CN108003605B - Halogen-free flame-retardant TPU (thermoplastic polyurethane) encapsulating material and preparation method thereof - Google Patents
Halogen-free flame-retardant TPU (thermoplastic polyurethane) encapsulating material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of chemical synthesis, and particularly relates to a halogen-free flame-retardant TPU (thermoplastic polyurethane) encapsulating material and a preparation method thereof. The method comprises the following raw materials: polyol, diisocyanate, a chain extender, an antioxidant, a light stabilizer, a catalyst, a halogen-free main flame retardant, a synergistic flame retardant and a plasticizer. The halogen-free main flame retardant is one or more of organic hypophosphorous acid metal salt, rare earth hypophosphite or melamine derivative series flame retardants; the synergistic flame retardant is one or more of aluminum hydroxide, magnesium hydroxide, aluminum oxide or magnesium oxide. The invention also provides a preparation method thereof, which comprises the steps of mixing the polyol, the diisocyanate and the chain extender, continuously adding the auxiliary agent dispersed by the plasticizer through a lateral feeding port, and then extruding, processing and granulating through a screw to obtain the product. The flame retardant agent has excellent flame retardant property, mechanical property and processing property, can realize self-extinguishing, does not generate hydrogen halide gas which is harmful to the environment when being combusted in the air, and is efficient and environment-friendly.
Description
Technical Field
The invention belongs to the technical field of chemical synthesis, and particularly relates to a halogen-free flame-retardant TPU (thermoplastic polyurethane) encapsulating material and a preparation method thereof.
Background
The thermoplastic polyurethane elastomer has better chemical corrosion resistance, electrical insulation property, low-temperature flexibility, wear resistance and weather resistance, prolongs the durability and the service life of the material, and has wide application. However, TPU has poor flame retardant property, and has the defects of flammability, large smoke generation amount, dripping and the like, and the application of TPU in automobile parts and other fields is restricted. Meanwhile, in the aspect of composite modification processing application technology, a secondary processing mode is used for production in the actual processing process, the produced TPU finished product is mixed with a physical property reinforcing agent, and then secondary processing is carried out through a single-screw or double-screw extruder, and secondary processing granulation causes high-temperature cracking of the TPU product when the TPU product is melted and mixed at high temperature in the extruder, and the solid auxiliary agent and the TPU product are easy to mix and disperse unevenly, so that the flowability of the product is poor, and the physical property strength is insufficient.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a halogen-free flame-retardant TPU encapsulating material which has excellent flame retardant property, mechanical property and processing property, can realize self-extinguishing, does not generate hydrogen halide gas which is harmful to the environment when being burnt in the air, is efficient and environment-friendly, and also provides a preparation method thereof, and is simple and easy to implement.
The halogen-free flame-retardant TPU encapsulating material comprises the following raw materials: polyol, diisocyanate, a chain extender, an antioxidant, a light stabilizer, a catalyst, a halogen-free main flame retardant, a synergistic flame retardant and a plasticizer;
wherein: the halogen-free main flame retardant is one or more of organic hypophosphorous acid metal salt, rare earth hypophosphite or melamine derivative series flame retardants;
the synergistic flame retardant is one or more of aluminum hydroxide, magnesium hydroxide, aluminum oxide or magnesium oxide.
Preferably, the halogen-free flame retardant TPU encapsulating material comprises the following raw materials in parts by weight:
38-55 parts of polyol
16-26 parts of diisocyanate
Chain extender 2.9-6 parts
0.2 to 0.6 portion of antioxidant
0.2 to 0.6 portion of light stabilizer
0.02-0.04 portion of catalyst
15-23 parts of halogen-free main flame retardant
2-5 parts of synergistic flame retardant
3-10 parts of a plasticizer.
Wherein:
the organic hypophosphorous acid metal salt is organic aluminum hypophosphite or organic manganese hypophosphite, and preferably diethyl aluminum hypophosphite; the rare earth hypophosphite is lanthanum hypophosphite or cerium hypophosphite; the melamine derivative series flame retardant is melamine cyanurate, melamine polyphosphate, melamine pyrophosphate or bisphenol A diphosphonate melamine salt.
The polyalcohol is polytetrahydrofuran diol with molecular weight of 1000-2000.
The diisocyanate is one or more of 4,4 '-diphenylmethane diisocyanate, dicyclohexylmethane diisocyanate, isophorone diisocyanate or xylylene diisocyanate, and 4,4' -diphenylmethane diisocyanate is preferred.
The chain extender is micromolecule diol with 2-10 carbon atoms, and comprises one or more of 1, 2-propylene glycol, 1, 3-butanediol, 1, 4-butanediol, 2-methyl-1, 3-propylene glycol, 1, 6-hexanediol or 3-methyl-1, 5-pentanediol, and preferably 1, 4-butanediol.
The antioxidant is one or more of Irganox 1010, Irganox1076, antioxidant 168 or antioxidant 626.
The light stabilizer is one or more of Tinuvin292, Tinuvin 770, Tinuvin 328 or UV-P.
The catalyst is an organic tin catalyst.
The plasticizer is a low viscosity liquid, preferably benzoates, benzoates or aliphatic dibasic acid esters, preferably diethylene glycol dibenzoate.
The preparation method of the halogen-free flame-retardant TPU encapsulating material comprises the following steps:
(1) adding polyalcohol into the A reaction kettle at the set temperature of 95-105 ℃; placing diisocyanate in a reaction kettle B, and setting the temperature to be 50-65 ℃; placing the chain extender in a C reaction kettle, and setting the temperature to be 40-60 ℃;
(2) mixing an antioxidant, a light stabilizer, a catalyst, a halogen-free main flame retardant and a synergistic flame retardant to obtain an auxiliary agent, and then mixing the auxiliary agent with a plasticizer to obtain the auxiliary agent dispersed by the plasticizer;
(3) and (2) mixing the polyol, the diisocyanate and the chain extender obtained in the step (1), injecting the mixture into a double-screw reactor, controlling the isocyanate index to be 0.99-1.03, adding an auxiliary agent dispersed by a plasticizer through a lateral charging port with a metering and mixing system, extruding and processing the mixture through a screw, granulating in an underwater granulating mode, and drying to obtain the halogen-free flame-retardant TPU encapsulating material.
Compared with the prior art, the invention has the following advantages:
(1) according to the invention, a double-screw reaction sectional adding mode is adopted, the high-efficiency compound flame retardant is added in the primary granulation process of the TPU, high-temperature melting cracking caused by secondary flame-retardant modification of the TPU product is avoided, the high-temperature resistance and the continuity of the flame-retardant modified TPU material are improved, and the prepared flame-retardant TPU can keep better mechanical properties.
(2) Firstly, dispersing the auxiliary agent by using a plasticizer to form a compound flame retardant homogeneous phase, so that the phenomenon of uneven mixing and dispersion is avoided, and the auxiliary agent is uniformly mixed and dissolved in the TPU material; on the other hand, the addition of the plasticizer improves the fluidity of the product, so that the product has good processability, and finally improves the dispersibility of the compound flame retardant and the processability of the TPU material.
(3) The halogen-free main flame retardant and the synergistic flame retardant have synergistic effect, and the system has double effects of gas-phase flame retardance and solid-phase flame retardance, and effectively inhibits the molten drop phenomenon in combustion due to high char forming rate; all components contained in the flame retardant system have good thermal stability, so that the prepared TPU material has stable quality, the whole addition amount of the flame retardant is reduced, and excellent processing operability and flame retardant property are obtained.
(4) The invention also provides a preparation method thereof, which adopts a simple one-step method, is simple and easy to implement, adopts the raw materials of the polyol, the diisocyanate and the chain extender, continuously and quantitatively adds the auxiliary agent dispersed by the plasticizer in proportion through a lateral charging opening with a metering and mixing system, and then carries out screw extrusion processing granulation to obtain the environment-friendly high-flame-retardant TPU with excellent flame retardant property, mechanical property and processing property, and obtains the formula combination of the high-efficiency halogen-free flame retardant; can realize self-extinguishing, does not generate hydrogen halide gas which is toxic to the environment when being burnt in the air, and is efficient and environment-friendly.
(5) The TPU material can be widely applied to automobile parts, including automobile bodies, interiors, engine cabins and chassis.
Detailed Description
The present invention will be further described with reference to the following examples.
Example 1
Polytetrahydrofuran diol (PTMG-1000) in parts by weight: 38.45 parts of the mixture is added into a reaction kettle A, and the temperature is set to be 105 ℃; MDI-100: 17.75 parts of the mixture is placed in a reaction kettle B, and the set temperature is 65 ℃; 1, 4-butanediol: 2.96 parts of the raw materials are placed in a C reaction kettle, and the set temperature is 60 ℃; the mixture is injected into a twin-screw reactor, the isocyanate index is controlled between 0.99 and 1.03, and the flame retardant aluminum diethylphosphinate dispersed with 8 parts of plasticizer diethylene glycol dibenzoate is added through a lateral feed with metering mixing system: 13 parts of flame retardant melamine polyphosphate: 9 parts, flame retardant magnesium hydroxide: 5 parts of Irganox1076, 0.25 part of antioxidant 168, 0.15 part of Tinuvin292 and UV-P, and a catalyst (T-9): 0.04 part by weight, extruding and injecting by a screw, granulating in an underwater granulating manner, and drying to obtain the halogen-free flame retardant TPU elastomer material.
Example 2
Polytetrahydrofuran diol (PTMG-2000) in parts by weight: 49.06 parts of the mixture is added into a reaction kettle A, and the temperature is set to 98 ℃; MDI-100: 21.02 parts of a reaction product, which is placed in a reaction kettle B, and the set temperature is 55 ℃; 1, 4-butanediol: 5.39 parts, placing in a C reaction kettle, setting the temperature at 45 ℃, injecting the mixed material into a double-screw reactor, controlling the isocyanate index at 0.99-1.03, adding diethyl aluminum hypophosphite dispersed with 4 parts of plasticizer diethylene glycol dibenzoate through a lateral feed inlet with a metering mixing system: 9 parts, melamine cyanurate: 6 parts of alumina: 3 parts, Irganox 1010 and an antioxidant 626, which are respectively 0.15 part, Tinuvin 770 and Tinuvin 328, which are respectively 0.1 part, and a catalyst (T-9): 0.03 part by weight, then extruding and injecting by a screw, granulating in an underwater granulating mode, and drying to obtain the halogen-free flame retardant TPU elastomer material.
Comparative example 1
Comparative example 1 was prepared in the same manner as in example 1, except that comparative example 1 used the following raw materials and contents:
PTMG-2000: 64.66 parts, MDI-100: 27.7 parts, 1, 4-butanediol: 7.11 parts of plasticizer diethylene glycol dibenzoate dispersed Irganox 1010 and 0.15 part of antioxidant 626, 0.1 part of Tinuvin 770 and Tinuvin 328, and catalyst (T-9): 0.03 part.
The products prepared in examples 1-2 and comparative example 1 were subjected to performance tests, and the results were as follows:
vertical burning was tested according to GB/T2408-1996 with sample sizes of 125mm by 12.5mm by 1.6 mm; the oxygen index is tested according to GB/T2406-1993, and the sample size is 85mm multiplied by 10mm multiplied by 1.6 mm; tensile strength was tested according to GB/T528-1998; shore A hardness was measured according to GB/T531-1992. The mechanical properties and combustion properties are shown in the table.
TABLE 1 Properties of rigid polyurethane articles obtained in examples
As can be seen from the table, compared with the comparative example 1, the invention adopts the organic hypophosphorous acid metal salt and the melamine derivative series as the main flame retardant and cooperates with the inorganic flame retardant, so that the flame retardant property of the TPU material can be effectively improved, meanwhile, the performance loss caused by secondary processing is avoided by adopting the back-end feeding, and the compatibility is improved by diluting and dissolving the auxiliary agent, so that the TPU material with excellent flame retardant property and good comprehensive property is prepared.
Claims (1)
1. A halogen-free flame-retardant TPU encapsulating material is characterized in that: according to parts by weight, polytetrahydrofuran diol PTMG-1000: 38.45 parts of the mixture is added into a reaction kettle A, and the temperature is set to be 105 ℃; MDI-100: 17.75 parts of the mixture is placed in a reaction kettle B, and the set temperature is 65 ℃; 1, 4-butanediol: 2.96 parts of the raw materials are placed in a C reaction kettle, and the set temperature is 60 ℃; the mixture is injected into a twin-screw reactor, the isocyanate index is controlled between 0.99 and 1.03, and the flame retardant aluminum diethylphosphinate dispersed with 8 parts of plasticizer diethylene glycol dibenzoate is added through a lateral feed with metering mixing system: 13 parts of flame retardant melamine polyphosphate: 9 parts, flame retardant magnesium hydroxide: 5 parts of Irganox1076, 0.25 part of antioxidant 168, 0.15 part of Tinuvin292 and UV-P, and the weight ratio of catalyst T-9: 0.04 part by weight, extruding and injecting by a screw, granulating in an underwater granulating manner, and drying to obtain the halogen-free flame retardant TPU elastomer material.
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| CN109503805A (en) * | 2018-12-14 | 2019-03-22 | 北京新晨办公设备有限公司 | A kind of preparation method and its cover material of paper-sheets rolling wheel cover material |
| JP7400156B2 (en) * | 2019-03-05 | 2023-12-19 | 大和化学工業株式会社 | Flame retardant polyurethane resin composition |
| CN112538147A (en) * | 2020-12-03 | 2021-03-23 | 广东金柏新材料科技股份有限公司 | Flame-retardant thermoplastic polyurethane material and preparation method thereof |
| EP4380991A1 (en) * | 2021-08-03 | 2024-06-12 | Basf Se | Flame retardant thermoplastic polyurethane composition |
| CN113881216B (en) * | 2021-11-24 | 2023-04-28 | 国网河南省电力公司镇平县供电公司 | Wear-resistant flame-retardant modified polyurethane cable material and preparation method thereof |
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| "无卤阻燃热塑性聚氨酯弹性体复合材料研究进展";周颖，等;《塑料助剂》;20170820(第4期);第1-4页 * |
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| CN108003605A (en) | 2018-05-08 |
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