One-component addition-type organosilicon adhesive and preparation method thereof

The controllable catalyst compounded with platinum catalyst and organosilicon phosphine compound solves the problems of insufficient stability and storage period of addition-type silicone at room temperature, achieves rapid curing at high temperature and good storage period, and improves the workability and flame retardant properties of silicone.

CN119529754BActive Publication Date: 2025-09-30GUANGZHOU BAIYUN CHEM IND +1
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Patent Information

Application Number
CN202411791392.8
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-12-06
Publication Date
2025-09-30
Estimated Expiration
2044-12-06

AI Technical Summary

Technical Problem

Existing addition-type silicone catalysts have insufficient stability and storage period at room temperature, and it is difficult to balance the curing speed at high temperatures. Traditional inhibitors may precipitate at low temperatures, affecting storage, making it difficult to meet construction and storage requirements.

Method used

A self-made controllable catalyst is used, which is compounded with a platinum catalyst and an organosilicon phosphine compound. The single-component addition-type organosilicon adhesive is prepared by catalyzing the hydrosilylation reaction at high temperature with good stability at room temperature.

Benefits of technology

It achieves good stability and long storage period at room temperature, and cures quickly at high temperature. The catalyst has good compatibility with the silicone system and is not easy to precipitate, which improves the flame retardant properties of silicone.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention belongs to the technical field of organosilicon adhesives, and specifically discloses a one-component addition-type organosilicon adhesive and a preparation method thereof. The one-component addition-type organosilicon adhesive comprises the following raw materials by weight: 100 parts of vinyl silicone oil, 5-15 parts of a cross-linking agent; 0.5-2 parts of a controllable catalyst, 1-2 parts of a tackifier, and 10-50 parts of a reinforcing filler. The controllable catalyst is compounded by a platinum catalyst and an organosilicon phosphine oxide compound; the organosilicon phosphine oxide compound is prepared by reacting a siloxane containing a vinyl functional group and an alkane phosphine oxide; the reaction is carried out at 60-100°C and an initiator. The present invention is applied to silica gel by making a self-made controllable catalyst, which can make silica gel have good stability and long storage period at room temperature, faster curing speed at high temperature, and also have a long storage period.
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Description

Technical Field

[0001] The present invention relates to the technical field of organosilicon adhesives, and in particular to a one-component addition-type organosilicon adhesive and a preparation method thereof. Background Art

[0002] Silicone rubber is an elastomeric polymer whose basic structure is an organosiloxane polymer. Unlike traditional organic rubbers, its structure dictates its unique properties. The coexistence of organic and inorganic groups within the polymer backbone creates a unique blend of organic and inorganic properties. Furthermore, because the Si-O bond energy is higher than the C-C bond energy of organic rubber, silicone rubber possesses greater stability. These advantages have led to its widespread application in aerospace, military, construction, electronics, and medical applications. Silicone rubber can be categorized by process and reaction mechanism. Addition-type silicone rubber has recently seen rapid growth. These rubbers primarily consist of hydrogenated silicone oils, vinyl silicone oils, catalysts, fillers, and additives. The curing mechanism of addition-type silicone rubber is primarily a platinum-catalyzed hydrosilylation reaction of carbon-carbon double bonds and silicon-hydrogen bonds. This reaction, without the release of small molecules, results in excellent performance and significant development potential. While research on silicone oils, fillers, and additives in addition-type silicone rubbers has been extensive, research on catalysts and inhibitors has been relatively limited.

[0003] Currently, the primary catalyst used is platinum, such as platinum-vinylsiloxane complexes. Platinum catalysts possess extremely high catalytic activity, enabling rapid crosslinking of low-molecular-weight polysiloxanes at room temperature at very low dosages. This is disadvantageous for time-consuming construction processes and the storage and use of single-component silicones. Therefore, inhibitors are added to adjust the curing time. There are many types of inhibitors, which can be broadly categorized into three main groups: 1. Compounds containing unsaturated bonds, such as acetylenic alcohols and vinylsiloxanes; 2. Organic compounds containing N, P, S, and other unshared electrons; and 3. Heavy metal ion compounds. Most of the latter two groups form stable coordination bonds with the catalyst, effectively reducing its activity. However, curing at high temperatures significantly increases the difficulty, making it difficult to balance construction and storage. Currently, acetylene cyclohexanol and its analogs are the most popular. However, acetylene cyclohexanol has a slightly higher melting point and may precipitate from the silicone at lower temperatures, reducing the silicone's shelf life or handling time, thus presenting certain limitations. Summary of the Invention

[0004] In response to the aforementioned shortcomings, the present invention provides a one-component addition-type organosilicon adhesive and its preparation method. This invention utilizes a self-made controllable catalyst (a novel platinum catalyst) applied to the silicone rubber. This catalyst imparts excellent stability and a long shelf life to the silicone rubber at room temperature. Furthermore, it efficiently catalyzes the hydrosilylation reaction at a specific temperature, enabling rapid curing of the one-component silicone rubber. The phosphine oxide compound used in this controllable catalyst is more stable than previously disclosed organophosphine ligand inhibitors, cures faster at high temperatures, and similarly offers a long shelf life.

[0005] In order to achieve the above object, the present invention provides a one-component addition-type organic silicone adhesive, wherein the silicone rubber is composed of the following raw materials in parts by weight:

[0006]

[0007] Wherein, the controllable catalyst is compounded by a platinum catalyst and an organic silicon phosphine compound;

[0008] The organic silicon phosphine oxide compound is prepared by reacting siloxane containing a vinyl functional group with an alkane phosphine oxide; the reaction is carried out at 60-100° C. and in the presence of an initiator.

[0009] Preferably, the molar ratio of the vinyl functional group-containing siloxane to the alkane phosphine oxide is 1:1 to 2;

[0010] Preferably, the amount of the initiator added is 0.1-1 wt.% of the total mass of the vinyl functional group-containing siloxane and the alkane phosphine oxide.

[0011] According to one aspect of the present invention, the structural formula of the vinyl functional group-containing siloxane is as shown in Formula I, the structural formula of the alkane phosphine oxide is as shown in Formula II, and the organosilicon phosphine oxide compound is as shown in Formula III:

[0012]

[0013]

[0014] Wherein, in formula I and formula III, n is 1-5, and R1 is one of methyl, ethyl, and vinyl;

[0015] In formula II, R2 is an alkyl group or a phenyl group.

[0016] According to one aspect of the present invention, the siloxane containing vinyl functional groups is vinyl terminated polydimethylsiloxane.

[0017] According to one aspect of the present invention, the viscosity of the vinyl silicone oil is 100-2000 mPa·s, and the vinyl content in the vinyl silicone oil is 0.1-0.5 wt.%.

[0018] According to one aspect of the present invention, the cross-linking agent is hydrogen-containing silicone oil, the hydrogen-containing silicone oil is a branched hydrogen-containing silicone oil, and the hydrogen content in the hydrogen-containing silicone oil is 0.1-1.0 wt.%.

[0019] According to one aspect of the present invention, the platinum content of the controllable catalyst is 1000-5000 ppm.

[0020] According to one aspect of the present invention, the tackifier is an organosilicon tackifier; the organosilicon tackifier is prepared by a hydrosilylation reaction of tetramethyltetravinylcyclotetrasiloxane and ethyl acrylate.

[0021] It should be noted that the conditions for the hydrosilylation reaction are: platinum catalyst, stirring at 60°C for 6 hours under nitrogen protection. After the hydrosilylation reaction is completed, low-boiling substances are removed by distillation under reduced pressure to obtain an organosilicon tackifier.

[0022] According to one aspect of the present invention, the reinforcing filler is one or more of fumed silica, precipitated silica, silicone resin, calcium carbonate, silicon powder, aluminum oxide, silicon carbide, and silicon nitride.

[0023] Based on the same inventive concept, the present invention also provides a method for preparing the above-mentioned one-component addition-type silicone adhesive, comprising the following steps:

[0024] S1. Adding a vinyl functional group-containing siloxane and an alkane phosphine oxide in a specific ratio to solvent A, and adding an initiator, reacting at 60-100° C. for 4-12 hours, and then distilling under reduced pressure to obtain an organosilicon phosphine oxide compound;

[0025] S2, adding the platinum catalyst and the organosilicon phosphine compound to solvent B, stirring at room temperature for 4-12 hours, and then distilling under reduced pressure to obtain a controllable catalyst;

[0026] S3, preparing a base material by kneading the reinforcing filler powder and vinyl silicone oil, and pre-treating it with a silane coupling agent or hexamethyldisilazane to obtain a vinyl-based adhesive;

[0027] Preferably, the amount of the silane coupling agent or hexamethyldisilazane added is 0.1-1 wt.% of the total mass of vinylpentamethyldisiloxane and dimethylphosphine oxide.

[0028] S4. Add vinyl-based adhesive, cross-linking agent, controllable catalyst and tackifier into the planetary machine in sequence, and stir evenly under a vacuum degree of 0.1 MPa to obtain a single-component addition-type silicone adhesive.

[0029] According to one aspect of the present invention, in step S1, the solvent A is any one of toluene, xylene, tetrahydrofuran, and isopropanol; the initiator is any one of dibenzoyl peroxide, tert-butyl perbenzoate, diisopropyl peroxide, and di-tert-butyl peroxide; in step S2, the solvent B is any one of toluene, xylene, tetrahydrofuran, and isopropanol; in step S3, the silane coupling agent is at least one of γ-glycidoxypropyltrimethoxysilane, γ-methacryloxypropyltrimethoxysilane, and γ-aminopropyltriethoxysilane.

[0030] Beneficial effects of the present invention:

[0031] (1) The present invention uses a self-made controllable catalyst (a new platinum catalyst) in silica gel. The catalyst can make silica gel have good stability and long storage period at room temperature, and can efficiently catalyze the hydrosilylation reaction at a certain temperature, which can enable the single-component silicone rubber to cure quickly.

[0032] (2) The phosphine oxide compound used as the controllable catalyst in the one-component addition-type silicone adhesive of the present invention is more stable than the disclosed organophosphine ligand inhibitor, cures faster at high temperatures, and also has a long shelf life.

[0033] (3) The one-component addition-type silicone rubber solution of the present invention can have a good storage period at room temperature and can be quickly cured under high temperature conditions.

[0034] (4) Compared with the inhibitors used in traditional single-component silica gel, the catalytic system used in the present invention has an organic silicon structure, has good compatibility with the organic silica gel system, is not easy to precipitate from the silica gel system, and the organic phosphine oxide structure in the catalytic system has good chemical stability. This structure can also improve the flame retardant properties of silica gel to a certain extent. DETAILED DESCRIPTION

[0035] To make the present invention easier to understand, the present invention is further described below with reference to specific examples. It should be understood that these examples are only used to illustrate the present invention and are not used to limit the scope of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments in the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention. Unless otherwise defined, the professional terms used below are consistent with the meanings understood by professional and technical personnel in this field; unless otherwise specified, the raw materials and reagents involved in this article can be purchased from the market or prepared by known methods.

[0036] Example 1

[0037] A method for preparing a one-component addition-type organosilicon adhesive comprises the following steps:

[0038] S1. Vinyl pentamethyldisiloxane and dimethylphosphine oxide (molar ratio 1:1) are added to toluene, and dibenzoyl peroxide (1 wt.%) is added, and the mixture is reacted at 80° C. for 12 h. The solvent and low-boiling substances are then removed by distillation under reduced pressure to obtain an organosilicon phosphine oxide compound as shown in Formula IV.

[0039]

[0040] S2, adding the platinum-vinylsiloxane complex catalyst and the organosilicon phosphine compound (molar ratio of 1:1) to isopropanol, stirring at room temperature for 12 hours, and then distilling under reduced pressure to obtain a controllable catalyst;

[0041] S3, 20 parts of fumed silica powder and 100 parts of vinyl silicone oil were prepared into a base material by a kneader, and pretreated with hexamethyldisilazane (10 wt.%) to obtain a vinyl-based adhesive;

[0042] S4. Add the above-mentioned vinyl-based adhesive, 5 parts of hydrogenated silicone oil, 0.5 parts of controllable catalyst, and 1 part of tackifier into a planetary machine in sequence, and stir evenly under a vacuum degree of 0.1 MPa to obtain a one-component addition-type silicone adhesive.

[0043] Take some samples of the prepared silica gel for high temperature curing test and record the data. The remaining silica gel is sealed and stored in a bottle. The curing and thickening of the samples are observed at a fixed time frequency.

[0044] Example 2

[0045] A method for preparing a one-component addition-type organosilicon adhesive comprises the following steps:

[0046] S1. Divinyltetramethyldisiloxane and dimethylphosphine oxide (molar ratio of 1:1) are added to toluene, and dibenzoyl peroxide (1 wt.%) is added, and the mixture is reacted at 80° C. for 12 hours, and then the solvent and low-boiling substances are removed by distillation under reduced pressure to obtain an organosilicon phosphine oxide compound, as shown in Formula V;

[0047]

[0048] S2, adding the platinum-vinylsiloxane complex catalyst and the organosilicon phosphine compound (molar ratio of 1:1) to isopropanol, stirring at room temperature for 12 hours, and then distilling under reduced pressure to obtain a controllable catalyst;

[0049] S3, 20 parts of fumed silica powder and 100 parts of vinyl silicone oil were prepared into a base material by a kneader, and pretreated with hexamethyldisilazane (10 wt.%) to obtain a vinyl-based adhesive;

[0050] S4. Add vinyl-based glue, 5 parts of hydrogenated silicone oil, 0.5 parts of controllable catalyst, and 1 part of tackifier into the planetary machine in sequence, and stir evenly under a vacuum degree of 0.1 MPa to obtain a one-component addition-type silicone adhesive.

[0051] Take some samples of the prepared silica gel for high temperature curing test and record the data. The remaining silica gel is sealed and stored in a bottle. The curing and thickening of the samples are observed at a fixed time frequency.

[0052] Example 3

[0053] A method for preparing a one-component addition-type organosilicon adhesive comprises the following steps:

[0054] S1. Divinyltetramethyldisiloxane and dimethylphosphine oxide (molar ratio 1:2) are added to toluene, and dibenzoyl peroxide (1 wt.%) is added, and the mixture is reacted at 80° C. for 12 h. The solvent and low-boiling substances are then removed by distillation under reduced pressure to obtain an organosilicon phosphine oxide compound, as shown in Formula VI.

[0055]

[0056] S2, adding the platinum-vinylsiloxane complex catalyst and the organosilicon phosphine compound (molar ratio of 1:1) to isopropanol, stirring at room temperature for 12 hours, and then distilling under reduced pressure to obtain a controllable catalyst;

[0057] S3, 20 parts of fumed silica powder and 100 parts of vinyl silicone oil were prepared into a base material by a kneader, and pretreated with hexamethyldisilazane (10 wt.%) to obtain a vinyl-based adhesive;

[0058] S4. Add vinyl-based glue, 5 parts of hydrogenated silicone oil, 0.5 parts of controllable catalyst, and 1 part of tackifier into the planetary machine in sequence, and stir evenly under a vacuum degree of 0.1 MPa to obtain a one-component addition-type silicone adhesive.

[0059] Take some samples of the prepared silica gel for high temperature curing test and record the data. The remaining silica gel is sealed and stored in a bottle. The curing and thickening of the samples are observed at a fixed time frequency.

[0060] Example 4

[0061] A method for preparing a one-component addition-type organosilicon adhesive comprises the following steps:

[0062] S1. Adding vinyl-terminated polydimethylsiloxane and dimethylphosphine oxide (molar ratio of 1:1) to toluene, and adding dibenzoyl peroxide (1 wt.%), reacting at 80° C. for 12 h, and then removing the solvent and low-boiling substances by distillation under reduced pressure to obtain an organosilicon phosphine oxide compound, as shown in Formula VII;

[0063]

[0064] S2, adding the platinum-vinylsiloxane complex catalyst and the organosilicon phosphine compound (molar ratio of 1:1) to isopropanol, stirring at room temperature for 12 hours, and then distilling under reduced pressure to obtain a controllable catalyst;

[0065] S3, 20 parts of fumed silica powder and 100 parts of vinyl silicone oil were prepared into a base material by a kneader, and pretreated with hexamethyldisilazane (10 wt.%) to obtain a vinyl-based adhesive;

[0066] S4. Add vinyl-based glue, 5 parts of hydrogenated silicone oil, 0.5 parts of controllable catalyst, and 1 part of tackifier into the planetary machine in sequence, and stir evenly under a vacuum degree of 0.1 MPa to obtain a one-component addition-type silicone adhesive.

[0067] Take some samples of the prepared silica gel for high temperature curing test and record the data. The remaining silica gel is sealed and stored in a bottle. The curing and thickening of the samples are observed at a fixed time frequency.

[0068] Example 5

[0069] A method for preparing a one-component addition-type organosilicon adhesive comprises the following steps:

[0070] S1. Adding vinyl-terminated polydimethylsiloxane and dimethylphosphine oxide (molar ratio of 1:2) to toluene, and adding dibenzoyl peroxide (1 wt.%), reacting at 80° C. for 12 h, and then removing the solvent and low-boiling substances by distillation under reduced pressure to obtain an organosilicon phosphine oxide compound as shown in Formula VIII;

[0071]

[0072] S2, adding the platinum-vinylsiloxane complex catalyst and the organosilicon phosphine compound (molar ratio of 1:1) to isopropanol, stirring at room temperature for 12 hours, and then distilling under reduced pressure to obtain a controllable catalyst;

[0073] S3, 20 parts of fumed silica powder and 100 parts of vinyl silicone oil were prepared into a base material by a kneader, and pretreated with hexamethyldisilazane (10 wt.%) to obtain a vinyl-based adhesive;

[0074] S4. Add vinyl-based glue, 5 parts of hydrogenated silicone oil, 0.5 parts of controllable catalyst, and 1 part of tackifier into the planetary machine in sequence, and stir evenly under a vacuum degree of 0.1 MPa to obtain a one-component addition-type silicone adhesive.

[0075] Take some samples of the prepared silica gel for high temperature curing test and record the data. The remaining silica gel is sealed and stored in a bottle. The curing and thickening of the samples are observed at a fixed time frequency.

[0076] Comparative Example 1

[0077] A method for preparing a one-component addition-type organosilicon adhesive comprises the following steps:

[0078] S1. 20 parts of fumed silica powder and 100 parts of vinyl silicone oil were prepared into a base material by a kneader, and pretreated with hexamethyldisilazane (10 wt.%) to obtain a vinyl-based adhesive;

[0079] S2. The above-mentioned vinyl-based adhesive, 5 parts of hydrogenated silicone oil, 0.5 parts of (acetylene cyclohexanol and platinum-vinylsiloxane complex catalyst (molar ratio 1:1)), and 1 part of tackifier are sequentially added into a planetary machine, and stirred evenly under a vacuum degree of 0.1 MPa to obtain a one-component addition-type silicone adhesive.

[0080] Except for the different catalyst and inhibitor systems, the platinum content, the amounts of other components, the storage temperature and environment in this comparative example are consistent with those in Example 1.

[0081] Take some samples of the prepared silica gel for high temperature curing test and record the data. The remaining silica gel is sealed and stored in a bottle. The curing and thickening of the samples are observed at a fixed time frequency.

[0082] Comparative Example 2

[0083] A method for preparing a one-component addition-type organosilicon adhesive comprises the following steps:

[0084] S1. 20 parts of fumed silica powder and 100 parts of vinyl silicone oil were prepared into a base material by a kneader, and pretreated with hexamethyldisilazane (10 wt.%) to obtain a vinyl-based adhesive;

[0085] S2. Vinyl-based adhesive, 5 parts of hydrogenated silicone oil, 0.5 parts of dimethyl maleate and platinum-vinylsiloxane complex catalyst (molar ratio 1:1) and tackifier are sequentially added into a planetary machine, and stirred evenly under a vacuum degree of 0.1 MPa to obtain a one-component addition-type silicone adhesive.

[0086] Except for the different catalyst and inhibitor systems, the platinum content, the amounts of other components, the storage temperature and environment in this comparative example are consistent with those in Example 1.

[0087] Take some samples of the prepared silica gel for high temperature curing test and record the data. The remaining silica gel is sealed and stored in a bottle. The curing and thickening of the samples are observed at a fixed time frequency.

[0088] Comparative Example 3

[0089] A method for preparing a one-component addition-type organosilicon adhesive comprises the following steps:

[0090] S1, 20 parts of fumed silica powder and 100 parts of vinyl silicone oil are prepared into a base material by a kneader, and pretreated with hexamethyldisilazane to obtain a vinyl-based adhesive;

[0091] S2. Vinyl-based glue, 5 parts of hydrogenated silicone oil, 0.5 parts of (vinyl pentamethyldisiloxane and platinum-vinylsiloxane complex (molar ratio 1:1)), and 1 part of tackifier are sequentially added into a planetary machine, and stirred evenly under a vacuum degree of 0.1 MPa to obtain a one-component addition-type silicone adhesive.

[0092] Except for the different catalyst and inhibitor systems, the platinum content, the amounts of other components, the storage temperature and environment in this comparative example are consistent with those in Example 1.

[0093] Take some samples of the prepared silica gel for high temperature curing test and record the data. The remaining silica gel is sealed and stored in a bottle. The curing and thickening of the samples are observed at a fixed time frequency.

[0094] Comparative Example 4

[0095] A method for preparing a one-component addition-type organosilicon adhesive comprises the following steps:

[0096] S1. 20 parts of fumed silica powder and 100 parts of vinyl silicone oil were prepared into a base material by a kneader, and pretreated with hexamethyldisilazane (10 wt.%) to obtain a vinyl-based adhesive;

[0097] S2. Vinyl-based glue, 5 parts of hydrogenated silicone oil, 0.5 parts of dimethylphosphine oxide and platinum-vinylsiloxane complex (molar ratio 1:1), and 1 part of tackifier are sequentially added into a planetary machine, and stirred evenly under a vacuum degree of 0.1 MPa to obtain a one-component addition-type silicone adhesive.

[0098] Except for the different catalyst and inhibitor systems, the platinum content, the amounts of other components, the storage temperature and environment in this comparative example are consistent with those in Example 1.

[0099] Take some samples of the prepared silica gel for high temperature curing test and record the data. The remaining silica gel is sealed and stored in a bottle. The curing and thickening of the samples are observed at a fixed time frequency.

[0100] Performance testing and result analysis:

[0101] Storage performance testing of the silica gels prepared in Examples 1-5 and Comparative Examples 1-4: Examples 1-5 and Comparative Examples 1-4 were placed in the same environment to test their high-temperature curing speed and storage period in normal packaging. The room-temperature test measured the initial curing time (gel formation), with the storage conditions for the room-temperature test sealed. The high-temperature curing test time represents the time required for the silica gel to fully cure. The results are shown in Table 1 below:

[0102] Table 1:

[0103]

[0104] As shown in Table 1, the storage period of Examples 1 to 5 is significantly longer than that of Comparative Examples 1 and 2 using conventional inhibitors, and the curing speeds at high temperatures are similar, indicating that the controllable catalyst of the present invention can guarantee a longer storage period while maintaining a high-temperature curing speed compared to conventional inhibitors. In fact, groups with coordination ability have more or less inhibitory effects on platinum catalysts. Among the five embodiments of the present application, the storage time of Example 1 is relatively short because it only has a single-ended phosphine oxide structure and does not contain a vinyl group, and its inhibitory ability is relatively weak. The controllable catalyst of the double-ended phosphine oxide structure has a stronger inhibitory ability than the single-ended one, and the storage period will be longer, but it will slightly affect the curing speed at high temperatures. For Examples 2 and 4, since they have vinyl groups, they can participate in the hydrosilylation reaction in the silica gel component and become part of the silica gel cross-linked structure. Therefore, the product as a whole is relatively more stable, and after the product is cured into a gel, it is not easily affected by external influences and causes exudation. Under normal storage, both the phosphine oxide structure and the vinyl group can inhibit. While Comparative Examples 1, 2, and 3 cure quickly at high temperatures, they have a short shelf life. Furthermore, Comparative Examples 1 and 2 do not participate in the silicone curing reaction, potentially leading to exudation. While Comparative Example 4 contains an organosilicon component and the vinyl group has a certain inhibitory effect, its actual performance is significantly inferior to that of the examples. While Comparative Example 5 has a good shelf life, its pure phosphine oxide structure is poorly compatible with the silicone system, making it susceptible to exudation due to external factors.

[0105] The controllable catalyst relative effect of five embodiments of the present invention is preferably embodiment 4, which can ensure good shelf life under the curing demand of ensuring normal construction, and inhibitor (organic silicon phosphine compound) can participate in silica gel curing reaction, will not release material at high temperature and affect environment. The silica gel prepared by embodiment has good tensile properties and bonding strength, and workability is excellent and has excellent shelf life. The inhibition principle of the inhibitor (organic silicon phosphine compound) of the present application is all to have the group of unshared electrons and to coordinate with the empty electron orbit, so as to limit the coordination catalytic activity of platinum catalyst at room temperature, the difficulty of coordination bond fracture at high temperature has just become the key of high temperature curing speed, the coordination ability of phosphine oxide structure mainly comes from oxygen, and relatively organophosphine structure is slightly weaker, thus can recover coordination catalytic activity faster at high temperature, so as to be able to fast cure.

[0106] The above description is merely a specific embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any changes or substitutions that can be easily conceived by a person skilled in the art within the technical scope disclosed in the present invention should be included in the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be based on the scope of protection of the claims.

Claims

1. A one-component addition-type silicone adhesive, characterized in that: The one-component addition-type silicone adhesive is composed of the following raw materials in parts by weight: 100 parts of vinyl silicone oil; 5-15 parts of cross-linking agent; 0.5-2 parts of controllable catalyst; 1-2 parts of tackifier; 10-50 parts of reinforcing filler; Wherein, the controllable catalyst is compounded by a platinum catalyst and an organic silicon phosphine compound; The organosilicon phosphine oxide compound is prepared by reacting a siloxane containing a vinyl functional group with an alkane phosphine oxide; the reaction is carried out at 60-100° C. and in the presence of an initiator; the structural formula of the alkane phosphine oxide is shown in Formula II: ; Formula II; In formula II, R2 is an alkyl group or a phenyl group.

2. The one-component addition-type silicone adhesive according to claim 1, characterized in that: The structural formula of the vinyl functional group-containing siloxane is shown in Formula I, and the organic silicon phosphine compound is shown in Formula III: ; Formula I; ; Formula III; Wherein, in Formula I and Formula III, n is 1-5, R1 is one of methyl and ethyl, and R3 is one of methyl, ethyl and vinyl.

3. The one-component addition-type silicone adhesive according to claim 1, characterized in that: The siloxane containing vinyl functional groups is vinyl terminated polydimethylsiloxane.

4. The one-component addition-type silicone adhesive according to claim 1, characterized in that: The viscosity of the vinyl silicone oil is 100-2000 mPa·s, and the vinyl content in the vinyl silicone oil is 0.1-0.5 wt.%.

5. The one-component addition-type silicone adhesive according to claim 1, characterized in that: The cross-linking agent is hydrogen-containing silicone oil, which is a branched hydrogen-containing silicone oil. The hydrogen content in the hydrogen-containing silicone oil is 0.1-1.0 wt.%.

6. The one-component addition-type silicone adhesive according to claim 1, characterized in that: The platinum content of the controllable catalyst is 1000-5000 ppm.

7. The one-component addition-type silicone adhesive according to claim 1, characterized in that: The reinforcing filler is one or more of fumed silica, precipitated silica, silicone resin, calcium carbonate, silicon micropowder, aluminum oxide, silicon carbide, and silicon nitride.

8. A method for preparing a one-component addition-type organosilicon adhesive according to any one of claims 1 to 7, characterized in that: The following steps are involved: S1. Adding a vinyl functional group-containing siloxane and an alkane phosphine oxide in a specific ratio to solvent A, and adding an initiator, reacting at 60-100° C. for 4-12 hours, and then distilling under reduced pressure to obtain an organosilicon phosphine oxide compound; S2, adding the platinum catalyst and the organosilicon phosphine compound to solvent B, stirring at room temperature for 4-12 hours, and then distilling under reduced pressure to obtain a controllable catalyst; S3, preparing a base material by kneading the reinforcing filler powder and vinyl silicone oil, and pre-treating it with a silane coupling agent or hexamethyldisilazane to obtain a vinyl-based adhesive; S4. Add vinyl-based adhesive, cross-linking agent, controllable catalyst and tackifier into the planetary machine in sequence, and stir evenly under a vacuum degree of 0.1 MPa to obtain a single-component addition-type silicone adhesive.

9. The preparation method according to claim 8, characterized in that In step S1, the solvent A is any one of toluene, xylene, tetrahydrofuran, and isopropanol; the initiator is any one of dibenzoyl peroxide, tert-butyl perbenzoate, diisopropyl peroxide, and di-tert-butyl peroxide; in step S2, the solvent B is any one of toluene, xylene, tetrahydrofuran, and isopropanol; in step S3, the silane coupling agent is at least one of γ-glycidyloxypropyltrimethoxysilane, γ-methacryloxypropyltrimethoxysilane, and γ-aminopropyltriethoxysilane.

Citation Information

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