CN117487509A - Ceramic flame-retardant fireproof silicone sealant - Google Patents
Ceramic flame-retardant fireproof silicone sealant Download PDFInfo
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- CN117487509A CN117487509A CN202311679966.8A CN202311679966A CN117487509A CN 117487509 A CN117487509 A CN 117487509A CN 202311679966 A CN202311679966 A CN 202311679966A CN 117487509 A CN117487509 A CN 117487509A
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- silicone sealant
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- 239000004590 silicone sealant Substances 0.000 title claims abstract description 70
- 239000003063 flame retardant Substances 0.000 title claims abstract description 67
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 62
- 239000000919 ceramic Substances 0.000 title claims abstract description 56
- 239000000203 mixture Substances 0.000 claims abstract description 67
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 38
- 239000002131 composite material Substances 0.000 claims abstract description 34
- 229920001709 polysilazane Polymers 0.000 claims abstract description 29
- 239000003054 catalyst Substances 0.000 claims abstract description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 26
- 229910021485 fumed silica Inorganic materials 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 23
- 239000004205 dimethyl polysiloxane Substances 0.000 claims abstract description 15
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims abstract description 15
- -1 polydimethylsiloxane Polymers 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims description 56
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 33
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 30
- NJLLQSBAHIKGKF-UHFFFAOYSA-N dipotassium dioxido(oxo)titanium Chemical compound [K+].[K+].[O-][Ti]([O-])=O NJLLQSBAHIKGKF-UHFFFAOYSA-N 0.000 claims description 30
- 239000000378 calcium silicate Substances 0.000 claims description 28
- 229910052918 calcium silicate Inorganic materials 0.000 claims description 28
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims description 28
- 238000002360 preparation method Methods 0.000 claims description 27
- 239000011812 mixed powder Substances 0.000 claims description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 16
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 15
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 15
- 238000011049 filling Methods 0.000 claims description 15
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 14
- 239000000843 powder Substances 0.000 claims description 14
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 claims description 13
- 229920002545 silicone oil Polymers 0.000 claims description 13
- XBIUWALDKXACEA-UHFFFAOYSA-N 3-[bis(2,4-dioxopentan-3-yl)alumanyl]pentane-2,4-dione Chemical compound CC(=O)C(C(C)=O)[Al](C(C(C)=O)C(C)=O)C(C(C)=O)C(C)=O XBIUWALDKXACEA-UHFFFAOYSA-N 0.000 claims description 12
- FMGBDYLOANULLW-UHFFFAOYSA-N 3-isocyanatopropyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)CCCN=C=O FMGBDYLOANULLW-UHFFFAOYSA-N 0.000 claims description 12
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 11
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 claims description 11
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 11
- 238000007599 discharging Methods 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 11
- 235000002949 phytic acid Nutrition 0.000 claims description 11
- 238000010992 reflux Methods 0.000 claims description 11
- 238000007789 sealing Methods 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 11
- RIUWBIIVUYSTCN-UHFFFAOYSA-N trilithium borate Chemical compound [Li+].[Li+].[Li+].[O-]B([O-])[O-] RIUWBIIVUYSTCN-UHFFFAOYSA-N 0.000 claims description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 8
- 239000004033 plastic Substances 0.000 claims description 8
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 7
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 6
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- 238000001291 vacuum drying Methods 0.000 claims description 5
- ISKQADXMHQSTHK-UHFFFAOYSA-N [4-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=C(CN)C=C1 ISKQADXMHQSTHK-UHFFFAOYSA-N 0.000 claims description 3
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 3
- BWLBGMIXKSTLSX-UHFFFAOYSA-N 2-hydroxyisobutyric acid Chemical compound CC(C)(O)C(O)=O BWLBGMIXKSTLSX-UHFFFAOYSA-N 0.000 claims description 2
- PNOXNTGLSKTMQO-UHFFFAOYSA-L diacetyloxytin Chemical compound CC(=O)O[Sn]OC(C)=O PNOXNTGLSKTMQO-UHFFFAOYSA-L 0.000 claims description 2
- 230000001070 adhesive effect Effects 0.000 abstract description 4
- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical compound O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 4
- 229940083037 simethicone Drugs 0.000 abstract description 4
- 239000000853 adhesive Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 11
- 239000000565 sealant Substances 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 229910052573 porcelain Inorganic materials 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 230000000903 blocking effect Effects 0.000 description 3
- 239000000084 colloidal system Substances 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 230000018109 developmental process Effects 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 229910010293 ceramic material Inorganic materials 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 239000013464 silicone adhesive Substances 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical group [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229920005601 base polymer Polymers 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000012767 functional filler Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 125000005375 organosiloxane group Chemical group 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives 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
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Sealing Material Composition (AREA)
Abstract
The ceramic flame-retardant fireproof silicone sealant belongs to the technical field of adhesives, and comprises the following specific formula in parts by weight: 95-130 parts of alpha, omega-dihydroxy polydimethylsiloxane, 13-28 parts of simethicone, 1-3 parts of fumed silica, 5-15 parts of organic polysilazane, 4-8 parts of composite fluxing agent, 25-50 parts of modified whisker mixture, 0.1-1 part of catalyst and 6-11 parts of cross-linking agent; the ceramic flame-retardant fireproof silicone sealant obtained by the invention has the surface drying time of 5-8 min, the bonding strength of 1.64-1.83 MPa, the tensile strength of 2.81-3.15 MPa, the elastic recovery rate of 89-92%, the Shore hardness of 63-65, the flame-retardant grade V0 and the fire-retardant integrity of 4.5-5.1 h.
Description
Technical Field
The invention relates to a ceramic flame-retardant fireproof silicone sealant, and belongs to the technical field of adhesives.
Background
With the rapid development of the building industry in China, the outer protective structure of the building gradually develops from a glass curtain wall mainly comprising hidden frames or semi-hidden frames into a metal plate curtain wall, a stone curtain wall, a point type glass curtain wall and a mixed curtain wall which is formed by various novel materials and is widely used at present. The silicone sealant used for bonding, sealing, caulking and the like has a main chain structure of a silica chain link and has excellent weather aging resistance. Through long-term practical application, silicone sealant is known by the domestic and foreign construction industry as a reliable high-performance chemical building material for elastic structures, adhesive sealing and caulking. However, conventional silicone sealants do not have flame retardancy and continue to burn when exposed to flame. With the improvement of the requirements of the fire-proof level of the building and the importance of the building industry on the fire-proof performance of the curtain wall, the fire-proof performance of the silicone sealant has become one of the necessary development directions.
The silicone sealant has the advantages that the flame retardant and fireproof performance is high-efficiency, but in practical application, the silicone sealant layer is easy to flow, pulverize or crack at high temperature, the ceramic body formed at high temperature is low in mechanical performance and is damaged in combination integrity, the loss and even failure of the blocking and isolating efficiency of the silicone sealant to high-temperature smoke and fire are directly caused, and the practical application requirements of application scenes cannot be met.
Chinese patent CN103509517A discloses a porcelain flame-retardant fireproof silicone sealant and a preparation method thereof, wherein the sealant is prepared by adding 100 parts of a base polymer, 3-40 parts of a plasticizer, 5-200 parts of a filler, 30-150 parts of porcelain 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 into a high-speed dispersion stirrer, and stirring for 60-180 minutes at a rotation speed of 20-600 rpm under the vacuum degree of 0.06-0.095 MPa. The patent can form compact ceramic material under the condition of continuous high temperature by adding ceramic powder, but the volume of the colloid is contracted in the process of forming ceramic material, so that cracks are generated at the sealing part, the diffusion of smoke and heat is difficult to prevent, and the requirement of fireproof blocking is difficult to meet.
Chinese patent CN110003844a discloses a method for preparing a porcelain silicone sealant, the sealant comprising: 80-100 parts of alpha, omega-dihydroxy polydimethylsiloxane, 1-50 parts of polydimethylsiloxane, 50-100 parts of functional filler, 2-24 parts of silane coupling agent, 2-15 parts of plasticizer, 0.5-3 parts of catalyst and 5-20 parts of water glass; the porcelain silicone sealant obtained by the patent has short fire-retarding time, and the colloid is easy to shrink and pulverize under high-temperature flame.
The above can show that the ceramic flame-retardant fireproof silicone sealant still has the defects of low mechanical property, poor bonding integrity, short fire-retarding time and the like of a ceramic body formed at high temperature, such as easy flowing, pulverization or cracking of a sealant layer at high temperature, so that the development of the ceramic flame-retardant fireproof silicone sealant with good high-temperature dimensional stability, difficult pulverization and cracking, easy formation of a ceramic body with high mechanical strength at high temperature and long fire-retarding time has very important practical significance.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a ceramic flame-retardant fireproof silicone sealant, which realizes the following aims: the ceramic flame-retardant fireproof silicone sealant has good high-temperature dimensional stability, is not easy to pulverize and crack, is easy to form a ceramic body with high mechanical strength at high temperature and has long fire resistance time.
In order to achieve the aim of the invention, the invention adopts the following technical scheme:
the specific formula of the ceramic flame-retardant fireproof silicone sealant comprises the following components in parts by weight:
95-130 parts of alpha, omega-dihydroxy polydimethylsiloxane,
13-28 parts of dimethyl silicone oil,
1-3 parts of fumed silica,
5-15 parts of organic polysilazane,
4-8 parts of composite fluxing agent,
25-50 parts of modified whisker mixture,
0.1-1 part of catalyst,
6-11 parts of a cross-linking agent;
the particle size of the fumed silica is 10-100 nm;
the viscosity of the organic polysilazane is 10-20mPa.s;
the catalyst is one of dibutyl tin dilaurate, dibutyl tin diacetate and tin diacetate Ding Yixian acetonate;
the cross-linking agent is one of methyltrimethoxysilane and methyltriethoxysilane;
the following is a further improvement of the above technical scheme:
step 1, preparation of composite fluxing agent
Mixing lithium borate and ammonium phytate according to a mass ratio of 1-10:20, putting the mixture into a ball mill, ball milling the mixture to a particle size of 0.5-5 mu m, discharging the mixture to obtain powder, then putting the powder into a reaction kettle for drying at 100-130 ℃ for 1-3 hours to obtain dried mixed powder, putting the mixed powder and acetone into the reaction kettle, stirring and dispersing the mixed powder and acetone for 1-2 hours at a rotating speed of 1000-2500 rpm, adding tetraethoxysilane and ammonia water, reducing the stirring speed to 500-900 rpm, heating the mixture to 45-65 ℃ for reacting for 5-9 hours at a condensing reflux state, then cooling the mixture to room temperature, discharging and suction filtering the mixture, and vacuum drying the filtered solid at 50-80 ℃ for 40-70 minutes to obtain a composite fluxing agent;
the mass ratio of the mixed powder to the acetone to the tetraethoxysilane to the ammonia water is 25-40:150-200:5-20:9-25;
the mass concentration of ammonia in the ammonia water is 8-15 wt%.
Step 2, preparation of modified whisker mixture
Drying calcium silicate whisker and potassium titanate whisker at 140-170 ℃ for 1-4 hours, cooling to room temperature, adding calcium silicate whisker, potassium titanate whisker, 3-isocyanatopropyl trimethoxysilane, aluminum acetylacetonate and toluene into a reaction kettle, heating to 75-100 ℃, controlling stirring speed to 500-900 r/min, reacting for 6-9 hours in a condensing reflux state, filtering, and drying the filtered solid at 80-95 ℃ for 2-5 hours to obtain a modified whisker mixture;
the mass ratio of the calcium silicate whisker to the potassium titanate whisker to the 3-isocyanatopropyl trimethoxysilane to the aluminum acetylacetonate to the toluene is 10-20:30-50:5-10:2-6:110-150;
the length of the calcium silicate whisker is 500-1000 nm, and the length-diameter ratio is 3-20:1;
the diameter of the potassium titanate whisker is 200-900 nm, and the length of the potassium titanate whisker is 1-8 mu m.
Step 3, preparation of ceramic flame-retardant fireproof silicone sealant
According to the specific formula of the ceramic flame-retardant fireproof silicone sealant in parts by weight, putting alpha, omega-dihydroxypolydimethylsiloxane, dimethyl silicone oil, organic polysilazane, a catalyst and a cross-linking agent into a double planetary stirrer, stirring and dispersing for 1-2 hours under the conditions of stirring speed of 70-120 r/min and dispersing speed of 3000-5000 r/min, then lifting the stirring speed to 100-150 r/min and dispersing speed to 4500-6000 r/min, then adding fumed silica, continuously stirring and dispersing for 2-4 hours, then adding a composite fluxing agent and a modified whisker mixture, continuously stirring and dispersing for 2-3 hours to obtain a mixed liquid, vacuum defoamating, filling into a plastic finished bottle, and sealing by nitrogen filling to obtain a ceramic flame-retardant fireproof silicone sealant finished product.
Compared with the prior art, the invention has the following beneficial effects:
1. according to the silicone adhesive formula, the fluxing agent which takes lithium borate and ammonium phytate as main components is added, and the two inorganic fluxing agents are subjected to surface coating by using tetraethoxysilane, so that the fluxing agent is uniformly dispersed in a silicone sealant substrate, the melting point is low, when the silicone sealant burns on fire, after the two inorganic matters are melted at high temperature, the melting of the two matters can obviously expand the colloid to maintain the blocking state of flame, and simultaneously, the melted lithium borate and ammonium phytate react with organosiloxane in a porcelain way to form a compact heat-insulating ceramic body with certain strength with calcium silicate whisker and potassium titanate whisker with very good heat insulation performance, so that the flame and the high temperature can be blocked for a long time;
2. according to the invention, 3-isocyanatopropyl trimethoxy silane and aluminum acetylacetonate are used for carrying out surface modification on calcium silicate whisker and potassium titanate whisker, so that the two inorganic whiskers can be uniformly dispersed in an organic silicon resin matrix of silicone sealant, the two whiskers have very excellent heat insulation performance and high temperature resistance, and an effective heat insulation ceramic layer is quickly established by matching with a low-temperature melting catalysis porcelain forming reaction of a fluxing agent, and the flame and high temperature are effectively blocked for a long time;
3. the organic polysilazane with higher reactivity and very low viscosity is added, the organic matters and the main components alpha, omega-dihydroxyl polydimethylsiloxane of the silicone sealant have good compatibility, the low viscosity can maintain good fluidity of the sealant, the higher reactivity can improve the curing rate of the sealant, the surface drying time is shortened, the bonding performance is improved, and in addition, the organic polysilazane is easy to form a ceramic body at high temperature, so that the silicone sealant has positive effects of improving the flame retardance and fire resistance;
4. the ceramic flame-retardant fireproof silicone sealant obtained by the invention has the surface drying time of 5-8 min, the bonding strength of 1.64-1.83 MPa, the tensile strength of 2.81-3.15 MPa, the elastic recovery rate of 89-92%, the Shore hardness of 63-65, the flame-retardant grade V0 and the fire-retardant integrity of 4.5-5.1 h.
Detailed Description
The following description of the preferred embodiments of the present invention is provided for the purpose of illustration and explanation only and is not intended to limit the present invention.
Example 1: ceramic flame-retardant fireproof silicone sealant
Step 1, preparation of composite fluxing agent
Mixing lithium borate and ammonium phytate according to a mass ratio of 8:20, putting the mixture into a ball mill, ball milling the mixture to a particle size of 3 mu m, discharging the mixture to obtain powder, then drying the powder at 120 ℃ for 2.5 hours to obtain dried mixed powder, putting the mixed powder and acetone into a reaction kettle, stirring and dispersing the mixed powder and acetone for 1.3 hours at a rotation speed of 2300 rpm, adding tetraethoxysilane and ammonia water, reducing the stirring rate to 750 rpm, heating the mixture to 60 ℃, reacting the mixture for 6 hours in a condensation reflux state, then cooling the mixture to room temperature, discharging and suction-filtering the mixture, and vacuum-drying the filtered solid at 75 ℃ for 60 minutes to obtain the composite fluxing agent;
the mass ratio of the mixed powder to the acetone to the tetraethoxysilane to the ammonia water is 30:180:15:20;
the mass concentration of ammonia in the ammonia water is 12wt%.
Step 2, preparation of modified whisker mixture
Drying calcium silicate whisker and potassium titanate whisker at 165 ℃ for 2 hours, cooling to room temperature, adding calcium silicate whisker, potassium titanate whisker, 3-isocyanatopropyl trimethoxysilane, aluminum acetylacetonate and toluene into a reaction kettle, heating to 85 ℃, controlling stirring speed to 800 r/min, reacting for 7 hours in a condensing reflux state, filtering, and drying the filtered solid at 90 ℃ for 4 hours to obtain a modified whisker mixture;
the mass ratio of the calcium silicate whisker to the potassium titanate whisker to the 3-isocyanatopropyl trimethoxysilane to the aluminum acetylacetonate to the toluene is 17:38:9:5:135;
the length of the calcium silicate whisker is 750nm, and the length-diameter ratio is 16:1;
the diameter of the potassium titanate whisker is 660nm, and the length is 3 mu m.
Step 3, preparation of ceramic flame-retardant fireproof silicone sealant
The ceramic flame-retardant fireproof silicone sealant comprises the following specific formula in parts by weight:
115 parts of alpha, omega-dihydroxy polydimethylsiloxane,
19 parts of dimethyl silicone oil,
2 parts of fumed silica,
13 parts of organic polysilazane,
7 parts of composite fluxing agent,
33 parts of modified whisker mixture,
0.8 part of catalyst,
9 parts of a cross-linking agent;
the particle size of the fumed silica is 85nm;
the viscosity of the organic polysilazane is 18 mPa.s;
the catalyst is dibutyl tin dilaurate;
the cross-linking agent is methyltrimethoxysilane;
according to the specific formula of the ceramic flame-retardant fireproof silicone sealant in parts by weight, putting alpha, omega-dihydroxypolydimethylsiloxane, dimethyl silicone oil, organic polysilazane, a catalyst and a cross-linking agent into a double planetary stirrer, stirring and dispersing for 1.6 hours under the conditions of stirring speed of 100 rpm and dispersing speed of 4500 rpm, then lifting the stirring speed to 130 rpm and dispersing speed to 5500 rpm, then adding fumed silica, continuously stirring and dispersing for 3.5 hours, then adding a composite fluxing agent and a modified whisker mixture, continuously stirring and dispersing for 2.6 hours to obtain a mixed material liquid, vacuum defoamating, filling into a plastic finished product bottle, and sealing by nitrogen filling to obtain the ceramic flame-retardant fireproof silicone sealant finished product.
Example 2: ceramic flame-retardant fireproof silicone sealant
Step 1, preparation of composite fluxing agent
Mixing lithium borate and ammonium phytate according to a mass ratio of 1:20, putting the mixture into a ball mill, ball milling the mixture to a particle size of 0.5 mu m, discharging the mixture to obtain powder, then drying the powder at 100 ℃ for 1 hour to obtain dried mixed powder, putting the mixed powder and acetone into a reaction kettle, stirring and dispersing the mixed powder and acetone for 1 hour at a rotating speed of 1000 rpm, adding tetraethoxysilane and ammonia water, reducing the stirring speed to 500 rpm, heating the mixture to 45 ℃, reacting the mixture for 5 hours in a condensing reflux state, cooling the mixture to room temperature, discharging and suction filtering the mixture, and vacuum drying the filtered solid at 50 ℃ for 40 minutes to obtain the composite fluxing agent;
the mass ratio of the mixed powder to the acetone to the tetraethoxysilane to the ammonia water is 25:150:5:9;
the mass concentration of ammonia in the ammonia water is 8wt%.
Step 2, preparation of modified whisker mixture
Drying calcium silicate whisker and potassium titanate whisker at 140 ℃ for 1 hour, cooling to room temperature, adding calcium silicate whisker, potassium titanate whisker, 3-isocyanatopropyl trimethoxysilane, aluminum acetylacetonate and toluene into a reaction kettle, heating to 75 ℃, controlling stirring speed to 500 r/min, reacting for 6 hours in a condensing reflux state, filtering, and drying the filtered solid at 80 ℃ for 2 hours to obtain a modified whisker mixture;
the mass ratio of the calcium silicate whisker to the potassium titanate whisker to the 3-isocyanatopropyl trimethoxysilane to the aluminum acetylacetonate to the toluene is 10:30:5:2:110;
the length of the calcium silicate whisker is 500nm, and the length-diameter ratio is 3:1;
the diameter of the potassium titanate whisker is 200nm, and the length is 1 mu m.
Step 3, preparation of ceramic flame-retardant fireproof silicone sealant
The ceramic flame-retardant fireproof silicone sealant comprises the following specific formula in parts by weight:
95 parts of alpha, omega-dihydroxy polydimethylsiloxane,
13 parts of dimethyl silicone oil,
1 part of fumed silica,
5 parts of organic polysilazane,
4 parts of composite fluxing agent,
25 parts of modified whisker mixture,
0.1 part of catalyst,
6 parts of a cross-linking agent;
the particle size of the fumed silica is 10nm;
the viscosity of the organic polysilazane is 10 mPa.s;
the catalyst is dibutyl tin diacetate;
the cross-linking agent is methyltriethoxysilane;
according to the specific formula of the ceramic flame-retardant fireproof silicone sealant in parts by weight, putting alpha, omega-dihydroxypolydimethylsiloxane, simethicone, organic polysilazane, a catalyst and a cross-linking agent into a double planetary stirrer, stirring and dispersing for 1 hour under the conditions of stirring rate of 70 rpm and dispersing rate of 3000 rpm, then lifting the stirring rate to 100 rpm and the dispersing rate to 4500 rpm, then adding fumed silica, continuously stirring and dispersing for 2 hours, then adding a composite fluxing agent and a modified whisker mixture, continuously stirring and dispersing for 2 hours to obtain a mixed material liquid, vacuum defoamating, filling into a plastic finished product bottle, and sealing by nitrogen filling to obtain a ceramic flame-retardant fireproof silicone sealant finished product.
Example 3: ceramic flame-retardant fireproof silicone sealant
Step 1, preparation of composite fluxing agent
Mixing lithium borate and ammonium phytate according to a mass ratio of 10:20, putting the mixture into a ball mill, ball milling the mixture to a particle size of 5 mu m, discharging the mixture to obtain powder, then drying the powder at 130 ℃ for 3 hours to obtain dried mixed powder, putting the mixed powder and acetone into a reaction kettle, stirring and dispersing the mixed powder and acetone for 2 hours at a rotation speed of 2500 rpm, adding tetraethoxysilane and ammonia water, reducing the stirring speed to 900 rpm, heating the mixture to 65 ℃, reacting the mixture for 9 hours in a condensation reflux state, then cooling the mixture to room temperature, discharging and suction-filtering the mixture, and vacuum-drying the filtered solid at 80 ℃ for 70 minutes to obtain the composite fluxing agent;
the mass ratio of the mixed powder to the acetone to the tetraethoxysilane to the ammonia water is 40:200:20:25;
the mass concentration of ammonia in the ammonia water is 15wt%.
Step 2, preparation of modified whisker mixture
Drying calcium silicate whisker and potassium titanate whisker at 170 ℃ for 4 hours, cooling to room temperature, adding calcium silicate whisker, potassium titanate whisker, 3-isocyanatopropyl trimethoxysilane, aluminum acetylacetonate and toluene into a reaction kettle, heating to 100 ℃, controlling stirring rate to 900 rpm, condensing and refluxing for reacting for 9 hours, filtering, and drying the filtered solid at 95 ℃ for 5 hours to obtain a modified whisker mixture;
the mass ratio of the calcium silicate whisker to the potassium titanate whisker to the 3-isocyanatopropyl trimethoxysilane to the aluminum acetylacetonate to the toluene is 20:50:10:6:150;
the length of the calcium silicate whisker is 1000nm, and the length-diameter ratio is 20:1;
the diameter of the potassium titanate whisker is 900nm, and the length is 8 mu m.
Step 3, preparation of ceramic flame-retardant fireproof silicone sealant
The ceramic flame-retardant fireproof silicone sealant comprises the following specific formula in parts by weight:
130 parts of alpha, omega-dihydroxy polydimethylsiloxane,
28 parts of dimethyl silicone oil,
3 parts of fumed silica,
15 parts of organic polysilazane,
8 parts of composite fluxing agent,
50 parts of modified whisker mixture,
1 part of catalyst,
11 parts of a cross-linking agent;
the particle size of the fumed silica is 100nm;
the viscosity of the organic polysilazane is 20 mPa.s;
the catalyst is tin dibutyl acetylacetonate;
the cross-linking agent is methyltrimethoxysilane;
according to the specific formula of the ceramic flame-retardant fireproof silicone sealant in parts by weight, putting alpha, omega-dihydroxypolydimethylsiloxane, simethicone, organic polysilazane, a catalyst and a cross-linking agent into a double planetary stirrer, stirring and dispersing for 2 hours under the conditions of stirring speed of 120 rpm and dispersing speed of 5000 rpm, then lifting the stirring speed to 150 rpm and the dispersing speed to 6000 rpm, then adding fumed silica, continuously stirring and dispersing for 4 hours, then adding a composite fluxing agent and modified whisker mixture, continuously stirring and dispersing for 3 hours to obtain mixed feed liquid, vacuum defoamating, filling into a plastic finished product bottle, and sealing by nitrogen filling to obtain a ceramic flame-retardant fireproof silicone sealant finished product.
Comparative example 1: based on example 1, the preparation of the composite fluxing agent in step 1 was not performed, and in step 3, 7 parts of the composite fluxing agent were replaced with 7 parts of alpha, omega-dihydroxy polydimethylsiloxane in equal amounts, and the specific operations are as follows:
the preparation of the composite fluxing agent in the step 1 is not carried out;
step 2 was performed as in example 1;
step 3, preparation of ceramic flame-retardant fireproof silicone sealant
The ceramic flame-retardant fireproof silicone sealant comprises the following specific formula in parts by weight:
122 parts of alpha, omega-dihydroxy polydimethylsiloxane,
19 parts of dimethyl silicone oil,
2 parts of fumed silica,
13 parts of organic polysilazane,
33 parts of modified whisker mixture,
0.8 part of catalyst,
9 parts of a cross-linking agent;
the particle size of the fumed silica is 85nm;
the viscosity of the organic polysilazane is 18 mPa.s;
the catalyst is dibutyl tin dilaurate;
the cross-linking agent is methyltrimethoxysilane;
according to the specific formula of the ceramic flame-retardant fireproof silicone sealant in parts by weight, putting alpha, omega-dihydroxypolydimethylsiloxane, simethicone, organic polysilazane, a catalyst and a cross-linking agent into a double planetary stirrer, stirring and dispersing for 1.6 hours under the conditions of stirring speed of 100 rpm and dispersing speed of 4500 rpm, then lifting the stirring speed to 130 rpm and dispersing speed to 5500 rpm, then adding fumed silica, continuously stirring and dispersing for 3.5 hours, then adding a modified whisker mixture, continuously stirring and dispersing for 2.6 hours to obtain a mixed material liquid, filling into a plastic finished product bottle after vacuum defoamation, and sealing by nitrogen filling to obtain a ceramic flame-retardant fireproof silicone sealant finished product.
Comparative example 2: based on the embodiment 1, in the preparation of the composite fluxing agent in the step 1, the lithium borate and the ammonium phytate are not subjected to surface coating, and the specific operation is as follows:
step 1, preparation of composite fluxing agent
Mixing lithium borate and ammonium phytate according to a mass ratio of 8:20, putting the mixture into a ball mill, discharging the mixture after ball milling until the particle size is 3 mu m to obtain powder, and then drying the powder at 120 ℃ for 2.5 hours to obtain dried mixed powder, namely the composite fluxing agent;
steps 2 and 3 were carried out in the same manner as in example 1.
Comparative example 3: in the preparation of the whisker mixture in the step 2 and the modification of the whisker mixture based on the example 1, the surface modification of the whisker mixture is carried out without adding 3-isocyanatopropyl trimethoxysilane and aluminum acetylacetonate, and the specific operation is as follows:
step 1 the procedure is as in example 1;
step 2, preparation of whisker mixture
Drying calcium silicate whisker and potassium titanate whisker at 165 ℃ for 2 hours, cooling to room temperature, adding calcium silicate whisker, potassium titanate whisker and toluene into a reaction kettle, heating to 85 ℃, controlling stirring speed to 800 r/min, reacting for 7 hours in a condensation reflux state, filtering, and drying the filtered solid at 90 ℃ for 4 hours to obtain a whisker mixture;
the mass ratio of the calcium silicate whisker to the potassium titanate whisker is 17:38;
the length of the calcium silicate whisker is 750nm, and the length-diameter ratio is 16:1;
the diameter of the potassium titanate whisker is 660nm, and the length is 3 mu m;
step 3, preparation of ceramic flame-retardant fireproof silicone sealant
The ceramic flame-retardant fireproof silicone sealant comprises the following specific formula in parts by weight:
115 parts of alpha, omega-dihydroxy polydimethylsiloxane,
19 parts of dimethyl silicone oil,
2 parts of fumed silica,
13 parts of organic polysilazane,
7 parts of composite fluxing agent,
33 parts of whisker mixture,
0.8 part of catalyst,
9 parts of a cross-linking agent;
the particle size of the fumed silica is 85nm;
the viscosity of the organic polysilazane is 18 mPa.s;
the catalyst is dibutyl tin dilaurate;
the cross-linking agent is methyltrimethoxysilane;
according to the specific formula of the ceramic flame-retardant fireproof silicone sealant in parts by weight, putting alpha, omega-dihydroxypolydimethylsiloxane, dimethyl silicone oil, organic polysilazane, a catalyst and a cross-linking agent into a double planetary stirrer, stirring and dispersing for 1.6 hours under the conditions of stirring speed of 100 rpm and dispersing speed of 4500 rpm, then lifting the stirring speed to 130 rpm and dispersing speed to 5500 rpm, then adding fumed silica, continuously stirring and dispersing for 3.5 hours, then adding a composite fluxing agent and whisker mixture, continuously stirring and dispersing for 2.6 hours to obtain a mixed material liquid, vacuum defoamating, filling into a plastic finished product bottle, and sealing by nitrogen filling to obtain the ceramic flame-retardant fireproof silicone sealant finished product.
Comparative example 4: based on the embodiment 1, in the preparation of the step 3, the ceramic flame-retardant fireproof silicone sealant, no organic polysilazane is added, 13 parts of organic polysilazane is replaced by 13 parts of alpha, omega-dihydroxy polydimethylsiloxane in equal quantity, and the specific operation is as follows:
steps 1 and 2 are the same as in example 1;
step 3, preparation of ceramic flame-retardant fireproof silicone sealant
The ceramic flame-retardant fireproof silicone sealant comprises the following specific formula in parts by weight:
128 parts of alpha, omega-dihydroxy polydimethylsiloxane,
19 parts of dimethyl silicone oil,
2 parts of fumed silica,
7 parts of composite fluxing agent,
33 parts of modified whisker mixture,
0.8 part of catalyst,
9 parts of a cross-linking agent;
the particle size of the fumed silica is 85nm;
the catalyst is dibutyl tin dilaurate;
the cross-linking agent is methyltrimethoxysilane;
according to the specific formula of the ceramic flame-retardant fireproof silicone sealant in parts by weight, the alpha, omega-dihydroxy polydimethylsiloxane, the dimethyl silicone oil, the catalyst and the cross-linking agent are placed into a double planetary mixer, and stirred and dispersed for 1.6 hours under the conditions of stirring speed of 100 rpm and dispersing speed of 4500 rpm, stirring speed is raised to 130 rpm, dispersing speed is raised to 5500 rpm, then fumed silica is added, stirring and dispersing are continued for 3.5 hours, then the mixture of the composite fluxing agent and the modified whisker is added, stirring and dispersing are continued for 2.6 hours to obtain mixed feed liquid, and after vacuum defoamation, the mixed feed liquid is filled into a plastic finished product bottle, and after nitrogen filling and sealing, the ceramic flame-retardant fireproof silicone sealant is obtained.
Performance test:
the ceramic flame-retardant fireproof silicone sealants obtained in examples 1, 2 and 3 and comparative examples 1, 2, 3 and 4 were subjected to the following performance tests:
1. surface drying time: testing is performed with reference to GB/T13477.3-2017;
2. adhesive properties: testing with reference to GB/T11211-2009;
3. tensile strength: testing is performed with reference to GB/T528-2009;
4. elastic recovery rate: testing is performed with reference to GB/T13477.17-2002;
5. shore hardness: testing is performed with reference to GB/T531.1-2008;
6. flame retardant properties and fire integrity: tests were performed with reference to GB/T24267-2009 and GB23864-2009, respectively;
the specific test results are shown in Table 1:
as can be seen from the data in table 1, comparative example 1 without the composite fluxing agent has little difference in tack-free time and mechanical properties from the three examples, and the flame retardant rating and the fire resistance integrity are significantly worse than the three examples, indicating that the addition of the composite fluxing agent has little effect on the curing rate and mechanical properties of the silicone sealant, but has a great effect on the flame retardant properties and fire resistance integrity; in the preparation of the composite fluxing agent in comparative example 2, the surface coating is not carried out on lithium borate and ammonium phytate, the surface drying time is slower than that of the three embodiments, the mechanical properties are also obviously lower than that of the three embodiments, and the flame retardant grade and the fire resistance integrity are greatly reduced, which means that the lithium borate and the ammonium phytate are not subjected to surface coating and are difficult to be well dispersed in a sealant matrix, and thus the performances of the silicone sealant are affected; in comparative example 3, the calcium silicate whiskers and the potassium titanate whiskers were not surface-modified, the curing rate and mechanical properties of the silicone sealant were comprehensively reduced, the flame retardant rating was reduced, and the fire resistance integrity became worst in all examples and comparative examples, which suggests that the calcium silicate whiskers and the potassium titanate whiskers were not surface-modified, and were difficult to uniformly disperse in the sealant matrix, resulting in comprehensive reduction of various properties; in comparative example 4, no organic polysilazane was added, the surface dry time was longest, the bonding strength was worst, and the tensile strength, elastic recovery rate and shore hardness were also minimized, thus it was found that the organic polysilazane plays a key role in improving the curing rate, bonding property and mechanical property of silicone adhesive, and the flame retardant rating and fire resistance integrity of comparative example 4 were also significantly lower than those of the three examples, which indicates that the organic polysilazane also plays an important role in improving the flame retardant and fire resistance properties of silicone sealant.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (4)
1. The ceramic flame-retardant fireproof silicone sealant is characterized in that:
the ceramic flame-retardant fireproof silicone sealant comprises the following specific formula in parts by weight:
95-130 parts of alpha, omega-dihydroxy polydimethylsiloxane,
13-28 parts of dimethyl silicone oil,
1-3 parts of fumed silica,
5-15 parts of organic polysilazane,
4-8 parts of composite fluxing agent,
25-50 parts of modified whisker mixture,
0.1-1 part of catalyst,
6-11 parts of a cross-linking agent;
the particle size of the fumed silica is 10-100 nm;
the viscosity of the organic polysilazane is 10-20mPa.s;
the catalyst is one of dibutyl tin dilaurate, dibutyl tin diacetate and tin diacetate Ding Yixian acetonate;
the cross-linking agent is one of methyltrimethoxysilane and methyltriethoxysilane;
the preparation method of the composite fluxing agent comprises the following steps: mixing lithium borate and ammonium phytate according to a mass ratio of 1-10:20, putting the mixture into a ball mill, ball milling the mixture to a particle size of 0.5-5 mu m, discharging the mixture to obtain powder, then putting the powder into a reaction kettle for drying at 100-130 ℃ for 1-3 hours to obtain dried mixed powder, putting the mixed powder and acetone into the reaction kettle, stirring and dispersing the mixed powder and acetone for 1-2 hours at a rotating speed of 1000-2500 rpm, adding tetraethoxysilane and ammonia water, reducing the stirring speed to 500-900 rpm, heating the mixture to 45-65 ℃ for reacting for 5-9 hours at a condensing reflux state, then cooling the mixture to room temperature, discharging and suction filtering the mixture, and vacuum drying the filtered solid at 50-80 ℃ for 40-70 minutes to obtain a composite fluxing agent;
the preparation method of the modified whisker mixture comprises the following steps: drying calcium silicate whisker and potassium titanate whisker at 140-170 ℃ for 1-4 hours, cooling to room temperature, adding calcium silicate whisker, potassium titanate whisker, 3-isocyanatopropyl trimethoxysilane, aluminum acetylacetonate and toluene into a reaction kettle, heating to 75-100 ℃, controlling stirring speed to 500-900 r/min, reacting for 6-9 hours in a condensing reflux state, filtering, and drying the filtered solid at 80-95 ℃ for 2-5 hours to obtain a modified whisker mixture.
2. The ceramicized flame retardant fire retardant silicone sealant according to claim 1, wherein:
the mass ratio of the mixed powder to the acetone to the tetraethoxysilane to the ammonia water is 25-40:150-200:5-20:9-25;
the mass concentration of ammonia in the ammonia water is 8-15 wt%.
3. The ceramicized flame retardant fire retardant silicone sealant according to claim 1, wherein:
the mass ratio of the calcium silicate whisker to the potassium titanate whisker to the 3-isocyanatopropyl trimethoxysilane to the aluminum acetylacetonate to the toluene is 10-20:30-50:5-10:2-6:110-150;
the length of the calcium silicate whisker is 500-1000 nm, and the length-diameter ratio is 3-20:1;
the diameter of the potassium titanate whisker is 200-900 nm, and the length of the potassium titanate whisker is 1-8 mu m.
4. The ceramicized flame retardant fire retardant silicone sealant according to claim 1, wherein:
the preparation method of the ceramic flame-retardant fireproof silicone sealant comprises the following steps: according to the specific formula of the ceramic flame-retardant fireproof silicone sealant in parts by weight, putting alpha, omega-dihydroxypolydimethylsiloxane, dimethyl silicone oil, organic polysilazane, a catalyst and a cross-linking agent into a double planetary stirrer, stirring and dispersing for 1-2 hours under the conditions of stirring speed of 70-120 r/min and dispersing speed of 3000-5000 r/min, then lifting the stirring speed to 100-150 r/min and dispersing speed to 4500-6000 r/min, then adding fumed silica, continuously stirring and dispersing for 2-4 hours, then adding a composite fluxing agent and a modified whisker mixture, continuously stirring and dispersing for 2-3 hours to obtain a mixed liquid, vacuum defoamating, filling into a plastic finished bottle, and sealing by nitrogen filling to obtain a ceramic flame-retardant fireproof silicone sealant finished product.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117965130A (en) * | 2024-03-28 | 2024-05-03 | 临朐县金迪胶业有限公司 | Silicone fireproof sealant for building |
| CN118006291A (en) * | 2024-04-10 | 2024-05-10 | 临朐县金迪胶业有限公司 | Moisture-heat resistant silicone structural adhesive suitable for photovoltaic module |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117965130A (en) * | 2024-03-28 | 2024-05-03 | 临朐县金迪胶业有限公司 | Silicone fireproof sealant for building |
| CN117965130B (en) * | 2024-03-28 | 2024-05-31 | 临朐县金迪胶业有限公司 | Silicone fireproof sealant for building |
| CN118006291A (en) * | 2024-04-10 | 2024-05-10 | 临朐县金迪胶业有限公司 | Moisture-heat resistant silicone structural adhesive suitable for photovoltaic module |
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