CN102516928B - Silicone sealant used for electronic products, preparation method thereof, and application thereof - Google Patents
Silicone sealant used for electronic products, preparation method thereof, and application thereof Download PDFInfo
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Abstract
The invention relates to a silicone sealant used for electronic products. The invention belongs to the technical field of high-molecular materials. The sealant comprises a component A and a component B. The component A is composed of raw materials of, by weight: 100-110 parts of alpha-omega-dihydroxyl polydimethylsiloxane, 25-40 parts of silicone oil, 5-8 parts of a heat-conductive filling material, 35-65 parts of a fire-retarding filling material, and 20-35 parts of nano-grade calcium carbonate. The component B is composed of raw materials of, by weight: 90-110 parts of silicone oil, 12-15 parts of a cross-linking agent, 3-4 parts of a coupling agent, 1-1.5 parts of a catalyst, and 1.5-3 parts of a colored slurry. The silicone sealant is advantaged in excellent fire retardance, improved heat conductivity, ideal steam-penetration inhibiting capacity, excellent electrical property, excellent weathering resistance, and ideal corrosion resistance. A provided preparation method is advantaged in simple technology, and non-harsh requirements on technologies and equipments. With a provided application method, a mixing effect of the components A and B can be ensured.
Description
Technical field
The invention belongs to technical field of polymer materials, be specifically related to a kind of use for electronic products silicone sealant, and relate to its preparation method and using method.
Background technology
Fast development along with electronic industry, electronics develops to microminiaturization, heavy body and high performance direction, highly integrated and ultrathinization of electronic devices and components become trend, especially popularizing along with precise treatment and case type unicircuit, requirement of shelter to electronic product is also more and more higher, and is particularly, more and more harsher to the applied environment of unicircuit, can not be exposed in the atmospheric environment, also not allow by contamination by dust and require it to have better heat radiating effect.
The aforementioned electronic product is placed the environment operation down of sealing, for example be equipped with tightness system and can play certain dustproof effect, but heat dispersion can significantly reduce, undoubtedly, for a long time heat accumulation can cause the work effect of accurate unicircuit to descend, and even breaks down or damage.In addition, the water vapor in the atmosphere also can cause corrosion to the precise electronic element, even can cause short circuit and cause fire failure.
In recent years, people's tackiness agent that electronic apparatus is used had been obtained considerable progress at aspects such as steam-preventing perviousness, cementability, curing speed and flame retardant resistances.For example: disclosed flame-proof silicone sealant for electronics of CN1865383A and manufacture method thereof, use magnesium hydroxide and aluminium hydroxide to replace halogen flame, in addition, expansion flame-proof organosilicon fluid sealant of providing of the flameproofing silicone structure sealant recommended of CN1687288A and manufacture thereof and CN101368080A and preparation method thereof all has good achievement to the flame retardant properties of tackiness agent.But, be not limited to the disclosed seal gum of these patent documentations and all do not have the heat-conducting effect that the electronics industry is more and more paid close attention to, and in disclosed patent and non-patent literature, all do not disclose the technology enlightenment of thermal conductivity how to improve seal gum.The applicant thinks, to make seal gum have flame retardant resistance only be passive but not positive behave only makes seal gum self possess good thermal conductivity and is only positive technical measures.For this reason, the applicant has done repeatedly and good try, and technical scheme described below produces under this background.
Summary of the invention
Top priority of the present invention is to provide that a kind of both to have helped to embody ideal self-leveling energy, electrical property, surface drying speed fast and deeply-curing speed is fast, helps again embodying excellent heat conductivility and uses radiating effect that ensures electron device and the use for electronic products silicone sealant that prolongs the work-ing life of electric equipment products.
The preparation method who also has a task to be to provide a kind of use for electronic products silicone sealant of the present invention, this method processing step letter and not numerous and can ensure comprehensive embodiment of the technique effect of described use for electronic products silicone sealant.
Of the present invention have a task to be to provide a kind of using method of use for electronic products silicone sealant again, and this method can make the A component that constitutes silicone sealant mix ideally with rational weight part ratio with the B component.
Top priority of the present invention is finished like this, and a kind of use for electronic products silicone sealant comprises A component and B component, and each raw material by following parts by weight of described A component and B component constitutes:
The raw material of A component is:
100～110 parts of α-alpha, omega-dihydroxy polydimethyl siloxanes;
25～40 parts of silicone oil;
5～8 parts of heat conductive fillers;
35～65 parts of fire-retardant fillers;
20～35 parts of nano-calcium carbonates;
The raw material of B component is:
90～110 parts of silicone oil;
12～15 parts of linking agents;
3～4 parts of coupling agents;
1～1.5 part of catalyzer;
1.5～3 parts in coloured slurry.
In a specific embodiment of the present invention, described silicone oil is dimethyl silicone oil, vinyl silicone oil or methyl ethylene silicone oil; The median size of described heat conductive filler is 40-52nm; Purity is greater than 99%; Specific surface area is 43-44m
2/ g; Volume density is 0.155-0.165g/cm
3
In another specific embodiment of the present invention, described heat conductive filler is the mixture of nano-silicon nitride, nano silicon nitride magnesium, nanometer silicon carbide, nano aluminum nitride, nm-class boron nitride and aluminum oxide.
In another specific embodiment of the present invention, the parts by weight of described nano-silicon nitride, nano silicon nitride magnesium, nanometer silicon carbide, nano aluminum nitride, nm-class boron nitride and aluminum oxide are identical.
In another specific embodiment of the present invention, described fire-retardant filler is magnesium hydroxide and/or aluminium hydroxide; Described nano-calcium carbonate is process resin acid or silane surface-treated nm-class active calcium carbonate.
Also have in the specific embodiment of the present invention, described linking agent is methyltrimethoxy silane, methyl three isobutyl ketone oximino silanes or vinyl three isobutyl ketone oximino silanes; Described coupling agent is hexamethyldisiloxane and/or γ-[2,3-epoxy third oxygen] propyl trimethoxy silicane.
More of the present invention and in specific embodiment, described catalyzer is dibutyl tin acetate or dibutyl two stannous octoates; The color of described coloured slurry is black, redness or grey.
Of the present invention also have a task to finish like this, and a kind of preparation method of use for electronic products silicone sealant may further comprise the steps:
A, produce the A component, α-alpha, omega-dihydroxy polydimethyl siloxane 100-110 part, silicone oil 25-40 part, heat conductive filler 5-8 part, fire-retardant filler 35-65 part and nano-calcium carbonate 20-35 part are joined vacuum kneader, the vacuum tightness of control kneader be-0.06～-0.08MPa, kneading temperature be controlled to be 100-115 ℃ and kneading time and be controlled to be 60-110min, obtain the A component, and encapsulation;
B, produce the B component, silicone oil 90-110 part, linking agent 12-15 part, coupling agent 3-4 part, catalyzer 1-1.5 part and coloured slurry 1.5-3 part dropped in the duplicate rows star homogenizer with revolution and rotation function stir, the control churning time is 40-60min, the control rotational velocity is that 350-450n/min and control revolution speed are 35-45n/min, obtain the B component, and encapsulation.
Of the present invention have a task to finish so again, and a kind of using method of use for electronic products silicone sealant, this using method were mixed A component 7-9 part and B component in 1 minute the back by weight and used.
The flame retardant properties excellence of technical scheme provided by the invention reaches the V0 level; Owing in A component prescription, added heat conductive filler, therefore can improve heat-conducting effect significantly, its thermal conductivity values＞1.0W/mK can derive the heat that element produced in electronic product such as the circuit card timely and effectively; Suppress steam permeable performance ideal, the transmitance (g/m of water vapor
2D)＜1.5; The electrical property excellence, volume specific resistance＞1 * 10
16Ω cm, voltage breakdown＞11kV/mm; Have excellent weathering resistance and corrodibility ideal.The preparation method's technology that provides is terse, and is not harsh to processing requirement and equipment.The using method that provides can ensure the mixed effect of A, B component.
Embodiment
By the description of applicant to embodiment; to make technique effect of the present invention more become bright and clear; but embodiment is not the restriction to the present invention program, any according to the present invention program done only be form but not the variation of essence all should be considered as the protection domain that the present invention advocates.
Embodiment 1:
The preparation method's of use for electronic products silicone sealant provided by the invention step is as follows:
A, produce the A component, by weight 105 parts of α-alpha, omega-dihydroxy polydimethyl siloxanes, 35 parts of methyl ethylene silicone oil, 5 parts of heat conductive fillers, active hydrogen magnesium oxide and active aluminium hydroxide were mixed back 35 parts by 1: 1, the nm-class active calcium carbonate that the resin acid surfaces is handled joins vacuum kneader for 20 parts, the vacuum tightness of kneader at-0.07MPa, mediate 100 ℃ of temperature, mediate 100min after, obtain the A component, and encapsulation (being can), aforesaid filler are that median size is 40-52nm, purity greater than 99%, specific surface area is 43-44m
2/ g and volume density are 0.155-0.165g/cm
3Heat conductive filler, and this heat conductive filler mixes by identical parts by weight by nano-silicon nitride, nano silicon nitride magnesium, nanometer silicon carbide, nano aluminum nitride, nm-class boron nitride and aluminum oxide and constitutes, and promptly all mixes formation by 1 parts by weight;
B, produce the B component, by weight with 90 parts of methyl ethylene silicone oil, 12 parts of methyltrimethoxy silanes, hexamethyldisiloxane and γ-[2,3-epoxy third oxygen] propyl trimethoxy silicane by 1: 1 composite back 3 parts, 1 part of dibutyl tin acetate, color is that the trade mark by the production and sales of the chemical company limited of Chinese Wenzhou City, Zhejiang Province temperatureization black and preferred is that 1.5 parts of inputs of the coloured slurry of 901 types have in the duplicate rows star homogenizer of rotation and revolution function, at rotational velocity 350n/min and revolution speed 45n/min, behind the blend 45min, obtain the B component, and encapsulation (being can).
By the A component of method for preparing and B component in use by weight than A: B=8: 1 mixes use.
Embodiment 2:
A, produce the A component, by weight 110 parts of α-alpha, omega-dihydroxy polydimethyl siloxanes, 25 parts of vinyl silicone oils, 7 parts of heat conductive fillers, 45 parts in active hydrogen magnesium oxide and silane surface-treated nm-class active calcium carbonate are added vacuum kneader for 25 parts, the vacuum tightness of kneader at-0.06MPa, mediate 105 ℃ of temperature, mediate 60min after, obtain the A component, all the other are all with the description to the steps A of embodiment 1;
B, produce the B component, by weight 110 parts, 14 parts of methyl three isobutyl ketone oximino silanes, 3.5 parts of hexamethyldisiloxane, 1.2 parts of dibutyl two stannous octoates in the vinyl silicone oil and the color coloured slurry for red (trade mark is 902 types) is dropped in the duplicate rows star homogenizer for 1.8 parts, at rotational velocity 450n/min and revolution speed 35n/min, behind the blend 50min, obtain the B component, all the other are all with the description to the step B of embodiment 1.
A, B component are by weight than A during use: B=7: 1 mixes use.
Embodiment 3:
A, produce the A component, the nm-class active calcium carbonate that 106 parts of α-alpha, omega-dihydroxy polydimethyl siloxanes, 30 parts of methyl ethylene silicone oil, 8 parts of heat conductive fillers, 55 parts of active aluminium hydroxides and resin acid surfaces are handled adds vacuum kneader for 30 parts, the vacuum tightness of kneader is at-0.08MPa, mediate 115 ℃ of temperature, after mediating 90min, obtain the A component;
B, produce the B component, with 100 parts, 15 parts of vinyl three isobutyl ketone oximino silanes, γ-[2 in the methyl ethylene silicone oil, 3-epoxy third oxygen] 3.8 parts of propyl trimethoxy silicanes and 1.2 parts of dibutyl two stannous octoates and color be that coloured slurry of gray (trade mark is 902-1) drops in the duplicate rows star homogenizer for 2.5 parts, at rotational velocity 400n/min and revolution speed 40n/min, behind the blend 60min, obtain the B component.
A, B component are by weight than A: B=9: 1 mixes use.The content that does not relate in the present embodiment is all with the description to embodiment 1.
Embodiment 4:
A, produce the A component, 109 parts of α-alpha, omega-dihydroxy polydimethyl siloxanes, 40 parts of vinyl silicone oils, 6 parts of heat conductive fillers, active hydrogen magnesium oxide are mixed back 65 parts of nm-class active calcium carbonates of handling with the resin acid surfaces with active aluminium hydroxide by 1: 1 add vacuum kneader for 35 parts, the vacuum tightness of kneader at-0.06MPa, mediate 115 ℃ of temperature, mediate 100min after, obtain the A component;
B, produce the B component, with 105 parts of dimethyl silicone oils, 13 parts of methyl three isobutyl ketone oximino silanes, hexamethyldisiloxane, γ-[2,3-epoxy third oxygen] propyl trimethoxy silicane is by 1.4 parts of 2: 1 composite back 4 parts and dibutyl tin acetates, coloured slurry drops in the duplicate rows star homogenizer for 3 parts, at rotational velocity 390n/min, revolution speed 35n/min, behind the blend 60min, obtain the B component;
During use, A, B component are by weight than A: B=8.5: 1 mixes use.The content that does not relate in the present embodiment is all with the description to embodiment 1.
Embodiment 5:
A, produce the A component, 100 parts of α-alpha, omega-dihydroxy polydimethyl siloxanes, 33 parts of dimethyl silicone oils, 7 parts of heat conductive fillers, 50 parts in active hydrogen magnesium oxide and silane surface-treated nm-class active calcium carbonate are added vacuum kneader for 33 parts, the vacuum tightness of kneader at-0.08MPa, mediate 100 ℃ of temperature, mediate 110min after, obtain the A component;
B, produce the B component, with 95 parts, 15 parts of vinyl three isobutyl ketone oximino silanes, γ-[2 in the methyl ethylene silicone oil, 3-epoxy third oxygen] 3.6 parts of propyl trimethoxy silicanes, 1.5 parts of dibutyl two stannous octoates and coloured slurry drop in the duplicate rows star homogenizer for 2 parts, at rotational velocity 380n/min, revolution speed 43n/min, behind the blend 55min, obtain the B component;
During use, A, B component are by weight than A: B=7.5: 1 mixes use.The content that does not relate in the present embodiment is all with the description to embodiment 1.
Comparative example 1:
100 parts of α-alpha, omega-dihydroxy polydimethyl siloxanes, 5 parts of polydimethylsiloxanes, 100 parts of active nano calcium, 20 parts of Meteorological Act silicon-dioxide, 0.01 part of magnesium hydroxide, titanium dioxide are joined in the homogenizer for 1 part, in 90 ℃ of temperature, vacuum tightness-0.01MPa is dehydration 4h down, makes the A component after the cooling;
0.5 part of poly-triethoxyl silane, 1 part of 3-Racemic glycidol propyl trimethoxy silicane, N-(β-aminoethyl)-1 part of α-aminopropyl trimethoxysilane, γ-1 part of aminomethyl triethoxyl silane, 0.5 part in silane of methyl ethylene (N-methyl kharophen), 2 parts of titanium propanolates, dibutyl tin dilaurate join in the sealed vessel for 1 part, obtain the B component after mixing;
With above-mentioned A, B component by weight A: B=100: 8 mix, obtain two component silicone sealants behind deaeration 5min under the vacuum tightness 0.01Mpa.The contrast of product salient features sees Table 1.
Comparative example 2:
With 100 parts of α-alpha, omega-dihydroxy polydimethyl siloxanes, 30 parts of polydimethylsiloxanes, 70 parts of silicon powders, heavyly decide 20 parts of method white carbon blacks, 10 parts in aluminium hydroxide, titanium dioxide and join in the homogenizer for 10 parts, in 120 ℃ of temperature, vacuum tightness-0.006MPa is dehydration 3h down, makes the A component after the cooling;
8 parts of methyl silicates, N-(β-aminoethyl)-0.2 part of α-aminopropyl trimethoxysilane, 1 part in silane of dimethyl two (N-methyl kharophen), 3 parts of titanate chelates, dibutyl tin dilaurate join in the sealed vessel for 2 parts, obtain the B component after mixing;
With above-mentioned A, B component by weight A: B=100: 10 mix, obtain two component silicone sealants behind deaeration 10min under vacuum tightness-0.008Mpa.The contrast of product salient features sees the following form.
The effect of the coloured slurry in the B component among the foregoing description 1-5 is to distinguish A component and B component for the user.By the key technical indexes of resulting pair of component joint sealant of the foregoing description 1-5 as: hardness is tested by GB/T531.1-2008; Volume specific resistance is tested by GB/T1692-2008; Voltage breakdown is tested by GB/T1695-2005; Thermal conductivity is tested by GB/T3399-1992; Flame retardant properties is tested by GB/T2408-2008; Wet electric leakage performance is tested by GB6553-2003.Technical indicator is by shown in the following table:
Claims (7)
1.
A kind of use for electronic products silicone sealant comprises A component and B component, it is characterized in that each raw material by following parts by weight of described A component and B component constitutes:
The raw material of A component is:
100 ~ 110 parts of α-alpha, omega-dihydroxy polydimethyl siloxanes;
25 ~ 40 parts of silicone oil;
5 ~ 8 parts of heat conductive fillers;
35 ~ 65 parts of fire-retardant fillers;
20 ~ 35 parts of nano-calcium carbonates;
The raw material of B component is:
90 ~ 110 parts of silicone oil;
12 ~ 15 parts of linking agents;
3 ~ 4 parts of coupling agents;
1 ~ 1.5 part of catalyzer;
1.5 ~ 3 parts in coloured slurry,
The median size of described heat conductive filler is 40-52 nm; Purity is greater than 99%; Specific surface area is 43-44m
2
/ g; Volume density is 0.155-0.165g/cm
3
Described heat conductive filler is the mixture of the identical nano-silicon nitride of parts by weight, nano silicon nitride magnesium, nanometer silicon carbide, nano aluminum nitride, nm-class boron nitride and aluminum oxide, in use, by weight with described A component 7-9 part with use after 1 part of described B component mixes.
2.
Use for electronic products silicone sealant according to claim 1 is characterized in that described silicone oil is dimethyl silicone oil, vinyl silicone oil or methyl ethylene silicone oil.
3.
Use for electronic products silicone sealant according to claim 1 is characterized in that the parts by weight of described nano-silicon nitride, nano silicon nitride magnesium, nanometer silicon carbide, nano aluminum nitride, nm-class boron nitride and aluminum oxide are identical.
4.
Use for electronic products silicone sealant according to claim 1 is characterized in that described fire-retardant filler is magnesium hydroxide and/or aluminium hydroxide; Described nano-calcium carbonate is process resin acid or silane surface-treated nm-class active calcium carbonate.
5.
Use for electronic products silicone sealant according to claim 1 is characterized in that described linking agent is methyltrimethoxy silane, methyl three isobutyl ketone oximino silanes or vinyl three isobutyl ketone oximino silanes; Described coupling agent is hexamethyldisiloxane and/or γ-[2,3-epoxy third oxygen] propyl trimethoxy silicane.
6.
Use for electronic products silicone sealant according to claim 1 is characterized in that described catalyzer is dibutyl tin acetate or dibutyl two stannous octoates; The color of described coloured slurry is black, redness or grey.
7.
A kind of preparation method of use for electronic products silicone sealant as claimed in claim 1 is characterized in that may further comprise the steps:
A, produce the A component, α-alpha, omega-dihydroxy polydimethyl siloxane 100-110 part, silicone oil 25-40 part, 8 parts of heat conductive filler 5-, fire-retardant filler 35-65 part and nano-calcium carbonate 20-35 part are joined vacuum kneader, the vacuum tightness of control kneader be-0.06～-0.08MPa, kneading temperature be controlled to be 100-115 ℃ and kneading time and be controlled to be 60-110min, obtain the A component, and encapsulation;
B, produce the B component, silicone oil 90-110 part, linking agent 12-15 part, coupling agent 3-4 part, catalyzer 1-1.5 part and coloured slurry 1.5-3 part dropped in the duplicate rows star homogenizer with revolution and rotation function stir, the control churning time is 40-60min, the control rotational velocity is that 350-450n/min and control revolution speed are 35-45n/min, obtain the B component, and encapsulation.
Priority Applications (1)
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Applications Claiming Priority (1)
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|---|---|---|---|
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| CN102516928B true CN102516928B (en) | 2013-07-31 |
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| JP5950450B2 (en) * | 2012-07-10 | 2016-07-13 | 信越化学工業株式会社 | Room temperature curable organopolysiloxane composition |
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| CN113801627A (en) * | 2021-11-01 | 2021-12-17 | 苏州达同新材料有限公司 | Organic silicon adhesive sealant and preparation method thereof |
| CN113913019A (en) * | 2021-12-06 | 2022-01-11 | 祥雅(嘉兴)科技有限公司 | High-heat-conductivity liquid silicone rubber for composite material mold |
| CN115160978A (en) * | 2022-09-07 | 2022-10-11 | 山东景茂新材料有限公司 | Flame-retardant silicone sealant and preparation method thereof |
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| CN102516928A (en) | 2012-06-27 |
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