CN1221626C - Neutral silicone fire-retardent sealing glue and its preparing method - Google Patents
Neutral silicone fire-retardent sealing glue and its preparing method Download PDFInfo
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- CN1221626C CN1221626C CN 03117403 CN03117403A CN1221626C CN 1221626 C CN1221626 C CN 1221626C CN 03117403 CN03117403 CN 03117403 CN 03117403 A CN03117403 A CN 03117403A CN 1221626 C CN1221626 C CN 1221626C
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- neutral silicone
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- seal gum
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Abstract
The present invention relates to neutral silicone fire-retardant sealing glue and a preparing method thereof, which is characterized in that 10 to 90 portions of alpha, omega-dihydroxyl polysiloxane, 90 to 10 portions of stuffing material and 10 to 90 portions of fire-retardant agent are added into a vacuum kneading machine and dewatered and mixed for 60 to 300 minutes at the temperature of 80 to 150 DEG C, and the vacuum degree of-0.06 to 0.095MPa; then, the mixture is moved into a high-speed dispersing and stirring vessel; subsequently, 1 to 10 portions of silane crosslinking agent, 1 to 10 portions of thixotropic agent. 1 to 10 portions of tackifier, 0.1 to 5 portions of catalytic curing agent and 1 to 10 portions of plasticizing agent are added into the stirring vessel at room temperature and mixed with the alpha, omega-dihydroxyl polysiloxane mixture so as to realize a chemical reaction for 30 to 180 minutes at the vacuum degree of-0.06 to-0.095MPa and the rotation speed of 100 to 600 rpm; thus, the neutral silicone fire-retardant sealing glue is obtained. The neutral silicone fire-retardant sealing glue has the key technical indexes that the pendent degree is zero by being tested according to GB/T13477, the extrusion property is from 2.3 to 2.8 by being tested according to GB16776, and the fire-retardant property is FV-0 grade by being tested according to GB/T2048-1996. All the indexes achieve and exceed the national specified indexes.
Description
One, technical field
The present invention relates to a kind of neutral silicone fireproof seal gum and manufacture method thereof, belong to the synthetic and Application Areas of polymer material of construction.
Two, background technology
Silicone sealant has excellent weather, warm, ultraviolet ray and ozone ageing performance thereof, is one of preferred material of building sealant.Widespread use along with building curtain wall, silicone sealant has obtained swift and violent development, fire-retardant sealing and fixing after the fire prevention of top-grade building, fire-retardant sealing, cable penetration, the Durchgangshohle, the fire prevention of building curtain wall are cut off (the interlayer fire prevention cuts off), and the surface etc. that needs the fire protection flame retarding sealing in the upholstery.The ordinary silicon ketone seal gum has been obtained certain achievement aspect adhesive property; Chinese patent 01107167.2 disclosed " neutral silicone sealant for stone material and manufacture method thereof " has also been obtained satisfied effect aspect adhesiveproperties.But be not resolved yet aspect fire protection flame retarding and the over-all properties.
Three, summary of the invention
The objective of the invention is provides a kind of neutral silicone fireproof seal gum and preparation method thereof at the deficiencies in the prior art.Be characterized in adopting α, alpha, omega-dihydroxy polysiloxane to be base-material, to introduce reactive silane tackifier and applied fireproofing thereof, make the neutral silicone fireproof seal gum of and fire protection flame retarding pollution-free base material.
Purpose of the present invention is realized that by following technical measures wherein said raw material umber is parts by weight except that specified otherwise.
10～90 parts of α, alpha, omega-dihydroxy polysiloxane
1～10 part in softening agent
90～10 parts of fillers
1～10 part of thixotropic agent
1～10 part of linking agent
1090 parts of fire retardants
1～10 part of tackifier
0.1～5 part of catalytic curing agent
Wherein α, alpha, omega-dihydroxy polysiloxane are at least a in the poly-di-ethyl siloxane of α, alpha, omega-dihydroxy polydimethyl siloxane, α, alpha, omega-dihydroxy, α, the poly-diphenyl siloxane of alpha, omega-dihydroxy.
Softening agent is α, ω-dimethyl polydimethylsiloxane, at least a in α, ω-diethyl polydimethylsiloxane, α, the ω-phenylbenzene polydimethylsiloxane.
Filler is at least a in lime carbonate, wilkinite, activated clay, silicon powder, the talcum powder.
Thixotropic agent is at least a in silicon-dioxide, hydrogenated castor oil, the polyethylene wax.
Linking agent is at least a in methyltrimethoxy silane, ethyl trimethoxy silane, methyl tributanoximo silane, the phenyltrimethoxysila,e.
Fire retardant is at least a in zinc subcarbonate, zinc borate, aluminium hydroxide, magnesium hydroxide, red iron oxide, decabromodiphenyl oxide, red phosphorus, the clorafin.
Tackifier are at least a in the ethyl acetoacetate chelate of isopropyl titanate, butyl (tetra) titanate, r-aminopropyltriethoxywerene werene, 1,2-epoxy oxyethyl group Trimethoxy silane, carbonic ether.
Catalytic curing agent is at least a in dibutyl tin laurate, dibutyltin diacetate, the stannic oxide methyl aceto acetate complex compound.
The manufacture method of neutral silicone fireproof seal gum:
1, with 10～90 parts of α, alpha, omega-dihydroxy polysiloxane, 90～10 parts of fillers and fire retardant add in the vacuum kneader for 10～90 parts, and in 80～150 ℃ of temperature, vacuum tightness is 0.06～0.095MPa, dehydration blend 60～300 minutes, move in the high speed dispersion stirring tank, standby;
2, at room temperature, 1～10 part of silane crosslinker, 1～10 part of thixotropic agent, 1～10 part of tackifier, 0.1～5 part of catalytic curing agent and softening agent are added in the stirring tank for 1～10 part, mix with above-mentioned standby α, alpha, omega-dihydroxy polysiloxane mixture, vacuum tightness is 0.06～0.095MPa, rotating speed 100～600rpm, carry out chemical reaction 30～180 minutes, and obtained the neutral silicone fireproof seal gum.
The main performance index of neutral silicone fireproof seal gum: sag is zero by GB/T13477 test, and extrudability is 2.3～2.8 by the GB/16776 test, and it is the FV-0 level that flame retardant resistance press the GB/T2048-1996 test, all reaches and surpasses state specified standards.
The present invention has following advantage:
1, adopt fire retardant, the product fire resistance is good, and its fire retardant performance reaches the FV-0 level of GB/T2408-1996, belongs to domestic initiation.
2, adopt neutral curing system,, base material is had good cohesive force base material non-corrosivenesss such as concrete, glass, stone material and metals.
3, product easy construction, weather, aging resistance brilliance, fire resistance are good, integrated performance index all reaches leading domestic level.
4, energy consumption is low in process of production, and the no three wastes produce, and environmentally safe has remarkable economic efficiency and social benefit.
Four, embodiment
Below by embodiment the present invention is carried out concrete description; be necessary to be pointed out that at this following examples only are used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, the person skilled in the art in this field can make some nonessential improvement and adjustment according to the content of the invention described above.
Embodiment 1
With α, 200 kilograms of alpha, omega-dihydroxy polydimethyl siloxanes, 45 kilograms in lime carbonate, 150 kilograms in aluminium hydroxide, 30 kilograms of red iron oxides, add in the vacuum kneader, in 100 ℃ of temperature, vacuum tightness is 0.06～0.095MPa, dehydration blend 60 minutes, moves in the high speed dispersion stirring tank; At room temperature, with 0.5 kilogram of 5 kilograms of silica 1s, 3 kilograms of isopropyl titanates, 12 kilograms of methyltrimethoxy silanes, α, ω-18 kilograms of dimethyl polydimethylsiloxanes and dibutyl tin laurate, add in the stirring tank, mix with above-mentioned α, alpha, omega-dihydroxy polydimethyl siloxane mixture, vacuum tightness is 0.06～0.095MPa, rotating speed 350rpm, carried out chemical reaction 80 minutes, obtain neutral silicone fireproof seal gum product, product and product see for details shown in table 1 and the table 2 in the performance test structure of different states.
Embodiment 2
With α, 200 kilograms of the poly-di-ethyl siloxane of alpha, omega-dihydroxy, 50 kilograms of silicon powders, 130 kilograms of magnesium hydroxides, 40 kilograms of zinc subcarbonates, add in the vacuum kneader, in 120 ℃ of temperature, vacuum tightness is 0.06～0.095MPa, dehydration blend 90 minutes, moves in the high speed dispersor; At room temperature, with 1.8 kilograms of 10 kilograms of ethyl trimethoxy silanes, 18 kilograms of hydrogenated castor oils and butyl (tetra) titanates, 1.0 kilograms of α, ω-5 kilograms of diethyl polydimethylsiloxanes and toxilic acid dibutyl tins, add in the stirring tank, mix with above-mentioned α, the poly-di-ethyl siloxane mixture of alpha, omega-dihydroxy, vacuum tightness is 0.06～0.095MPa, rotating speed 360rpm, carried out chemical reaction 60 minutes, obtain neutral silicone fireproof seal gum product, product and product see for details shown in table 1 and the table 2 in the performance test structure of different states.
Embodiment 3
With α, 150 kilograms of the poly-diphenyl siloxane of alpha, omega-dihydroxy, 50 kilograms of activated clays, 20 kilograms of red iron oxides, 140 kilograms of decabromodiphenyl oxides, add in the vacuum kneader, in 120 ℃ of temperature, vacuum tightness is 0.06～0.095MPa, dehydration blend 180 minutes, moves in the high speed dispersor; At room temperature, with 1.8 kilograms of the ethyl acetoacetate chelates of 15 kilograms of phenyltrimethoxysila,e, 16 kilograms of polyethylene waxs and titanic acid ester, 0.5 kilogram in α, ω-13 kilograms of phenylbenzene polydimethylsiloxanes and stannic oxide methyl aceto acetate complex compound, add in the stirring tank, mix with above-mentioned α, the poly-diphenyl siloxane mixture of alpha, omega-dihydroxy, vacuum tightness is 0.06～0.095MPa, rotating speed 380rpm, carried out chemical reaction 60 minutes, obtain neutral silicone fireproof seal gum product, product and product see for details shown in table 1 and the table 2 in the performance test structure of different states.
Table 1 is the product performance test result
Table 2 is the adhesive property test result of product at different states
Claims (8)
1, neutral silicone fireproof seal gum is characterized in that the starting raw material recipe ingredient of this fireproof seal gum is by weight:
10～90 parts of α, alpha, omega-dihydroxy polysiloxane
1～10 part in softening agent
90～10 parts of fillers
1～10 part of thixotropic agent
1～10 part of linking agent
10～90 parts of fire retardants
1～10 part of tackifier
0.1～5 part of catalytic curing agent
α wherein, the alpha, omega-dihydroxy polysiloxane is α, alpha, omega-dihydroxy polydimethyl siloxane, α, alpha, omega-dihydroxy gathers di-ethyl siloxane, α, at least a in the poly-diphenyl siloxane of alpha, omega-dihydroxy, fire retardant is a zinc subcarbonate, zinc borate, aluminium hydroxide, magnesium hydroxide, red iron oxide, decabromodiphenyl oxide, red phosphorus, at least a in the clorafin, the main performance index of neutral silicone fireproof seal gum: sag is zero by the GB/T13477 test, extrudability is 2.3～2.8 by the GB/16776 test, and flame retardant resistance is pressed the GB/T2048-1996 test and is the FV-0 level.
2,, it is characterized in that softening agent is α, ω-dimethyl polydimethylsiloxane, at least a in α, ω-diethyl polydimethylsiloxane, α, the ω-phenylbenzene polydimethylsiloxane according to the described neutral silicone fireproof seal gum of claim 1.
3,, it is characterized in that filler is at least a in lime carbonate, wilkinite, activated clay, silicon powder, the talcum powder according to the described neutral silicone fireproof seal gum of claim 1.
4,, it is characterized in that thixotropic agent is at least a in silicon-dioxide, hydrogenated castor oil, the polyethylene wax according to the described neutral silicone fireproof seal gum of claim 1.
5,, it is characterized in that linking agent is at least a in methyltrimethoxy silane, ethyl trimethoxy silane, methyl tributanoximo silane, the phenyltrimethoxysila,e according to the described neutral silicone fireproof seal gum of claim 1.
6,, it is characterized in that tackifier are at least a in the ethyl acetoacetate chelate of isopropyl titanate, butyl (tetra) titanate, r-aminopropyltriethoxywerene werene, 1,2-epoxy oxyethyl group Trimethoxy silane, carbonic ether according to the described neutral silicone fireproof seal gum of claim 1.
7,, it is characterized in that catalytic curing agent is at least a in dibutyl tin laurate, dibutyltin diacetate, the stannic oxide methyl aceto acetate complex compound according to the described neutral silicone fireproof seal gum of claim 1.
8, according to the manufacture method of the described neutral silicone fireproof seal gum of one of claim 1～7, it is characterized in that:
(1) with α, alpha, omega-dihydroxy polysiloxane 10～90 weight parts, filler 90～10 weight parts and fire retardant 10～90 weight parts add in the vacuum kneader, in 80～150 ℃ of temperature, vacuum tightness is 0.06～0.095MPa, dehydration blend 60～300 minutes, move in the high speed dispersion stirring tank, standby
(2) at room temperature, silane crosslinker 1～10 weight part, thixotropic agent 1～10 weight part, tackifier 1～10 weight part, catalytic curing agent 0.1～5 weight part and softening agent 1～10 weight part are added in the stirring tank, mix with above-mentioned standby α, alpha, omega-dihydroxy polysiloxane mixture, vacuum tightness is 0.06～0.095MPa, rotating speed 100～600rpm, carry out chemical reaction 30～180 minutes, and obtained the neutral silicone fireproof seal gum.
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| CN 03117403 CN1221626C (en) | 2003-03-06 | 2003-03-06 | Neutral silicone fire-retardent sealing glue and its preparing method |
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2003
- 2003-03-06 CN CN 03117403 patent/CN1221626C/en not_active Expired - Lifetime
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