CN105601991B - Application of the aluminate material as fire retardant in flame retardant thermoplastic - Google Patents
Application of the aluminate material as fire retardant in flame retardant thermoplastic Download PDFInfo
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 98
- 229920001169 thermoplastic Polymers 0.000 title claims abstract description 58
- 239000004416 thermosoftening plastic Substances 0.000 title claims abstract description 54
- 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 52
- 239000000463 material Substances 0.000 title claims description 16
- 150000004645 aluminates Chemical class 0.000 title description 49
- -1 aluminate compound Chemical class 0.000 claims abstract description 75
- 238000000034 method Methods 0.000 claims abstract description 8
- 239000004594 Masterbatch (MB) Substances 0.000 claims description 36
- 238000002360 preparation method Methods 0.000 claims description 34
- 239000005038 ethylene vinyl acetate Substances 0.000 claims description 27
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims description 27
- 238000002156 mixing Methods 0.000 claims description 26
- 238000002844 melting Methods 0.000 claims description 24
- 230000008018 melting Effects 0.000 claims description 24
- 238000011056 performance test Methods 0.000 claims description 17
- DQXBYHZEEUGOBF-UHFFFAOYSA-N but-3-enoic acid;ethene Chemical compound C=C.OC(=O)CC=C DQXBYHZEEUGOBF-UHFFFAOYSA-N 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 3
- 239000011159 matrix material Substances 0.000 abstract description 8
- 239000002105 nanoparticle Substances 0.000 abstract description 7
- 229920000642 polymer Polymers 0.000 abstract description 7
- 235000019504 cigarettes Nutrition 0.000 abstract description 6
- 229910052809 inorganic oxide Inorganic materials 0.000 abstract description 6
- 238000001556 precipitation Methods 0.000 abstract description 3
- 239000000779 smoke Substances 0.000 abstract description 3
- 238000013508 migration Methods 0.000 abstract description 2
- 230000005012 migration Effects 0.000 abstract description 2
- 239000002243 precursor Substances 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002131 composite material Substances 0.000 description 62
- 239000007822 coupling agent Substances 0.000 description 44
- 239000004743 Polypropylene Substances 0.000 description 29
- 229920001155 polypropylene Polymers 0.000 description 29
- 238000004786 cone calorimetry Methods 0.000 description 18
- 238000001514 detection method Methods 0.000 description 18
- 239000004433 Thermoplastic polyurethane Substances 0.000 description 14
- 229920001971 elastomer Polymers 0.000 description 14
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 14
- 239000000806 elastomer Substances 0.000 description 13
- 229920001038 ethylene copolymer Polymers 0.000 description 11
- JTXMVXSTHSMVQF-UHFFFAOYSA-N 2-acetyloxyethyl acetate Chemical compound CC(=O)OCCOC(C)=O JTXMVXSTHSMVQF-UHFFFAOYSA-N 0.000 description 10
- 229920002635 polyurethane Polymers 0.000 description 8
- 239000004814 polyurethane Substances 0.000 description 8
- 229920003023 plastic Polymers 0.000 description 6
- 239000004033 plastic Substances 0.000 description 6
- 238000002485 combustion reaction Methods 0.000 description 5
- 235000013339 cereals Nutrition 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 150000001336 alkenes Chemical class 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 3
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 3
- 239000000347 magnesium hydroxide Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229920006311 Urethane elastomer Polymers 0.000 description 2
- ADCOVFLJGNWWNZ-UHFFFAOYSA-N antimony trioxide Chemical compound O=[Sb]O[Sb]=O ADCOVFLJGNWWNZ-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229920003225 polyurethane elastomer Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 229940117958 vinyl acetate Drugs 0.000 description 2
- 229910000951 Aluminide Inorganic materials 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 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
- RJZNFXWQRHAVBP-UHFFFAOYSA-I aluminum;magnesium;pentahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Al+3] RJZNFXWQRHAVBP-UHFFFAOYSA-I 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000000413 hydrolysate Substances 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 231100001231 less toxic Toxicity 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229920006113 non-polar polymer Polymers 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000000979 retarding effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 239000012815 thermoplastic material Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 description 1
- 230000010148 water-pollination Effects 0.000 description 1
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- 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
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/20—Compounding polymers with additives, e.g. colouring
- C08J3/22—Compounding polymers with additives, e.g. colouring using masterbatch techniques
- C08J3/223—Packed additives
-
- 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
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0846—Copolymers of ethene with unsaturated hydrocarbons containing other atoms than carbon or hydrogen atoms
- C08L23/0853—Vinylacetate
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- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/08—Copolymers of ethene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/10—Homopolymers or copolymers of propene
- C08J2323/12—Polypropene
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- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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- C08K2201/00—Specific properties of additives
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- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The invention discloses application of the aluminate compound as fire retardant in flame retardant thermoplastic, aluminate compound well can be dispersed in polymeric matrix as nano inorganic oxide presoma, when running into the moisture in air, nano inorganic oxide is generated in polymer molecule segment reclaimed water solution, inierpeneirating network structure is formed with polymeric matrix, compared with being directly added into nano-particle oxide, this method for adding inorganic oxide precursor body effectively reduces reunion, migration and precipitation of the nano-particle in polymeric matrix.The flame retardant thermoplastic prepared using aluminate compound as fire retardant, HRR, total heat release, raw cigarette speed, always raw smoke, the cigarette factor significantly reduce, and breeze residual mass then greatly improves.
Description
Technical field
The invention belongs to the technical field that flame retardant thermoplastic is modified, it is related to aluminate material, i.e. aluminate thing
Application of the matter as fire retardant in flame retardant thermoplastic, especially in flame retardant thermoplastic polyurethane elastomer, polypropylene, second
Application in alkene-vinylacetate.
Background technology
TPUE (TPU) is one of more commonly used plastics in the world at present, and it has had plastics concurrently
The physical and mechanical properties of process industrial art performance and rubber, have high resiliency, high intensity, high-wearing feature, radiation resistance, oil resistivity,
Low temperature resistant fragility and hardness can the mechanical property such as adjustable in very large range, widely should have in many fields of national economy
With.But TPU is easy to burning because this body structure is special, flame is acutely and with strong black smoke, warm when TPU burns
Burst size is big, while has serious molten drop drip phenomenon, and it is applied directly to industry has significant limitation, so resistance
The research for firing thermoplastic polyurethane material is always the focus of current polyurethane material research.According to《The development of fire retardant and moulding
Application in material》(plastics, 31:11-15,2002) introduce, traditional fire retardant (such as halogenated flame retardant) is in a fire often
Many harmful smokes are produced, or even improve the toxicity and corrosivity of flue gas, easily cause great casualties.And traditional Halogen resistance
Agent, such as aluminum-magnesium hydroxide good flame retardation effect, LSZH are fired, but the addition of required fire retardant is larger, makes the power of material
Performance such as tensile strength is learned, fracture strength declines.
According to《Polymer combustion and flame-retarded technology》(Zhang Jun, Ji Kuijiang, summer prolong cause etc. and write, Interpharm Press, 2005 4
Month) introduce, polypropylene (PP) belongs to combustible material in itself, its oxygen index (OI) only 17.0-18.0%, and charring rate is low, during burning
Produce molten drop, so required in many application scenarios it is carried out it is flame-retardant modified.It is main to polypropylene fire retardant both at home and abroad at present
Using addition fire retardant.Ethylene-vinyl acetate copolymer (EVA) belongs in itself compares combustible polymers material, its oxygen index (OI)
It only 17.0-19.0%, increased with the increase of vinyl acetate content, but charring rate is low, produce molten drop during burning, so
Required in many application scenarios it is carried out it is flame-retardant modified.At present, it is main to ethylene-vinyl acetate flame retardant treatment both at home and abroad
Using additive flame retardant.
Aluminate uses as coupling agent in the prior art, suitable for inorganic combustion inhibitor (such as magnesium hydroxide, aluminium hydroxide,
Firebrake ZB, antimony trioxide etc.) surface active be modified.
Inorganic combustion inhibitor has stronger polarity and hydrophily, difficult with poor compatibility between non-polar polymer material, interface
To form good combination and bonding.Received to improve cohesive force between magnesium hydroxide and polymer and interface affinity, preparation
Rice flame retardant of magnesium hydroxide and surface modification treatment is carried out to it is one of method the most effective.Nano-particle is in sample
In it is well dispersed, but because nano-particle is without any surface treatment, some particles tend to reunite.
To sum up, it is not added at present using aluminate compound as fire retardant in thermoplastic still, as thermoplastic
The report of property plastic flame.
The content of the invention
It is an object of the invention to provide a kind of fire retardant, flame retarding efficiency is high, dosage is few, less toxic, and uses it for fire-retardant heat
Thermoplastic plastic, especially polyurethane elastomer, polypropylene, ethylene-vinyl acetate modification in, overcome existing thermoplastic poly ammonia
Ester elastomer, polypropylene, ethylene-vinyl acetate burning Heat liberation unit be big and what nano-particle was easy to reunite in the base lacks
Point.
Application of the aluminate compound as fire retardant in flame retardant thermoplastic.
Preferably, described aluminate compound includes aluminate coupling agent UP801, SG-Al821 (distearyl acyl-oxygen
Isopropyl Aluminate), DL-411, DL-411AF, DL-411D, DL-411DF, anti-settling Aluminate ASA at least one.
Application based on aluminate compound as fire retardant in flame retardant thermoplastic is prepared, a kind of high concentration resistance
Fire thermoplastic plastic parent particles, the master batch by thermoplastic, aluminate compound group into, in parts by weight, the thermoplastic
90 parts of plastics of property, 10 parts of aluminate compound.
Preferably, the thermoplastic includes polyurethane elastomer, polypropylene, ethylene-vinyl acetate.
Application based on the aluminate compound as fire retardant in flame retardant thermoplastic is prepared, it is a kind of fire-retardant
Thermoplastic material, it is made up of, is calculated in mass percent thermoplastic, high concentration flame retardant thermoplastic's master batch, it is described
Thermoplastic is 98-99.875%, and high concentration flame retardant thermoplastic master batch is 0.125-2%.
Preferably, it is calculated in mass percent, each component content is that thermoplastic is 99-99.875%, and high concentration is fire-retardant
Thermoplastic plastic parent particles are 0.125-1%.
Further, flame retardant thermoplastic's material preparation method is：
1) high concentration flame retardant thermoplastic's master batch is prepared：By banbury temperature control at 120-190 DEG C, rotating speed 10-
50 revs/min, thermoplastic is added in banbury, treats that its melting adds aluminate compound, 5-30 points of melt blending
Clock, high concentration flame retardant thermoplastic's master batch is obtained, is sealed；
2) by banbury temperature control at 120-190 DEG C, rotating speed is 10-50 revs/min, and thermoplastic is added into banburying
In machine, treat that its melting adds the master batch, melt blending 5-30 minutes, it is compressing to take out material；
3) resulting materials are positioned in constant-temperature constant-humidity environment (25 DEG C, relative humidity 60%) before performance test is carried out and put
Put 72 hours.
Preferably, when the thermoplastic be TPUE, polypropylene when, step 1), 2) described in
Banbury temperature control is 170-190 DEG C.
Preferably, when the thermoplastic is ethylene-vinyl acetate, step 1), 2) described in banbury temperature
Control as 120-160 DEG C.
The present invention adds the presoma aluminate of aluminide using the method for master batch-melt blending in thermoplastic
Compound, thermoplastic and aluminate compound are all used as organic system, there is good compatibility, the long-chain portion of Aluminate
Point with the entanglement of polymer molecule and miscible, make what aluminate compound can be well in thermoplastic matrix to disperse,
And not easy to migrate, precipitation.After treating that aluminate compound hydrolyzes in thermoplastic matrix, its hydrolysate aluminum oxide
It similar to in-situ polymerization, can well be applied in thermoplastic molecule segment, form inierpeneirating network structure.
The beneficial effects of the invention are as follows：
Used first using aluminate compound as fire retardant, and elaborate its answering in flame retardant thermoplastic
With aluminate compound well can be dispersed in polymeric matrix as nano inorganic oxide presoma, when running into
During moisture in air, coupling agent generates nano inorganic oxide in polymer molecule segment reclaimed water solution, with the polymer matrix bodily form
Into inierpeneirating network structure, compared with being directly added into nano-particle oxide, this method for adding inorganic oxide precursor body has
Reunion, migration and precipitation of the reduction nano-particle of effect in polymeric matrix.Fire retardant is used as using aluminate compound
The flame retardant thermoplastic of preparation, HRR, total heat discharge, raw cigarette speed, and always raw smoke, the cigarette factor significantly reduce, and
Breeze residual mass then greatly improves.
Embodiment
The present invention is further described with embodiment below, the aluminate coupling agent UP801 that following instance is mentioned is commercially available production
Product.
Comparative example 1：
TPUE (TPU) is put into 100 × 100 × 3_mm3Mould in, with vulcanizing press pressure
Piece, 180 DEG C of temperature control, pressurize 10 minutes.By sample 35_kW/m2Cone calorimetry test detection is carried out under radiant power, is as a result seen
Table 1.
Embodiment 1：
Aluminate compound prepares flame retardant thermoplastic polyurethane elastomer composite -1 as fire retardant.
The aluminate compound is aluminate coupling agent UP801.
The preparation method of the flame retardant thermoplastic polyurethane elastomer composite is：
1) preparation of master batch, the master batch are made up of TPUE, aluminate coupling agent UP801, with weight
Measure part meter, 90 parts of the TPUE, 10 parts of aluminate coupling agent UP801.Banbury temperature control is existed
180 DEG C, rotating speed is 30 revs/min, and TPUE is added in banbury, treats that its melting adds a certain amount of aluminium
Acid esters coupling agent UP801, melt blending 10 minutes.The fire-retardant TPU/ aluminate coupling agents UP801 master batches of high concentration are obtained, are closed at
It is sealed in hermetic bag.
2) by banbury temperature control at 180 DEG C, rotating speed is 30 revs/min, by the heat that mass percent is 99.875wt%
Plastic polyurethane elasticity is added in banbury, treats that its melting adds the fire-retardant of the high concentration that mass percent is 0.125wt%
Thermoplastic polyurethane elastic master batch, melt blending 10 minutes, it is compressing to take out composite.
3) prepare complete all samples be positioned over before performance test is carried out constant temperature humidity chamber (25 DEG C, relatively
Humidity 60%) in place 72 hours.
100 × 100 × 3_mm is pressed into vulcanizing press to the flame-proof composite material obtained by step 3)3Sample.35_
kW/m2Cone calorimetry detection is carried out to sample under radiant power, the results are shown in Table 1.
Embodiment 2：
Aluminate compound prepares flame retardant thermoplastic polyurethane elastomer composite -2 as fire retardant.
The preparation method of the flame retardant thermoplastic polyurethane elastomer composite is：
1) preparation of master batch, with embodiment 1；
2) by banbury temperature control at 180 DEG C, rotating speed is 30 revs/min, by the thermoplastic that mass percent is 99.75wt%
Property elastic polyurethane be added in banbury, treat its melting add mass percent be 0.25wt% high concentration fire-retardant thermoplastic
Property elastic polyurethane master batch, melt blending 10 minutes, take out composite it is compressing.
3) prepare complete all samples be positioned over before performance test is carried out constant temperature humidity chamber (25 DEG C, relatively
Humidity 60%) in place 72 hours.
100 × 100 × 3mm is pressed into vulcanizing press to the flame-proof composite material obtained by step 3)3Sample.35kW/m2
Cone calorimetry detection is carried out to sample under radiant power, the results are shown in Table 1.
Embodiment 3：
Aluminate compound prepares flame retardant thermoplastic polyurethane elastomer composite -3 as fire retardant.
The preparation method of the flame retardant thermoplastic polyurethane elastomer composite is：
1) preparation of master batch, with embodiment 1；
2) by banbury temperature control at 180 DEG C, rotating speed is 30 revs/min, by the thermoplastic that mass percent is 99.5wt%
Property elastic polyurethane be added in banbury, treat its melting add mass percent be 0.5wt% high concentration fire-retardant thermoplastic
Property elastic polyurethane master batch, melt blending 10 minutes, take out composite it is compressing.
3) prepare complete all samples be positioned over before performance test is carried out constant temperature humidity chamber (25 DEG C, relatively
Humidity 60%) in place 72 hours.
100 × 100 × 3mm is pressed into vulcanizing press to the flame-proof composite material obtained by step 3)3Sample.35kW/m2
Cone calorimetry detection is carried out to sample under radiant power, the results are shown in Table 1.
Embodiment 4：
Aluminate compound prepares flame retardant thermoplastic polyurethane elastomer composite -4 as fire retardant.
The preparation method of the flame retardant thermoplastic polyurethane elastomer composite is：
1) preparation of master batch, with embodiment 1；
2) by banbury temperature control at 180 DEG C, rotating speed is 30 revs/min, by the thermoplasticity that mass percent is 99wt%
Elastic polyurethane is added in banbury, treats that its melting adds mass percent and gathered for the flame-proofed thermoplastic of 1wt% high concentration
Urethane elastomer master batch, melt blending 10 minutes, it is compressing to take out composite；
3) prepare complete all samples be positioned over before performance test is carried out constant temperature humidity chamber (25 DEG C, relatively
Humidity 60%) in place 72 hours.
100 × 100 × 3mm is pressed into vulcanizing press to the flame-proof composite material obtained by step 3)3Sample.35kW/m2
Cone calorimetry detection is carried out to sample under radiant power, the results are shown in Table 1.
Embodiment 5
Aluminate compound prepares flame retardant thermoplastic polyurethane elastomer composite -5 as fire retardant.
The preparation method of the flame retardant thermoplastic polyurethane elastomer composite is：
1) preparation of master batch, with embodiment 1；
2) by banbury temperature control at 180 DEG C, rotating speed is 30 revs/min, by the thermoplasticity that mass percent is 98wt%
Elastic polyurethane is added in banbury, treats that its melting adds mass percent and gathered for the flame-proofed thermoplastic of 2wt% high concentration
Urethane elastomer master batch, melt blending 10 minutes, it is compressing to take out composite；
3) prepare complete all samples be positioned over before performance test is carried out constant temperature humidity chamber (25 DEG C, relatively
Humidity 60%) in place 72 hours.
100 × 100 × 3mm is pressed into vulcanizing press to the flame-proof composite material obtained by step 3)3Sample.35kW/m2
Cone calorimetry detection is carried out to sample under radiant power, the results are shown in Table 1.
The flame retardant thermoplastic polyurethane elastomer composite property table of the present invention of table 1
As it can be seen from table 1 aluminate coupling agent UP801 addition can equally reduce TPU HRR, peak value
Raw cigarette speed and the cigarette factor, while burning time extends, when aluminate coupling agent UP801 master batches content is 0.25wt%,
There is minimum peak value HRR.
Comparative example 2:
Polypropylene (PP) is put into 100 × 100 × 3mm3Mould in, with vulcanizing press tabletting, 180 DEG C of temperature control, protect
Pressure 10 minutes.By sample 35kW/m2Cone calorimetry test detection is carried out under radiant power, the results are shown in Table 2.
Embodiment 6：
Aluminate compound prepares flame-retardant polypropylene composite material -1 as fire retardant
The aluminate compound is aluminate coupling agent UP801.
The preparation method of the flame-retardant polypropylene composite material is：
1) preparation of master batch, the master batch are made up of polypropylene, aluminate coupling agent UP801, in parts by weight, described poly-
90 parts of propylene, 10 parts of aluminate coupling agent UP801.By banbury temperature control at 180 DEG C, rotating speed is 30 revs/min, by poly- third
Alkene is added in banbury, treats that its melting adds a certain amount of aluminate coupling agent UP801, melt blending 10 minutes.Obtain height
The fire-retardant PP/ aluminate coupling agents UP801 master batches of concentration, close in hermetic bag and are sealed.
2) by banbury temperature control at 180 DEG C, rotating speed is 30 revs/min, is the poly- of 99.875wt% by mass percent
Propylene is added in banbury, treats that its melting adds polypropylene flame redardant/aluminate coupling agent that mass percent is 0.125wt%
UP801 master batches, melt blending 10 minutes, it is compressing to take out composite.
3) prepare complete all samples be positioned over before performance test is carried out constant temperature humidity chamber (25 DEG C, relatively
Humidity 60%) in place 72 hours.
100 × 100 × 3mm is pressed into vulcanizing press to the flame-proof composite material obtained by step 3)3Sample.35kW/m2
Cone calorimetry detection is carried out to sample under radiant power, the results are shown in Table 2.
Embodiment 7：
Aluminate compound prepares flame-retardant polypropylene composite material -2 as fire retardant.
The aluminate compound is aluminate coupling agent UP801.
The preparation method of the flame-retardant polypropylene composite material is：
1) preparation of master batch, with embodiment 6.
2) by banbury temperature control at 180 DEG C, rotating speed is 30 revs/min, by mass percent is 99.75wt% poly- third
Alkene is added in banbury, treats that its melting adds polypropylene flame redardant/aluminate coupling agent that mass percent is 0.25wt%
UP801 master batches, melt blending 10 minutes, it is compressing to take out composite.
3) prepare complete all samples be positioned over before performance test is carried out constant temperature humidity chamber (25 DEG C, relatively
Humidity 60%) in place 72 hours.
100 × 100 × 3mm is pressed into vulcanizing press to the flame-proof composite material obtained by step 3)3Sample.35kW/m2
Cone calorimetry detection is carried out to sample under radiant power, the results are shown in Table 2.
Embodiment 8：
Aluminate compound prepares flame-retardant polypropylene composite material -3 as fire retardant.
The aluminate compound is aluminate coupling agent UP801.
The preparation method of the flame-retardant polypropylene composite material is：
1) preparation of master batch, with embodiment 6.
2) by banbury temperature control at 180 DEG C, rotating speed is 30 revs/min, by mass percent is 99.5wt% poly- third
Alkene is added in banbury, treats that its melting adds polypropylene flame redardant/aluminate coupling agent that mass percent is 0.5wt%
UP801 master batches, melt blending 10 minutes, it is compressing to take out composite.
3) prepare complete all samples be positioned over before performance test is carried out constant temperature humidity chamber (25 DEG C, relatively
Humidity 60%) in place 72 hours.
100 × 100 × 3mm is pressed into vulcanizing press to the flame-proof composite material obtained by step 3)3Sample.35kW/m2
Cone calorimetry detection is carried out to sample under radiant power, the results are shown in Table 2.
Embodiment 9：
Aluminate compound prepares flame-retardant polypropylene composite material -4 as fire retardant.
The aluminate compound is aluminate coupling agent UP801.
The preparation method of the flame-retardant polypropylene composite material is：
1) preparation of master batch, with embodiment 6.
2) by banbury temperature control at 180 DEG C, rotating speed is 30 revs/min, by the polypropylene that mass percent is 99wt%
It is added in banbury, it is female treats that its melting adds polypropylene flame redardant/aluminate coupling agent UP801 that mass percent is 1wt%
Grain, melt blending 10 minutes, it is compressing to take out composite.
3) prepare complete all samples be positioned over before performance test is carried out constant temperature humidity chamber (25 DEG C, relatively
Humidity 60%) in place 72 hours.
100 × 100 × 3mm is pressed into vulcanizing press to the flame-proof composite material obtained by step 3)3Sample.35kW/m2
Cone calorimetry detection is carried out to sample under radiant power, the results are shown in Table 2.
Embodiment 10：
Aluminate compound prepares flame-retardant polypropylene composite material -5 as fire retardant.
The aluminate compound is aluminate coupling agent UP801.
The preparation method of the flame-retardant polypropylene composite material is：
1) preparation of master batch, with embodiment 6.
2) by banbury temperature control at 180 DEG C, rotating speed is 30 revs/min, by the polypropylene that mass percent is 98wt%
It is added in banbury, it is female treats that its melting adds polypropylene flame redardant/aluminate coupling agent UP801 that mass percent is 2wt%
Grain, melt blending 10 minutes, it is compressing to take out composite.
3) prepare complete all samples be positioned over before performance test is carried out constant temperature humidity chamber (25 DEG C, relatively
Humidity 60%) in place 72 hours.
100 × 100 × 3mm is pressed into vulcanizing press to the flame-proof composite material obtained by step 3)3Sample.35kW/m2
Cone calorimetry detection is carried out to sample under radiant power, the results are shown in Table 2.
The anti-flaming polypropylene material performance table of the present invention of table 2
It can be drawn by table 2, with the increase of aluminate coupling agent UP801 addition, in polypropylene combustion process
Peak value HRR, total heat release are gradually reduced, and breeze residual mass gradually increases, when aluminate coupling agent UP801 is female
When grain content is 0.5wt%, there are minimum peak HRR, total heat release and maximum neat coal amout, as Aluminate is even
Connection agent UP801 contents further increase, and Heat liberation unit increased.Therefore, when aluminate coupling agent UP801 master batch contents in PP
To there is best flame retardant effect during 0.5wt%.
Comparative example 3:
Ethylene-vinyl acetate copolymer (EVA) is put into 100 × 100 × 3mm3Mould in, with vulcanizing press pressure
Piece, 130 DEG C of temperature control, pressurize 10 minutes.By sample 35kW/m2Cone calorimetry test detection is carried out under radiant power, is as a result seen
Table 3.
Embodiment 11：
Aluminate compound prepares flame-proof ethylene-acetate ethylene copolymer composite -1 as fire retardant
The aluminate compound is aluminate coupling agent UP801.
The preparation method of flame-proof ethylene-acetate ethylene copolymer (EVA) composite is：
1) preparation of master batch, the master batch are made up of ethylene-vinyl acetate copolymer, aluminate coupling agent UP801, with weight
Measure part meter, 90 parts of the ethylene-vinyl acetate copolymer, 10 parts of aluminate coupling agent UP801.Banbury temperature control is existed
130 DEG C, rotating speed is 30 revs/min, and ethylene-vinyl acetate copolymer is added in banbury, and it is a certain amount of to treat that its melting adds
Aluminate coupling agent UP801, melt blending 10 minutes.The fire-retardant EVA/ aluminate coupling agents UP801 master batches of high concentration are obtained, are received
It is sealed in hermetic bag.
2) by banbury temperature control at 130 DEG C, rotating speed is 30 revs/min, by the EVA that mass percent is 99.875wt%
It is added in banbury, it is female treats that its melting adds the fire-retardant EVA/ aluminate coupling agents UP801 that mass percent is 0.125wt%
Grain, melt blending 10 minutes, it is compressing to take out composite.
3) prepare complete all samples be positioned over before performance test is carried out constant temperature humidity chamber (25 DEG C, relatively
Humidity 60%) in place 72 hours.
100 × 100 × 3mm is pressed into vulcanizing press to the flame-proof composite material obtained by step 3)3Sample.35kW/m2
Cone calorimetry detection is carried out to sample under radiant power, the results are shown in Table 3.
Embodiment 12：
Aluminate compound prepares flame-proof ethylene-acetate ethylene copolymer composite -2 as fire retardant
The aluminate compound is aluminate coupling agent UP801.
The preparation method of flame-proof ethylene-acetate ethylene copolymer (EVA) composite is：
1) preparation of master batch, with embodiment 11.
2) by banbury temperature control at 130 DEG C, rotating speed is 30 revs/min, by the EVA that mass percent is 99.75wt%
It is added in banbury, treats that its melting adds the fire-retardant EVA/ aluminate coupling agents UP801 that mass percent is 0.25wt%, melt
Melt blending 10 minutes, it is compressing to take out composite.
3) prepare complete all samples be positioned over before performance test is carried out constant temperature humidity chamber (25 DEG C, relatively
Humidity 60%) in place 72 hours.
100 × 100 × 3mm is pressed into vulcanizing press to the flame-proof composite material obtained by step 3)3Sample.35kW/m2
Cone calorimetry detection is carried out to sample under radiant power, the results are shown in Table 3.
Embodiment 13：
Aluminate compound prepares flame-proof ethylene-acetate ethylene copolymer composite -3 as fire retardant
The aluminate compound is aluminate coupling agent UP801.
The preparation method of flame-proof ethylene-acetate ethylene copolymer (EVA) composite is：
1) preparation of master batch, with embodiment 11.
2) by banbury temperature control at 130 DEG C, rotating speed is 30 revs/min, and the EVA that mass percent is 99.5wt% is added
Enter into banbury, treat that its melting adds the fire-retardant EVA/ aluminate coupling agents UP801 master batches that mass percent is 0.5wt%,
Melt blending 10 minutes, it is compressing to take out composite.
3) prepare complete all samples be positioned over before performance test is carried out constant temperature humidity chamber (25 DEG C, relatively
Humidity 60%) in place 72 hours.
100 × 100 × 3mm is pressed into vulcanizing press to the flame-proof composite material obtained by step 3)3Sample.35kW/m2
Cone calorimetry detection is carried out to sample under radiant power, the results are shown in Table 3.
Embodiment 14：
Aluminate compound prepares flame-proof ethylene-acetate ethylene copolymer composite -4 as fire retardant
The aluminate compound is aluminate coupling agent UP801.
The preparation method of flame-proof ethylene-acetate ethylene copolymer (EVA) composite is：
1) preparation of master batch, with embodiment 11.
2) by banbury temperature control at 130 DEG C, rotating speed is 30 revs/min, and the EVA that mass percent is 99wt% is added
Into banbury, treat that its melting adds the fire-retardant EVA/ aluminate coupling agents UP801 master batches that mass percent is 1wt%, melting
Blending 10 minutes, it is compressing to take out composite.
3) prepare complete all samples be positioned over before performance test is carried out constant temperature humidity chamber (25 DEG C, relatively
Humidity 60%) in place 72 hours.
100 × 100 × 3mm is pressed into vulcanizing press to the flame-proof composite material obtained by step 3)3Sample.35kW/m2
Cone calorimetry detection is carried out to sample under radiant power, the results are shown in Table 3.
Embodiment 15：
Aluminate compound prepares flame-proof ethylene-acetate ethylene copolymer composite -5 as fire retardant
The aluminate compound is aluminate coupling agent UP801.
The preparation method of flame-proof ethylene-acetate ethylene copolymer (EVA) composite is：
1) preparation of master batch, with embodiment 11.
2) by banbury temperature control at 130 DEG C, rotating speed is 30 revs/min, and the EVA that mass percent is 98wt% is added
Into banbury, treat that its melting adds the fire-retardant EVA/ aluminate coupling agents UP801 master batches that mass percent is 2wt%, melting
Blending 10 minutes, it is compressing to take out composite.
3) prepare complete all samples be positioned over before performance test is carried out constant temperature humidity chamber (25 DEG C, relatively
Humidity 60%) in place 72 hours.
100 × 100 × 3mm is pressed into vulcanizing press to the flame-proof composite material obtained by step 3)3Sample.35kW/m2
Cone calorimetry detection is carried out to sample under radiant power, the results are shown in Table 3.
The flame-proof ethylene of the present invention of table 3-acetate ethylene copolymer composite property table
As shown in Table 3, the peak value HRR in ethylene-vinyl acetate combustion process, total heat release are with aluminic acid
The increase of ester coupling agent UP801 contents be first gradually reduced and then and increase, and breeze residual mass is into opposite variation tendency, when
When the content of aluminate coupling agent UP801 master batches is 0.5wt%, peak value HRR, total heat release have minimum value, now have
Optimal flame retardant effect.
Claims (5)
1. a kind of high concentration flame retardant thermoplastic master batch, it is characterised in that the master batch is by thermoplastic, aluminate
Compound forms, in parts by weight, 90 parts of the thermoplastic, 10 parts of aluminate compound.
2. a kind of flame retardant thermoplastic's material, it is characterised in that as the high concentration described in thermoplastic and claim 1
Flame retardant thermoplastic's master batch forms, and is calculated in mass percent, the thermoplastic is 98-99.875%, and high concentration is fire-retardant
Thermoplastic plastic parent particles are 0.125-2%.
3. a kind of preparation method of flame retardant thermoplastic, it is characterised in that using the method for master batch-melt blending, step is such as
Under：
1) high concentration flame retardant thermoplastic's master batch is prepared：By banbury temperature control at 120-190 DEG C, rotating speed be 10-50 turn/
Point, thermoplastic is added in banbury, treats that its melting adds aluminate compound, melt blending 5-30 minutes, obtains
To high concentration flame retardant thermoplastic's master batch, it is sealed；
2) by banbury temperature control at 120-190 DEG C, rotating speed is 10-50 revs/min, and thermoplastic is added into banbury
In, treat that its melting adds the master batch, melt blending 5-30 minutes, it is compressing to take out material；
3) resulting materials are positioned over constant-temperature constant-humidity environment before performance test is carried out, and maintain 25 DEG C of temperature, relative humidity 60%,
Place 72 hours.
4. method as claimed in claim 3, it is characterised in that the thermoplastic is TPUE or gathered
During propylene, step 1), 2) banbury temperature control described in melt blending are 170-190 DEG C.
5. method as claimed in claim 3, it is characterised in that when the thermoplastic is ethylene-vinyl acetate, step
1), 2) banbury temperature control described in melt blending is 120-160 DEG C.
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| CN110105746A (en) * | 2019-05-24 | 2019-08-09 | 青岛科技大学 | A kind of fire retardant and the application in thermoplastic polyurethane elastomer is fire-retardant |
| CN112159625B (en) * | 2020-09-09 | 2022-05-10 | 广西青龙化学建材有限公司 | Smokeless non-cured rubber asphalt waterproof coating capable of being constructed at low temperature and preparation method thereof |
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| CN1915828A (en) * | 2006-09-11 | 2007-02-21 | 中国铝业股份有限公司 | Method for preparing superfine aluminium hydroxide in flame retardant grade with high initial dehydration temperature |
| CN101445877A (en) * | 2007-11-27 | 2009-06-03 | 大连核心铸造技术工程研究所 | Fire retardant |
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| CN1915828A (en) * | 2006-09-11 | 2007-02-21 | 中国铝业股份有限公司 | Method for preparing superfine aluminium hydroxide in flame retardant grade with high initial dehydration temperature |
| CN101445877A (en) * | 2007-11-27 | 2009-06-03 | 大连核心铸造技术工程研究所 | Fire retardant |
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| 新型无毒铝酸酯偶联剂的研制;朱进 等;《山东化工》;20111231;第40卷(第12期);1-3 * |
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