CN116004182A - Anti-poisoning bi-component addition type organic silicon pouring sealant and preparation method thereof - Google Patents
Anti-poisoning bi-component addition type organic silicon pouring sealant and preparation method thereof Download PDFInfo
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- CN116004182A CN116004182A CN202211297946.XA CN202211297946A CN116004182A CN 116004182 A CN116004182 A CN 116004182A CN 202211297946 A CN202211297946 A CN 202211297946A CN 116004182 A CN116004182 A CN 116004182A
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Abstract
The invention discloses an anti-poisoning double-component addition type organic silicon pouring sealant and a preparation method thereof, wherein the organic silicon pouring sealant comprises a component A and a component B, and the component A comprises, by mass, 24-60 parts of vinyl silicone oil, 0.05-1 part of a silicon-oxygen addition reaction catalyst, 0.05-1 part of a condensation reaction catalyst and 39-75 parts of a filler; the component B comprises, by mass, 20-40 parts of vinyl silicone oil, 30-70 parts of filler, 1-10 parts of hydrogen-containing silicone oil, 1-10 parts of trimethoxy terminated organosilicon polymer and 0.1-2 parts of tackifier. The condensation reaction catalyst and the trimethoxy terminated organosilicon polymer are introduced into the organosilicon pouring sealant, so that the problem of catalyst poisoning frequently existing in addition organosilicon pouring sealants is effectively solved.
Description
Technical Field
The invention belongs to the technical field of organic silicon pouring sealants, and particularly relates to an anti-poisoning double-component addition type organic silicon pouring sealant and a preparation method thereof.
Background
The organic silicon polymer material has unique weather resistance and ageing resistance due to a special silicon-oxygen bond main chain structure, excellent high and low temperature resistance, good hydrophobicity, mechanical property, electrical insulation and other properties, so that the organic silicon polymer material is widely used for encapsulation protection of electronic and electric elements and mainly plays a role in protection such as sealing, moisture resistance, dust resistance, heat conduction, flame retardance and the like. The two-component addition type organic silicon pouring sealant is favored by people because of high curing speed and no curing byproducts. Generally, it is mainly formed by hydrosilylation reaction of vinyl silicone oil and hydrogen-containing silicone oil under the action of a platinum catalyst to form a cured cross-linked product. Since the platinum catalyst in its composition is easily blocked by impurities in the electronic components or the case, the potting adhesive is not cured or is not cured completely (also commonly referred to as catalyst poisoning), so that its use is affected.
Disclosure of Invention
Aiming at the technical problems, the invention provides the anti-poisoning bi-component addition type organic silicon pouring sealant and the preparation method thereof, and the condensation reaction catalyst and the trimethoxy terminated organic silicon polymer are introduced into the organic silicon pouring sealant, so that the catalyst poisoning problem frequently existing in the addition type organic silicon pouring sealant is effectively solved.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
an anti-poisoning double-component addition type organic silicon pouring sealant comprises a component A and a component B, wherein the component A comprises, by mass, 24-60 parts of vinyl silicone oil, 0.05-1 part of a silicon-oxygen addition reaction catalyst, 0.05-1 part of a condensation reaction catalyst and 39-75 parts of a filler;
the component B comprises, by mass, 20-40 parts of vinyl silicone oil, 30-70 parts of filler, 1-10 parts of hydrogen-containing silicone oil, 1-10 parts of trimethoxy terminated organosilicon polymer and 0.1-2 parts of tackifier.
Preferably, the trimethoxy terminated silicone polymer is a trimethoxy terminated polydimethylsiloxane.
Preferably, the condensation reaction catalyst is a chelated titanium compound or phthalate ester.
Preferably, the phthalate is a tetraalkoxy phthalate, a tetrabutyl phthalate or an isopropylacetyl acetonate phthalate or a mixture thereof.
Preferably, the silicon-oxygen addition reaction catalyst is a platinum catalyst.
Preferably, the platinum catalyst is platinum chloride, chloroplatinic acid, an alcoholic solution of chloroplatinic acid, or a reactant of chloroplatinic acid and an alcohol, or a reactant of chloroplatinic acid and an olefinic compound, or a reactant of chloroplatinic acid and a vinyl-containing siloxane, or a platinum-olefin complex, or a complex of platinum-vinyl-containing siloxane.
Preferably, the filler of the A component and the B component is at least one of silicon dioxide, aluminum oxide, aluminum hydroxide or calcium carbonate or a mixture thereof respectively.
Preferably, the tackifier is a silane coupling agent, the silane coupling agent comprises a siloxy group and an organic group, and the organic group can be any one of an isocyanurate group, an allyl group or an epoxy group.
The invention also provides a preparation method of the anti-poisoning double-component addition type organic silicon pouring sealant, which comprises the steps of uniformly mixing and stirring the component A and the component B of the anti-poisoning double-component addition type organic silicon pouring sealant according to the mass ratio of 1:1, curing in an oven, and curing in the oven at 60 ℃ generally for 1h.
By adopting the technical scheme, the invention has the following advantages and positive effects compared with the prior art:
in the organic silicon pouring sealant, a condensation reaction catalyst is added in the component A, a trimethoxy terminated organic silicon polymer is added in the component B, a condensation type curing system is introduced in an addition type curing system, and the organic silicon pouring sealant is formed in the addition/condensation type dual-curing system. After the component A and the component B are mixed, the trimethoxy terminated organosilicon polymer is solidified at the interface of the colloid and the base material under the action of the condensation reaction catalyst, which is equivalent to forming a protective layer, thereby effectively avoiding the addition type solidified part in the system from being interfered by impurities, improving the problem of catalyst poisoning and having high use value.
Detailed Description
The anti-poisoning bi-component addition type organic silicon pouring sealant and the preparation method thereof are described in further detail below with reference to specific embodiments. The advantages and features of the present invention will become more apparent from the following description.
The organic silicon is widely used in the electronic field, and mainly comprises addition type curing and condensation type curing in terms of curing mode. Among them, addition type curing generally uses a platinum catalyst, but the platinum catalyst is relatively sensitive to impurities in electronic components or housings, and is easily affected by the platinum catalyst, so that the colloid cannot be cured or is not cured completely (also commonly referred to as catalyst poisoning), so that the use of the platinum catalyst is affected.
In order to solve the problem of poisoning of the addition type silicone potting adhesive, it is common practice to increase the amount of catalyst in the composition or to clean/clean the electronic components and the potting case, which increases the formulation cost and increases the use process for the customer, and the effect is not very ideal.
The anti-poisoning double-component addition type organosilicon pouring sealant provided by the invention contains a condensation reaction catalyst and trimethoxy end-capped organosilicon polymer, and specifically comprises a component A and a component B, wherein the component A comprises, by mass, 24-60 parts of vinyl silicone oil, 0.05-1 part of a siloxane addition reaction catalyst, 0.05-1 part of the condensation reaction catalyst and 39-75 parts of a filler;
the component B comprises 20-40 parts by mass of vinyl silicone oil, 30-70 parts by mass of filler, 1-10 parts by mass of hydrogen-containing silicone oil, 1-10 parts by mass of trimethoxy end-capped organosilicon polymer and 0.1-2 parts by mass of tackifier.
The trimethoxy terminated silicone polymer is preferably trimethoxy terminated polydimethylsiloxane.
The invention adds a condensation type curing system into the original addition type curing system, belonging to an addition/condensation dual-curing system. Unlike addition-type curing, condensation-type curing is insensitive to impurities. The trimethoxy end-capped polydimethylsiloxane is firstly solidified at the interface of the colloid and the base material under the action of the condensation reaction catalyst, which is equivalent to forming a protective layer, so that the addition-type solidified part in the system can be effectively prevented from being interfered by impurities, the problem of catalyst poisoning can be solved, and the catalyst has great use value. The organic silicon pouring sealant can improve the problem of catalyst poisoning, and can not increase the formula cost and the using procedures of customers.
The condensation catalyst is a chelated titanium compound or phthalate ester. Wherein the phthalate is tetraalkoxy phthalate, tetrabutyl phthalate or isopropyl acetyl acetonate phthalate or mixture thereof.
The silicon-oxygen addition reaction catalyst is a platinum catalyst, wherein the platinum catalyst is platinum chloride, chloroplatinic acid, an alcohol solution of chloroplatinic acid, a reactant of chloroplatinic acid and alcohol, a reactant of chloroplatinic acid and olefin compounds, a reactant of chloroplatinic acid and vinyl-containing siloxane, a platinum-olefin complex, a platinum-vinyl-containing siloxane complex or the like.
The filler of the component A and the filler of the component B are at least one of silicon dioxide, aluminum oxide, aluminum hydroxide or calcium carbonate or the mixture thereof respectively.
The tackifier is a silane coupling agent, the silane coupling agent comprises a siloxy group and an organic group, and the organic group can be any one of an isocyanurate group, an allyl group or an epoxy group.
The invention also provides a preparation method of the anti-poisoning double-component addition type organic silicon pouring sealant, which comprises the steps of uniformly mixing and stirring the component A and the component B of the anti-poisoning double-component addition type organic silicon pouring sealant according to the mass ratio of 1:1, curing in an oven, and curing in the oven at 60 ℃ generally for 1h.
The following will illustrate the invention in more detail with reference to specific examples
Example 1
An anti-poisoning double-component addition type organic silicon pouring sealant comprises a component A and a component B:
the component A comprises the following raw materials in parts by weight:
vinyl silicone oil, 40wt%;
0.2wt% of a hydrosilylation catalyst;
0.1wt% of a condensation reaction catalyst;
silica, 59.7wt%;
the component B comprises the following raw materials in parts by weight:
vinyl silicone oil, 28wt%;
alumina, 59wt%;
hydrogen-containing silicone oil, 7wt%;
trimethoxy-terminated polydimethylsiloxane, 5wt%;
isocyanurate group, 1wt%.
Example 2
An anti-poisoning double-component addition type organic silicon pouring sealant comprises a component A and a component B: the component A comprises the following raw materials in parts by weight:
vinyl silicone oil, 40wt%;
0.2wt% of a hydrosilylation catalyst;
0.1wt% of a condensation reaction catalyst;
59.7wt% of aluminum hydroxide;
the component B comprises the following raw materials in parts by weight:
vinyl silicone oil, 24wt%;
alumina, 59wt%;
hydrogen-containing silicone oil, 7wt%;
trimethoxy-terminated polydimethylsiloxane, 9wt%;
isocyanurate group, 1wt%.
Comparative example 1
The addition type organic silicon pouring sealant comprises a component A and a component B:
the component A comprises the following raw materials in parts by weight:
vinyl silicone oil, 40wt%;
0.2wt% of a hydrosilylation catalyst;
silica, 59.8wt%;
the component B comprises the following raw materials in parts by weight:
vinyl silicone oil, 32wt%;
alumina, 59wt%;
8wt% of hydrogen-containing silicone oil;
isocyanurate group, 1wt%.
Comparative example 2
The addition type organic silicon pouring sealant comprises a component A and a component B:
the component A comprises the following raw materials in parts by weight:
vinyl silicone oil, 40wt%;
0.6wt% of a hydrosilylation catalyst;
59.4wt% of aluminum hydroxide;
the component B comprises the following raw materials in parts by weight:
vinyl silicone oil, 32wt%;
alumina, 59wt%;
8wt% of hydrogen-containing silicone oil;
isocyanurate group, 1wt%.
Comparative example 3
The addition type organic silicon pouring sealant comprises a component A and a component B:
the component A comprises the following raw materials in parts by weight:
vinyl silicone oil, 40wt%;
0.2wt% of a hydrosilylation catalyst;
0.1wt% of a condensation reaction catalyst;
silica, 59.7wt%;
the component B comprises the following raw materials in parts by weight:
vinyl silicone oil, 32wt%;
alumina, 59wt%;
8wt% of hydrogen-containing silicone oil;
isocyanurate group, 1wt%.
Comparative example 4
The addition type organic silicon pouring sealant comprises a component A and a component B:
the component A comprises the following raw materials in parts by weight:
vinyl silicone oil, 40wt%;
0.2wt% of a hydrosilylation catalyst;
59.8wt% of aluminum hydroxide;
the component B comprises the following raw materials in parts by weight:
vinyl silicone oil, 28wt%;
alumina, 59wt%;
hydrogen-containing silicone oil, 7wt%;
trimethoxy-terminated polydimethylsiloxane, 5wt%;
isocyanurate group, 1wt%.
The types of raw materials used in examples 1 to 2 and comparative examples and mass fractions of the respective raw materials in the whole silicone potting adhesive are shown in table 1. A, B components of the pouring sealant obtained in each example and comparative example are prepared by the following components in percentage by mass: 1 are uniformly mixed and stirred, then are smeared on the same base material, and are cured for 1h by an oven at 60 ℃, and the hardness is tested, and specific test data are shown in table 2.
TABLE 1 raw materials and mass fraction of raw materials in each of examples and comparative examples
Table 2 hardness results for examples and comparative examples
Hardness of | |
Example 1 | Shore A 23 |
Example 2 | Shore A 36 |
Comparative example 1 | Uncured state |
Comparative example 2 | Shore 00 40 |
Comparative example 3 | Uncured state |
Comparative example 4 | Uncured state |
As can be seen from the results in table 2, comparative examples 1 and 3 to 4 are cured, and comparative example 2 is cured but the hardness after curing is significantly lower than that of examples 1 and 2. Comparative examples 3 and 4 illustrate that the condensation reaction catalyst and trimethoxy terminated polydimethylsiloxane in the present invention are indispensible and require a combination of curing at the interface of the colloid and the substrate to form a "protective layer" over the substrate, thereby avoiding the interference of impurities in the addition-type cured portion of the system, fully curing, and improving the catalyst poisoning problem, and thus the hardness of examples 1 and 2 is much higher than that of comparative examples. Comparative examples 1-2 were free of condensation catalyst and trimethoxy terminated polydimethylsiloxane, comparative example 1 was uncured, and comparative example 2 was cured, but the hardness after curing was Shore 00 40, the hardness was very small, indicating incomplete cure. The results of comparative examples 1-2 showed no condensation reaction catalyst and trimethoxy-terminated polydimethylsiloxane in the casting compound material, and only the addition-type cured portion of the casting compound system resulted in catalyst poisoning.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the above embodiments. Even if various changes are made to the present invention, it is within the scope of the appended claims and their equivalents to fall within the scope of the invention.
Claims (9)
1. The anti-poisoning double-component addition type organic silicon pouring sealant is characterized by comprising a component A and a component B, wherein the component A comprises, by mass, 24-60 parts of vinyl silicone oil, 0.05-1 part of a silicon-oxygen addition reaction catalyst, 0.05-1 part of a condensation reaction catalyst and 39-75 parts of a filler;
the component B comprises, by mass, 20-40 parts of vinyl silicone oil, 30-70 parts of filler, 1-10 parts of hydrogen-containing silicone oil, 1-10 parts of trimethoxy terminated organosilicon polymer and 0.1-2 parts of tackifier.
2. The poisoning-resistant two-component addition type silicone potting adhesive of claim 1, wherein the trimethoxy terminated silicone polymer is trimethoxy terminated polydimethylsiloxane.
3. The anti-poisoning two-component addition type silicone potting adhesive according to claim 1, wherein the condensation reaction catalyst is a chelated titanium compound or phthalate ester.
4. The poisoning-resistant two-component addition type silicone potting adhesive according to claim 3, wherein the phthalate is tetraalkoxy phthalate, tetrabutyl phthalate, or isopropyl acetyl acetonate phthalate, or a mixture thereof.
5. The poisoning-resistant two-component addition type silicone pouring sealant according to claim 1, wherein the silicon-oxygen addition reaction catalyst is a platinum catalyst.
6. The anti-poisoning two-component addition type silicone potting adhesive according to claim 5, wherein the platinum catalyst is platinum chloride, chloroplatinic acid, an alcohol solution of chloroplatinic acid, a reactant of chloroplatinic acid and an alcohol, a reactant of chloroplatinic acid and an olefin compound, a reactant of chloroplatinic acid and a vinyl-containing siloxane, or a platinum-olefin complex, or a complex of platinum-vinyl-containing siloxane.
7. The anti-poisoning two-component addition type silicone pouring sealant according to claim 1, wherein the filler of the a component and the B component is at least one of silica, alumina, aluminum hydroxide, calcium carbonate, or a mixture thereof, respectively.
8. The anti-poisoning two-component addition type silicone potting adhesive according to claim 1, wherein the adhesion promoter is a silane coupling agent, and the silane coupling agent is an adhesion promoter of isocyanurate group, allyl group or epoxy group and siloxy group.
9. The preparation method of the poisoning-resistant double-component addition type organic silicon pouring sealant according to any one of claims 1 to 8, wherein the A component and the B component of the poisoning-resistant double-component addition type organic silicon pouring sealant are uniformly mixed and stirred according to a mass ratio of 1:1, and are cured in an oven.
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