CN108997967A - A kind of high displacement performance fire prevention silicone sealant and preparation method thereof suitable for skyscraper - Google Patents

A kind of high displacement performance fire prevention silicone sealant and preparation method thereof suitable for skyscraper Download PDF

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Publication number
CN108997967A
CN108997967A CN201810902804.9A CN201810902804A CN108997967A CN 108997967 A CN108997967 A CN 108997967A CN 201810902804 A CN201810902804 A CN 201810902804A CN 108997967 A CN108997967 A CN 108997967A
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skyscraper
catalyst
fire prevention
silicone sealant
fire retardant
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谢丽莎
林坤华
黄承相
石正金
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Ji Tai Chemical Inc Guangzhou
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Ji Tai Chemical Inc Guangzhou
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J183/00Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
    • C09J183/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/06Non-macromolecular additives organic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • C08K2003/265Calcium, strontium or barium carbonate
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/014Additives containing two or more different additives of the same subgroup in C08K
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

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  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Sealing Material Composition (AREA)

Abstract

The high displacement performance fire prevention silicone sealant and preparation method thereof that the present invention relates to a kind of suitable for skyscraper, belong to fire prevention silicone sealant field, it is prepared with the substance for including following components: α, alpha, omega-dihydroxy polydimethyl siloxane, dimethyl silicone polymer, the polysiloxanes of alkyl sealing end, inorganic filler, ceramic powder, silane crosslinker, silane coupling agent, the first catalyst, the structure of the polysiloxanes of alkyl sealing end are

Description

A kind of high displacement performance suitable for skyscraper is prevented fires silicone sealant and its preparation Method
Technical field
The high displacement performance fire prevention silicone sealant and preparation method thereof that the present invention relates to a kind of suitable for skyscraper, belongs to In fire prevention silicone sealant field.
Background technique
Common silicone sealant is one of the sealant of common building joint sealing, common silicone sealant it is main Raw material is that linear polysiloxanes, the main chains such as 107 glue are mainly made of Si-O-Si key, in the curing process crosslinking agent and basis The webbed structure of polymer reaction shape, and Si-O-Si key bond energy be higher than ultraviolet light bond energy, therefore silicone sealant relative to For other kinds of sealant, there is excellent caking property, weatherability and uvioresistant.Since 107 glue are at 200-300 DEG C Burn, and the fire of skyscraper easily collapses after having fast sprawling, evacuating personnel difficulty, building burning, difficulty of saving is big The characteristics of, therefore each producer develops fireproof gum to meet building for fireproof requirement.
Fireproof gum refers to the sealant for joint seal for there is fire protection requirement.It is compared with common silicone sealant, It is few when fire prevention silicone sealant is with burning that cigarette is nontoxic, combustion heat value is low, flame propagation velocity is slow, it is complete to be able to maintain in a fire The characteristics of property and thermal insulation.Fireproof gum has not required nothing more than good anti-flammability, caking property, displacement capacity, watertightness and longer Service life also requires glue-line not collapse, free from flaw, is pierced by without flame, and unexposed surface temperature is less than 180 DEG C.Displacement capacity refers to Be insert seam sealant adapt to seam be displaced and keep the deflection effectively sealed.If than certain sealant have ± 25% displacement capacity, when glue-line width is 12mm, then it represents that the glue-line of this sealant can bear original width 25% It stretches and compresses, i.e., it at most can be compressed to 9mm, be stretched to 15mm.Therefore, the displacement capacity of sealant is higher, can bear Deflection it is also bigger, be more suitable for the facilities such as super high-rise building joint filling, large-sized concrete facility, road, bridge, airfield runway The sealing of concrete extension joint.
Fireproof gum must have an anti-flammability first, fireproof gum by be added fire retardant to achieve the effect that fire-retardant, fire retardant Fire retardant mechanism have at 4 points: 1, heat-absorbing action;2, covering acts on;3, inhibit chain effect;4, non-flammable compressive gas smothering action, and it is practical There are several fire retardant mechanisms to work simultaneously in upper many fireproof gums.Outstanding fireproof seal gum does not require nothing more than self-extinguishing without fire, also It is non-fusible, do not drip, be not ashed, not dusting it is required that ceramic forms hard shell after combustion, keep building element complete Property, continue to play gap plugging action, prevents flame and smog from spreading from gap.
Chinese invention patent application prospectus CN106350001A discloses a kind of the organic of ceramic at high temperature Silicone sealant and preparation method thereof, the organosilicon sealant include matrix resin, reinforcing agent, silane coupling agent, catalyst, fill out Fill powder, wherein filling powder by glass powder, fire retardant and helps porcelain agent to form, help porcelain agent be selected from di-iron trioxide, titanium dioxide, One of antimony oxide, silicon carbide, mica powder, magnesium phosphate and diatomite are a variety of.Although the invention has fire-retardant sealing The self-extinguishing fire retardancy of glue, and can not be ashed under high temperature, that is, fire condition, not dusting, ceramic occurs, after continuation of insurance Sealant plugging action is held, building element integrality is effectively kept.But there is also following deficiencies for the silicone sealant: displacement energy The demand of the not high enough fireproof gum for not being able to satisfy skyscraper of power.
Chinese invention patent application prospectus CN103160239A discloses high displacement capacity silicone fireproof seal gum And its manufacturing method, first by α, alpha, omega-dihydroxy polydimethyl siloxane, dimethyl silicone polymer, inorganic filler, nitrogen-phosphorus system resistance Combustion agent is added in kneader, dehydration be blended it is cooling after obtain base-material, at room temperature, by the base-material be added to planetary mixer or In high velocity dispersators, then will be in fumed silica, multiple crosslinking agent, silane coupling agent, catalyst addition blender It reacts that high displacement capacity silicone fireproof seal gum is made with base-material one.Although the invention fire protecting performance is good, have good Caking property and water-fast caking property, displacement capacity up to 25 grades, curtain wall normally stretch and shear-deformable situation under, can play The sealant of effect acts on.But there is also following deficiencies for the silicone sealant: displacement capacity is not high enough be not able to satisfy skyscraper, The even fireproof gum demand of super high-rise building.
In order to cater to the demand in market and the development trend of future architecture, suitable for high-rise, even super high-rise building Fireproof gum is one of the hot spot of research and development.
Summary of the invention
The present invention has made improvements in view of the above-mentioned problems of the prior art, i.e., the technical problem to be solved by the present invention is to mention For a kind of high displacement performance fire prevention silicone sealant and preparation method thereof suitable for skyscraper, the fire prevention silicon that the present invention obtains The displacement capacity of ketone seal gum is stronger, is more suitable for applying in high-rise, super high-rise building sealing.And the present invention obtain it is anti- Ceramics turn to hard shell after fiery silicone sealant burning, and the shell is not molten in fire hazard environment and do not drip, in fire In play firm protective effect, not only keep the integrality of building, building burning will not be made to fall and injure people by a crashing object, also can avoid The diffusion of poison gas dense smoke after burning.
In order to solve the above technical problems, the technical scheme adopted by the invention is that providing a kind of height suitable for skyscraper Displacement performance fire prevention silicone sealant, is prepared: α, alpha, omega-dihydroxy polydimethyl silicon oxygen with the substance for including following components Alkane, dimethyl silicone polymer, alkyl sealing end polysiloxanes, inorganic filler, ceramic powder, silane crosslinker, silane coupling agent, First catalyst.No. CAS of the dimethyl silicone polymer is 9006-65-9, is abbreviated as PDMS, is that a kind of colorless and odorless is nontoxic Clear viscous liquids are widely used in insulation, heat-resisting, damp proof filler, high effective antifoaming agent, release agent, lubricant and surface treatment Agent.The structure of the polysiloxanes of alkyl sealing end isWherein n is selected The integer of 2-4 is selected from from 80-230, x.Wherein Me is methyl.
Preferably, the component for preparing the polysiloxanes of the alkyl sealing end includes end containing hydrogen silicone oil, the second catalysis The structure of agent and alkene, the end containing hydrogen silicone oil isWherein n is selected from 80-230, Me For methyl.The alkene is preferably at least one of ethylene, propylene, butylene.Second catalyst is preferably Karst catalysis Agent, i.e. platinum (0) -1,3- divinyl -1,1,3,3- tetramethyl disiloxanes, No. CAS is 68478-92-2, the end containing hydrogen silicone oil Mass ratio with the alkene is 50-310:1.Under conditions of logical nitrogen, reaction temperature are 70-85 DEG C, toward being mixed with described the It is passed through the alkene in the end containing hydrogen silicone oil of two catalyst, is 100-110 in temperature after reacting 100min-300min DEG C, vacuum degree be evaporated under reduced pressure under conditions of being 0.08-0.1MPa, the polysiloxanes of alkyl sealing end finally can be obtained.
Preferably, the α, alpha, omega-dihydroxy polydimethyl siloxane is 5000-100000mPa in 25 DEG C of viscosity S, the dimethyl silicone polymer are 10000-20000mPas in 25 DEG C of viscosity, the polysiloxanes of the alkyl sealing end It is 100-500mPas in 25 DEG C of viscositys.Although the viscosity of the dimethyl silicone polymer used is larger, due to also It is compounded using the polysiloxanes of the lesser alkyl sealing end of viscosity, in addition also uses inorganic filler, can effectively change It is apt to the viscosity of finally obtained fire prevention silicone sealant, so that obtained fire prevention silicone sealant has good elasticity, displacement Ability is high, be more suitable for applying skyscraper, super high-rise building sealing in.
Preferably, the ceramic powder includes glass powder, fire retardant and helps porcelain agent, the fire retardant is inorganic non-halogen Plain fire retardant, the fire retardant include the first fire retardant and the second fire retardant, and first fire retardant is borate or hydrogen-oxygen Compound, second fire retardant are inorganic phosphorus series compound or inorganic compound nitrogen series.
Preferably, the dosage of first fire retardant and second fire retardant is 1-2:1 in mass ratio.By to nothing The selection of machine non-halogen flame retardant type and ratio guarantees fire-retardant effect by cooperative flame retardant effect.
Preferably, it is described help porcelain agent be selected from di-iron trioxide, titanium dioxide, antimony oxide, silicon carbide, mica powder, One of magnesium sulfate, aluminum sulfate, magnesium phosphate and diatomite are a variety of.If the fire prevention silicone sealant combustion that the present invention obtains It is described to help porcelain agent that the fire prevention silicone sealant is helped not to be ashed, not dusting, form hard shell when burning, guarantee building While complete, the entrance of dense smoke poison gas is avoided, effectively prevents the sprawling of fire.
Preferably, the glass powder, the fire retardant and the dosage helped between porcelain agent are 1:(1- in mass ratio 3):(1-3)。
Preferably, the inorganic filler is selected from least one of calcium carbonate or fumed silica.
Preferably, the calcium carbonate includes the calcium carbonate of high-specific surface area and the calcium carbonate of low specific surface area, it is described High-specific surface area is >=25m2/ g, the low specific surface area are < 25m2/g。
Preferably, the dosage between the calcium carbonate of the high-specific surface area and the calcium carbonate of the low specific surface area is pressed Mass ratio is 1:1-5:1.By the intensity and thixotropy of the calcium carbonate guarantee system of the high-specific surface area, pass through the low ratio The calcium carbonate of surface area improves the viscosity of system, and the two compounding, which can be avoided, occurs that rubber cement viscosity is excessive or dispersion is non-uniform existing As.
Preferably, the silane crosslinker is ketoxime removing type silane crosslinker, the silane crosslinker is three fourth of methyl Ketoximinosilanes, vinyl tributyl ketoximyl silane, propyl tributanoximo silane, phenyl tributanoximo silane, four butanone Oximino silane, methyl tri acetylacetonate oximino silane, vinyl tri acetylacetonate oximino silane, four butanone oximino silane mixtures, four (methyl Isobutyl ketone oximido) silane, vinyl three (methylisobutylketone oximido) silane, one in methyl three (methylisobutylketone oximido) silane Kind is several.
Preferably, the silane coupling agent is vinyltrimethoxysilane, vinyltriethoxysilane, γ-ammonia Propyl-triethoxysilicane, γ-aminopropyltrimethoxysilane, one in γ-glycidyl ether oxygen propyl trimethoxy silicane Kind is several.
Preferably, first catalyst is preferably organic tin catalyst, the organic tin catalyst is February One or more of dilaurylate, dibutyltin diacetate, stannous octoate, tin dilaurate dioctyl tin.
Preferably, in parts by weight, being prepared with the substance for including following components:
Preferably, the α, alpha, omega-dihydroxy polydimethyl siloxane is selected from the production of He Shenggui industry limited liability company Methyl silicone rubber at room temperature cure, the dimethyl silicone polymer are selected from Zhejiang Xinan Chemical Industry Group Co.Ltd's production XHG-201 methyl-silicone oil, the inorganic filler are selected from Kailong Chemical Group Co., Ltd., Hubei Prov or Shanxi orchid Hua Mingna The nanometer calcium carbonate of rice material limited liability company production or the fumed silica of He Shenggui industry limited liability company production, institute The glass powder that glass powder is selected from the production of Nanhai District Foshan City Dong Gu new material Co., Ltd is stated, the fire retardant is selected from Shandong lion AH-108, AH-1011, AH1015, at least one of AH-1020 of Chemical Industry Science Co., Ltd of nation production, it is described that porcelain agent is helped to select R-298, at least one of the R-258 produced from vanadium and titanium resources limited liability company of Pan Gang group, the silane crosslinker are selected from The D-35, D-30, D-32 of Hubei Xiantao Blue Sky Chemical Co., Ltd's production, D-31, D-90, at least one in D-91, D-36 Kind, the silane coupling agent is selected from JH-A110, JH-A111, the JH-A112 of Jingzhou Jianghan Fine Chemical Co., Ltd.'s production, At least one of JH-A113, JH-A114, JH-A1151, first catalyst are produced selected from Beijing Zheng Heng Chemical Co., Ltd. ZT-101, ZT-102, ZT-212, ZT-812, the end containing hydrogen silicone oil be selected from Foshan Hua Gu organosilicon Co., Ltd production Containing hydrogen silicone oil is held, second catalyst is selected from the platinum catalyst of Shanghai Xi Bao new high-tech material Co., Ltd production.
The present invention is also to provide a kind of high displacement performance fire prevention silicone suitable for skyscraper using another technical solution The preparation method of sealant, comprising the following steps:
(1) first by α, alpha, omega-dihydroxy polydimethyl siloxane, dimethyl silicone polymer, alkyl sealing end polysiloxanes, 100- is mixed under the conditions of reaction temperature is 100-130 DEG C, vacuum degree is 0.08-0.1MPa in inorganic filler and ceramic powder 300min obtains rubber cement after cooling;
(2) under the conditions of reaction temperature is 20-40 DEG C, vacuum degree is 0.06-0.08MPa, crosslinkable silane is added in rubber cement Join agent;
(3) it is 20-40 DEG C in reaction temperature, under the conditions of vacuum degree is 0.08-0.1MPa, then silane idol is added in rubber cement Join agent and the first catalyst, discharges after stirring 10-30min.
In short, can be reached following using the high displacement performance fire prevention silicone sealant suitable for skyscraper of the invention The utility model has the advantages that
1, the application of the polysiloxanes blocked by using full-bodied dimethyl silicone polymer and low-viscosity alkyl is come Elongation is improved, to improve the displacement capacity of sealant to meet the seal request of skyscraper, even super high-rise building;
2, by the compounding of the inorganic filler of high low specific surface area, guarantee sealant intensity and it is thixotropic simultaneously, can change The viscosity of kind system, avoids the occurrence of that rubber cement viscosity is excessive or dispersion is uneven;
3, reach fireproof requirement by the introducing of ceramic powder, and association is reached by the compounding of different types of fire retardant Same fire retarding effect, smokeless also unharmful substance generates in combustion process, keeps building integrality simultaneously, avoids poison gas dense smoke The sprawling of diffusion and fire, will not endanger environmental and human health impacts, meet the trend of environmental protection.
Specific embodiment
The following detailed description of embodiments of the present invention, but it is not intended to limit the scope of the invention.
Embodiment 1
The present invention provides a kind of high displacement performance fire prevention silicone sealant suitable for skyscraper, according to parts by weight Meter includes: α, the poly- silicon that 100 parts of alpha, omega-dihydroxy polydimethyl siloxane, 15 parts of dimethyl silicone polymer, alkyl block 10 parts of oxygen alkane, 20 parts of inorganic filler, 51 parts of ceramic powder, 10 parts of silane crosslinker, 2 parts of silane coupling agent, the first catalyst 0.2 Part.
The wherein α, alpha, omega-dihydroxy polydimethyl siloxane are selected from the room temperature sulphur of He Shenggui industry limited liability company production Change methyl silicone rubber, viscosity at a temperature of 25 DEG C is 20000mPas.
The dimethyl silicone polymer is selected from the XHG-201 methyl silicon of Zhejiang Xinan Chemical Industry Group Co.Ltd's production Oil, viscosity at a temperature of 25 DEG C are 20000mPas.
The polysiloxane structure formula of alkyl sealing end isIts Middle n is 75, x 3, and viscosity at a temperature of 25 DEG C is 100mPas.
The component for preparing the polysiloxanes of the alkyl sealing end includes to hold containing hydrogen silicone oil, the second catalyst and alkene, The end containing hydrogen silicone oil is selected from the end containing hydrogen silicone oil of Foshan Hua Gu organosilicon Co., Ltd production, and second catalyst is selected from upper The platinum catalyst of Hai Xibao new high-tech material Co., Ltd production, the alkene are propylene, the end containing hydrogen silicone oil and described third The mass ratio of alkene is 68:1.Under conditions of logical nitrogen, reaction temperature are 70 DEG C, toward the end for being mixed with second catalyst It is passed through the alkene in containing hydrogen silicone oil, after reacting 300min, subtracts under conditions of temperature is 100 DEG C, vacuum degree is 0.1MPa The polysiloxanes of the alkyl sealing end finally can be obtained in pressure distillation.
The inorganic filler is selected from Kailong Chemical Group Co., Ltd., Hubei Prov and orchid Huaming, Shanxi nano material stock The mixture of the fumed silica of the nanometer calcium carbonate and He Shenggui industry limited liability company production of part Co., Ltd production, institute The mass ratio for stating nanometer calcium carbonate and the fumed silica is 1:1, wherein the nanometer calcium carbonate of high-specific surface area and Dosage between the nanometer calcium carbonate of low specific surface area is 1:1 in mass ratio.
The glass powder in the ceramic powder is selected from the glass of Nanhai District Foshan City Dong Gu new material Co., Ltd production Glass powder;First fire retardant is selected from the AH-108 of Shandong Shi Bang Chemical Industry Science Co., Ltd production, the second fire retardant choosing From ammonium polyphosphate, the dosage of first fire retardant and second fire retardant is 1:1 in mass ratio;It is described help porcelain agent be selected from climb The R-298 of vanadium and titanium resources limited liability company of steel group production.
The glass powder, the fire retardant and the dosage helped between porcelain agent are 1:1:1 in mass ratio.
The silane crosslinker is selected from the D-35 of Hubei Xiantao Blue Sky Chemical Co., Ltd's production.
The silane coupling agent is selected from the JH-A110 of Jingzhou Jianghan Fine Chemical Co., Ltd.'s production.
First catalyst is selected from the ZT-101 of Beijing Zheng Heng Chemical Co., Ltd. production.
The preparation method of the high displacement performance fire prevention silicone sealant suitable for skyscraper of embodiment 1, including it is following Step:
(1) first by α, alpha, omega-dihydroxy polydimethyl siloxane, dimethyl silicone polymer, alkyl sealing end polysiloxanes, 300min is mixed under the conditions of reaction temperature is 130 DEG C, vacuum degree is 0.1MPa in inorganic filler and ceramic powder, after cooling Obtain rubber cement;
(2) under the conditions of reaction temperature is 40 DEG C, vacuum degree is 0.08MPa, silane crosslinker is added in rubber cement;
(3) it is 40 DEG C in reaction temperature, under the conditions of vacuum degree is 0.1MPa, then silane coupling agent and the is added in rubber cement One catalyst discharges after stirring 30min.
Embodiment 2
The difference of high displacement performance the fire prevention silicone sealant and embodiment 1 suitable for skyscraper of embodiment 2 It is: α, 85 parts of alpha, omega-dihydroxy polydimethyl siloxane, 20 parts of dimethyl silicone polymer, 50 parts of inorganic filler, ceramic powder 30 Part, 8 parts of silane crosslinker.
The wherein α, viscosity of alpha, omega-dihydroxy polydimethyl siloxane at a temperature of 25 DEG C are 50000mPas.
Viscosity of dimethyl silicone polymer at a temperature of 25 DEG C is 15000mPas.
The polysiloxane structure formula of alkyl sealing end isIts Middle n is 140, x 4, and viscosity at a temperature of 25 DEG C is 250mPas.
The component for preparing the polysiloxanes of the alkyl sealing end includes to hold containing hydrogen silicone oil, the second catalyst and alkene, The end containing hydrogen silicone oil is selected from the end containing hydrogen silicone oil of Foshan Hua Gu organosilicon Co., Ltd production, and second catalyst is selected from upper The platinum catalyst of Hai Xibao new high-tech material Co., Ltd production, the alkene are butylene, the end containing hydrogen silicone oil and the fourth The mass ratio of alkene is 94:1.Under conditions of logical nitrogen, reaction temperature are 85 DEG C, toward the end for being mixed with second catalyst It is passed through the alkene in containing hydrogen silicone oil, after reacting 100min, subtracts under conditions of temperature is 110 DEG C, vacuum degree is 0.08MPa The polysiloxanes of the alkyl sealing end finally can be obtained in pressure distillation.
The inorganic filler is selected from Kailong Chemical Group Co., Ltd., Hubei Prov and orchid Huaming, Shanxi nano material stock The mixture of the nanometer calcium carbonate of part Co., Ltd production, the wherein nanometer calcium carbonate and low specific surface area of high-specific surface area The nanometer calcium carbonate between dosage be in mass ratio 2:1.
First fire retardant described in the ceramic powder is selected from magnesium hydroxide, and second fire retardant is selected from monoammonium phosphate;Institute State the R-258 for helping porcelain agent to be selected from the production of vanadium and titanium resources limited liability company of Pan Gang group.
The silane crosslinker is selected from the D-32 of Hubei Xiantao Blue Sky Chemical Co., Ltd's production.
The silane coupling agent is selected from the JH-A113 of Jingzhou Jianghan Fine Chemical Co., Ltd.'s production.
First catalyst is selected from the ZT-102 of Beijing Zheng Heng Chemical Co., Ltd. production.
The preparation method and embodiment 1 of the high displacement performance fire prevention silicone sealant suitable for skyscraper of embodiment 2 The difference is that:
(1) first by α, alpha, omega-dihydroxy polydimethyl siloxane, dimethyl silicone polymer, alkyl sealing end polysiloxanes, 100min is mixed under the conditions of reaction temperature is 100 DEG C, vacuum degree is 0.08MPa in inorganic filler and ceramic powder, to be cooled After obtain rubber cement;
(2) under the conditions of reaction temperature is 20 DEG C, vacuum degree is 0.06MPa, silane crosslinker is added in rubber cement;
(3) reaction temperature be 20 DEG C, vacuum degree be 0.08MPa under the conditions of, then in rubber cement be added silane coupling agent and First catalyst discharges after stirring 10min.
Embodiment 3
The difference of high displacement performance the fire prevention silicone sealant and embodiment 1 suitable for skyscraper of embodiment 3 It is: α, 70 parts of alpha, omega-dihydroxy polydimethyl siloxane, 18 parts of dimethyl silicone polymer, 60 parts of inorganic filler, ceramic powder 27 Part, 8.5 parts of silane crosslinker, 1 part of silane coupling agent, 0.1 part of the first catalyst.
The wherein α, viscosity of alpha, omega-dihydroxy polydimethyl siloxane at a temperature of 25 DEG C are 10000mPas.
Viscosity of dimethyl silicone polymer at a temperature of 25 DEG C is 10000mPas.
The polysiloxane structure formula of alkyl sealing end isIts Middle n is 230, x 4, and viscosity at a temperature of 25 DEG C is 500mPas.
The component for preparing the polysiloxanes of the alkyl sealing end includes to hold containing hydrogen silicone oil, the second catalyst and alkene, The end containing hydrogen silicone oil is selected from the end containing hydrogen silicone oil of Foshan Hua Gu organosilicon Co., Ltd production, and second catalyst is selected from upper The platinum catalyst of Hai Xibao new high-tech material Co., Ltd production, the alkene are butylene, the end containing hydrogen silicone oil and the fourth The mass ratio of alkene is 155:1.It is past to be mixed with the described of second catalyst under conditions of logical nitrogen, reaction temperature are 78 DEG C It is passed through the alkene in the containing hydrogen silicone oil of end, after reacting 200min, under conditions of temperature is 105 DEG C, vacuum degree is 0.09MPa The polysiloxanes of the alkyl sealing end finally can be obtained in vacuum distillation.
The inorganic filler is selected from Kailong Chemical Group Co., Ltd., Hubei Prov and orchid Huaming, Shanxi nano material stock The mixture of the nanometer calcium carbonate of part Co., Ltd production, the wherein nanometer calcium carbonate and low specific surface area of high-specific surface area The nanometer calcium carbonate between dosage be in mass ratio 1:1.
First fire retardant described in the ceramic powder is selected from zinc borate, and second fire retardant is selected from ammonium chloride.
The silane crosslinker is selected from the D-30 of Hubei Xiantao Blue Sky Chemical Co., Ltd's production.
The silane coupling agent is selected from the JH-A114 of Jingzhou Jianghan Fine Chemical Co., Ltd.'s production.
First catalyst is selected from the ZT-212 of Beijing Zheng Heng Chemical Co., Ltd. production.
The preparation method and embodiment 1 of the high displacement performance fire prevention silicone sealant suitable for skyscraper of embodiment 3 The difference is that:
(1) first by α, alpha, omega-dihydroxy polydimethyl siloxane, dimethyl silicone polymer, alkyl sealing end polysiloxanes, 200min is mixed under the conditions of reaction temperature is 120 DEG C, vacuum degree is 0.09MPa in inorganic filler and ceramic powder, to be cooled After obtain rubber cement;
(2) under the conditions of reaction temperature is 30 DEG C, vacuum degree is 0.07MPa, silane crosslinker is added in rubber cement;
(3) reaction temperature be 30 DEG C, vacuum degree be 0.09MPa under the conditions of, then in rubber cement be added silane coupling agent and First catalyst discharges after stirring 20min.
Embodiment 4
The difference of high displacement performance the fire prevention silicone sealant and embodiment 1 suitable for skyscraper of embodiment 4 Be: 12 parts of polysiloxanes, 30 parts of inorganic filler, 50 parts of ceramic powder, 7.5 parts of silane crosslinker, the silane of alkyl sealing end are even Join 3 parts of agent, 0.25 part of the first catalyst.
The wherein α, viscosity of alpha, omega-dihydroxy polydimethyl siloxane at a temperature of 25 DEG C are 30000mPas.
Viscosity of dimethyl silicone polymer at a temperature of 25 DEG C is 18000mPas.
The polysiloxane structure formula of alkyl sealing end isIts Middle n is 105, x 3, and viscosity at a temperature of 25 DEG C is 180mPas.
The component for preparing the polysiloxanes of the alkyl sealing end includes to hold containing hydrogen silicone oil, the second catalyst and alkene, The end containing hydrogen silicone oil is selected from the end containing hydrogen silicone oil of Foshan Hua Gu organosilicon Co., Ltd production, and second catalyst is selected from upper The platinum catalyst of Hai Xibao new high-tech material Co., Ltd production, the alkene are propylene, the end containing hydrogen silicone oil and described third The mass ratio of alkene is 95:1.Under conditions of logical nitrogen, reaction temperature are 80 DEG C, toward the end for being mixed with second catalyst It is passed through the alkene in containing hydrogen silicone oil, after reacting 200min, subtracts under conditions of temperature is 100 DEG C, vacuum degree is 0.1MPa The polysiloxanes of the alkyl sealing end finally can be obtained in pressure distillation.
The inorganic filler is selected from Kailong Chemical Group Co., Ltd., Hubei Prov and orchid Huaming, Shanxi nano material stock The mixture of the nanometer calcium carbonate of part Co., Ltd production, the wherein nanometer calcium carbonate and low specific surface area of high-specific surface area The nanometer calcium carbonate between dosage be in mass ratio 2:1.
First fire retardant described in the ceramic powder is selected from the AH-108 of Shandong Shi Bang Chemical Industry Science Co., Ltd production, institute It states the second fire retardant and is selected from melamine cyanurate, the dosage of first fire retardant and second fire retardant is in mass ratio For 1.5:1;The R-258 for helping porcelain agent to be selected from the production of vanadium and titanium resources limited liability company of Pan Gang group.
The glass powder, the fire retardant and the dosage helped between porcelain agent are 1:1:1 in mass ratio.
The silane crosslinker is selected from the D-91 of Hubei Xiantao Blue Sky Chemical Co., Ltd's production.
The silane coupling agent is selected from the JH-A1151 of Jingzhou Jianghan Fine Chemical Co., Ltd.'s production.
First catalyst is selected from the ZT-812 of Beijing Zheng Heng Chemical Co., Ltd. production.
Embodiment 5
The difference of high displacement performance the fire prevention silicone sealant and embodiment 1 suitable for skyscraper of embodiment 5 It is: α, 90 parts of alpha, omega-dihydroxy polydimethyl siloxane, 25 parts of dimethyl silicone polymer, 25 parts of inorganic filler, ceramic powder 36 Part, 8 parts of silane crosslinker, 3 parts of silane coupling agent.
The wherein α, alpha, omega-dihydroxy polydimethyl siloxane are selected from the room temperature sulphur of He Shenggui industry limited liability company production Change methyl silicone rubber, viscosity at a temperature of 25 DEG C is 80000mPas.
The polysiloxane structure formula of alkyl sealing end isIts Middle n is 125, x 3, and viscosity at a temperature of 25 DEG C is 200mPas.
The component for preparing the polysiloxanes of the alkyl sealing end includes to hold containing hydrogen silicone oil, the second catalyst and alkene, The end containing hydrogen silicone oil is selected from the end containing hydrogen silicone oil of Foshan Hua Gu organosilicon Co., Ltd production, and second catalyst is selected from upper The platinum catalyst of Hai Xibao new high-tech material Co., Ltd production, the alkene are propylene, the end containing hydrogen silicone oil and described third The mass ratio of alkene is 115:1.It is past to be mixed with the described of second catalyst under conditions of logical nitrogen, reaction temperature are 85 DEG C It is passed through the alkene in the containing hydrogen silicone oil of end, after reacting 250min, under conditions of temperature is 110 DEG C, vacuum degree is 0.09MPa The polysiloxanes of the alkyl sealing end finally can be obtained in vacuum distillation.
The inorganic filler is selected from Kailong Chemical Group Co., Ltd., Hubei Prov and orchid Huaming, Shanxi nano material stock The mixture of the fumed silica of the nanometer calcium carbonate and He Shenggui industry limited liability company production of part Co., Ltd production, institute The mass ratio for stating nanometer calcium carbonate and the fumed silica is 1:5, wherein the nanometer calcium carbonate of high-specific surface area and Dosage between the nanometer calcium carbonate of low specific surface area is 3:1 in mass ratio.
First fire retardant described in the ceramic powder is selected from zinc borate, and second fire retardant is selected from ammonium polyphosphate, described The dosage of first fire retardant and second fire retardant is 1.7:1 in mass ratio.
The glass powder, the fire retardant and the dosage helped between porcelain agent are 1:3:2 in mass ratio.
Preference
Preference exists suitable for the high displacement performance fire prevention silicone sealant of skyscraper and the difference of embodiment 1 In: 20 parts of dimethyl silicone polymer, 25 parts of inorganic filler, 50 parts of ceramic powder, 9 parts of silane crosslinker, 3 parts of silane coupling agent.
The wherein α, viscosity of alpha, omega-dihydroxy polydimethyl siloxane at a temperature of 25 DEG C are 80000mPas.
The polysiloxane structure formula of alkyl sealing end isIts Middle n is 80, x 3.
The component for preparing the polysiloxanes of the alkyl sealing end includes to hold containing hydrogen silicone oil, the second catalyst and alkene, The end containing hydrogen silicone oil is selected from the end containing hydrogen silicone oil of Foshan Hua Gu organosilicon Co., Ltd production, and second catalyst is selected from upper The platinum catalyst of Hai Xibao new high-tech material Co., Ltd production, the alkene are propylene, the end containing hydrogen silicone oil and described third The mass ratio of alkene is 75:1.Under conditions of logical nitrogen, reaction temperature are 75 DEG C, toward the end for being mixed with second catalyst It is passed through the alkene in containing hydrogen silicone oil, after reacting 280min, subtracts under conditions of temperature is 300 DEG C, vacuum degree is 0.1MPa The polysiloxanes of the alkyl sealing end finally can be obtained in pressure distillation.
The inorganic filler is selected from Kailong Chemical Group Co., Ltd., Hubei Prov and orchid Huaming, Shanxi nano material stock The mixture of the nanometer calcium carbonate of part Co., Ltd production, the wherein nanometer calcium carbonate and low specific surface area of high-specific surface area The nanometer calcium carbonate between dosage be in mass ratio 4:1.
First fire retardant described in the ceramic powder is selected from zinc borate, and second fire retardant is selected from melamine cyanurate The dosage of salt, first fire retardant and second fire retardant is 2:1 in mass ratio.
The glass powder, the fire retardant and the dosage helped between porcelain agent are 1:3:3 in mass ratio.
Comparative example is the commercially available fireproof gum for publicizing and being equally used for skyscraper.
The present invention is by the embodiment 1-5 finished product physicochemical property related to comparative example obtained after preference and examines mark It is quasi- as shown in the table:
It follows that the displacement capacity for the fire prevention silicone sealant that the present invention obtains is stronger, it is more suitable for applying high-rise, super In the sealing of skyscraper.And the present invention obtain fire prevention silicone sealant burning after ceramics turn to hard shell, it is described Shell is not molten in fire hazard environment and do not drip, and plays firm protective effect in a fire, not only keeps the complete of building Property, building burning will not be made to fall and injure people by a crashing object, also can avoid the diffusion of the poison gas dense smoke after burning.

Claims (10)

  1. The silicone sealant 1. a kind of high displacement performance suitable for skyscraper is prevented fires, which is characterized in that include following components Substance be prepared: α, alpha, omega-dihydroxy polydimethyl siloxane, dimethyl silicone polymer, alkyl sealing end polysiloxanes, Inorganic filler, ceramic powder, silane crosslinker, silane coupling agent, the first catalyst, the knot of the polysiloxanes of the alkyl sealing end Structure isWherein n is selected from 80-230, and x is selected from the integer of 2-4.
  2. 2. a kind of high displacement performance fire prevention silicone sealant suitable for skyscraper, feature exist according to claim 1 In, the component for preparing the polysiloxanes of alkyl sealing end includes end containing hydrogen silicone oil, the second catalyst and alkene, and described the Two catalyst are Karst catalyst;Under conditions of logical nitrogen, toward the end containing hydrogen silicone oil for being mixed with second catalyst In be passed through the alkene, the polysiloxanes of alkyl sealing end can be obtained in vacuum distillation after complete reaction, and the end contains The mass ratio of hydrogen silicone oil and the alkene is 50-310:1.
  3. 3. a kind of high displacement performance fire prevention silicone sealant suitable for skyscraper, feature exist according to claim 1 In the α, alpha, omega-dihydroxy polydimethyl siloxane is 5000-100000mPas, the poly dimethyl in 25 DEG C of viscosity Siloxanes is 10000-20000mPas in 25 DEG C of viscosity, and the polysiloxanes of the alkyl sealing end is in 25 DEG C of viscosity 100-500mPas, first catalyst are organic tin catalyst, and the organic tin catalyst is two fourth of tin dilaurate One or more of Ji Xi, dibutyltin diacetate, stannous octoate, tin dilaurate dioctyl tin.
  4. 4. a kind of high displacement performance fire prevention silicone sealant suitable for skyscraper, feature exist according to claim 1 In the ceramic powder includes glass powder, fire retardant and helps porcelain agent, and the fire retardant is inorganic non-halogen flame retardant, described Fire retardant includes the first fire retardant and the second fire retardant, and first fire retardant is borate or hydroxide, and described second Fire retardant be inorganic phosphorus series compound or inorganic compound nitrogen series, it is described help porcelain agent be selected from di-iron trioxide, titanium dioxide, three oxygen Change one of two antimony, silicon carbide, mica powder, magnesium sulfate, aluminum sulfate, magnesium phosphate and diatomite or a variety of, the glass powder, institute State fire retardant and the dosage helped between porcelain agent is 1:(1-3 in mass ratio): (1-3).
  5. 5. a kind of high displacement performance fire prevention silicone sealant suitable for skyscraper, feature exist according to claim 4 In the dosage of first fire retardant and second fire retardant is 1-2:1 in mass ratio.
  6. 6. a kind of high displacement performance fire prevention silicone sealant suitable for skyscraper, feature exist according to claim 1 In the inorganic filler is selected from least one of calcium carbonate or fumed silica.
  7. 7. a kind of high displacement performance fire prevention silicone sealant suitable for skyscraper, feature exist according to claim 6 It include the calcium carbonate of high-specific surface area and the calcium carbonate of low specific surface area in, the calcium carbonate, the high-specific surface area is >= 25m2/ g, the low specific surface area are < 25m2/g。
  8. 8. a kind of high displacement performance fire prevention silicone sealant suitable for skyscraper, feature exist according to claim 7 In the dosage between the calcium carbonate of the high-specific surface area and the calcium carbonate of the low specific surface area is 1:1-5:1 in mass ratio.
  9. 9. a kind of high displacement performance fire prevention silicone sealant suitable for skyscraper, feature exist according to claim 1 In in parts by weight, being prepared with the substance for including following components:
  10. 10. a kind of preparation method of the high displacement performance fire prevention silicone sealant suitable for skyscraper, which is characterized in that including Following steps:
    (1) first by α, alpha, omega-dihydroxy polydimethyl siloxane, dimethyl silicone polymer, alkyl sealing end polysiloxanes, inorganic 100- is mixed under the conditions of reaction temperature is 100-130 DEG C, vacuum degree is 0.08-0.1MPa in filler and ceramic powder 300min obtains rubber cement after cooling;
    (2) under the conditions of reaction temperature is 20-40 DEG C, vacuum degree is 0.06-0.08MPa, silane crosslinker is added in rubber cement;
    (3) it is 20-40 DEG C in reaction temperature, under the conditions of vacuum degree is 0.08-0.1MPa, then silane coupling agent is added in rubber cement With the first catalyst, discharge after stirring 10-30min.
CN201810902804.9A 2018-08-09 2018-08-09 A kind of high displacement performance fire prevention silicone sealant and preparation method thereof suitable for skyscraper Pending CN108997967A (en)

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CN110003844A (en) * 2019-04-24 2019-07-12 陈果 A kind of preparation method of ceramic fire prevention silicone sealant
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CN115893928A (en) * 2021-08-18 2023-04-04 茂名市茂南奥邦涂料有限公司 Building grouting material
CN113956834A (en) * 2021-10-25 2022-01-21 广州集泰化工股份有限公司 Silicone sealant and preparation method and application thereof
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