CN106751873A - A kind of fire retardant containing fire-resistant synergistic composition and preparation method thereof - Google Patents
A kind of fire retardant containing fire-resistant synergistic composition and preparation method thereof Download PDFInfo
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- CN106751873A CN106751873A CN201710067136.8A CN201710067136A CN106751873A CN 106751873 A CN106751873 A CN 106751873A CN 201710067136 A CN201710067136 A CN 201710067136A CN 106751873 A CN106751873 A CN 106751873A
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- 230000002195 synergetic effect Effects 0.000 title claims abstract description 71
- 239000000203 mixture Substances 0.000 title claims abstract description 70
- 230000009970 fire resistant effect Effects 0.000 title claims abstract description 64
- 239000003063 flame retardant Substances 0.000 title claims abstract description 63
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910000077 silane Inorganic materials 0.000 claims abstract description 27
- 239000002699 waste material Substances 0.000 claims abstract description 23
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 14
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 239000004721 Polyphenylene oxide Substances 0.000 claims abstract description 10
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims abstract description 10
- 239000003921 oil Substances 0.000 claims abstract description 10
- 229920000570 polyether Polymers 0.000 claims abstract description 10
- 150000003376 silicon Chemical class 0.000 claims abstract description 10
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 21
- 238000001914 filtration Methods 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 13
- 239000002808 molecular sieve Substances 0.000 claims description 11
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000007795 chemical reaction product Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- 238000002525 ultrasonication Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000003809 water extraction Methods 0.000 claims description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims 1
- 238000009210 therapy by ultrasound Methods 0.000 claims 1
- -1 polypropylene Polymers 0.000 abstract description 18
- 239000004743 Polypropylene Substances 0.000 abstract description 16
- 229920001155 polypropylene Polymers 0.000 abstract description 16
- 239000000463 material Substances 0.000 abstract description 14
- 230000002209 hydrophobic effect Effects 0.000 abstract description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 abstract description 6
- 239000001301 oxygen Substances 0.000 abstract description 6
- 239000000779 smoke Substances 0.000 abstract description 4
- 238000005452 bending Methods 0.000 abstract description 3
- 229920000642 polymer Polymers 0.000 description 11
- 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 10
- WXZMFSXDPGVJKK-UHFFFAOYSA-N pentaerythritol Chemical compound OCC(CO)(CO)CO WXZMFSXDPGVJKK-UHFFFAOYSA-N 0.000 description 8
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 description 7
- 239000006227 byproduct Substances 0.000 description 7
- 238000001354 calcination Methods 0.000 description 7
- 238000002485 combustion reaction Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 239000000047 product Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 235000019504 cigarettes Nutrition 0.000 description 3
- 229910052901 montmorillonite Inorganic materials 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- YUWBVKYVJWNVLE-UHFFFAOYSA-N [N].[P] Chemical compound [N].[P] YUWBVKYVJWNVLE-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000011156 evaluation Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000001629 suppression Effects 0.000 description 2
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 description 2
- 206010020741 Hyperpyrexia Diseases 0.000 description 1
- MKYBYDHXWVHEJW-UHFFFAOYSA-N N-[1-oxo-1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propan-2-yl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(C(C)NC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 MKYBYDHXWVHEJW-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004079 fireproofing Methods 0.000 description 1
- 239000012757 flame retardant agent Substances 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of fire retardant containing fire-resistant synergistic composition and preparation method thereof, the fire retardant containing fire-resistant synergistic composition is according to the raw material of weight portion：10 20 parts of 20 40 parts of organic silicon rubber waste material, melamine and/or cdicynanmide, 15 parts of silane coupler, 5 15 parts of highly basic, 80 120 parts of alcohol, 30 50 parts of water, 1 10 parts of fire-resistant synergistic composition；The fire-resistant synergistic composition is according to the component of weight portion：46 parts of CNT, 46 parts of nano mesoporous molecular screen, 46 parts of polyether modified silicon oil, 13 parts of nanometer silicon carbide, 13 parts of nano aluminum nitride.Hydrophobic performance of the present invention very well, may be such that polyacrylic fire resistance is significantly improved, and fire resistance reaches 0 grade of 94 V of UL, and limited oxygen index is up to more than 39%.In addition, smoke situation and drippage situation when polypropylene is burnt, and material mechanical property (tensile strength, bending strength and impact strength) also be improved significantly.
Description
The application is application number 2015103925390, the applying date 2015 year 07 month 06, " one kind is containing fire-retardant for denomination of invention
The divisional application of fire retardant of synergistic composition and preparation method thereof ".
Technical field
The present invention relates to the recycling field of organic silicon rubber waste material, specifically a kind of resistance containing fire-resistant synergistic composition
Combustion agent and preparation method thereof.
Background technology
Organic silicon rubber is due to the flexion of prominent resistance to elevated temperatures, inoxidizability, resistance to ag(e)ing, weatherability and low temperature
Property, its range of application is more and more extensive.But, its expensive raw material price, and always there is waste material to occur in machine-shaping and application.
These waste materials are because by high temperature vulcanized, strand is cross-linked with each other, therefore is unable to natural degradation；If do not dealt carefully with, can be tight
Heavily contaminated environment.At present, how to reclaim waste material and rationally utilize it once again, people is attract with the sustainable development for realizing resource
Sight.
Current macromolecular material high polymer is widely used in industrial production and daily life.Most of macromolecular materials
High polymer is all inflammable, and leading position is occupied in flammable solid fire.Therefore flame retardant type macromolecular material high polymer into
It is a primary study direction of Material Field, additive flame retardant is the most widely used at present.At present, additive flame retardant
Agent year usage amount more than 1,000,000 tons.Wherein：(1) although inorganic combustion inhibitor such as magnesium hydroxide and aluminium hydroxide have resistance simultaneously
Toxic gas and corrosive gas are not produced when combustion and the effect of suppression cigarette and burning, but are had a strong impact on because required addition is larger
By the physics of fire proofing, mechanical performance and processing characteristics.(2) although organic halogenated flame retardant has high fire-retardance efficiency and property high
The features such as valency ratio, but because its HX for playing fire retardation is poisonous corrosive gas, it is harmful to environment and human body, therefore its application
Field has been restricted, and oneself is gradually eliminated.(3) halogen-free flame retardants (IFR) has the advantages that low cigarette, nontoxic, IFR with phosphorus, nitrogen,
Carbon is main core ingredient, and cooperative flame retardant effect can be produced when being heated；The IFR of compounding is acid generally with APP (APP)
Source, with melamine and/or cdicynanmide (MEL) as foaming agent, with pentaerythrite (PER) as carbon forming agent, can generate during by hyperpyrexia
The carbonaceous froth bed of even compact, can heat-insulated, oxygen barrier, suppression cigarette, anti-molten drop, with good fire resistance；But the based flame retardant
It is mostly hydrophilic, and polymer base poor compatibility, and required addition is larger, have impact on flame retarded polymeric material high poly-
The physical property of thing, therefore the demand of macromolecular material can not be met.(4) organic silicon fibre retardant is the one kind for developing in recent years
New and effective, low toxicity, anti-molten drop, environment-friendly halogen-free flame retardants, are also a kind of charcoal becoming smoke suppressant.Organic silicon fibre retardant exists
Assign outside the excellent fire resistance of base material, moreover it is possible to improve processing characteristics, heat resistance of base material etc.；But because expensive, answer
With also by a definite limitation.
According to Britain《Depolymerization and stabilization》(Polymer DegradationandStability,90:523-534,
2005) introduce, addition account for system gross mass 40% by melamine and/or cdicynanmide ammonium sulfate and pentaerythrite constitute it is swollen
Polypropylene flame redardant obtained by swollen fire retardant can be only achieved UL-94V0 ranks, but because the total amount of addition expanding fire retardant is larger
The mechanical property such as tensile strength of material and fracture strength can be caused to decline.
According to the U.S.《Polymer science magazine》(Journal of Polymer Science,part A:Ploymer
chemistry 42:6163-6173,2004) introduce, during by organo montmorillonite and expansion type flame retardant synergistic polypropylene flame redardant,
When it is 4% that organo montmorillonite quality accounts for system gross mass percentage composition ratio, the heat release of polypropylene flame redardant can be substantially reduced
Speed；But the increase (after 4%) with organo montmorillonite content aggravates because reuniting, and its flame retardant effect declines on the contrary.
In addition, existing use melt-blending process is obtained contains nitrogen-phosphorus expansion fire retardant or fire-retardant containing nitrogen-phosphorus expansion
Although the flame-retardant polymer of agent and retardant synergist has the characteristic such as LSZH and resistance to dissolved drip, flame retardant effect is still not enough managed
Think, resistance to dissolved drip need to be improved, also because the flame retardant amount of required addition is larger the mechanical property of material can be made as strong in stretched
Degree, fracture strength decline, and production cost is higher.
The content of the invention
Macromolecular material high polymer is not influenceed it is an object of the invention to provide a kind of cheap, environmental protection, good flame retardation effect and
Fire retardant containing fire-resistant synergistic composition of mechanical property and preparation method thereof.
To achieve the above object, the present invention provides following technical scheme：
A kind of fire retardant containing fire-resistant synergistic composition, be according to the raw material of weight portion：Organic silicon rubber waste material 20-40
Part, melamine and/or cdicynanmide 10-20 parts, silane coupler 1-5 parts, highly basic 5-15 parts, alcohol 80-120 parts, water 30-50
Part, 1-10 parts of fire-resistant synergistic composition；The fire-resistant synergistic composition is according to the component of weight portion：CNT 4-6 parts, receive
4-6 parts, polyether modified silicon oil 4-6 parts, nanometer silicon carbide 1-3 parts, nano aluminum nitride 1-3 parts of mesopore molecular sieve of rice.
As further scheme of the invention：The fire retardant containing fire-resistant synergistic composition, according to the raw material of weight portion
For：25-35 parts of organic silicon rubber waste material, melamine and/or cdicynanmide 14-16 parts, silane coupler 2-4 parts, highly basic 8-12
Part, alcohol 90-110 parts, water 35-45 parts, 4-6 parts of fire-resistant synergistic composition.
As further scheme of the invention：The fire-resistant synergistic composition is according to the component of weight portion：CNT 5
Part, 5 parts of nano mesoporous molecular screen, 5 parts of polyether modified silicon oil, 2 parts of nanometer silicon carbide, 2 parts of nano aluminum nitride.
As further scheme of the invention：The silane coupler is KH550 silane couplers, KH560 silane coupled
Any one or more in agent and KH570 silane couplers.
As further scheme of the invention：The highly basic is NaOH and/or potassium hydroxide.
As further scheme of the invention：The carbon number of the alcohol is 2-6.
As further scheme of the invention：The nano mesoporous molecular screen is MCM-41 mesopore molecular sieves, MCM-48 Jie
Any one or more in porous molecular sieve, SBA-15 mesopore molecular sieves and SBA-16 mesopore molecular sieves.
A kind of preparation method of the fire retardant containing fire-resistant synergistic composition, concretely comprises the following steps：
(1) organic silicon rubber waste material is first ground into the particle diameter no more than particle of 2mm, then with silane coupler, highly basic
Reactor is added together with alcohol, and under stirring, heating using microwave is incubated 1-3 hours to 30-80 DEG C；The heating using microwave
Power is 0.8-1.2kW, and frequency is 1200-3600MHz；
(2) add water extraction after filtering, and standing separation is removed layer liquid and is placed in reactor；
(3) again to melamine and/or cdicynanmide and fire-resistant synergistic composition is added in reactor, under stirring,
It is ultrasonically treated 0.5-1.5 hours；The power of the ultrasonication is 150-250W, and frequency is 20-40kHz；
(4) cool down, filtering, washing reaction product, after drying, that is, obtain the fire retardant containing fire-resistant synergistic composition.
As further scheme of the invention：Heating using microwave is incubated 1.5-2.5 hours to 40-60 DEG C in step (1)；Institute
The power of heating using microwave is stated for 0.9-1.1kW, frequency is 2000-2800MHz.
As further scheme of the invention：It is ultrasonically treated 0.8-1.2 hours in step (3)；The ultrasonication
Power is 180-220W, and frequency is 25-35kHz.
Compared with prior art, the beneficial effects of the invention are as follows：
Fire retardant hydrophobic performance of the present invention containing fire-resistant synergistic composition very well, is added in polypropylene, may be such that poly- third
The fire resistance of alkene is significantly improved, and fire resistance reaches UL-94V-0 grades, and limited oxygen index is up to more than 39%.In addition, may be used also
Smoke situation and drippage situation when polypropylene is burnt, and material mechanical property (tensile strength, bending strength and impact
Intensity) also be improved significantly.
Specific embodiment
The technical scheme of this patent is described in more detail with reference to specific embodiment.
Embodiment 1
A kind of fire retardant containing fire-resistant synergistic composition, be according to the raw material of weight portion：20 parts of organic silicon rubber waste material, three
Poly cyanamid and/or 10 parts of cdicynanmide, 1 part of KH550 silane couplers, 5 parts of NaOH, 80 parts of ethanol, 30 parts of water, fire-resistant synergistic
1 part of composition；The fire-resistant synergistic composition is according to the component of weight portion：4 parts of CNT, MCM-41 mesopore molecular sieves 4
Part, 4 parts of polyether modified silicon oil, 1 part of nanometer silicon carbide, 1 part of nano aluminum nitride.
The preparation method of the fire retardant containing fire-resistant synergistic composition, concretely comprises the following steps：
(1) organic silicon rubber waste material is first ground into the particle diameter no more than particle of 2mm, then with silane coupler, highly basic
Reactor is added together with unit alcohol, and under stirring, heating using microwave is incubated 3 hours to 30 DEG C；The work(of the heating using microwave
Rate is 0.8kW, and frequency is 1200MHz；
(2) add water extraction after filtering, and standing separation is removed layer liquid and is placed in reactor；
(3) again to melamine and/or cdicynanmide and fire-resistant synergistic composition is added in reactor, under stirring,
Ultrasonically treated 1.5 hours；The power of the ultrasonication is 150W, and frequency is 20kHz；
(4) cool down, filtering, washing reaction product, after drying, that is, obtain the fire retardant containing fire-resistant synergistic composition.
The present embodiment product yield is 92.7%；300 DEG C of calcinations 30 minutes in Muffle furnace, weightless 1.48%, by product
Do not sink within one week in placement water, illustrate that hydrophobic performance is fine.
Embodiment 2
A kind of fire retardant containing fire-resistant synergistic composition, be according to the raw material of weight portion：30 parts of organic silicon rubber waste material, three
Poly cyanamid and/or 15 parts of cdicynanmide, 3 parts of KH560 silane couplers, 10 parts of potassium hydroxide, 100 parts of pentaerythrite, 40 parts of water, resistance
5 parts of synergistic composition of combustion；The fire-resistant synergistic composition is according to the component of weight portion：5 parts of CNT, mesoporous point of MCM-48
5 parts of son sieve, 5 parts of polyether modified silicon oil, 2 parts of nanometer silicon carbide, 2 parts of nano aluminum nitride.
The preparation method of the fire retardant containing fire-resistant synergistic composition, concretely comprises the following steps：
(1) organic silicon rubber waste material is first ground into the particle diameter no more than particle of 2mm, then with silane coupler, highly basic
Reactor is added together with unit alcohol, and under stirring, heating using microwave is incubated 2 hours to 60 DEG C；The work(of the heating using microwave
Rate is 1kW, and frequency is 2400MHz；
(2) add water extraction after filtering, and standing separation is removed layer liquid and is placed in reactor；
(3) again to melamine and/or cdicynanmide and fire-resistant synergistic composition is added in reactor, under stirring,
Ultrasonically treated 1 hour；The power of the ultrasonication is 200W, and frequency is 30kHz；
(4) cool down, filtering, washing reaction product, after drying, that is, obtain the fire retardant containing fire-resistant synergistic composition.
The present embodiment product yield is 93.7%；300 DEG C of calcinations 30 minutes in Muffle furnace, weightless 1.17%, by product
Do not sink within one week in placement water, illustrate that hydrophobic performance is fine.
Embodiment 3
A kind of fire retardant containing fire-resistant synergistic composition, be according to the raw material of weight portion：40 parts of organic silicon rubber waste material, three
Poly cyanamid and/or 20 parts of cdicynanmide, 5 parts of KH570 silane couplers, 15 parts of highly basic, 120 parts of ethanol, 50 parts of water, fire-resistant synergistic group
10 parts of compound；The fire-resistant synergistic composition is according to the component of weight portion：6 parts of CNT, SBA-16 mesopore molecular sieves 6
Part, 6 parts of polyether modified silicon oil, 3 parts of nanometer silicon carbide, 3 parts of nano aluminum nitride.
The preparation method of the fire retardant containing fire-resistant synergistic composition, concretely comprises the following steps：
(1) organic silicon rubber waste material is first ground into the particle diameter no more than particle of 2mm, then with silane coupler, highly basic
Reactor is added together with unit alcohol, and under stirring, heating using microwave is incubated 1 hour to 80 DEG C；The work(of the heating using microwave
Rate is 1.2kW, and frequency is 3600MHz；
(2) add water extraction after filtering, and standing separation is removed layer liquid and is placed in reactor；
(3) again to melamine and/or cdicynanmide and fire-resistant synergistic composition is added in reactor, under stirring,
Ultrasonically treated 1.5 hours；The power of the ultrasonication is 250W, and frequency is 40kHz；
(4) cool down, filtering, washing reaction product, after drying, that is, obtain the fire retardant containing fire-resistant synergistic composition.
The present embodiment product yield is 92.9%；300 DEG C of calcinations 30 minutes in Muffle furnace, weightless 1.24%, by product
Do not sink within one week in placement water, illustrate that hydrophobic performance is fine.
Comparative example 1
A kind of fire retardant containing fire-resistant synergistic composition, be according to the raw material of weight portion：30 parts of organic silicon rubber waste material, three
Poly cyanamid and/or 15 parts of cdicynanmide, 3 parts of KH560 silane couplers, 10 parts of potassium hydroxide, 100 parts of pentaerythrite, 40 parts of water.
The preparation method of the fire retardant containing fire-resistant synergistic composition, concretely comprises the following steps：
(1) organic silicon rubber waste material is first ground into the particle diameter no more than particle of 2mm, then with silane coupler, highly basic
Reactor is added together with unit alcohol, and under stirring, heating using microwave is incubated 2 hours to 60 DEG C；The work(of the heating using microwave
Rate is 1kW, and frequency is 2400MHz；
(2) add water extraction after filtering, and standing separation is removed layer liquid and is placed in reactor；
(3) again to addition melamine and/or cdicynanmide in reactor, under stirring, ultrasonically treated 1 hour；Institute
The power of ultrasonication is stated for 200W, frequency is 30kHz；
(4) cool down, filtering, washing reaction product, after drying, that is, obtain the fire retardant containing fire-resistant synergistic composition.
The present embodiment product yield is 86.2%；300 DEG C of calcinations 30 minutes in Muffle furnace, weightless 4.55%, by product
Do not sink within one week in placement water, illustrate that hydrophobic performance is fine.
Comparative example 2
A kind of fire retardant containing fire-resistant synergistic composition, be according to the raw material of weight portion：30 parts of organic silicon rubber waste material, three
Poly cyanamid and/or 15 parts of cdicynanmide, 3 parts of KH560 silane couplers, 10 parts of potassium hydroxide, 100 parts of pentaerythrite, 40 parts of water, resistance
5 parts of synergistic composition of combustion；The fire-resistant synergistic composition is according to the component of weight portion：5 parts of CNT, mesoporous point of MCM-48
5 parts of son sieve.The preparation method of the fire retardant containing fire-resistant synergistic composition, with embodiment 2.
The present embodiment product yield is 89.3%；300 DEG C of calcinations 30 minutes in Muffle furnace, weightless 2.41%, by product
Do not sink within one week in placement water, illustrate that hydrophobic performance is fine.
Comparative example 3
A kind of fire retardant containing fire-resistant synergistic composition, be according to the raw material of weight portion：30 parts of organic silicon rubber waste material, three
Poly cyanamid and/or 15 parts of cdicynanmide, 3 parts of KH560 silane couplers, 10 parts of potassium hydroxide, 100 parts of pentaerythrite, 40 parts of water, resistance
5 parts of synergistic composition of combustion；The fire-resistant synergistic composition is according to the component of weight portion：5 parts of polyether modified silicon oil, nano silicon carbide
3 parts of silicon, 3 parts of nano aluminum nitride.The preparation method of the fire retardant containing fire-resistant synergistic composition, with embodiment 2.
The present embodiment product yield is 90.1%；300 DEG C of calcinations 30 minutes in Muffle furnace, weightless 2.26%, by product
Do not sink within one week in placement water, illustrate that hydrophobic performance is fine.
Comparative example 4
A kind of fire retardant containing fire-resistant synergistic composition, be according to the raw material of weight portion：30 parts of organic silicon rubber waste material, three
Poly cyanamid and/or 15 parts of cdicynanmide, 3 parts of KH560 silane couplers, 10 parts of potassium hydroxide, 100 parts of pentaerythrite, 40 parts of water, resistance
5 parts of synergistic composition of combustion；The fire-resistant synergistic composition is according to the component of weight portion：5 parts of CNT, mesoporous point of MCM-48
5 parts of son sieve, 5 parts of polyether modified silicon oil, 2 parts of nanometer silicon carbide, 2 parts of nano aluminum nitride.
The preparation method of the fire retardant containing fire-resistant synergistic composition, concretely comprises the following steps：
(1) organic silicon rubber waste material is first ground into the particle diameter no more than particle of 2mm, then with silane coupler, highly basic
Reactor is added together with unit alcohol, under stirring, 60 DEG C is electrically heated to, and is incubated 2 hours；
(2) add water extraction after filtering, and standing separation is removed layer liquid and is placed in reactor；
(3) stirred 2 hours to melamine and/or cdicynanmide and fire-resistant synergistic composition is added in reactor again；
(4) cool down, filtering, washing reaction product, after drying, that is, obtain the fire retardant containing fire-resistant synergistic composition.
The present embodiment product yield is 89.8%；300 DEG C of calcinations 30 minutes in Muffle furnace, weightless 2.83%, by product
Do not sink within one week in placement water, illustrate that hydrophobic performance is fine.
Application examples
Fire retardant prepared by embodiment and comparative example is added in high polymer polypropylene (PP), and be not added with fire retardant
High polymer polypropylene contrasted.Preparation method of sample is：20 weight portion above-described embodiments are respectively adopted and are prepared by comparative example
Fire retardant and 75 parts by weight of polypropylene and 5 parts by weight of maleic with grafting polypropylene fusion blending, that is, obtain polypropylene flame redardant.
Then the polypropylene flame redardant is dried into rear fender, cut into 130mm × 13mm × 3mm and 130mm × 6.5mm ×
The standard batten of 3mm, carries out UL-94 and vertically fires by ASTM D635-77 standards on CZF-3 types horizontal vertical burning analyzer
Burn test；Limited oxygen index is pressed ASTM D2863-77 standards and is tested on HC-2 type oxygen index instruments；According to CNS pair
Other physical properties are tested；Its evaluation result is as shown in table 1.
The polypropylene flame redardant evaluation result of table 1
As it can be seen from table 1 the polypropylene flame redardant of the fire retardant of addition embodiment 1-3 preparations has good anti-flammability,
May be such that polyacrylic fire resistance is significantly improved, fire resistance reaches UL-94V-0 grades, and limited oxygen index is up to more than 39%；
Its anti-flammability is significantly better than fire retardant prepared by addition comparative example 1-4.In addition, smoke situation and drippage feelings when polypropylene burns
Condition, and the mechanical property (tensile strength, bending strength and impact strength) of material is also obviously improved.
The better embodiment to this patent is explained in detail above, but this patent is not limited to above-mentioned embodiment party
Formula, in the ken that one skilled in the relevant art possesses, can also be on the premise of this patent objective not be departed from
Make a variety of changes.
Claims (7)
1. a kind of preparation method of the fire retardant containing fire-resistant synergistic composition, it is characterised in that the composition containing fire-resistant synergistic
Fire retardant, be according to the raw material of weight portion：20-40 parts of organic silicon rubber waste material, melamine and/or cdicynanmide 10-20 parts,
Silane coupler 1-5 parts, highly basic 5-15 parts, alcohol 80-120 parts, water 30-50 parts, 1-10 parts of fire-resistant synergistic composition；It is described fire-retardant
Synergistic composition is according to the component of weight portion：CNT 4-6 parts, nano mesoporous molecular screen 4-6 parts, polyether modified silicon oil 4-
6 parts, nanometer silicon carbide 1-3 parts, nano aluminum nitride 1-3 parts；The preparation method of the described fire retardant containing fire-resistant synergistic composition,
Concretely comprise the following steps：
（1）Organic silicon rubber waste material is first ground into the particle diameter no more than particle of 2mm, then with silane coupler, highly basic and alcohol
Reactor is added together, and under stirring, heating using microwave is incubated 1-3 hours to 30-80 DEG C；The power of the heating using microwave
It is 0.8-1.2kW, frequency is 1200-3600MHz；
（2）Add water extraction after filtering, standing separation, removes layer liquid and is placed in reactor；
（3）Again to melamine and/or cdicynanmide and fire-resistant synergistic composition is added in reactor, under stirring, ultrasound
Treatment 0.5-1.5 hours；The power of the ultrasonication is 150-250W, and frequency is 20-40kHz；
（4）Cooling, filtering, washing reaction product after drying, that is, obtains the fire retardant containing fire-resistant synergistic composition.
2. the preparation method of the fire retardant containing fire-resistant synergistic composition according to claim 1, it is characterised in that described to contain
The fire retardant of fire-resistant synergistic composition, be according to the raw material of weight portion：25-35 parts of organic silicon rubber waste material, melamine and/or
Cdicynanmide 14-16 parts, silane coupler 2-4 parts, highly basic 8-12 parts, alcohol 90-110 parts, water 35-45 parts, fire-resistant synergistic composition
4-6 parts.
3. the preparation method of the fire retardant containing fire-resistant synergistic composition according to claim 1 and 2, it is characterised in that institute
State fire-resistant synergistic composition is according to the component of weight portion：5 parts of CNT, 5 parts of nano mesoporous molecular screen, polyether modified silicon oil
5 parts, 2 parts of nanometer silicon carbide, 2 parts of nano aluminum nitride.
4. the preparation method of the fire retardant containing fire-resistant synergistic composition according to claim 1 and 2, it is characterised in that institute
State silane coupler be in KH550 silane couplers, KH560 silane couplers and KH570 silane couplers any one or
It is various.
5. the preparation method of the fire retardant containing fire-resistant synergistic composition according to claim 1 and 2, it is characterised in that institute
Highly basic is stated for NaOH and/or potassium hydroxide.
6. the preparation method of the fire retardant containing fire-resistant synergistic composition according to claim 1 and 2, it is characterised in that institute
It is 2-6 to state the carbon number of alcohol.
7. the preparation method of the fire retardant containing fire-resistant synergistic composition according to claim 1 and 2, it is characterised in that institute
Nano mesoporous molecular screen is stated for MCM-41 mesopore molecular sieves, MCM-48 mesopore molecular sieves, SBA-15 mesopore molecular sieves and SBA-16
Any one or more in mesopore molecular sieve.
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| CN105139925A (en) * | 2015-09-23 | 2015-12-09 | 陈薇 | Fireproof type Internet of Things bus cable and preparation method thereof |
| CN105139948A (en) * | 2015-09-23 | 2015-12-09 | 陈薇 | Fireproof integrated bus of cables, optical cables and data cables and preparation method thereof |
| CN105139955A (en) * | 2015-09-23 | 2015-12-09 | 陈薇 | Photoelectric data integrated bus cable and preparation method thereof |
| CN105118560A (en) * | 2015-09-23 | 2015-12-02 | 陈薇 | Fire resistance type photoelectric data bus cable and preparation method thereof |
| CN105206322A (en) * | 2015-09-28 | 2015-12-30 | 安徽华星电缆集团有限公司 | High-temperature-prevention fire-resistant cable for computer |
| CN105206347A (en) * | 2015-09-28 | 2015-12-30 | 安徽神州缆业集团有限公司 | Fire-resistant and high-temperature-resistant communication cable |
| CN108841322B (en) * | 2018-07-10 | 2020-05-19 | 武汉露能科技有限公司 | Low surface energy coating and preparation method thereof |
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| FR2901799B1 (en) * | 2006-06-02 | 2008-08-01 | Arkema France | HIGH THERMOMECHANICAL, FALSE-FREE THERMOPLASTIC THERMOPLASTIC COMPOSITIONS WITHOUT HALOGEN |
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| CN104693580A (en) * | 2015-03-18 | 2015-06-10 | 苏州安鸿泰新材料有限公司 | Halogen-free flame-retardant masterbatch for ethylene-propylene-diene monomer and preparation method of halogen-free flame-retardant masterbatch |
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