CN113789148A - Organic silicon foaming pouring sealant and preparation method thereof - Google Patents

Organic silicon foaming pouring sealant and preparation method thereof Download PDF

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Publication number
CN113789148A
CN113789148A CN202111139165.3A CN202111139165A CN113789148A CN 113789148 A CN113789148 A CN 113789148A CN 202111139165 A CN202111139165 A CN 202111139165A CN 113789148 A CN113789148 A CN 113789148A
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parts
component
pouring sealant
raw materials
foaming
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谢冬
柯明新
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Jiangsu Csi Material Technology Co ltd
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Jiangsu Csi Material Technology Co ltd
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Priority to CN202111139165.3A priority Critical patent/CN113789148A/en
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2296Oxides; Hydroxides of metals of zinc
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant

Abstract

The invention discloses an organic silicon foaming pouring sealant and a preparation method thereof, and belongs to the technical field of pouring materials. The pouring sealant comprises a component A and a component B, wherein the component A comprises the following components in parts by weight: 50-80 parts of vinyl polysiloxane, 1-5 parts of alpha, omega-hydroxyl-terminated liquid silicone rubber, 40-60 parts of inorganic flame retardant, 1.0-10.0 parts of auxiliary agent, 0.1-0.5 part of anti-settling agent and 0.5-1.0 part of platinum catalyst; the component B comprises the following components in parts by weight: 50-80 parts of alpha, omega-hydroxyl-terminated liquid silicone rubber, 3-5 parts of hydrogen-containing silicone oil, 40-60 parts of inorganic flame retardant, 1.0-10.0 parts of auxiliary agent, 0.5-1.0 part of carbon black, 0.5-1.0 part of anti-settling agent and 0.01-0.02 part of polymerization inhibitor. The organic silicon foaming pouring sealant has the advantages of low hardness, good elasticity, low thermal conductivity, good flame retardance, good fluidity, easy encapsulation, simple and convenient storage and long shelf life, and has wide application prospect.

Description

Organic silicon foaming pouring sealant and preparation method thereof
Technical Field
The invention relates to an organic silicon foaming pouring sealant and a preparation method thereof, belonging to the technical field of pouring materials.
Background
In the pouring sealant industry, there are three major potting materials, epoxy resin pouring sealant, polyurethane pouring sealant and organic silicon pouring sealant. The main defects of the epoxy resin pouring sealant are that the repairability after the potting is poor, the epoxy resin pouring sealant cannot simultaneously have good high and low temperature resistance, the heat productivity in the curing process is large, and the impact damage resistance is poor. The polyurethane pouring sealant has certain toxicity and poor temperature resistance, can release heat in the curing process, generates certain stress and has poor weather resistance. The organic silicon pouring sealant is basically non-toxic, is mostly an elastomer material after being cured, has low linear expansion coefficient, basically has no stress damage to components, can be repaired after being cured, and has good high and low temperature impact resistance, good weather resistance, good ultraviolet resistance and better insulating property, so the organic silicon pouring sealant is more and more favored by people.
Although people have made a great deal of research on the organosilicon pouring sealant foam material, the organosilicon pouring sealant foam material has the advantages of low density, low thermal conductivity, high flame retardant property, room temperature curing, addition and condensation type curing adhesives, and a few products are available, wherein the chemical dehydrogenation foaming method is simple and easy to operate.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides the organosilicon foaming pouring sealant which has low density, low thermal conductivity, high flame retardant property and room temperature curing property and the preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that: the organic silicon foaming pouring sealant comprises a component A and a component B, wherein the component A comprises the following components in parts by weight: 50-80 parts of vinyl polysiloxane, 1-5 parts of alpha, omega-hydroxyl-terminated liquid silicone rubber, 40-60 parts of inorganic flame retardant, 1.0-10.0 parts of auxiliary agent, 0.1-0.5 part of anti-settling agent and 0.5-1.0 part of platinum catalyst;
the component B comprises the following components in parts by weight: 50-80 parts of alpha, omega-hydroxyl-terminated liquid silicone rubber, 3-5 parts of hydrogen-containing silicone oil, 40-60 parts of inorganic flame retardant, 1.0-10.0 parts of auxiliary agent, 0.5-1.0 part of carbon black, 0.5-1.0 part of anti-settling agent and 0.01-0.02 part of polymerization inhibitor.
The viscosity of the vinyl polysiloxane and the alpha, omega-hydroxyl-terminated liquid silicone rubber at 25 ℃ is 1000-5000 cps.
Although the inorganic flame retardant can improve the flame retardant performance of the halogen-free flame retardant organosilicon potting adhesive, the physical and mechanical properties and the fluidity of the potting adhesive are damaged. The invention adopts the mixture of vinyl polysiloxane with the viscosity of 1000-5000cps at 25 ℃ and alpha, omega-hydroxyl-terminated liquid silicon rubber as a base, and can adjust the vinyl content of the base adhesive, so that the pouring sealant has excellent fluidity and better performance.
As a preferred embodiment of the silicone foaming pouring sealant of the invention, the mass ratio of the vinyl polysiloxane to the α ω -hydroxyl-terminated liquid silicone rubber is vinyl polysiloxane: the alpha omega-hydroxyl-terminated liquid silicone rubber is 1: 1-3.
The inventor finds that when the mass ratio of the vinyl polysiloxane to the alpha, omega-hydroxyl-terminated liquid silicone rubber is vinyl polysiloxane: when the alpha, omega-hydroxyl-terminated liquid silicone rubber is 1: 1-3, the performance of the organic silicon foaming pouring sealant is good.
As a preferred embodiment of the organic silicon foaming pouring sealant, the vinyl contents of the vinyl polysiloxane in the component A and the component B are independently selected from 0.18-0.38%.
As the vinyl content in the vinyl silicone oil increases, the crosslink density increases, the hardness, tensile strength of the vulcanizate increases, and the elongation and compression set decrease. Vulcanizates exhibit a relatively low tear strength at lower vinyl contents because of the low number of crosslinking points, while at too high vinyl contents, too much crosslinking results in "embrittlement" of the vulcanizate, which also results in a decrease in tear strength. A suitable vinyl content therefore leads to a comparatively high strength.
As a preferred embodiment of the organic silicon foaming pouring sealant, the auxiliary agent is surface-modified hollow glass beads, and the average particle size is 75 μm.
As a preferred embodiment of the silicone foaming pouring sealant of the present invention, the inorganic flame retardant is at least one of aluminum hydroxide and zinc oxide.
As a preferred embodiment of the organic silicon foaming pouring sealant, the anti-settling agent is surface-modified fumed silica with the particle size of 20-30 nm.
As a preferable embodiment of the organic silicon foaming pouring sealant, the hydrogen-containing silicone oil is high hydrogen-containing silicone oil.
The hydrogen-containing silicone oil is a cross-linking agent of the addition type organic silicon pouring sealant, and the molecular structure and the molecular mass of the hydrogen-containing silicone oil not only influence the structure and the performance of vulcanized rubber, but also influence the corresponding vulcanization process, so the position, the content and the molecular mass of active hydrogen in the hydrogen-containing silicone oil are controlled, and the cross-linking agent has proper activity so as to ensure the service life of a rubber material. When the amount of the hydrogen-containing silicone oil added is too small, the curing reaction is incomplete and the surface is sticky, but when the amount is too large, the residual hydrogen-containing silicone oil undergoes a dehydrogenation side reaction under the action of a platinum catalyst, and a plurality of bubbles are formed on the surface and in the rubber material.
As a preferred embodiment of the organic silicon foaming pouring sealant, the concentration of the platinum catalyst is 5000 ppm.
As a preferred embodiment of the organic silicon foaming pouring sealant, the polymerization inhibitor is ethynyl cyclohexanol.
On the other hand, the invention provides a preparation method of the organic silicon foaming pouring sealant, which comprises the following steps:
(1) weighing raw materials of the component A according to a proportion, premixing the raw materials except the catalyst and the auxiliary agent by a planetary stirrer, mixing the raw materials to be uniform and fine by a three-roll grinder, adding the catalyst and the auxiliary agent, and uniformly mixing the mixture by the planetary stirrer to obtain the component A;
(2) weighing raw materials of the component B according to a proportion, premixing the raw materials except the polymerization inhibitor and the auxiliary agent by a planetary mixer, mixing the raw materials by a three-roll grinder until the raw materials are uniform and fine, adding the polymerization inhibitor and the auxiliary agent, and uniformly mixing the raw materials by the planetary mixer to obtain the component B;
(3) and mixing the component A and the component B, and foaming to obtain the organic silicon foaming pouring sealant.
Compared with the prior art, the invention has the beneficial effects that:
Detailed Description
To better illustrate the objects, aspects and advantages of the present invention, the present invention will be further described with reference to specific examples.
Examples 1 to 5
The components of the silicone foaming pouring sealant of examples 1-5 of the present invention are shown in table 1 below.
Wherein, the viscosity of the vinyl polysiloxane of the embodiment 1-5 at 25 ℃ is 1000-5000cps, and the viscosity of the alpha omega-hydroxyl-terminated liquid silicone rubber at 25 ℃ is 1000-5000 cps;
the vinyl contents of the vinyl polysiloxane in the component A and the component B are independently selected from 0.18 to 0.38 percent;
the auxiliary agent is surface modified hollow glass beads, and the average particle size is 75 micrometers.
The inorganic flame retardant is at least one of aluminum hydroxide and zinc oxide.
The anti-settling agent is surface modified fumed silica, and the particle size is 20-30 nm.
The hydrogen-containing silicone oil is high hydrogen-containing silicone oil, and the hydrogen content is 1.5%.
The concentration of the platinum catalyst is 5000 ppm.
The polymerization inhibitor is ethynyl cyclohexanol.
The preparation method of the organic silicon foaming pouring sealant in the embodiments 1-5 of the invention comprises the following steps:
(1) putting the inorganic flame retardant, the carbon black, the auxiliary agent and the fumed silica into an oven, heating to 100 ℃, and drying for 2 hours;
(2) weighing raw materials of the component A according to a proportion, premixing the raw materials except the catalyst and the auxiliary agent by a planetary stirrer, mixing the raw materials to be uniform and fine by a three-roll grinder, adding the catalyst and the auxiliary agent, and uniformly mixing the mixture by the planetary stirrer to obtain the component A;
(3) weighing raw materials of the component B according to a proportion, premixing the raw materials except the polymerization inhibitor and the auxiliary agent by a planetary mixer, mixing the raw materials by a three-roll grinder until the raw materials are uniform and fine, adding the polymerization inhibitor and the auxiliary agent, and uniformly mixing the raw materials by the planetary mixer to obtain the component B;
(4) and mixing the component A and the component B, and standing at room temperature for 24 hours to obtain the organic silicon foaming pouring sealant.
TABLE 1
Figure BDA0003281588990000051
The organosilicon foaming pouring sealant obtained by the method is used for testing performance, and the performance testing method and results are shown in table 2.
TABLE 2
Figure BDA0003281588990000061
As can be seen from Table 2, the organosilicon foaming pouring sealant disclosed by the invention is low in hardness, good in elasticity, low in thermal conductivity, good in flame retardance and good in fluidity, is beneficial to pouring, is simple and convenient to store, is long in quality guarantee period, and has wide application prospects.
Effect example 1
The effect example investigates the influence of the mass ratio of the vinyl polysiloxane and the alpha, omega-hydroxyl-terminated liquid silicone rubber on the performance of the organic silicon foaming encapsulating glue. The specific method for investigation is as follows: in this effect example, the organosilicon potting adhesives of test groups 1 to 5 were prepared according to the preparation methods of the organosilicon potting adhesives described in examples 1 to 5. Test groups 1 to 5 the silicone potting compounds were the same except that the silicone potting compounds were different from those of example 1 in the mass ratio of vinyl polysiloxane to α, ω -hydroxyl terminated liquid silicone rubber. The performance of the silicone pouring sealant prepared in this effect example was tested according to the performance test method of the silicone pouring sealant of examples 1-5, and the results are shown in Table 3.
TABLE 3
Figure BDA0003281588990000062
Figure BDA0003281588990000071
Compared with the test groups 1-5, for the organic silicon pouring sealant of the invention, on the premise of a certain amount of hydrogen-containing silicone oil, the mass ratio of the vinyl polysiloxane and the alpha, omega-hydroxyl-terminated liquid silicone rubber has a great influence on the mechanical properties of the pouring sealant, and as can be seen from the above experimental results, as the mass ratio of the vinyl polysiloxane and the alpha, omega-hydroxyl-terminated liquid silicone rubber increases, the hardness, the apparent density and the tensile strength of the pouring sealant become lower and lower, the foaming rate becomes higher and higher, and the elongation rate increases and then decreases, because to a certain extent, as the amount of the alpha, omega-hydroxyl-terminated liquid silicone rubber increases, the foaming rate becomes higher and higher, and the elongation rate decreases rather after the colloidal strength decreases to a certain extent.
Finally, it should be noted that the above embodiments are intended to illustrate the technical solutions of the present invention and not to limit the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.

Claims (10)

1. The organic silicon foaming pouring sealant is characterized by comprising a component A and a component B, wherein the component A comprises the following components in parts by weight: 50-80 parts of vinyl polysiloxane, 1-5 parts of alpha, omega-hydroxyl-terminated liquid silicone rubber, 40-60 parts of inorganic flame retardant, 1.0-10.0 parts of auxiliary agent, 0.1-0.5 part of anti-settling agent and 0.5-1.0 part of platinum catalyst;
the component B comprises the following components in parts by weight: 50-80 parts of alpha, omega-hydroxyl-terminated liquid silicone rubber, 3-5 parts of hydrogen-containing silicone oil, 40-60 parts of inorganic flame retardant, 1.0-10.0 parts of auxiliary agent, 0.5-1.0 part of carbon black, 0.5-1.0 part of anti-settling agent and 0.01-0.02 part of polymerization inhibitor;
the viscosity of the vinyl polysiloxane and the alpha, omega-hydroxyl-terminated liquid silicone rubber at 25 ℃ is 1000-5000 cps.
2. The silicone foaming pouring sealant as claimed in claim 1, wherein the mass ratio of the vinyl polysiloxane to the α, ω -hydroxyl terminated liquid silicone rubber is vinyl polysiloxane: alpha, omega-hydroxyl-terminated liquid silicone rubber is 1: 1-3.
3. The silicone foaming pouring sealant as claimed in claim 1, wherein the vinyl polysiloxane in the component A and the component B has a vinyl content of 0.18% to 0.38%.
4. The silicone foaming pouring sealant as claimed in claim 1, wherein the adjuvant is surface-modified hollow glass beads with an average particle size of 75 μm.
5. The silicone foaming pouring sealant as claimed in claim 1, wherein the inorganic flame retardant is at least one of aluminum hydroxide and zinc oxide.
6. The silicone foaming pouring sealant as claimed in claim 1, wherein the anti-settling agent is surface-modified fumed silica with a particle size of 20-30 nm.
7. The silicone foaming pouring sealant as claimed in claim 1, wherein the hydrogen-containing silicone oil is a high hydrogen-containing silicone oil.
8. The silicone foaming pouring sealant as claimed in claim 1, wherein the concentration of the platinum catalyst is 5000 ppm.
9. The silicone foaming pouring sealant as claimed in claim 1, wherein the polymerization inhibitor is ethynylcyclohexanol.
10. The preparation method of the organic silicon foaming pouring sealant as claimed in any one of claims 1 to 9, characterized by comprising the following steps:
(1) weighing raw materials of the component A according to a proportion, premixing the raw materials except the catalyst and the auxiliary agent by a planetary stirrer, mixing the raw materials to be uniform and fine by a three-roll grinder, adding the catalyst and the auxiliary agent, and uniformly mixing the mixture by the planetary stirrer to obtain the component A;
(2) weighing raw materials of the component B according to a proportion, premixing the raw materials except the polymerization inhibitor and the auxiliary agent by a planetary mixer, mixing the raw materials by a three-roll grinder until the raw materials are uniform and fine, adding the polymerization inhibitor and the auxiliary agent, and uniformly mixing the raw materials by the planetary mixer to obtain the component B;
(3) and mixing the component A and the component B, and foaming to obtain the organic silicon foaming pouring sealant.
CN202111139165.3A 2021-09-27 2021-09-27 Organic silicon foaming pouring sealant and preparation method thereof Pending CN113789148A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116120891A (en) * 2023-04-20 2023-05-16 德朗聚(常州)新材料有限公司 Silicone resin composition for HJT or TOPCON or PERC process and preparation method thereof
CN116496752A (en) * 2023-04-11 2023-07-28 上海德朗聚新材料有限公司 High-toughness organosilicon shingle conductive adhesive and preparation method thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109749697A (en) * 2019-01-14 2019-05-14 江苏科琪高分子材料研究院有限公司 Three components foaming silicone adhesive compositions and application thereof
CN110396295A (en) * 2019-08-02 2019-11-01 北京化工大学 A kind of room temperature vulcanization organosilicon foaming sealant of high temperature resistant heat insulation and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109749697A (en) * 2019-01-14 2019-05-14 江苏科琪高分子材料研究院有限公司 Three components foaming silicone adhesive compositions and application thereof
CN110396295A (en) * 2019-08-02 2019-11-01 北京化工大学 A kind of room temperature vulcanization organosilicon foaming sealant of high temperature resistant heat insulation and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116496752A (en) * 2023-04-11 2023-07-28 上海德朗聚新材料有限公司 High-toughness organosilicon shingle conductive adhesive and preparation method thereof
CN116496752B (en) * 2023-04-11 2023-10-03 上海德朗聚新材料有限公司 High-toughness organosilicon shingle conductive adhesive and preparation method thereof
CN116120891A (en) * 2023-04-20 2023-05-16 德朗聚(常州)新材料有限公司 Silicone resin composition for HJT or TOPCON or PERC process and preparation method thereof
CN116120891B (en) * 2023-04-20 2023-06-16 德朗聚(常州)新材料有限公司 Silicone resin composition for HJT or TOPCON or PERC process and preparation method thereof

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Application publication date: 20211214