A phenyl silicone resin containing branched structures, and a method of making and using the same

Abstract

The application provides a phenyl silicone resin containing a branched structure and a preparation method and application thereof. The resin structure is prepared by the following steps: ring-opening polymerization reaction of methylphenylsiloxane mixed ring and 1,1,3,3-tetramethyldisiloxane; addition reaction of a polymerization product and an enamine under a rhodium catalyst; condensation reaction of an addition product and vinylphosphonic acid, and removal of unreacted small molecules to obtain a target product. The phenyl silicone resin prepared by the application has high refractive index, good bending resistance and impact resistance, and can improve the service life and stability of a flexible LED lamp.

Description

Technical Field

[0001] This invention belongs to the field of phenyl silicone resins, and particularly relates to a phenyl silicone resin containing a branched structure, its preparation method, and its application. Background Technology

[0002] Due to the high molar refractive index and relatively small molecular volume of benzene rings, high-refractive-index LED encapsulation materials are mainly phenyl-type organosilicon materials. The higher the mass fraction of phenyl groups, the higher the refractive index, and the lower the shrinkage rate of the material. However, because phenyl groups are relatively rigid and have significant steric hindrance, their molecular motion is restricted under stress, resulting in poor impact resistance and tensile strength. Therefore, it is necessary to introduce other groups to enhance the resin's stress absorption, improve its impact resistance, tensile strength, and bending resistance, and enhance its application performance in flexible LED encapsulation materials. Summary of the Invention

[0003] To address the above technical problems, the present invention aims to provide a phenyl silicone resin containing a branched structure. This resin improves the resin's impact resistance, tensile strength, and flexural strength, making it suitable for use in flexible LED encapsulation materials.

[0004] To achieve the above objectives, the technical solution adopted by the present invention is as follows:

[0005] A phenyl silicone resin containing a branched structure, the resin having the structure shown in Formula 1:

[0006]

[0007] Wherein, n is an integer ≥1, preferably n is 10 to 40, and m is an integer ≥1, preferably m is 3 to 6.

[0008] This invention provides a phenyl silicone resin containing a branched structure. The presence of phenyl groups in the resin molecule can improve the refractive index of the silicone resin. At the same time, the ionic bonds formed between the phosphonic acid group and the amino group, the hydrogen bonds formed between the O on the phosphonic acid group and the H on the amino group, and the Si-O-Si bonds in the resin backbone can absorb energy by breaking hydrogen bonds under low stress and by breaking ionic and covalent bonds under high stress. This improves the impact resistance, tensile strength, and bending resistance of the silicone resin, giving the encapsulation material excellent elastic recovery and stress absorption capabilities. Moreover, the synthesis process is stable and feasible, suitable for industrial production.

[0009] Another object of the present invention is to provide a method for preparing a phenyl silicone resin containing a branched structure.

[0010] A method for preparing a phenyl silicone resin containing a branched structure, wherein the resin is the resin described above, the method comprising the following steps:

[0011] S1: A mixed ring of methylphenylsiloxane and 1,1,3,3-tetramethyldisiloxane under an acid catalyst undergoes ring-opening polymerization. After the reaction, the acid catalyst is neutralized, and the solid is filtered to remove unreacted small molecules, yielding the compound shown in Formula 3.

[0012]

[0013] Where n is an integer ≥ 1, preferably n is 10 to 40;

[0014] S2: Compound S3 undergoes an addition reaction with an enamine in the presence of a rhodium catalyst, removing unreacted small molecules to obtain compound S2:

[0015]

[0016] Wherein, n is an integer ≥1, preferably n is 10 to 40, and m is an integer ≥1, preferably m is 3 to 6;

[0017] S3: The compound of Formula 2 undergoes a condensation reaction with vinylphosphonic acid to remove unreacted small molecules, yielding the target product shown in Formula 1.

[0018] In this invention, the methylphenylsiloxane mixed cyclic body described in S1 contains one or more of 2,4,6-trimethyl-2,4,6-triphenylcyclotrisiloxane, 2,4,6,8-tetramethyl-2,4,6,8-tetraphenylcyclotetrasiloxane, and 2,4,6,8,10-pentamethyl-2,4,6,8,10-pentaphenylcyclopentasiloxane; preferably, the mass ratio of the methylphenylsiloxane mixed cyclic body to 1,1,3,3-tetramethyldisiloxane is (12.6~50.7):1.

[0019] In this invention, the reaction described in S1 is carried out under an inert atmosphere.

[0020] In this invention, the acid catalyst in S1 is a fluorinated organic acid with 1-7 carbon atoms, preferably trifluoromethanesulfonic acid; preferably, the amount of the acid catalyst is 1‰ to 5‰ of the total mass of the methylphenylsiloxane mixed ring and 1,1,3,3-tetramethyldisiloxane.

[0021] In this invention, the reaction temperature in S1 is 60-80°C and the reaction time is 3-4 hours.

[0022] In this invention, the neutralization in S1 uses carbonates, preferably one or more alkali metal carbonates, more preferably calcium carbonate; preferably, the amount of carbonate used is 3 to 5% of the total mass of methylphenylsiloxane mixed ring and 1,1,3,3-tetramethyldisiloxane; preferably, the reaction time for the carbonate to neutralize the acid catalyst is 1 to 2 hours.

[0023] In this invention, the unreacted small molecules in step S1 are removed using a short-path evaporator; preferably, the temperature for removing unreacted small molecules is 100-120°C and the pressure is 0.1 kPaA-1 kPaA.

[0024] In this invention, the enamine in S2 is a C3-C6 enamine, preferably one or more of acrylamine, 3-buten-1-amine, 4-penten-1-amine, and 5-hexen-1-amine, more preferably 3-buten-1-amine; preferably, the molar ratio of the compound of formula 3 to the enamine is 1:(2-2.4).

[0025] In this invention, the reaction described in S2 is carried out under an inert atmosphere.

[0026] In this invention, the rhodium catalyst in S2 is one or more of tris(triphenylphosphine) rhodium chloride (I), triphenylphosphine acetylacetone carbonyl rhodium (I), and 2-ethylhexanoate rhodium (I); preferably, the amount of the rhodium catalyst is 1 to 5 ppm of the total mass of the compound of formula 3 and the enamine, calculated as rhodium.

[0027] In this invention, the reaction temperature in step S2 is 40–60°C, and the reaction time is 2–4 hours.

[0028] In this invention, the temperature for removing unreacted small molecules in step S2 is 60–80°C, and the pressure is 0.1 kPaA–1 kPaA.

[0029] In this invention, the molar ratio of the compound of formula 2 described in S3 to vinylphosphonic acid is (2-2.5):1.

[0030] In this invention, the reaction temperature in step S3 is 80–100°C, and the reaction time is 8–10 h.

[0031] In this invention, the temperature for removing unreacted small molecules in step S3 is 100-120°C, and the pressure is 0.1 kPaA-1 kPaA.

[0032] Another object of the present invention is to provide a use for a phenyl silicone resin containing a branched structure.

[0033] Use of a phenyl silicone resin containing a branched structure, wherein the resin is the resin described above or the resin prepared by the method described above, the resin being used for encapsulation of high refractive index flexible LEDs.

[0034] In one embodiment, a high refractive index flexible LED encapsulation material is prepared using the aforementioned branched phenyl silicone resin as a raw material. Specifically, the high refractive index flexible LED encapsulation material is prepared by the following method: a high refractive index flexible LED encapsulation material includes component A and component B, wherein component A includes a branched phenyl silicone resin and a rhodium catalyst; component B includes a branched phenyl silicone resin, phenyl hydrogen-containing silicone oil, and an inhibitor; specifically, the inhibitor may be ethynylcyclohexanol, and the viscosity of the phenyl hydrogen-containing silicone oil may be 1800-2200 cP.

[0035] Compared with the prior art, the advantages of this invention are as follows:

[0036] 1) After curing, it has a refractive index of over 1.56 and a light transmittance of over 98%;

[0037] 2) Because the system contains ionic bonds formed by phosphonic acid groups and amino groups, hydrogen bonds formed between O on phosphonic acid groups and H on amino groups, and Si-O-Si bonds in the resin backbone, hydrogen bonds break and absorb energy when subjected to small stress, and ionic bonds and covalent bonds break and absorb energy when subjected to large stress. Therefore, this encapsulation material has impact resistance, tensile strength, and bending resistance, and has excellent elastic recovery and stress absorption capabilities. Attached Figure Description

[0038] Figure 1 The 1H NMR spectrum of the phenyl silicone resin in Example 1 ( 1 H NMR);

[0039] Figure 2 The carbon NMR spectrum of the phenyl silicone resin in Example 1 ( 13 (C NMR). Detailed Implementation

[0040] The present invention will be further illustrated below with specific embodiments. These embodiments are merely illustrative and do not limit the scope of the invention.

[0041] Main raw material sources:

[0042] Methylphenyl cyclosiloxane mixed ring: Sisbo Organosilicon PC9181, a mixture of methylphenyl cyclosiloxanes, including tricyclic, tetracyclic and pentacyclic rings, with a total active ingredient of more than 98.5%, CAS No. 68037-54-7;

[0043] 1,1,3,3-Tetramethyldisiloxane: Qufu Chenguang Chemical Co., Ltd., purity >99%, CAS No. 3277-26-7;

[0044] Trifluoromethanesulfonic acid and trifluorohexanesulfonic acid: Jiangxi Guohua Industrial Co., Ltd., purity > 99.5%;

[0045] 3-Butene-1-amine: Zhengzhou Kaipuri Biotechnology Co., Ltd., purity >95%, CAS No. 2524-49-4;

[0046] 4-Penten-1-amine: Shanghai Teber Chemical Technology Co., Ltd., purity >95%, CAS No. 22537-07-1;

[0047] 5-Hexene-1-amine: Nanjing Kangmanlin Chemical Industry Co., Ltd., purity >95%, CAS No. 34825-70-2;

[0048] Tris(triphenylphosphine) rhodium chloride (I), triphenylphosphine acetylacetone carbonyl rhodium (I), 2-ethylhexanoate rhodium (I): Shaanxi Ruike New Materials Co., Ltd., purity > 99%;

[0049] Vinyl phosphate: Herderui (Shanghai) New Materials Co., Ltd., purity >97%, CAS No. 1746-03-8;

[0050] Phenyl hydrogen silicone oil: viscosity 2000 cP, Shin-Etsu Chemical Industry Co., Ltd.

[0051] Ethynylcyclohexanol: Sichuan Yibin Hengde Chemical Co., Ltd., purity > 99%, CAS No. 78-27-3;

[0052] Calcium carbonate, potassium carbonate, magnesium carbonate, sodium bicarbonate, sodium carbonate, Aladdin, analytical grade.

[0053] Unless otherwise specified, all other raw materials and reagents can be purchased through ordinary commercial channels.

[0054] The refractive index was tested according to the national standard GB / T 6488-2008, and the testing instrument was the ATAGO high refractive index Abbe refractometer NAR-4T;

[0055] The transmittance was tested in accordance with the national standard GB / T 2410-2008, and the testing instrument was a TH-100 color transmittance haze meter.

[0056] Tensile properties were tested in accordance with the national standard GB / T 2568-1995, and the testing instrument was Rongjida Electronic Tensile Testing Machine WDW-50S;

[0057] Tensile shear properties were tested in accordance with the national standard GB / T 7124-2008, and the testing instrument was Rongjida Electronic Tensile Testing Machine WDW-50S;

[0058] Impact resistance was tested according to the national standard GB / T 1732-, and the testing instrument was the Jingge Instrument QCJ paint film impact tester.

[0059] Example 1

[0060] Take a 5000ml four-necked flask, reflux it under nitrogen protection, and add 4086g of methylphenyl cyclic compound, 324.3g of 1,1,3,3-tetramethyldisiloxane, and 4.41g of trifluoromethanesulfonic acid to the reaction vessel. Heat to 60℃ and allow to equilibrate for 3 hours. After the reaction is complete, add 132.3g of calcium carbonate to the reaction vessel and stir to neutralize for 2 hours. After the reaction is complete, filter to remove the solid. Use a short-path evaporator to perform devolatilization on the filtrate at 0.1kPaA and 120℃ to remove unreacted small molecules. Cool the system to 40℃. 74.9 g of 3-buten-1-amine was added to the system, followed by 0.0189 g of rhodium tris(triphenylphosphine)chloride (I). The temperature was then raised to 60 °C for an addition reaction for 2 h. After the reaction, unreacted small molecules were removed by distillation at 80 °C under a negative pressure of 0.1 kPaA. 42.23 g of vinyl phosphoric acid was then added to the system, and a condensation reaction was carried out at 80 °C for 10 h. After the reaction, unreacted small molecules were removed by distillation at 120 °C under a negative pressure of 0.1 kPaA, yielding a phenyl silicone resin with a branched structure as shown in Formula 1. Characterization results are shown in [Figure 1]. Figure 1 , 2 .

[0061] Example 2

[0062] Take a 5000ml four-necked flask, reflux it under nitrogen protection, and add 4086g of methylphenyl cyclic compound, 324.3g of 1,1,3,3-tetramethyldisiloxane, and 13.23g of trifluoromethanesulfonic acid to the reaction vessel. Heat to 60℃ and allow to equilibrate for 3 hours. After the reaction is complete, add 176.5g of potassium carbonate to the reaction vessel and stir to neutralize for 2 hours. After the reaction is complete, filter to remove the solid. Use a short-path evaporator to volatilize the filtrate at 0.5kPaA and 100℃ to remove unreacted small molecules. Cool the system to 40℃. 89.7 g of 4-penten-1-amine was added to the system, followed by 0.0190 g of rhodium tris(triphenylphosphine)chloride (I). The temperature was then raised to 60 °C for an addition reaction for 2 h. After the reaction was completed, unreacted small molecules were removed by distillation at 80 °C under a negative pressure of 0.1 kPaA. 42.23 g of vinyl phosphoric acid was added to the system, followed by a condensation reaction at 80 °C for 10 h. After the reaction was completed, unreacted small molecules were removed by distillation at 120 °C under a negative pressure of 0.1 kPaA to obtain a phenyl silicone resin with a branched structure as shown in Formula 1.

[0063] Example 3

[0064] Take a 5000ml four-necked flask, reflux it under nitrogen protection, and add 4086g of methylphenyl cyclic compound, 324.3g of 1,1,3,3-tetramethyldisiloxane, and 22.05g of trifluoromethanesulfonic acid to the reactor. Heat to 60℃ and allow to equilibrate for 4 hours. After the reaction is complete, add 220.5g of magnesium carbonate to the reactor and stir to neutralize for 2 hours. After the reaction is complete, filter to remove the solid. Use a short-path evaporator to perform devolatilization on the filtrate at 0.1kPaA and 120℃ to remove unreacted small molecules. Cool the system to 40℃. 74.9 g of 5-hexen-1-amine was added to the system, followed by 0.0038 g of triphenylphosphine acetylacetone carbonyl rhodium (I). The temperature was then raised to 60 °C for an addition reaction for 4 h. After the reaction was completed, unreacted small molecules were removed by distillation at 60 °C under a negative pressure of 0.1 kPa. 42.23 g of vinyl phosphoric acid was added to the system, and a condensation reaction was carried out at 80 °C for 10 h. After the reaction was completed, unreacted small molecules were removed by distillation at 120 °C under a negative pressure of 0.1 kPa to obtain a phenyl silicone resin with a branched structure as shown in Formula 1.

[0065] Example 4

[0066] Take a 5000ml four-necked flask, reflux it under nitrogen protection, and add 4086g of methylphenyl cyclic compound, 160.8g of 1,1,3,3-tetramethyldisiloxane, and 4.25g of trifluorohexanesulfonic acid to the reaction vessel. Heat to 60℃ and allow to equilibrate for 3 hours. After the reaction is complete, add 127.4g of sodium bicarbonate to the reaction vessel and stir to neutralize for 2 hours. After the reaction is complete, filter to remove the solid. Use a short-path evaporator to perform devolatilization on the filtrate at 0.1kPaA and 120℃ to remove unreacted small molecules. Cool the system to 40℃. 34.7 g of 3-buten-1-amine was added to the system, followed by 0.0184 g of rhodium tris(triphenylphosphine)chloride (I). The temperature was then raised to 60 °C for an addition reaction for 2 h. After the reaction was completed, unreacted small molecules were removed by distillation at 80 °C under a negative pressure of 0.1 kPa. 16.89 g of vinyl phosphoric acid was added to the system, followed by a condensation reaction at 100 °C for 8 h. After the reaction was completed, unreacted small molecules were removed by distillation at 100 °C under a negative pressure of 0.1 kPa to obtain a phenyl silicone resin with a branched structure as shown in Formula 1.

[0067] Example 5

[0068] Take a 5000ml four-necked flask, reflux it under nitrogen protection, and add 4086g of methylphenyl cyclic compound, 80.6g of 1,1,3,3-tetramethyldisiloxane, and 4.16g of trifluoromethanesulfonic acid to the reactor. Heat to 50℃ and react for 3 hours to equilibrate. After the reaction is complete, add 125.0g of sodium carbonate to the reactor and stir to neutralize for 2 hours. After the reaction is complete, filter to remove the solid. Take the filtrate and use a short-path evaporator to volatilize unreacted small molecules at 0.1kPaA and 120℃. Cool the system to 40℃ and add 93.6g of 3-buten-1-amine and 0.0194g of... Rhodium 2-ethylhexanoate (I) was heated to 60°C for an addition reaction for 2 hours. After the reaction was completed, unreacted small molecules were removed by distillation at 80°C under a negative pressure of 0.5 kPaA. 63.3 g of vinyl phosphoric acid was added to the system, and a condensation reaction was carried out at 80°C for 10 hours. After the reaction was completed, unreacted small molecules were removed by distillation at 120°C under a negative pressure of 1 kPaA to obtain a phenyl silicone resin with a branched structure as shown in Formula 1.

[0069] Application Example 1

[0070] Using the branched phenyl silicone resin synthesized in Example 1 above as one of the main agents in the formulation of the flexible LED encapsulation material, the flexible LED encapsulation material was prepared according to the following steps:

[0071] Preparation of component A: 100g of phenyl silicone resin containing branched structure was added to a 250ml reactor and stirred at a stirring speed of 300r / min. 0.1 part of the catalyst tris(triphenylphosphine) rhodium chloride (I) was added and stirred under vacuum for 30min to obtain component A.

[0072] Preparation of component B: 100g of phenyl silicone resin containing branched structure, 30g of phenyl hydrogen silicone oil, and 0.01g of ethynylcyclohexanol were sequentially added into a 250ml reactor and stirred at a stirring speed of 1200r / min. The vacuum was turned on and maintained at -0.1MPa for 30min to obtain component B.

[0073] Components A and B were mixed and stirred at 250 r / min for 5 min, and then cured at room temperature. The prepared sample A1 was cured and tested to obtain data such as refractive index, transmittance, tensile properties, tensile shear properties, and impact resistance. The test results are shown in Table 1.

[0074] Application Example 2-5

[0075] Flexible LED encapsulation materials were prepared according to the method in Application Example 1, with the only difference being that the branched phenyl silicone resin used was replaced with the flexible LED encapsulation materials A2-A5 prepared in Examples 2-5. The performance tests shown in Table 1 were performed as described above.

[0076] Comparative Example 1

[0077] Flexible LED encapsulation materials were prepared according to the method in Application Example 1, except that the branched phenyl silicone resin was replaced with commercially available linear phenyl vinyl silicone oil (IOTA252 from Ayota Silicone Co., Ltd.) to prepare flexible LED encapsulation material D1. The performance tests shown in Table 1 were performed as described in Table 1.

[0078] Table 1 Performance Test Results

[0079] A1 A2 A3 A4 A5 D1 Refractive index / % 1.5840 1.5822 1.5803 1.5835 1.5843 1.5432 transmittance / % 98.2 98.1 97.9 98.2 98.2 97.8 Elongation at break / % 10.8 10.3 10.5 10.9 10.2 3.4 Tensile strength / MPa 31 30 31 35 34 8 Steel tensile shear strength / MPa 20 28 24 24 26 5 Impact resistance height / cm 80 72 74 83 81 25

[0080] As shown in Table 1, when the product prepared by this invention is used as a flexible LED packaging material, it can effectively enhance the tensile properties, bending resistance, and impact resistance of the cured material, thereby achieving a toughening effect. It also has excellent elastic recovery and stress absorption capabilities, which can significantly improve the lifespan of flexible LEDs in various application scenarios.

[0081] The above description is only a preferred embodiment of the present invention. It should be noted that those skilled in the art can make several improvements and additions without departing from the method of the present invention, and these improvements and additions should also be considered within the scope of protection of the present invention.

Claims

1. A phenyl silicone resin containing a branched structure, characterized in that, The resin has the structure shown in Formula 1: Formula 1 Where n is an integer ≥ 1 and m is an integer ≥ 1.

2. The phenyl silicone resin according to claim 1, characterized in that, In the resin structure, n is 10 to 40 and m is 3 to 6.

3. A method for preparing a phenyl silicone resin containing a branched structure, wherein the resin is the resin according to claim 1, characterized in that, The method includes the following steps: S1: A mixed ring of methylphenylsiloxane and 1,1,3,3-tetramethyldisiloxane under an acid catalyst undergoes ring-opening polymerization. After the reaction, the acid catalyst is neutralized, and the solid is filtered to remove unreacted small molecules, yielding the compound shown in Formula 3. Formula 3 Where n is an integer ≥ 1; S2: Compound S3 undergoes an addition reaction with an enamine in the presence of a rhodium catalyst, removing unreacted small molecules to obtain compound S2: Formula 2 Where n is an integer ≥ 1, and m is an integer ≥ 1; S3: The compound of Formula 2 undergoes a condensation reaction with vinylphosphonic acid to remove unreacted small molecules, yielding the target product shown in Formula 1.

4. The method according to claim 3, characterized in that, In the compound shown in Formula 3 of S1, n is 10 to 40; In compound S2 of formula 2, n is 10–40 and m is 3–6.

5. The method according to claim 3, characterized in that, The methylphenylsiloxane mixed ring of S1 contains one or more of 2,4,6-trimethyl-2,4,6-triphenylcyclotrisiloxane, 2,4,6,8-tetramethyl-2,4,6,8-tetraphenylcyclotetrasiloxane, and 2,4,6,8,10-pentamethyl-2,4,6,8,10-pentaphenylcyclopentasiloxane; And / or, the reaction described in S1 is carried out under an inert atmosphere; And / or, the acid catalyst described in S1 is a fluorinated organic acid having 1-7 carbon atoms; And / or, the reaction temperature described in S1 is 60–80°C, and the reaction time is 3–4 h; And / or, the neutralization described in S1 uses carbonates; And / or, the removal of unreacted small molecules described in S1 is performed using a short-path evaporator.

6. The method according to claim 5, characterized in that, The mass ratio of the methylphenylsiloxane mixed ring and 1,1,3,3-tetramethyldisiloxane in S1 is (12.6–50.7):1; And / or, the acid catalyst described in S1 is trifluoromethanesulfonic acid; The amount of acid catalyst mentioned in S1 is 1‰ to 5‰ of the total mass of the methylphenylsiloxane mixed ring and 1,1,3,3-tetramethyldisiloxane; And / or, the neutralization described in S1 employs one or more alkali metal carbonates; The amount of carbonate used in S1 is 3 to 5% of the total mass of the methylphenylsiloxane mixed cyclic compound and 1,1,3,3-tetramethyldisiloxane; The reaction time for the carbonate neutralization of the acid catalyst described in S1 is 1 to 2 hours; The temperature for removing unreacted small molecules in S1 is 100–120°C, and the pressure is 0.1 kPaA–1 kPaA.

7. The method according to claim 6, characterized in that, S1 describes the neutralization process using calcium carbonate.

8. The method according to claim 3, characterized in that, The enamine in S2 is a C3-C6 enamine; And / or, the reaction described in S2 is carried out under an inert atmosphere; And / or, the rhodium catalyst described in S2 is one or more of tris(triphenylphosphine)chloride rhodium (I), triphenylphosphine acetylacetone carbonyl rhodium (I), and 2-ethylhexanoate rhodium (I); And / or, the reaction temperature described in S2 is 40–60°C, and the reaction time is 2–4 hours; And / or, the temperature for removing unreacted small molecules described in S2 is 60–80°C, and the pressure is 0.1 kPaA–1 kPaA.

9. The method according to claim 8, characterized in that, The enamine in S2 is one or more of acrylamine, 3-buten-1-amine, 4-penten-1-amine, and 5-hexen-1-amine; The molar ratio of the compound of formula 3 described in S2 to the enamine is 1:(2-2.4); And / or, the rhodium catalyst described in S2 is one or more of tris(triphenylphosphine)chloride rhodium (I), triphenylphosphine acetylacetone carbonyl rhodium (I), and 2-ethylhexanoate rhodium (I); The amount of rhodium catalyst mentioned in S2 is 1 to 5 ppm of the total mass of the compound of Formula 3 and the enamine, calculated as rhodium.

10. The method according to claim 9, characterized in that, The enamine in S2 is 3-butene-1-amine.

11. The method according to claim 3, characterized in that, The molar ratio of the compound of formula 2 described in S3 to vinylphosphonic acid is (2-2.5):1; And / or, the reaction temperature described in S3 is 80–100°C, and the reaction time is 8–10 h; And / or, the temperature for removing unreacted small molecules described in S3 is 100–120°C, and the pressure is 0.1 kPaA–1 kPaA.

12. Use of a phenyl silicone resin containing a branched structure, wherein the resin is the resin according to claim 1 or 2, or the resin prepared by the method according to any one of claims 3-11, characterized in that, The resin is used for encapsulating high refractive index flexible LEDs.

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