CN102643549B - Dealcoholized flame-retardant silicone sealant and preparation method thereof - Google Patents
Dealcoholized flame-retardant silicone sealant and preparation method thereof Download PDFInfo
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- CN102643549B CN102643549B CN201210037265.XA CN201210037265A CN102643549B CN 102643549 B CN102643549 B CN 102643549B CN 201210037265 A CN201210037265 A CN 201210037265A CN 102643549 B CN102643549 B CN 102643549B
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Abstract
The invention discloses dealcoholized flame-retardant silicone sealant and a preparation method thereof. The dealcoholized flame-retardant silicone sealant prepared by adopting the method has good flame-retardant property and good self-extinguishment property during use, the common problem that the flame retardant property of the dealcoholized flame-retardant silicone sealant cannot satisfy the standard and is poor during use is solved, and the wide application of the dealcoholized flame-retardant silicone sealant is greatly facilitated. At the same time, the sealant has very good storage stability and the storage duration is long and can reach 12 months.
Description
Technical field
The present invention relates to a kind of silicone sealant and preparation method thereof, belong to sealing material technical field.
Background technology
The features such as silicone sealant has excellent anti-weathering age, UV stable, crushing resistance, shock resistance, moisture resistant, high-low temperature resistant, can keep elasticity in harsh climate environment, do not tear and not chap, are therefore widely used in the industries such as building, automobile, electric, mechanical, chemical industry.Along with the usage quantity of the personnel compact district silicone sealants such as Highrise buildings, hospital, station and large-scale public place of entertainment increases, security against fire problem 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.Though common silicone sealant has certain flame retardant resistance, do not there is flame retardancy and self-extinguishing.Particularly dealcoholizing-type silicone sealant, its ubiquity flame retardant properties is not up to standard, the problem that stability in storage is bad, this has just limited the widespread use of dealcoholizing-type silicone sealant greatly.
Summary of the invention
Technical problem
The object of the invention is to overcome defect of the prior art, provide a kind of flame retardant properties good, dealcoholizing-type flame-proof silicone sealant of stable storing and preparation method thereof.
Technical scheme
The present invention is achieved by the following technical programs.
A kind of dealcoholizing-type flame-proof silicone sealant, the recipe ingredient of described seal gum is by mass:
Described base polymer is at least one in the polydimethylsiloxane of trimethoxy end-blocking and the polydimethylsiloxane of methyl dimethoxy oxygen base end-blocking, and their structural formula is respectively
n=50-2000, the viscosity 25 ℃ time is 0.5-200Pas.
Above-mentioned a kind of dealcoholizing-type flame-proof silicone sealant, wherein, described softening agent is at least one in methyl-silicone oil, white oil and the alkoxyl silicone oil of 0.01-0.1Pas of viscosity.
Above-mentioned a kind of dealcoholizing-type flame-proof silicone sealant, wherein, described filler is at least one in nm-class active calcium carbonate, gas-phase silica, precipitated silica, diatomite, silicon powder and organobentonite.Described nm-class active calcium carbonate be by the surface of calcium carbonate through perstearic acid processing, make its particle size range at 40-80nm.
Above-mentioned a kind of dealcoholizing-type flame-proof silicone sealant, wherein, described fire retardant is at least one in aluminium hydroxide, magnesium hydroxide, melamine cyanurate, zinc subcarbonate, zinc borate, carbon black and glass micro mist, particle diameter is controlled at 0.01-10 μ m.
Above-mentioned a kind of dealcoholizing-type flame-proof silicone sealant, wherein, described linking agent is at least one in methyltrimethoxy silane, Union carbide A-162, vinyltrimethoxy silane and phenyltrimethoxysila,e.
Above-mentioned a kind of dealcoholizing-type flame-proof silicone sealant, wherein, described catalyzer is at least one in 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, dibutyl tin laurate and dibutyltin diacetate.
Above-mentioned a kind of dealcoholizing-type flame-proof silicone sealant, wherein, described silane coupling agent is at least one in γ-aminopropyl triethoxysilane, β-aminoethyl-γ-aminopropyltrimethoxysilane, two (γ-trimethoxy silicomethane propyl group) amine and glycidyl ether propyl trimethoxy silicane.
Above-mentioned a kind of dealcoholizing-type flame-proof silicone sealant, wherein, described stablizer is at least one in carbimide propyl-triethoxysilicane, molecular sieve, calcium chloride and magnesium chloride.
The preparation method of above-mentioned a kind of dealcoholizing-type flame-proof silicone sealant, preparation process is as follows: press mass fraction, by 100 parts of base polymers, filler 5-200 part, fire retardant 30-150 part joins in vacuum kneader, maintain the temperature at 105-150 ℃, the vacuum tightness blend 2-3h that dewaters under-0.1～-0.06MPa, grind 2 times through three-roll grinder, proceed to again and in high speed dispersion stirring tank, be cooled to room temperature and obtain base-material, then at room temperature by linking agent 1-15 part, silane coupling agent 0.5-3 part, softening agent 3-40 part, stablizer 0.1-3 part joins in high speed dispersion stirring tank mixes with base-material, be-0.1～-0.06MPa in vacuum tightness, rotating speed is to stir 1h under the condition of 250rpm, and then add catalyzer 0.5-3 part, be-0.1～-0.06MPa in vacuum tightness, rotating speed is under the condition of 250rpm, to stir discharging tinning after 1h, can make dealcoholizing-type flame-proof silicone sealant.
Beneficial effect
It is base polymer that the present invention adopts the polydimethylsiloxane of trimethoxy end-blocking and the polydimethylsiloxane of methyl dimethoxy oxygen base end-blocking, make each component in reaction, organically combine generation dealcoholizing-type flame-proof silicone sealant by adding the auxiliary agents such as fire retardant, softening agent, sealing glue in use has flame retardancy and self-extinguishing, solve the dealcoholizing-type silicone sealant problem that in use ubiquitous flame retardant properties is not up to standard, flame retardant properties is poor, thereby greatly promoted the widespread use of dealcoholizing-type silicone sealant.The formula of dealcoholizing-type flame-proof silicone sealant of the present invention adopts halogen-free environment-friendly type flame-proof agent, has advantages of that low toxicity, low burn into flame retarding efficiency are high, environmentally safe, thereby has improved the safety in utilization of silicone sealant.Dealcoholizing-type flame-proof silicone sealant of the present invention has solved the defect of thickening in seal gum production process, and without viscosity peak, has greatly improved the stability in storage of seal gum, and storage period is 12 months.While preparation process is less demanding to equipment, and the equipment using in production process is existing conventional equipment.
Embodiment
Below in conjunction with specific embodiment, the present invention is further detailed explanation.
Embodiment 1
Press mass fraction, 100 parts of the polydimethylsiloxanes of the trimethoxy end-blocking that is 20Pas by viscosity, 100 parts of nm-class active calcium carbonates, 6 parts of silicon powders, 100 parts, aluminium hydroxide joins in vacuum kneader, keep 150 ℃ of temperature, the vacuum tightness blend 2h that dewaters under-0.06MPa, grind 2 times through three-roll grinder, proceed to again 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, 1 part, calcium chloride, 20 parts of methyl-silicone oils join in high speed dispersion stirring tank and mix with base-material, in vacuum tightness be-0.09MPa, rotating speed is to stir 1h under the condition of 250rpm, and then add 0.7 part, two (methyl aceto acetate) two (isopropoxy) titanic acid ester complex compound, in vacuum tightness be-0.09MPa, rotating speed is under the condition of 250rpm, to stir discharging tinning after 1h, make dealcoholizing-type flame-proof silicone sealant.Product performance test result is in table 1.
Embodiment 2
Press mass fraction, 100 parts of the polydimethylsiloxanes of the methyl dimethoxy oxygen base end-blocking that is 20Pas by viscosity, 60 parts of nm-class active calcium carbonates, 15 parts of gas-phase silicas, 80 parts of magnesium hydroxides, 30 parts of glass micro mists join in vacuum kneader, maintain the temperature at 105 ℃, the vacuum tightness blend 2h that dewaters under-0.09MPa, grind 2 times through three-roll grinder, proceed to again and in high speed dispersion stirring tank, be cooled to room temperature and obtain base-material, then 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 white oils join in high speed dispersion stirring tank and mix with base-material, in vacuum tightness be-0.07MPa, rotating speed is to stir 1h under the condition of 250rpm, and then add 0.7 part of isopropyl titanate, in vacuum tightness be-0.07MPa, rotating speed is under the condition of 250rpm, to stir discharging tinning after 1h, make dealcoholizing-type flame-proof silicone sealant.Product performance test result is in table 1.
Embodiment 3
Press mass fraction, 100 parts of the polydimethylsiloxanes of the trimethoxy end-blocking that is 20Pas by viscosity, 100 parts of nm-class active calcium carbonates, 10 parts of precipitated silicas, 30 parts of zinc subcarbonates join in vacuum kneader, maintain the temperature at 120 ℃, blend 3h dewaters under vacuum tightness-0.08MPa, grind 2 times through three-roll grinder, proceed to again and in high speed dispersion stirring tank, be cooled to room temperature and obtain base-material, then at room temperature by 8 parts of methyltrimethoxy silanes, 1 part of carbimide propyl-triethoxysilicane, 0.6 part of two (γ-trimethoxy silicomethane propyl group) amine, 20 parts of methyl-silicone oils join in high speed dispersion stirring tank and mix with base-material, in vacuum tightness be-0.06MPa, rotating speed is to stir 1h under the condition of 250rpm, and then add 1 part of dibutyl tin laurate, in vacuum tightness be-0.06MPa, rotating speed is under the condition of 250rpm, to stir discharging tinning after 1h, make dealcoholizing-type flame-proof silicone sealant.Product performance test result is in table 1.
Embodiment 4
Press mass fraction, 100 parts of the polydimethylsiloxanes of the methyl dimethoxy oxygen base end-blocking that is 20Pas by viscosity, 100 parts of nm-class active calcium carbonates, 5 parts of gas-phase silicas, 50 parts of magnesium hydroxides, 30 parts of zinc borates join in vacuum kneader, maintain the temperature at 150 ℃, vacuum tightness is the blend 3h that dewaters under-0.1MPa, grind 2 times through three-roll grinder, proceed to again and in high speed dispersion stirring tank, be cooled to room temperature and obtain base-material, then at room temperature by 7 parts of methyltrimethoxy silanes, 0.8 part of vinyltrimethoxy silane, 0.5 part of glycidyl ether propyl trimethoxy silicane, 3 parts of carbimide propyl-triethoxysilicanes, 15 parts of methyl-silicone oils join in high speed dispersion stirring tank and mix with base-material, in vacuum tightness be-0.1MPa, rotating speed is to stir 1h under the condition of 250rpm, and then add 2 parts of dibutyl tin laurates, in vacuum tightness be-0.1MPa, rotating speed is under the condition of 250rpm, to stir discharging tinning after 1h, make dealcoholizing-type flame-proof silicone sealant.Product performance test result is in table 1.
Comparative example
Press mass fraction, 100 parts of the hydroxy-end capped polydimethylsiloxanes that is 20Pas by viscosity, 100 parts of nm-class active calcium carbonates join in vacuum kneader, keep 150 ℃ of temperature, vacuum tightness is the blend 2h that dewaters under-0.09MPa, grind 2 times through three-roll grinder again, proceed to again and in high speed dispersion stirring tank, be cooled to room temperature and obtain base-material, then at room temperature by 8 parts of methyltrimethoxy silanes, 0.8 part of vinyltrimethoxy silane, 0.5 part of glycidyl ether propyl trimethoxy silicane, 15 parts of methyl-silicone oils join in high speed dispersion stirring tank and mix with base-material, in vacuum tightness be-0.09MPa, rotating speed is to stir 1h under the condition of 250rpm, and then add 0.15 part of dibutyl tin laurate, in vacuum tightness be-0.09MPa, rotating speed is under the condition of 250rpm, to stir discharging tinning after 1h.Product performance test result is in table 1.
Table 1 product performance test result
| Test event | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Comparative example |
| Surface drying time (min) | 11 | 10 | 8 | 8 | 8 |
| Hardness (Shore A) | 34 | 39 | 38 | 39 | 33 |
| Tensile strength (MPa) | 2.31 | 2.33 | 2.54 | 2.50 | 2.28 |
| Elongation at break (%) | 540 | 340 | 480 | 469 | 580 |
| Storage period (moon) | 12 | 12 | 12 | 12 | 9 |
| Fire-retardant rank | V0 level | V0 level | V0 level | V0 level | HB |
Claims (2)
1. a dealcoholizing-type flame-proof silicone sealant, is characterized in that, the recipe ingredient of described seal gum is by mass:
Viscosity is 100 parts of the polydimethylsiloxanes of the trimethoxy end-blocking of 20Pas
100 parts of nm-class active calcium carbonates
10 parts of precipitated silicas
30 parts of zinc subcarbonates
8 parts of methyltrimethoxy silanes
1 part of carbimide propyl-triethoxysilicane
0.6 part of two (γ-trimethoxy silicomethane propyl group) amine
20 parts of methyl-silicone oils
1 part of dibutyl tin laurate;
The structural formula of the polydimethylsiloxane of described trimethoxy end-blocking is:
n=50-2000, the viscosity 25 ℃ time is 0.5-200Pas.
2. the preparation method of a kind of dealcoholizing-type flame-proof silicone sealant as claimed in claim 1, it is characterized in that, preparation process is as follows: press mass fraction, 100 parts of the polydimethylsiloxanes of the trimethoxy end-blocking that is 20Pas by viscosity, 100 parts of nm-class active calcium carbonates, 10 parts of precipitated silicas, 30 parts of zinc subcarbonates join in vacuum kneader, maintain the temperature at 120 ℃, blend 3h dewaters under vacuum tightness-0.08MPa, grind 2 times through three-roll grinder, proceed to again and in high speed dispersion stirring tank, be cooled to room temperature and obtain base-material, then at room temperature by 8 parts of methyltrimethoxy silanes, 1 part of carbimide propyl-triethoxysilicane, 0.6 part of two (γ-trimethoxy silicomethane propyl group) amine, 20 parts of methyl-silicone oils join in high speed dispersion stirring tank and mix with base-material, in vacuum tightness be-0.06MPa, rotating speed is to stir 1h under the condition of 250rpm, and then add 1 part of dibutyl tin laurate, in vacuum tightness be-0.06MPa, rotating speed is under the condition of 250rpm, to stir discharging tinning after 1h, make dealcoholizing-type flame-proof silicone sealant.
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| CN103408941A (en) * | 2013-08-23 | 2013-11-27 | 山东永安胶业有限公司 | Transparent dealcoholized single-component room temperature vulcanized silicone rubber and preparation method thereof |
| CN103602073A (en) * | 2013-12-09 | 2014-02-26 | 江苏天辰硅材料有限公司 | High-flame-retardancy fireproof silicone sealant and preparation method thereof |
| CN104388041A (en) * | 2014-12-01 | 2015-03-04 | 公安部四川消防研究所 | High-performance fireproof silicone sealant and preparation method thereof |
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| CN110862801B (en) * | 2019-11-29 | 2021-11-16 | 湖北环宇化工有限公司 | Dealcoholized transparent silicone sealant with long storage life |
| CN110922936A (en) * | 2019-12-13 | 2020-03-27 | 东莞市博君来胶粘材料科技有限公司 | Dealcoholized silicone adhesive and preparation method and application thereof |
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| CN113956834B (en) * | 2021-10-25 | 2023-01-24 | 广州集泰化工股份有限公司 | Silicone sealant and preparation method and application thereof |
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| CN100482761C (en) * | 2007-01-29 | 2009-04-29 | 成都硅宝科技实业有限责任公司 | Single-component room-temperature fast sulfidization dealcoholization type sealing rubber with silicone structure and preparing method thereof |
| CN101565596B (en) * | 2009-05-27 | 2011-07-13 | 深圳市百丽春粘胶实业有限公司 | Neutral silicone weather resistant glue formula and technique for preparing the same |
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