CN103087504A - Flame-retardant thermoplastic polyurethane and preparation method thereof - Google Patents
Flame-retardant thermoplastic polyurethane and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a flame-retardant application of phenyl aluminum hypophosphite in thermoplastic polyurethane (TPU), and flame-retardant TPU comprises the following components in parts by weight: 10-20 parts of the phenyl aluminum hypophosphite, 100 parts of TPU, 1-15 parts of flame-retardant synergist, 1-10 parts of smoke suppressant, 0.5-2 parts of antioxidant, 1 part of coupling agent and 0.5 part of lubricating agent. According to the flame-retardant TPU disclosed by the invention, coating modification treatment is firstly performed on the surface of the phenyl aluminum hypophosphite by using the flame-retardant synergist, then the phenyl aluminum hypophosphite is mixed with TPU masterbatch and other materials uniformly at a high speed, a twin-screw extruding machine is further used for mixing, extrusion and granulation, then molding treatment is performed, and the flame-retardant TPU prepared by the method has excellent fire resistance on the basis of ensuring mechanical properties; and simultaneously, the materials of the flame-retardant TPU disclosed by the invention are halogen-free, so that smoke generated during combustion is less, the environmental pollution is low, and the flame-retardant TPU can be widely applied to public places, home decoration and other occasions.
Description
Technical field
The present invention relates to polymeric material field, be specifically related to a kind of flame-proof thermoplastic polyurethane and preparation method thereof.
Background technology
Thermoplastic polyurethane (TPU) has that wear resistance is good, durometer level is wide, high-tenacity and elongation high, the characteristics such as good damping effect, oil resistance are good are the synthetic materials of a class between plastics and rubber, are described as " third generation synthetic rubber ".Be widely used in industries such as automotive industry, aerospace, telecommunications, textile industries.
The weak point of TPU is very easily to burn, and discharges the toxic gases such as HCN, CO after burning, very easily causes people's death by suffocation.A large amount of heat is emitted in burning simultaneously, and flame transmission speed is fast, and follows drip phenomenon, very easily causes fire.Because TPU is widely used, therefore also more and more stricter to the requirement of its over-all properties, particularly more urgent to the raising of its flame retardant properties.
General TPU fire retardant contains halogen, not only to environment, but also can discharge harmful corrosive gases, serious threat people's life and health, and then limited the application of TPU.
Summary of the invention
The object of the invention is to the defective for above-mentioned thermoplastic polyurethane (TPU), a kind of flame-proof thermoplastic polyurethane and preparation method thereof is provided, this flame-proof thermoplastic polyurethane is on the basis that guarantees its mechanical property, have excellent flame retardant properties, can be applied to widely the occasions such as public place, home decoration.
The present invention is achieved through the following technical solutions:
A kind of flame-proof thermoplastic polyurethane is made by following parts by weight of component, phenyl hypo-aluminum orthophosphate 10-20 part, 100 parts of thermoplastic polyurethanes, retardant synergist 1-15 part, smoke suppressant 1-10 part, oxidation inhibitor 0.5-2 part, 1 part of coupling agent, 0.5 part of lubricant.
The further improvement project of the present invention is, described retardant synergist is one or several of zinc borate, Precondensed UreaFormaldehyde Resin, resol.
The present invention further improvement project is that described smoke suppressant is one or several of magnesium hydroxide, aluminium hydroxide.
The present invention further improvement project is that described oxidation inhibitor is irgasfos 168 or antioxidant 1010.
The present invention further improvement project is that described coupling agent is silane coupling agent.
The present invention further improvement project is that described lubricant is Zinic stearas or calcium stearate.
A kind of preparation method of flame-proof thermoplastic polyurethane comprises the following steps, by parts by weight of component claimed in claim 1,
(1) first with retardant synergist, the phenyl hypo-aluminum orthophosphate is carried out surface coating modification and process, and then even with thermoplastic polyurethane, smoke suppressant, oxidation inhibitor, coupling agent, lubricant high-speed mixing;
(2) mixture that step (1) is obtained pack into further mixing, melting of twin screw extruder, extrude, then carry out forming processes, finally obtain flame-proof thermoplastic polyurethane.
The present invention further improvement project is that the melting of described twin screw extruder, extrusion temperature scope are 100-150 ℃.
The present invention further improvement project is that described forming processes condition is: temperature 195 ℃ of left and right, pressure 1.5Mpa left and right, hot pressing 20min left and right, the 15min left and right of colding pressing.
Beneficial effect of the present invention:
At first the present invention coats modification with retardant synergist to phenyl hypo-aluminum orthophosphate surface, then to carry out high-speed mixing even with TPU master batch and other materials, further mix extruding pelletization with twin screw extruder again, then carry out forming processes, the fire-retardant TPU that makes by this method is on the basis that guarantees its mechanical property, had excellent flame retardant properties, simultaneously, material Halogen of the present invention, the burning fuming amount is few, environmental pollution is little, can be applied to widely the occasions such as public place, home decoration.
Embodiment
Describe the present invention in detail below in conjunction with each embodiment, the component in following table mixed in twin screw extruder, according to the chemical property of TPU the twin screw extruder Temperature Setting between 100-150 ℃.Then will make master batch and be injection molded into sample, according to the flammability test of UL94 standard, its concrete regulation:
1. with 23 ℃ and 50% relative humidity adjustment sample;
2. the sample vertical position of regulating is placed on apart from the following about 20cm of cotton pad place;
3. each sample burns 2 times with flame.
Table one
| Component | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 | Embodiment 9 | Embodiment 10 | Embodiment 11 |
| TPU | 100 | 100 | 100 | 100 | 100 | 100 | 100 | 100 | 100 | 100 | 100 |
| The phenyl hypo-aluminum orthophosphate | 20 | 18 | 16 | 14 | 10 | 12 | 10 | 16 | 20 | 14 | 14 |
| Magnesium hydroxide | 7 | 10 | 3 | 7 | 2 | ? | ? | ? | ? | 7 | 7 |
| Aluminium hydroxide | ? | ? | ? | 3 | 5 | 4 | 1 | 8 | 7 | 3 | 3 |
| Zinc borate | 15 | ? | ? | 5 | ? | 3 | 1 | 10 | ? | 5 | ? |
| Precondensed UreaFormaldehyde Resin | ? | 15 | ? | ? | 5 | 4 | ? | ? | 3 | ?5 | ?5 |
| Resol | ? | ? | 15 | 5 | 5 | 5 | ? | 4 | 3 | ? | 5 |
| Irgasfos 168 | 0.5 | 1 | 1.5 | 1.5 | 2 | ? | ? | ? | ? | ? | 1.5 |
| Antioxidant 1010 | ? | ? | ? | ? | ? | 2 | 1.5 | 1 | 0.5 | ?1.5 | ? |
| Silane coupling agent | 1 | 1 | 1 | 1 | 1 | 1 | 1 | 1 | 1 | 1 | 1 |
| Zinic stearas | 0.5 | 0.5 | 0.5 | 0.5 | ? | ? | ? | ? | ? | ?0.5 | ? |
| Calcium stearate | ? | ? | ? | ? | ?0.5 | 0.5 | 0.5 | 0.5 | 0.5 | ? | 0.5 |
The preparation method is as follows:
Embodiment 1
With each component weighing by weight in upper table, at first with zinc borate, phenyl hypo-aluminum orthophosphate surface is coated modification, with each component at high-speed mixer mixing 15min, then utilize twin screw extruder further to mix, melting in 100-150 ℃ of temperature range, extrude, and on vulcanizer compressing tablet, 195 ℃ of left and right of temperature, 1.5MPa the left and right, about hot pressing 20min, the 15min left and right of colding pressing.
Embodiment 2
With each component weighing by weight in upper table, at first with Precondensed UreaFormaldehyde Resin, phenyl hypo-aluminum orthophosphate surface is coated modification, with each component at high-speed mixer mixing 15min, then utilize twin screw extruder further to mix, melting in 100-150 ℃ of temperature range, extrude, and on vulcanizer compressing tablet, 195 ℃ of temperature, 1.5MPa, hot pressing 20min, 15min colds pressing.
Embodiment 3
With each component weighing by weight in upper table, at first with resol, phenyl hypo-aluminum orthophosphate surface is coated modification, with each component at high-speed mixer mixing 15min, then utilize twin screw extruder further to mix, melting in 100-150 ℃ of temperature range, extrude, and on vulcanizer compressing tablet, 195 ℃ of temperature, 1.5MPa, hot pressing 20min, 15min colds pressing.
Embodiment 4
With each component weighing by weight in upper table, at first with zinc borate, resol, phenyl hypo-aluminum orthophosphate surface is coated modification, with each component at high-speed mixer mixing 15min, then utilize twin screw extruder further to mix, melting in 100 ℃ of-150 ℃ of temperature ranges, extrude, and on vulcanizer compressing tablet, 195 ℃ of temperature, 1.5MPa, hot pressing 20min, 15min colds pressing.
Embodiment 5
With each component weighing by weight in upper table, at first with Precondensed UreaFormaldehyde Resin, resol, phenyl hypo-aluminum orthophosphate surface is coated modification, with each component at high-speed mixer mixing 15min, then utilize twin screw extruder further to mix, melting in 100-150 ℃ of temperature range, extrude, and on vulcanizer compressing tablet, 195 ℃ of temperature, 1.5MPa, hot pressing 20min, 15min colds pressing.
Embodiment 6
With each component weighing by weight in upper table, at first with zinc borate, Precondensed UreaFormaldehyde Resin, resol, phenyl hypo-aluminum orthophosphate surface is coated modification, with each component at high-speed mixer mixing 15min, then utilize twin screw extruder further to mix, melting in 100-150 ℃ of temperature range, extrude, and on vulcanizer compressing tablet, 195 ℃ of temperature, 1.5MPa, hot pressing 20min, 15min colds pressing.
Embodiment 7
With each component weighing by weight in upper table, at first with zinc borate, phenyl hypo-aluminum orthophosphate surface is coated modification, with each component at high-speed mixer mixing 15min, then utilize twin screw extruder further to mix, melting in 100-150 ℃ of temperature range, extrude, and on vulcanizer compressing tablet, temperature 195OC, 1.5MPa, hot pressing 20min, 15min colds pressing.
Embodiment 8
With each component weighing by weight in upper table, at first with zinc borate, resol, phenyl hypo-aluminum orthophosphate surface is coated modification, with each component at high-speed mixer mixing 15min, then utilize twin screw extruder further to mix, melting in 100-150 ℃ of temperature range, extrude, and on vulcanizer compressing tablet, 195 ℃ of temperature, 1.5MPa, hot pressing 20min, 15min colds pressing.
Embodiment 9
With each component weighing by weight in upper table, at first with Precondensed UreaFormaldehyde Resin, resol, phenyl hypo-aluminum orthophosphate surface is coated modification, with each component at high-speed mixer mixing 15min, then utilize twin screw extruder further to mix, melting in 100-150 ℃ of temperature range, extrude, and on vulcanizer compressing tablet, 195 ℃ of temperature, 1.5MPa, hot pressing 20min, 15min colds pressing.
Embodiment 10
With each component weighing by weight in upper table, at first with zinc borate, Precondensed UreaFormaldehyde Resin, phenyl hypo-aluminum orthophosphate surface is coated modification, with each component at high-speed mixer mixing 15min, then utilize twin screw extruder further to mix, melting in 100 ℃ of-150 ℃ of temperature ranges, extrude, and on vulcanizer compressing tablet, 195 ℃ of temperature, 1.5MPa, hot pressing 20min, 15min colds pressing.
Embodiment 11
With each component weighing by weight in upper table, at first with Precondensed UreaFormaldehyde Resin, resol, phenyl hypo-aluminum orthophosphate surface is coated modification, with each component at high-speed mixer mixing 15min, then utilize twin screw extruder further to mix, melting in 100 ℃ of-150 ℃ of temperature ranges, extrude, and on vulcanizer compressing tablet, 195 ℃ of temperature, 1.5MPa, hot pressing 20min, 15min colds pressing.
Gained sample in embodiment 1-11 is carried out flame retardant test, and bar-shaped sample is of a size of: 125mm, and wide 13.0mm, thickness are 3.2mm, combustionproperty is carried out according to the UL94 standard, the results are shown in Table two.
Table two
| Performance index | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Embodiment 7 | Embodiment 8 | Embodiment 9 | Embodiment 10 | Embodiment 11 |
| Combustionproperty | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 | V-1 | V-0 | V-0 | V-0 | V-0 |
To sum up, the phenyl hypo-aluminum orthophosphate system that is applied in the present invention, it has good flame retardant effect to TPU.
Above-mentioned embodiment does not limit technical scheme of the present invention in any form, and every employing is equal to replaces or technology that mode that equivalence becomes obtains all drops on protection scope of the present invention.
Claims (9)
1. flame-proof thermoplastic polyurethane, it is characterized in that: made phenyl hypo-aluminum orthophosphate 10-20 part, 100 parts of thermoplastic polyurethanes, retardant synergist 1-15 part, smoke suppressant 1-10 part, oxidation inhibitor 0.5-2 part, 1 part of coupling agent, 0.5 part of lubricant by following parts by weight of component.
2. flame-proof thermoplastic polyurethane according to claim 1 is characterized in that: described retardant synergist is one or several of zinc borate, Precondensed UreaFormaldehyde Resin, resol.
3. flame-proof thermoplastic polyurethane according to claim 1, it is characterized in that: described smoke suppressant is one or several of magnesium hydroxide, aluminium hydroxide.
4. flame-proof thermoplastic polyurethane according to claim 1, it is characterized in that: described oxidation inhibitor is irgasfos 168 or antioxidant 1010.
5. flame-proof thermoplastic polyurethane according to claim 1, it is characterized in that: described coupling agent is silane coupling agent.
6. flame-proof thermoplastic polyurethane according to claim 1, it is characterized in that: described lubricant is Zinic stearas or calcium stearate.
7. the preparation method of a flame-proof thermoplastic polyurethane is characterized in that: comprises the following steps, and by parts by weight of component claimed in claim 1,
(1) first with retardant synergist, the phenyl hypo-aluminum orthophosphate is carried out surface coating modification and process, and then even with thermoplastic polyurethane, smoke suppressant, oxidation inhibitor, coupling agent, lubricant high-speed mixing;
(2) mixture that step (1) is obtained pack into further mixing, melting of twin screw extruder, extrude, then carry out forming processes, finally obtain flame-proof thermoplastic polyurethane.
8. preparation method according to claim 7, it is characterized in that: the melting of described twin screw extruder, extrusion temperature scope are 100-150 ℃.
9. according to claim 7 or 8 described preparation methods, it is characterized in that: described forming processes condition is: temperature 195 ℃ of left and right, pressure 1.5Mpa left and right, hot pressing 20min left and right, the 15min left and right of colding pressing.
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Cited By (10)
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|---|---|---|---|---|
| CN103709432A (en) * | 2013-12-18 | 2014-04-09 | 南京师范大学 | High-flame retardant rigid polyurethane foaming plastic and preparation method thereof |
| WO2016059882A1 (en) * | 2014-10-15 | 2016-04-21 | 大和化学工業株式会社 | Flame-retardant polyurethane resin and flame-retardant synthetic leather |
| CN105778151A (en) * | 2016-05-11 | 2016-07-20 | 闽江学院 | Halogen-free flame retardant for silica gel, application of halogen-free flame retardant and flame-retardant silica gel product |
| CN105860594A (en) * | 2016-05-10 | 2016-08-17 | 什邡市太丰新型阻燃剂有限责任公司 | Synthesis method of organosilicone modified superfine aluminum hypophosphite |
| CN105924932A (en) * | 2016-05-18 | 2016-09-07 | 安徽华能电缆集团有限公司 | Explosion-proof cable sheath material and preparation method thereof |
| CN106832884A (en) * | 2017-01-22 | 2017-06-13 | 江苏欣润塑胶有限公司 | A kind of halogen-free flame-retardant TPU |
| CN111333913A (en) * | 2020-03-18 | 2020-06-26 | 博硕科技(江西)有限公司 | Preparation method and application of functional microencapsulated hypophosphite flame retardant |
| CN111961331A (en) * | 2020-10-23 | 2020-11-20 | 中广核高新核材科技（苏州）有限公司 | Flame-retardant waterproof thermoplastic polyurethane elastomer cable material and preparation method thereof |
| CN115260745A (en) * | 2022-08-31 | 2022-11-01 | 北京化工大学 | TPU flame-retardant composite material and preparation method and application thereof |
| CN116948386A (en) * | 2023-06-08 | 2023-10-27 | 江苏通上新材料科技有限公司 | Flame-retardant composite cable material and preparation method and application thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709432A (en) * | 2013-12-18 | 2014-04-09 | 南京师范大学 | High-flame retardant rigid polyurethane foaming plastic and preparation method thereof |
| WO2016059882A1 (en) * | 2014-10-15 | 2016-04-21 | 大和化学工業株式会社 | Flame-retardant polyurethane resin and flame-retardant synthetic leather |
| JP2016079375A (en) * | 2014-10-15 | 2016-05-16 | 大和化学工業株式会社 | Flame-retardant polyurethane resin and flame-retardant synthetic leather |
| CN105860594A (en) * | 2016-05-10 | 2016-08-17 | 什邡市太丰新型阻燃剂有限责任公司 | Synthesis method of organosilicone modified superfine aluminum hypophosphite |
| CN105778151A (en) * | 2016-05-11 | 2016-07-20 | 闽江学院 | Halogen-free flame retardant for silica gel, application of halogen-free flame retardant and flame-retardant silica gel product |
| CN105924932A (en) * | 2016-05-18 | 2016-09-07 | 安徽华能电缆集团有限公司 | Explosion-proof cable sheath material and preparation method thereof |
| CN106832884A (en) * | 2017-01-22 | 2017-06-13 | 江苏欣润塑胶有限公司 | A kind of halogen-free flame-retardant TPU |
| CN111333913A (en) * | 2020-03-18 | 2020-06-26 | 博硕科技(江西)有限公司 | Preparation method and application of functional microencapsulated hypophosphite flame retardant |
| CN111961331A (en) * | 2020-10-23 | 2020-11-20 | 中广核高新核材科技（苏州）有限公司 | Flame-retardant waterproof thermoplastic polyurethane elastomer cable material and preparation method thereof |
| CN111961331B (en) * | 2020-10-23 | 2021-02-02 | 中广核高新核材科技（苏州）有限公司 | Flame-retardant waterproof thermoplastic polyurethane elastomer cable material and preparation method thereof |
| CN115260745A (en) * | 2022-08-31 | 2022-11-01 | 北京化工大学 | TPU flame-retardant composite material and preparation method and application thereof |
| CN116948386A (en) * | 2023-06-08 | 2023-10-27 | 江苏通上新材料科技有限公司 | Flame-retardant composite cable material and preparation method and application thereof |
| CN116948386B (en) * | 2023-06-08 | 2023-12-22 | 江苏通上新材料科技有限公司 | Flame-retardant composite cable material and preparation method and application thereof |
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Effective date of registration: 20160524 Address after: 224555, Yancheng City Binhai County, Jiangsu Province Coastal Industrial Zone, Zhongshan Road Patentee after: JIANGSU FUBIYA CHEMICALS CO., LTD. Address before: 224500 North Zone of Coastal Industrial Park, Yancheng City Binhai Economic Development Zone, Jiangsu Patentee before: Binhai Jinxiang Chemical Auxiliary Co., Ltd. |