CN112625405B - Low-smoke density halogen-free flame-retardant reinforced PBT/PET compound and preparation method and application thereof - Google Patents
Low-smoke density halogen-free flame-retardant reinforced PBT/PET compound and preparation method and application thereof Download PDFInfo
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- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
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Abstract
The invention discloses a low-smoke density halogen-free flame-retardant reinforced PBT/PET compound, and a preparation method and application thereof. The low-smoke density halogen-free flame-retardant reinforced PBT/PET compound comprises the following components: PBT, PET, glass fiber, halogen-free flame retardant, epoxy resin, boehmite, kaolin and magnesium stearate; the weight ratio of the PBT to the PET is (1-3) to 1, and the particle size D50 of the magnesium stearate is less than or equal to 5 mu m. By compounding PET with PBT in a proper proportion and the synergistic effect of boehmite, kaolin and magnesium stearate with specific particle size, the smoke density Ds max of the PBT/PET compound is less than or equal to 150, and meanwhile, the PET/PET product prepared by using the PBT/PET compound has high appearance glossiness. The low-smoke density halogen-free flame-retardant reinforced PBT/PET compound is suitable for occasions with extremely high requirements on smoke density and good appearance of products.
Description
Technical Field
The invention relates to the technical field of engineering plastics, and particularly relates to a low-smoke density halogen-free flame-retardant reinforced PBT/PET compound, and a preparation method and application thereof.
Background
Plastic materials are generally produced with a large amount of smoke in the combustion process, and can cause environmental pollution and great harm to human bodies. In recent years, with the development of plastic flame retardant technology, low-smoke flame retardant has become a new direction for the development of flame retardant plastics. The demand of industries such as rail transit, building materials, cables and the like on the aspect of low smoke and flame retardance is more obvious and standardized, and the industries have clear requirements that plastic parts in application must reach the smoke density level 2 or above required by EN45545-2 standard (the smoke density Ds max is less than or equal to 300 required by ISO5659-2 test level 2).
Polybutylene terephthalate (PBT) is polymerized by terephthalic acid and butanediol through polycondensation reaction, and the PBT material reinforced by glass fiber is widely applied to lighting lamps, cooling fans, connectors, coil frameworks, electric appliance shells and other electronic and electrical components at present. With the development of the technology, people have higher and higher requirements on the performance of the PBT modified material, and meanwhile, the pressure of the cost also forces the change, and under the condition, the glass fiber reinforced PBT/PET alloy material with better performance is produced. Polyethylene terephthalate (PET) has good heat resistance and lower cost, and the PET can effectively prevent glass fiber from being exposed in a glass fiber reinforced PBT system, thereby having the effect of high light on the surface of the product.
When the glass fiber reinforced PBT/PET alloy is applied to the industries of rail transit, building materials, cables and the like, the flame retardance of the glass fiber reinforced PBT/PET alloy is indispensable. The use of halogen flame retardants in the market is still the mainstream at present, subject to factors such as price and performance. However, with the increasing environmental protection concerns of the european union and countries around the world and the continuous introduction of various environmental regulations in recent years, the trend of non-halogenation of plastic materials has not been reversible. Chinese patent application CN101460591A discloses a halogen-free flame-retardant molding composition, which comprises thermoplastic polyesters such as PBT and PET, a fiber reinforcing agent, a halogen-free flame retardant and other components, and the prepared halogen-free flame-retardant molding composition has good flame retardant property and impact resistance.
However, the research on the smoke suppression performance of the halogen-free flame-retardant reinforced PBT/PET alloy is less at present, and although the smoke density of the material is reduced by adding the smoke suppression additive commonly used in PBT and PET, the toughness of the material is greatly reduced, so that the application of the material in the field with higher requirements on the smoke suppression performance is limited.
Therefore, the development of a halogen-free flame retardant reinforced PBT/PET compound with low smoke density and good toughness is needed.
Disclosure of Invention
The invention aims to overcome the defects of fiber floating on the surface, high smoke density and poor toughness of the prior art, and provides the low-smoke-density flame-retardant reinforced PBT/PET compound which has good glossiness, flame retardance and toughness and smoke density reaching the level of EN45545-2 standard level 3.
The invention also aims to provide a preparation method of the low-smoke density halogen-free flame-retardant reinforced PBT/PET compound.
The invention also aims to provide application of the low-smoke density halogen-free flame-retardant reinforced PBT/PET compound.
In order to solve the technical problems, the invention adopts the technical scheme that:
a low-smoke density halogen-free flame-retardant reinforced PBT/PET compound comprises the following components in parts by weight:
the total weight of the PBT and the PET is 42-70 parts, and the weight ratio of the PBT to the PET is (1-3) to 1;
10-30 parts of glass fiber,
15-25 parts of a halogen-free flame retardant,
0.5 to 1 part of epoxy resin,
2-4 parts of boehmite,
2-8 parts of kaolin clay, namely,
1-4 parts of magnesium stearate;
particle size D of the magnesium stearate50≤5μm。
The inventor finds that in a halogen-free flame-retardant system, when the sum of the weight of polybutylene terephthalate (PBT) and polyethylene terephthalate (PET) is 42-70 parts and the weight ratio of PBT to PET is (1-3) to 1, the floating fiber can be obviously reduced, the surface gloss of the material can be improved, and the smoke density level of the composite can be effectively reduced. Meanwhile, the PBT/PET compound can obtain excellent smoke suppression performance under the condition of maintaining good toughness of the material by adding the three components of boehmite, kaolin and magnesium stearate into a halogen-free flame-retardant reinforced PBT/PET system in proper weight. According to the technical scheme, the smoke density Ds max of the prepared low-smoke-density halogen-free flame-retardant reinforced PBT/PET compound is less than or equal to 150 by using an ISO5659-2-2016 method, and meets the EN45545-2 standard grade 3 requirement. The particle size D of the magnesium stearate in the technical scheme of the invention50The particle size of magnesium stearate is required to be less than or equal to 5 mu m, and if the particle size of magnesium stearate is too large, the smoke suppression effect of the invention cannot be achieved.
The magnesium stearate is preferably a product of Shangxi Macro-Yuan chemical industry brand YZM-32C.
The molecular formula of the boehmite is gamma-AlOOH, and the average grain size of the boehmite is more than or equal to 10 nm.
Due to the characteristics of low density, larger surface area, special structure and morphology and the like, the boehmite with lower grain size has special physical and chemical properties different from those of the boehmite with large grain size, and the smoke generation amount of the material during combustion can be more remarkably reduced in a halogen-containing flame-retardant reinforced PBT/PET system. Preferably, the boehmite preferably has an average grain size of 10 to 20 nm.
The boehmite is preferably a product of Nanjing Epsilon nano-material Co., Ltd, and the model is boehmite 235.
The inventor finds that the kaolin with moderate acidity and lower particle size can play a better smoke suppression effect in a PBT/PET system.
Preferably, the particle size of the kaolin is preferably D50≤0.5μm。
Preferably, the pH value of the kaolin is preferably 4-5.
The kaolin is preferably a product of the Hangzhou Chongke new materials Co., Ltd, with the mark of Eckalite 1 PLUS.
Preferably, the weight ratio of the boehmite to the kaolin to the magnesium stearate is 1: 1-2: 0.5-1.
The inventor researches and discovers that when boehmite, kaolin and magnesium stearate are compounded in a weight ratio of 1: 1-2: 0.5-1, the prepared halogen-free flame-retardant reinforced PBT/PET compound can obtain a better smoke suppression effect. When the weight of boehmite, kaolin and magnesium stearate is too much, the toughness of the PBT/PET compound is deteriorated; when the weight of boehmite, kaolin and magnesium stearate is too small, it is difficult to obtain a good smoke suppressing effect.
Preferably, the PBT has an intrinsic viscosity of 1.1-1.4 dL/g at 25 ℃, and the PET has an intrinsic viscosity of 0.7-0.9 dL/g at 25 ℃. The intrinsic viscosity test method is in accordance with GB/T14190-2017.
In the intrinsic viscosity range, the PBT/PET compound can obtain better comprehensive performance, and particularly, the PBT/PET compound is beneficial to maintaining good toughness.
The halogen-free flame retardant is a compound of hypophosphite and melamine phosphate.
Preferably, the halogen-free flame retardant is a compound of organic aluminum hypophosphite and melamine polyphosphate.
Preferably, the weight ratio of the organic aluminum hypophosphite to the melamine polyphosphate is (2-5) to 1.
Preferably, the glass fibers are treated with a coupling agent.
More preferably, the coupling agent is a blend of N- (beta-aminoethyl) -gamma-aminopropyltrimethoxysilane, gamma-methacryloxypropyltrimethoxysilane, and isopropylbis (methacryloyl) isostearyl titanate in a weight ratio of 1: 2: 1.
Preferably, the epoxy resin is bisphenol A type glycidyl ether, and the epoxy equivalent is 2500-3100 g/eq. The epoxy equivalent test method is in accordance with GB/T4612-2008.
The addition of the epoxy resin can obviously improve the performance stability of the PBT/PET compound.
The invention also provides a preparation method of the low-smoke density halogen-free flame-retardant reinforced PBT/PET compound, which comprises the following steps:
mixing an epoxy resin with boehmite, kaolin, and magnesium stearate to form a first premix;
and adding the PBT, the PET, the glass fiber, the halogen-free flame retardant and the first premix into an extruder, and mixing, dispersing, melting, extruding and granulating to obtain the low-smoke density halogen-free flame-retardant reinforced PBT/PET compound.
Preferably, the extruder is a twin screw extruder.
More preferably, the temperature of the twin-screw extruder from the feeding port to the head in the first zone is 200-230 ℃, the temperature of the twin-screw extruder in the second zone is 240-260 ℃, the temperature of the third zone is 235-255 ℃, the temperature of the fourth zone is 235-255 ℃, the temperature of the fifth zone is 235-255 ℃, the temperature of the sixth zone is 240-260 ℃, the temperature of the seventh zone is 240-260 ℃, the temperature of the eighth zone is 220-240 ℃, the temperature of the ninth zone is 220-240 ℃, the temperature of the tenth zone is 240-260 ℃, and the screw rotating speed of the twin-screw extruder is 200-450 revolutions per minute.
The invention also protects the application of the low-smoke density halogen-free flame-retardant reinforced PBT/PET compound in preparing low-smoke density flame-retardant reinforced PBT/PET products.
Compared with the prior art, the invention has the beneficial effects that:
the invention develops a halogen-free flame-retardant reinforced PBT/PET compound with low smoke density and good surface glossiness. The PBT/PET compound can maintain good toughness, the smoke density reaches grade 3 of the smoke density required by EN45545-2 standard, the smoke density Ds max of ISO5659-2 test is less than or equal to 150, and meanwhile, the PET/PET product prepared by the PBT/PET compound has high appearance glossiness. The low-smoke density halogen-free flame-retardant reinforced PBT/PET compound is suitable for occasions with extremely high requirements on smoke density and good appearance of products.
Detailed Description
The present invention will be further described with reference to the following embodiments.
The raw materials in the examples are all commercially available;
reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Examples 1 to 19
The contents of the components in the PBT/PET composites of examples 1 to 19 are shown in Table 1.
The preparation method comprises the following steps: mixing an epoxy resin with boehmite, kaolin, magnesium stearate to form a first premix according to table 1; and adding the PBT, the PET, the glass fiber, the halogen-free flame retardant and the first premix into a double-screw extruder, and mixing, dispersing, melting, extruding and granulating to obtain the low-smoke density halogen-free flame-retardant reinforced PBT/PET compound.
The temperature of a first zone from a feeding port to a machine head of the double-screw extruder is 200-230 ℃, the temperature of a second zone is 240-260 ℃, the temperature of a third zone is 235-255 ℃, the temperature of a fourth zone is 235-255 ℃, the temperature of a fifth zone is 235-255 ℃, the temperature of a sixth zone is 240-260 ℃, the temperature of a seventh zone is 240-260 ℃, the temperature of an eighth zone is 220-240 ℃, the temperature of a ninth zone is 220-240 ℃, the temperature of a tenth zone is 240-260 ℃, and the screw rotating speed of the double-screw extruder is 200-450 revolutions per minute.
TABLE 1 component content (parts by weight) of PBT/PET composite of examples 1 to 19
TABLE 1 component content (parts by weight) of PBT/PET composites of the subsequent examples 1 to 19
Comparative examples 1 to 8
The contents of the components in the PBT/PET composites of comparative examples 1 to 8 are shown in Table 2.
The preparation method comprises the following steps: mixing an epoxy resin with boehmite, kaolin, magnesium stearate to form a first premix according to table 2; and adding the PBT, the PET, the glass fiber, the halogen-free flame retardant and the first premix into a double-screw extruder, and mixing, dispersing, melting, extruding and granulating to obtain the low-smoke density halogen-free flame-retardant reinforced PBT/PET compound.
The temperature of a first zone from a feeding port to a machine head of the double-screw extruder is 200-230 ℃, the temperature of a second zone is 240-260 ℃, the temperature of a third zone is 235-255 ℃, the temperature of a fourth zone is 235-255 ℃, the temperature of a fifth zone is 235-255 ℃, the temperature of a sixth zone is 240-260 ℃, the temperature of a seventh zone is 240-260 ℃, the temperature of an eighth zone is 220-240 ℃, the temperature of a ninth zone is 220-240 ℃, the temperature of a tenth zone is 240-260 ℃, and the screw rotating speed of the double-screw extruder is 200-450 revolutions per minute.
TABLE 2 component contents (parts by weight) of PBT/PET composites of comparative examples 1 to 8
Performance testing
The PBT/PET compound prepared in the above examples and comparative examples was tested for properties according to the following test methods:
gloss: injecting the PBT/PET compound into a color plate with a smooth surface, and testing by using a gloss meter, wherein the incidence angle is 60 degrees, and the size of the color plate is more than or equal to 60 x 60 mm;
flame retardancy @1.0 mm: UL94: 2003;
smoke density Ds max @1.0 mm: ISO5659-2: 2012;
notched impact strength: ISO180:2000, units kJ/m2
Test results
The results of the performance tests of the PBT/PET composites of the examples are shown in Table 3, and the results of the performance tests of the comparative PBT/PET composites are shown in Table 4.
TABLE 3 results of the Performance test of examples 1 to 18
As can be seen from Table 3, the PBT/PET compound prepared by each example of the application has good glossiness and toughness, the flame retardance is V0, and the smoke density reaches the smoke density grade 3 standard required by EN45545-2 standard. According to the embodiments 1 and 6 to 9, when the boehmite, the kaolin and the magnesium stearate are compounded in the weight ratio of 1: 1-2: 0.5-1, the PBT/PET compound has lower smoke density. According to the embodiments 1 and 13 to 15, the boehmite average grain size is preferably 10 to 20nm, and the kaolin particle size is preferably D50Less than or equal to 0.5 mu m, and the preferable pH value of the kaolin is 4-5.
TABLE 4 Performance test results for comparative examples 1-8
According to the detection results in the table 4, according to the comparative examples 1 to 4, when one or more of boehmite, kaolin and magnesium stearate is/are lack of one component, the PBT/PET compound has good flame retardance and glossiness, but has high smoke density, and Ds max is not less than or equal to 350, so that the requirement of low smoke density cannot be met. From comparative example 5, when the particle size of magnesium stearate is too high, the smoke density is 189, and the smoke density grade 3 required by EN45545-2 standard is not achieved. Compared with the comparative examples 6-7, when the weight ratio of the PBT to the PET is beyond the range of the technical scheme, the glossiness of the PBT/PET compound is poor. Compared with the comparative example 8, the addition amount of PBT and PET is too large, and the flame retardance of the PBT/PET compound is HB, so that the actual flame retardant requirement cannot be met.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (7)
1. The low-smoke density halogen-free flame-retardant reinforced PBT/PET compound is characterized by comprising the following components in parts by weight:
the total weight of the PBT and the PET is 42-70 parts, and the weight ratio of the PBT to the PET is (1-3) to 1; 10-30 parts of glass fiber, 15-25 parts of halogen-free flame retardant, 0.5-1 part of epoxy resin, 2-4 parts of boehmite, 2-8 parts of kaolin and 1-4 parts of magnesium stearate;
particle size D of the magnesium stearate50≤5μm；
The average grain size of the boehmite is 10-20 nm;
the particle diameter of the kaolin is D50Less than or equal to 0.5 mu m; the pH value of the kaolin is 4-5.
2. The low-smoke density halogen-free flame-retardant reinforced PBT/PET compound as claimed in claim 1, wherein the weight ratio of boehmite, kaolin and magnesium stearate is 1: 1-2: 0.5-1.
3. The low smoke density halogen-free flame retardant reinforced PBT/PET compound of claim 1 wherein the PBT has an intrinsic viscosity of 1.1-1.4 dL/g at 25 ℃ and the PET has an intrinsic viscosity of 0.7-0.9 dL/g at 25 ℃.
4. The low smoke density halogen-free flame retardant reinforced PBT/PET compound of claim 1, wherein the halogen-free flame retardant is a compound of hypophosphite and melamine phosphate.
5. The low-smoke density halogen-free flame-retardant reinforced PBT/PET compound as claimed in claim 1, wherein the epoxy resin is bisphenol A glycidyl ether, and the epoxy equivalent is 2500-3100 g/eq.
6. The preparation method of the low-smoke density halogen-free flame-retardant reinforced PBT/PET compound as claimed in any one of claims 1 to 5, characterized by comprising the following steps:
mixing an epoxy resin with boehmite, kaolin, and magnesium stearate to form a first premix;
and adding the PBT, the PET, the glass fiber, the halogen-free flame retardant and the first premix into an extruder, and mixing, dispersing, melting, extruding and granulating to obtain the low-smoke density halogen-free flame-retardant reinforced PBT/PET compound.
7. The application of the low-smoke density halogen-free flame-retardant reinforced PBT/PET compound disclosed by any one of claims 1-5 in preparation of a low-smoke density flame-retardant reinforced PBT/PET product.
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| PCT/CN2021/092769 WO2022110664A1 (en) | 2020-11-26 | 2021-05-10 | Low-smoke density halogen-free flame-retardant reinforced pbt/pet composite, and preparation method therefor and application thereof |
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| CN112592566B (en) * | 2020-11-26 | 2022-03-22 | 金发科技股份有限公司 | Low-smoke-density halogen-containing flame-retardant reinforced PBT/PET compound and preparation method and application thereof |
| CN114605789B (en) * | 2022-02-28 | 2023-12-05 | 金发科技股份有限公司 | PBT composite material and preparation method and application thereof |
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