CN104513473A - Halogen-free flame-retarded thermoplastic polyurethane elastomer composite materials and preparation method thereof - Google Patents
Halogen-free flame-retarded thermoplastic polyurethane elastomer composite materials and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of thermoplastic polyurethane elastomer composite materials, and particularly relates to halogen-free flame-retarded thermoplastic polyurethane elastomer composite materials which are prepared from the following components in percentage by weight: 75-92% of thermoplastic polyurethane elastomers, 6-23% of a halogen-free flame retardant, 1-5% of a flame retardant synergist, 0.1-1% of an antioxidant, 0.1-1% of a lubricant and 0.01-0.5% of an anti-hydrolysis agent, wherein the flame retardant synergist is nanomaterials doped with graphene and double hydroxide. The halogen-free flame-retarded thermoplastic polyurethane elastomer composite materials provided by the invention have excellent flame retardant properties and mechanical properties, as well as excellent durability and weather resistance. In addition, the invention also discloses a method for preparing the halogen-free flame-retarded thermoplastic polyurethane elastomer composite materials.
Description
Technical field
The invention belongs to thermoplastic polyurethane elastomer composite material technical field, particularly relate to a kind of halogen-free fire retardation thermoplastic polyurethane elastic composite and preparation method thereof.
Background technology
Polyurethane material is one of large synthetic materials in the world today six.Based on urethane resin, the product that can be made into has porous plastics, rubber, coating, tackiness agent, fiber, synthetic leather, waterproof paint, pavement material etc., is widely used in the national economy every field such as electromechanics, boats and ships, aviation, vehicle, civil construction, light industry, weaving.Output and kind increase year by year, occupy suitable status in material industry, and therefore, each major company of the world competitively develops polyurethane industrial.But theirs is inflammable, and produce a large amount of smog, toxic gas during burning, cause a tremendous loss of lives and property damage, become the serious problem of society today of people's growing interest.Bring loss in order to reduce fire to human society, national departments concerned proposes fire-retardant requirement to polyurethane elastomer.
At present, less to the fire-retardant research of polyurethane elastomer both at home and abroad, mainly concentrate in the selection of fire retardant.And its conventional fire retardant comprises as antimonous oxide (Sb
20
3), tricresyl phosphate (2,3-bis-chloropropyl) ester (TDCPP), hydrated aluminum oxide (Al
20
3.3H
20), bromine one chlorine alkylphosphonic acid carboxylic acid dibasic acid esters (PUR-101), decabromodiphenyl oxide, composite expansion type flame retardant (ammonium polyphosphate, tetramethylolmethane, melamine etc.) and adopt chemosynthesis method introduce phosphorous-containing monomers.These methods can both change the combustioncharacteristics of polyurethane elastomer, make it be converted into flame retardant material, improve flame retardant properties, reduce polyurethane elastomer combustionvelocity, stop fire to expand.But also bring some serious problems simultaneously, be mainly manifested in: poor compatibility between fire retardant and elastomerics; Mechanical Properties of Polyurethane Elastomers is caused to decline; Durability of fire-retardant is poor; Release a large amount of toxic gases (as HCl, HCN etc.), produce a large amount of smog and release a large amount of corrosivess; Flame retarding efficiency is not high, easily produces drippage; Due to the existence of these problems, limit the use range of polyurethane elastomer to a great extent.
Microencapsulation technology is the effective ways solving above-mentioned polyurethane elastic composite.As Chinese patent ZL200910144076.0 reports core-shell type ammonium polyphosphate synergetic flame-retardant polyurethane elastic composite material, good flame retardation effect, and resistance to molten drop is good, improves the shortcoming containing ammonium polyphosphate flame-proof composite material poor water resistance simultaneously, enhance the consistency of fire retardant and polyurethane elastomer.In addition, research shows that nano lamellar material significantly can not only reduce material Thermal release peak value and Thermal release total amount, can also significantly improve flame retarding efficiency.In order to improve the flame retarding efficiency of micro encapsulation fire retardant further, generally among flame-retardant system, adding fire retarding synergist, mainly containing metal oxide, polynite and carbon nanotube etc.
Have not yet to see the report using micro encapsulation fire retardant and Graphene and double-hydroxide doped nano-material synergistic flame retardant thermoplastic polyurethane elastomer.
Summary of the invention
An object of the present invention is: for the deficiency of current flame retardant thermoplastic polyurethane elastomer matrix material, and a kind of environmental protection, weather-proof, halogen-free fire retardation thermoplastic polyurethane elastic composite are proposed, this halogen-free fire retardation thermoplastic polyurethane elasticity has excellent flame retardant properties and excellent mechanical property.
To achieve these goals, the technical solution used in the present invention is:
A kind of halogen-free fire retardation thermoplastic polyurethane elastic composite, by weight percentage, composed of the following components:
Polyurethane Thermoplastic Elastomer 75% ~ 92%;
Halogen-free flame retardants 6% ~ 23%;
Fire retarding synergist 1% ~ 5%;
Oxidation inhibitor 0.1% ~ 1%;
Lubricant 0.1% ~ 1%;
Hydrolysis-resisting agent 0.01% ~ 0.5%;
Wherein, described fire retarding synergist is Graphene and double-hydroxide doped nano-material.
One as halogen-free fire retardation thermoplastic polyurethane elastic composite of the present invention is improved, by weight percentage, composed of the following components:
Polyurethane Thermoplastic Elastomer 80% ~ 90%;
Halogen-free flame retardants 7% ~ 17%;
Fire retarding synergist 2% ~ 4%;
Oxidation inhibitor 0.1% ~ 1%;
Lubricant 0.1% ~ 1%;
Hydrolysis-resisting agent 0.08% ~ 0.5%.
One as halogen-free fire retardation thermoplastic polyurethane elastic composite of the present invention is improved, and described Polyurethane Thermoplastic Elastomer is at least one in thermoplastic polyester type polyurethane elastomerics and thermoplastic polyether urethane elastomerics.
One as halogen-free fire retardation thermoplastic polyurethane elastic composite of the present invention is improved, and described halogen-free flame retardants is at least one in Silica hydrogel micro encapsulation ammonium polyphosphate, melmac micro encapsulation ammonium polyphosphate, polyurethane micro-encapsulated ammonium polyphosphate, Mierocrystalline cellulose micro encapsulation ammonium polyphosphate and epoxy resin micro-capsule ammonium polyphosphate.The present invention has selected the micro encapsulation fire retardant of halogen-free environmental, improve water tolerance and the weather resistance of fire retardant, due to shell compatibilization, improve the consistency of micro encapsulation fire retardant and Polyurethane Thermoplastic Elastomer, decrease to the damage of material mechanical performance and fire retardant along with the various migrations in polyurethane elastomer use procedure, thus improve comprehensive physical property and the weather resistance of Polyurethane Thermoplastic Elastomer flame-proof composite material.
One as halogen-free fire retardation thermoplastic polyurethane elastic composite of the present invention is improved, and described Graphene and double-hydroxide doped nano-material are at least one in Graphene and magnesium aluminum double hydroxide doped nano-material, Graphene and zinc-aluminium double-hydroxide doped nano-material and Graphene and nickel aluminium double-hydroxide doped nano-material.First, Graphene and double-hydroxide sheet layer material are dispersed among Polyurethane Thermoplastic Elastomer with nm regime, and the layer blocking effect of graphene film and double-hydroxide significantly reduces the Thermal release of material and total Thermal release, improve the fire safety of material; Again, Graphene and double-hydroxide are dispersed among Polyurethane Thermoplastic Elastomer uniformly, synergistic fire retardation can be played with micro encapsulation fire retardant, have and improve flame retarding efficiency, improve into charcoal speed and the not advantage such as molten drop, thus the usage quantity of fire retardant in polyurethane system can be reduced further.
One as halogen-free fire retardation thermoplastic polyurethane elastic composite of the present invention is improved, described oxidation inhibitor is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester (antioxidant 1010), 4, at least one in 4 '-thiobis (the 6-tertiary butyl-3-methylphenol) (antioxidant 300), Tyox B (anti-oxidant DLTP), tetramethylolmethane four (3-lauryl thiopropionate) (oxidation inhibitor S4P) and three [2.4-di-tert-butyl-phenyl] phosphorous acid ester (irgasfos 168s).
One as halogen-free fire retardation thermoplastic polyurethane elastic composite of the present invention is improved, and described lubricant is at least one in Zinic stearas, hydroxy silicon oil, silicone powder and fluorine containing lubricant.
One as halogen-free fire retardation thermoplastic polyurethane elastic composite of the present invention is improved, and described hydrolysis-resisting agent is at least one in carbodiimide, two carbodiimide and polycarbodiimide.
Halogen-free fire retardation thermoplastic polyurethane elastic composite beneficial effect of the present invention is: the invention provides a kind of environmental protection, weather-proof, halogen-free fire retardation thermoplastic polyurethane elastic composite, it has excellent flame retardant properties and excellent mechanical property, has excellent weather resistance and weathering resistance simultaneously.
Another object of the present invention is the preparation method providing a kind of halogen-free fire retardation thermoplastic polyurethane elastic composite, by weight percentage, the fire retarding synergist of 1% ~ 5% is added in the Polyurethane Thermoplastic Elastomer of 75% ~ 92%, and described fire retarding synergist is Graphene and double-hydroxide doped nano-material, then mixing to even in Banbury mixer or forcing machine, then the halogen-free flame retardants of 6% ~ 23% is added, the oxidation inhibitor of 0.1% ~ 1%, part lubricant of 0.1% ~ 1% and the hydrolysis-resisting agent of 0.01% ~ 0.5% mix, halogen-free fire retardation thermoplastic polyurethane elastic composite is a granulated at 170 ~ 200 DEG C after mixing.Can prepare halogen-free fire retardation thermoplastic polyurethane elastic composite rapidly by above-mentioned preparation method, importantly this preparation method is simple and practical.
One as the preparation method of halogen-free fire retardation thermoplastic polyurethane elastic composite of the present invention is improved, and temperature mixing in Banbury mixer or forcing machine is 170 ~ 200 DEG C.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
embodiment 1,by weight percentage, Graphene and the magnesium aluminum double hydroxide doped nano-material of 1% will be added in the thermoplastic polyester type polyurethane elastomerics of 92%, then mixing to even in Banbury mixer, this mixing temperature is 170 DEG C, then add the Silica hydrogel micro encapsulation ammonium polyphosphate of 8%, 0.1% oxidation inhibitor S4P, 0.1% Zinic stearas and 0.01% carbodiimide mix, become halogen-free fire retardation thermoplastic polyurethane elastic composite at 170 DEG C of extruding pelletizations after mixing.
Detected result shows: the tensile strength of halogen-free fire retardation thermoplastic polyurethane elastic composite prepared by the present embodiment is 42.5MPa, and elongation at break is 680%, and oxygen index is 29.5%, and testing vertical flammability is by UL-94 V0 level.After 80 degree of hot-water soaks one week, tensile strength is 25.8MPa, and elongation at break is 480%, and oxygen index is 28%, and testing vertical flammability is by UL-94 V0 level.
embodiment 2,by weight percentage, Graphene and the zinc-aluminium double-hydroxide doped nano-material of 3% will be added in 75% thermoplastic polyether urethane elastomerics, then mixing to even in an extruder, this mixing temperature is 200 DEG C, then add the melmac micro encapsulation ammonium polyphosphate of 20%, the antioxidant 1010 of 1%, the silicone powder of 0.9% and 0.1% two carbodiimide mix, become halogen-free fire retardation thermoplastic polyurethane elastic composite at 200 DEG C of extruding pelletizations after mixing.
Detected result shows: the tensile strength of halogen-free fire retardation thermoplastic polyurethane elastic composite prepared by the present embodiment is 30.8MPa, and elongation at break is 610%, and oxygen index is 32.5%, and testing vertical flammability is by UL-94 V0 level.After 80 degree of hot-water soaks one week, tensile strength is 28.5MPa, and elongation at break is 580%, and oxygen index is 32%, and testing vertical flammability is by UL-94 V0 level.
embodiment 3,by weight percentage, by the thermoplastic polyester type polyurethane elastomerics of 50% and 30% thermoplastic polyether urethane elastomerics in add 3% Graphene and nickel aluminium double-hydroxide doped nano-material, then mixing to even in an extruder, this mixing temperature is 190 DEG C, then add the Mierocrystalline cellulose micro encapsulation ammonium polyphosphate of 15%, the irgasfos 168 of 1%, the fluorine containing lubricant of 0.5% and 0.5% polycarbodiimide mix, become halogen-free fire retardation thermoplastic polyurethane elastic composite at 190 DEG C of extruding pelletizations after mixing.
Detected result shows: the tensile strength of halogen-free fire retardation thermoplastic polyurethane elastic composite prepared by the present embodiment is 35.8MPa, and elongation at break is 630%, and oxygen index is 35.5%, and testing vertical flammability is by UL-94 V0 level.After 80 degree of hot-water soaks one week, tensile strength is 28.8MPa, and elongation at break is 510%, and oxygen index is 33.5%, and testing vertical flammability is by UL-94 V0 level.
embodiment 4,by weight percentage, Graphene and the nickel aluminium double-hydroxide doped nano-material of 2% will be added in the thermoplastic polyether urethane elastomerics of 90%, then mixing to even in an extruder, this mixing temperature is 195 DEG C, then add the epoxy resin micro-capsule ammonium polyphosphate of 7%, the antioxidant 300 of 0.5% and anti-oxidant DLTP mixture, the hydroxy silicon oil of 0.42% and the polycarbodiimide of 0.08% to mix, after mixing, become halogen-free fire retardation thermoplastic polyurethane elastic composite at 195 DEG C of extruding pelletizations.
Detected result shows: the tensile strength of halogen-free fire retardation thermoplastic polyurethane elastic composite prepared by the present embodiment is 39.8MPa, and elongation at break is 640%, and oxygen index is 34.5%, and testing vertical flammability is by UL-94 V0 level.After 80 degree of hot-water soaks one week, tensile strength is 30.8MPa, and elongation at break is 440%, and oxygen index is 31.5%, and testing vertical flammability is by UL-94 V0 level.
embodiment 5,by weight percentage, Graphene and the nickel aluminium double-hydroxide doped nano-material of 4% will be added in the thermoplastic polyether urethane elastomerics of 85%, then mixing to even in an extruder, this mixing temperature is 180 DEG C, then add 9% epoxy resin micro-capsule ammonium polyphosphate and Mierocrystalline cellulose micro encapsulation ammonium polyphosphate mixture, 0.5% antioxidant 300 and antioxidant 1010 mixture, the hydroxy silicon oil of 1% and the polycarbodiimide of 0.5% mix, become halogen-free fire retardation thermoplastic polyurethane elastic composite at 180 DEG C of extruding pelletizations after mixing.
Detected result shows: the tensile strength of halogen-free fire retardation thermoplastic polyurethane elastic composite prepared by the present embodiment is 40.8MPa, and elongation at break is 630%, and oxygen index is 35.5%, and testing vertical flammability is by UL-94 V0 level.After 80 degree of hot-water soaks one week, tensile strength is 31.8MPa, and elongation at break is 450%, and oxygen index is 32.5%, and testing vertical flammability is by UL-94 V0 level.
In the various embodiments described above, the tensile strength of fire-retardant product and elongation at break testing standard are ASTM D412; Oxygen index testing standard is ASTM D2863; Testing vertical flammability testing standard is ASTM D3801.
From above embodiment result, use micro encapsulation fire retardant and Graphene and double-hydroxide synergistic flame retardant that doped nano-material forms, there is flame retarding efficiency high, water tolerance excellent in durability, to the mechanics of material and comprehensively physical property damage the features such as little.
The above; be only preferred embodiment of the present invention, but protection scope of the present invention is not limited thereto, is anyly familiar with those skilled in the art in the technical scope that the present invention discloses; the change that can expect easily or replacement, all should be encompassed within protection scope of the present invention.Therefore, protection scope of the present invention should be as the criterion with the protection domain of claims.
Claims (10)
1. a halogen-free fire retardation thermoplastic polyurethane elastic composite, is characterized in that, by weight percentage, composed of the following components:
Polyurethane Thermoplastic Elastomer 75% ~ 92%;
Halogen-free flame retardants 6% ~ 23%;
Fire retarding synergist 1% ~ 5%;
Oxidation inhibitor 0.1% ~ 1%;
Lubricant 0.1% ~ 1%;
Hydrolysis-resisting agent 0.01% ~ 0.5%;
Wherein, described fire retarding synergist is Graphene and double-hydroxide doped nano-material.
2. halogen-free fire retardation thermoplastic polyurethane elastic composite according to claim 1, is characterized in that, by weight percentage, composed of the following components:
Polyurethane Thermoplastic Elastomer 80% ~ 90%;
Halogen-free flame retardants 7% ~ 17%;
Fire retarding synergist 2% ~ 4%;
Oxidation inhibitor 0.1% ~ 1%;
Lubricant 0.1% ~ 1%;
Hydrolysis-resisting agent 0.08% ~ 0.5%.
3. halogen-free fire retardation thermoplastic polyurethane elastic composite according to claim 1, is characterized in that: described Polyurethane Thermoplastic Elastomer is at least one in thermoplastic polyester type polyurethane elastomerics and thermoplastic polyether urethane elastomerics.
4. halogen-free fire retardation thermoplastic polyurethane elastic composite according to claim 1, is characterized in that: described halogen-free flame retardants is at least one in Silica hydrogel micro encapsulation ammonium polyphosphate, melmac micro encapsulation ammonium polyphosphate, polyurethane micro-encapsulated ammonium polyphosphate, Mierocrystalline cellulose micro encapsulation ammonium polyphosphate and epoxy resin micro-capsule ammonium polyphosphate.
5. halogen-free fire retardation thermoplastic polyurethane elastic composite according to claim 1, is characterized in that: described Graphene and double-hydroxide doped nano-material are at least one in Graphene and magnesium aluminum double hydroxide doped nano-material, Graphene and zinc-aluminium double-hydroxide doped nano-material and Graphene and nickel aluminium double-hydroxide doped nano-material.
6. halogen-free fire retardation thermoplastic polyurethane elastic composite according to claim 1, it is characterized in that: described oxidation inhibitor is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, 4, at least one in 4 '-thiobis (the 6-tertiary butyl-3-methylphenol), Tyox B, tetramethylolmethane four (3-lauryl thiopropionate) and three [2.4-di-tert-butyl-phenyl] phosphorous acid ester.
7. halogen-free fire retardation thermoplastic polyurethane elastic composite according to claim 1, is characterized in that: described lubricant is at least one in Zinic stearas, hydroxy silicon oil, silicone powder and fluorine containing lubricant.
8. halogen-free fire retardation thermoplastic polyurethane elastic composite according to claim 1, is characterized in that: described hydrolysis-resisting agent is at least one in carbodiimide, two carbodiimide and polycarbodiimide.
9. the preparation method of a halogen-free fire retardation thermoplastic polyurethane elastic composite, it is characterized in that: by weight percentage, the fire retarding synergist of 1% ~ 5% is added in the Polyurethane Thermoplastic Elastomer of 75% ~ 92%, and described fire retarding synergist is Graphene and double-hydroxide doped nano-material, then mixing to even in Banbury mixer or forcing machine, then the halogen-free flame retardants of 6% ~ 23% is added, the oxidation inhibitor of 0.1% ~ 1%, part lubricant of 0.1% ~ 1% and the hydrolysis-resisting agent of 0.01% ~ 0.5% mix, halogen-free fire retardation thermoplastic polyurethane elastic composite is a granulated at 170 ~ 200 DEG C after mixing.
10. the preparation method of halogen-free fire retardation thermoplastic polyurethane elastic composite according to claim 9, is characterized in that: temperature mixing in Banbury mixer or forcing machine is 170 ~ 200 DEG C.
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| CN104804410A (en) * | 2015-04-21 | 2015-07-29 | 广州敬信高聚物科技有限公司 | Halogen-free flame-retardant thermoplastic polyurethane elastomer composite containing synergistic agent and preparation method of halogen-free flame-retardant thermoplastic polyurethane elastomer composite |
| CN105330818A (en) * | 2015-12-01 | 2016-02-17 | 中国科学技术大学苏州研究院 | Flame retardant rigid polyurethane foam material and preparation method thereof |
| CN105754323A (en) * | 2016-03-08 | 2016-07-13 | 深圳市沃尔核材股份有限公司 | High-strength flame-retardant wear-resistant hydrolysis-resistant identification card and production method thereof |
| CN105949744A (en) * | 2016-05-11 | 2016-09-21 | 洛阳辰祥机械科技有限公司 | Flame-retardant and hydrophobic material and preparation method thereof |
| CN107163289A (en) * | 2017-06-20 | 2017-09-15 | 安徽建筑大学 | Graphene anti-flaming smoke-inhibiting agent that layered double-hydroxide molybdenum acid ion is modified and preparation method thereof |
| CN108795016A (en) * | 2018-05-17 | 2018-11-13 | 株洲时代新材料科技股份有限公司 | A kind of modified thermoplastic material and preparation method |
| CN108864399A (en) * | 2018-07-06 | 2018-11-23 | 汕头大学 | A kind of organic-silicon-modified flame retardant polyurethane and its preparation |
| CN109251402A (en) * | 2018-08-22 | 2019-01-22 | 东莞市安高瑞新材料科技有限公司 | Fire-retardant electromagnetic shielding thermoplastic elastomer (TPE) nanocomposite of one kind and preparation method thereof |
| CN110305467A (en) * | 2019-07-12 | 2019-10-08 | 常州大学 | A kind of graphene synergistic flame-retardant smoke inhibition material and preparation method thereof |
| CN110577741A (en) * | 2019-08-30 | 2019-12-17 | 东莞毅工工程塑料有限公司 | low-smoke halogen-free flame-retardant nylon composite material and preparation method thereof |
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| CN113278276A (en) * | 2021-04-27 | 2021-08-20 | 骏能化工（龙南）有限公司 | Preparation method of polyurethane composite material |
| CN116082822A (en) * | 2023-01-17 | 2023-05-09 | 盛鼎高新材料有限公司 | Preparation method of high-temperature-resistant halogen-free flame-retardant polyurethane elastomer |
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| CN105330818A (en) * | 2015-12-01 | 2016-02-17 | 中国科学技术大学苏州研究院 | Flame retardant rigid polyurethane foam material and preparation method thereof |
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