CN103396757A - 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 PDFInfo
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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
Technical field
The present invention relates to the silicon rubber preparing technical field, be specifically related to fire-retardant RTV silicon rubber sealant of a kind of single-component dealcoholization-type and preparation method thereof.
Background technology
High speed development along with electric, building and Aviation Industry, the room temperature silicone sulphurated siliastic, owing to having neutral character, to advantages such as base material non-corrosiveness, nontoxic, strong adaptability and cost value are lower, enjoys sector application and investigator's favor and obtains develop rapidly.Simultaneously, single-component room-temperature vulcanized silicone rubber (RTV), namely at room temperature without adding other component namely curable, easy to use, solidify post-shrinkage ratio little, good to most of material adhesive performances, have good anti-electrical insulating property, weathering resistance, flexible resistance, high thermal resistance and ageing resistance etc.At industrial circles such as building, electronics, automobile makings, application is very widely arranged, 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, alpha, omega-dihydroxy polydimethyl siloxane and filler dehydration blend, obtain base-material; Get base-material, at vacuum state, stir, add linking agent, at vacuum state, stir; Add coupling agent, stir; Add catalyzer, vacuumize, pass into rare gas element, stir, vacuumize, stir, get final product to obtain finished product.
CN102757759A discloses a kind of single-component dealcoholization-type RTV silicon rubber sealant, wherein base-material comprises by weight: α, 100 parts of alpha, omega-dihydroxy polydimethyl siloxanes, 1～150 part, softening agent, 1～150 part of nano level reinforced filling, 0.1～20 part of hydroxyl scavenging agent, finished product comprises by weight: 100 parts of base-materials, 0.1～30 part of linking agent, 0.1～8 part of coupling agent.The preparation method of described single-component dealcoholization-type RTV silicon rubber sealant comprises: by α, and alpha, omega-dihydroxy polydimethyl siloxane, softening agent, nano level reinforced filling and hydroxyl scavenging agent, the dehydration blend, obtain 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: the employing nano material is filler, and adds softening agent, makes product that good physicals be arranged; Add the silane treatment Nano filling, extend the seal gum shelf lives.
But in prior art, disclosed RTV silicon rubber sealant 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, one of purpose of the present invention is to provide a kind of single-component dealcoholization-type fire-retardant RTV silicon rubber sealant, and the flame retardant properties of described RTV silicon rubber sealant and yellowing resistance can be excellent, and excellent heat resistance.
In order to achieve the above object, the present invention has adopted following technical scheme:
The fire-retardant RTV silicon rubber sealant of a kind of single-component dealcoholization-type, described RTV silicon rubber sealant comprises following raw material by mass parts:
The mass parts of described dimethyl silicone oil is for example 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 the described reinforced filling of nanometer is for example 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 for example 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 for example 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 for example 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 for example 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 silicon rubber sealant comprises following raw material by mass parts:
Preferably, described RTV silicon rubber sealant comprises following raw material by mass parts:
Preferably, described α, alpha, omega-dihydroxy polydimethyl siloxane is that kinetic viscosity is the α of 1500～50000cps, the combination of any one in alpha, omega-dihydroxy polydimethyl siloxane or at least two kinds, preferred kinetic viscosity is the α of 2000～45000cps, the combination of any one in alpha, omega-dihydroxy polydimethyl siloxane or at least two kinds, further preferred kinetic viscosity is the α of 3000～40000cps, the combination of any one in alpha, omega-dihydroxy polydimethyl siloxane or at least two kinds.described α, alpha, omega-dihydroxy polydimethyl siloxane is for example the α of 2500cps for kinetic viscosity, 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, described dimethyl silicone oil is that kinetic viscosity is the mixture of any one or at least two kinds in the dimethyl silicone oil of 50～5000cps, preferred kinetic viscosity is the mixture of any one or at least two kinds in the dimethyl silicone oil of 60～4800cps, the mixture of any one in the dimethyl silicone oil that further preferred kinetic viscosity is 70～4500cps or at least two kinds.Described dimethyl silicone oil is for example the dimethyl silicone oil of 55cps for kinetic viscosity, 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.Described mixture is the mixture of hydrophilic gas-phase silica and nano-calcium carbonate for example, 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 is that aluminium hydroxide is or/and magnesium hydroxide, preferably magnesium hydroxide and aluminium hydroxide.
Using aluminium hydroxide and magnesium hydroxide collocation as main fire-retardant filler, then add nano zine oxide auxiliary, improved thermotolerance and the thixotropy of seal gum, flame retardant rating reaches the 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 the third oxygen) propyl trimethoxy silicane, vinyltriethoxysilane, N-aminoethyl-γ-aminopropyltrimethoxysilane or γ-(methacryloxypropyl) propyl trimethoxy silicane.described mixture is the mixture of γ-(methacryloxypropyl) propyl trimethoxy silicane and N-aminoethyl-γ-aminopropyltrimethoxysilane for example, N-aminoethyl-γ-aminopropyltrimethoxysilane and γ-(2, 3-epoxy the third oxygen) mixture of propyl trimethoxy silicane, γ-(2, 3-epoxy the 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 the 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 the 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 the third oxygen) mixture of propyl trimethoxy silicane and vinyltriethoxysilane, preferred γ-(2, 3-epoxy the third oxygen) propyl trimethoxy silicane and N-aminoethyl-γ-aminopropyltrimethoxysilane.
Interworking between γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane and N-aminoethyl-γ-aminopropyltrimethoxysilane is used, and has improved 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.described mixture is the mixture of diethylin Union carbide A-162 and methyltrimethoxy silane for example, 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, the diethylin Union carbide A-162, methyltrimethoxy silane, the mixture of vinyltrimethoxy silane and methyl silicate, tetraethoxy, the diethylin Union carbide A-162, the mixture of methyltrimethoxy silane and vinyltrimethoxy silane, the diethylin Union carbide A-162, methyltrimethoxy silane, vinyltrimethoxy silane, the mixture of methyl silicate and tetraethoxy.
Preferably, described catalyzer is that the diethylin Union carbide A-162 is or/and anilinomethyl triethoxysilane.
Two of purpose of the present invention is to provide the preparation method of the fire-retardant RTV silicon 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 in power mixer in 120～150 ℃ of temperature, 60～240 minutes acquisition base-materials of vacuum tightness 0.09～0.1MPa dehydration blend;
(2) at normal temperatures, this base-material is evacuated to vacuum tightness 0.09～0.1MPa, stirs 10min, under the linking agent that adds formula ratio, vacuum condition, stir 15～30min, then add the coupling agent of formula ratio, under vacuum condition, stir 10～30min, can be packaged as finished product.
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 auxiliary, improved thermotolerance and the thixotropy of seal gum, and flame retardant rating reaches the UL94V-0 rank.
(2) γ-(2,3-epoxy the third oxygen) interworking between propyl trimethoxy and N-aminoethyl-γ-aminopropyl trimethoxy is used, and improves the yellowing resistance of seal gum, and the yellowing resistance specific performance is: after seal gum is extruded sizing material from sebific duct, put into 120 ℃ of baking ovens, 24 hours non-yellowing at once.
Embodiment
For the present invention is described better, 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 silicon rubber sealant of a kind of single-component dealcoholization-type, described RTV silicon rubber sealant comprises following raw material by mass parts:
Described α, alpha, omega-dihydroxy polydimethyl siloxane is that kinetic viscosity is the α of 1500cps, alpha, omega-dihydroxy polydimethyl siloxane, described dimethyl silicone oil is that kinetic viscosity is the dimethyl silicone oil of 50cps, described nanometer reinforced filling is the 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 silicon 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 in power mixer in 120～150 ℃ of temperature, 60～240 minutes acquisition base-materials of vacuum tightness 0.09～0.1MPa dehydration blend;
(2) at normal temperatures, this base-material is evacuated to vacuum tightness 0.09～0.1MPa, stirs 10min, under the linking agent that adds formula ratio, vacuum condition, stir 15～30min, then add the coupling agent of formula ratio, under vacuum condition, stir 10～30min, can be packaged as finished product.
Embodiment 2
The fire-retardant RTV silicon rubber sealant of a kind of single-component dealcoholization-type, described RTV silicon rubber sealant comprises following raw material by mass parts:
described α, alpha, omega-dihydroxy polydimethyl siloxane is that kinetic viscosity is the α of 50000cps, alpha, omega-dihydroxy polydimethyl siloxane, described dimethyl silicone oil is that kinetic viscosity is the dimethyl silicone oil of 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 the 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 silicon rubber sealant of above-mentioned single-component dealcoholization-type, comprise 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 in power mixer in 120～150 ℃ of temperature, 60～240 minutes acquisition base-materials of vacuum tightness 0.09～0.1MPa dehydration blend;
(2) at normal temperatures, this base-material is evacuated to vacuum tightness 0.09～0.1MPa, stirs 10min, under the linking agent that adds formula ratio, vacuum condition, stir 15～30min, then add the coupling agent of formula ratio, under vacuum condition, stir 10～30min, can be packaged as finished product.
Embodiment 3
The fire-retardant RTV silicon rubber sealant of a kind of single-component dealcoholization-type, described RTV silicon rubber sealant comprises following raw material by mass parts:
Described α, alpha, omega-dihydroxy polydimethyl siloxane is that kinetic viscosity is the α of 26000cps, alpha, omega-dihydroxy polydimethyl siloxane, described dimethyl silicone oil is that kinetic viscosity is the dimethyl silicone oil of 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 the 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 silicon 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 in power mixer in 120～150 ℃ of temperature, 60～240 minutes acquisition base-materials of vacuum tightness 0.09～0.1MPa dehydration blend;
(2) at normal temperatures, this base-material is evacuated to vacuum tightness 0.09～0.1MPa, stirs 10min, under the linking agent that adds formula ratio, vacuum condition, stir 15～30min, then add the coupling agent of formula ratio, under vacuum condition, stir 10～30min, can be packaged as finished product.
Should be noted that and understand, in the situation that do not break away from the desired the spirit and scope of the present invention of accompanying claim, can make to the present invention of foregoing detailed description various modifications and improvement.Therefore, the scope of claimed technical scheme is not subjected to the restriction of given any specific exemplary teachings.
Applicant's statement, 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 mean that namely the present invention must rely on above-mentioned method detailed and could implement.The person of ordinary skill in the field should understand, any improvement in the present invention, to the interpolation of the equivalence replacement of each raw material of product of the present invention and ancillary component, the selection of concrete mode etc., within all dropping on protection scope of the present invention and open scope.
Claims (10)
1. the fire-retardant RTV silicon rubber sealant of single-component dealcoholization-type, is characterized in that, described RTV silicon rubber sealant comprises following raw material by mass parts:
2. seal gum as claimed in claim 1, is characterized in that, described RTV silicon rubber sealant comprises following raw material by mass parts:
3. seal gum as claimed in claim 1, is characterized in that, described RTV silicon rubber sealant comprises following raw material by mass parts:
4. seal gum as described as one of claim 1-3, it is characterized in that, described α, alpha, omega-dihydroxy polydimethyl siloxane is that kinetic viscosity is the α of 1500～50000cps, the combination of any one in alpha, omega-dihydroxy polydimethyl siloxane or at least two kinds, preferred kinetic viscosity is the α of 2000～45000cps, the combination of any one in alpha, omega-dihydroxy polydimethyl siloxane or at least two kinds, further preferred kinetic viscosity is the α of 3000～40000cps, the combination of any one in alpha, omega-dihydroxy polydimethyl siloxane or at least two kinds.
5. seal gum as described as one of claim 1-4, it is characterized in that, described dimethyl silicone oil is that kinetic viscosity is the mixture of any one or at least two kinds in the dimethyl silicone oil of 50～5000cps, preferred kinetic viscosity is the mixture of any one or at least two kinds in the dimethyl silicone oil of 60～4800cps, the mixture of any one in the dimethyl silicone oil that further preferred kinetic viscosity is 70～4500cps or at least two kinds.
6. seal gum as described as one of claim 1-5, is characterized in that, 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;
Preferably, described fire-retardant filler is that aluminium hydroxide is or/and magnesium hydroxide, preferably magnesium hydroxide and aluminium hydroxide.
7. seal gum as described as one of claim 1-6, is characterized in that, described hydroxyl scavenging agent is hexamethyldisilazane.
8. seal gum as described as one of claim 1-7, it is characterized in that, described coupling agent is selected from γ-aminopropyl triethoxysilane, γ-(2,3-epoxy the third oxygen) mixture of any one in propyl trimethoxy silicane, vinyltriethoxysilane, N-aminoethyl-γ-aminopropyltrimethoxysilane or γ-(methacryloxypropyl) propyl trimethoxy silicane or at least two kinds, preferred γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane and N-aminoethyl-γ-aminopropyltrimethoxysilane.
9. seal gum as described as one of claim 1-8, it is characterized in that, 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.
10. the preparation method of the fire-retardant RTV silicon rubber sealant of single-component dealcoholization-type as described as one of claim 1-9, is characterized in that, 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 in power mixer in 120～150 ℃ of temperature, 60～240 minutes acquisition base-materials of vacuum tightness 0.09～0.1MPa dehydration blend;
(2) at normal temperatures, this base-material is evacuated to vacuum tightness 0.09～0.1MPa, stir 10min, the linking agent that adds formula ratio, under vacuum condition, stir 15～30min, then add the coupling agent of formula ratio, under vacuum condition, stir 10～30min, can be packaged as finished product, obtain the fire-retardant RTV silicon rubber sealant of single-component dealcoholization-type.
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Address after: Two street 523233 Guangdong province Dongguan City Chudo Zhen Dong Bo Cun Da Xin Wei Lu Daxin Road No. 1 Patentee after: Zhaoshun Technology (Guangdong) Co., Ltd Address before: Two street 523233 Guangdong province Dongguan City Chudo Zhen Dong Bo Cun Da Xin Wei Lu Daxin Road No. 1 Patentee before: Dongguan million Shun's organosilicon Science and Technology Co., Ltd. |