CN103509517A - Ceramic flame-retardant fireproof silicone sealant and preparation method thereof - Google Patents
Ceramic flame-retardant fireproof silicone sealant and preparation method thereof Download PDFInfo
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- CN103509517A CN103509517A CN201310401446.0A CN201310401446A CN103509517A CN 103509517 A CN103509517 A CN 103509517A CN 201310401446 A CN201310401446 A CN 201310401446A CN 103509517 A CN103509517 A CN 103509517A
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Abstract
The invention provides a ceramic flame-retardant fireproof silicone sealant and a preparation method thereof. The ceramic flame-retardant fireproof silicone sealant is prepared from 100 parts of a base polymer, 3-40 parts of a plasticizer, 5-200 parts of a filling material, 30-150 parts of ceramic powder, 1-15 parts of a cross-linking agent, 0.1-3 parts of a stabilizer, 0.5-3 parts of a catalyst and 0.5-3 parts of a coupling agent. The preparation method comprises the following steps of adding the above raw materials into a high-speed dispersion mixer, and carrying out stirring for 60-180min under the conditions of a vacuum degree of 0.06-0.095MPa and a rotation rate of 20-600rpm to obtain the ceramic flame-retardant fireproof silicone sealant. The ceramic flame-retardant fireproof silicone sealant can form a hard ceramic material under the action of continuous ablation at a high temperature above 500 DEG C, does not lose fixing and sealing effects, has flame retardation, smoke isolation and fire prevention functions, and guarantees escape safety of people in the case of fire disaster. The invention provides the preparation of the ceramic flame-retardant fireproof silicone sealant. The preparation method has simple processes.
Description
Technical field
The invention belongs to high molecule sealing materials technical field, be specifically related to a kind of porcelain fire-retardant fireproof silicone sealant and preparation method thereof.
Background technology
Therefore silicone sealant has excellent ageing resistance, uvioresistant, shock resistance, high-low temperature resistant, in harsh climate environment, can keep the features such as elasticity, is widely used in industries such as building, automobile, electric, mechanical, chemical industry.Along with the usage quantity of Highrise buildings, hospital, station and large-scale personnel compact district silicone sealants such as public place of entertainment increases, security against fire also more and more causes people's attention, and this also makes building trade require more and more higher to the fire rating of seal gum.Although common flame-proof silicone sealant has flame retardant resistance and self-extinguishing, under continuous high temperature ablation, can become inorganic powder, thereby lose fixing and sealing function.
Summary of the invention
The invention provides a kind of porcelain fire-retardant fireproof silicone sealant that can high temperature continues to form under ablation hard ceramic material, sealing glue continues to form hard ceramic material under ablation at more than 500 ℃ high temperature, can not lose fixing and sealing function, play isolated flame, smog, fp effect, under fire condition, guaranteed personnel escape's safety; In addition, the invention provides the preparation method of sealing glue, this preparation method is easy to operate.
For reaching above-mentioned purpose, the present invention by the following technical solutions:
A fire-retardant fireproof silicone sealant, consists of the following composition, in weight part:
Described base polymer is the polydimethylsiloxane of hydroxyl-terminated injecting two methyl siloxane, trimethoxy end-blocking, at least one in methyl dimethoxy oxygen base end-blocking polydimethylsiloxane, and in the time of 25 ℃, viscosity is 0.5-200Pas.
Described filler is at least one in gas-phase silica, precipitated silica, nano-calcium carbonate, silicon powder, silica powder, organobentonite, and wherein the specific surface area of gas-phase silica is 100-300m2/g, and packing material size is 40-80nm.
Described Vitrified powder, through roasting, be take maturing temperature as 350 ℃, and roasting 30 minutes, by Vitrified powder roasting dehydration, makes short texture between molecule, is easy to react with base polymer, makes the dispersion of Vitrified powder more even., particle diameter is 0.01-10 μ m; Described Vitrified powder is that aluminium sesquioxide, boron trioxide, silicon-dioxide, Lithium Oxide 98min, sodium oxide, potassium oxide, barium oxide, calcium oxide, magnesium oxide, oxidation are secret, one or two or more kinds in zirconium white.Described linking agent is at least one in methyltrimethoxy silane, vinyltrimethoxy silane or phenyltrimethoxysila,e.
Described catalyzer is isopropyl titanate, butyl (tetra) titanate, two (methyl aceto acetate) two (isopropoxy) titanic acid ester complex compound, two (methyl ethyl diketone) two (isopropoxy) titanic acid ester complex compounds; At least one in the organo-metallic catalyst such as dibutyl tin laurate, dibutyltin diacetate
Described silane coupling agent is at least one in γ-aminopropyl triethoxysilane, β-aminoethyl-γ-aminopropyltrimethoxysilane, two (γ-trimethoxy silicomethane propyl group) amine, glycidyl ether propyl trimethoxy silicane.
Described stablizer is at least one in carbimide propyl-triethoxysilicane, molecular sieve, calcium chloride, magnesium chloride.
Described softening agent is at least one in the methyl-silicone oil moored in 50-500 of viscosity, white oil, alkoxyl silicone oil.
A kind of preparation method of porcelain fire-retardant fireproof dealcoholizing-type silicone sealant comprises the steps:
1. 100 parts of base polymers, filler 5-200 part, Vitrified powder 30-150 part are joined in vacuum kneader, and at 105-150 ℃ to the vacuum tightness 2-3h that dewaters, the base-material of cooling system under 0.06-0.1MPa;
2. above-mentioned base-material, softening agent 3-40 part, linking agent 4-15 part, catalyzer 0.5-3 part, silane coupling agent 0.5-5 part are joined in planetary mixer, keep vacuum tightness-0.1-0.06MPa, stirring velocity is 20-80 rev/min, stir 0.5-3h, make porcelain fire-retardant fireproof silicone sealant.
The present invention by adding Vitrified powder in ordinary silicon ketone seal gum, at more than 500 ℃ high temperature, continue under ablation, after absorbing heat, ashes after Vitrified powder and silicone sealant burning form ceramic material, raising and the prolongation of ablation time along with ablation temperature, the ceramic material forming can be more and more harder, avoid seal gum to lose fixing and sealing function, play isolated flame, smog, fp effect, under fire condition, guaranteed personnel escape's safety; In addition, the present invention has cohesiveness and the stability in storage of good physical and mechanical property, porcelain fire-retardant fireproof performance, excellence.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described:
Embodiment 1:
Mark by weight, 100 parts of the polydimethylsiloxanes of the trimethoxy end-blocking that is 20000cps by viscosity, 6 parts of silicon powders, 100 parts of aluminium sesquioxides are put in kneader, keep 150 ℃ of temperature, the vacuum tightness blend 2h that dewaters between 0.06-0.09MPa, crossing runner milling mills 2 times, proceed to and in high speed dispersion stirring tank, be cooled to room temperature and obtain base-material, at room temperature by 6.5 parts of methyltrimethoxy silanes, 1.5 parts of vinyltrimethoxy silanes, 0.8 part of γ-aminopropyl triethoxysilane, 0.8 part of glycidyl ether propyl trimethoxy silicane, 20 parts of methyl-silicone oils join in high speed dispersion stirring tank, mix with base-material, vacuum keep is at-0.1-0.06MPa, rotating speed remains on 250rpm, stir 1h, add 0.7 part, two (methyl aceto acetate) two (isopropoxy) titanic acid ester complex compound, stir, vacuum keep is at-0.1-0.06MPa, rotating speed remains on 250rpm, discharging tinning after stirring 1h.Make single-component porcelain fire-retardant fireproof dealcoholizing-type silicone sealant.Product performance test result is in Table 1.
Embodiment 2.
Mark by weight, 100 parts of the hydroxyl-terminated injecting two methyl siloxanes that is 20000cps by viscosity, 15 parts of gas-phase silicas, 80 parts of silicon-dioxide are put in kneader, keep 150 ℃ of temperature, the vacuum tightness blend 2h that dewaters between 0.06-0.09MPa, crossing runner milling mills 2 times, proceed to and in high speed dispersion stirring tank, be cooled to room temperature and obtain base-material, at room temperature by 8 parts of methyltrimethoxy silanes, 1 part of vinyltrimethoxy silane, 0.5 part of carbimide propyl-triethoxysilicane, 0.6 part of β-aminoethyl-γ-aminopropyltrimethoxysilane, 20 parts of methyl-silicone oils join in high speed dispersion stirring tank, mix with base-material, vacuum keep is at-0.1-0.06MPa, rotating speed remains on 250rpm, stir 1h, add 0.7 part of isopropyl titanate, stir, vacuum keep is at-0.1-0.06MPa, rotating speed remains on 250rpm, discharging tinning after stirring 1h.Make single-component porcelain fire-retardant fireproof dealcoholizing-type silicone sealant.Product performance test result is in Table 1.
Embodiment tri-
Mark by weight, 100 parts of the methyl dimethoxy oxygen base end-blocking polydimethylsiloxanes that is 20000cps by viscosity, nano-calcium carbonate 2, silicon powder 3, 1 part of silica powder, potassium oxide 65, 35 parts, barium oxide is put in kneader, keep 150 ℃ of temperature, the vacuum tightness blend 2h that dewaters between 0.06-0.09MPa, crossing runner milling mills 2 times, proceed to and in high speed dispersion stirring tank, be cooled to room temperature and obtain base-material, at room temperature by 4.5 parts of methyltrimethoxy silanes, 1.5 parts of vinyltrimethoxy silanes, 0.8 part of γ-aminopropyl triethoxysilane, 0.8 part of β-aminoethyl-γ-aminopropyltrimethoxysilane, 20 parts of alkoxyl silicone oils, 10 parts of white oils, join in high speed dispersion stirring tank, mix with base-material, vacuum keep is at-0.1-0.06MPa, rotating speed remains on 250rpm, stir 1h, add 0.5 part, two (methyl aceto acetate) two (isopropoxy) titanic acid ester complex compound, 0.2 part of dibutyl tin laurate, stir, vacuum keep is at-0.1-0.06MPa, rotating speed remains on 250rpm, discharging tinning after stirring 1h.Make single-component porcelain fire-retardant fireproof dealcoholizing-type silicone sealant.Product performance test result is in Table 1.
Embodiment tetra-
Mark by weight, 90 parts of the hydroxyl-terminated injecting two methyl siloxanes that is 20000cps by viscosity, 10 parts of methyl dimethoxy oxygen base end-blocking polydimethylsiloxanes, 6 parts of gas-phase silicas, silica powder 5, organobentonite 4, 80 parts of silicon-dioxide, 10 parts of Lithium Oxide 98mins, 10 parts, magnesium oxide is put in kneader, keep 150 ℃ of temperature, the vacuum tightness blend 2h that dewaters between 0.06-0.09MPa, crossing runner milling mills 2 times, proceed to and in high speed dispersion stirring tank, be cooled to room temperature and obtain base-material, at room temperature by 9 parts of phenyltrimethoxysila,e, 0.3 part of carbimide propyl-triethoxysilicane, 0.2 part, calcium chloride, 0.6 part of β-aminoethyl-γ-aminopropyl trimethoxysilane, 15 parts of methyl-silicone oils, 15 parts of alkoxyl silicone oils join in high speed dispersion stirring tank, mix with base-material, vacuum keep is at-0.1-0.06MPa, rotating speed remains on 250rpm, stir 1h, add 0.5 part of isopropyl titanate, 0.2 part of dibutyl tin laurate, stir, vacuum keep is at-0.1-0.06MPa, rotating speed remains on 250rpm, discharging tinning after stirring 1h.Make single-component porcelain fire-retardant fireproof dealcoholizing-type silicone sealant.Product performance test result is in Table 1.
Table 1 test result
Claims (10)
2. according to the porcelain fire-retardant fireproof silicone sealant of claim 1, it is characterized in that: described base polymer is at least one in hydroxyl-terminated injecting two methyl siloxane, trimethoxy end-blocking polydimethylsiloxane, methyl dimethoxy oxygen base end-blocking polydimethylsiloxane.
3. according to the porcelain fire-retardant fireproof silicone sealant of claim 1, it is characterized in that: described softening agent is at least one in the methyl-silicone oil moored in 50-500 of viscosity, white oil, alkoxyl silicone oil.
4. according to the porcelain fire-retardant fireproof seal gum of claim 1, it is characterized in that: described filler is at least one in gas-phase silica, precipitated silica, nano-calcium carbonate, silicon powder, silica powder, organobentonite, the specific surface area of gas-phase silica is 100-300m2/g, and packing material size is 40-80nm.
5. according to the porcelain fire-retardant fireproof silicone sealant of claim 1, it is characterized in that: described Vitrified powder is that aluminium sesquioxide, boron trioxide, silicon-dioxide, Lithium Oxide 98min, sodium oxide, potassium oxide, barium oxide, calcium oxide, magnesium oxide, oxidation are secret, at least one in zirconium white.
6. according to the porcelain fire-retardant fireproof silicone sealant of claim 1, it is characterized in that: described linking agent is at least one in methyltrimethoxy silane, Union carbide A-162, vinyltrimethoxy silane.
7. according to the porcelain fire-retardant fireproof silicone sealant of claim 1, it is characterized in that: described catalyzer is isopropyl titanate, butyl (tetra) titanate, two (methyl aceto acetate) two (isopropoxy) titanic acid ester complex compound, two (methyl ethyl diketone) two (isopropoxy) titanic acid ester complex compounds; At least one in the organo-metallic catalyst such as dibutyl tin laurate, dibutyltin diacetate.
8. according to the porcelain fire-retardant fireproof silicone sealant of claim 1, it is characterized in that: described silane coupling agent is at least one in γ-aminopropyl triethoxysilane, β-aminoethyl-γ-aminopropyltrimethoxysilane, two (γ-trimethoxy silicomethane propyl group) amine, glycidyl ether propyl trimethoxy silicane.
9. according to the porcelain fire-retardant fireproof silicone sealant of claim 1, it is characterized in that: described stablizer is at least one in carbimide propyl-triethoxysilicane, molecular sieve, calcium chloride, magnesium chloride.
10. the preparation method of porcelain fire-retardant fireproof silicone sealant described in claim 1, is characterized in that, comprises the steps:
A, 100 parts of base polymers, filler 5-200 part, Vitrified powder 30-150 part are joined in vacuum kneader, and at 105-150 ℃ to the vacuum tightness 2-3h that dewaters, the base-material of cooling system under 0.06-0.1MPa;
B, above-mentioned base-material, softening agent 3-40 part, linking agent 4-15 part, catalyzer 0.5-3 part, silane coupling agent 0.5-5 part are joined in planetary mixer, keep vacuum tightness-0.1-0.06MPa, stirring velocity is 20-80 rev/min, stir 0.5-3h, make porcelain fire-retardant fireproof silicone sealant.
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