CN109385071B - TPU material with flame retardant property reaching vertical burning V0 grade and preparation method thereof - Google Patents
TPU material with flame retardant property reaching vertical burning V0 grade and preparation method thereof Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
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- C08L75/08—Polyurethanes from polyethers
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
The invention provides a TPU material with flame retardant property reaching a vertical combustion V0 grade and a preparation method thereof, wherein the TPU material is prepared by mixing 100 parts by weight of thermoplastic polyurethane, 35-65 parts by weight of a phosphorus-nitrogen flame retardant system, 2-10 parts by weight of a char forming agent and 3-15 parts by weight of a flame retardant auxiliary agent.
Description
Technical Field
The invention belongs to the field of flame-retardant materials, and particularly relates to a TPU material with flame retardant property reaching a vertical burning V0 grade and a preparation method thereof.
Background
Polyurethane, especially Thermoplastic Polyurethane (TPU) materials, have a wide range of applications in many fields, however, they have a fatal disadvantage that they are inflammable and not easy to self-extinguish, the molecular structure of TPU materials contains a large amount of combustible hydrocarbon segments, the density is small, the specific surface area is large, the thermal conductivity is low, TPU materials which are not subjected to flame retardant treatment are common inflammables, the limiting oxygen index is generally lower than 19, a large amount of toxic smoke is generated when the TPU materials are combusted in a fire, the fire extinguishment is difficult, especially, the TPU materials can expand and open pores during the combustion process, the aperture ratio is high, the combustible components are many, once the TPU materials are ignited, the combustion process is difficult to self-extinguish due to high air circulation and oxygen supply caused by source interruption, and the wide application of the TPU materials is severely limited.
With the rapid development of global economy and the enhancement of human environmental awareness, the requirements of various fields on the quality and performance of TPU materials are higher and higher, and especially in the aspect of flame retardant performance, in order to reduce the occurrence rate of fire and the death rate of the fire, low smoke, no halogen, flame retardant and environmental protection become the mainstream development direction of the TPU material industry. The traditional flame-retardant modification method is to add a large amount of chlorinated paraffin, inorganic filler and other components into a TPU material to achieve the flame-retardant effect, however, the addition of a large amount of the flame-retardant material has great influence on the physical and mechanical properties and the processing properties of the TPU material, so that the TPU material has poor softness, weather resistance, oil resistance, low-temperature resistance and the like at normal temperature. A reaction type flame retardant is added into a TPU material to be a more convenient, economic and effective method for improving the flame retardant property of the TPU material, and the method is mainly characterized in that a chemical combination reaction is carried out between inorganic flame retardants such as compounds of antimony, aluminum, boron, phosphorus and the like, organic flame retardants such as phosphorus-halogen organic ester, halogen phosphate, halogen aliphatic hydrocarbon, organic phosphorus compounds and the like and flame retardant synergistic agents such as a char forming agent, a flame retardant auxiliary agent and the like in the combustion process to generate a carbonized layer with poor heat conductivity so as to isolate the influence of oxygen and high temperature on internal materials and avoid the further generation of the combustion process.
At present, a flame retardant and a flame retardant synergist which can be used for a TPU material are mainly organic compounds containing elements such as phosphorus, chlorine, bromine and the like, for example, CN104650441A discloses a flame retardant polymer composite material which can be ceramized, and comprises 30-40 parts by weight of a thermoplastic polyurethane elastomer, 25-45 parts by weight of a porcelain forming filler, 20-30 parts by weight of a halogen-free flame retardant, 1-5 parts by weight of a synergistic flame retardant, 1-3 parts by weight of a plasticizer, 0.5-2 parts by weight of an antioxidant and 0.02-0.15 part by weight of a cross-linking agent, wherein the performance index of a vertical combustion test can reach V0 level, and the limiting oxygen index can reach 28%; CN104693782A discloses a halogen-free flame-retardant polyether thermoplastic polyurethane elastomer, which comprises the following raw material components of 100 parts of polyether thermoplastic polyurethane elastomer resin, 30-50 parts by weight of a phosphorus-nitrogen flame-retardant system, 1-5 parts by weight of a flame-retardant synergist, 0.5-2 parts by weight of an antioxidant, 0.5-2 parts by weight of a surface modifier, 0.5-2 parts by weight of a coupling agent and 0.5-4 parts by weight of a lubricant, wherein the obtained worry-free flame-retardant TPU material also has a good flame-retardant effect, a UL-94 test can reach a V0 level, and the limiting oxygen index can reach more than 33%; however, the flame retardant effect of the above organic flame retardant system when used in TPU materials still needs to be further improved, and after the organic flame retardant system is blended with polyurethane materials, the mechanical properties of the polyurethane materials, such as toughness, modulus and the like, are greatly reduced, the compatibility of the organic flame retardant system after being blended with the polyurethane materials is poor, the organic flame retardant system is difficult to uniformly disperse in the polyurethane materials through processing, the price of the organic flame retardant system is relatively expensive, and the application of the organic flame retardant system is limited.
Therefore, on the basis of the prior art, a person skilled in the art needs to develop a novel flame retardant system with good flame retardant performance, so that the flame retardant system is low in cost, suitable for thermoplastic polyurethane elastomer materials, simple and convenient in processing technology, and uniform in dispersion in polyurethane elastomers, and cannot cause reduction of mechanical properties of TPU materials, and meanwhile, the obtained TPU materials have excellent flame retardant performance, the flame retardant performance reaches the vertical combustion V0 level, and the limit oxygen index can reach more than 33%.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a novel flame-retardant system with good flame-retardant property, so that the flame-retardant system is low in cost, suitable for thermoplastic polyurethane elastomer materials, simple and convenient in processing technology, and uniform in dispersion in polyurethane elastomers, and can not cause the reduction of the mechanical property of TPU materials, and meanwhile, the obtained TPU materials have excellent flame-retardant property, the flame-retardant property reaches the vertical combustion V0 grade, and the limit oxygen index can reach more than 33%.
To achieve the purpose, one of the purposes of the invention is to provide a TPU material with flame retardant property reaching a vertical burning V0 grade, which is obtained by mixing the following components in parts by weight:
the phosphorus-nitrogen flame-retardant system can be 37 parts, 39 parts, 41 parts, 43 parts, 45 parts, 47 parts, 49 parts, 51 parts, 53 parts, 55 parts, 57 parts, 59 parts, 61 parts or 63 parts by weight, the char forming agent can be 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts or 9 parts by weight, and the flame-retardant auxiliary agent can be 5 parts, 7 parts, 9 parts, 11 parts, 13 parts or 14 parts by weight.
The phosphorus-nitrogen flame-retardant system is prepared by blending melamine cyanurate and aluminum diethylphosphinate according to a weight ratio of 0.5-1.5: 1 (for example, 0.6:1, 0.7:1, 0.8:1, 0.9:1, 1:1, 1.1:1, 1.2:1, 1.3:1 or 1.4: 1) under the above proportioning conditions, and the obtained phosphorus-nitrogen flame-retardant system has an optimal flame-retardant effect and also has an optimal synergistic effect with a char-forming agent and a flame-retardant auxiliary agent.
Preferably, the TPU material is blended from the following components, by weight:
preferably, the charring agent is lignin which is a compound obtained by purifying waste wood materials and containing polyphenyl, alkyl chains and phenolic hydroxyl groups, the lignin is easy to burn when being used alone, but when the lignin is used together with a flame retardant and a flame retardant auxiliary agent, when the lignin is blended in a polyurethane system, the phenolic hydroxyl groups in the lignin can be dehydrated at high temperature and react with other benzene rings for ring merging, crosslinking and the like to obtain a heat-insulating charring structure, the charring effect is excellent, the lignin has various phenyl and hydroxyl functional groups, the effect of a toughening agent can be achieved when the lignin is blended in the polyurethane, and the obtained TPU material can still maintain high mechanical properties such as toughness at high temperature.
Preferably, the lignin has a number average molecular weight of 1000 to 10000, such as 1500, 2000, 2500, 3000, 3500, 4000, 4500, 5000, 5500, 6000, 6500, 7000, 7500, 8000, 8500, 9000, or 9500.
Preferably, the number average molecular weight of the lignin is 3000-8000, and under the molecular weight, the synergistic effect among the lignin, the flame retardant and the flame retardant auxiliary agent is optimal.
Preferably, the flame retardant auxiliary agent is any one or a mixture of at least two of hydrotalcite, organic montmorillonite, zinc borate or rare earth oxide.
Preferably, the flame retardant auxiliary agent is a mixture of zinc borate and organic montmorillonite in a weight ratio of 0.4-2: 1 (e.g., 0.5:1, 0.6:1, 0.7:1, 0.8:1, 0.9:1, 1:1, 1.1:1, 1.2:1, 1.3:1, 1.4:1, 1.5:1, 1.6:1, 1.7:1, 1.8:1, or 1.9: 1).
Preferably, the thermoplastic polyurethane is a polyether polyurethane.
The invention also aims to provide a preparation method of the TPU material, which comprises the following steps:
uniformly mixing the thermoplastic polyurethane, the phosphorus-nitrogen flame-retardant system, the char forming agent and the flame-retardant auxiliary agent according to the formula ratio, and placing the mixture into an internal mixer for mixing to obtain the TPU material.
Preferably, the mixing is carried out homogeneously in a high-speed mixer.
Preferably, the temperature of the kneading is 160 to 190 ℃, for example 165 ℃, 170 ℃, 175 ℃, 180 ℃, 185 ℃ or 188 ℃.
Preferably, the mixing time is 0.5 to 1 hour, for example, 0.6 hour, 0.65 hour, 0.7 hour, 0.75 hour, 0.8 hour, 0.85 hour, 0.9 hour, or 0.95 hour.
The recitation of numerical ranges herein includes not only the above-recited numerical values, but also any numerical values between non-recited numerical ranges, and is not intended to be exhaustive or to limit the invention to the precise numerical values encompassed within the range for brevity and clarity.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the phosphorus-nitrogen flame retardant system is applied to thermoplastic polyurethane, and the proportion relationship among the components is changed, so that the TPU material which has excellent flame retardant property, the vertical combustion grade reaches V0 grade, the oxygen index reaches 39% and the mechanical property is basically not changed can be obtained, and the requirements of most TPU material use occasions on the flame retardant property can be met.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments.
Example 1
TPU material 1 was prepared by the following method:
10kg of polyether type thermoplastic polyurethane, 2.5kg of melamine cyanurate, 2.5kg of aluminum diethylphosphinate, 0.8kg of charring agent lignin with the number average molecular weight of 5000, 0.5kg of zinc borate and 0.5kg of organic montmorillonite are uniformly mixed by a high-speed mixer, and are placed into an internal mixer for mixing, wherein the mixing temperature is 180 ℃, and the mixing time is 40min, so that the TPU material 1 is obtained.
Example 2
TPU material 2 was prepared by the following method:
10kg of polyether type thermoplastic polyurethane, 3kg of melamine cyanurate, 2kg of aluminum diethylphosphinate, 0.8kg of charring agent lignin with the number average molecular weight of 5000, 0.5kg of zinc borate and 0.5kg of organic montmorillonite are uniformly mixed by a high-speed mixer, and are placed into an internal mixer for mixing, wherein the mixing temperature is 180 ℃, and the mixing time is 40min, so that the TPU material 2 is obtained.
Example 3
TPU material 3 was prepared by the following method:
10kg of polyether type thermoplastic polyurethane, 2kg of melamine cyanurate, 4kg of aluminum diethylphosphinate, 0.8kg of charring agent lignin with the number average molecular weight of 5000, 0.5kg of zinc borate and 0.5kg of organic montmorillonite are uniformly mixed by a high-speed mixer, and are placed into an internal mixer for mixing, wherein the mixing temperature is 180 ℃, and the mixing time is 40min, so that the TPU material 3 is obtained.
Example 4
TPU material 4 was prepared by the following method:
10kg of polyether type thermoplastic polyurethane, 2.5kg of melamine cyanurate, 2.5kg of aluminum diethylphosphinate, 0.8kg of charring agent lignin with the number average molecular weight of 5000, 1kg of zinc borate and 0.5kg of organic montmorillonite are uniformly mixed by a high-speed mixer, and are placed into an internal mixer for mixing, wherein the mixing temperature is 180 ℃, and the mixing time is 40min, so that the TPU material 4 is obtained.
Example 5
TPU material 5 was prepared by the following method:
10kg of polyether type thermoplastic polyurethane, 2.5kg of melamine cyanurate, 2.5kg of aluminum diethylphosphinate, 0.8kg of charring agent lignin with the number average molecular weight of 5000, 0.09kg of zinc borate and 0.21kg of organic montmorillonite are uniformly mixed by a high-speed mixer, and are placed into an internal mixer for mixing, wherein the mixing temperature is 180 ℃, and the mixing time is 40min, so that the TPU material 5 is obtained.
Example 6
TPU material 6 was prepared by the following method:
10kg of polyether type thermoplastic polyurethane, 2.5kg of melamine cyanurate, 2.5kg of aluminum diethylphosphinate, 0.2kg of charring agent lignin with the number average molecular weight of 5000, 0.5kg of zinc borate and 0.5kg of organic montmorillonite are uniformly mixed by a high-speed mixer, and are placed into an internal mixer for mixing, wherein the mixing temperature is 160 ℃, and the mixing time is 30min, so that the TPU material 6 is obtained.
Example 7
TPU material 7 was prepared by the following method:
10kg of polyether type thermoplastic polyurethane, 2.5kg of melamine cyanurate, 2.5kg of aluminum diethylphosphinate, 1kg of charring agent lignin with the number average molecular weight of 5000, 0.5kg of zinc borate and 0.5kg of organic montmorillonite are uniformly mixed by a high-speed mixer, and are placed into an internal mixer for mixing at the temperature of 190 ℃ for 60min to obtain the TPU material 7.
Example 8
TPU material 8 was prepared by the following method:
10kg of polyether type thermoplastic polyurethane, 2.5kg of melamine cyanurate, 2.5kg of aluminum diethylphosphinate, 0.8kg of charring agent lignin with the number average molecular weight of 8000, 0.5kg of zinc borate and 0.5kg of organic montmorillonite are uniformly mixed by a high-speed mixer, and are placed into an internal mixer for mixing, wherein the mixing temperature is 180 ℃, and the mixing time is 40min, so that the TPU material 8 is obtained.
Example 9
TPU material 9 was prepared by the following method:
10kg of polyether type thermoplastic polyurethane, 2.5kg of melamine cyanurate, 2.5kg of aluminum diethylphosphinate, 0.8kg of charring agent lignin with the number average molecular weight of 3000, 0.5kg of zinc borate and 0.5kg of organic montmorillonite are uniformly mixed by a high-speed mixer, and are placed into an internal mixer for mixing, wherein the mixing temperature is 180 ℃, and the mixing time is 40min, so that the TPU material 9 is obtained.
Example 10
TPU material 10 was prepared by the following method:
10kg of polyether type thermoplastic polyurethane, 2.5kg of melamine cyanurate, 2.5kg of aluminum diethylphosphinate, 0.8kg of charring agent lignin with the number average molecular weight of 12000, 0.5kg of zinc borate and 0.5kg of organic montmorillonite are uniformly mixed by a high-speed mixer, and the mixture is placed into an internal mixer for mixing, wherein the mixing temperature is 180 ℃, and the mixing time is 40min, so that the TPU material 10 is obtained.
Example 11
TPU material 11 was prepared by the following method:
10kg of polyether type thermoplastic polyurethane, 2.5kg of melamine cyanurate, 2.5kg of aluminum diethylphosphinate, 1.2kg of charring agent lignin with the number average molecular weight of 5000, 0.5kg of zinc borate and 0.5kg of organic montmorillonite are uniformly mixed by a high-speed mixer, and are placed into an internal mixer for mixing, wherein the mixing temperature is 180 ℃, and the mixing time is 40min, so that the TPU material 11 is obtained.
Example 12
TPU material 12 was prepared by the following method:
10kg of polyether type thermoplastic polyurethane, 2.5kg of melamine cyanurate, 2.5kg of aluminum diethylphosphinate, 0.8kg of charring agent piperazine pyrophosphate, 0.5kg of zinc borate and 0.5kg of organic montmorillonite are uniformly mixed by a high-speed mixer, and are placed into an internal mixer for mixing, wherein the mixing temperature is 180 ℃, and the mixing time is 40min, so that the TPU material 12 is obtained.
Comparative example 1
TPU material 13 was prepared by the following method:
10kg of polyether type thermoplastic polyurethane, 3.5kg of melamine cyanurate, 3.5kg of aluminum diethylphosphinate, 0.8kg of charring agent lignin with the number average molecular weight of 5000, 0.5kg of zinc borate and 0.5kg of organic montmorillonite are uniformly mixed by a high-speed mixer, and are placed into an internal mixer for mixing, wherein the mixing temperature is 180 ℃, and the mixing time is 40min, so that the TPU material 13 is obtained.
Comparative example 2
TPU material 14 was prepared by the following method:
10kg of polyether type thermoplastic polyurethane, 1.5kg of melamine cyanurate, 1.5kg of aluminum diethylphosphinate, 0.8kg of charring agent lignin with the number average molecular weight of 5000, 0.5kg of zinc borate and 0.5kg of organic montmorillonite are uniformly mixed by a high-speed mixer, and are placed into an internal mixer for mixing, wherein the mixing temperature is 180 ℃, and the mixing time is 40min, so that the TPU material 14 is obtained.
Comparative example 3
The TPU material 15 was prepared by the following method:
10kg of polyether type thermoplastic polyurethane, 2.5kg of melamine cyanurate, 2.5kg of aluminum diethylphosphinate, 0.5kg of zinc borate and 0.5kg of organic montmorillonite are uniformly mixed by a high-speed mixer, and are placed into an internal mixer for mixing, wherein the mixing temperature is 180 ℃, and the mixing time is 40min, so that the TPU material 15 is obtained.
The properties of the TPU materials 1 to 15 obtained in the above examples and comparative examples were tested according to the following test methods, and the test results are shown in Table 1:
(1) mechanical Property test
The elongation at break of the obtained TPU materials 1 to 15 was tested according to the method described in JIS K7311-1995 "test method for thermoplastic polyurethane elastomer".
(2) Test for flame retardancy
The flame retardant performance of the TPU material is characterized by testing the vertical combustion grade and the oxygen index of 1-15 obtained by the method described in GB/T10707-2008 'determination Standard for rubber Combustion Performance', wherein the flame retardant performance is better when the vertical combustion grade is V0 grade and the oxygen index is higher.
TABLE 1 comparison table of TPU material 1-15 performance
| TPU material | Vertical combustion class (grade) | Oxygen index (%) | Elongation at Break (%) |
| 1 | V0 | 39 | 591 |
| 2 | V0 | 38 | 566 |
| 3 | V0 | 37 | 581 |
| 4 | V0 | 37 | 585 |
| 5 | V0 | 37 | 580 |
| 6 | V0 | 35 | 567 |
| 7 | V0 | 38 | 575 |
| 8 | V0 | 37 | 584 |
| 9 | V0 | 37 | 570 |
| 10 | V0 | 37 | 562 |
| 11 | V0 | 36 | 571 |
| 12 | V0 | 37 | 520 |
| 13 | V0 | 32 | 532 |
| 14 | V1 | 33 | 565 |
| 15 | V1 | 30 | 514 |
It can be seen from the comparison of the performances of the TPU materials obtained in the example 1 and the examples 12 and the comparative example 3 in table 1 that the char-forming agent in the invention has a very significant influence on the flame retardant performance, and when the lignin material is used as the char-forming agent, the char-forming effect is better than that of the char-forming agent compounded with the flame retardant, and simultaneously the toughness of the obtained TPU material can be significantly improved, so that the elongation at break is improved by about 15%.
As can be seen from the comparison of the performances between the TPU materials obtained in the examples 1 to 5 and the comparative examples 1 to 2 in the table 1, when the content of the phosphorus-nitrogen flame-retardant system in the components is too much or too little or the component proportion thereof is changed, the flame retardant performance and the mechanical performance of the obtained TPU material are correspondingly reduced, but the reduction is not obvious.
In conclusion, the phosphorus-nitrogen flame retardant system is applied to the thermoplastic polyurethane, and the proportion relationship among the components is changed, so that the TPU material which has excellent flame retardant property, the vertical combustion grade reaches V0 grade, the oxygen index reaches 39% and the mechanical property is basically not changed can be obtained, and the requirements of most TPU material use occasions on the flame retardant property can be met.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (7)
1. The TPU material with the flame retardant property reaching a vertical burning V0 grade is characterized by being prepared by mixing the following components in parts by weight:
the phosphorus-nitrogen flame-retardant system is obtained by blending melamine cyanurate and aluminum diethylphosphinate according to the weight ratio of 0.5-1.5: 1;
the carbon forming agent is lignin, and the number average molecular weight of the lignin is 3000-8000;
the flame-retardant auxiliary agent is a mixture of zinc borate and organic montmorillonite in a weight ratio of 0.4-2: 1.
2. The TPU material of claim 1, wherein the TPU material is obtained by blending, in parts by weight:
3. the TPU material of claim 1 wherein the thermoplastic polyurethane is a polyether polyurethane.
4. A process for preparing the TPU material of any of claims 1 through 3 comprising the steps of:
uniformly mixing the thermoplastic polyurethane, the phosphorus-nitrogen flame-retardant system, the char forming agent and the flame-retardant auxiliary agent according to the formula ratio, and placing the mixture into an internal mixer for mixing to obtain the TPU material.
5. The method of claim 4, wherein the mixing is performed in a high-speed mixer.
6. The method according to claim 4, wherein the kneading temperature is 160 to 190 ℃.
7. The method according to claim 4, wherein the kneading is carried out for 0.5 to 1 hour.
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| CN114437425B (en) * | 2020-11-02 | 2023-08-15 | 中国石油化工股份有限公司 | Thermoplastic vulcanized rubber composition, thermoplastic vulcanized rubber, and preparation method and application thereof |
| US20240034857A1 (en) * | 2020-12-21 | 2024-02-01 | Basf Se | Flame-retarded thermoplastic polyurethane |
| CN112812366B (en) * | 2020-12-30 | 2022-08-09 | 浙江新化化工股份有限公司 | Flame-retardant composition and application thereof, PBT composite material and preparation method thereof |
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