CN110982261A - Flame-retardant reinforced high-temperature-resistant nylon composite material - Google Patents
Flame-retardant reinforced high-temperature-resistant nylon composite material Download PDFInfo
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- CN110982261A CN110982261A CN201911323181.0A CN201911323181A CN110982261A CN 110982261 A CN110982261 A CN 110982261A CN 201911323181 A CN201911323181 A CN 201911323181A CN 110982261 A CN110982261 A CN 110982261A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/0405—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres
- C08J5/043—Reinforcing macromolecular compounds with loose or coherent fibrous material with inorganic fibres with glass fibres
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/06—Polyamides derived from polyamines and polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2439/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Derivatives of such polymers
- C08J2439/04—Homopolymers or copolymers of monomers containing heterocyclic rings having nitrogen as ring member
- C08J2439/06—Homopolymers or copolymers of N-vinyl-pyrrolidones
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Abstract
The invention discloses a flame-retardant reinforced high-temperature-resistant nylon composite material which comprises the following raw materials in parts by weight: 30-45 parts of high-temperature nylon resin, 30-55 parts of glass fiber, 10-20 parts of a flame retardant and 0.1-2.0 parts of polyvinylpyrrolidone. According to the invention, the polyvinylpyrrolidone is introduced into the formula system of the flame-retardant reinforced high-temperature-resistant nylon composite material, so that the initial whiteness of the composite material can be obviously improved, titanium dioxide is not required to be added when a light-color product is prepared, the L value of the initial whiteness of the obtained molded product is more than 80, and the prepared molded product has an excellent visual effect and is beneficial to reducing the cost; and the molded product has smooth surface, thus effectively solving the problem of fiber floating on the surface of the product.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a flame-retardant reinforced high-temperature-resistant nylon composite material.
Background
The flame-retardant high-temperature-resistant nylon has the performances of light weight, high temperature resistance, high strength, stable size, flame retardance and the like, and is widely applied to the automobile industry and the electronic industry. At present, when the flame-retardant high-temperature-resistant nylon is prepared, a flame retardant and glass fiber are usually added to improve the flame-retardant performance and the mechanical strength of the flame-retardant high-temperature-resistant nylon. However, the addition of the flame retardant can cause the molded product made of the flame-retardant high-temperature-resistant material to generate degradation and yellowing phenomena, which are specifically represented by that the yellow index of the resin is higher (yellowing), the whiteness value is reduced, and the appearance is dull, and the glass fiber can cause that the fiber floating on the surface of the molded product (the glass fiber is exposed on the surface of the product) is very obvious, so that the quality requirement of the product appearance is influenced.
At present, a large amount of titanium dioxide is usually added into a flame-retardant high-temperature-resistant nylon composite material to improve the whiteness of a product, but the titanium dioxide is high in price (15-30 yuan/kg), the usage amount is large (generally accounting for 3-5% of the total mass of the flame-retardant high-temperature-resistant material), the production cost of the flame-retardant high-temperature-resistant nylon material is greatly increased, in addition, the titanium dioxide is high in specific gravity, precipitation can be caused after long-time placement, the appearance attractiveness of the product is influenced, and most importantly, the addition of the titanium dioxide can reduce the mechanical property of the product, reduce the impact strength and the toughness, and influence.
In addition, the risk of thermal degradation and yellowing of the flame-retardant reinforced high-temperature-resistant nylon composite material in the extrusion granulation or injection molding process is reduced by adding an antioxidant and a heat stabilizer, most of high-temperature nylon resins have higher melting points, for example, the melting point of a PA6T/66 material reaches 310 ℃, and most of the antioxidant and the heat stabilizer have decomposition risk in the processing process at the processing temperature, so that the initial color effect of the material is improved generally by adding the antioxidant and the heat stabilizer, and the risk of mold pollution caused by the formation of a layer of oily matter due to the gradual enrichment of decomposition products at the exhaust position of the mold is also stored.
Disclosure of Invention
The invention aims to solve the problems of the flame-retardant high-temperature-resistant nylon composite material in the prior art, and provides the flame-retardant reinforced high-temperature-resistant nylon composite material which has a reasonable and scientific formula, can reduce the production cost, improve the whiteness of a molded product and effectively solve the problem of fiber floating on the surface of the molded product.
In order to achieve the purpose, the invention adopts the following technical scheme:
the flame-retardant reinforced high-temperature-resistant nylon composite material comprises the following raw materials in parts by weight: 30-45 parts of high-temperature nylon resin, 30-55 parts of glass fiber, 10-20 parts of a flame retardant and 0.1-2.0 parts of polyvinylpyrrolidone. L-values are a common measure of whiteness in the CIELAB color space, and typical whiteness L-values above 80 can be referred to as high whiteness. The whiteness of the product is high, visual comfort can be brought to people, the visual impression is better, the more obvious the grade is high, meanwhile, when the product is used for matching white and other light colors or more bright colors, color matching is easier, the more positive, more stable and uniform the color is, the inventor discovers that the polyvinylpyrrolidone is added into a formula system of the flame-retardant reinforced high-temperature-resistant nylon composite material in the production process, when a light-color product is prepared, titanium dioxide does not need to be added, the L value of the initial whiteness of the obtained composite material can reach more than 80, the prepared molded product has excellent visual effect, the surface of the molded product is smooth, and the problem of fiber floating is avoided.
Preferably, the high-temperature nylon resin is nylon 46 or semi-aromatic nylon with the melting point of 280-330 ℃.
Preferably, the semi-aromatic nylon is nylon 6T/66, nylon 6T/6I, nylon 6T/6, nylon 6T/1010, nylon 6T/1212, nylon 6T/612, nylon 6T/610, nylon 6I/66, nylon 6I/6, nylon 6I/1010, nylon 6I/1212, nylon 6I/612 or nylon 9T.
Preferably, the flame retardant is a brominated flame retardant.
Preferably, the brominated flame retardant is brominated polystyrene or polybrominated styrene.
Preferably, the raw materials of the flame-retardant reinforced high-temperature-resistant nylon composite material also comprise 3-6 parts by weight of a flame-retardant synergist.
Preferably, the flame retardant synergist is selected from antimony trioxide or anhydrous zinc borate.
Preferably, the glass fiber is a short glass fiber with the monofilament diameter of 6-13 μm and the length of 3-5 mm.
Preferably, the flame-retardant high-temperature nylon composite material is prepared by the following method: weighing the components according to the weight part ratio, and uniformly mixing the components except the glass fiber to obtain a premix; and then putting the obtained premix into a double-screw extruder, adding glass fiber by adopting a side feeding process, melting and mixing, extruding and granulating to obtain the flame-retardant reinforced high-temperature-resistant nylon composite material. The technological parameters of the double-screw extruder are as follows: the temperature of the feeding section is 290-320 ℃, the temperature of the melting plasticizing section is 280-330 ℃, the temperature of the mixing homogenizing section is 250-260 ℃, the temperature of the melt conveying section is 260-290 ℃, the temperature of the machine head is 290-330 ℃, and the rotating speed of a main machine of the double-screw extruder is 280-350 rpm.
A molded article made of a flame retardant reinforced high temperature resistant nylon composite.
Therefore, the invention has the following beneficial effects:
(1) the polyvinylpyrrolidone is introduced into the formula system of the flame-retardant reinforced high-temperature-resistant nylon composite material, so that the initial whiteness of the composite material can be obviously improved, titanium dioxide is not required to be added when a light-color product is prepared, the L value of the initial whiteness of the obtained molded product is more than 80, the prepared molded product has excellent visual effect, and the cost is favorably reduced;
(2) a small amount of polyvinylpyrrolidone is introduced into a formula system of the flame-retardant reinforced high-temperature-resistant nylon composite material, so that the surface of a molded product is smooth, and the problem of fiber floating on the surface of the product is effectively solved.
Detailed Description
The invention is further described below by means of specific embodiments.
Example 1
Weighing the components according to the weight ratio of 30kg of nylon 46, 30kg of short glass fibers (the diameter of each filament is 6 mu m, the length of each filament is 3mm), 10kg of flame retardant (brominated polystyrene), 3kg of antimony trioxide and 0.1kg of polyvinylpyrrolidone, and then uniformly mixing the components except the glass fibers to obtain a premix; and then putting the obtained premix into a double-screw extruder, adding glass fiber by adopting a side feeding process, melting and mixing, extruding and granulating to obtain the flame-retardant reinforced high-temperature-resistant nylon composite material, wherein the process parameters of the double-screw extruder are as follows: the temperature of the feeding section is 290 ℃, the temperature of the melting and plasticizing section is 280 ℃, the temperature of the mixing and homogenizing section is 250 ℃, the temperature of the melt conveying section is 260 ℃, the temperature of the machine head is 290 ℃, and the rotating speed of a main machine of the double-screw extruder is 280 rpm.
Comparative example 1
Comparative example 1 is identical to example 1 except that no polyvinylpyrrolidone is added, as compared to example 1.
Example 2
Weighing the components according to the weight ratio of 34kg of nylon 6T/66 to 50kg of short glass fiber (the monofilament diameter is 12 microns, the length is 4mm), 12kg of flame retardant (brominated polystyrene), 4kg of antimony trioxide, 0.5kg of polyvinylpyrrolidone and 0.5kg of ethylene acrylic acid copolymer, and then uniformly mixing the components except the glass fiber to obtain a premix; and then putting the obtained premix into a double-screw extruder, adding glass fiber by adopting a side feeding process, melting and mixing, extruding and granulating to obtain the flame-retardant reinforced high-temperature-resistant nylon composite material, wherein the process parameters of the double-screw extruder are as follows: the temperature of the feeding section is 300 ℃, the temperature of the melting and plasticizing section is 310 ℃, the temperature of the mixing and homogenizing section is 255 ℃, the temperature of the melt conveying section is 270 ℃, the temperature of the machine head is 300 ℃, and the rotating speed of a main machine of the double-screw extruder is 300 rpm.
Comparative example 2
Comparative example 2 is identical to example 2 except that no polyvinylpyrrolidone was added, as compared to example 2.
Example 3
Weighing the components according to the weight ratio of 45kg of nylon 6T/6I, 55kg of short glass fiber (the monofilament diameter is 13 mu m, the length is 5mm), 20kg of flame retardant (polybrominated styrene), 6kg of anhydrous zinc borate, 1kg of polyvinylpyrrolidone and 0.5kg of ethylene acrylic acid copolymer, and then uniformly mixing the components except the glass fiber to obtain a premix; and then putting the obtained premix into a double-screw extruder, adding glass fiber by adopting a side feeding process, melting and mixing, extruding and granulating to obtain the flame-retardant reinforced high-temperature-resistant nylon composite material, wherein the process parameters of the double-screw extruder are as follows: the temperature of the feeding section is 320 ℃, the temperature of the melting and plasticizing section is 330 ℃, the temperature of the mixing and homogenizing section is 260 ℃, the temperature of the melt conveying section is 290 ℃, the temperature of the machine head is 330 ℃, and the rotating speed of a main machine of the double-screw extruder is 350 rpm.
Comparative example 3
Comparative example 3 is identical to example 3 except that no polyvinylpyrrolidone is added, as compared to example 3.
Example 4
Weighing 42kg of nylon 9T, 30kg of short glass fiber (the monofilament diameter is 10 mu m, the length is 4mm), 5kg of talcum powder, 15kg of flame retardant (poly brominated styrene), 4kg of antimony trioxide, 0.5kg of polyvinylpyrrolidone and 0.5kg of ethylene acrylic acid copolymer in parts by weight, and then uniformly mixing the other components except the glass fiber to obtain a premix; and then putting the obtained premix into a double-screw extruder, adding glass fiber by adopting a side feeding process, melting and mixing, extruding and granulating to obtain the flame-retardant reinforced high-temperature-resistant nylon composite material, wherein the process parameters of the double-screw extruder are as follows: the temperature of the feeding section is 315 ℃, the temperature of the melting and plasticizing section is 300 ℃, the temperature of the mixing and homogenizing section is 250 ℃, the temperature of the melt conveying section is 270 ℃, the temperature of the machine head is 310 ℃, and the rotating speed of a main machine of the double-screw extruder is 310 rpm.
Comparative example 4
Comparative example 4 is identical to example 4 except that no polyvinylpyrrolidone is added, as compared to example 4.
Drying the flame-retardant reinforced high-temperature-resistant nylon composite material prepared in each embodiment and each proportion in a blast drying oven at 120 ℃ for 6 hours, then proofing and molding the dried flame-retardant reinforced high-temperature-resistant nylon composite material on an MA600/150 injection molding machine, controlling the processing temperature at 280-350 ℃ and the mold temperature at 90-150 ℃, and respectively carrying out the following performance tests on the prepared parts.
(1) Tensile strength: 150X 10X 4mm bars were produced by injection moulding and tested according to International Standard ISO 527-2 at a tensile speed of 5 mm/min.
(2) Bending strength: 80X 10X 4mm specimens were produced by injection moulding and tested according to International Standard ISO 178 at a bending speed of 2mm/min and a span of 64 mm.
(3) Vertical combustion: the test was carried out in accordance with UL-94 standard, and the test specimen was 125 mm. times.13 mm. times.0.4 mm.
(4) Heat distortion temperature: the test was carried out according to the national standard GB/T1634.1, applying a force of 1.80MPa and the test specimens were 80 mm. times.10 mm. times.4 mm.
(5) Whiteness L value: the test specimen was 70 mm. times.45 mm. times.3 mm as measured by a spectrophotometer (model: Datacolor 110).
(6) Fiber floating condition of the product: the large square piece with the size of 150mm multiplied by 1mm is manufactured by injection molding, and the observation of the floating fiber on the surface is carried out by adopting a visual method, and the large square piece can be divided into four grades of no floating fiber, no obvious floating fiber, obvious floating fiber and serious floating fiber.
The test results are shown in table 1.
TABLE 1 results of performance tests of articles made from the flame retardant reinforced high temperature resistant nylon composites of the examples and comparative examples
As can be seen from table 1, the whiteness L value of the parts made of the flame-retardant reinforced high-temperature-resistant nylon composite materials in examples 1, 2, 3 and 4 is significantly improved compared with the whiteness L value of the parts made of the flame-retardant reinforced high-temperature-resistant nylon composite materials in comparative examples 1, 2, 3 and 4, and the L values are all above 80, and the fiber floating condition of the parts made of the flame-retardant reinforced high-temperature-resistant nylon composite materials in examples 1, 2, 3 and 4 is also significantly better than that of the parts made of the flame-retardant reinforced high-temperature-resistant nylon composite materials in comparative examples 1, 2, 3 and 4. Therefore, the method can be used for obviously improving the initial whiteness of the composite material and effectively solving the problem of fiber floating on the surface of a product by introducing a small amount of polyvinylpyrrolidone into the formula system of the flame-retardant reinforced high-temperature-resistant nylon composite material.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way, and other variations and modifications may be made without departing from the spirit of the invention as set forth in the claims.
Claims (10)
1. The flame-retardant reinforced high-temperature-resistant nylon composite material is characterized by comprising the following raw materials in parts by weight: 30-45 parts of high-temperature nylon resin, 30-55 parts of glass fiber, 10-20 parts of a flame retardant and 0.1-2.0 parts of polyvinylpyrrolidone.
2. The flame-retardant reinforced high-temperature-resistant nylon composite material as claimed in claim 1, wherein the high-temperature nylon resin is nylon 46 or semi-aromatic nylon with a melting point of 280-330 ℃.
3. The flame-retardant reinforced high-temperature-resistant nylon composite material as claimed in claim 2, wherein the semi-aromatic nylon is nylon 6T/66, nylon 6T/6I, nylon 6T/6, nylon 6T/1010, nylon 6T/1212, nylon 6T/612, nylon 6T/610, nylon 6I/66, nylon 6I/6, nylon 6I/1010, nylon 6I/1212, nylon 6I/612 or nylon 9T.
4. The flame-retardant reinforced high-temperature-resistant nylon composite material as claimed in claim 1, wherein the flame retardant is a brominated flame retardant.
5. The flame-retardant reinforced high-temperature-resistant nylon composite material as claimed in claim 4, wherein the brominated flame retardant is brominated polystyrene or polybrominated styrene.
6. The flame-retardant reinforced high-temperature-resistant nylon composite material as claimed in claim 1, wherein the raw materials of the flame-retardant reinforced high-temperature-resistant nylon composite material further comprise 3-6 parts by weight of a flame-retardant synergist.
7. The flame-retardant reinforced high-temperature-resistant nylon composite material as claimed in claim 6, wherein the flame-retardant synergist is selected from antimony trioxide or anhydrous zinc borate.
8. The flame-retardant reinforced high-temperature-resistant nylon composite material as claimed in claim 1, wherein the glass fiber is a short glass fiber with a monofilament diameter of 6-13 μm and a length of 3-5 mm.
9. The flame-retardant reinforced high-temperature-resistant nylon composite material as claimed in claim 1, which is prepared by the following method: weighing the components according to the weight part ratio, and uniformly mixing the components except the glass fiber to obtain a premix; and then putting the obtained premix into a double-screw extruder, melting and mixing the glass fibers by adopting a side feeding process, and extruding and granulating to obtain the flame-retardant reinforced high-temperature-resistant nylon composite material.
10. A molded article made of the flame-retardant reinforced high-temperature-resistant nylon composite material according to any one of claims 1 to 9.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112322033A (en) * | 2020-10-13 | 2021-02-05 | 天津金发新材料有限公司 | Low-crystallization-temperature high-performance polyamide composite material |
| CN112552674A (en) * | 2020-12-11 | 2021-03-26 | 天津金发新材料有限公司 | Polyamide composite material with low floating fiber and high impact strength |
| CN114292517A (en) * | 2021-12-27 | 2022-04-08 | 金发科技股份有限公司 | Flame-retardant polyamide composite material and preparation method and application thereof |
| CN115449157A (en) * | 2022-09-30 | 2022-12-09 | 江苏金发科技新材料有限公司 | Long glass fiber reinforced polypropylene material and preparation method and application thereof |
| CN115960457A (en) * | 2022-12-16 | 2023-04-14 | 江苏金发科技新材料有限公司 | Flame-retardant semi-aromatic polyamide composite material and preparation method and application thereof |
| CN116178942A (en) * | 2022-12-16 | 2023-05-30 | 江苏金发科技新材料有限公司 | Semi-aromatic polyamide composite material and preparation method and application thereof |
| CN116253994A (en) * | 2023-02-24 | 2023-06-13 | 上海金发科技发展有限公司 | Polyamide composite material with good appearance and high performance and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112322033A (en) * | 2020-10-13 | 2021-02-05 | 天津金发新材料有限公司 | Low-crystallization-temperature high-performance polyamide composite material |
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| CN112552674A (en) * | 2020-12-11 | 2021-03-26 | 天津金发新材料有限公司 | Polyamide composite material with low floating fiber and high impact strength |
| CN112552674B (en) * | 2020-12-11 | 2022-06-07 | 天津金发新材料有限公司 | Polyamide composite material with low floating fiber and high impact strength |
| CN114292517A (en) * | 2021-12-27 | 2022-04-08 | 金发科技股份有限公司 | Flame-retardant polyamide composite material and preparation method and application thereof |
| CN115449157A (en) * | 2022-09-30 | 2022-12-09 | 江苏金发科技新材料有限公司 | Long glass fiber reinforced polypropylene material and preparation method and application thereof |
| CN115449157B (en) * | 2022-09-30 | 2023-12-19 | 江苏金发科技新材料有限公司 | Long glass fiber reinforced polypropylene material and preparation method and application thereof |
| CN115960457A (en) * | 2022-12-16 | 2023-04-14 | 江苏金发科技新材料有限公司 | Flame-retardant semi-aromatic polyamide composite material and preparation method and application thereof |
| CN116178942A (en) * | 2022-12-16 | 2023-05-30 | 江苏金发科技新材料有限公司 | Semi-aromatic polyamide composite material and preparation method and application thereof |
| CN116253994A (en) * | 2023-02-24 | 2023-06-13 | 上海金发科技发展有限公司 | Polyamide composite material with good appearance and high performance and preparation method thereof |
| CN116253994B (en) * | 2023-02-24 | 2024-04-16 | 上海金发科技发展有限公司 | Polyamide composite material with good appearance and high performance and preparation method thereof |
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Application publication date: 20200410 |