CN103396757B - Single-component dealcoholization-type flame-retardant room temperature vulcanized (RTV) silicone rubber sealant and preparation method thereof - Google Patents

Single-component dealcoholization-type flame-retardant room temperature vulcanized (RTV) silicone rubber sealant and preparation method thereof Download PDF

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CN103396757B
CN103396757B CN201310335563.1A CN201310335563A CN103396757B CN 103396757 B CN103396757 B CN 103396757B CN 201310335563 A CN201310335563 A CN 201310335563A CN 103396757 B CN103396757 B CN 103396757B
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silicone rubber
omega
alpha
rubber sealant
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CN103396757A (en
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翁祝强
王地林
陈超
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Zhaoshun Technology (Guangdong) Co., Ltd
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Dongguan Million Shun's Organosilicon Science And Technology Co Ltd
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Abstract

The invention relates to a single-component dealcoholization-type flame-retardant room temperature vulcanized (RTV) silicone rubber sealant and a preparation method thereof. A base material is obtained by dewatering and blending of 100 parts by mass of alpha, omega-dihydroxyl polydimethylsiloxane, 10-50 parts by mass of dimethicone, 80-150 parts by mass of a nanometer reinforced filler, 100-150 parts by mass of a flame-retardant filler and 0.5-5 parts by mass of a hydroxyl clearing agent in a power mixer at the temperature of 120-150 DEG C with the vacuum degree of 0.09-0.1 MPa for 60-240 min; and at the normal temperature, the base material is vacuumized to the vacuum degree of 0.09-0.1MPa, after 10 min of stirring, 1-15 parts by mass of a cross-linking agent is added, after 15 min-30 min of stirring under the vacuum condition, 0.5-4 parts by mass of a coupling agent is added, and after 10 min-30min of stirring under the vacuum condition, the base material can be packaged into a finished product.

Description

Fire-retardant RTV silicone rubber sealant of a kind of single-component dealcoholization-type and preparation method thereof
Technical field
The present invention relates to silicon rubber preparing technical field, be specifically related to fire-retardant RTV silicone rubber sealant of a kind of single-component dealcoholization-type and preparation method thereof.
Background technology
Along with electric, building and the high speed development of Aviation Industry, room temperature silicone sulphurated siliastic is owing to having neutral character, to the advantage such as base material non-corrosiveness, nontoxic, strong adaptability and cost value be lower, enjoy the favor of sector application and investigator and obtain develop rapidly.Meanwhile, single-component room-temperature vulcanized silicone rubber (RTV), namely at room temperature without the need to adding other component and curable, easy to use, solidification post-shrinkage ratio is little, good to most of material adhesive performance, has good resistance to electrical insulating property, weathering resistance, flexible resistance, high thermal resistance and ageing resistance etc.Have application widely at industrial circles such as building, electronics, automobile makings, its development prospect is considerable.
CN102757647A discloses a kind of single component catalysis dealcoholized type room temperature vulcanized silicone rubber seal gum, it comprises according to weight part: 100 parts of α, alpha, omega-dihydroxy polydimethyl siloxane, 10 ~ 450 parts of functional stuffings, 0.4 ~ 20 part of linking agent, 0.1 ~ 8 part of coupling agent, 0.1 ~ 12 part of catalyzer.This invention also relates to a kind of preparation method of described single component catalysis dealcoholized type room temperature vulcanized silicone rubber seal gum, comprising: the preparation of base-material: by α, and alpha, omega-dihydroxy polydimethyl siloxane and filler dewater blended, obtain base-material; Get base-material, stir at vacuum state, add linking agent, stir at vacuum state; Add coupling agent, stir; Add catalyzer, vacuumize, pass into rare gas element, stir, vacuumize, stir, finished product.
CN102757759A discloses a kind of single-component dealcoholization-type RTV silicone rubber sealant, wherein base-material comprises by weight: α, alpha, omega-dihydroxy polydimethyl siloxane 100 parts, 1 ~ 150 part, softening agent, nano level reinforced filling 1 ~ 150 part, hydroxyl scavenging agent 0.1 ~ 20 part, finished product comprises by weight: base-material 100 parts, linking agent 0.1 ~ 30 part, coupling agent 0.1 ~ 8 part.The preparation method of described single-component dealcoholization-type RTV silicone rubber sealant comprises: by α, and alpha, omega-dihydroxy polydimethyl siloxane, softening agent, nano level reinforced filling and hydroxyl scavenging agent, dewater blended, obtains base-material; Get base-material, vacuumize, stir, add linking agent, vacuumize, stir; Add coupling agent, vacuumize, stir, obtain finished product.Advantage of the present invention is: employing nano material is filler, and adds softening agent, makes product have good physicals; Add silane treatment Nano filling, extend the seal gum shelf lives.
But RTV silicone rubber sealant disclosed in prior art does not all relate to its flame retardant properties and yellowing resistance energy, and thermotolerance is poor.
Summary of the invention
For problems of the prior art, an object of the present invention is to provide a kind of single-component dealcoholization-type fire-retardant RTV silicone rubber sealant, and the flame retardant properties of described RTV silicone rubber sealant and yellowing resistance can be excellent, and excellent heat resistance.
In order to achieve the above object, present invention employs following technical scheme:
The fire-retardant RTV silicone rubber sealant of a kind of single-component dealcoholization-type, described RTV silicone rubber sealant comprises following raw material by mass parts:
The mass parts of described dimethyl silicone oil is such as 13 parts, 16 parts, 19 parts, 22 parts, 27 parts, 32 parts, 37 parts, 42 parts, 45 parts or 48 parts.
The mass parts of reinforced filling described in nanometer is such as 85 parts, 91 parts, 96 parts, 101 parts, 106 parts, 111 parts, 116 parts, 121 parts, 126 parts, 131 parts, 136 parts, 141 parts or 146 parts.
The mass parts of described fire-retardant filler is such as 101 parts, 106 parts, 111 parts, 116 parts, 121 parts, 126 parts, 131 parts, 136 parts, 141 parts or 146 parts.
The mass parts of described hydroxyl scavenging agent is such as 0.6,1.2 part, 1.6 parts, 2 parts, 2.4 parts, 2.8 parts, 3.2 parts, 3.6 parts, 4 parts, 4.4 parts, 4.6 parts or 4.8 parts.
The mass parts of described coupling agent is such as 0.4 part, 0.6 part, 0.8 part, 1 part, 1.2 parts, 1.4 parts, 1.6 parts, 1.8 parts, 2.1 parts, 2.4 parts, 2.7 parts, 3.0 parts, 3.3 parts, 3.6 parts or 3.9 parts.
The mass parts of described linking agent is such as 1.4 parts, 1.8 parts, 2.2 parts, 2.7 parts, 3.2 parts, 3.7 parts, 4.2 parts, 4.7 parts, 5.2 parts, 5.7 parts, 6.3 parts, 6.8 parts, 7.5 parts, 8.1 parts, 8.6 parts, 9.1 parts, 9.7 parts, 10.5 parts, 11 parts, 11.5 parts, 12 parts, 12.5 parts, 13 parts, 13.5 parts, 14 parts or 14.5 parts.
Preferably, described RTV silicone rubber sealant comprises following raw material by mass parts:
Preferably, described RTV silicone rubber sealant comprises following raw material by mass parts:
Preferably, described α, the α of alpha, omega-dihydroxy polydimethyl siloxane to be kinetic viscosity be 1500 ~ 50000cps, the combination of any one or at least two kinds in alpha, omega-dihydroxy polydimethyl siloxane, preferred kinetic viscosity is the α of 2000 ~ 45000cps, the combination of any one or at least two kinds in alpha, omega-dihydroxy polydimethyl siloxane, further preferably kinetic viscosity is the α of 3000 ~ 40000cps, the combination of any one or at least two kinds in alpha, omega-dihydroxy polydimethyl siloxane.Described α, alpha, omega-dihydroxy polydimethyl siloxane is such as kinetic viscosity is the α of 2500cps, alpha, omega-dihydroxy polydimethyl siloxane, kinetic viscosity is the α of 3500cps, alpha, omega-dihydroxy polydimethyl siloxane, kinetic viscosity is the α of 5000cps, alpha, omega-dihydroxy polydimethyl siloxane, kinetic viscosity is the α of 8000cps, alpha, omega-dihydroxy polydimethyl siloxane, kinetic viscosity is the α of 12000cps, alpha, omega-dihydroxy polydimethyl siloxane, kinetic viscosity is the α of 22000cps, alpha, omega-dihydroxy polydimethyl siloxane, kinetic viscosity is the α of 30000cps, alpha, omega-dihydroxy polydimethyl siloxane, kinetic viscosity is the α of 36000cps, alpha, omega-dihydroxy polydimethyl siloxane, kinetic viscosity is the α of 42000cps, alpha, omega-dihydroxy polydimethyl siloxane, kinetic viscosity is the α of 48000cps, alpha, omega-dihydroxy polydimethyl siloxane.
Preferably, the mixture of described dimethyl silicone oil to be kinetic viscosity be in the dimethyl silicone oil of 50 ~ 5000cps any one or at least two kinds, preferred kinetic viscosity is the mixture of any one or at least two kinds in the dimethyl silicone oil of 60 ~ 4800cps, and preferably kinetic viscosity is the mixture of any one or at least two kinds in the dimethyl silicone oil of 70 ~ 4500cps further.Described dimethyl silicone oil is such as kinetic viscosity is the dimethyl silicone oil of 55cps, kinetic viscosity is the dimethyl silicone oil of 750cps, kinetic viscosity is the dimethyl silicone oil of 1050cps, kinetic viscosity is the dimethyl silicone oil of 1250cps, kinetic viscosity is the dimethyl silicone oil of 1800cps, and kinetic viscosity is the dimethyl silicone oil of 2700cps, and kinetic viscosity is the dimethyl silicone oil of 3500cps, kinetic viscosity is the dimethyl silicone oil of 4200cps, and kinetic viscosity is the dimethyl silicone oil of 4800cps.
Preferably, described nanometer reinforced filling is selected from the mixture of any one or at least two kinds in hydrophilic gas-phase silica, nano-calcium carbonate or nano zine oxide.The mixture of described mixture such as hydrophilic gas-phase silica and nano-calcium carbonate, the mixture of nano zine oxide and hydrophilic gas-phase silica, the mixture of nano-calcium carbonate and nano zine oxide, the mixture of hydrophilic gas-phase silica, nano-calcium carbonate and nano zine oxide.
Preferably, described fire-retardant filler be aluminium hydroxide or/and magnesium hydroxide, preferred magnesium hydroxide and aluminium hydroxide.
Using aluminium hydroxide and magnesium hydroxide collocation as main fire-retardant filler, then add nano zine oxide and assist, improve thermotolerance and the thixotropy of seal gum, flame retardant rating reaches UL94V-0 rank.
Preferably, described hydroxyl scavenging agent is hexamethyldisilazane.
Preferably, described coupling agent is selected from the mixture of any one or at least two kinds in γ-aminopropyl triethoxysilane, γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane, vinyltriethoxysilane, N-aminoethyl-γ-aminopropyltrimethoxysilane or γ-(methacryloxypropyl) propyl trimethoxy silicane.The mixture of described mixture such as γ-(methacryloxypropyl) propyl trimethoxy silicane and N-aminoethyl-γ-aminopropyltrimethoxysilane, N-aminoethyl-γ-aminopropyltrimethoxysilane and γ-(2, 3-epoxy third oxygen) mixture of propyl trimethoxy silicane, γ-(2, 3-epoxy third oxygen) mixture of propyl trimethoxy silicane and vinyltriethoxysilane, the mixture of vinyltriethoxysilane and γ-aminopropyl triethoxysilane, γ-(methacryloxypropyl) propyl trimethoxy silicane, N-aminoethyl-γ-aminopropyltrimethoxysilane and γ-(2, 3-epoxy third oxygen) mixture of propyl trimethoxy silicane, vinyltriethoxysilane, the mixture of γ-aminopropyl triethoxysilane and N-aminoethyl-γ-aminopropyltrimethoxysilane, γ-(methacryloxypropyl) propyl trimethoxy silicane, N-aminoethyl-γ-aminopropyltrimethoxysilane, γ-(2, 3-epoxy third oxygen) mixture of propyl trimethoxy silicane and vinyltriethoxysilane, γ-aminopropyl triethoxysilane, γ-(methacryloxypropyl) propyl trimethoxy silicane, N-aminoethyl-γ-aminopropyltrimethoxysilane, γ-(2, 3-epoxy third oxygen) mixture of propyl trimethoxy silicane and vinyltriethoxysilane, preferred γ-(2, 3-epoxy third oxygen) propyl trimethoxy silicane and N-aminoethyl-γ-aminopropyltrimethoxysilane.
The interworking of γ-(2,3-epoxy third oxygen) between propyl trimethoxy silicane and N-aminoethyl-γ-aminopropyltrimethoxysilane uses, and improves the yellowing resistance of seal gum.
Preferably, described linking agent is selected from the mixture of any one or at least two kinds in tetraethoxy, methyl silicate, vinyltrimethoxy silane, methyltrimethoxy silane or diethylin Union carbide A-162.The mixture of described mixture such as diethylin Union carbide A-162 and methyltrimethoxy silane, the mixture of methyltrimethoxy silane and vinyltrimethoxy silane, the mixture of vinyltrimethoxy silane and methyl silicate, the mixture of methyl silicate and tetraethoxy, the mixture of tetraethoxy and diethylin Union carbide A-162, methyltrimethoxy silane, the mixture of vinyltrimethoxy silane and methyl silicate, methyl silicate, the mixture of tetraethoxy and diethylin Union carbide A-162, diethylin Union carbide A-162, methyltrimethoxy silane, the mixture of vinyltrimethoxy silane and methyl silicate, tetraethoxy, diethylin Union carbide A-162, the mixture of methyltrimethoxy silane and vinyltrimethoxy silane, diethylin Union carbide A-162, methyltrimethoxy silane, vinyltrimethoxy silane, the mixture of methyl silicate and tetraethoxy.
Preferably, described catalyzer is that diethylin Union carbide A-162 is or/and anilinomethyl triethoxysilane.
Two of object of the present invention is the preparation method providing the fire-retardant RTV silicone rubber sealant of a kind of single-component dealcoholization-type as above, and described method comprises the steps:
(1) by the α of formula ratio, alpha, omega-dihydroxy polydimethyl siloxane, dimethyl silicone oil, nanometer reinforced filling, fire-retardant filler and hydroxyl scavenging agent are in temperature 120 ~ 150 DEG C in power mixer, and vacuum tightness 0.09 ~ 0.1MPa dewaters blended 60 ~ 240 minutes acquisition base-materials;
(2) at normal temperatures, this base-material is evacuated to vacuum tightness 0.09 ~ 0.1MPa, stirs 10min, add the linking agent of formula ratio, stir 15 ~ 30min under vacuum condition, then add the coupling agent of formula ratio, stir 10 ~ 30min under vacuum condition, can finished product be packaged as.
Compared with prior art, the present invention has following beneficial effect:
(1) flame retardant resistance aspect, using aluminium hydroxide and magnesium hydroxide collocation as main fire-retardant filler, then add nano zine oxide and assist, improve thermotolerance and the thixotropy of seal gum, flame retardant rating reaches UL94V-0 rank.
(2) γ-(2,3-epoxy third oxygen) interworking between propyl trimethoxy and N-aminoethyl-γ-aminopropyl trimethoxy uses, improve the yellowing resistance of seal gum, yellowing resistance specific performance is: after seal gum extrudes sizing material from sebific duct, put into 120 DEG C of baking ovens, 24 hours non-yellowing at once.
Embodiment
For better the present invention being described, be convenient to understand technical scheme of the present invention, typical but non-limiting embodiment of the present invention is as follows:
Embodiment 1
The fire-retardant RTV silicone rubber sealant of a kind of single-component dealcoholization-type, described RTV silicone rubber sealant comprises following raw material by mass parts:
Described α, the α of alpha, omega-dihydroxy polydimethyl siloxane to be kinetic viscosity be 1500cps, alpha, omega-dihydroxy polydimethyl siloxane, the dimethyl silicone oil of described dimethyl silicone oil to be kinetic viscosity be 50cps, described nanometer reinforced filling is hydrophilic gas-phase silica, and described fire-retardant filler is aluminium hydroxide and magnesium hydroxide, and described hydroxyl scavenging agent is hexamethyldisilazane, described coupling agent is γ-aminopropyl triethoxysilane, and described linking agent is tetraethoxy.
The preparation method of the fire-retardant RTV silicone rubber sealant of above-mentioned single-component dealcoholization-type is as follows:
(1) by the α of formula ratio, alpha, omega-dihydroxy polydimethyl siloxane, dimethyl silicone oil, nanometer reinforced filling, fire-retardant filler and hydroxyl scavenging agent are in temperature 120 ~ 150 DEG C in power mixer, and vacuum tightness 0.09 ~ 0.1MPa dewaters blended 60 ~ 240 minutes acquisition base-materials;
(2) at normal temperatures, this base-material is evacuated to vacuum tightness 0.09 ~ 0.1MPa, stirs 10min, add the linking agent of formula ratio, stir 15 ~ 30min under vacuum condition, then add the coupling agent of formula ratio, stir 10 ~ 30min under vacuum condition, can finished product be packaged as.
Embodiment 2
The fire-retardant RTV silicone rubber sealant of a kind of single-component dealcoholization-type, described RTV silicone rubber sealant comprises following raw material by mass parts:
Described α, the α of alpha, omega-dihydroxy polydimethyl siloxane to be kinetic viscosity be 50000cps, alpha, omega-dihydroxy polydimethyl siloxane, the dimethyl silicone oil of described dimethyl silicone oil to be kinetic viscosity be 5000cps, described nanometer reinforced filling is nano-calcium carbonate, described fire-retardant filler is magnesium hydroxide, described hydroxyl scavenging agent is hexamethyldisilazane, described coupling agent is γ-aminopropyl triethoxysilane and γ-(2, 3-epoxy third oxygen) mixture of propyl trimethoxy silicane, described linking agent is the mixture of positive methyltrimethoxy silane and diethylin Union carbide A-162.
The preparation method of the fire-retardant RTV silicone rubber sealant of above-mentioned single-component dealcoholization-type, comprises the steps:
(1) by the α of formula ratio, alpha, omega-dihydroxy polydimethyl siloxane, dimethyl silicone oil, nanometer reinforced filling, fire-retardant filler and hydroxyl scavenging agent are in temperature 120 ~ 150 DEG C in power mixer, and vacuum tightness 0.09 ~ 0.1MPa dewaters blended 60 ~ 240 minutes acquisition base-materials;
(2) at normal temperatures, this base-material is evacuated to vacuum tightness 0.09 ~ 0.1MPa, stirs 10min, add the linking agent of formula ratio, stir 15 ~ 30min under vacuum condition, then add the coupling agent of formula ratio, stir 10 ~ 30min under vacuum condition, can finished product be packaged as.
Embodiment 3
The fire-retardant RTV silicone rubber sealant of a kind of single-component dealcoholization-type, described RTV silicone rubber sealant comprises following raw material by mass parts:
Described α, the α of alpha, omega-dihydroxy polydimethyl siloxane to be kinetic viscosity be 26000cps, alpha, omega-dihydroxy polydimethyl siloxane, the dimethyl silicone oil of described dimethyl silicone oil to be kinetic viscosity be 3400cps, described nanometer reinforced filling is nano zine oxide, described hydroxyl scavenging agent is hexamethyldisilazane, described coupling agent is γ-aminopropyl triethoxysilane and γ-(2,3-epoxy third oxygen) mixture of propyl trimethoxy silicane, described linking agent is the mixture of tetraethoxy, methyl silicate and vinyltrimethoxy silane.
The preparation method of the fire-retardant RTV silicone rubber sealant of above-mentioned single-component dealcoholization-type, described method comprises the steps:
(1) by the α of formula ratio, alpha, omega-dihydroxy polydimethyl siloxane, dimethyl silicone oil, nanometer reinforced filling, fire-retardant filler and hydroxyl scavenging agent are in temperature 120 ~ 150 DEG C in power mixer, and vacuum tightness 0.09 ~ 0.1MPa dewaters blended 60 ~ 240 minutes acquisition base-materials;
(2) at normal temperatures, this base-material is evacuated to vacuum tightness 0.09 ~ 0.1MPa, stirs 10min, add the linking agent of formula ratio, stir 15 ~ 30min under vacuum condition, then add the coupling agent of formula ratio, stir 10 ~ 30min under vacuum condition, can finished product be packaged as.
It should be noted that and understand, when not departing from the spirit and scope of the present invention required by accompanying claim, various amendment and improvement can be made to the present invention of foregoing detailed description.Therefore, the scope of claimed technical scheme is not by the restriction of given any specific exemplary teachings.
Applicant states, the present invention illustrates method detailed of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned method detailed, does not namely mean that the present invention must rely on above-mentioned method detailed and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.

Claims (1)

1. the fire-retardant RTV silicone rubber sealant of single-component dealcoholization-type, described RTV silicone rubber sealant comprises following raw material by mass parts:
Described α, the α of alpha, omega-dihydroxy polydimethyl siloxane to be kinetic viscosity be 26000cps, alpha, omega-dihydroxy polydimethyl siloxane, the dimethyl silicone oil of described dimethyl silicone oil to be kinetic viscosity be 3400cps, described nanometer reinforced filling is nano zine oxide, described hydroxyl scavenging agent is hexamethyldisilazane, described coupling agent is γ-aminopropyl triethoxysilane and γ-(2,3-epoxy third oxygen) mixture of propyl trimethoxy silicane, described linking agent is the mixture of tetraethoxy, methyl silicate and vinyltrimethoxy silane;
The preparation method of the fire-retardant RTV silicone rubber sealant of above-mentioned single-component dealcoholization-type, described method comprises the steps:
(1) by the α of formula ratio, alpha, omega-dihydroxy polydimethyl siloxane, dimethyl silicone oil, nanometer reinforced filling, fire-retardant filler and hydroxyl scavenging agent are in temperature 120 ~ 150 DEG C in power mixer, and vacuum tightness 0.09 ~ 0.1MPa dewaters blended 60 ~ 240 minutes acquisition base-materials;
(2) at normal temperatures, this base-material is evacuated to vacuum tightness 0.09 ~ 0.1MPa, stirs 10min, add the linking agent of formula ratio, stir 15 ~ 30min under vacuum condition, then add the coupling agent of formula ratio, stir 10 ~ 30min under vacuum condition, can finished product be packaged as.
CN201310335563.1A 2013-08-02 2013-08-02 Single-component dealcoholization-type flame-retardant room temperature vulcanized (RTV) silicone rubber sealant and preparation method thereof Active CN103396757B (en)

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