CN110003474A - A kind of silicon substrate expansion type flame retardant and preparation method thereof - Google Patents
A kind of silicon substrate expansion type flame retardant and preparation method thereof Download PDFInfo
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- CN110003474A CN110003474A CN201910351910.7A CN201910351910A CN110003474A CN 110003474 A CN110003474 A CN 110003474A CN 201910351910 A CN201910351910 A CN 201910351910A CN 110003474 A CN110003474 A CN 110003474A
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- flame retardant
- retardant
- silicon substrate
- expansion type
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 64
- 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 45
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 34
- 239000010703 silicon Substances 0.000 title claims abstract description 34
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000000758 substrate Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 43
- 239000004114 Ammonium polyphosphate Substances 0.000 claims abstract description 19
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims abstract description 19
- 229920001276 ammonium polyphosphate Polymers 0.000 claims abstract description 19
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 15
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 10
- 239000000654 additive Substances 0.000 claims abstract description 8
- 230000000996 additive effect Effects 0.000 claims abstract description 8
- 239000004615 ingredient Substances 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 4
- 229910021389 graphene Inorganic materials 0.000 claims description 26
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 22
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 21
- 239000006185 dispersion Substances 0.000 claims description 17
- -1 polysiloxanes Polymers 0.000 claims description 17
- 229920001296 polysiloxane Polymers 0.000 claims description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 229910002804 graphite Inorganic materials 0.000 claims description 12
- 239000010439 graphite Substances 0.000 claims description 12
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 9
- 229920000548 poly(silane) polymer Polymers 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 6
- 239000002270 dispersing agent Substances 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 239000000908 ammonium hydroxide Substances 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 238000004108 freeze drying Methods 0.000 claims description 5
- 239000008187 granular material Substances 0.000 claims description 5
- 239000004115 Sodium Silicate Substances 0.000 claims description 4
- 235000021355 Stearic acid Nutrition 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 235000014113 dietary fatty acids Nutrition 0.000 claims description 4
- 239000000194 fatty acid Substances 0.000 claims description 4
- 229930195729 fatty acid Natural products 0.000 claims description 4
- 150000004665 fatty acids Chemical class 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical group CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 4
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 4
- 239000012188 paraffin wax Chemical class 0.000 claims description 4
- 229950008882 polysorbate Drugs 0.000 claims description 4
- 229920000136 polysorbate Polymers 0.000 claims description 4
- 239000000344 soap Substances 0.000 claims description 4
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 4
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 4
- 239000003381 stabilizer Substances 0.000 claims description 4
- 239000008117 stearic acid Substances 0.000 claims description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
- 238000007711 solidification Methods 0.000 claims description 3
- 230000008023 solidification Effects 0.000 claims description 3
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 claims description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 claims description 2
- QDAYJHVWIRGGJM-UHFFFAOYSA-B [Mo+4].[Mo+4].[Mo+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O Chemical compound [Mo+4].[Mo+4].[Mo+4].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QDAYJHVWIRGGJM-UHFFFAOYSA-B 0.000 claims description 2
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 2
- 239000011609 ammonium molybdate Substances 0.000 claims description 2
- 229940010552 ammonium molybdate Drugs 0.000 claims description 2
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 2
- 150000002148 esters Chemical class 0.000 claims description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 239000003365 glass fiber Substances 0.000 claims description 2
- 125000005456 glyceride group Chemical group 0.000 claims description 2
- 230000036571 hydration Effects 0.000 claims description 2
- 238000006703 hydration reaction Methods 0.000 claims description 2
- 235000010445 lecithin Nutrition 0.000 claims description 2
- 239000000787 lecithin Substances 0.000 claims description 2
- 229940067606 lecithin Drugs 0.000 claims description 2
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 claims description 2
- 150000003856 quaternary ammonium compounds Chemical class 0.000 claims description 2
- 229910021332 silicide Inorganic materials 0.000 claims description 2
- FVBUAEGBCNSCDD-UHFFFAOYSA-N silicide(4-) Chemical compound [Si-4] FVBUAEGBCNSCDD-UHFFFAOYSA-N 0.000 claims description 2
- NVIFVTYDZMXWGX-UHFFFAOYSA-N sodium metaborate Chemical compound [Na+].[O-]B=O NVIFVTYDZMXWGX-UHFFFAOYSA-N 0.000 claims description 2
- 230000006641 stabilisation Effects 0.000 claims description 2
- 238000011105 stabilization Methods 0.000 claims description 2
- 239000001993 wax Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 4
- 230000002195 synergetic effect Effects 0.000 abstract description 4
- 150000001335 aliphatic alkanes Chemical class 0.000 abstract description 2
- 230000002787 reinforcement Effects 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 239000004743 Polypropylene Substances 0.000 description 4
- 239000004033 plastic Substances 0.000 description 4
- 229920003023 plastic Polymers 0.000 description 4
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002411 thermogravimetry Methods 0.000 description 3
- 230000004580 weight loss Effects 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 230000001965 increasing effect Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 206010054949 Metaplasia Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000008107 benzenesulfonic acids Chemical class 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 235000019504 cigarettes Nutrition 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000005453 pelletization Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920000137 polyphosphoric acid Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
-
- 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
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- 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
- C08K3/32—Phosphorus-containing compounds
-
- 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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
- C08K7/26—Silicon- containing compounds
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- 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
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/322—Ammonium phosphate
- C08K2003/323—Ammonium polyphosphate
-
- 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
Abstract
The invention discloses a kind of silicon substrate expansion type flame retardants and preparation method thereof, the fire retardant includes following mass fraction formula components: 10-70 parts of carbon material, 20-50 parts of organosilan, 10-20 parts of ammonium polyphosphate, 3-10 parts of curing agent, 1-20 parts of flame-retardant additive, the present invention effectively combines organosilicon alkanes flame-retardant composition and expandable flame retardant ingredient, it is prepared for the organic-inorganic fire retardant of synergistic expandable flame retardant effect, and have both acid source, gas source, the expandable flame retardant ingredient of carbon source, by the way of having abandoned traditional simple blend, the shortcomings that effectively compensating for all kinds of flame retardance elements, flame retardant effect can be obviously improved, it can increase the compatibility of fire retardant and high molecular material again, energy reinforcement mechanical strength again, simultaneously, whole preparation process mildly carries out under normal pressure, it is simple and easy, convenient for large-scale production.
Description
Technical field
The present invention relates to high molecular fire retardant technical fields, in particular to a kind of silicon substrate expansion type flame retardant and its preparation
Method.
Background technique
For high molecular material because it is with lot of superiority energy, the dosage in industrial production and life is increasing.With
The enhancing of raising and disaster reduction and prevention theory that people realize fire disasters protection, people to the flame-retardancy requirements of material also more and more
Height, therefore, it is necessary to carry out flame retardant treatment to inflammable high molecular material.Being usually used in the fire retardant of high molecular material at present is mainly
Halogen system, phosphorus flame retardant, they have certain toxicity, and because its general polarity is stronger, are damaged to the mechanical performance of material
Wound.Increasingly stringent with environmental protection and security legislation, Halogen, the research of phosphorus-free flame-retarding technology and fire retardant are developed very urgent.
The last century 80's, people begin to the exploitation of concern Silicone-containing Flame Retardant, and are successfully applied in plastics
Achieve good flame retardant effect.Silicone-containing Flame Retardant and its flame-retarded technology have obtained extensive research and development at present, due to containing
The polymer of silicon fire retardant lacks that cigarette is nontoxic, combustion heat value is low, flame propagation velocity is slow and is taken seriously, development potentiality and application
Prospect is very huge.However, single flame retardance element can not give full play to the efficiency of Silicone-containing Flame Retardant, need further to pass through
Efficient silane-containing synergistic flame-retardant system is developed, its integrated performance index for being applied to high molecular material is further increased.
Summary of the invention
In order to solve the above technical problems, inventor chooses carbon material with surface hydroxyl and with the organic of reactivity
Silane carries out situ-formed graft combined polymerization under certain conditions, is aided with ammonium polyphosphate and flame-retardant additive to prepare collection acid source, gas
The siliceous expansion type flame retardant that source and carbon source are integrated keeps silicon substrate fire-retardant and expandable flame retardant organic unity, it is fire-retardant to play synergistic
Effect.Simultaneously as the dispersibility for being introduced into carbon material in the system of improving of organic structure, effectively increases high molecular material
Mechanical performance.
To achieve the above object, the invention provides the following technical scheme:
A kind of silicon substrate expansion type flame retardant, including following mass fraction formula components:
10-70 parts of carbon material, 20-50 parts of organosilan, 10-20 parts of ammonium polyphosphate, 3-10 parts of curing agent, flame-retardant additive 1-20
Part.
Preferably, the carbon material is one of carbon nanotube, graphene oxide, graphene, expansible graphite, graphite
Or several combinations；
The organosilan be the polysiloxanes containing methoxy group or polysilane in structure, the polysiloxanes containing hydroxyl or
The polyalkamer of polysilane, the oligo-ether of silicon methoxy group or silicon methoxy group；
The curing agent is the one or more combination of sodium hydroxide, ammonium hydroxide, triethylamine, phosphoric acid, hydrochloric acid, sulfuric acid, formic acid；
The flame-retardant additive be aluminium oxide, molybdenum phosphate, silica, glass fibre, glass microballoon, kodalk, ammonium molybdate,
Silicate or hydration silicide.
Preferably, including following mass fraction formula components:
40.5 parts of graphene oxide, three 33.8 parts of silicon methoxyl group polysilanes, 12.2 parts of ammonium polyphosphate, 5 parts of phosphoric acid, aluminium oxide 8.5
Part.
Preferably, including following mass fraction formula components:
38.3 parts of expansible graphite, two 35.6 parts of silicon methoxy based polysiloxanes, 12.5 parts of ammonium polyphosphate, 3 parts of phosphoric acid, 1 part of hydrochloric acid,
0.6 part of silica 1.
Preferably, including following mass fraction formula components:
5 parts of graphene, 30 parts of graphene oxide, 38.8 parts of hydroxy-terminated polysiloxane, 11.6 parts of ammonium polyphosphate, 6 parts of ammonium hydroxide,
8.6 parts of sodium metasilicate.
The present invention also provides a kind of preparation methods of silicon substrate expansion type flame retardant, comprising the following steps:
Carbon material dispersion liquid and organosilan are stirred, are uniformly mixed, ammonium polyphosphate and flame-retardant additive is added in sequence, is heated to
40-80 DEG C, pH value is adjusted to 3-9 with curing agent, is stirred with the speed of 200-500r/min, reacts 1-3h, solidification freezes dry
It is dry, keep cryogenic temperature, it is broken to granulate or powdered.
Preferably, the temperature of the freeze-drying is subzero 60 DEG C to subzero 10 DEG C.
Preferably, the carbon material dispersion liquid the preparation method comprises the following steps:
Dispersing agent addition ethyl alcohol is obtained into solution one, the dispersing agent accounts for the 0.1%-2% of one weight of solution, by carbon material and stabilization
Agent is added solution one and obtains solution two, and the stabilizer accounts for the 1%-5% of two weight of solution, disperses 10- with high speed disperser
20min, then disperse 10-50min with ultrasonic wave, carbon material dispersion liquid is made.
Preferably, the dispersing agent is fatty acid, fatty acyl amide, esters, paraffin class, metal soap, low-molecular-weight wax
The one or more combination of class；
The stabilizer is stearic acid, neopelex, quaternary ammonium compound, lecithin, fatty glyceride, polysorbate
One or more combination.
The beneficial effects of the present invention are:
Organosilicon alkanes flame-retardant composition and expandable flame retardant ingredient are effectively combined, organic nothing of synergistic expandable flame retardant effect is prepared for
Machine fire retardant, and have both acid source, gas source, carbon source expandable flame retardant ingredient, by the way of having abandoned traditional simple blend, effectively
The shortcomings that compensating for all kinds of flame retardance elements can be obviously improved the phase of flame retardant effect and fire retardant with high molecular material
Capacitive, and energy reinforcement mechanical strength, meanwhile, whole preparation process mildly carries out under normal pressure, and it is simple and easy, it is convenient for scale metaplasia
It produces.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Embodiment one:
A kind of silicon substrate expansion type flame retardant, including following mass fraction formula components:
40.5 parts of graphene oxide, three 33.8 parts of silicon methoxyl group polysilanes, 12.2 parts of ammonium polyphosphate, 5 parts of phosphoric acid, aluminium oxide 8.5
Part.
A kind of silicon substrate expansion type flame retardant the preparation method is as follows:
S1: preparation graphene oxide dispersion；
Fatty acid addition ethyl alcohol is obtained into solution one, the fatty acid accounts for the 0.1% of one weight of solution, by graphene oxide
Solution one is added with stearic acid and obtains solution two, the stearic acid accounts for the 1% of two weight of solution, dispersed with high speed disperser
10min, then disperse 10min with ultrasonic wave, graphene oxide dispersion is made.
S2: graphene oxide dispersion and three silicon methoxyl group polysilanes are stirred, and are uniformly mixed, and ammonium polyphosphate is added in sequence
And aluminium oxide, 40 DEG C are heated to, with phosphorus acid for adjusting pH value to 3-9, is stirred with the speed of 200r/min, 3h is reacted, solidification is subzero
60 DEG C under subzero 10 DEG C of environment, freeze-drying keeps cryogenic temperature, broken to granulate.
By thermogravimetric analysis, fire retardant decomposition starting temperature manufactured in the present embodiment is 255 DEG C, and the most fast temperature of thermal weight loss is
390 DEG C, 800 DEG C of mass excess 47%, 1000 DEG C of mass excess 44.3%.
Embodiment two:
A kind of silicon substrate expansion type flame retardant, including following mass fraction formula components:
38.3 parts of expansible graphite, two 35.6 parts of silicon methoxy based polysiloxanes, 12.5 parts of ammonium polyphosphate, 3 parts of phosphoric acid, 1 part of hydrochloric acid,
0.6 part of silica 1.
A kind of silicon substrate expansion type flame retardant the preparation method is as follows:
S1: expansible graphite dispersion liquid is prepared；
Paraffin class addition ethyl alcohol is obtained into solution one, the paraffin class accounts for the 1.2% of one weight of solution, by expansible graphite and ten
Dialkyl benzene sulfonic acids sodium is added solution one and obtains solution two, and the neopelex accounts for the 3% of two weight of solution, with height
Fast dispersion machine disperses 15min, then disperses 30min with ultrasonic wave, and expansible graphite dispersion liquid is made.
S2: expansible graphite dispersion liquid and two silicon methoxy based polysiloxanes are stirred, and are uniformly mixed, and polyphosphoric acid is added in sequence
Ammonium and silica are heated to 60 DEG C, with phosphoric acid, salt acid for adjusting pH value to 3-9, are stirred with the speed of 350r/min, react 2h,
Solidify, under subzero 60 DEG C to subzero 10 DEG C of environment, freeze-drying keeps cryogenic temperature, broken to granulate.
By thermogravimetric analysis, fire retardant decomposition starting temperature manufactured in the present embodiment is 263 DEG C, and the most fast temperature of thermal weight loss is
387 DEG C, 800 DEG C of mass excess 48.1%, 1000 DEG C of mass excess 45.3%.
Embodiment three:
A kind of silicon substrate expansion type flame retardant, including following mass fraction formula components:
5 parts of graphene, 30 parts of graphene oxide, 38.8 parts of hydroxy-terminated polysiloxane, 11.6 parts of ammonium polyphosphate, 6 parts of ammonium hydroxide,
8.6 parts of sodium metasilicate.
A kind of silicon substrate expansion type flame retardant the preparation method is as follows:
S1: graphene and graphene oxide dispersion are prepared；
By metal soap addition ethyl alcohol obtain solution one, the metal soap accounts for the 0.1%-2% of one weight of solution, by graphene,
Graphene oxide and polysorbate are added solution one and obtain solution two, and the polysorbate accounts for the 1%-5% of two weight of solution, with height
Fast dispersion machine disperses 10-20min, then disperses 10-50min with ultrasonic wave, and graphene and graphene oxide dispersion is made.
S2: graphene and graphene oxide dispersion and hydroxy-terminated polysiloxane are stirred, and are uniformly mixed, and sequence is added
Ammonium polyphosphate and sodium metasilicate are heated to 80 DEG C, adjust pH value to 3-9 with curing agent, are stirred with the speed of 500r/min, reaction
1h solidifies, and under subzero 60 DEG C to subzero 10 DEG C of environment, freeze-drying keeps cryogenic temperature, is broken into powdered.
By thermogravimetric analysis, fire retardant decomposition starting temperature manufactured in the present embodiment is 266 DEG C, and the most fast temperature of thermal weight loss is
381 DEG C, 800 DEG C of mass excess 46.8%, 1000 DEG C of mass excess 42.7%.
Example IV:
The part that the present embodiment is the same as example 1 repeats no more, unlike:
10 parts of graphene oxide, three 20 parts of silicon methoxyl group polysilanes, 10 parts of ammonium polyphosphate, 3 parts of phosphoric acid, 1 part of aluminium oxide.
Embodiment five:
The present embodiment part identical with embodiment two repeats no more, unlike: 70 parts of expansible graphite, two silicon methoxyl groups are poly-
50 parts of siloxanes, 20 parts of ammonium polyphosphate, 6 parts of phosphoric acid, 4 parts of hydrochloric acid, 20 parts of silica.
Comparative experiments:
Embodiment one to fire retardant prepared by embodiment three is respectively labeled as sample one, sample two and sample three, by above-mentioned sample
Product one, sample two, sample three are respectively added in PP plastics (polypropylene plastics) in 8% ratio, are obtained by extruding pelletization
Fire-retardant master granule, oxygen index (OI) result such as table 1.
Table 1:
| Project | Sample one | Sample two | Sample three | Polysiloxanes | Pure PP |
| Tensile strength/N | 405 | 401 | 398 | 382 | 380 |
| Oxygen index (OI)/% | 26 | 25 | 26 | 22 | 17 |
Above-mentioned experiment carries out in Qingdao University of Science and Technology laboratory
By can intuitively find out in table: fire retardant prepared by the present invention improves the flame retardant property of basis material (i.e. PP plastics)
Effect is obvious, simultaneously as the compatibility of fire retardant prepared by the present invention and basis material is improved, can effectively promote base
The intensity of body material, reinforcing effect are obvious.
In addition, it should be understood that although this specification is described in terms of embodiments, but not each embodiment is only wrapped
Containing an independent technical solution, this description of the specification is merely for the sake of clarity, and those skilled in the art should
It considers the specification as a whole, the technical solutions in the various embodiments may also be suitably combined, forms those skilled in the art
The other embodiments being understood that.
Claims (9)
1. a kind of silicon substrate expansion type flame retardant, which is characterized in that including following mass fraction formula components:
10-70 parts of carbon material, 20-50 parts of organosilan, 10-20 parts of ammonium polyphosphate, 3-10 parts of curing agent, flame-retardant additive 1-20
Part.
2. a kind of silicon substrate expansion type flame retardant according to claim 1, which is characterized in that the carbon material is carbon nanometer
The combination of one or more of pipe, graphene oxide, graphene, expansible graphite, graphite；
The organosilan be the polysiloxanes containing methoxy group or polysilane in structure, the polysiloxanes containing hydroxyl or
The polyalkamer of polysilane, the oligo-ether of silicon methoxy group or silicon methoxy group；
The curing agent is the one or more combination of sodium hydroxide, ammonium hydroxide, triethylamine, phosphoric acid, hydrochloric acid, sulfuric acid, formic acid；
The flame-retardant additive be aluminium oxide, molybdenum phosphate, silica, glass fibre, glass microballoon, kodalk, ammonium molybdate,
Silicate or hydration silicide.
3. a kind of silicon substrate expansion type flame retardant according to claim 2, which is characterized in that including following mass fraction formula
Ingredient:
40.5 parts of graphene oxide, three 33.8 parts of silicon methoxyl group polysilanes, 12.2 parts of ammonium polyphosphate, 5 parts of phosphoric acid, aluminium oxide 8.5
Part.
4. a kind of silicon substrate expansion type flame retardant according to claim 2, which is characterized in that including following mass fraction formula
Ingredient:
38.3 parts of expansible graphite, two 35.6 parts of silicon methoxy based polysiloxanes, 12.5 parts of ammonium polyphosphate, 3 parts of phosphoric acid, 1 part of hydrochloric acid,
0.6 part of silica 1.
5. a kind of silicon substrate expansion type flame retardant according to claim 2, which is characterized in that including following mass fraction formula
Ingredient:
5 parts of graphene, 30 parts of graphene oxide, 38.8 parts of hydroxy-terminated polysiloxane, 11.6 parts of ammonium polyphosphate, 6 parts of ammonium hydroxide,
8.6 parts of sodium metasilicate.
6. a kind of method for preparing silicon substrate expansion type flame retardant a method as claimed in any one of claims 1 to 5, which is characterized in that including such as
Lower step:
Carbon material dispersion liquid and organosilan are stirred, are uniformly mixed, ammonium polyphosphate and flame-retardant additive is added in sequence, is heated to
40-80 DEG C, pH value is adjusted to 3-9 with curing agent, is stirred with the speed of 200-500r/min, reacts 1-3h, solidification freezes dry
It is dry, keep cryogenic temperature, it is broken to granulate or powdered.
7. preparation method according to claim 6, which is characterized in that the temperature of the freeze-drying is subzero 60 DEG C to zero
Lower 10 DEG C.
8. preparation method according to claim 7, which is characterized in that the carbon material dispersion liquid the preparation method comprises the following steps:
Dispersing agent addition ethyl alcohol is obtained into solution one, the dispersing agent accounts for the 0.1%-2% of one weight of solution, by carbon material and stabilization
Agent is added solution one and obtains solution two, and the stabilizer accounts for the 1%-5% of two weight of solution, disperses 10- with high speed disperser
20min, then disperse 10-50min with ultrasonic wave, carbon material dispersion liquid is made.
9. preparation method according to claim 8, which is characterized in that the dispersing agent be fatty acid, fatty acyl amide,
Esters, paraffin class, metal soap, low molecule wax class one or more combination；
The stabilizer is stearic acid, neopelex, quaternary ammonium compound, lecithin, fatty glyceride, polysorbate
One or more combination.
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| CN114685848A (en) * | 2020-12-29 | 2022-07-01 | 洛阳尖端技术研究院 | Intumescent flame retardant, plastic and preparation method and application thereof |
| CN115260767A (en) * | 2022-08-05 | 2022-11-01 | 廖颖 | Flame-retardant high-temperature vulcanized silicone rubber and preparation method thereof |
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| CN107383599A (en) * | 2017-07-28 | 2017-11-24 | 江苏长海复合材料股份有限公司 | A kind of environment protective and flame-retardant polypropelene material and preparation method thereof |
| CN109265787A (en) * | 2018-06-27 | 2019-01-25 | 福建师范大学 | A kind of preparation method for the expansible graphite flame-retardant ultra-high molecular weight polyvinyl coating silicone resin |
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| US20090215926A1 (en) * | 2005-09-01 | 2009-08-27 | Instytut Wlokien Naturalnych | Intumescent Fire Retardant and the Method of its Manufacture |
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| CN114685848A (en) * | 2020-12-29 | 2022-07-01 | 洛阳尖端技术研究院 | Intumescent flame retardant, plastic and preparation method and application thereof |
| CN115260767A (en) * | 2022-08-05 | 2022-11-01 | 廖颖 | Flame-retardant high-temperature vulcanized silicone rubber and preparation method thereof |
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