Waterproof organic silica gel and preparation method thereof

By introducing composite micro-nanofiber materials and bio-waterproofing agents into the silicone gel, a high-density mesh structure and micro-nano roughness are formed, the hydrophobicity and adhesion of the silicone gel are solved, and the waterproof performance and adhesion in rainwater environments are improved, and it is suitable for instruments and meters.

CN120442056APending Publication Date: 2025-08-08THREE GORGES JINSHAJIANG CHUANYUN HYDROPOWER DEV CO LTD
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Patent Information

Application Number
CN202510765282.2
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-06-10
Publication Date
2025-08-08

AI Technical Summary

Technical Problem

The hydrophobic properties of existing silicone gels are unstable and are prone to fall off or damage, and cannot meet the waterproof requirements of instruments and instruments in rainwater environments.

Method used

Compound micro-nanofiber materials are introduced into silicone gels, and bio-waterproofing agents are uniformly sprayed on their surfaces to form high-density mesh structures and micro-nano roughness, enhancing waterproofing performance and adhesion.

Benefits of technology

It realizes the stable waterproof performance and excellent adhesion of silicone gel under rainwater conditions, meets the waterproof requirements of instruments and meters, and has a wide range of application prospects.

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Abstract

The invention relates to the technical field of gel materials, in particular to waterproof organosilicone gel and a preparation method thereof.The waterproof organosilicone gel is prepared from a component A, a component B and a component C in parts by weight; the component A is prepared from 10 to 50 parts of vinyl silicone oil, 5 to 30 parts of terminated hydrogen-containing silicone oil, 1 to 10 parts of hydrogen-containing silicone oil and 0.1 to 0.8 part of inhibitor; the component B is prepared from the following components in parts by weight: 80 to 120 parts of vinyl silicone oil and 0.01 to 0.15 part of platinum catalyst; and the component C comprises 5-10 parts of a composite micro-nano fiber material and 10-30 parts of a biological waterproof agent. According to the invention, the composite micro-nano fibers are added into the organic silica gel and the biological waterproof agent is sprayed, so that the water resistance and adhesion of the organic silica gel are remarkably improved, and the organic silica gel can meet the waterproof application requirements of instruments and meters in a rainwater environment.
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Description

Technical Field

[0001] The present invention relates to the technical field of gel materials, in particular to a waterproof organic silicone gel and a preparation method thereof. Background Art

[0002] Silicone gel is a very soft silicone rubber product that cures after curing. It exhibits the same characteristics as silicone rubber, including high and low temperature resistance, weather resistance, and physiological inertness. The curing principle of silicone gel is a hydrosilylation reaction. After curing, silicone gel does not release small molecules and does not shrink in volume. Its curing speed is solely dependent on temperature, and it can be cured at room temperature or heated. It is easy to use and has found widespread application in electronics, IGBTs, display screens, and medical applications.

[0003] For example, the invention patent with publication number CN11 3583626A discloses a silicone gel and a preparation method thereof. The silicone gel comprises component A and component B in a mass ratio of 1:1, wherein component A comprises at least the following components in parts by mass: 50-80 parts of vinyl-terminated silicone oil; 10-30 parts of hydrogen-terminated silicone oil; 0.1-5 parts of cross-linked hydrogen silicone oil; and 0.2-1 parts of a tackifier. Component B comprises at least the following components in parts by mass: 99-99.99 parts of vinyl silicone oil; and 0.1-1 parts of a platinum catalyst. The tackifier is vinyltrimethoxysilane and / or vinyltriethoxysilane. The cross-linked hydrogen silicone oil comprises at least cross-linked hydrogen silicone oil A, wherein the hydrogen content of the cross-linked hydrogen silicone oil A is ≥1.2%, and the number of silicon-hydrogen bonds contained in the cross-linked hydrogen silicone oil A accounts for 50-100% of the number of silicon-hydrogen bonds contained in all cross-linked hydrogen silicone oils. The ratio of the number of silicon-hydrogen bonds to vinyl groups in the silicone gel system is >0.85. The silicone gel of the present application has both high hardness and adhesion, which effectively improves the overall bonding strength of the silicone gel; however, the hydrophobic properties of the silicone gel are unstable, and it is easy to fall off or be damaged, which cannot meet the working requirements of waterproofing of instruments and meters, resulting in limited application scope. Summary of the Invention

[0004] To address the problems existing in the prior art, the present invention aims to provide a waterproof organosilicon gel and a method for preparing the same. By introducing a composite micro-nanofiber material into the organosilicon gel and uniformly spraying a biorepellent on its surface, the present invention achieves excellent waterproof properties while significantly enhancing its adhesion. This allows the organosilicon gel to withstand normal use in rainy conditions, meeting waterproof requirements when used in instruments and meters, and has broad application prospects.

[0005] To achieve the above objectives, the present invention provides the following specific technical solutions:

[0006] A waterproof organic silicone gel, which is prepared from component A, component B and component C;

[0007] In parts by weight, the component A comprises: 10-50 parts of vinyl silicone oil, 5-30 parts of terminal hydrogen silicone oil, 1-10 parts of hydrogen-containing silicone oil, and 0.1-0.8 parts of inhibitor;

[0008] The component B comprises: 80-120 parts of vinyl silicone oil and 0.01-0.15 parts of platinum catalyst;

[0009] The component C comprises: 5-10 parts of composite micro-nano fiber material and 10-30 parts of biological waterproofing agent.

[0010] As a further preferred embodiment of the present invention, in component A, the vinyl silicone oil is one or both of polydimethylsiloxane containing vinyl groups at both ends and polydimethylsiloxane containing vinyl groups at only one end and a non-reactive trimethylsilyl group at the other end;

[0011] The viscosity of the vinyl silicone oil is 100-20000 mPa·s, and the vinyl content is 1-8%;

[0012] As a further preferred embodiment of the present invention, in the component B, the vinyl silicone oil is one or both of polydimethylsiloxane containing vinyl groups at both ends and polydimethylsiloxane containing vinyl groups at only one end and a non-reactive trimethylsilyl group at the other end;

[0013] The viscosity of the vinyl silicone oil is 100-20000 mPa·s, and the vinyl content is 1-8%.

[0014] As a further preferred embodiment of the present invention, the viscosity of the hydrogen-terminated silicone oil is 1-1000 mPa·s and the hydrogen content is 0.5-3.0%;

[0015] The hydrogen-containing silicone oil has a viscosity of 1-1000 mPa·s and a hydrogen content of 0.5-2.0%;

[0016] The inhibitor is selected from at least one of tetramethyltetravinylcyclotetrasiloxane, polyvinylpolysiloxane, 3-methyl-1-pentyn-3-ol, and 1-ethynyl-1-cyclohexanol;

[0017] The platinum catalyst is selected from at least one of chloroplatinic acid and tetramethyldivinyldisiloxane coordinated platinum catalysts.

[0018] As a further preferred embodiment of the present invention, the preparation method of the composite micro-nano fiber material is as follows:

[0019] 1) adding polyester polyurethane and polyethylene glycol octylphenyl ether to N,N-dimethylformamide, stirring at room temperature for 15-20 hours to obtain a spinning solution, electrospinning the spinning solution, and drying the obtained spun fibers to obtain a fiber material;

[0020] 2) adding dehydrated hexafluorobutyl methacrylate to a reaction vessel and stirring, then adding glycidyl methacrylate, ethyl 2-bromoisobutyrate, copper bromide, and pentamethyldiethylenetriamine, introducing nitrogen for 5-15 minutes, and reacting at 80-85° C. for 2-5 hours to obtain a fluorinated acrylate solution;

[0021] 3) Immersing the fiber material in a fluorinated acrylate solution at room temperature at a mass-to-volume ratio of 1 g: (30-50) mL for 20-30 seconds, removing the fiber material from the solution, drying the solution, and then immersing the fiber material in the fluorinated acrylate solution again. Repeating this operation 3-5 times, the composite micro-nano fiber material is obtained.

[0022] As a further preferred embodiment of the present invention, in the spinning solution, the ratio of polyester polyurethane, polyethylene glycol octylphenyl ether, and N,N-dimethylformamide is (15-20) g: (3-7) g: (120-150) mL;

[0023] The electrospinning parameters are as follows: spinning voltage of 40-60 kV, receiving distance of 10-15 cm, and liquid feeding speed of 0.2-0.5 m / min.

[0024] As a further preferred embodiment of the present invention, the mass ratio of hexafluorobutyl methacrylate, glycidyl methacrylate, ethyl 2-bromoisobutyrate, copper bromide, and pentamethyldiethylenetriamine is (10-15): (3-4): (0.1-0.3): (0.001-0.005): (0.03-0.07).

[0025] As a further preferred embodiment of the present invention, the preparation method of the biological waterproofing agent is as follows:

[0026] 1) Choline chloride and oxalic acid are mixed in a molar ratio of 1:1, placed in an 80-85°C oil bath, and magnetically stirred until a clear liquid is obtained. The oil bath is then heated to 100-105°C, and bean curd residue is added to the clear liquid in a solid-liquid mass ratio of 1:(18-25). The mixture is stirred for 40-60 minutes, and filtered to obtain a solid.

[0027] 2) adding the solid, deionized water, acetic acid, and sodium chlorite to a container and magnetically stirring at a constant temperature of 75-78° C. for 1-3 hours. After the reaction is completed, cellulose is precipitated using distilled water as a reverse-phase solvent and high-pressure homogenized at 60-70 MPa for 15-20 times using distilled water as a solvent to prepare a suspension with a concentration of 1-3 wt %, which is then refrigerated for later use;

[0028] 3) adding an alkyl ketene dimer emulsion having a concentration of 15-18 wt % to the suspension, magnetically stirring for 30-50 min, then adding calcium carbonate in an amount of 0.1-0.8% by mass of the suspension, and adjusting the total volume to 30-50 mL with deionized water. After magnetic stirring for 30-50 min, ultrasonic treatment was performed for 15-30 min to obtain a uniformly mixed biowaterproofing agent.

[0029] As a further preferred embodiment of the present invention, the usage ratio of the solid, deionized water, acetic acid, and sodium chlorite is (2-5) g: (40-100) mL: (0.5-1.5) mL: (0.6-1.8) g;

[0030] The mass ratio of the alkyl ketene dimer emulsion to the suspension is 1:(80-100).

[0031] A method for preparing a waterproof silicone gel comprises the following steps:

[0032] Vinyl silicone oil, terminal hydrogen silicone oil, hydrogen-containing silicone oil and inhibitor are mixed in parts by weight to obtain component A; vinyl silicone oil and platinum catalyst are mixed to obtain component B; component A, component B and composite micro-nano fiber material are mixed and solidified, and then a biological waterproofing agent is evenly sprayed on the surface to obtain a waterproof silicone gel.

[0033] Compared with the prior art, the present invention has the following beneficial effects:

[0034] In the present invention, polyester polyurethane is used as the main raw material, polyethylene glycol octylphenyl ether is added as an auxiliary agent, and a needle-free electrospinning machine is used to prepare a fiber material. The fiber material is subjected to surface hydrophobic treatment with the prepared fluorine-containing acrylate solution by pulling and impregnating, thereby obtaining a composite micro-nano fiber material with waterproof performance. In the electrospinning process, polyethylene glycol octylphenyl ether is a non-ionic surfactant that can reduce the viscosity of the spinning solution and form a connected sheet structure on the surface of the material, thereby alleviating the uneven spinning, fiber shrinkage, and curling phenomena of the polyester polyurethane in the electrospinning process, so that the obtained fiber material has a uniform structure and a good morphology. Moreover, the introduction of polyethylene glycol octylphenyl ether does not destroy the molecular structure of the polyester polyurethane. structure, thereby improving the contact angle, hydrostatic pressure and breaking strength of the fiber material, thereby further improving the waterproof performance and mechanical properties of the composite micro-nano fiber material; by introducing the composite micro-nano fiber material into the silicone gel, a high-density network structure is formed through the entanglement and cross-linking of the composite micro-nano fiber material, and the formed waterproof network structure forms a hydrophobic network inside the silicone gel, preventing water from penetrating into the silicone gel, thereby making the silicone gel have stable hydrophobicity, which can meet normal use under rainy conditions, so that when it is used in instruments and meters, it can meet the waterproof requirements. At the same time, the high-density network structure also further improves the bonding strength of the silicone gel, making it have excellent adhesion.

[0035] In the present invention, bean dregs nanofibers are also used as a basis and hydrophobically modified with alkyl ketene dimer as a binder for precipitated calcium carbonate. After mechanical stirring and ultrasonic treatment, a biological waterproofing agent is obtained. By evenly spraying the biological waterproofing agent on the surface of the silicone gel, the bean dregs nanofibers can be wrapped on the surface of the calcium carbonate due to their high aspect ratio and curling, and can also form cross-linking connections with the composite micro-nano fiber material, playing the role of a "binder" between the calcium carbonate and the silicone gel, so that the roughness of the silicone gel surface is further increased, and the retention rate of calcium carbonate is increased. A large amount of retained calcium carbonate forms a micro-nano structure on the silicone surface, thereby greatly increasing the micro-nano roughness of the silicone gel surface, thereby achieving a super-hydrophobic effect, which can effectively prevent the intrusion of external water and further improve the waterproof performance of the silicone gel.

[0036] In the present invention, by introducing a composite micro-nano fiber material into the silicone gel and uniformly spraying a biological waterproofing agent on its surface, the silicone gel not only has excellent waterproof performance, but also has significantly improved adhesion, which can meet normal use under rain conditions. When it is used in instruments and meters, it can meet the waterproof requirements and has broad application prospects. DETAILED DESCRIPTION

[0037] The following is a clear and complete description of the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection of the present invention.

[0038] In the present invention, 5 not explicitly stated indicates mass percentage, i.e., wt%.

[0039] In the embodiment of the present invention, the vinyl silicone oil in component A is polydimethylsiloxane containing vinyl groups at both ends, with a viscosity of 20,000 mPa·s and a vinyl content of 8%;

[0040] The vinyl silicone oil in component B is a polydimethylsiloxane with a vinyl group at one end and a non-reactive trimethylsilyl group at the other end, with a viscosity of 20,000 mPa·s and a vinyl content of 8%.

[0041] The viscosity of the hydrogen-terminated silicone oil is 1000 mPa·s and the hydrogen content is 3.0%;

[0042] The viscosity of hydrogenated silicone oil is 1000 mPa·s and the hydrogen content is 2.0%;

[0043] The inhibitor is selected from tetramethyltetravinylcyclotetrasiloxane;

[0044] The platinum catalyst is selected from chloroplatinic acid.

[0045] Example 1

[0046] A waterproof organic silicone gel, which is prepared from component A, component B and component C;

[0047] In parts by weight, component A includes: 10 parts of vinyl silicone oil, 5 parts of terminal hydrogen silicone oil, 1 part of hydrogen-containing silicone oil, and 0.1-0.8 parts of inhibitor;

[0048] Component B includes: 80 parts of vinyl silicone oil and 0.01 parts of platinum catalyst;

[0049] Component C includes: 5 parts of composite micro-nano fiber material and 10 parts of biological waterproofing agent;

[0050] The preparation method of the waterproof organic silicone gel specifically comprises the following steps:

[0051] Vinyl silicone oil, terminal hydrogen silicone oil, hydrogen-containing silicone oil and inhibitor are mixed in parts by weight to obtain component A; vinyl silicone oil and platinum catalyst are mixed to obtain component B; component A, component B and composite micro-nano fiber material are mixed and cured; and then a biological waterproofing agent is evenly sprayed on the surface to obtain a waterproof silicone gel.

[0052] The preparation method of the composite micro-nano fiber material is as follows:

[0053] 1) adding 15 g of polyester polyurethane and 3 g of polyethylene glycol octylphenyl ether to 120 mL of N,N-dimethylformamide, stirring the mixture at room temperature for 15 h to obtain a spinning solution, and subjecting the spinning solution to electrospinning at a spinning voltage of 40 kV, a receiving distance of 10 cm, and a liquid feeding speed of 0.2 m / min. The obtained spun fibers were dried to obtain a fiber material;

[0054] 2) Add 10 g of dehydrated hexafluorobutyl methacrylate to a reaction vessel and stir, then add 3 g of glycidyl methacrylate, 0.1 g of ethyl 2-bromoisobutyrate, 0.001 g of copper bromide, and 0.03 g of pentamethyldiethylenetriamine, introduce nitrogen for 5 minutes, and react at 80° C. for 2 hours to obtain a fluorinated acrylate solution;

[0055] 3) Immersing the fiber material in a fluorinated acrylate solution at room temperature at a mass-to-volume ratio of 1 g:30 mL for 20 seconds, removing the fiber material from the solution, drying the solution, and then immersing the fiber material in the fluorinated acrylate solution again. Repeating this operation three times yields a composite micro-nano fiber material.

[0056] The preparation method of the biological waterproofing agent is as follows:

[0057] 1) Choline chloride and oxalic acid were mixed in a molar ratio of 1:1, placed in an 80°C oil bath, and magnetically stirred at 300 rpm until a clear liquid was obtained. The oil bath was then heated to 100°C, and bean curd residue was added to the clear liquid at a solid-liquid mass ratio of 1:18. The mixture was stirred for 40 minutes, and the solid was filtered to obtain a solid.

[0058] 2) 2 g of the solid, 40 mL of deionized water, 0.5 mL of acetic acid, and 0.6 g of sodium chlorite were added to a container and magnetically stirred at 75° C. for 1 h. After the reaction, cellulose was precipitated using distilled water as a reverse-phase solvent and high-pressure homogenized 15 times at 60 MPa using distilled water as the solvent to prepare a 1 wt% suspension, which was then refrigerated for later use.

[0059] 3) Adding a 15 wt% alkyl ketene dimer emulsion to the suspension at a mass ratio of 1:80, magnetically stirring for 30 min, then adding calcium carbonate at 0.1% of the mass of the suspension, and adjusting the total volume to 30 mL with deionized water. After magnetic stirring at 400 r / min for 30 min, ultrasonic treatment at 200 W for 15 min was performed to obtain a uniformly mixed biowaterproofing agent.

[0060] Example 2

[0061] A waterproof organic silicone gel, which is prepared from component A, component B and component C;

[0062] In parts by weight, component A includes: 35 parts of vinyl silicone oil, 20 parts of terminal hydrogen silicone oil, 5 parts of hydrogen silicone oil, and 0.5 parts of inhibitor;

[0063] Component B includes: 100 parts of vinyl silicone oil and 0.1 parts of platinum catalyst;

[0064] Component C includes: 7 parts of composite micro-nano fiber material and 20 parts of biological waterproofing agent;

[0065] The preparation method of the waterproof organic silicone gel specifically comprises the following steps:

[0066] Vinyl silicone oil, terminal hydrogen silicone oil, hydrogen-containing silicone oil and inhibitor are mixed in parts by weight to obtain component A; vinyl silicone oil and platinum catalyst are mixed to obtain component B; component A, component B and composite micro-nano fiber material are mixed and cured; and then a biological waterproofing agent is evenly sprayed on the surface to obtain a waterproof silicone gel.

[0067] The preparation method of the composite micro-nano fiber material is as follows:

[0068] 1) adding 18 g of polyester polyurethane and 5 g of polyethylene glycol octylphenyl ether to 140 mL of N,N-dimethylformamide, stirring the mixture at room temperature for 18 h to obtain a spinning solution, and subjecting the spinning solution to electrospinning at a spinning voltage of 50 kV, a receiving distance of 13 cm, and a liquid feeding speed of 0.3 m / min. The obtained spun fibers were dried to obtain a fiber material;

[0069] 2) Add 12 g of dehydrated hexafluorobutyl methacrylate to a reaction vessel and stir, then add 3.5 g of glycidyl methacrylate, 0.2 g of ethyl 2-bromoisobutyrate, 0.003 g of copper bromide, and 0.05 g of pentamethyldiethylenetriamine. After nitrogen is introduced for 10 minutes, react at 83° C. for 3 hours to obtain a fluorinated acrylate solution.

[0070] 3) Immersing the fiber material in a fluorinated acrylate solution at room temperature at a mass-to-volume ratio of 1 g:40 mL for 25 seconds, removing the fiber material from the solution, drying the solution, and then immersing the fiber material in the fluorinated acrylate solution again. Repeating this operation four times yields a composite micro-nano fiber material.

[0071] The preparation method of the biological waterproofing agent is as follows:

[0072] 1) Choline chloride and oxalic acid were mixed in a molar ratio of 1:1, placed in an 83°C oil bath, and magnetically stirred at 400 rpm until a clear liquid was obtained. The oil bath was then heated to 103°C, and bean curd residue was added to the clear liquid in a solid-liquid mass ratio of 1:20. The mixture was stirred for 50 minutes, and the solid was filtered to obtain a solid.

[0073] 2) 3 g of the solid, 80 mL of deionized water, 1.0 mL of acetic acid, and 1.3 g of sodium chlorite were added to a container and magnetically stirred at 76° C. for 2 h. After the reaction, cellulose was precipitated using distilled water as a reverse-phase solvent and high-pressure homogenized 18 times at 65 MPa using distilled water as the solvent to prepare a 2 wt% suspension, which was then refrigerated for later use.

[0074] 3) Adding a 17 wt % alkyl ketene dimer emulsion to the suspension at a mass ratio of 1:90, magnetically stirring for 40 min, then adding calcium carbonate at a mass ratio of 0.5% of the suspension, adjusting the total volume to 40 mL with deionized water, and magnetically stirring at 500 rpm for 40 min, and then ultrasonically treating at 250 W for 20 min to obtain a uniformly mixed biowaterproofing agent.

[0075] Example 3

[0076] A waterproof organic silicone gel, which is prepared from component A, component B and component C in parts by weight;

[0077] Component A includes: 50 parts of vinyl silicone oil, 30 parts of terminal hydrogen silicone oil, 10 parts of hydrogen silicone oil, and 0.8 parts of inhibitor;

[0078] Component B includes: 120 parts of vinyl silicone oil and 0.15 parts of platinum catalyst;

[0079] Component C includes: 10 parts of composite micro-nano fiber material and 30 parts of biological waterproofing agent;

[0080] The preparation method of the waterproof organic silicone gel specifically comprises the following steps:

[0081] Vinyl silicone oil, terminal hydrogen silicone oil, hydrogen-containing silicone oil and inhibitor are mixed in parts by weight to obtain component A; vinyl silicone oil and platinum catalyst are mixed to obtain component B; component A, component B and composite micro-nano fiber material are mixed and cured; and then a biological waterproofing agent is evenly sprayed on the surface to obtain a waterproof silicone gel.

[0082] The preparation method of the composite micro-nano fiber material is as follows:

[0083] 1) adding 20 g of polyester polyurethane and 7 g of polyethylene glycol octylphenyl ether to 150 mL of N,N-dimethylformamide, stirring the mixture at room temperature for 20 h to obtain a spinning solution, and subjecting the spinning solution to electrospinning at a spinning voltage of 60 kV, a receiving distance of 15 cm, and a liquid feeding speed of 0.5 m / min. The obtained spun fibers were dried to obtain a fiber material;

[0084] 2) Add 15 g of dehydrated hexafluorobutyl methacrylate to a reaction vessel and stir, then add 4 g of glycidyl methacrylate, 0.3 g of ethyl 2-bromoisobutyrate, 0.005 g of copper bromide, and 0.07 g of pentamethyldiethylenetriamine, introduce nitrogen for 15 minutes, and react at 85° C. for 5 hours to obtain a fluorinated acrylate solution;

[0085] 3) Immersing the fiber material in a fluorinated acrylate solution at room temperature at a mass-to-volume ratio of 1 g:50 mL for 30 seconds, removing the fiber material from the solution, drying the solution, and then immersing the fiber material in the fluorinated acrylate solution again. Repeating this operation five times yields a composite micro-nano fiber material.

[0086] The preparation method of the biological waterproofing agent is as follows:

[0087] 1) Choline chloride and oxalic acid were mixed in a molar ratio of 1:1, placed in an 85°C oil bath, and magnetically stirred at 500 rpm until a clear liquid was obtained. The oil bath was then heated to 105°C, and bean curd residue was added to the clear liquid in a solid-liquid mass ratio of 1:25. The mixture was stirred for 60 minutes, and the solid was filtered to obtain a solid.

[0088] 2) 5 g of the solid, 100 mL of deionized water, 1.5 mL of acetic acid, and 1.8 g of sodium chlorite were added to a container and magnetically stirred at 78° C. for 3 h. After the reaction, cellulose was precipitated using distilled water as a reverse-phase solvent and high-pressure homogenized 20 times at 70 MPa using distilled water as the solvent to prepare a 3 wt% suspension, which was then refrigerated for later use.

[0089] 3) Adding an alkyl ketene dimer emulsion with a concentration of 18 wt% to the suspension at a mass ratio of 1:100, magnetically stirring for 50 min, then adding calcium carbonate at a concentration of 0.8% by mass of the suspension, and adjusting the total volume to 50 mL with deionized water. After magnetic stirring at 600 r / min for 50 min, ultrasonic treatment at 300 W for 30 min was performed to obtain a uniformly mixed biowaterproofing agent.

[0090] Comparative Example 1: This comparative example is basically the same as Example 1, except that it does not contain the composite micro-nano fiber material.

[0091] Comparative Example 2: This comparative example is basically the same as Example 1, except that it does not contain a biological waterproofing agent.

[0092] Comparative Example 3: This comparative example is basically the same as Example 1, except that, in the preparation of the composite micro-nano fiber material, steps 2) to 3) are omitted.

[0093] Comparative Example 4: This comparative example is basically the same as Example 1, except that the alkyl ketene dimer emulsion in step 3) is omitted in the preparation of the biological waterproofing agent.

[0094] Comparative Example 5: This comparative example is basically the same as Example 1, except that calcium carbonate in step 3) is omitted in the preparation of the biological waterproofing agent.

[0095] Test experiment:

[0096] The same type of PP substrate was used as the element to be coated. The surface of the PP substrate was wiped clean with ethanol to remove surface oil and impurities. The viscosity of the gel samples in Examples 1-3 and Comparative Examples 1-5 was then measured using a viscometer at room temperature. These samples were then coated on the surface of the PP substrate, and the water repellency was measured according to the national standard. The test results are shown in Table 1.

[0097] Table 1

[0098] Example 1 Example 2 Example 3 Comparative Example 1 Viscosity Pa.s 2.93 3.01 2.97 2.13 Test water column height (mm) 15000 16000 15500 12000 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 Viscosity Pa.s 2.80 2.35 2.83 2.86 Test water column height (mm) 10700 12200 11300 11500

[0099] As can be seen from Table 1, the organosilicon gel of the present invention has stable hydrophobicity and excellent adhesion, which can meet the requirements of normal use under rain conditions. When used in instruments and meters, it can meet the waterproof requirements and has broad application prospects.

[0100] The preferred embodiments of the present invention disclosed above are intended only to help illustrate the present invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the present invention to the specific embodiments described. Obviously, many modifications and variations are possible based on the content of this specification. These embodiments are selected and described in detail in this specification to better explain the principles and practical applications of the present invention, thereby enabling those skilled in the art to better understand and utilize the present invention. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. A waterproof silicone gel, characterized in that: The waterproof silicone gel is prepared from component A, component B and component C; In parts by weight, the component A comprises: 10-50 parts of vinyl silicone oil, 5-30 parts of terminal hydrogen silicone oil, 1-10 parts of hydrogen-containing silicone oil, and 0.1-0.8 parts of inhibitor; The component B comprises: 80-120 parts of vinyl silicone oil and 0.01-0.15 parts of platinum catalyst; The component C comprises: 5-10 parts of composite micro-nano fiber material and 10-30 parts of biological waterproofing agent.

2. The waterproof silicone gel according to claim 1, characterized in that: In the component A, the vinyl silicone oil is any one of polydimethylsiloxane containing vinyl groups at both ends, polydimethylsiloxane containing vinyl groups at only one end and a non-reactive trimethylsilyl group at the other end, or a mixture of the two; The viscosity of the vinyl silicone oil is 100-20000 mPa·s, and the vinyl content is 1-8 wt%.

3. The waterproof silicone gel according to claim 1, characterized in that: In the component B, the vinyl silicone oil is any one of polydimethylsiloxane containing vinyl groups at both ends, polydimethylsiloxane containing vinyl groups at only one end and a non-reactive trimethylsilyl group at the other end, or a mixture of the two; The viscosity of the vinyl silicone oil is 100-20000 mPa·s, and the vinyl content is 1-8 wt %.

4. The waterproof silicone gel according to claim 1, characterized in that: The hydrogen-terminated silicone oil has a viscosity of 1-1000 mPa·s and a hydrogen content of 0.5-3.0 wt%; The hydrogen-containing silicone oil has a viscosity of 1-1000 mPa·s and a hydrogen content of 0.5-2.0 wt%; The inhibitor is selected from at least one of tetramethyltetravinylcyclotetrasiloxane, polyvinylpolysiloxane, 3-methyl-1-pentyn-3-ol, and 1-ethynyl-1-cyclohexanol; The platinum catalyst is selected from at least one of chloroplatinic acid and tetramethyldivinyldisiloxane coordinated platinum catalysts.

5. The waterproof silicone gel according to claim 1, characterized in that: The preparation method of the composite micro-nano fiber material comprises the following steps: 1) adding polyester polyurethane and polyethylene glycol octylphenyl ether to N,N-dimethylformamide, stirring at room temperature for 15-20 hours to obtain a spinning solution, electrospinning the spinning solution, and drying the obtained spun fibers to obtain a fiber material; 2) adding dehydrated hexafluorobutyl methacrylate to a reaction vessel and stirring, then adding glycidyl methacrylate, ethyl 2-bromoisobutyrate, copper bromide, and pentamethyldiethylenetriamine, introducing nitrogen for 5-15 minutes, and reacting at 80-85° C. for 2-5 hours to obtain a fluorinated acrylate solution; 3) Immersing the fiber material in a fluorinated acrylate solution at room temperature at a mass-to-volume ratio of 1 g: (30-50) mL for 20-30 seconds, removing the fiber material from the solution, drying the solution, and then immersing the fiber material in the fluorinated acrylate solution again. Repeating this operation 3-5 times, the composite micro-nano fiber material is obtained.

6. The waterproof silicone gel according to claim 5, characterized in that: In the spinning solution, the ratio of the mass g of polyester polyurethane, the mass g of polyethylene glycol octylphenyl ether and the volume mL of N,N-dimethylformamide is 15-20:3-7:120-150; The electrospinning parameters are as follows: spinning voltage of 40-60 kV, receiving distance of 10-15 cm, and liquid feeding speed of 0.2-0.5 m / min.

7. The waterproof silicone gel according to claim 5, characterized in that: The mass ratio of hexafluorobutyl methacrylate, glycidyl methacrylate, ethyl 2-bromoisobutyrate, copper bromide and pentamethyldiethylenetriamine is 10-15: 3-4: 0.1-0.3: 0.001-0.005: 0.03-0.

07.

8. The waterproof silicone gel according to claim 1, characterized in that: The preparation method of the biological waterproofing agent is as follows: 1) Choline chloride and oxalic acid are mixed in a molar ratio of 1:1, placed in an 80-85°C oil bath, and magnetically stirred until a clear liquid is obtained. The oil bath is then heated to 100-105°C, and bean curd residue is added to the clear liquid in a solid-liquid mass ratio of 1:18-25. The mixture is stirred for 40-60 minutes, and filtered to obtain a solid. 2) adding the solid, deionized water, acetic acid, and sodium chlorite to a container and magnetically stirring at a constant temperature of 75-78° C. for 1-3 hours. After the reaction is completed, cellulose is precipitated using distilled water as a reverse-phase solvent and high-pressure homogenized at 60-70 MPa for 15-20 times using distilled water as a solvent to prepare a suspension with a concentration of 1-3 wt %, which is then refrigerated for later use; 3) adding an alkyl ketene dimer emulsion having a concentration of 15-18 wt % to the suspension, magnetically stirring for 30-50 min, then adding calcium carbonate in an amount of 0.1-0.8% by mass of the suspension, and adjusting the total volume to 30-50 mL with deionized water. After magnetic stirring for 30-50 min, ultrasonic treatment was performed for 15-30 min to obtain a uniformly mixed biowaterproofing agent.

9. The waterproof silicone gel according to claim 8, characterized in that: The ratio of the mass g of the solid, the volume mL of deionized water, the volume mL of acetic acid, and the mass g of sodium chlorite is 2-5:40-100:0.5-1.5:0.6-1.8; The mass ratio of the alkyl ketene dimer emulsion to the suspension is 1:80-100.

10. The method for preparing a waterproof organic silicone gel according to any one of claims 1 to 9, characterized in that: The specific steps include: Vinyl silicone oil, terminal hydrogen silicone oil, hydrogen-containing silicone oil and inhibitor are mixed in parts by weight to obtain component A; vinyl silicone oil and platinum catalyst are mixed to obtain component B; component A, component B and composite micro-nano fiber material are mixed and solidified, and then a biological waterproofing agent is evenly sprayed on the surface to obtain a waterproof silicone gel.

Citation Information

Patent Citations

  • Organosilicone gel and preparation method thereof

    CN113583626A