CN101629063A - Expanding type flame-resistant silicone sealant and preparation method thereof - Google Patents
Expanding type flame-resistant silicone sealant and preparation method thereof Download PDFInfo
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- CN101629063A CN101629063A CN200910101904A CN200910101904A CN101629063A CN 101629063 A CN101629063 A CN 101629063A CN 200910101904 A CN200910101904 A CN 200910101904A CN 200910101904 A CN200910101904 A CN 200910101904A CN 101629063 A CN101629063 A CN 101629063A
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Abstract
The invention relates to a flame-resistant sealing material for an opening of a building penetrated object and a preparation method thereof. The provided silicone sealant has better flame-resistant effect, larger expanding rate, lower flame spreading factor, low smoke and no poison. The provided preparation process has simple preparation method and lower consumption in the production process. The expanding type flame-resistant silicone sealant comprises the following raw materials in parts by weight: 100 parts of alpha, omega-dihydroxyl-polyorganosiloxane, 1-50 parts of polydimethylsiloxane, 120-400 parts of flame-resistant filler, 5-20 parts of expanding filler, 2-15 parts of cross-linking agent, 0.2-4 parts of silane coupling agent and 0.1-5 parts of catalyst, wherein the alpha, omega-dihydroxyl-polyorganosiloxane has the structural formula shown as above, n is equal to 50 to 2,000, and R is CH3-, CH3CH2- or phenyl. The preparation method comprises the following steps: (1) preparing a base material; and (2) compounding the sealant.
Description
Technical field
The present invention relates to fire-proof sealing material and manufacture method that a kind of building runs through the thing opening, especially not halogen-containing novel environment friendly expanding type flame-resistant silicone sealant and manufacture craft thereof.
Background technology
In commercial, civilian and industrial and mining enterprises build now, because building interior uses and the needs of building operation, form the empty opening and the building slit of many cable penetrations aperture, electrical equipment reservation on the fire-resisting division member in building or between member and the member, if these not being run through opening and slit carries out fireproof blocking and handles, in case presence of fire, flame and flue gas will run through thing opening and slit by these and spread and come, and single spark just may develop into the disaster that the personnel property of causing takes a bath.
Existing fireproof blocking adopts organic fire prevention calking and inorganic fireproofing plugging mostly, organic fire prevention calking is to be binding agent with the organic synthetic resin, and join fire-proof flame-retarded agent, filler and make, owing to contain toxic volatile matter, in the use that is under an embargo of some occasions to the environmental requirement strictness; Inorganic fireproofing plugging is base-material with the mineral binder bond, and be equipped with inorganic fire proof material, fire retardant etc. and make, though nontoxicity, but become hard block at the shutoff after fixing that finishes, when object maintain and replace through walls such as pipeline and cable, need plug is pounded out, to the very inconvenience of maintenance of pipeline and cable.
Moreover, existing fire-proof sealing material has the micro-expansibility except that the back-fire relief bag, does not have significant expansion character basically, when fire takes place, flame and poison gas just may spread by the hole that stays after the ablations such as plastic conduit, cable insulation skin, cause the heavy losses of personnel and property.
Summary of the invention
Technical problem to be solved by this invention is the deficiency that overcomes the above-mentioned background technology, a kind of not halogen-containing environmental protection expanding type flame-resistant silicone sealant is provided, this silicone sealant has flame retardant effect, bigger rate of expansion, lower flame spread coefficient preferably, and LSZH; The manufacture craft manufacture method that is provided is simple, in the production process loss lower.
Technical scheme provided by the invention is:
Expanding type flame-resistant silicone sealant, included starting material and parts by weight are:
α, 100 parts of alpha, omega-dihydroxy polysiloxane
1～50 part of polydimethylsiloxane
120～400 parts of fire-retardant fillers
5～20 parts of bulking fillers
2～15 parts of linking agents
0.2～4 part of silane coupling agent
0.1～5 part of catalyzer
Wherein:
α, alpha, omega-dihydroxy polysiloxane structure formula is
N=50～2000,
R is CH
3-, CH
3CH
2-or phenyl;
Described bulking filler is at least a in pearlstone, expanded vermiculite, kyanite, the expanded graphite.
Described fire-retardant filler is at least two kinds in surface-treated magnesium hydrate powder, surface-treated aluminium hydroxide powder and the melamine cyanurate.
Described linking agent is at least a in methyltrimethoxy silane, Union carbide A-162, vinyltriethoxysilane, tetraethyl silicate and the silicic acid propyl ester.
Described catalyzer is at least a in butyl (tetra) titanate, titanium propanolate, isopropyl titanate and the iso-butyl titanate.
The manufacture method of expanding type flame-resistant silicone sealant the steps include:
1) system base-material
With α, the alpha, omega-dihydroxy polysiloxane, fire-retardant filler joins in the kneader, and mixing dehydration 30～360 minutes under 110～180 ℃, vacuum tightness 0.06～0.1MPa, after the cooling base-material.
2) seal gum is synthetic
At room temperature, base-material is joined in the stirrer, again bulking filler, polydimethylsiloxane, linking agent, silane coupling agent, catalyzer are joined in the stirrer and stir with base-material, vacuum tightness 0.06～0.1MPa, reacted 0.5～4 hour, and made expanding type flame-resistant silicone sealant.
Described through surface treatment aluminium hydroxide, magnesium hydrate powder, be that the nitrogenous Trimethoxy silane coupling agent of 1～15% weight ratio and 85～99% magnesium hydroxides or aluminium hydroxide powder are added in the reactor, cascade raising temperature, pressurization are gasified totally coupling agent while stirring then, under 150～300 ℃, 0.1～0.5Mpa condition, 4～6 hours treatment times postcooling.
Described nitrogenous Trimethoxy silane coupling agent then is that vinyltriacetoxy silane and aminomethyl isobutyl-Trimethoxy silane are joined in the reactor by 1: 0.5～3 weight ratio, heats, backflow, underpressure distillation and get.
Adopt planetary mixer when described seal gum is synthetic, stirring velocity is 20～80 rev/mins.
The invention has the beneficial effects as follows: the bulking filler that is added in the seal gum, to meet under the fire or the situation of being heated, the seal gum volume can expand rapidly (the product coefficient of thermal expansion is 3～10 times), and the building of shutoff immediately runs through the thing opening, plays the effect of fireproof blocking; And surface-treated aluminium hydroxide or surface-treated magnesium hydrate powder have been added in the seal gum, the addition of powder can significantly increase during synthetic sealant, the flame retardant properties of product is greatly improved, and flame retardant effect all can reach the FV-0 level, and LSZH; The manufacture method of sealing glue is also comparatively simple, and production unit all is some conventional equipments, thereby has improved production efficiency of products greatly, has reduced the loss in the production process, and the no three wastes produce in the production process.
Embodiment
Characteristics of the present invention are to adopt α, and the magnesium hydroxide that alpha, omega-dihydroxy polysiloxane matching surface was handled, aluminium hydroxide powder react with an amount of bulking filler, catalyzer, linking agent, silane coupling agent and make.Wherein adopt surface-treated aluminium hydroxide powder or surface-treated magnesium hydrate powder, the addition of magnesium hydroxide or aluminium hydroxide can significantly increase when making synthetic sealant, has improved the flame retardant resistance of product; Add bulking filler, make seal gum under the situation of being heated, volume energy expands rapidly, and the building of shutoff immediately runs through the thing opening, reaches the purpose of fireproof blocking.
Expanding type flame-resistant silicone sealant, the starting material and the parts by weight that comprise are:
α, 100 parts of alpha, omega-dihydroxy polysiloxane
1～50 part of polydimethylsiloxane
120～400 parts of fire-retardant fillers
5～20 parts of bulking fillers
2～15 parts of linking agents
0.2～4 part of silane coupling agent
0.1～5 part of catalyzer
Wherein:
α, alpha, omega-dihydroxy polysiloxane structure formula is
N=50～2000,
R is CH
3-, CH
3CH
2-or phenyl.
Described bulking filler is at least a in pearlstone, expanded vermiculite, kyanite, the expanded graphite.
Fire-retardant filler is at least two kinds in surface-treated magnesium hydrate powder, surface-treated aluminium hydroxide powder and the melamine cyanurate.
Linking agent is at least a in methyltrimethoxy silane, Union carbide A-162, vinyltriethoxysilane, tetraethyl silicate and the silicic acid propyl ester.
Catalyzer is at least a in butyl (tetra) titanate, titanium propanolate, isopropyl titanate and the iso-butyl titanate.
The manufacture method of expanding type flame-resistant silicone sealant is:
1) system base-material
With α, alpha, omega-dihydroxy polysiloxane (25 ℃ time viscosity be 20Pa.s) 100 weight parts, fire-retardant filler 120～400 weight parts join in the kneader, and mixing dehydration is 30～360 minutes under 110～180 ℃ of temperature, vacuum tightness 0.06～0.1MPa, get base-material after the cooling.
2) synthetic sealant
At room temperature, base-material is joined in the planetary mixer, again 5～20 parts of bulking fillers, 1～50 part of polydimethylsiloxane, 2～15 parts of linking agents, 0.2～4 part of silane coupling agent, catalyzer are joined in the stirrer for 0.1～5 part and stir with base-material, in vacuum tightness 0.06～0.1MPa, carry out chemical reaction 0.5～4 hour under 20～80 rev/mins of the rotating speeds, make expanding type flame-resistant silicone sealant.
Described through surface treatment aluminium hydroxide, magnesium hydrate powder, be that the nitrogenous Trimethoxy silane coupling agent of 1～15% weight ratio and 85～99% magnesium hydroxides or aluminium hydroxide powder are added in the reactor, cascade raising temperature, pressurization are gasified totally coupling agent while stirring then, under 150～300 ℃, 0.1～0.5Mpa condition, 4～6 hours treatment times postcooling.Described nitrogenous Trimethoxy silane coupling agent then is that vinyltriacetoxy silane and aminomethyl isobutyl-Trimethoxy silane are joined in the reactor by 1: 0.5～3 weight ratio, heats, backflow, underpressure distillation and get.Particular content sees for details
Still it should be noted that: above-described α, alpha, omega-dihydroxy polysiloxane, polydimethylsiloxane, aluminium hydroxide, magnesium hydroxide, melamine cyanurate, bulking filler, linking agent, the equal buyable of catalyzer obtain; Described reactor, kneader and other equipment are existing conventional equipment.
Embodiment 1:
Viscosity is the α of 20Pa.s during with 25 ℃, alpha, omega-dihydroxy polysiloxane 100 weight parts (hereinafter to be referred as part), surface-treated magnesium hydrate powder and aluminium hydroxide powder join in the kneader in 150 ℃ of temperature for each 200 parts, mixing dehydration is 360 minutes under the vacuum tightness 0.1MPa, gets base-material after the cooling.At room temperature, base-material is joined in the planetary mixer, again 20 parts of pearlstones, 2 parts of polydimethylsiloxanes, 8 parts of methyltrimethoxy silanes, 4 parts of γ-An Bingjisanyiyangjiguiwans, isopropyl titanate are joined in the planetary mixer for 3 parts and arise from vacuum tightness 0.08MPa, carry out chemical reaction under 80 rev/mins of the rotating speeds and made expansible fireproof shutoff silicone sealant in 4 hours with base-material one.The product performance test result sees for details shown in the table one.
Embodiment 2:
Viscosity is the α of 20Pa.s during with 25 ℃, 100 parts of alpha, omega-dihydroxy polysiloxane, surface-treated magnesium hydrate powder and aluminium hydroxide powder join in the kneader in 110 ℃ of temperature for each 100 parts, and mixing dehydration is 300 minutes under the vacuum tightness 0.08MPa, after the cooling base-material.At room temperature, base-material is joined in the planetary mixer, again 10 parts of expanded vermiculites, 1 part of polydimethylsiloxane, 3 parts of methyltrimethoxy silanes, 2 parts of γ-An Bingjisanyiyangjiguiwans, isopropyl titanate are joined in the planetary mixer for 2 parts and arise from vacuum tightness 0.09MPa, carry out chemical reaction under 60 rev/mins of the rotating speeds and made expansible fireproof shutoff silicone sealant in 4 hours with base-material one.The product performance test result sees for details shown in the table one.
Embodiment 3:
Viscosity is the α of 20Pa.s during with 25 ℃, 100 parts of alpha, omega-dihydroxy polysiloxane, surface-treated magnesium hydroxide and aluminium hydroxide powder join in the kneader in 160 ℃ of temperature for each 70 parts, mixing dehydration is 250 minutes under the vacuum tightness 0.06MPa, after the cooling base-material.At room temperature, base-material is joined in the planetary mixer, again 15 parts of expanded graphites, 2 parts of polydimethylsiloxanes, 5 parts of methyltrimethoxy silanes, 2 parts of γ-An Bingjisanyiyangjiguiwans, isopropyl titanate are joined in the planetary mixer for 4 parts and arise from vacuum tightness 0.06MPa, carry out chemical reaction under 50 rev/mins of the rotating speeds and made expansible fireproof shutoff silicone sealant in 4 hours with base-material one.The product performance test result sees for details shown in the table one.
Embodiment 4:
Viscosity is the α of 20Pa.s during with 25 ℃, 100 parts of alpha, omega-dihydroxy polysiloxane, each 160 parts of surface-treated magnesium hydroxides, aluminium hydroxide powder join in the kneader in 140 ℃ of temperature, and mixing dehydration is 200 minutes under the vacuum tightness 0.08MPa, after the cooling base-material.At room temperature, base-material is joined in the planetary mixer, again 10 parts of expanded graphites, 2 parts of polydimethylsiloxanes, 3 parts of methyltrimethoxy silanes, 2 parts of γ-An Bingjisanyiyangjiguiwans, isopropyl titanate are joined in the planetary mixer for 2 parts and arise from vacuum tightness 0.08MPa, carry out chemical reaction under 40 rev/mins of the rotating speeds and made expansible fireproof shutoff silicone sealant in 4 hours with base-material one.The product performance test result sees for details shown in the table one.
Embodiment 5:
Viscosity is the α of 20Pa.s during with 25 ℃, alpha, omega-dihydroxy polysiloxane 100 weight parts (hereinafter to be referred as part), 100 parts of surface-treated magnesium hydrate powders, melamine cyanurate join in the kneader in 150 ℃ of temperature for 120 parts, mixing dehydration is 360 minutes under the vacuum tightness 0.06MPa, gets base-material after the cooling.At room temperature, base-material is joined in the planetary mixer, again 20 parts of pearlstones, 2 parts of polydimethylsiloxanes, 5 parts of methyltrimethoxy silanes, 2 parts of γ-An Bingjisanyiyangjiguiwans, isopropyl titanate are joined in the planetary mixer for 4 parts and arise from vacuum tightness 0.1MPa, carry out chemical reaction under 80 rev/mins of the rotating speeds and made expansible fireproof shutoff silicone sealant in 4 hours with base-material one.The product performance test result sees for details shown in the table one.
Comparative example 1:
Viscosity is the α of 20Pa.s during with 25 ℃, alpha, omega-dihydroxy polysiloxane 100 weight parts, each 100 parts of surface-treated magnesium hydroxides, aluminium hydroxide powder join in the kneader in 150 ℃ of temperature, and mixing dehydration is 360 minutes under the vacuum tightness 0.1MPa, after the cooling base-material.At room temperature, base-material is joined in the planetary mixer, 2 parts of polydimethylsiloxanes, 8 parts of methyltrimethoxy silanes, 4 parts of γ-An Bingjisanyiyangjiguiwans, isopropyl titanate join in the planetary mixer for 3 parts and arise from vacuum tightness 0.08MPa with base-material one again, carry out chemical reaction under 80 rev/mins of the rotating speeds and make silicone sealant in 4 hours.The product performance test result sees for details shown in the table one.
Table one
Obviously, seal gum provided by the present invention, its flame retardant rating and rate of expansion all have significantly raising.
Claims (8)
1, expanding type flame-resistant silicone sealant, included starting material and parts by weight are:
α, 100 parts of alpha, omega-dihydroxy polysiloxane
1～50 part of polydimethylsiloxane
120～400 parts of fire-retardant fillers
5～20 parts of bulking fillers
2～15 parts of linking agents
0.2～4 part of silane coupling agent
0.1～5 part of catalyzer
Wherein:
α, alpha, omega-dihydroxy polysiloxane structure formula is HO
N=50～2000,
R is CH
3-, CH
3CH
2-or phenyl;
It is characterized in that described bulking filler is at least a in pearlstone, expanded vermiculite, kyanite, the expanded graphite.
2, expanding type flame-resistant silicone sealant according to claim 1 is characterized in that described fire-retardant filler is at least two kinds in surface-treated magnesium hydrate powder, surface-treated aluminium hydroxide powder and the melamine cyanurate.
3, expanding type flame-resistant silicone sealant according to claim 1 and 2 is characterized in that described linking agent is at least a in methyltrimethoxy silane, Union carbide A-162, vinyltriethoxysilane, tetraethyl silicate and the silicic acid propyl ester.
4, expanding type flame-resistant silicone sealant according to claim 3 is characterized in that described catalyzer is at least a in butyl (tetra) titanate, titanium propanolate, isopropyl titanate and the iso-butyl titanate.
5, the manufacture method of expanding type flame-resistant silicone sealant the steps include:
1) system base-material
With α, the alpha, omega-dihydroxy polysiloxane, fire-retardant filler joins in the kneader, and mixing dehydration 30～360 minutes under 110～180 ℃, vacuum tightness 0.06～0.1MPa, after the cooling base-material.
2) seal gum is synthetic
At room temperature, base-material is joined in the stirrer, again bulking filler, polydimethylsiloxane, linking agent, silane coupling agent, catalyzer are joined in the stirrer and stir with base-material, vacuum tightness 0.06～0.1MPa, reacted 0.5～4 hour, and made expanding type flame-resistant silicone sealant.
6, according to the manufacture method of the described expanding type flame-resistant silicone sealant of claim 5, it is characterized in that described through surface treatment aluminium hydroxide, magnesium hydrate powder, be that the nitrogenous Trimethoxy silane coupling agent of 1～15% weight ratio and 85～99% magnesium hydroxides or aluminium hydroxide powder are added in the reactor, cascade raising temperature, pressurization are gasified totally coupling agent while stirring then, under 150～300 ℃, 0.1～0.5Mpa condition, 4～6 hours treatment times postcooling.
7, according to the manufacture method of the described expanding type flame-resistant silicone sealant of claim 6, it is characterized in that nitrogenous Trimethoxy silane coupling agent, then be that vinyltriacetoxy silane and aminomethyl isobutyl-Trimethoxy silane are joined in the reactor by 1: 0.5～3 weight ratio, heat, backflow, underpressure distillation and get.
8, according to the manufacture method of the described expanding type flame-resistant silicone sealant of claim 7, it is characterized in that adopting planetary mixer when described seal gum is synthetic, stirring velocity is 20～80 rev/mins.
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| CN102181295A (en) * | 2011-01-27 | 2011-09-14 | 海龙核材科技（江苏）有限公司 | Environment-friendly fire-retardant module |
| CN102181264A (en) * | 2011-04-15 | 2011-09-14 | 东莞兆舜有机硅新材料科技有限公司 | High-performance organosilicone sealant for photovoltaic (PV) module and preparation method thereof |
| CN102964846A (en) * | 2012-12-19 | 2013-03-13 | 吴孟怀 | Thermal-expansion fireproof puddle |
| CN103146340A (en) * | 2013-03-06 | 2013-06-12 | 广州市高士实业有限公司 | Low-viscosity high-heat-conductivity organic silicon electronic pouring sealant and preparation method thereof |
| CN104099059A (en) * | 2013-04-03 | 2014-10-15 | 上海华硅化工新材料有限公司 | Silicone sealant for automobile side windscreen and preparation method thereof |
| CN105086925A (en) * | 2015-08-25 | 2015-11-25 | 湖北兴瑞化工有限公司 | Novel environment-friendly flame-retardant silicone sealant and preparation method thereof |
| CN105153993A (en) * | 2015-09-21 | 2015-12-16 | 国网山东莒南县供电公司 | Expansive fireproof organic sealant |
| CN106543953A (en) * | 2016-10-28 | 2017-03-29 | 天长市永泰密封材料有限公司 | A kind of fire protection flame retarding polyurethane building sealant and preparation method thereof |
| CN106753206A (en) * | 2017-01-19 | 2017-05-31 | 四川省俊川科技有限公司 | Expansion organic fluid sealant of One-component alcohol fire-retardant fireproof and preparation method thereof |
| CN106916563A (en) * | 2017-04-19 | 2017-07-04 | 常熟市恒信粘胶有限公司 | Flame retardant type silicone structure sealant |
| WO2018076337A1 (en) * | 2016-10-31 | 2018-05-03 | Wacker Chemie Ag | One-part room-temperature curable compositions on basis of organosilicon compounds and titanium curing catalysts |
| CN110172304A (en) * | 2019-04-18 | 2019-08-27 | 浙江上青元电力科技有限公司 | A kind of cable fire insulation adhesive tape |
| CN110564295A (en) * | 2019-09-17 | 2019-12-13 | 中国石油大学(华东) | Silicon-based ultrathin fireproof coating material and preparation method thereof |
| CN110819284A (en) * | 2019-11-16 | 2020-02-21 | 烟台德邦科技有限公司 | Preparation method of silane-terminated sealant with excellent environmental protection and flame retardance |
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| CN102181295A (en) * | 2011-01-27 | 2011-09-14 | 海龙核材科技（江苏）有限公司 | Environment-friendly fire-retardant module |
| CN102181264A (en) * | 2011-04-15 | 2011-09-14 | 东莞兆舜有机硅新材料科技有限公司 | High-performance organosilicone sealant for photovoltaic (PV) module and preparation method thereof |
| CN102964846A (en) * | 2012-12-19 | 2013-03-13 | 吴孟怀 | Thermal-expansion fireproof puddle |
| CN103146340A (en) * | 2013-03-06 | 2013-06-12 | 广州市高士实业有限公司 | Low-viscosity high-heat-conductivity organic silicon electronic pouring sealant and preparation method thereof |
| CN103146340B (en) * | 2013-03-06 | 2014-08-06 | 广州市高士实业有限公司 | Low-viscosity high-heat-conductivity organic silicon electronic pouring sealant and preparation method thereof |
| CN104099059B (en) * | 2013-04-03 | 2016-01-20 | 上海华硅化工新材料有限公司 | A kind of silicone sealant for side windshield of automobile and preparation method thereof |
| CN104099059A (en) * | 2013-04-03 | 2014-10-15 | 上海华硅化工新材料有限公司 | Silicone sealant for automobile side windscreen and preparation method thereof |
| CN105086925A (en) * | 2015-08-25 | 2015-11-25 | 湖北兴瑞化工有限公司 | Novel environment-friendly flame-retardant silicone sealant and preparation method thereof |
| CN105086925B (en) * | 2015-08-25 | 2018-05-29 | 湖北兴瑞化工有限公司 | A kind of environmental protection flame retardant silicone sealant and preparation method thereof |
| CN105153993A (en) * | 2015-09-21 | 2015-12-16 | 国网山东莒南县供电公司 | Expansive fireproof organic sealant |
| CN106543953A (en) * | 2016-10-28 | 2017-03-29 | 天长市永泰密封材料有限公司 | A kind of fire protection flame retarding polyurethane building sealant and preparation method thereof |
| WO2018076337A1 (en) * | 2016-10-31 | 2018-05-03 | Wacker Chemie Ag | One-part room-temperature curable compositions on basis of organosilicon compounds and titanium curing catalysts |
| US11814522B2 (en) | 2016-10-31 | 2023-11-14 | Wacker Chemie Ag | One-part room-temperature curable compositions on the basis of organosilicon compounds and titanium curing catalysts |
| CN106753206A (en) * | 2017-01-19 | 2017-05-31 | 四川省俊川科技有限公司 | Expansion organic fluid sealant of One-component alcohol fire-retardant fireproof and preparation method thereof |
| CN106916563A (en) * | 2017-04-19 | 2017-07-04 | 常熟市恒信粘胶有限公司 | Flame retardant type silicone structure sealant |
| CN110172304A (en) * | 2019-04-18 | 2019-08-27 | 浙江上青元电力科技有限公司 | A kind of cable fire insulation adhesive tape |
| CN110564295A (en) * | 2019-09-17 | 2019-12-13 | 中国石油大学(华东) | Silicon-based ultrathin fireproof coating material and preparation method thereof |
| CN110819284A (en) * | 2019-11-16 | 2020-02-21 | 烟台德邦科技有限公司 | Preparation method of silane-terminated sealant with excellent environmental protection and flame retardance |
| CN110900773A (en) * | 2019-12-17 | 2020-03-24 | 马鞍山市谷庆门业有限公司 | Preparation method of small-gap sound-insulation combined door pocket line |
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