CN104650597B - Preparation method of ceramizable fireproof and fire-resistant silicone rubber - Google Patents
Preparation method of ceramizable fireproof and fire-resistant silicone rubber Download PDFInfo
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- CN104650597B CN104650597B CN201510073286.0A CN201510073286A CN104650597B CN 104650597 B CN104650597 B CN 104650597B CN 201510073286 A CN201510073286 A CN 201510073286A CN 104650597 B CN104650597 B CN 104650597B
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- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 230000009970 fire resistant effect Effects 0.000 title abstract description 8
- 239000004945 silicone rubber Substances 0.000 title description 2
- 239000000919 ceramic Substances 0.000 claims abstract description 67
- 239000000463 material Substances 0.000 claims abstract description 4
- 229920001971 elastomer Polymers 0.000 claims description 49
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 38
- 229910052710 silicon Inorganic materials 0.000 claims description 38
- 239000010703 silicon Substances 0.000 claims description 38
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 22
- 239000000843 powder Substances 0.000 claims description 19
- RGPUVZXXZFNFBF-UHFFFAOYSA-K diphosphonooxyalumanyl dihydrogen phosphate Chemical compound [Al+3].OP(O)([O-])=O.OP(O)([O-])=O.OP(O)([O-])=O RGPUVZXXZFNFBF-UHFFFAOYSA-K 0.000 claims description 14
- 229920002554 vinyl polymer Polymers 0.000 claims description 14
- 230000000903 blocking effect Effects 0.000 claims description 12
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 10
- 238000012545 processing Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 8
- 239000003607 modifier Substances 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 238000010792 warming Methods 0.000 claims description 8
- OGPNXGJLKXGASM-UHFFFAOYSA-N [Si].CC=C Chemical compound [Si].CC=C OGPNXGJLKXGASM-UHFFFAOYSA-N 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 229910002012 Aerosil® Inorganic materials 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 3
- MOSXLDGILGBOSZ-UHFFFAOYSA-N ethenyl-methyl-phenylsilicon Chemical compound C=C[Si](C)C1=CC=CC=C1 MOSXLDGILGBOSZ-UHFFFAOYSA-N 0.000 claims description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 3
- 238000005086 pumping Methods 0.000 claims description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 239000001257 hydrogen Substances 0.000 claims description 2
- 229910052739 hydrogen Inorganic materials 0.000 claims description 2
- 239000004411 aluminium Substances 0.000 claims 1
- SEGLCEQVOFDUPX-UHFFFAOYSA-N di-(2-ethylhexyl)phosphoric acid Chemical compound CCCCC(CC)COP(O)(=O)OCC(CC)CCCC SEGLCEQVOFDUPX-UHFFFAOYSA-N 0.000 claims 1
- 238000005336 cracking Methods 0.000 abstract description 4
- 230000009467 reduction Effects 0.000 abstract description 2
- 230000015556 catabolic process Effects 0.000 abstract 1
- 238000006731 degradation reaction Methods 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 14
- 239000002131 composite material Substances 0.000 description 12
- 238000000034 method Methods 0.000 description 11
- 238000007792 addition Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 239000004744 fabric Substances 0.000 description 7
- 239000011521 glass Substances 0.000 description 7
- 238000003756 stirring Methods 0.000 description 7
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 229920002545 silicone oil Polymers 0.000 description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 5
- 239000004020 conductor Substances 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 5
- 239000010949 copper Substances 0.000 description 5
- 239000011268 mixed slurry Substances 0.000 description 5
- 229920000260 silastic Polymers 0.000 description 5
- 239000005977 Ethylene Substances 0.000 description 4
- 238000002679 ablation Methods 0.000 description 4
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 4
- 239000000839 emulsion Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000011056 performance test Methods 0.000 description 4
- 229920001296 polysiloxane Polymers 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 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 description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 3
- 229910003978 SiClx Inorganic materials 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- OLLFKUHHDPMQFR-UHFFFAOYSA-N dihydroxy(diphenyl)silane Chemical compound C=1C=CC=CC=1[Si](O)(O)C1=CC=CC=C1 OLLFKUHHDPMQFR-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000003063 flame retardant Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 239000010445 mica Substances 0.000 description 3
- 229910052618 mica group Inorganic materials 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 229910052573 porcelain Inorganic materials 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000004073 vulcanization Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 230000009977 dual effect Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- XQSFXFQDJCDXDT-UHFFFAOYSA-N hydroxysilicon Chemical group [Si]O XQSFXFQDJCDXDT-UHFFFAOYSA-N 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- -1 methyl phenyl vinyl Chemical group 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004804 winding Methods 0.000 description 2
- 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 description 1
- NALFRYPTRXKZPN-UHFFFAOYSA-N 1,1-bis(tert-butylperoxy)-3,3,5-trimethylcyclohexane Chemical class CC1CC(C)(C)CC(OOC(C)(C)C)(OOC(C)(C)C)C1 NALFRYPTRXKZPN-UHFFFAOYSA-N 0.000 description 1
- HSLFISVKRDQEBY-UHFFFAOYSA-N 1,1-bis(tert-butylperoxy)cyclohexane Chemical compound CC(C)(C)OOC1(OOC(C)(C)C)CCCCC1 HSLFISVKRDQEBY-UHFFFAOYSA-N 0.000 description 1
- OSNIIMCBVLBNGS-UHFFFAOYSA-N 1-(1,3-benzodioxol-5-yl)-2-(dimethylamino)propan-1-one Chemical compound CN(C)C(C)C(=O)C1=CC=C2OCOC2=C1 OSNIIMCBVLBNGS-UHFFFAOYSA-N 0.000 description 1
- YNJSNEKCXVFDKW-UHFFFAOYSA-N 3-(5-amino-1h-indol-3-yl)-2-azaniumylpropanoate Chemical compound C1=C(N)C=C2C(CC(N)C(O)=O)=CNC2=C1 YNJSNEKCXVFDKW-UHFFFAOYSA-N 0.000 description 1
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical class CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 238000007259 addition reaction Methods 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 235000019400 benzoyl peroxide Nutrition 0.000 description 1
- 229910052810 boron oxide Inorganic materials 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 238000003490 calendering Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 0.000 description 1
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 description 1
- ZXPDYFSTVHQQOI-UHFFFAOYSA-N diethoxysilane Chemical compound CCO[SiH2]OCC ZXPDYFSTVHQQOI-UHFFFAOYSA-N 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000007688 edging Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000000505 pernicious effect Effects 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000011819 refractory material Substances 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 229920005573 silicon-containing polymer Polymers 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 230000005619 thermoelectricity Effects 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 229910001928 zirconium oxide Inorganic materials 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
- Insulated Conductors (AREA)
Abstract
The invention belongs to the technical field of fireproof and fireproof materials, and discloses a preparation method of ceramizable fireproof and fireproof silicon rubber. The ceramic fireproof fire-resistant silicon rubber prepared by the invention has improved mechanical stability, avoids the severe degradation of the silicon rubber layer in a lower-temperature environment to cause cracking or density reduction of a final ceramic shell layer, and effectively improves the reliability of a fire-resistant cable taking the silicon rubber as a fire-resistant layer material in practical application.
Description
Technical field
The present invention relates to a kind of refractory material, especially it is a kind of can ceramic fireproof silicon rubber preparation method.
Background technology
Fire-resisting cable refers to there is defined fire resistance, can ensure that circuit continues stable operation one under flame condition
The section time, make power system and the whistle control system normal work under flame condition, loss caused by fire is preferably minimized
Limit.
At present, domestic and international fire-resisting cable mainly has magnesium oxide mineral insulated fireproof cable and Mica tape inorganic insulation
Fire-resisting cable.Though mineral insulated cable has good fire resistance, its manufacturing process is complicated, production cost is high,
Difficulty of construction is very high, it is difficult to extensive use.Although Mica tape fire-resisting cable work technique is simple, mica tape generally existing
One shortcoming, become fragile after high-temp combustion, by easy powder of detached after strenuous vibration, cause fire resisting ineffective.With ceramic SiClx
Fire resistant belt construction is simple is easy to operate made from rubber, and production cost is low, can mass production.Ceramic silicon rubber has excellent
High-low temperature resistant, weather-proof, resistance to ozone, arc resistant, electric insulating quality, when running into flame can the ablated stiff shell into ceramic-like,
One layer of hard protective layer is formed, so that protected object is without damage.
Chinese patent CN103236309A discloses a kind of preparation method of ceramifiable silicon rubber composite belt for fire-resistant cable, should
The wrapped obtained fire-resisting cable of fire resistant belt prepared by method is in 650-950 DEG C of flame, and ablation 180 minutes, circuit remains to normally
Work.However, in incipient fire, fireproof cable local environment temperature is not up to 650 DEG C, lapping layer environment temperature by
Edging up during height, significant degraded, softening can takes place in silicon rubber therein from 350 DEG C of even lower temperature, and not
Ceramic forms crust layer, thus causes the reduction of lapping layer mechanical property, and the now vibrations of scene of fire or water leaching may
Cause lapping layer cracking, peel off, the normal work of circuit can not be ensured, or cause the shell after ceramic crack to be present, meet water
Short circuit easily occurs for circuit during leaching.
The content of the invention
In order to solve the above problems, the present invention provide it is a kind of can ceramic fireproof silicon rubber preparation method, the party
Method prepare can fire-resisting ceramic silicone rubber there is good mechanical property, and preferably (350 DEG C or so) crust property of low temperature
And mechanical stability.
Inventing the technical scheme used is：
It is a kind of can ceramic fireproof silicon rubber preparation method, it is described can ceramic fireproof silicon rubber preparation
Raw material includes organic silicon compounded rubber stock and ceramic powder, and organic silicon compounded rubber stock is by including silicon raw rubber, aerosil, structure
The raw material for changing controlling agent and ceramic modifier is made；
The preparation method comprises the following steps：
A, silicon raw rubber, aerosil, antistructurizing agent are mixed with ceramic modifier, is warming up to 80 DEG C -100
DEG C 1-1.5 hours are kneaded, then are warming up to 160 DEG C -170 DEG C, pumping vacuum and mixing 1.5-2.5 hours, obtain organic silicon compounded rubber stock；
B, 0.5-1.5 hours are ground after ceramic powder is mixed, in 150-160 DEG C of dry 2-3h, are obtained pretreated
Ceramic powder；
C, pretreated ceramic powder is added in organic silicon compounded rubber stock and mixed, it is small to be kneaded 0.5-1 at 25 DEG C -90 DEG C
When, natural cooling, cut into slices in mill it is thin it is logical add vulcanizing agent for several times and be kneaded 0.5-1 hours, obtain can ceramic fire prevention it is resistance to
Fiery silicon rubber.
Preferably, the ceramic modifier is that molecular formula is Fe (CO)3[(CH2=CHSiMe2O)3SiR] complex compound,
It has following structural formula：
Wherein, R is methyl or phenyl.
Preferably, in step A, the vacuum pressure of the pumping vacuum and mixing process is -0.08Mpa--0.06Mpa.
Preferably, in step C, the vulcanizing agent is from 2,5- dimethyl -2,5- bis(t-butylperoxy)s hexane, peroxide
Change double-(2,4 dichloro benzene formyl), peroxidating double (4- toluyls), dibenzoyl peroxide, the tertiary fourths of perbenzoic acid
One kind in ester, 1,1- bis(t-butylperoxy) -3,3,5- trimethyl-cyclohexanes, 1,1-bis(t-butylperoxy)cyclohexane
Or it is several, addition measures convention amount can.
Preferably, organic silicon compounded rubber stock is made by the following raw material counted in parts by weight：
Preferably, the silicon raw rubber is the mixing of the following silicon raw rubber counted in parts by weight：
Vinyl mass content is 0.20%-0.30% ethenyl blocking methyl ethylene silicon raw rubber 15-25 parts；
Vinyl mass content is 0.08%-0.15% ethenyl blocking methyl ethylene silicon raw rubber 40-50 parts；
Vinyl mass content is 0.03%-0.08% methyl blocking methyl phenyl vinyl silicon raw rubber 35-45 parts；
The total number of the silicon raw rubber is 100 parts.
Vinyl mass content of the present invention is the mass percent of silicon raw rubber medium vinyl.
It is highly preferred that the ethenyl blocking methyl ethylene silicon that the vinyl mass content is 0.20%-0.30% is given birth to
The molecular weight of glue is 80-90 ten thousand, and the vinyl mass content is 0.08%-0.15% ethenyl blocking methyl ethylene silicon
The molecular weight of rubber is 70-80 ten thousand, and the vinyl mass content is 0.03%-0.08% methyl blocking methyl phenyl vinyl
The molecular weight of base silicon raw rubber is 40-60 ten thousand.In the present invention, the molecular weight of silicon raw rubber is viscosity average molecular weigh.
Preferably, the aerosil is the hydrophobic type gas phase silica handled through dimethyl silicone polymer.Dredge
The preparation method of water type aerosil is not particularly limited.
Preferably, the antistructurizing agent is hydroxy silicon oil, vinyl hydroxy silicone oil, diphenyl silanediol, dimethyl
One or more in diethoxy silane, dimethyldimethoxysil,ne, hydroxy silicon oil.It is highly preferred that the structuring control
Preparation is diphenyl silanediol.
Preferably, the ceramic powder includes by weight：
Preferably, in terms of the silicon raw rubber of 100 parts by weight, the dosage of the ceramic powder is 70-100 parts by weight.
Preferably, can the preparing raw material of ceramic fireproof silicon rubber include aluminium dihydrogen phosphate, by phosphoric acid in step C
Aluminum dihydrogen is added in organic silicon compounded rubber stock together with pretreated ceramic powder and mixed.
It is highly preferred that the aluminium dihydrogen phosphate is the aluminium dihydrogen phosphate of coated processing, the inorganic agent of the cladding processing
For bi-component addition type liquid silastic.The bi-component addition type liquid silastic is not particularly limited, and generally comprises A, B group
Point, component A is mainly made up of vinyl silicone oil, platinum catalyst, inhibitor and filler, and B component is mainly by vinyl silicone oil, hydrogeneous
Silicone oil and filler composition, in room temperature or heated after in certain mass ratio, component A is mixed with B component, vinyl silicone oil and
Addition reaction occurs for containing hydrogen silicone oil, and then vulcanizes.
Preferably, the preparation method of the aluminium dihydrogen phosphate of the coated processing is：Take aluminium dihydrogen phosphate 145-165g with
Dimethylbenzene 200-600ml mixed grinding 1-3h, the component A 5-20g for adding bi-component addition type liquid silastic continue to grind 2-
3h, mixed slurry is obtained, the two-component diluted by 100-150ml dimethylbenzene will be added in mixed slurry, under stirring condition and is added
The B component 5-20g of molding liquid silicon rubber, continue to stir 1-2h, be warming up to 90-110 DEG C and continue to stir 1-2.5h, then be warming up to
120-130 DEG C is continued to stir 1-2h, is filtered, is dried, obtain the aluminium dihydrogen phosphate of coated processing.
Preferably, in terms of the silicon raw rubber of 100 parts by weight, the dosage of the aluminium dihydrogen phosphate is 10-20 parts by weight.
The present invention prepare can ceramic fireproof silicon rubber fire-resisting cable preparation in application process can be by
It is described can ceramic fireproof silicon rubber and glass cloth enhancement layer roll compound after cure, it is compound to obtain Ceramic silicon rubber
Band, it is wrapped to cable progress by Ceramic silicon rubber composite band, obtain fire-resisting cable；Or can porcelain fire-resistant silicon rubber by low temperature
Directly it is extruded on cable and vulcanizes and form flame retardant coating, obtains fire-resisting cable.
The invention has the advantages that：
The present invention prepare can ceramic fireproof silicon rubber there is good mechanical property, and preferable low temperature
(350 DEG C or so) crust property and mechanical stability, the silicon rubber are degraded under 350-400 DEG C of hot environment, while can
Certain mechanical property is kept, causes to produce obvious crack without softening, mechanical shock is run into and water leaching is not also ftractureed
And peeling, effectively improve the fire-resisting cable reliability in actual applications using the silicon rubber as fire resisting layer material, and preparation side
Method is simple.
Embodiment
Specific embodiment of the invention given below.
The present invention can ceramic fireproof silicon rubber be made by the raw material including organic silicon compounded rubber stock and ceramic powder,
Prepared by following methods：
A, by silicon raw rubber 1000g, hydrophobic type fumed silica 150g (goldschmidt chemical corporation R202), diphenyl silanediol
27g, ceramic modifier 20g mixing are added in kneader, add 100g hydrophobic type vapor phase methods after kneading is agglomerating every time in three times
Silica (goldschmidt chemical corporation R202), all mix it is agglomerating after be heated up to 100 DEG C and be kneaded 1 hour, continue to be heated up to 160 DEG C-
170 DEG C, vacuumize (vacuum pressure is maintained at -0.08MPa--0.06MPa) and be kneaded 2 hours, obtain organic silicon compounded rubber stock；
Wherein, silicon raw rubber is included by contents of ethylene is 0.23%, molecular weight is 830,000 ethenyl blocking ethylene methacrylic
Base silicon raw rubber 200g, the ethenyl blocking methyl ethylene silicon raw rubber 400g that contents of ethylene 0.10%, molecular weight are 750,000
And the methyl blocking methyl phenyl vinyl silicon raw rubber 400g that contents of ethylene is 0.05%, molecular weight is 550,000；
The molecular formula of ceramic modifier is Fe (CO)3[(CH2=CHSiMe2O)3SiR], and there is following structural formula：
Wherein, R is methyl or phenyl.
Specifically with Fe (CO)3[(CH2=CH Me2SiO)3Si(CH3)] exemplified by, its preparation method is：
118g Fe (CO) are added in the three-necked flask with condenser5With 4L pentanes, by 104g (CH2=CH Me2SiO)3Si(CH3) slowly instill in three-necked flask, argon gas is passed through, is stirred under the conditions of wavelength is 320-400nm ultraviolet light anti-
2h is answered, is filtered, the solvent in filtrate is evaporated, vacuum drying, obtains Fe (CO)3[(CH2=CH Me2SiO)3Si(CH3)], instead
Answer formula as follows：
B, carborundum 400g, aluminum oxide 120g, zirconium oxide 100g, boron oxide 24g, montmorillonite 240g are placed in mixed at high speed
0.5h is mixed in machine, 1h is then ground in ball mill, then is placed in baking oven in 150 DEG C of dry 3h, obtains pretreated pottery
Vitrified powder.
It C1, will mix, mediate with organic silicon compounded rubber stock in pretreated ceramic powder 284g additions kneader in step B
Divide again after agglomerating 2 times and add remaining pretreated ceramic powder, be allowed to be sufficiently mixed uniformly, then with organic silicon compounded rubber stock
It is kneaded 1 hour, natural cooling after taking-up, is cut into slices in thin logical 3-5 times in mill, addition 2,4- dichloro benzoyl peroxide first at 85 DEG C
Acyl 15g mills 0.5 hour, obtain can ceramic fireproof silicon rubber, be designated as 1# fireproof silicon rubber.
C2, pretreated ceramic powder 284g in step B, coated processing aluminium dihydrogen phosphate 160g will be added and pinched
Mix with organic silicon compounded rubber stock in conjunction machine, mediate it is agglomerating after divide 2 remaining pretreated ceramic powder of addition again, be allowed to and
Organic silicon compounded rubber stock, the aluminium dihydrogen phosphate of coated processing are sufficiently mixed uniformly, are then kneaded 1 hour at 70 DEG C, after taking-up certainly
So cooling, cut into slices in thin logical 3-5 time in mill, addition 2,4- dichlorobenzoperoxide 15g mills 0.5 hour, obtaining can
Ceramic fireproof silicon rubber, it is designated as 2# fireproof silicon rubber.
Wherein, the preparation method of the aluminium dihydrogen phosphate of coated processing is in step C2：Take aluminium dihydrogen phosphate 150g and two
Toluene 500ml, mixing add in colloid mill and grind 1h, take the component A 10g of dual composition addition type liquid silastic (to pacify Shenzhen
Product organosilicon material Co., Ltd, AP-2046) add in mixed slurry and continue to grind 2h, mixed slurry is obtained, by mixed slurry
Add in beaker, the B component of the 10g dual composition addition type liquid silastics diluted by 100ml dimethylbenzene is added under stirring condition
(Anpin Organic Silicon Material Co., Ltd., Shenzhen City, AP-2046), 1h is stirred, be warming up to 100 DEG C and continue to stir 2h, then be warming up to
130 DEG C are continued to stir 1h, are dried in vacuo after suction filtration, are produced the aluminium dihydrogen phosphate of coated processing.
Performance test embodiment
First, pair can ceramic fireproof silicon rubber and contrast can Ceramic silicon rubber carry out heat resistance test, specifically
It is as follows：
By can ceramic fireproof silicon rubber and contrast can Ceramic silicon rubber (referred to as contrast) prepare test specimens respectively
Product, preparation method are：Take 100g silicon rubber and 1.3g 2,4- dichlorobenzoperoxides uniform in being fully kneaded in mill,
It is then placed in mould on vulcanizing press and is molded vulcanization, conditions of vulcanization：130 DEG C × 5min, molding pressure 15MPa, cut
Size is obtained afterwards as long 210mm, wide 135mm, thick 2mm sample；
Performance test is carried out to testing sample, is then heat-treated and investigates sample mechanics performance change, specifically will
Sample is respectively placed in 250 DEG C of baking 7d, tests mechanical property N1, then at 350 DEG C of baking 0.5h, tests mechanical property N2, and divide
It is listed in Mechanics Performance Testing project and method reference table 1 not compared with the sample mechanical property N0 not being heat-treated
Standard, test data are shown in Table 1.
Table 1
In table 1, "/" represents the corresponding mechanical property of the sample without valid data.As seen from the data in Table 1, it is of the invention can
Ceramic fireproof silicon rubber has good stable mechanical property in hot environment, beneficial to improve its in low temperature calcination
Under the conditions of mechanical property and fire protecting performance.
2nd, preparing fireproof cable use by 1# fireproofs silicon rubber and 2# fireproof silicon rubber respectively can porcelain SiClx
Rubber composite belt simultaneously carries out performance test, specific as follows：
1st, the preparation method of composite band comprises the following steps：
Silicone acrylic emulsion is configured to the dilution that solid content is 8%, glass cloth is handled in a manner of brushing, in 90 DEG C of temperature
8min is baked down, obtains the glass cloth handled through silicone acrylic emulsion, wherein, the silicon mass content of silicone acrylic emulsion is 8%；
By can ceramic fireproof silicon rubber and through silicone acrylic emulsion handle glass cloth individual layer is carried out by calendering technology
It is compound, after lamination is good, by toasting vulcanization 10-20min at 115-125 DEG C, finally cut into width be 10mm, thickness be
The fireproof cable of 0.8mm one side glass cloth enhancing is used can porcelain SiClx rubber composite belt.
Using method of testing generally in the art to gained waterproof fireproof ceramic silicon rubber composite tape carry out performance test, measure by
The electrical strength of waterproof fireproof ceramic silicon rubber composite tape prepared by 1# fireproofs silicon rubber and 2# fireproofs silicon rubber is big
In equal to 25kV/mm, specific insulation is all higher than being equal to 2 × 1014Ω cm, tensile strength are all higher than being equal to 75N/10mm, reached
Around-packing technology requirement into cable making process.
2nd, the above-mentioned ceramic silicon of resistance to extreme misery prepared by 1# fireproofs silicon rubber and 2# fireproofs silicon rubber is respectively adopted
Rubber composite belt is wrapped to prepare fireproof cable, obtains 1# fireproof cables to be measured and 2# fireproof cables to be measured.It is anti-
The wrapped method of fiery fire-resisting cable is specially：On winding machine, by the glass cloth one side face of waterproof fireproof ceramic silicon rubber composite tape
To copper conductor side, it is set in area of section to be 38mm2Copper conductor on carry out 1/2 lap wound, after 3 layers of lap wound, obtain preventing fires resistance to
Fire bed, the thick polyvinyl resin insulating barriers of 4.0mm are then extruded on fireproof layer, obtain insulated wire cores, take 3 strands absolutely
Edge core is twisted, then extrudes external sheath layer, obtains fireproof cable；
According to British Standard BS 6387:1994, fire resisting test is carried out to fireproof cable, in fire resisting test, fire prevention is resistance to
Thermoelectricity cable power-on voltage is 450/750V, and 1# fireproof cables to be measured and 2# fireproof cables to be measured are in 950 ± 40 DEG C of fire
Under the conditions of flame ablation 3h still keep circuit complete and can normal power-up, and discharged in combustion process without pernicious gas.
3rd, the ceramic silicon of the resistance to extreme misery rubber prepared using above-mentioned 1# fireproofs silicon rubber and 2# fireproofs silicon rubber is answered
Crossed belt and it is of the prior art can the wrapped copper conductor of Ceramic silicon rubber composite band (be designated as contrast composite band) to prepare band respectively anti-
The cable of fiery flame retardant coating, obtain 1# fireproofs cable, 2# fireproofs cable and contrast fireproof cable.Fireproof cable
The preparation method of line is specially：On winding machine, by the glass cloth one side of composite band towards copper conductor side, make it in section face
Product is 38mm2Copper conductor on carry out 1/2 lap wound, after 3 layers of lap wound, obtain fireproof cable.
The fireproof cable that length is 0.5m is taken, it is horizontal positioned and make fireproof cable under 400 ± 50 DEG C of flame
Ablation 15min, ablation, which finishes, makes fireproof cable freely be fallen from the height of 1m from the ground, investigates and prevents on fireproof cable
The integrity degree of fiery flame retardant coating.Experiment finds that the fireproof layer of 1# fireproofs cable and 2# fireproof cables is without obvious
Cracking, and the fireproof layer for contrasting fireproof cable is cracking, peels off.
Above test result shows that prepared by the present invention can mechanics of the ceramic fireproof silicon rubber in hot environment
Stability is good, beneficial to fire line of the raising fireproof cable prepared therefrom when lower temperature scene of fire uses
Energy.
Above content is to combine specific preferred embodiment further description made for the present invention, it is impossible to is assert
The specific implementation of the present invention is confined to these explanations.For general technical staff of the technical field of the invention,
On the premise of not departing from present inventive concept, some simple deduction or replace can also be made, should all be considered as belonging to the present invention's
Protection domain.
Claims (4)
1. it is a kind of can ceramic fireproof silicon rubber preparation method, it is described can ceramic fireproof silicon rubber preparation it is former
Material includes organic silicon compounded rubber stock and ceramic powder, and organic silicon compounded rubber stock is by including silicon raw rubber, aerosil, structuring
Controlling agent and the raw material of ceramic modifier are made；
The preparation method comprises the following steps：
A, silicon raw rubber, aerosil, antistructurizing agent are mixed with ceramic modifier, is warming up to 80 DEG C -100 DEG C and mixes
1-1.5 hours are refined, then are warming up to 160 DEG C -170 DEG C, pumping vacuum and mixing 1.5-2.5 hours, obtain organic silicon compounded rubber stock；
B, 0.5-1.5 hours are ground after ceramic powder is mixed, in 150-160 DEG C of dry 2-3h, obtain pretreated ceramics
Change powder；
C, pretreated ceramic powder is added in organic silicon compounded rubber stock and mixed, in 25 DEG C of -90 DEG C of mixing 0.5-1 hours, certainly
So cooling, cut into slices and lead to for several times in thin in mill, add vulcanizing agent and be kneaded 0.5-1 hours, obtaining can ceramic fireproof silicon
Rubber,
The ceramic modifier is that molecular formula is Fe (CO)3[(CH2=CHSiMe2O)3SiR] complex compound, it has following knot
Structure formula：
Wherein, R is methyl or phenyl,
The silicon raw rubber is the mixing of the following silicon raw rubber counted in parts by weight：
Vinyl mass content is 0.20%-0.30% ethenyl blocking methyl ethylene silicon raw rubber 15-25 parts；
Vinyl mass content is 0.08%-0.15% ethenyl blocking methyl ethylene silicon raw rubber 40-50 parts；
Vinyl mass content is 0.03%-0.08% methyl blocking methyl phenyl vinyl silicon raw rubber 35-45 parts；
The total number of the silicon raw rubber is that 100 parts of organic silicon compounded rubber stocks are made by the following raw material counted in parts by weight：
2. as described in any one of claim 1 can ceramic fireproof silicon rubber preparation method, it is characterised in that it is described
Ceramic powder includes by weight：
3. as described in claim any one of 1-2 can ceramic fireproof silicon rubber preparation method, it is characterised in that institute
State can the preparing raw material of ceramic fireproof silicon rubber also include aluminium dihydrogen phosphate.
4. as claimed in claim 3 can ceramic fireproof silicon rubber preparation method, it is characterised in that the di(2-ethylhexyl)phosphate
Hydrogen aluminium is the aluminium dihydrogen phosphate of coated processing, and the inorganic agent of the parcel processing is add-on type liquid silicon rubber.
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| CN105924979B (en) * | 2016-05-27 | 2019-01-08 | 成都硅宝科技股份有限公司 | Ceramic organic silicon rubber |
| CN107057365B (en) * | 2016-12-29 | 2020-07-28 | 深圳市安品有机硅材料有限公司 | Flame-retardant ceramifiable silicon rubber for fire-resistant cable and preparation method thereof |
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Effective date of registration: 20220120 Address after: 523000 Room 301, building 5, No. 770, Xie Cao Road, Xiegang Town, Dongguan City, Guangdong Province Patentee after: Guangdong Andy New Material Technology Co.,Ltd. Address before: 518103 1st, 2nd and 3rd floors, building 4, zone 2, Sanxing Industrial Zone, Fuhai Avenue, Fuyong street, Bao'an District, Shenzhen City, Guangdong Province Patentee before: SHENZHEN ANPIN SILICONE MATERIAL Co.,Ltd. |