A high-performance polysiloxane elastomer based on silyl ether bond and preparation method thereof

By introducing hydrogen bonds and dynamic silicone ether bond crosslinking into the polysiloxane elastomer to form a dynamic crosslinking network, the shortcomings of polysiloxane elastomer in terms of mechanical properties, thermal stability and reprocessable properties are solved. High performance and reprocessability of materials are achieved.

CN115716900BActive Publication Date: 2025-02-07TIANJIN UNIV
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Patent Information

Application Number
CN202210278234.7
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-03-21
Publication Date
2025-02-07
Estimated Expiration
2042-03-21

AI Technical Summary

Technical Problem

The existing polysiloxane elastomer materials have shortcomings in mechanical properties, thermal stability and reprocessable properties, resulting in their limitations in practical applications.

Method used

By introducing hydrogen bonds as sacrificial bonds and crosslinking of dynamic siloxane bonds, an amino-terminated polydimethylsiloxane (APDMS) reacts with isofluorone diisocyanate (IPDI) to form a polysiloxane long chain , and a dynamic crosslinking network is formed in the material.

Benefits of technology

It improves the mechanical properties and thermal stability of the polysiloxane elastomer, while also imparts good reprocessable properties to the material, solving the problem of insufficient application of the material in practical applications.

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Abstract

The present invention discloses a high-performance polysiloxane elastomer based on siloxane bonds and a preparation method thereof. First, amino-terminated polysiloxane is reacted with isophorone diisocyanate to obtain a long polysiloxane chain, and hydrogen bonds are introduced into the material as sacrificial bonds to enhance mechanical properties; then, dynamic siloxane bonds are used to form a dynamic cross-linking network inside the material to prepare a polysiloxane elastomer material with good mechanical properties, thermal stability and reprocessability. The present invention provides a reprocessable polysiloxane elastomer material with hydrogen bonds as sacrificial bonds and dynamic siloxane bonds cross-linking and a preparation method thereof, which can improve the mechanical properties of the polysiloxane elastomer.
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Description

Technical Field

[0001] The present invention belongs to the field of polymers, and more specifically, relates to a polysiloxane elastic material, in particular, a polysiloxane-based material, diisocyanate-based material, hydrogen bonds introduced to enhance mechanical properties, silyl ether bonds added to regulate mechanical properties, improve thermal stability of the material, and give the material reprocessability. Background Art

[0002] Polysiloxane is a polymer with repeated silicon-oxygen bonds as the main chain and organic groups such as methyl and phenyl groups connected to the silicon atoms. Due to its unique Si-O structure, polysiloxane is a typical semi-inorganic and semi-organic polymer. It has both the heat resistance of inorganic substances and the flexibility of organic polymers. It also has good aging resistance, weather resistance, resistance to organic solvents, and is non-toxic and odorless. These unique properties make it widely used as an elastic material in smart wearables, sensors, high-end manufacturing, military industry and other fields.

[0003] However, commercial polysiloxane elastomers use permanent crosslinking, and once the material fails, it cannot be reprocessed and recycled, which greatly wastes resources and harms the environment. At the same time, due to the weak interaction between molecular chains, polysiloxane elastomers usually have poor mechanical properties. Previously reported dynamic covalent crosslinked polysiloxane elastomers have given the material reprocessable properties, which is beneficial to saving resources and protecting the environment, but the thermal stability of these dynamic bonds is generally poor and cannot be compared with polysiloxane matrices. While giving the structure dynamic properties, it also reduces thermal stability. These shortcomings limit the application of polysiloxane elastomers in actual production, so it is of great practical significance to prepare polysiloxane elastomers with high mechanical properties, thermal stability and reprocessability. Summary of the invention

[0004] The purpose of the present invention is to overcome the deficiencies of the prior art and provide a reprocessable polysiloxane elastomer material with hydrogen bonds as sacrificial bonds and dynamic silyl ether bonds as cross-links and a preparation method thereof.

[0005] The technical purpose of the present invention is achieved through the following technical solutions.

[0006] A high-performance polysiloxane elastomer based on silyl ether bonds and a preparation method thereof are carried out according to the following steps:

[0007] Step 1, uniformly dispersing polysiloxane in a solvent, adding diisocyanate, chain extender and modifier in sequence under an inert protective atmosphere and reacting them fully, the amount of polysiloxane is 100 parts by weight, the amount of diisocyanate is 20-30 parts by weight, the amount of chain extender is 1-5 parts by weight, and the amount of modifier is 0.5-3 parts by weight; preferably, the amount of polysiloxane is 100 parts by weight, the amount of diisocyanate is 25-30 parts by weight, the amount of chain extender is 1-3 parts by weight, and the amount of modifier is 1-3 parts by weight.

[0008] In step 1, the polysiloxane is aminopropyl-terminated polydimethylsiloxane (APDMS).

[0009] In step 1, the diisocyanate is one of toluene diisocyanate, isophorone diisocyanate, diphenylmethane diisocyanate, dicyclohexylmethane diisocyanate, hexamethylene diisocyanate or lysine diisocyanate, preferably isophorone diisocyanate.

[0010] In step 1, the chain extender is one of 3,3'-(1,1,3,3-tetramethyl-1,3-disiloxy)bis(1-propylamine) (AES), 1,4-ethylenediamine (EI), 1,6-hexanediamine (HI) or 1,4-butanediol (BDO), preferably 3,3'-(1,1,3,3-tetramethyl-1,3-disiloxy)bis(1-propylamine) (AES).

[0011] In step 1, the modifier is one of 2-aminoethanol (AT), 3-amino-1,2-propanediol (3-AP), and 2-amino-1,3-propanediol (2-AP), preferably 3-amino-1,2-propanediol (3-AP).

[0012] In step 1, stirring is used to uniformly disperse and react each addition, the stirring speed is 100-500 revolutions per minute, and the stirring time is 1-24 hours. After adding isophorone diisocyanate, chain extender, and modifier (including cross-linking agent), stirring needs to be long enough according to the amount of additives to ensure that the additives can achieve a high reaction rate.

[0013] Step 2, adding a crosslinking agent to the mixed solution obtained in step 1, pouring it into a mold after being evenly dispersed, removing the solvent to obtain an uncured product, then raising the temperature to 140-180° C. and keeping it for 5-10 hours, and then naturally cooling it to room temperature to obtain a crosslinked product; the amount of the crosslinking agent is 0.1-3 parts by weight;

[0014] In step 2, stirring is used for uniform dispersion, the stirring speed is 100-500 revolutions per minute, and the stirring time is 2-6 hours.

[0015] In step 2, the crosslinking agent is tetramethoxysilane (TMS), tetramethoxysilane (TES), methyltrimethoxysilane (MTMS), N,N'-bis[3-(trimethoxysilyl)propyl]ethylenediamine (AES), preferably N,N'-bis[3-(trimethoxysilyl)propyl]ethylenediamine (AES).

[0016] In step 2, the mixed solution is poured into a mold and placed in a vacuum oven at 60-80° C. for 16-24 hours to remove the solvent to obtain an uncured product.

[0017] In step 2, the reaction is carried out under an inert protective atmosphere, wherein the inert protective atmosphere is one of nitrogen, helium or argon, preferably nitrogen.

[0018] Step 3, loading the cross-linked product obtained in step 2 into a mold, hot pressing at a temperature of 140-180° C. and a pressure of 8-12 MPa to promote cross-linking, and demolding after natural cooling to room temperature to obtain the target elastomer (i.e., the polysiloxane elastomer material of the present invention).

[0019] In step 3, the hot pressing time is 30-120 minutes.

[0020] In step 3, the mold size is 100×100×2mm 3 .

[0021] The technical solution of the present invention can improve the mechanical properties of polysiloxane elastomers. First, amino-terminated polysiloxane (PDMS) is reacted with isophorone diisocyanate (IPDI) to obtain polysiloxane long chains, and hydrogen bonds are introduced into the material as sacrificial bonds to enhance the mechanical properties. Then, dynamic silyl ether bonds are used to form a dynamic cross-linking network inside the material to prepare a polysiloxane elastomer material with good mechanical properties, thermal stability and reprocessability. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] Figure 1 The infrared spectra of the raw materials of the present invention, namely, isophorone diisocyanate, aminopropyl-terminated polydimethylsiloxane, N,N'-bis[3-(trimethoxysilyl)propyl]ethylenediamine and the product of Example 1.

[0023] Figure 2 It is the infrared spectrum chart of Example 1, Example 2, Example 3 and Example 4 of the present invention.

[0024] Figure 3 It is a schematic diagram of the dissolution test results of Example 1, Example 2, Example 3, Example 4 and Comparative Example 1 of the present invention in tetrahydrofuran.

[0025] Figure 4It is a uniaxial stretching curve diagram of Example 1, Example 2, Example 3, Example 4 and Comparative Example 1 of the present invention.

[0026] Figure 5 This is a uniaxial stretching curve diagram of Example 3 of the present invention at the beginning and after different times of recycling.

[0027] Figure 6 It is a thermogravimetric curve diagram of Example 1, Example 2, Example 3, Example 4 and Comparative Example 1 of the present invention. DETAILED DESCRIPTION

[0028] In order to better understand the present invention, the present invention is further described below in conjunction with the accompanying drawings and examples, but the embodiments of the present invention are not limited thereto. The main raw materials used are shown in the following table:

[0029]

[0030]

[0031] The main equipment and instruments used are shown in the following table:

[0032] name model Manufacturer Electronic balance AL104 Mettler-Toledo Instruments Ltd. Electric vacuum drying oven DZG-401B Tianjin Tianyu Experimental Instrument Co., Ltd. Electric heating blast drying oven DGG-101-0B Tianjin Tianyu Experimental Instrument Co., Ltd. High temperature hydraulic forming machine YJ450 Yuyao Huacheng Hydraulic and Electrical Co., Ltd. Heat collecting constant temperature heating magnetic stirrer DF-101S Gongyi Yingyu High-tech Instrument Factory Universal tensile testing machine M350-20KN Testometric Thermogravimetric Analyzer STA449f3 Netzsch

[0033] Example 1

[0034] Step 1, dissolve 2.0 g of aminopropyl-terminated polydimethylsiloxane in 5 mL of tetrahydrofuran, disperse evenly by ultrasonication, add the solution into a sealed three-necked flask filled with nitrogen, and stir for later use.

[0035] Step 2, dissolve 0.5113 g of isophorone diisocyanate in 5 mL of tetrahydrofuran, disperse evenly by ultrasonication, heat the solution into the solution obtained in step 1, and stir for 1 hour to allow for sufficient reaction.

[0036] Step 3, adding 0.0373 g of 3,3'-(1,1,3,3-tetramethyl-1,3-disiloxy)bis(1-propylamine) to the solution prepared in step 2, and continuing stirring for 24 hours, and reacting at room temperature throughout the process;

[0037] Step 4, add 0.0273 g of 3-amino-1,2-propanediol dropwise to the uniform solution obtained in step 3, and continue stirring evenly for 5 hours;

[0038] Step 5, add 0.0038 g of N,N'-bis[3-(trimethoxysilyl)propyl]ethylenediamine to the solution obtained in step 4, continue stirring for 1 hour, pour the mixed solution into a tetrafluoroethylene mold, place it in a 60°C vacuum oven for 12 hours to remove the solvent, and obtain an uncured product; then increase the temperature to 160°C and heat cure for 6 hours; finally, cool the sample naturally to room temperature to obtain a cross-linked product.

[0039] Step 6, loading the cross-linked product obtained in step 5 into a mold, hot pressing for 1 hour at a temperature of 160° C. and a pressure of 10 MPa to promote cross-linking, and demolding after natural cooling to room temperature to obtain the target elastomer, recorded as PDMS-1.

[0040] Example 2

[0041] Step 1, dissolve 2.0 g of aminopropyl-terminated polydimethylsiloxane in 5 mL of tetrahydrofuran, disperse evenly by ultrasonication, add the solution into a sealed three-necked flask filled with nitrogen, and stir for later use.

[0042] Step 2, dissolve 0.5113 g of isophorone diisocyanate in 5 mL of tetrahydrofuran, disperse evenly by ultrasonication, heat the solution into the solution obtained in step 1, and stir for 1 hour to allow for sufficient reaction.

[0043] Step 3, adding 0.0373 g of 3,3'-(1,1,3,3-tetramethyl-1,3-disiloxy)bis(1-propylamine) to the solution prepared in step 2, and continuing stirring for 24 hours, and reacting at room temperature throughout the process;

[0044] Step 4, add 0.0273 g of 3-amino-1,2-propanediol dropwise to the uniform solution obtained in step 3, and continue stirring evenly for 5 hours;

[0045] Step 5, add 0.0115g of N,N'-bis[3-(trimethoxysilyl)propyl]ethylenediamine to the solution obtained in step 4, continue stirring for 1h, pour the mixed solution into a tetrafluoroethylene mold, place it in a 60°C vacuum oven for 12h to remove the solvent, and obtain an uncured product; then increase the temperature to 160°C and heat cure for 6h; finally, cool the sample naturally to room temperature to obtain a cross-linked product.

[0046] Step 6, loading the cross-linked product obtained in step 5 into a mold, hot pressing for 1 h at a temperature of 160° C. and a pressure of 10 MPa to promote cross-linking, and demolding after natural cooling to room temperature to obtain the target elastomer, recorded as PDMS-2.

[0047] Example 3

[0048] Step 1, dissolve 2.0 g of aminopropyl-terminated polydimethylsiloxane in 5 mL of tetrahydrofuran, disperse evenly by ultrasonication, add the solution into a sealed three-necked flask filled with nitrogen, and stir for later use.

[0049] Step 2, dissolve 0.5113 g of isophorone diisocyanate in 5 mL of tetrahydrofuran, disperse evenly by ultrasonication, heat the solution into the solution obtained in step 1, and stir for 1 hour to allow for sufficient reaction.

[0050] Step 3, adding 0.0373 g of 3,3'-(1,1,3,3-tetramethyl-1,3-disiloxy)bis(1-propylamine) to the solution prepared in step 2, and continuing stirring for 24 hours, and reacting at room temperature throughout the process;

[0051] Step 4, add 0.0273 g of 3-amino-1,2-propanediol dropwise to the uniform solution obtained in step 3, and continue stirring evenly for 5 hours;

[0052] Step 5, add 0.0192 g of N,N'-bis[3-(trimethoxysilyl)propyl]ethylenediamine to the solution obtained in step 4, continue stirring for 1 hour, pour the mixed solution into a tetrafluoroethylene mold, place it in a 60°C vacuum oven for 12 hours to remove the solvent, and obtain an uncured product; then increase the temperature to 160°C and heat cure for 6 hours; finally, cool the sample naturally to room temperature to obtain a cross-linked product.

[0053] Step 6, loading the cross-linked product obtained in step 5 into a mold, hot pressing for 1 h at a temperature of 160° C. and a pressure of 10 MPa to promote cross-linking, and demolding after natural cooling to room temperature to obtain the target elastomer, recorded as PDMS-3.

[0054] Example 4

[0055] Step 1, dissolve 2.0 g of aminopropyl-terminated polydimethylsiloxane in 5 mL of tetrahydrofuran, disperse evenly by ultrasonication, add the solution into a sealed three-necked flask filled with nitrogen, and stir for later use.

[0056] Step 2, dissolve 0.5113 g of isophorone diisocyanate in 5 mL of tetrahydrofuran, disperse evenly by ultrasonication, heat the solution into the solution obtained in step 1, and stir for 1 hour to allow for sufficient reaction.

[0057] Step 3, adding 0.0373 g of 3,3'-(1,1,3,3-tetramethyl-1,3-disiloxy)bis(1-propylamine) to the solution prepared in step 2, and continuing stirring for 24 hours, and reacting at room temperature throughout the process;

[0058] Step 4, add 0.0273 g of 3-amino-1,2-propanediol dropwise to the uniform solution obtained in step 3, and continue stirring evenly for 5 hours;

[0059] Step 5, add 0.0269 g of N,N'-bis[3-(trimethoxysilyl)propyl]ethylenediamine to the solution obtained in step 4, continue stirring for 1 hour, pour the mixed solution into a tetrafluoroethylene mold, place it in a 60°C vacuum oven for 12 hours to remove the solvent, and obtain an uncured product; then increase the temperature to 160°C and heat cure for 6 hours; finally, cool the sample naturally to room temperature to obtain a cross-linked product.

[0060] Step 6, loading the cross-linked product obtained in step 5 into a mold, hot pressing for 1 h at a temperature of 160° C. and a pressure of 10 MPa to promote cross-linking, and demolding after natural cooling to room temperature to obtain the target elastomer, recorded as PDMS-4.

[0061] Comparative Example 1

[0062] The raw materials were gradually added according to the steps of Example 1 to react, but the N,N'-bis[3-(trimethoxysilyl)propyl]ethylenediamine crosslinking agent was not added to prepare a control example of the elastomer, which was recorded as PDMS-0. From Example 1 (PDMS-1) to Example 4 (PDMS-4), the mass ratio of N,N'-bis[3-(trimethoxysilyl)propyl]ethylenediamine was 1:3:5:7.

[0063] Figure 1 The infrared spectra of the raw materials IPDI, APDMS, TED, and PDMS-1 are shown. In the infrared spectrum of IPDI, 2270 cm -1 The characteristic absorption peak at 2270 cm is attributed to the isocyanate group. However, in the infrared spectrum of PDMS-1, -1 The absorption peak at 3340 cm -1 and 1570cm -1 The stretching vibration and bending vibration absorption peaks of NH in the newly generated urea bond appeared respectively. These changes indicate the successful reaction of the amino group with the isocyanate group, proving the successful progress of steps 1-3 to obtain a long polysiloxane chain.

[0064] Figure 2 The infrared spectra of Example 1, Example 2, Example 3 and Example 4 are shown in Figure 1. At 1025 cm -1 The broad peak at 1074 cm corresponds to the stretching vibration of Si-O-Si in aminopropyl polysiloxane, while the characteristic absorption peak of silyl ether bond (Si-OC) should be located at 1074 cm -1 The absorption peak of the siloxane main chain structure interferes with the formation of silyl ether bonds by infrared spectroscopy. Therefore, swelling experiments are required to study the cross-linking process. Figure 3 The swelling test diagrams of Example 1, Example 2, Example 3, Example 4 and Comparative Example 1 are shown. The samples were immersed in tetrahydrofuran solvent for 24 hours, and the cross-linking structure was evaluated by the swelling degree of the samples before and after immersion. Since no cross-linking agent (N, N'-bis[3-(trimethoxysilyl)propyl]ethylenediamine) was added to Comparative Example 1, no silyl ether cross-linking network was formed in the system, and the sample was completely dissolved in tetrahydrofuran; while Example 1, Example 2, Example 3, and Example 4 only swelled, and the sample shape remained intact, indicating that the cross-linking agent underwent an exchange reaction in the system to form a silyl ether bond.

[0065] Figure 4 The uniaxial tensile curves of the comparative example and the embodiment are shown in the figure. The curves show that the tensile strength and elongation at break of the elastomer can be regulated by adding the crosslinking agent N,N'-bis[3-(trimethoxysilyl)propyl]ethylenediamine to the system. As the content of the crosslinking agent increases, the tensile strength of the elastomer gradually increases; while the elongation at break increases first and then decreases, among which PDMS-3 has the best mechanical properties, as shown in the following table.

[0066] Stress(MPa) strain(%) Comparative Example 1 4.49 262 Example 1 5.64 276 Example 2 7.10 364 Example 3 10.03 402 Example 4 10.98 233

[0067] Figure 5 The uniaxial tensile curve after reprocessing of Example 3. The elastomer prepared in Example 3 was cut into pieces and placed in a mold, and then hot-pressed in a high-temperature hydraulic molding machine (hot-pressing conditions: 160°C, 10MPa, 2h), and then the reprocessed elastomer was obtained, and its mechanical properties were tested by uniaxial tensile test. The hot pressing was repeated three times using the same method, and its mechanical properties were tested after each hot pressing. Figure 5 It shows that Example 3 has good reprocessability. Even after three consecutive processings, its tensile strength can still reach 78% of the initial sample, indicating that the introduction of dynamic silyl ether bonds gives the elastomer good reprocessability, as shown in the following table.

[0068]

[0069] Figure 6 The thermal weight loss curves of the comparative example and the example are shown in Figure 2. The sample was heated from 40°C to 700°C at a rate of 10°C / min under an argon atmosphere, and the mass change of the sample during the heating process was observed to evaluate its thermal stability. The main indicators are the temperature corresponding to the loss of 5% of the sample mass (T5), the temperature corresponding to the loss of 10% (T 10 ), detailed data are shown in the following table:

[0070] <![CDATA[T5(℃)]]> <![CDATA[T 10 (℃)]]> Comparative Example 1 280.0 309.6 Example 1 314.2 329.4 Example 2 319.4 333.8 Example 3 322.2 335.0 Example 4 314.6 328.2

[0071] T5 is usually used as an important indicator to measure the thermal stability of materials (initial thermal degradation temperature). The test results show that the examples containing silyl ether bond cross-linking structures have higher T5 than the comparative examples without silyl ether bonds, especially the T5 of Example 3 is increased by about 42°C; 10 It also shows a similar pattern. The T 10 The temperature was increased by about 25°C compared with Comparative Example 1. The thermogravimetric results show that the introduction of silyl ether bonds into the long chain of linear polysiloxane significantly improves the thermal stability of the material.

[0072] According to the content of the present invention, the process parameters can be adjusted to achieve the preparation of polysiloxane elastomer materials, and after testing, the performance is basically consistent with that of the present invention. The above is an exemplary description of the present invention. It should be noted that any simple deformation, modification or other equivalent replacement that can be made by other technicians in this field without spending creative labor falls within the protection scope of the present invention without departing from the core of the present invention.

Claims

1. A high-performance polysiloxane elastomer based on silyl ether bonds, characterized in that: Follow the steps below: Step 1, uniformly dispersing the amino-terminated polysiloxane in a solvent, and sequentially adding diisocyanate, chain extender and modifier under an inert protective atmosphere and reacting them fully, wherein the amount of the amino-terminated polysiloxane is 100 parts by weight, the amount of the diisocyanate is 20-30 parts by weight, the amount of the chain extender is 1-5 parts by weight, and the modifier is 0.5-3 parts by weight; the diisocyanate is toluene diisocyanate, isophorone diisocyanate, diphenylmethane diisocyanate, dicyclohexylmethyl One of alkane diisocyanate, hexamethylene diisocyanate or lysine diisocyanate; the chain extender is one of 3,3'-(1,1,3,3-tetramethyl-1,3-disiloxy)bis(1-propylamine), 1,4-ethylenediamine, 1,6-hexanediamine or 1,4-butanediol; the modifier is one of 2-aminoethanol, 3-amino-1,2-propylene glycol, 2-amino-1,3-propylene glycol; the inert protective atmosphere is one of nitrogen, helium or argon; Step 2, adding a crosslinking agent to the mixed solution obtained in step 1, pouring it into a mold after being evenly dispersed, removing the solvent to obtain an uncured product, then raising the temperature to 140-180° C. and keeping it for 5-10 hours, and then naturally cooling it to room temperature to obtain a crosslinked product; the amount of the crosslinking agent is 0.1-3 parts by weight; the crosslinking agent is tetramethoxysilane, methyltrimethoxysilane or N,N'-bis[3-(trimethoxysilyl)propyl]ethylenediamine; Step 3, loading the cross-linked product obtained in step 2 into a mold, hot pressing at a temperature of 140-180° C. and a pressure of 8-12 MPa to promote cross-linking, and demolding after naturally cooling to room temperature to obtain the polysiloxane elastomer material.

2. A high-performance polysiloxane elastomer based on silyl ether bonds according to claim 1, characterized in that: In step 1, the amount of amino-terminated polysiloxane is 100 parts by weight, the amount of diisocyanate is 25-30 parts by weight, the amount of chain extender is 1-3 parts by weight, and the amount of modifier is 1-3 parts by weight.

3. The high-performance polysiloxane elastomer based on silyl ether bonds according to claim 1, characterized in that: In step 1, the amino-terminated polysiloxane is aminopropyl-terminated polydimethylsiloxane, the diisocyanate is isophorone diisocyanate, the chain extender is 3,3'-(1,1,3,3-tetramethyl-1,3-disiloxy)bis(1-propylamine), and the modifier is 3-amino-1,2-propylene glycol; stirring is used to uniformly disperse and react each addition, the stirring speed is 100-500 revolutions per minute, and the stirring time is 1-24 hours.

4. The high-performance polysiloxane elastomer based on silyl ether bonds according to claim 1, characterized in that: In step 2, stirring is used for uniform dispersion, the stirring speed is 100-500 revolutions per minute, and the stirring time is 2-6 hours; the crosslinking agent is N,N'-bis[3-(trimethoxysilyl)propyl]ethylenediamine; the mixed solution is poured into a mold, and placed in a vacuum oven at 60-80°C for 16-24 hours to remove the solvent to obtain an uncured product; the reaction is carried out under an inert protective atmosphere, and the inert protective atmosphere is one of nitrogen, helium or argon.

5. The high-performance polysiloxane elastomer based on silyl ether bonds according to claim 1, characterized in that: In step 3, the hot pressing time is 30-120 minutes, and the mold size is 100×100×2mm 3 .

6. A method for preparing a high-performance polysiloxane elastomer based on a silyl ether bond, characterized in that: Follow the steps below: Step 1, uniformly dispersing the amino-terminated polysiloxane in a solvent, and sequentially adding diisocyanate, chain extender and modifier under an inert protective atmosphere and reacting them fully, wherein the amount of the amino-terminated polysiloxane is 100 parts by weight, the amount of the diisocyanate is 20-30 parts by weight, the amount of the chain extender is 1-5 parts by weight, and the modifier is 0.5-3 parts by weight; the diisocyanate is toluene diisocyanate, isophorone diisocyanate, diphenylmethane diisocyanate, dicyclohexylmethyl One of alkane diisocyanate, hexamethylene diisocyanate or lysine diisocyanate; the chain extender is one of 3,3'-(1,1,3,3-tetramethyl-1,3-disiloxy)bis(1-propylamine), 1,4-ethylenediamine, 1,6-hexanediamine or 1,4-butanediol; the modifier is one of 2-aminoethanol, 3-amino-1,2-propylene glycol, 2-amino-1,3-propylene glycol; the inert protective atmosphere is one of nitrogen, helium or argon; Step 2, adding a crosslinking agent to the mixed solution obtained in step 1, pouring it into a mold after being evenly dispersed, removing the solvent to obtain an uncured product, then raising the temperature to 140-180° C. and keeping it for 5-10 hours, and then naturally cooling it to room temperature to obtain a crosslinked product; the amount of the crosslinking agent is 0.1-3 parts by weight; the crosslinking agent is tetramethoxysilane, methyltrimethoxysilane or N,N'-bis[3-(trimethoxysilyl)propyl]ethylenediamine; Step 3, loading the cross-linked product obtained in step 2 into a mold, hot pressing at a temperature of 140-180° C. and a pressure of 8-12 MPa to promote cross-linking, and demolding after naturally cooling to room temperature to obtain the polysiloxane elastomer material.

7. The method for preparing a high-performance polysiloxane elastomer based on silyl ether bonds according to claim 6, characterized in that: In step 1, the amount of amino-terminated polysiloxane is 100 parts by weight, the amount of diisocyanate is 25-30 parts by weight, the amount of chain extender is 1-3 parts by weight, and the amount of modifier is 1-3 parts by weight.

8. The method for preparing a high-performance polysiloxane elastomer based on silyl ether bonds according to claim 6, characterized in that: In step 1, the amino-terminated polysiloxane is aminopropyl-terminated polydimethylsiloxane, the diisocyanate is isophorone diisocyanate, the chain extender is 3,3'-(1,1,3,3-tetramethyl-1,3-disiloxy)bis(1-propylamine), and the modifier is 3-amino-1,2-propylene glycol; stirring is used to uniformly disperse and react each addition, the stirring speed is 100-500 revolutions per minute, and the stirring time is 1-24 hours.

9. The method for preparing a high-performance polysiloxane elastomer based on silyl ether bonds according to claim 6, characterized in that: In step 2, stirring is used for uniform dispersion, the stirring speed is 100-500 revolutions per minute, and the stirring time is 2-6 hours; the crosslinking agent is N,N'-bis[3-(trimethoxysilyl)propyl]ethylenediamine; the mixed solution is poured into a mold, and placed in a vacuum oven at 60-80°C for 16-24 hours to remove the solvent to obtain an uncured product; the reaction is carried out under an inert protective atmosphere, and the inert protective atmosphere is one of nitrogen, helium or argon.

10. The method for preparing a high-performance polysiloxane elastomer based on silyl ether bonds according to claim 6, characterized in that: In step 3, the hot pressing time is 30-120 minutes, and the mold size is 100×100×2mm 3 .

Citation Information

Patent Citations

  • Reversible covalent crosslinking polysiloxane elastomer, preparation method therefor and application thereof

    CN105111470A

  • Preparation method of thermosetting polymer capable of being welded, repaired and reprocessed for shaping under moderate temperature

    CN109762139A