4

[0062] This example provides a preparation method of a flexible sealant, and its formula weight parts ratio is as follows:

[0063]

[0064] Preparation of modified epoxy POSS:

[0065] Dissolve 10 g of epoxy POSS in 50 g of absolute ethanol, slowly add 5 g of phenyltrimethoxysilane dropwise. After the addition is complete, add 0.5 g of APTES, then stir and heat to 45 °C, keep stirring and reacting for 2 h, then filter and dry. Mix the obtained material with toluene, polydicyclopentadiene and boron trifluoride diethyl ether complex in a mass ratio of 1:1:0.1, stir, heat to 65 °C, keep reacting for 6 h, then cool to 30 °C, filter and dry to obtain modified epoxy POSS.

[0066] Preparation of flexible sealant:

[0067] Mix polydimethylsiloxane, methyltriethoxysilane and silicone oil evenly, and slowly add modified epoxy POSS under stirring, stir mechanically until evenly mixed, then add dibutyltin dilaurate and stir evenly to obtain a flexible sealant.

[0068] Example 5

[0069] This example provides a preparation method of a flexible sealant, and its formula weight portion ratio is as follows:

[0070]

[0071]

[0072] Preparation of modified epoxy POSS:

[0073] Dissolve 10 g of epoxy POSS in 50 g of absolute ethanol, slowly add 5 g of phenyltrimethoxysilane dropwise. After the addition is complete, add 0.5 g of APTES, then stir and heat to 45 °C, keep stirring and reacting for 2 h, then filter and dry. Mix the obtained material with toluene, polydicyclopentadiene and boron trifluoride diethyl ether complex in a mass ratio of 1:3:0.1, stir, heat to 65 °C, keep reacting for 6 h, then cool to 30 °C, filter and dry to obtain modified epoxy POSS.

[0074] Preparation of flexible sealant:

[0075] Mix polydimethylsiloxane, methyltriethoxysilane and silicone oil evenly, and slowly add modified epoxy POSS under stirring, stir mechanically until evenly mixed, then add dibutyltin dilaurate and stir evenly to obtain a flexible sealant.

[0076] Example 6

[0077] This example provides a preparation method of a flexible sealant, and its formula weight portion ratio is as follows:

[0078]

[0079]

[0080] Preparation of modified epoxy POSS:

[0081] Dissolve 10 g of epoxy POSS in 50 g of absolute ethanol, slowly add 5 g of phenyltrimethoxysilane dropwise. After the addition is completed, add 0.5 g of APTES, then stir and heat to 45 °C, keep stirring and reacting for 2 h, then filter and dry. Mix the obtained material with toluene, polydicyclopentadiene and boron trifluoride diethyl ether complex in a mass ratio of 1:2:0.1, stir, heat to 65 °C, keep reacting for 6 h, then cool to 30 °C, filter and dry to obtain modified epoxy POSS.

[0082] Preparation of flexible plugging agent:

[0083] Mix polydimethylsiloxane, methyltriethoxysilane and silicone oil evenly, and slowly add modified epoxy POSS under stirring, stir mechanically evenly, then add dibutyltin dilaurate and stir evenly to obtain a flexible plugging agent.

[0084] Example 7

[0085] This example provides a preparation method of a flexible plugging agent, and its formula weight parts ratio is as follows:

[0086]

[0087] Preparation of modified epoxy POSS:

[0088] Dissolve 10 g of epoxy POSS in 50 g of absolute ethanol, slowly add 5 g of phenyltrimethoxysilane dropwise. After the addition is completed, add 0.5 g of APTES, then stir and heat to 45 °C, keep stirring and reacting for 2 h, then filter and dry. Mix the obtained material with toluene, polydicyclopentadiene and boron trifluoride diethyl ether complex in a mass ratio of 1:2:0.1, stir, heat to 65 °C, keep reacting for 6 h, then cool to 30 °C, filter and dry. Then dissolve the dried modified epoxy POSS in absolute ethanol, then add the third-generation PAMAM, stir for 4 h, filter and dry to obtain the modified epoxy POSS with composite treatment, where the mass ratio of modified epoxy POSS:absolute ethanol:third-generation PAMAM is 1:10:0.15.

[0089] Preparation of flexible plugging agent:

[0090] Mix polydimethylsiloxane, methyltriethoxysilane and silicone oil evenly, and slowly add the modified epoxy POSS with composite treatment under stirring, stir mechanically evenly, then add dibutyltin dilaurate and stir evenly to obtain a flexible plugging agent.

[0091] Example 8

[0092] On the basis of Example 7, while keeping other conditions the same, the difference lies in that the PAMAM used is the second generation.

[0093] Example 9

[0094] On the basis of Example 7, while keeping other conditions the same, the difference lies in that the PAMAM used is the fourth generation.

[0095] Example 10

[0096] This example provides a preparation method of a flexible plugging agent, and its formula weight ratio is as follows:

[0097]

[0098]

[0099] Preparation of modified epoxy POSS:

[0100] Dissolve 10 g of epoxy POSS in 50 g of absolute ethanol, slowly dropwise add 5 g of phenyltrimethoxysilane. After the addition is completed, add 0.5 g of APTES, then stir and heat to 45 °C, keep stirring and reacting for 2 h, then filter and dry. Then dissolve the obtained modified epoxy POSS after drying in absolute ethanol, then add the third-generation PAMAM, stir for 4 h, filter and dry to obtain the modified epoxy POSS with composite treatment, where the mass ratio of modified epoxy POSS: absolute ethanol: third-generation PAMAM is 1:10:0.15.

[0101] Preparation of flexible plugging agent:

[0102] Mix polydimethylsiloxane, methyltriethoxysilane, and silicone oil and stir evenly. Under stirring, slowly add the modified epoxy POSS with composite treatment, stir mechanically until evenly mixed, then add dibutyltin dilaurate and stir evenly to obtain the flexible plugging agent.

[0103] Example 11

[0104] On the basis of Example 10, while keeping other conditions the same, the difference lies in that the PAMAM used is the second generation.

[0105] Example 12

[0106] On the basis of Example 10, while keeping other conditions the same, the difference lies in that the PAMAM used is the fourth generation.

[0107] Comparative Example 1

[0108] This comparative example provides a preparation method of a flexible sealant using conventional epoxy POSS, and its formula weight parts ratio is as follows:

[0109]

[0110]

[0111] Preparation of the flexible sealant:

[0112] Mix polydimethylsiloxane, methyltriethoxysilane, and silicone oil and stir evenly. Under stirring, slowly add epoxy POSS and mechanically stir evenly. Then add dibutyltin dilaurate and stir evenly to obtain the flexible sealant.

[0113] Comparative Example 2

[0114] This comparative example provides a preparation method using conventional fillers, and its formula weight parts ratio is as follows:

[0115]

[0116] Preparation of the flexible sealant:

[0117] Mix polydimethylsiloxane, methyltriethoxysilane, and silicone oil and stir evenly. Under stirring, slowly add silica and mechanically stir evenly. Then add dibutyltin dilaurate and stir evenly to obtain the flexible sealant.

[0118] Perform performance verification on the sealants prepared in the above examples and comparative examples respectively. The verification method is as follows:

[0119] Machine-process a 40mm * 40mm square plane area on the surface of the container, drill a round hole with a diameter of 0.5mm at the center of this square plane area, evenly coat and fill the sealants prepared in the above examples and comparative examples in this square area, with a coating thickness of 3mm. After coating, fill nitrogen into the container. Start timing when the nitrogen pressure is 0.3MPa, maintain 0.3MPa for 1min, then increase the pressure to 0.4MPa and maintain for 1min, and so on, until the pressure is increased to 0.9MPa and maintained for 1min. Observe the height change of the sealant film in the square plane area through a camera. When the height change exceeds 1mm, record the corresponding gas pressure value and the corresponding pressure holding time. If it exceeds 1mm during the pressure increase process, record it as 0s of the pressure value after the pressure increase. The specific recorded data is shown in the following table:

[0120] Grouping Pressure / MPa when exceeding 1 mm Corresponding pressure holding time / s when exceeding 1 mm Example 1 0.5 12 Example 2 0.4 34 Example 3 0.5 6 Example 4 0.7 15 Example 5 0.7 44 Example 6 0.7 57 Example 7 0.9 ＞60 Example 8 0.9 22 Example 9 0.8 49 Example 10 0.6 54 Example 11 0.5 31 Example 12 0.6 25 Comparative Example 1 0.3 22 Comparative Example 2 0.3 0

[0121] Examples 1-3 above respectively used raw materials with different ratios. The modified epoxy POSS was epoxy POSS grafted with a benzene ring. Compared with Comparative Example 1, the pressure resistance performance was significantly improved. It could maintain no bubbling for 12 s under a pressure of 0.5 MPa at most. Examples 4-6 adopted a further improvement scheme. On the premise of using benzene ring graft modification, poly(dicyclopentadiene) was also introduced for graft modification, further improving the

[0122] pressure resistance performance of the plugging agent. After coating, the coated surface could remain unchanged under a pressure of 0.7 MPa. Examples 7-9 further introduced PAMAM on the basis of Example 6. Among them, the third generation was introduced in Example 7, and the second and fourth generations were introduced in Examples 8-9 respectively. It can be seen that the comprehensive performance of the third generation was significantly better than that of the second and fourth generations. Similarly, PAMAM was introduced in Examples 10-12 on the basis of Example 1. Again, the comprehensive performance of the third generation was better than that of the second and fourth generations, and there was an obvious performance improvement compared with Example 1.

[0123] In summary, the present application provides a flexible plugging agent using modified epoxy POSS, which has good performance in the scenario of plugging high-pressure gas leakage, especially in dealing with gas impact and bubbling risk problems.

[0124] The above are only the preferred embodiments of the present invention and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A flexible plugging agent, characterized in that, Its raw material formula is calculated by weight parts as follows: 60 - 80 parts of polydimethylsiloxane 10 - 20 parts of modified epoxy POSS 2 - 5 parts of silane coupling agent 5 - 10 parts of plasticizer 0.1 - 0.5 parts of catalyst; The modified epoxy POSS is epoxy POSS grafted with a benzene ring. The preparation method of the modified epoxy POSS includes: dissolving epoxy POSS in absolute ethanol, slowly dropping phenyltrimethoxysilane, then adding APTES, heating to 40 - 50 °C, keeping warm and stirring for 2 h, filtering and then drying to obtain the modified epoxy POSS. The mass ratio of epoxy POSS: absolute ethanol: phenyltrimethoxysilane: APTES is 1:(5 - 10):(0.4 - 0.6):(0.04 - 0.06).

2. The flexible plugging agent according to claim 1, wherein In the preparation method of the modified epoxy POSS, after heating to 40 - 50 °C and keeping warm and stirring for 1 - 3 h, and after filtering and drying, it further includes adding toluene, poly(dicyclopentadiene) and a catalyst, stirring and heating to 60 - 70 °C, keeping warm and reacting for 5 - 7 h, cooling to 25 - 35 °C, filtering and drying to obtain the modified epoxy POSS. The catalyst is boron trifluoride diethyl ether complex.

3. The flexible plugging agent according to claim 2, wherein, After heating to 40 - 50 °C and keeping warm and stirring for 1 - 3 h, the mass ratio of the solid material obtained after filtering and drying to poly(dicyclopentadiene) is 1:(1 - 3).

4. The flexible plugging agent according to claim 1, characterized in that, The modified epoxy POSS also undergoes a composite treatment. The steps of the composite treatment include: dissolving the modified epoxy POSS in absolute ethanol, adding PAMAM, stirring for 3 - 5 h, filtering and then drying to obtain the modified epoxy POSS after composite treatment.

5. The flexible plugging agent according to claim 4, wherein The PAMAM is the third-generation polyamidoamine.

6. The flexible plugging agent according to claim 1, wherein The epoxy POSS is EP0408 produced by Hybrid Plastics Company.

7. The flexible plugging agent according to claim 1, wherein The silane coupling agent is methyltriethoxysilane, and / or; the plasticizer is silicone oil, and / or; the catalyst is dibutyltin dilaurate or platinum catalyst.

8. The preparation method of the flexible plugging agent according to any one of claims 1-7, characterized in that, It includes the following steps: Step 1: Mix polydimethylsiloxane, silane coupling agent and plasticizer, and slowly add the modified epoxy POSS under stirring, and mechanically stir evenly; Step 2: Add the catalyst, and stir and disperse to obtain a flexible plugging agent.

9. A GIS device, characterized in that, The GIS equipment is plugged with the flexible organic plugging agent described in any one of claims 1 - 7.

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