CN116179150A - Impact-resistant energy-absorbing organosilicon pouring sealant and preparation method thereof - Google Patents

Impact-resistant energy-absorbing organosilicon pouring sealant and preparation method thereof Download PDF

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Publication number
CN116179150A
CN116179150A CN202111421468.4A CN202111421468A CN116179150A CN 116179150 A CN116179150 A CN 116179150A CN 202111421468 A CN202111421468 A CN 202111421468A CN 116179150 A CN116179150 A CN 116179150A
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parts
impact
vinyl
pouring sealant
thickening fluid
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Chinese (zh)
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刘忠平
钟发春
毛超英
魏春
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Institute of Chemical Material of CAEP
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Institute of Chemical Material of CAEP
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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
    • 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
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • C08L2203/206Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts

Abstract

The invention discloses an impact-resistant energy-absorbing organosilicon pouring sealant and a preparation method thereof, wherein the impact-resistant energy-absorbing organosilicon pouring sealant is prepared from the following components in parts by weight: and (3) a component A: 100 parts of vinyl end-capped polysiloxane, 5-60 parts of shear thickening fluid, 0.05-30 parts of filler and 0.01-1.5 parts of platinum catalyst; and the component B comprises the following components: 100 parts of vinyl end-capped polysiloxane, 5-60 parts of shear thickening fluid, 0.05-30 parts of filler, 0.01-1 part of alkynol inhibitor and 10-40 parts of hydrogen-containing silicone oil. The pouring sealant can better meet the protection requirements of components under the high impact condition, and has good economic and social effects in the fields of army and civil of weaponry, ships, machinery, electronics and the like.

Description

Impact-resistant energy-absorbing organosilicon pouring sealant and preparation method thereof
Technical Field
The invention belongs to the technical field of pouring sealant materials, and particularly relates to an impact-resistant energy-absorbing organic silicon pouring sealant and a preparation method thereof.
Background
The pouring sealant is an important functional material, and can fix, isolate and seal each part of the component so as to prevent the damage of moisture and dust and harmful gas to the component, and simultaneously slow down the damage of external force impact such as vibration, drop and the like to the component and stabilize the parameters of the component. Along with the application development, the requirements of the pouring sealant are not only limited to basic performances such as dielectric insulation, fixation and isolation, but also higher and higher for impact resistance capability, so that the use safety and reliability of the poured device under severe conditions such as high-speed flight and large drop are met. The organic silicon pouring sealant is a pouring sealant made of silicon rubber, has physical and chemical properties such as moisture-proof sealing property, high and low temperature resistance, ageing resistance, flexibility and the like, and mechanical properties such as high elasticity, low impedance, viscoelasticity and the like, and is widely applied to the industries such as weaponry, ships, electronics, machinery and the like. The impact resistance and energy absorption performance of the organic silicon pouring sealant are improved, and the organic silicon pouring sealant has important significance for application under high impact conditions.
Shear thickening fluids are a functional material that has attracted great attention in recent years. The material shows non-Newtonian mechanical behavior, and shows a fluid state under a general steady state condition, and shows a solid-like mechanical behavior when being subjected to external impacts such as shearing, extrusion and the like. The shear thickening fluid has excellent impact resistance, energy absorption and vibration reduction capability due to the fact that the liquid-solid conversion occurs when the shear thickening fluid is impacted and a large amount of energy is dissipated. Therefore, the shear thickening liquid is introduced into the organic silicon pouring sealant, which is beneficial to the improvement of impact resistance and energy absorption of the organic silicon pouring sealant.
Disclosure of Invention
The invention aims to provide an impact-resistant energy-absorbing organic silicon pouring sealant and a preparation method thereof.
In order to achieve the technical effects, the invention provides the following technical scheme:
the shock-resistant energy-absorbing organosilicon pouring sealant is prepared from the following components in parts by weight:
and (3) a component A: 100 parts of vinyl end-capped polysiloxane, 5-60 parts of shear thickening fluid, 0.05-30 parts of filler and 0.01-1.5 parts of platinum catalyst;
and the component B comprises the following components: 100 parts of vinyl end-capped polysiloxane, 5-60 parts of shear thickening fluid, 0.05-30 parts of filler, 0.01-1 part of alkynol inhibitor and 10-40 parts of hydrogen-containing silicone oil.
The further technical proposal is that the vinyl end-capped polysiloxane is a viscous liquid formed by one or more of vinyl-terminated polydimethylsiloxane, vinyl-terminated polymethylvinylsiloxane, vinyl-terminated polymethylphenylsiloxane and vinyl-terminated polymethylvinylphenylsiloxane.
The further technical scheme is that the shear thickening fluid is prepared by taking micro-nano particles as a disperse phase and polyethylene glycol oligomer as a disperse medium.
The further technical proposal is that the micro-nano particles are hydrophilic silica micro-nano spheres with the particle size range of 20-1000 nm; the molecular weight of the polyethylene glycol oligomer is 100-400; the mass fraction of the micro-nano particles is 40-70% based on 100% of the mass of the shearing thickening fluid.
The further technical proposal is that the filler is one or more selected from gas phase white carbon black, precipitated white carbon black, silicon carbide, alumina, mica powder and graphite.
The further technical scheme is that the platinum catalyst is a Karster platinum catalyst, and the platinum content is 3000ppm.
According to a further technical scheme, the alkynol inhibitor is 1-butyn-3-ol or 1-hexyn-3-ol or 2-propyn-1-ol.
The invention also provides a preparation method of the impact-resistant energy-absorbing organosilicon pouring sealant, which comprises the following steps: 1) Uniformly mixing vinyl-terminated polysiloxane, shear thickening fluid, filler and platinum catalyst according to the formula amount to obtain a component A; 2) Uniformly mixing vinyl-terminated polysiloxane, shear thickening fluid, filler, alkynol inhibitor and hydrogen-containing silicone oil according to the formula amount to obtain a component B; 3) And uniformly mixing the A, B components, vacuum defoaming, filling, sealing and curing to obtain the impact-resistant energy-absorbing organosilicon pouring sealant.
Aiming at the increasingly high requirements of the encapsulated protective device on the impact resistance and energy absorption capacity of the pouring sealant under the severe conditions of high-speed flight, large drop and the like, the invention firstly provides the impact resistance and energy absorption organic pouring sealant based on the solid-liquid coupling energy absorption effect, and the impact resistance and energy absorption organic pouring sealant with a solid-liquid dispersion composite structure is formed by compositing the shear thickening liquid and the silicon rubber. The pouring sealant can better meet the protection requirements of components under the high impact condition, has good economic and social effects in the army and civil fields such as weaponry, ships, machinery, electronics and the like, and has no similar thought and method at home and abroad.
Compared with the prior art, the invention has the following beneficial effects: in the organic silicon pouring sealant, when external force impact is applied to the shear thickening fluid, the liquid-solid mechanical state is converted, so that the external force impact energy is dissipated. Therefore, through the mutual coupling action of the silicone rubber and the shearing thickening fluid, the organic silicon pouring sealant provided by the invention has excellent impact resistance and energy absorption performance effects, and better meets the protection requirements of components under high impact conditions. Compared with an organic silicon material without shear thickening fluid, the organic pouring sealant has the advantages that the protection effect is improved by about 20%, the protection requirement of components under the high impact condition can be better met, and the organic pouring sealant has good economic and social effects in the army and civil fields such as weaponry, ships, machinery, electronics and the like.
Detailed Description
The present invention will be described in further detail with reference to examples.
The unit of measurement "parts" in each of the following examples refers to parts by weight.
Example 1
And (3) a component A: 100 parts of vinyl-terminated polysiloxane, 20 parts of shear thickening fluid, 5 parts of gas-phase white carbon black and 1 part of platinum catalyst with Pt content of 3000 ppm; the shear thickening fluid is prepared from 68 parts of 300nm silicon dioxide nano particles and 32 parts of polyethylene glycol with molecular weight of 200.
And the component B comprises the following components: 100 parts of vinyl-terminated polysiloxane, 20 parts of shear thickening fluid, 5 parts of gas-phase white carbon black, 0.05 part of 1-butyn-3-ol and 40 parts of hydrogen-containing silicone oil. The shear thickening fluid is prepared from 68 parts of 300nm silicon dioxide nano particles and 32 parts of polyethylene glycol with molecular weight of 200.
The vinyl-terminated polysiloxane, the shearing thickening fluid, the filler and the platinum catalyst with the formula amount are added into a batching container, and are fully dispersed by using a dispersing machine, so that the materials are uniformly mixed, and the component A can be obtained.
Adding the vinyl-terminated polysiloxane, the shearing thickening fluid, the filler, the alkynol inhibitor and the hydrogen-containing silicone oil with the formula amount into a batching container, and fully dispersing by using a dispersing machine to uniformly mix the materials to obtain a component B; when the adhesive is used, the component A and the component B are added into a batching container according to the mass ratio of 1:1, and are uniformly mixed by using a dispersing machine, then the materials are defoamed, and then the defoamed materials are poured into a part to be sealed, and the mixture is heated to 80 ℃ to be solidified.
Example 2
And (3) a component A: 100 parts of vinyl-terminated polysiloxane, 30 parts of shear thickening fluid, 5 parts of gas-phase white carbon black and 1 part of platinum catalyst with Pt content of 3000 ppm; the shear thickening fluid is prepared from 68 parts of 300nm silicon dioxide nano particles and 32 parts of polyethylene glycol with molecular weight of 200.
And the component B comprises the following components: 100 parts of vinyl-terminated polysiloxane, 30 parts of shear thickening fluid, 5 parts of gas-phase white carbon black, 0.05 part of 1-butyn-3-ol and 40 parts of hydrogen-containing silicone oil. The shear thickening fluid is prepared from 68 parts of 300nm silicon dioxide nano particles and 32 parts of polyethylene glycol with molecular weight of 200.
The vinyl-terminated polysiloxane, the shearing thickening fluid, the filler and the platinum catalyst with the formula amount are added into a batching container, and are fully dispersed by using a dispersing machine, so that the materials are uniformly mixed, and the component A can be obtained.
Adding the vinyl-terminated polysiloxane, the shearing thickening fluid, the filler, the alkynol inhibitor and the hydrogen-containing silicone oil with the formula amount into a batching container, and fully dispersing by using a dispersing machine to uniformly mix the materials to obtain a component B; when the adhesive is used, the component A and the component B are added into a batching container according to the mass ratio of 1:1, and are uniformly mixed by using a dispersing machine, then the materials are defoamed, and then the defoamed materials are poured into a part to be sealed, and the mixture is heated to 80 ℃ to be solidified.
Example 3
And (3) a component A: 100 parts of vinyl-terminated polysiloxane, 40 parts of shear thickening fluid, 5 parts of gas-phase white carbon black and 1 part of platinum catalyst with Pt content of 3000 ppm; the shear thickening fluid is prepared from 68 parts of 300nm silicon dioxide nano particles and 32 parts of polyethylene glycol with molecular weight of 200.
And the component B comprises the following components: 100 parts of vinyl-terminated polysiloxane, 40 parts of shear thickening fluid, 5 parts of gas-phase white carbon black, 0.05 part of 1-butyn-3-ol and 40 parts of hydrogen-containing silicone oil. The shear thickening fluid is prepared from 68 parts of 300nm silicon dioxide nano particles and 32 parts of polyethylene glycol with molecular weight of 200.
The vinyl-terminated polysiloxane, the shearing thickening fluid, the filler and the platinum catalyst with the formula amount are added into a batching container, and are fully dispersed by using a dispersing machine, so that the materials are uniformly mixed, and the component A can be obtained.
Adding the vinyl-terminated polysiloxane, the shearing thickening fluid, the filler, the alkynol inhibitor and the hydrogen-containing silicone oil with the formula amount into a batching container, and fully dispersing by using a dispersing machine to uniformly mix the materials to obtain a component B; when the adhesive is used, the component A and the component B are added into a batching container according to the mass ratio of 1:1, and are uniformly mixed by using a dispersing machine, then the materials are defoamed, and then the defoamed materials are poured into a part to be sealed, and the mixture is heated to 80 ℃ to be solidified.
Example 4
And (3) a component A: 100 parts of vinyl-terminated polysiloxane, 50 parts of shear thickening fluid, 5 parts of gas-phase white carbon black and 1 part of platinum catalyst with Pt content of 3000 ppm; the shear thickening fluid is prepared from 68 parts of 300nm silicon dioxide nano particles and 32 parts of polyethylene glycol with molecular weight of 200.
And the component B comprises the following components: 100 parts of vinyl-terminated polysiloxane, 50 parts of shear thickening fluid, 5 parts of gas-phase white carbon black, 0.05 part of 1-butyn-3-ol and 40 parts of hydrogen-containing silicone oil. The shear thickening fluid is prepared from 68 parts of 300nm silicon dioxide nano particles and 32 parts of polyethylene glycol with molecular weight of 200.
The vinyl-terminated polysiloxane, the shearing thickening fluid, the filler and the platinum catalyst with the formula amount are added into a batching container, and are fully dispersed by using a dispersing machine, so that the materials are uniformly mixed, and the component A can be obtained.
Adding the vinyl-terminated polysiloxane, the shearing thickening fluid, the filler, the alkynol inhibitor and the hydrogen-containing silicone oil with the formula amount into a batching container, and fully dispersing by using a dispersing machine to uniformly mix the materials to obtain a component B; when the adhesive is used, the component A and the component B are added into a batching container according to the mass ratio of 1:1, and are uniformly mixed by using a dispersing machine, then the materials are defoamed, and then the defoamed materials are poured into a part to be sealed, and the mixture is heated to 80 ℃ to be solidified.
Example 5
And (3) a component A: 100 parts of vinyl-terminated polysiloxane, 60 parts of shear thickening fluid, 15 parts of gas-phase white carbon black and 1 part of platinum catalyst with Pt content of 3000 ppm; the shear thickening fluid is prepared from 68 parts of 300nm silicon dioxide nano particles and 32 parts of polyethylene glycol with molecular weight of 200.
And the component B comprises the following components: 100 parts of vinyl-terminated polysiloxane, 60 parts of shear thickening fluid, 15 parts of gas-phase white carbon black, 0.05 part of 1-butyn-3-ol and 40 parts of hydrogen-containing silicone oil. The shear thickening fluid is prepared from 68 parts of 300nm silicon dioxide nano particles and 32 parts of polyethylene glycol with molecular weight of 200.
The vinyl-terminated polysiloxane, the shearing thickening fluid, the filler and the platinum catalyst with the formula amount are added into a batching container, and are fully dispersed by using a dispersing machine, so that the materials are uniformly mixed, and the component A can be obtained.
Adding the vinyl-terminated polysiloxane, the shearing thickening fluid, the filler, the alkynol inhibitor and the hydrogen-containing silicone oil with the formula amount into a batching container, and fully dispersing by using a dispersing machine to uniformly mix the materials to obtain a component B; when the adhesive is used, the component A and the component B are added into a batching container according to the mass ratio of 1:1, and are uniformly mixed by using a dispersing machine, then the materials are defoamed, and then the defoamed materials are poured into a part to be sealed, and the mixture is heated to 80 ℃ to be solidified.
Comparative examples
And (3) a component A: 100 parts of vinyl-terminated polysiloxane, 5 parts of fumed silica and 1 part of platinum catalyst with Pt content of 3000 ppm; the shear thickening fluid is prepared from 68 parts of 300nm silicon dioxide nano particles and 32 parts of polyethylene glycol with molecular weight of 200.
And the component B comprises the following components: 100 parts of vinyl-terminated polysiloxane, 5 parts of fumed silica, 0.05 part of 1-butyn-3-ol and 40 parts of hydrogen-containing silicone oil. The shear thickening fluid is prepared from 68 parts of 300nm silicon dioxide nano particles and 32 parts of polyethylene glycol with molecular weight of 200.
The vinyl-terminated polysiloxane, the filler and the platinum catalyst with the formula amounts are added into a batching container, and are fully dispersed by using a dispersing machine, so that the materials are uniformly mixed, and the component A can be obtained.
Adding the vinyl-terminated polysiloxane filler, the alkynol inhibitor and the hydrogen-containing silicone oil with the formula amounts into a batching container, and fully dispersing by using a dispersing machine to uniformly mix the materials to obtain a component B; when the adhesive is used, the component A and the component B are added into a batching container according to the mass ratio of 1:1, and are uniformly mixed by using a dispersing machine, then the materials are defoamed, and then the defoamed materials are poured into a part to be sealed, and the mixture is heated to 80 ℃ to be solidified.
The impact resistance of the potting adhesive materials of examples 1 to 5 and comparative examples was tested by a drop hammer impact tester. The drop hammer impact tester meets the test standard of EN1621-1-2012, and the test conditions are as follows: the drop weight was 4.977kg, the drop height was 42.6cm, the impact energy was 20J, and the thickness of the test specimens was 4.8mm. And the peak value of an impact force curve penetrating through the pouring sealant material in the process of impacting the sample by the drop hammer is utilized to represent the impact resistance and energy absorption effect of the sample. Under the condition that the impact energy is 20J, the smaller the impact force peak value is, the better the impact resistance and energy absorption effect is. Table 1 shows the peak penetration force in drop impact tests for the potting adhesive materials of examples 1-5 and comparative examples. As can be seen from Table 1, the penetration force of the silicone potting adhesive material of example 5 is reduced by about 20% compared with that of the silicone potting adhesive material of comparative example without the shear thickening fluid, which indicates that the silicone potting adhesive material provided by the invention has better impact resistance and energy absorption performance and can better meet the protection requirements of components under high impact conditions
Table 1 drop hammer impact test for each example and comparative example
Example names Peak penetration force/KN
Example 1 23.91
Example 2 22.52
Example 3 21.93
Example 4 21.03
Example 5 20.04
Comparative examples 24.54
Although the invention has been described herein with reference to the above-described illustrative embodiments thereof, the above-described embodiments are merely preferred embodiments of the present invention, and the embodiments of the present invention are not limited by the above-described embodiments, it should be understood that numerous other modifications and embodiments can be devised by those skilled in the art that will fall within the scope and spirit of the principles of this disclosure.

Claims (8)

1. The impact-resistant energy-absorbing organosilicon pouring sealant is characterized by being prepared from the following components in parts by weight:
and (3) a component A: 100 parts of vinyl end-capped polysiloxane, 5-60 parts of shear thickening fluid, 0.05-30 parts of filler and 0.01-1.5 parts of platinum catalyst;
and the component B comprises the following components: 100 parts of vinyl end-capped polysiloxane, 5-60 parts of shear thickening fluid, 0.05-30 parts of filler, 0.01-1 part of alkynol inhibitor and 10-40 parts of hydrogen-containing silicone oil.
2. The impact-resistant energy-absorbing organosilicon pouring sealant according to claim 1, wherein the vinyl-terminated polysiloxane is a viscous liquid formed by one or more of vinyl-terminated polydimethylsiloxane, vinyl-terminated polymethylvinylsiloxane, vinyl-terminated polymethylphenylsiloxane and vinyl-terminated polymethylvinylphenylsiloxane.
3. The impact-resistant energy-absorbing organosilicon pouring sealant according to claim 1, wherein the shear thickening fluid is prepared by taking micro-nano particles as a disperse phase and polyethylene glycol oligomer as a disperse medium.
4. The impact resistant and energy absorbing organosilicon pouring sealant according to claim 3, wherein the micro-nano particles are hydrophilic silica micro-nano spheres with the particle size range of 20-1000 nm; the molecular weight of the polyethylene glycol oligomer is 100-400; the mass fraction of the micro-nano particles is 40-70% based on 100% of the mass of the shearing thickening fluid.
5. The impact-resistant energy-absorbing organosilicon pouring sealant according to claim 1, wherein the filler is one or more selected from the group consisting of fumed silica, precipitated silica, silicon carbide, alumina, mica powder and graphite.
6. The impact resistant and energy absorbing silicone potting adhesive of claim 1, wherein the platinum catalyst is a cassiterite platinum catalyst and the platinum content is 3000ppm.
7. The impact resistant and energy absorbing silicone potting adhesive of claim 1, wherein the alkynol inhibitor is 1-butyn-3-ol or 1-hexyn-3-ol or 2-propyn-1-ol.
8. A method for preparing the impact-resistant energy-absorbing organosilicon pouring sealant according to any one of claims 1 to 7, which is characterized by comprising the following steps: 1) Uniformly mixing vinyl-terminated polysiloxane, shear thickening fluid, filler and platinum catalyst according to the formula amount to obtain a component A; 2) Uniformly mixing vinyl-terminated polysiloxane, shear thickening fluid, filler, alkynol inhibitor and hydrogen-containing silicone oil according to the formula amount to obtain a component B; 3) And uniformly mixing the A, B components, vacuum defoaming, filling, sealing and curing to obtain the impact-resistant energy-absorbing organosilicon pouring sealant.
CN202111421468.4A 2021-11-26 2021-11-26 Impact-resistant energy-absorbing organosilicon pouring sealant and preparation method thereof Pending CN116179150A (en)

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