A silicone polyoxyalkane composition, and a method of making and using the same

By using an organosilicon polyoxyalkylene composition, the problem of corrosive gas corrosion caused by the permeability of organosilicon rubber is solved, providing a protective layer with good sulfur corrosion resistance for protecting electronic and electrical components.

CN115975593BActive Publication Date: 2025-11-18GUANGZHOU HUITIAN FINE CHEM
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Patent Information

Application Number
CN202211743624.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2022-12-30
Publication Date
2025-11-18
Estimated Expiration
2042-12-30

AI Technical Summary

Technical Problem

The molecular chain structure of silicone rubber results in good air permeability, which cannot effectively prevent corrosive gases in the air, such as hydrogen sulfide and sulfur dioxide, from corroding electronic and electrical components, leading to circuit failure.

Method used

An organosilicon polyoxyalkylene composition, comprising organosilicon polyoxyalkylene, alkoxysilane crosslinking agent, thickener and catalyst, is prepared by means of a specific ratio and process to form a protective layer with good resistance to sulfur corrosion.

Benefits of technology

It effectively prevents corrosive gases such as hydrogen sulfide and sulfur dioxide from corroding electronic and electrical components, protecting the integrity of the circuit.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application discloses a kind of organic silicon polyoxyalkane compositions and its preparation method and application, belong to the field of organic silicon materials.The organic silicon polyoxyalkane composition provided by the application includes the following components: organic silicon polyoxyalkane, alkoxysilane crosslinking agent, tackifier, first catalyst;The structure general formula of the organic silicon polyoxyalkane is as shown in formula (I): in formula (I), R1~R 12 Respectively independently selected from C1~C5 alkyl;Z is C1~C10 bivalent saturated hydrocarbon group;A is 1~3;P is 1~20;M is 15~1200;N is 2~25;Q is 1~25.The application provides an organic silicon polyoxyalkane composition by selecting organic silicon polyoxyalkane, and the corrosion resistance to sulfur is good, which can be used to protect electronic and electrical components, so as to prevent them from being damaged by corrosive gases such as hydrogen sulfide, sulfur dioxide and the like in atmospheric environment.
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Description

Technical Field

[0001] This invention belongs to the field of organosilicon materials, and particularly relates to an organosilicon polyoxyalkylene composition, its preparation method, and its application. Background Technology

[0002] Silicone rubber possesses excellent resistance to high and low temperatures, weather resistance, and electrical insulation properties, and is commonly used as insulation protection for electronic and electrical circuit boards. However, due to its helical molecular chain structure, silicone has good air permeability. With the current changes in atmospheric pollution and the increasingly harsh conditions under which electronic products are used, corrosive gases such as hydrogen sulfide and sulfur dioxide in the air can penetrate the protective layer of silicone, corroding silver, copper, and other electrodes or circuits, causing circuit failure. Summary of the Invention

[0003] In order to overcome the problems existing in the prior art, one of the objectives of the present invention is to provide an organosilicon polyoxyalkylene composition with good sulfur corrosion resistance, which is used to protect electronic and electrical components from the damage caused by corrosive gases such as hydrogen sulfide and sulfur dioxide in the atmospheric environment.

[0004] The second objective of this invention is to provide a method for preparing the above-mentioned organosilicon polyoxyalkylene composition.

[0005] The third objective of this invention is to provide an application of the above-mentioned organosilicon polyoxyalkylene composition.

[0006] To achieve the above objectives, the technical solution adopted by the present invention is as follows:

[0007] A first aspect of the present invention provides an organosilicone polyoxyalkylene composition comprising the following raw materials: organosilicone polyoxyalkylene, alkoxysilane crosslinking agent, thickener, and first catalyst; the organosilicone polyoxyalkylene has the general structural formula shown in formula (I):

[0008]

[0009] In the formula (I), R1~R 12 Each is independently selected from C1 to C5 alkyl groups; Z is a C1 to C10 divalent saturated hydrocarbon group; a is 1 to 3; p is 1 to 20; m is 15 to 1200; n is 2 to 25; q is 1 to 25.

[0010] In the formula (I), a, p, m, n, and q are all positive integers.

[0011] Preferably, in formula (I), R1 to R 12 Each of the following is independently selected from methyl, ethyl, or propyl; more preferably, in formula (I), R1 to R2 are selected from methyl, ethyl, or propyl. 12 Each is independently selected from methyl or ethyl; more preferably, in formula (I), R1 to R2 are selected from methyl or ethyl.12 Each is independently selected from methyl groups.

[0012] Preferably, in formula (I), Z is a divalent saturated hydrocarbon group of C2 to C8; more preferably, in formula (I), Z is -(CH2)2-, -(CH3)CHCH2-, or -(CH2)6-; even more preferably, in formula (I), Z is selected from -(CH2)2-.

[0013] Preferably, in formula (I), a is 2 or 3; more preferably, in formula (I), a is 3.

[0014] Preferably, in formula (I), p is 2 to 15; more preferably, in formula (I), p is 3 to 10; even more preferably, in formula (I), p is 3, 5, 8 or 10.

[0015] Preferably, in formula (I), m is 20 to 1000; more preferably, in formula (I), m is 40 to 700; even more preferably, in formula (I), m is 45 to 650.

[0016] Preferably, in formula (I), n is 4 to 20; more preferably, in formula (I), n is 6 to 17; even more preferably, in formula (I), n is 8 to 16.

[0017] Preferably, in formula (I), q is 3 to 20; more preferably, in formula (I), q is 5 to 15; even more preferably, in formula (I), q is 5, 10, 11 or 15.

[0018] Preferably, the organosilicon polyoxyalkylene comprises the following raw materials: hydrosilicone oil, vinyltrimethoxysilane, and olefin.

[0019] Preferably, the organosilicon polyoxyalkylene comprises the following raw materials in parts by weight: 100 parts of hydrogen-containing silicone oil, 1-15 parts of vinyltrimethoxysilane, and 5-16 parts of olefin.

[0020] Preferably, the hydrogen-containing silicone oil in the raw materials for preparing the organosilicon polyoxyalkylene has a viscosity of 30–6000 mPa·s at 25°C; more preferably, the hydrogen-containing silicone oil in the raw materials for preparing the organosilicon polyoxyalkylene has a viscosity of 35–5700 mPa·s at 25°C; and even more preferably, the hydrogen-containing silicone oil in the raw materials for preparing the organosilicon polyoxyalkylene has a viscosity of 40–5200 mPa·s at 25°C.

[0021] Preferably, the Si-H content of the hydrogen-containing silicone oil in the raw materials for preparing the organosilicon polyoxyalkylene is 0.3–2.5 mmol / g; more preferably, the Si-H content of the hydrogen-containing silicone oil in the raw materials for preparing the organosilicon polyoxyalkylene is 0.35–2.3 mmol / g; and even more preferably, the Si-H content of the hydrogen-containing silicone oil in the raw materials for preparing the organosilicon polyoxyalkylene is 0.4–2.0 mmol / g.

[0022] Preferably, the raw materials for preparing the organosilicon polyoxyalkylene contain 1.5 to 14 parts by mass of vinyltrimethoxysilane; more preferably, the raw materials for preparing the organosilicon polyoxyalkylene contain 2 to 13 parts by mass of vinyltrimethoxysilane; and even more preferably, the raw materials for preparing the organosilicon polyoxyalkylene contain 2.5 to 12 parts by mass of vinyltrimethoxysilane.

[0023] Preferably, the olefins in the raw materials for preparing the organosilicon polyoxyalkylene are C6 to C20 olefins; more preferably, the olefins in the raw materials for preparing the organosilicon polyoxyalkylene are C9 to C18 olefins; and even more preferably, the olefins in the raw materials for preparing the organosilicon polyoxyalkylene are C8 to C16 olefins.

[0024] Preferably, the olefin content in the raw materials for preparing the organosilicon polyoxyalkylene is 5.5 to 15.5 parts by mass; more preferably, the olefin content in the raw materials for preparing the organosilicon polyoxyalkylene is 6 to 15 parts by mass; and even more preferably, the olefin content in the raw materials for preparing the organosilicon polyoxyalkylene is 6.5 to 14.5 parts by mass.

[0025] Preferably, the organosilicon polyoxyalkylene is prepared under the catalysis of a second catalyst.

[0026] Preferably, the concentration of the second catalyst in the raw materials for preparing the organosilicon polyoxyalkylene is 3 to 50 ppm; more preferably, the concentration of the second catalyst in the raw materials for preparing the organosilicon polyoxyalkylene is 5 to 30 ppm; and even more preferably, the concentration of the second catalyst in the raw materials for preparing the organosilicon polyoxyalkylene is 10 to 20 ppm.

[0027] Preferably, in the raw materials for preparing the organosilicon polyoxyalkylene, the second catalyst is selected from a platinum catalyst; more preferably, in the raw materials for preparing the organosilicon polyoxyalkylene, the second catalyst includes at least one of a platinum-vinylsiloxane complex, an alcohol-modified chloroplatinic acid, and a platinum-alkynyl group complex; even more preferably, in the raw materials for preparing the organosilicon polyoxyalkylene, the second catalyst is selected from a platinum-vinylsiloxane complex.

[0028] Preferably, in the raw materials for preparing the organosilicon polyoxyalkylene, the Pt concentration of the platinum catalyst is 3-50 ppm; more preferably, in the raw materials for preparing the organosilicon polyoxyalkylene, the Pt concentration of the platinum catalyst is 5-30 ppm; and even more preferably, in the raw materials for preparing the organosilicon polyoxyalkylene, the Pt concentration of the platinum catalyst is 10-20 ppm.

[0029] Preferably, the organosilicon polyoxyalkylene comprises the following raw materials in parts by weight: 100 parts of hydrogen-containing silicone oil, 1.5 to 14 parts of vinyltrimethoxysilane, and 5.5 to 15.5 parts of olefin.

[0030] More preferably, the organosilicon polyoxyalkylene comprises the following raw materials in parts by weight: 100 parts of side-containing hydrogen silicone oil, 2-13 parts of vinyltrimethoxysilane, and 6-15 parts of olefin.

[0031] More preferably, the organosilicon polyoxyalkylene comprises the following raw materials in parts by weight: 100 parts of hydrogen-containing silicone oil, 2.5 to 12 parts of vinyltrimethoxysilane, and 6.5 to 14.5 parts of olefin.

[0032] Preferably, the organosilicon polyoxyalkylene is prepared by the following method: at 20-30°C, a side-containing silicone oil, vinyltrimethoxysilane and a second catalyst are mixed, heated to 65-115°C, and reacted for 0.5-5.5 hours, then an olefin is added, and the reaction is carried out for 2.5-7.5 hours to obtain the organosilicon polyoxyalkylene.

[0033] Preferably, in the method for preparing the organosilicon polyoxyalkylene, the heating temperature of the side-containing silicone oil, vinyltrimethoxysilane, and the second catalyst is 70-110°C; more preferably, in the method for preparing the organosilicon polyoxyalkylene, the heating temperature of the side-containing silicone oil, vinyltrimethoxysilane, and the second catalyst is 75-105°C; even more preferably, in the method for preparing the organosilicon polyoxyalkylene, the heating temperature of the side-containing silicone oil, vinyltrimethoxysilane, and the second catalyst is 80-100°C.

[0034] Preferably, in the method for preparing the organosilicon polyoxyalkylene, the reaction time of the side-containing silicone oil, vinyltrimethoxysilane, and the second catalyst is 1 to 5 hours; more preferably, in the method for preparing the organosilicon polyoxyalkylene, the reaction time of the side-containing silicone oil, vinyltrimethoxysilane, and the second catalyst is 1.5 to 4.5 hours; even more preferably, in the method for preparing the organosilicon polyoxyalkylene, the reaction time of the side-containing silicone oil, vinyltrimethoxysilane, and the second catalyst is 2 to 4 hours.

[0035] Preferably, in the method for preparing the organosilicon polyoxyalkylene, the reaction time after adding the olefin is 3 to 7 hours; more preferably, in the method for preparing the organosilicon polyoxyalkylene, the reaction time after adding the olefin is 3.5 to 6.5 hours; even more preferably, in the method for preparing the organosilicon polyoxyalkylene, the reaction time after adding the olefin is 4 to 6 hours.

[0036] Preferably, the organosilicon polyoxyalkylene composition comprises the following raw materials in parts by weight: 100 parts organosilicon polyoxyalkylene, 0.1 to 20 parts alkoxysilane crosslinking agent, 0.01 to 5 parts thickener, and 0.01 to 10 parts first catalyst.

[0037] Preferably, in the organosilicon polyoxyalkylene composition, the alkoxysilane crosslinking agent includes at least one of dimethyldimethoxysilane, tetramethoxysilane, methyltrimethoxysilane, vinyltrimethoxysilane, phenyltrimethoxysilane, tetraethoxysilane, methyltriethoxysilane, vinyltriethoxysilane, phenyltriethoxysilane, or a hydrolysis condensate of the above-mentioned alkoxysilanes; more preferably, in the organosilicon polyoxyalkylene composition, the alkoxysilane crosslinking agent includes at least one of dimethyldimethoxysilane, tetramethoxysilane, methyltrimethoxysilane, vinyltrimethoxysilane, phenyltrimethoxysilane, or tetraethoxysilane; even more preferably, in the organosilicon polyoxyalkylene composition, the alkoxysilane crosslinking agent includes at least one of dimethyldimethoxysilane, methyltrimethoxysilane, or phenyltrimethoxysilane.

[0038] Preferably, the alkoxysilane crosslinking agent in the organosilicon polyoxyalkylene composition is 0.1 to 10 parts by mass; more preferably, the alkoxysilane crosslinking agent in the organosilicon polyoxyalkylene composition is 1.5 to 10 parts by mass; and even more preferably, the alkoxysilane crosslinking agent in the organosilicon polyoxyalkylene composition is 5 to 10 parts by mass.

[0039] Preferably, in the organosilicon polyoxyalkylene composition, the tackifier has the structural formula as shown in formula (II):

[0040]

[0041] In formula (II), R1' to R2' are each independently selected from C1 to C5 alkyl groups; b is 1, 2 or 3; Y is an epoxy group, methacryloxy group, mercapto group, amino group or isocyanate group.

[0042] Preferably, in the organosilicon polyoxyalkylene composition, R1' to R2" in formula (II) are each independently selected from methyl, ethyl, or propyl; more preferably, in the organosilicon polyoxyalkylene composition, R1' to R2' in the tackifier are each independently selected from methyl or ethyl.

[0043] Preferably, in the organosilicon polyoxyalkylene composition, b in formula (II) is 2 or 3.

[0044] Preferably, in the organosilicon polyoxyalkylene composition, Y in formula (II) is an epoxy group, an amino group, or an isocyanate group; more preferably, in the organosilicon polyoxyalkylene composition, Y in formula (II) is an epoxy group or an amino group; even more preferably, in the organosilicon polyoxyalkylene composition, Y in formula (II) is an epoxy group or a diamino group.

[0045] Preferably, the tackifier in the organosilicone polyoxyalkylene composition includes at least one of glycidyltrimethoxysilane, aminopropyltrimethoxysilane, N-(2-aminoethyl)-3-aminopropyltrimethoxysilane, N-(2-aminoethyl)-3-aminopropyltriethoxysilane, N-(2-aminoethyl)-3-aminopropylmethyldimethoxysilane, and N-(2-aminoethyl)-3-aminopropylmethyldiethoxysilane; more preferably, the organosilicone polyoxyalkylene... In the composition, the tackifier includes at least one of glycidyltrimethoxysilane, aminopropyltrimethoxysilane, N-(2-aminoethyl)-3-aminopropyltrimethoxysilane, or N-(2-aminoethyl)-3-aminopropyltriethoxysilane; more preferably, in the organosilicon polyoxyalkylene composition, the tackifier includes at least one of glycidyltrimethoxysilane, aminopropyltrimethoxysilane, or N-(2-aminoethyl)-3-aminopropyltrimethoxysilane.

[0046] Preferably, the tackifier in the organosilicon polyoxyalkylene composition is 0.1 to 3 parts by weight; more preferably, the tackifier in the organosilicon polyoxyalkylene composition is 0.5 to 2.5 parts by weight; and even more preferably, the tackifier in the organosilicon polyoxyalkylene composition is 1 to 2 parts by weight.

[0047] Preferably, in the organosilicone polyoxyalkylene composition, the first catalyst comprises an organotin compound, a titanate compound, or a combination thereof; more preferably, in the organosilicone polyoxyalkylene composition, the first catalyst comprises dibutyltin dilaurate, dibutyltin diacetate, dibutyltin diethylhexanoate, dibutyltin dioctanoate, dibutyltin dimethylmaleate, dibutyltin maleate, dioctyltin diacetate, dioctyltin distearate, dioctyltin dilaurate, dimethyl dibutyltin, diphenoxy dibutyltin, dimethoxy di At least one of butyltin, dibutyltin diacetylacetone, ethyl diacetylacetone dibutyltin, dibutyltin bis(triethoxysilane), dioctyltin bis(triethoxysilane), tin diethoxyoxide, tetraisopropyl titanate, tetrabutyl titanate, a complex of titanate and ethyl acetoacetate, or a complex of titanate and acetylacetone; more preferably, in the organosilicon polyoxyalkylene composition, the first catalyst includes at least one of tetrabutyl dilaurate titanate and diisopropyl bis(ethyl acetoacetate) titanate.

[0048] Preferably, the first catalyst in the organosilicon polyoxyalkylene composition is 0.05 to 8 parts by mass; more preferably, the first catalyst in the organosilicon polyoxyalkylene composition is 0.08 to 6 parts by mass; and even more preferably, the first catalyst in the organosilicon polyoxyalkylene composition is 0.1 to 5 parts by mass.

[0049] Preferably, the organosilicon polyoxyalkylene composition comprises the following raw materials in parts by weight: 100 parts organosilicon polyoxyalkylene, 0.1 to 10 parts alkoxysilane crosslinking agent, 0.1 to 3 parts thickener, and 0.05 to 8 parts first catalyst.

[0050] More preferably, the organosilicon polyoxyalkylene composition comprises the following raw materials in parts by weight: 100 parts organosilicon polyoxyalkylene, 1.5 to 10 parts alkoxysilane crosslinking agent, 0.5 to 2.5 parts thickener, and 0.08 to 6 parts first catalyst.

[0051] More preferably, the organosilicon polyoxyalkylene composition comprises the following raw materials in parts by weight: 100 parts organosilicon polyoxyalkylene, 5-10 parts alkoxysilane crosslinking agent, 1-2 parts thickener, and 0.1-5 parts first catalyst.

[0052] Preferably, the raw materials for preparing the organosilicon polyoxyalkylene composition further include fillers, processing aids, or combinations thereof.

[0053] Preferably, in the organosilicon polyoxyalkylene composition, the filler includes at least one of fumed silica, silica powder, aluminum hydroxide, aluminum oxide, or magnesium oxide; more preferably, in the organosilicon polyoxyalkylene composition, the filler includes at least one of fumed silica, silica powder, or aluminum hydroxide; even more preferably, in the organosilicon polyoxyalkylene composition, the filler is selected from fumed silica.

[0054] Preferably, the fumed silica in the filler is surface-modified fumed silica; more preferably, the surface modifier of the surface-modified fumed silica includes at least one of chlorosilane, silazane, siloxane, acryloyloxysilane, or methoxysilane; even more preferably, the surface modifier of the surface-modified fumed silica includes at least one of trimethylchlorosilane, dimethyldichlorosilane, methyltrichlorosilane, hexamethyldisilazane, divinyltetramethyldisilazane, divinyltetramethyldisilazane, polydimethylsiloxane, octamethylcyclotetrasiloxane, methacryloxysilane, or octyltrimethoxysilane; more preferably, the surface modifier of the surface-modified fumed silica includes at least one of hexamethyldisilazane, divinyltetramethyldisilazane, or divinyltetramethyldisilazane.

[0055] Preferably, in the organosilicon polyoxyalkylene composition, the specific surface area of ​​the filler is 50-600 m². 2 / g; More preferably, in the organosilicon polyoxyalkylene composition, the specific surface area of ​​the filler is 100-500 m² / g. 2 / g; More preferably, in the organosilicone polyoxyalkylene composition, the specific surface area of ​​the filler is 150-400m². 2 / g.

[0056] Preferably, the filler in the organosilicone polyoxyalkylene composition is 0.1 to 20 parts by mass; more preferably, the filler in the organosilicone polyoxyalkylene composition is 1 to 15 parts by mass; and even more preferably, the filler in the organosilicone polyoxyalkylene composition is 3 to 10 parts by mass.

[0057] Preferably, the processing aid in the organosilicon polyoxyalkylene composition includes at least one of toluene, polyisobutylene, alkane, or dimethyl silicone oil; more preferably, the processing aid in the organosilicon polyoxyalkylene composition includes at least one of alkane or dimethyl silicone oil; even more preferably, the processing aid in the organosilicon polyoxyalkylene composition is selected from dimethyl silicone oil.

[0058] Preferably, in the organosilicon polyoxyalkylene composition, the viscosity of the processing aid at 25°C is 50–200 mPa·s; more preferably, in the organosilicon polyoxyalkylene composition, the viscosity of the processing aid at 25°C is 70–170 mPa·s; even more preferably, in the organosilicon polyoxyalkylene composition, the viscosity of the processing aid at 25°C is 90–150 mPa·s.

[0059] Preferably, the processing aid in the organosilicone polyoxyalkylene composition is 1 to 30 parts by weight; more preferably, the processing aid in the organosilicone polyoxyalkylene composition is 5 to 25 parts by weight; and even more preferably, the processing aid in the organosilicone polyoxyalkylene composition is 10 to 20 parts by weight.

[0060] Preferably, the organosilicon polyoxyalkylene composition comprises the following raw materials in parts by weight: 100 parts organosilicon polyoxyalkylene, 0.1 to 20 parts alkoxysilane crosslinking agent, 0.01 to 5 parts tackifier, 0.01 to 10 parts first catalyst, and 0.1 to 20 parts filler.

[0061] More preferably, the organosilicon polyoxyalkylene composition comprises the following raw materials in parts by weight: 100 parts organosilicon polyoxyalkylene, 0.1 to 10 parts alkoxysilane crosslinking agent, 0.1 to 3 parts thickener, 0.05 to 8 parts first catalyst, and 1 to 15 parts filler.

[0062] More preferably, the organosilicon polyoxyalkylene composition comprises the following raw materials in parts by weight: 100 parts organosilicon polyoxyalkylene, 1.5 to 10 parts alkoxysilane crosslinking agent, 0.5 to 2.5 parts tackifier, 0.08 to 6 parts first catalyst, and 3 to 10 parts filler.

[0063] Preferably, the organosilicon polyoxyalkylene composition comprises the following raw materials in parts by weight: 100 parts organosilicon polyoxyalkylene, 0.1 to 20 parts alkoxysilane crosslinking agent, 0.01 to 5 parts tackifier, 0.01 to 10 parts first catalyst, 0.1 to 20 parts filler, and 1 to 30 parts processing aid.

[0064] More preferably, the organosilicon polyoxyalkylene composition comprises the following raw materials in parts by weight: 100 parts organosilicon polyoxyalkylene, 0.1 to 10 parts alkoxysilane crosslinking agent, 0.1 to 3 parts tackifier, 0.05 to 8 parts first catalyst, 1 to 15 parts filler, and 5 to 25 parts processing aid.

[0065] More preferably, the organosilicon polyoxyalkylene composition comprises the following raw materials in parts by weight: 100 parts organosilicon polyoxyalkylene, 1.5 to 10 parts alkoxysilane crosslinking agent, 0.5 to 2.5 parts tackifier, 0.08 to 6 parts first catalyst, 3 to 10 parts filler, and 10 to 20 parts processing aid.

[0066] A second aspect of the present invention provides a method for preparing the organosilicone polyoxyalkylene composition described in the first aspect of the present invention, comprising the following steps: mixing the components in a moisture-free environment to obtain the organosilicone polyoxyalkylene composition.

[0067] A third aspect of the present invention provides the application of the organosilicone polyoxyalkylene composition described in the first aspect of the present invention or the organosilicone polyoxyalkylene composition prepared by the preparation method described in the second aspect of the present invention in the field of electronic and electrical components.

[0068] Preferably, the organosilicon polyoxyalkylene composition can be used to protect electronic and electrical components.

[0069] The beneficial effects of this invention are:

[0070] This invention provides an organosilicon polyoxyalkylene composition with good sulfur corrosion resistance by selecting organosilicon polyoxyalkylene compounds. It can be used to protect electronic and electrical components from the harmful effects of corrosive gases such as hydrogen sulfide and sulfur dioxide in the atmospheric environment. Detailed Implementation

[0071] The following specific embodiments further illustrate the content of the present invention in detail. It should also be understood that the following embodiments are only for further explanation of the present invention and should not be construed as limiting the scope of protection of the present invention. Non-essential improvements and adjustments made by those skilled in the art based on the principles described herein are all within the scope of protection of the present invention. The specific process parameters, etc., in the following examples are merely examples within a suitable range; that is, those skilled in the art can make selections within a suitable range based on the description herein, and are not intended to be limited to the specific data in the examples below. Except for the raw materials specifically described, other raw materials can be obtained commercially available or through conventional means.

[0072] In the comparative examples of this invention, the trimethoxy-terminated polydimethylsiloxane used has a viscosity of 1000 mPa·s at 25°C. The surface modifier for the surface-modified fumed silica used in the embodiments and comparative examples of this invention is hexamethyldisilazane, which has a specific surface area of ​​300 m² / s. 2 / g. Processing aids can adjust the viscosity of the composition and improve its workability. The processing aid used in the embodiments and comparative examples of this invention is dimethyl silicone oil, which has a viscosity of 100 mPa·s at 25°C.

[0073] Example 1 of preparation of organosilicon polyoxyalkylene

[0074] At 25°C, 1000 g of hydrosilicone oil (viscosity 50 mPa·s at 25°C, Si-H content 1.98 mmol / g) and 110 g of vinyltrimethoxysilane were added to a three-necked flask. While stirring, 10 ppm (Pt concentration in the total reactants) of a platinum-vinylsiloxane complex was added. The temperature was raised to 80°C and the reaction was carried out for 4 h. Infrared spectroscopy revealed the disappearance of the characteristic peak of the vinyl groups in the mixture. Subsequently, 140 g of octene was added, and the reaction was continued for 6 h. Infrared spectroscopy revealed the disappearance of the characteristic peak of the silane groups in the mixture. NMR analysis of the final product yielded an organosilicon polyoxane (polymer 1) with the following structural formula:

[0075]

[0076] Example 2 of preparation of organosilicon polyoxyalkylene

[0077] At 25°C, 1000 g of hydrogen-containing silicone oil (viscosity at 25°C: 500 mPa·s, Si-H content: 0.9 mmol / g) and 44.5 g of vinyltrimethoxysilane were added to a three-necked flask. While stirring, 15 ppm (concentration of Pt in the total reactants) of platinum-vinylsiloxane complex was added. The temperature was raised to 90°C and the reaction was carried out for 3.5 h. Then, 90 g of decene was added, and the reaction was continued for another 5.5 h.

[0078] The final product, analyzed by NMR, yielded an organosilicon polyoxyalkylene (polymer 2) with the following structural formula:

[0079]

[0080] Example 3 of Organosilicon Polyoxyalkylene Preparation

[0081] At 25°C, 1000 g of hydrosilicone oil (viscosity 1000 mPa·s at 25°C, Si-H content 0.73 mmol / g) and 44.5 g of vinyltrimethoxysilane were added to a three-necked flask. While stirring, 15 ppm (Pt concentration in the total reactants) of a platinum-vinylsiloxane complex was added. The temperature was raised to 95°C and the reaction was carried out for 3 h. Then, 70 g of n-dodecene was added, and the reaction was continued for another 5 h. NMR analysis of the final product yielded an organosilicon polyoxane (polymer 3) with the following structural formula:

[0082]

[0083] Example 4 of Organosilicon Polyoxyalkylene Preparation

[0084] At 25°C, 1000 g of hydrosilicone oil (viscosity 5000 mPa·s at 25°C, Si-H content 0.5 mmol / g) and 30 g of vinyltrimethoxysilane were added to a three-necked flask. While stirring, 15 ppm (Pt concentration in the total reactants) of a platinum-vinylsiloxane complex was added. The temperature was raised to 100°C and the reaction was carried out for 2.5 h. Then, 65 g of n-hexadecene was added, and the reaction was continued for another 4.5 h. NMR analysis of the final product yielded an organosilicon polyoxane (polymer 4) with the following structural formula:

[0085]

[0086] Examples 1-4 and Comparative Example 1 were prepared by mixing the raw materials as described in Table 1 to obtain organosilicon polyoxyalkylene compositions. The units in Table 1 are parts by mass.

[0087] Table 1. Raw materials used in Examples 1-4 and Comparative Example 1

[0088]

[0089]

[0090] Viscosity test: The viscosity of the compositions of Examples 1-4 and Comparative Example 1 was tested at 25°C.

[0091] Adhesion test: The adhesion of the compositions of Examples 1-4 and Comparative Example 1 to copper plates, aluminum plates, PCs, PCBs, and nickel plates was tested respectively. Wherein, ○: able to adhere; ×: unable to adhere.

[0092] Sulfur corrosion resistance test: The compositions of Examples 1-4 and Comparative Example 1 were coated onto a silver-plated copper plate with a coating thickness of 2 mm and cured at room temperature for seven days. Subsequently, the test specimens were placed in a 100 mL glass bottle along with 0.2 g of sulfur powder and sealed. The test bottle was placed in an oven at 80°C for one week, and the coating was peeled off to observe the degree of corrosion of the silver plating. ○: No corrosion (no discoloration); ×: Corrosion present (blackening). The results are shown in Table 2.

[0093] Table 2 shows the performance test results of the compositions in Examples 1-4 and Comparative Example 1.

[0094]

[0095] The addition of tackifiers in this invention improves the adhesive properties of the compositions. Specifically, in Example 2, N-(2-aminoethyl)-3-aminopropyltrimethoxysilane and glycidyltrimethoxysilane were added as tackifiers, and in Example 4, N-(2-aminoethyl)-3-aminopropyltrimethoxysilane was added as a tackifier, resulting in compositions with better adhesive properties. The compositions of Examples 1-4 all exhibit good sulfur corrosion resistance.

[0096] As can be seen from the above tests, the present invention provides an organosilicon polyoxyalkylene composition with good sulfur corrosion resistance by selecting organosilicon polyoxyalkylene. It can be used to protect electronic and electrical components from the damage of corrosive gases (such as hydrogen sulfide, sulfur dioxide, etc.) in the atmospheric environment.

Claims

1. A silicone polyoxyalkane composition characterized in that, The preparation raw materials include the following components by mass: 100 parts of organosilicon polyoxyalkane, 0.1-20 parts of alkoxy silane crosslinking agent, 0.01-5 parts of tackifier, and 0.01-10 parts of first catalyst; the general structure of the organosilicon polyoxyalkane is shown in formula (I): In the formula (I), R1to R 12 are each independently selected from C1to C5alkyl; Z is a C1to C10divalent saturated hydrocarbon group; a is 1 to 3; p is 1 to 20; m is 15 to 1200; n is 2 to 25; q is 1 to 25; The alkoxy silane crosslinking agent includes at least one of dimethyldimethoxysilane, tetramethoxysilane, methyltrimethoxysilane, vinyltrimethoxysilane, phenyltrimethoxysilane, tetraethoxysilane, methyltriethoxysilane, vinyltriethoxysilane, phenyltriethoxysilane, or a hydrolysis condensate of the above alkoxy silane; The tackifier has a structural formula shown in formula (II): In formula (II), R1'-R2' are independently selected from C1-C5 alkyl; b is 1, 2 or 3; and Y is amino. The first catalyst includes an organotin compound, a titanate compound, or a combination thereof.

2. The organosilicon polyoxyalkane composition of claim 1, wherein, In the formula (I), R1to R 12 are each independently selected from methyl, ethyl or propyl; And / or, Z is a C2-C8 bivalent saturated hydrocarbon group; And / or, a is 2 or 3; And / or, p is 2-15; And / or, m is 20-1000; And / or, n is 4-20; And / or, q is 3-20.

3. The organosilicon polyoxyalkane composition of claim 1 or 2, wherein, The organosilicon polyoxyalkane is prepared from the following components by mass: 100 parts of hydrogen-containing silicone oil, 1-15 parts of vinyltrimethoxysilane, and 5-16 parts of olefin.

4. The organosilicon polyoxyalkane composition of claim 3, wherein, The organosilicon polyoxyalkane is prepared under catalysis of a second catalyst; And / or, the concentration of the second catalyst in the preparation raw materials of the organosilicon polyoxyalkane is 3-50 ppm; And / or, the second catalyst is selected from a platinum catalyst.

5. The organosilicon polyoxyalkane composition of claim 1, wherein, The preparation raw materials of the organosilicon polyoxyalkane composition further include a filler, a processing aid, or a combination thereof.

6. The organosilicon polyoxyalkane composition of claim 5, wherein, The filler includes at least one of fumed silica, silicon powder, aluminum hydroxide, aluminum oxide, or magnesium oxide; and / or the specific surface area of the filler is 50 to 600 m 2 / g; And / or, the processing aid includes at least one of toluene, polyisobutylene, alkane, or dimethyl silicone oil; And / or, the viscosity of the processing aid at 25°C is 50-200 mPa·s.

7. A process for the production of the organosilicon polyoxyalkane composition according to any one of claims 1 to 6, characterized in that, The method includes the following steps: The components are mixed in a moisture-proof environment to prepare the organosilicon polyoxyalkane composition.

8. Use of a silicone polyoxyalkane composition in the field of electronic and electrical components, characterized in that, The organosilicon polyoxyalkane composition is the organosilicon polyoxyalkane composition according to any one of claims 1-6, or is prepared by the preparation method of claim 7.

Citation Information

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