CN117186645A - Halogen-free flame-retardant anti-dripping fireproof blocking silica gel mud and preparation method thereof - Google Patents
Halogen-free flame-retardant anti-dripping fireproof blocking silica gel mud and preparation method thereof Download PDFInfo
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- CN117186645A CN117186645A CN202311158528.7A CN202311158528A CN117186645A CN 117186645 A CN117186645 A CN 117186645A CN 202311158528 A CN202311158528 A CN 202311158528A CN 117186645 A CN117186645 A CN 117186645A
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- silica gel
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- free flame
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 239000000741 silica gel Substances 0.000 title claims abstract description 58
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 58
- 239000003063 flame retardant Substances 0.000 title claims abstract description 51
- 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 50
- 230000000903 blocking effect Effects 0.000 title claims description 20
- 238000002360 preparation method Methods 0.000 title abstract description 7
- -1 polysiloxane Polymers 0.000 claims abstract description 27
- 239000000945 filler Substances 0.000 claims abstract description 26
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 24
- 239000003999 initiator Substances 0.000 claims abstract description 17
- 239000011159 matrix material Substances 0.000 claims abstract description 17
- 239000003607 modifier Substances 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 150000002978 peroxides Chemical class 0.000 claims abstract description 6
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 20
- 238000004898 kneading Methods 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 16
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 13
- 239000005995 Aluminium silicate Substances 0.000 claims description 11
- 235000012211 aluminium silicate Nutrition 0.000 claims description 11
- 239000011521 glass Substances 0.000 claims description 11
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims description 11
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 11
- 239000000347 magnesium hydroxide Substances 0.000 claims description 11
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims description 11
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 10
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 10
- 239000006229 carbon black Substances 0.000 claims description 10
- 239000004114 Ammonium polyphosphate Substances 0.000 claims description 9
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims description 9
- 229920001276 ammonium polyphosphate Polymers 0.000 claims description 9
- 239000011324 bead Substances 0.000 claims description 9
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 9
- 229920002545 silicone oil Polymers 0.000 claims description 8
- 229920002554 vinyl polymer Polymers 0.000 claims description 8
- 230000009970 fire resistant effect Effects 0.000 claims description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 7
- YEECOJZAMZEUBB-UHFFFAOYSA-N 2,2,3,3,6,6,7,7-octamethyloctane Chemical compound CC(C)(C)C(C)(C)CCC(C)(C)C(C)(C)C YEECOJZAMZEUBB-UHFFFAOYSA-N 0.000 claims description 6
- 239000007822 coupling agent Substances 0.000 claims description 6
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical group CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 6
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 5
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 5
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- WRXCBRHBHGNNQA-UHFFFAOYSA-N (2,4-dichlorobenzoyl) 2,4-dichlorobenzenecarboperoxoate Chemical compound ClC1=CC(Cl)=CC=C1C(=O)OOC(=O)C1=CC=C(Cl)C=C1Cl WRXCBRHBHGNNQA-UHFFFAOYSA-N 0.000 claims description 4
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- 229920001971 elastomer Polymers 0.000 claims description 3
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical group C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 2
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 2
- 229920000877 Melamine resin Polymers 0.000 claims description 2
- 125000000217 alkyl group Chemical group 0.000 claims description 2
- 150000004645 aluminates Chemical class 0.000 claims description 2
- LSXWFXONGKSEMY-UHFFFAOYSA-N di-tert-butyl peroxide Chemical group CC(C)(C)OOC(C)(C)C LSXWFXONGKSEMY-UHFFFAOYSA-N 0.000 claims description 2
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 2
- 239000010445 mica Substances 0.000 claims description 2
- 229910052618 mica group Inorganic materials 0.000 claims description 2
- 239000004005 microsphere Substances 0.000 claims description 2
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 2
- 125000000725 trifluoropropyl group Chemical group [H]C([H])(*)C([H])([H])C(F)(F)F 0.000 claims description 2
- 239000010455 vermiculite Substances 0.000 claims description 2
- 229910052902 vermiculite Inorganic materials 0.000 claims description 2
- 235000019354 vermiculite Nutrition 0.000 claims description 2
- UPIWXMRIPODGLE-UHFFFAOYSA-N butyl benzenecarboperoxoate Chemical group CCCCOOC(=O)C1=CC=CC=C1 UPIWXMRIPODGLE-UHFFFAOYSA-N 0.000 claims 1
- 239000012969 di-tertiary-butyl peroxide Chemical group 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 21
- 229920002379 silicone rubber Polymers 0.000 abstract description 11
- 238000006243 chemical reaction Methods 0.000 abstract description 6
- 239000004945 silicone rubber Substances 0.000 abstract description 6
- 230000009471 action Effects 0.000 abstract description 4
- 238000004132 cross linking Methods 0.000 abstract description 4
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 abstract description 4
- 239000003292 glue Substances 0.000 description 17
- 239000000853 adhesive Substances 0.000 description 8
- 230000001070 adhesive effect Effects 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000919 ceramic Substances 0.000 description 7
- 238000001816 cooling Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000003921 oil Substances 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- APSBXTVYXVQYAB-UHFFFAOYSA-M sodium docusate Chemical group [Na+].CCCCC(CC)COC(=O)CC(S([O-])(=O)=O)C(=O)OCC(CC)CCCC APSBXTVYXVQYAB-UHFFFAOYSA-M 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000005496 eutectics Effects 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- 239000000499 gel Substances 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000008093 supporting effect Effects 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910004298 SiO 2 Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N phenylbenzene Natural products C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 description 1
- 238000010257 thawing Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Fireproofing Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The application belongs to the field of fireproof plugging materials, and discloses halogen-free flame-retardant anti-dripping fireproof plugging silica gel mud and a preparation method thereof, wherein the halogen-free flame-retardant anti-dripping fireproof plugging silica gel mud comprises the following raw materials in parts by weight: 100 parts of polysiloxane matrix; 100-600 parts of refractory filler; 50-300 parts of a flame retardant; 0.01-20 parts of an initiator; 0.5-10 parts of modifier. The silica gel mud prepared by the application has the properties of halogen-free flame retardance, fire resistance, moisture resistance, no dry crack, no oil flowing, softness in four seasons and no molten drop at high temperature; the peroxide initiator is added into the silica gel mud, so that the silica gel mud is stable at room temperature or low temperature for a long time, when a fire disaster occurs, the initiator is decomposed to generate free radicals under the action of high temperature to trigger polysiloxane crosslinking reaction to form a crosslinked network, the fire-receiving side of the silica gel mud is changed into a hard silicone rubber state, the occurrence of a molten drop phenomenon is avoided, and the safety of a plugging structure can be effectively protected.
Description
Technical Field
The application belongs to the field of fireproof blocking materials, and particularly relates to halogen-free flame-retardant anti-dripping fireproof blocking silica gel and a preparation method thereof.
Background
According to GB 50016-2014 building design fireproof Specification, GB 50745-2012 conventional island design fireproof Specification for nuclear power plants and GB/T51410-2020 building fireproof blocking application technical Standard, in order to avoid building fire and reduce fire hazard, fireproof separation should be carried out between different using sites of a building, and fireproof blocking should be carried out on openings formed when penetrations (such as cables, air pipes and air pipes) of walls and floors of the fireproof partitions of the building pass through, so that smoke and toxic gases in case of fire or gas leakage are prevented from spreading through holes, and the production and living safety of people are seriously affected.
Among the fire-proof plugging materials, the flexible organic plugging material has excellent fire-proof performance, and has specific flexibility and plasticity, so that the flexible organic plugging material can be conveniently applied to plugging various holes and is widely applied.
The silica gel is a flexible organic fireproof blocking material with excellent sealing, fireproof, moistureproof and other performances, and is widely applied to various openings formed when cables, oil pipes, natural gas pipes and the like pass through walls (bin) walls and building (A) plates and segmented fireproof separation of cable bridges. The prior art patent CN 112961500A discloses a non-solidified sealing fireproof moistureproof silica gel and a preparation method thereof, wherein liquid organic silicon resin is used as a matrix, and auxiliaries such as a silane coupling agent and the like are used as a modifier to modify a filler, so that the compatibility of powder and the organic silicon resin is improved, and the environment-friendly silica gel is obtained. Although the problem of compatibility between a silicone resin matrix and a filler is solved, the structural phenomenon of silica gel mud is relieved, the problem that the plasticity and the supporting property of a fireproof blocking part are difficult to be compatible still exists in the existing flexible organic blocking material, particularly when a fire disaster occurs, the phenomena of pulverization, molten drops and the like of the flexible organic blocking material can occur under the action of high temperature, the damage of a fireproof structure is caused, and the safety of the fireproof blocking structure is seriously influenced.
Disclosure of Invention
In order to solve the problems, the application provides halogen-free flame-retardant anti-dripping fireproof plugging silica gel which has excellent performances of halogen-free flame retardance, fire prevention, moisture resistance, no dry crack, no oil flowing, softness in four seasons and no pulverization and dripping phenomena during fire disaster.
The application further aims at providing a preparation method of the halogen-free flame-retardant anti-dripping fireproof plugging silica gel.
In order to achieve the above purpose, the application adopts the following technical scheme:
a halogen-free flame-retardant anti-dripping fireproof blocking silica gel mud comprises a polysiloxane matrix, fireproof filler, a flame retardant, an initiator and a modifier.
Preferably, the halogen-free flame-retardant anti-dripping fireproof plugging silica gel mud comprises the following raw materials in parts by weight: 100 parts of polysiloxane matrix, 100-600 parts of refractory filler, 50-300 parts of flame retardant, 0.01-20 parts of initiator and 0.5-10 parts of modifier.
Preferably, the polysiloxane matrix relates to a polysiloxane of the structure shown in the following formula (I):
（I）
wherein:
R 1 and R is 2 Is a saturated or unsaturated group selected from methyl, ethyl, propyl, phenyl, trifluoropropyl, vinyl, long chain alkyl, R 1 And R is 2 May be the same or different; r is R 3 Represents vinyl; r is R 4 And R is 5 Is a saturated or unsaturated group selected from methyl, ethyl, hydroxy, hydroxypropyl, vinyl, R 4 And R is 5 May be the same or different; m, n and z are integers, m is more than or equal to 0, n is more than or equal to 0, z is more than or equal to 0, and (m+n+z) is more than or equal to 400 and less than or equal to 5000; the polysiloxane matrix is composed of one or a mixture of more than one polysiloxane of the structural general formula (I), at least one polysiloxane contains vinyl in the molecules of the polysiloxane matrix, and the viscosity of the polysiloxane matrix is 30000 mPa.s-1500000 mPa.s at 25 ℃; further preferably, the polysiloxane matrix is 107 glue.
Preferably, the refractory filler comprises one or more of kaolin, diatomite, hollow glass microspheres, calcium carbonate, mica powder, expanded vermiculite and white carbon black; further preferably, the refractory filler is a mixture formed by kaolin, hollow glass beads, calcium carbonate and white carbon black, and the mass ratio of the four substances is 10:10:5:1.
Preferably, the flame retardant comprises one or more of aluminum hydroxide, magnesium hydroxide, melamine, ammonium polyphosphate and hexaphenoxy cyclotriphosphazene; further preferably, the flame retardant is a blend of aluminum hydroxide, magnesium hydroxide and ammonium polyphosphate, and the mass ratio of the three substances is 2:1:2.
Preferably, the initiator is a peroxide initiator, which can generate free radicals at high temperature and initiate a silicone rubber crosslinking reaction, and comprises one or a mixture of a plurality of bis-2, 4 (2, 4-dichloro-benzoyl), bis-2, 5 (2, 5-bis (tert-butyl) -2, 5-dimethylhexane), benzoyl peroxide, dibenzoyl peroxide, tert-butyl peroxybenzoate, di-tert-butyl peroxide and dicumyl peroxide; preferably, the peroxide initiator is bis-2, 5 (2, 5-bis (t-butyl) -2, 5-dimethylhexane).
The modifier is hydroxyl silicone oil, a silane coupling agent, a titanate coupling agent or an aluminate coupling agent and the like, and can be used for carrying out surface modification on the powder, improving the compatibility between the powder and a matrix and preventing the generation of a structuring phenomenon; the silane coupling agent is vinyl triethoxysilane, and the titanate coupling agent is isopropyl tri (dioctyl pyrophosphoryloxy) titanate; further preferred is a mixture of hydroxy silicone oil, vinyl triethoxysilane and isopropyl tri (dioctyl pyrophosphoryl oxy) titanate, the mass ratio of the three substances being 4:2:3.
The preparation method of the halogen-free flame-retardant anti-dripping fireproof plugging silica gel mud comprises the following steps:
(1) The polysiloxane matrix, the fire-resistant filler, the fire retardant and the modifier are put into a kneader according to the proportion, heated to 100 ℃ to 150 ℃ and kneaded for 2h to 4h, then decompressed and kneaded for 1h to 2h under the pressure of minus 0.09MPa, and cooled to the room temperature to obtain the base rubber;
(2) And adding an initiator into a kneader according to a formula amount, kneading for 0.5-1 h, and extruding through a screw to obtain the halogen-free flame-retardant anti-dripping fireproof plugging silica gel.
The application has the following beneficial effects:
1. the application uses the peroxide initiator for preparing halogen-free flame-retardant anti-dripping fireproof plugging silica gel mud for the first time, can stably keep soft gel mud shape for a long time at room temperature or low temperature, and is convenient for construction and preservation.
2. Compared with the prior art that after the silica gel mud prepared in the prior art encounters fire, organic components in the silica gel mud are broken at high temperature due to no fixed form and no cross-linking structure of the silica gel mud to enable the silica gel mud to be molten and pulverized, so that the original structure cannot be kept, and a good fireproof blocking effect cannot be achieved.
3. Compared with the ceramic silicon rubber in the prior art, the halogen-free flame-retardant anti-dripping fireproof plugging silica gel paste prepared by the application can be kept in a soft state for a long time and can be quickly porcelain when meeting fire, and the defects that the ceramic silicon rubber can not be kept in a soft state and can not be used as a fireproof plugging material due to a hard state are overcome.
4. The halogen-free flame-retardant anti-dripping fireproof plugging silica gel mud prepared by specific raw material proportion can be ceramic when meeting fire, and can be used for generating fire disasterWhen the fluxing filler, the refractory filler and the polysiloxane contained in the silicon dioxide are decomposed to generate SiO 2 The eutectic forms a hard and compact ceramic structure and is tightly combined on the side of the hard silicon rubber, so that flame erosion is effectively prevented, and the fireproof capacity of the plugging position can be greatly improved.
5. The halogen-free flame-retardant anti-dripping fireproof plugging silica gel mud prepared by the method has the excellent performances of halogen-free flame retardance, heat insulation, fireproof and dampproof properties, softness in four seasons, no dry crack, no oil flowing, ceramic property, crosslinking property and the like, and can be widely applied to fireproof plugging of electric power facilities such as wind power, thermal power, hydropower, nuclear power, photovoltaic power, energy storage and the like.
6. The performance test of the halogen-free flame-retardant anti-dripping type fireproof blocking silica gel mud shows that the halogen-free flame-retardant anti-dripping type fireproof blocking silica gel mud with excellent performances in all aspects can be obtained only if the silica gel mud raw material contains the components such as the fireproof filler, the initiator, the flame retardant, the modifier and the like in a specific proportion.
Drawings
Fig. 1 shows a fire situation of a fire-blocking material a commonly used in the market at present.
Fig. 2 shows a fire condition of a fire blocking material B commonly used in the market at present.
Fig. 3 shows the fire condition of the halogen-free flame retardant anti-dripping fireproof plugging silica gel slurry prepared in example 4.
Detailed Description
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present application, however, the present application may be practiced in other ways than those described herein, and therefore the scope of the present application is not limited to the specific embodiments disclosed below.
The raw materials and equipment used in the examples and comparative examples are conventional commercial products.
Fire-resistant integrality, fire-resistant thermal insulation, apparent density, corrosion resistance, water resistance, oil resistance, moist heat resistance, freeze thawing cycle performance detection all are according to: GB23864-2009 fire-proof sealing Material.
[ example 1 ]
(1) Pouring 100kg 40000mPa.s107 gel into a 1000L kneader, sequentially adding 150kg of kaolin, 200kg of magnesium hydroxide and 1kg of hydroxyl silicone oil, putting into the kneader according to a proportion, heating to 100 ℃ for kneading for 4 hours, then kneading for 2 hours under the pressure of-0.09 MPa, and cooling to room temperature to obtain base gel;
(2) Adding 0.8kg of bis-2, 4 (2, 4-dichloro benzoyl peroxide) into the base adhesive according to the proportion, and kneading for 1h to obtain the halogen-free flame-retardant anti-dripping fireproof plugging silica gel mud material.
[ example 2 ]
(1) 100kg 100000mPa.s107, pouring into a 1000L kneader, sequentially adding 300kg of refractory filler (kaolin and hollow glass beads are mixed according to the mass ratio of 2:1), 110kg of flame retardant (aluminum hydroxide and magnesium hydroxide are mixed according to the mass ratio of 3:8), and 4kg of modifier (vinyltriethoxysilane and isopropyl tri (dioctyl pyrophosphoryl oxy) titanate according to the mass ratio of 1:1), heating to 120 ℃ and kneading for 4 hours, then reducing the pressure and kneading for 2 hours under-0.09 MPa, and cooling to room temperature to obtain base rubber;
(2) Adding 6kg of bis-2, 5 (2, 5-bis (tert-butyl) -2, 5-dimethylhexane) into the base adhesive according to the proportion, and kneading for 0.5h to obtain the halogen-free flame-retardant anti-dripping fireproof plugging silica gel mud material.
[ example 3 ]
(1) 50kg 1200000mPa.s107 glue and 50kg30000mPa.s107 glue are poured into a 1000L kneader, 450kg of fire-resistant filler (hollow glass beads, calcium carbonate and white carbon black are mixed according to the mass ratio of 1:1:1), 90kg of flame retardant (aluminum hydroxide, magnesium hydroxide and ammonium polyphosphate are mixed according to the mass ratio of 1:1:1) and 5kg of modifier (hydroxy silicone oil, vinyl triethoxysilane and isopropyl tri (dioctyl pyrophosphoryl oxy) titanate are put into the kneader according to the mass ratio of 1:1:3) are sequentially added, the temperature is raised to 140 ℃ for kneading for 3 hours, then the mixture is depressurized and kneaded for 1 hour under the pressure of-0.09 MPa, and the mixture is cooled to room temperature to obtain base glue;
(2) 10kg of dibenzoyl peroxide is added into the base adhesive according to the proportion, and kneaded for 0.5h, thus obtaining the halogen-free flame-retardant anti-dripping fireproof plugging silica gel mud material.
[ example 4 ]
(1) 20kg of 100000mPa.s terminal vinyl diphenyl silicone oil and 80kg 200000mPa.s107 glue are poured into a 1000L kneader, 598kg of refractory filler (kaolin, hollow glass beads, calcium carbonate and white carbon black are mixed according to the mass ratio of 10:10:5:1), 60kg of flame retardant (aluminum hydroxide, magnesium hydroxide and ammonium polyphosphate are mixed according to the mass ratio of 2:1:2), 9kg of modifier (hydroxy silicone oil, vinyl triethoxysilane and isopropyl tri (dioctyl pyrophosphoric acid acyloxy) titanate are mixed according to the mass ratio of 4:2:3) are sequentially added into the kneader, the temperature is raised to 150 ℃ for kneading for 3 hours, then the mixture is decompressed and kneaded under the pressure of-0.09 MPa for 2 hours, and the mixture is cooled to room temperature, so that the base glue is obtained;
(2) 5kg of bis-2, 5 (2, 5-bis (tert-butyl) -2, 5-dimethylhexane) is added into the base adhesive according to the proportion, and the mixture is kneaded for 0.5h to obtain the halogen-free flame-retardant anti-dripping fireproof plugging silica gel mud material.
[ example 5 ]
(1) 20kg 100000mPa.s107 glue and 80kg 200000mPa.s107 glue are poured into a 1000L kneader, 598kg of refractory filler (kaolin, hollow glass beads, calcium carbonate and white carbon black are mixed according to the mass ratio of 10:10:5:1), 60kg of flame retardant (aluminum hydroxide, magnesium hydroxide and ammonium polyphosphate are mixed according to the mass ratio of 2:1:2) and 9kg of hydroxyl silicone oil are sequentially added into the kneader, the temperature is raised to 150 ℃ and kneaded for 3 hours, then the mixture is decompressed and kneaded for 2 hours under the pressure of-0.09 MPa, and the mixture is cooled to room temperature to obtain base glue;
(2) 5kg of bis-2, 5 (2, 5-bis (tert-butyl) -2, 5-dimethylhexane) is added into the base adhesive according to the proportion, and the mixture is kneaded for 0.5h to obtain the halogen-free flame-retardant anti-dripping fireproof plugging silica gel mud material.
[ example 6 ]
(1) Adding 40kg 600000mPa.s107 glue and 60kg 100000mPa.s107 glue into a 1000L kneader, sequentially adding 286kg of refractory filler (kaolin, hollow glass beads, calcium carbonate and white carbon black are mixed according to the mass ratio of 10:10:5:1), 100kg of flame retardant (aluminum hydroxide, magnesium hydroxide are mixed according to the mass ratio of 2:1:2 of ammonium polyphosphate) and 4kg of isopropyl tri (dioctyl pyrophosphoric acid acyloxy) titanate into the kneader, heating to 150 ℃ for kneading for 3 hours, then reducing the pressure for kneading for 2 hours under-0.09 MPa, and cooling to room temperature to obtain base glue;
(2) 8kg of bis-2, 4 (2, 4-dichloro benzoyl peroxide) is added into the base adhesive according to the proportion, and the mixture is kneaded for 1h to obtain the halogen-free flame-retardant anti-dripping fireproof plugging silica gel mud material.
Comparative example 1
(1) Adding 40kg 600000mPa.s107 glue and 60kg 100000mPa.s107 glue into a 1000L kneader, sequentially adding 286kg of refractory filler (kaolin, hollow glass beads, calcium carbonate and white carbon black are mixed according to the mass ratio of 10:10:5:1), 100kg of flame retardant (aluminum hydroxide, magnesium hydroxide are mixed according to the mass ratio of 2:1:2 of ammonium polyphosphate) and 4kg of isopropyl tri (dioctyl pyrophosphoric acid acyloxy) titanate into the kneader, heating to 150 ℃ for kneading for 3 hours, then reducing the pressure for kneading for 2 hours under-0.09 MPa, and cooling to room temperature to obtain base glue;
(2) And kneading the base adhesive for 1h to obtain the fireproof plugging material.
Comparative example 2
(1) Pouring 100kg 1000mPa.s107 glue into a 1000L kneader, sequentially adding 78kg of refractory filler (kaolin, hollow glass beads, calcium carbonate and white carbon black are mixed according to the mass ratio of 10:10:5:1), 20kg of flame retardant (aluminum hydroxide, magnesium hydroxide and ammonium polyphosphate are mixed according to the mass ratio of 2:1:2), and 0.1kg of isopropyl tri (dioctyl pyrophosphoric acid acyloxy) titanate, putting into the kneader according to the proportion, heating to 150 ℃ for kneading for 3 hours, then reducing the pressure for kneading for 2 hours under-0.09 MPa, and cooling to room temperature to obtain base glue;
(2) Adding 0.001kg of bis-2, 4 (2, 4-dichloro benzoyl peroxide) into the base adhesive according to the proportion, and kneading for 1h to obtain the fireproof blocking material.
Table 1 examples and comparative examples are given in parts by weight of the components
Table 2 results of the performance tests of the products prepared in examples and comparative examples
From the experimental results in table 2, it can be seen that: the products prepared by the embodiments 1-6 can keep the daub shape for a long time, and the peroxide initiator can exist stably at normal temperature or low temperature and cannot cause the reaction of the polysiloxane matrix; the products of examples 1-6 do not have the phenomenon of molten drops after being fired, and the products harden after being fired, which shows that when the products are fired, under the action of high temperature, the initiator is decomposed to generate free radicals to trigger polysiloxane reaction, so that a cross-linked network is formed, the fire-receiving side of the silica gel mud is changed into a hard silicone rubber state, the hard silicone rubber structure can play a good supporting role, the damage of the fireproof structure is prevented, the phenomena of pulverization and molten drops of the silica gel mud in the prior art are effectively avoided, and the safety of the plugging structure can be effectively protected; comparative example 1 does not contain an initiator, and can not initiate the reaction of the polysiloxane matrix when meeting fire, so that the product is subject to fire, molten drop and chalking phenomena and is not hardened; the products of examples 4-6 were ceramized after fire, indicating that the products of the specific component materials decomposed to SiO with the fluxing filler, the refractory filler and the polysiloxane upon fire 2 The eutectic forms a hard and compact ceramic structure, and is tightly combined on the hard silicon rubber side, so that flame can be effectively prevented from further corrosion; the products of examples 1-6 perform excellently in fire-resistant integrity and fire-resistant insulation tests compared to comparative example 1; the performance of the silica gel mud prepared in the comparative example 2 in fire and fire resistance tests is far lower than that of the silica gel mud prepared by the technical scheme of the application, which shows that the silica gel mud prepared by the specific range of the raw material proportion can only show excellent fireproof blocking performance.
As can be seen from fig. 1 to 3 of the specification, fig. 1 and 2 show that the fire-proof plugging materials a and B commonly used in the market at present have a molten drop phenomenon during the firing process, and fig. 3 shows that the halogen-free flame-retardant molten drop-proof type fire-proof plugging silica gel prepared in example 4 has no molten drop phenomenon during the firing process and still maintains the original skeleton structure after the firing. FIG. 3 further demonstrates that when the product prepared by the technical scheme of the application is subjected to fire, under the action of high temperature, the initiator is decomposed to generate free radicals to trigger polysiloxane reaction to form a crosslinked networkThe fire side of the silica gel mud is changed into a hard silicone rubber state, the hard silicone rubber structure can play a good supporting role, the damage of a fireproof structure is prevented, the phenomena of pulverization and molten drops of the silica gel mud in the prior art are effectively avoided, the safety of a plugging structure can be effectively protected, and the fluxing filler, the fireproof filler and polysiloxane are decomposed to generate SiO when the product of the raw material of a specific component meets fire 2 The eutectic forms a hard and compact ceramic structure, and is tightly combined on the hard silicon rubber side, so that further corrosion of flame can be effectively prevented.
In conclusion, the halogen-free flame-retardant anti-dripping fireproof plugging silica gel mud with excellent performances can be widely applied to fireproof plugging of electric facilities such as wind power, thermal power, hydroelectric power, nuclear power, photovoltaic power, energy storage and the like.
In this specification, each embodiment is described in a progressive manner, and identical and similar parts of each embodiment are all referred to each other, and each embodiment mainly describes differences from other embodiments. In particular, for system embodiments, since they are substantially similar to method embodiments, the description is relatively simple, as relevant to see a section of the description of method embodiments.
The foregoing is merely exemplary of the present application and is not intended to limit the present application. Various modifications and variations of the present application will be apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. which come within the spirit and principles of the application are to be included in the scope of the claims of the present application.
Claims (6)
1. The halogen-free flame-retardant anti-dripping fireproof blocking silica gel is characterized in that: the halogen-free flame-retardant anti-dripping fireproof blocking silica gel mud consists of the following raw material components in parts by weight: 100 parts of polysiloxane matrix, 100-600 parts of refractory filler, 50-300 parts of flame retardant, 0.01-20 parts of initiator and 0.5-10 parts of modifier; the refractory filler is a mixture formed by kaolin, hollow glass beads, calcium carbonate and white carbon black, and the mass ratio of the mixture is 10:10:5:1; the peroxide is one or more of bis-2, 4 (2, 4-dichloro benzoyl peroxide), bis-2, 5 (2, 5-bis (tertiary butyl) -2, 5-dimethylhexane), benzoyl peroxide, dibenzoyl peroxide, tertiary butyl peroxybenzoate, di-tertiary butyl peroxide and dicumyl peroxide.
2. The halogen-free flame-retardant anti-dripping fireproof plugging silica gel mud disclosed in claim 1, wherein the silica gel mud is characterized by: the refractory filler is one or more of kaolin, diatomite, hollow glass microspheres, calcium carbonate, mica powder, expanded vermiculite and white carbon black.
3. The halogen-free flame-retardant anti-dripping fireproof plugging silica gel mud disclosed in claim 1, wherein the silica gel mud is characterized by: the flame retardant is one or more of aluminum hydroxide, magnesium hydroxide, melamine, ammonium polyphosphate and hexaphenoxy cyclotriphosphazene.
4. The halogen-free flame-retardant anti-dripping fireproof plugging silica gel mud disclosed in claim 1, wherein the silica gel mud is characterized by: the modifier is hydroxyl silicone oil, a silane coupling agent, a titanate coupling agent or an aluminate coupling agent; the silane coupling agent is vinyl triethoxysilane, and the titanate coupling agent is isopropyl tri (dioctyl pyrophosphoric acid acyloxy) titanate.
5. The halogen-free flame-retardant anti-dripping fireproof plugging silica gel mud disclosed in claim 1, wherein the silica gel mud is characterized by: the polysiloxane matrix is polysiloxane with a structure shown in the following general formula (I):
（I）
wherein:
R 1 and R is 2 Is a saturated or unsaturated group selected from methyl, ethyl, propyl, phenyl, trifluoropropyl, vinyl, long chain alkyl, R 1 And R is 2 May be the same or different；R 3 Represents vinyl; r is R 4 And R is 5 Is a saturated or unsaturated group selected from methyl, ethyl, hydroxy, hydroxypropyl, vinyl, R 4 And R is 5 May be the same or different; m, n and z are integers, m is more than or equal to 0, n is more than or equal to 0, z is more than or equal to 0, and (m+n+z) is more than or equal to 400 and less than or equal to 5000.
6. The method for preparing the halogen-free flame-retardant anti-dripping fireproof plugging silica gel mud according to any one of claims 1 to 5, which is characterized by comprising the following steps: the method comprises the following steps:
(1) The polysiloxane matrix, the fire-resistant filler, the fire retardant and the modifier are put into a kneader according to the proportion, heated to 100 ℃ to 150 ℃ and kneaded for 2h to 4h, then decompressed and kneaded for 1h to 2h under the pressure of minus 0.09MPa, and cooled to the room temperature to obtain the base rubber;
(2) And adding an initiator into a kneader according to a formula amount, kneading for 0.5-1 h, and extruding through a screw to obtain the halogen-free flame-retardant anti-dripping fireproof plugging silica gel.
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