CN114292517A - Flame-retardant polyamide composite material and preparation method and application thereof - Google Patents
Flame-retardant polyamide composite material and preparation method and application thereof Download PDFInfo
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- CN114292517A CN114292517A CN202111611123.5A CN202111611123A CN114292517A CN 114292517 A CN114292517 A CN 114292517A CN 202111611123 A CN202111611123 A CN 202111611123A CN 114292517 A CN114292517 A CN 114292517A
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Abstract
The invention discloses a flame-retardant polyamide composite material which comprises the following components in parts by weight: polyamide resin, polyvinylpyrrolidone, hypophosphite flame retardant, melamine polyphosphate, borate flame retardant synergist and glass fiber. According to the invention, by adding a certain amount of polyvinylpyrrolidone, the flame retardance (the content of the flame retardant, particularly melamine polyphosphate, is reduced) can be improved, the precipitation of the flame retardant can be inhibited, and the crystallization speed of the flame-retardant polyamide composite material is reduced, so that the appearance of a product is improved.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a flame-retardant polyamide composite material and a preparation method and application thereof.
Background
The halogen-free flame-retardant polyamide has excellent flame retardant property, mechanical property, electrical property, low smoke, low toxicity and environmental protection, and is widely applied to the fields of low-voltage electric appliances, new energy, automobiles and the like. However, compared with other flame-retardant polyamides, the halogen-free flame-retardant polyamides have the problems of poor appearance, precipitation after long-term storage and the like, and the wide application of the halogen-free flame-retardant polyamides is severely limited.
In order to solve the appearance problem of the organic phosphine flame-retardant polyamide, the conventional method is to improve the flowability of the material, although the flowability is improved to a certain extent, the effect is limited, and flash is easily formed in the injection molding process. Researches find that the problem of surface precipitation of the halogen-free flame-retardant polyamide is mainly caused by melamine polyphosphate. At present, the most common method is to reduce the content of melamine polyphosphate, even the melamine polyphosphate is not used, but the melamine polyphosphate is an important component of the halogen-free flame retardant, and the content of the melamine polyphosphate has a crucial influence on the flame retardant property of the halogen-free flame retardant polyamide. The Chinese patent CN 108976471A introduces an organic silicon synergist to improve the flame retardant property of the halogen-free flame retardant polyamide compound and reduce the content of melamine polyphosphate, thereby improving the precipitation property of the material. However, surface precipitates, which are generally improved, remain and deteriorate the impact properties of the material. In addition, the scheme is not suitable for industries with tighter silicon control, such as household appliances. In the field of engineering application, a novel organic phosphine flame retardant named OP 1400 is developed by Craine to replace an OP 1230/MPP scheme to prepare the low-precipitation halogen-free flame-retardant polyamide composite material, but the OP 1400 has low flame-retardant efficiency and large addition amount, and can reduce the flow property of the material, thereby deteriorating the appearance of the halogen-free flame-retardant polyamide composite material.
When the glass fiber is reinforced, the defect of fiber floating is easy to occur, and particularly when the resin crystallization speed is too high, the defect is aggravated.
Therefore, the development of the halogen-free flame-retardant polyamide compound with good appearance and low precipitation rate has very important significance for widening the application of the halogen-free flame-retardant polyamide.
Disclosure of Invention
The invention aims to provide a flame-retardant polyamide composite material which has the advantages of good flame-retardant property and good appearance.
Another object of the present invention is to provide a method for preparing the flame retardant polyamide composite material and its use.
The invention is realized by the following technical scheme:
the flame-retardant polyamide composite material comprises the following components in parts by weight:
60 parts of polyamide resin;
1-6 parts of polyvinylpyrrolidone;
8-30 parts of a hypophosphite flame retardant;
0.5-2 parts of melamine polyphosphate;
1-5 parts of borate flame-retardant synergist;
10-40 parts of glass fiber.
Preferably, the composition comprises the following components in parts by weight:
60 parts of polyamide resin;
2-4 parts of polyvinylpyrrolidone;
12-20 parts of a hypophosphite flame retardant;
0.8-1.5 parts of melamine polyphosphate;
1.5-3 parts of borate flame-retardant synergist;
10-40 parts of glass fiber.
The polyamide resin is selected from at least one of PA6, PA56, PA66, PA6/66, PA66/6, PA66/6T, PA6T/66 and MXD 6.
The number average molecular weight of the polyvinylpyrrolidone is 8000-; the number average molecular weight is preferably 12000-220000 g/mol.
The hypophosphite flame retardant is selected from at least one of aluminum hypophosphite and diethyl aluminum hypophosphite.
Preferably, the melamine polyphosphate has an average degree of polymerization of 100-300.
The borate flame-retardant synergist is at least one of zinc borate, magnesium borate and aluminum borate.
Whether 0-1 part of antioxidant is added can be determined according to actual requirements. May be a hindered phenol type antioxidant.
The preparation method of the flame-retardant polyamide composite material comprises the following steps: according to the proportion, the components are uniformly mixed and then extruded and granulated by a double-screw extruder, the temperature range of the screw is 200-280 ℃, and the rotating speed range is 250-350rpm, so as to obtain the flame-retardant polyamide composite material.
The flame-retardant polyamide composite material is applied to preparing shells of electronic and electric appliances.
The invention has the following beneficial effects:
first, polyvinylpyrrolidone can promote carbon formation and improve the quality of the carbon layer. Therefore, when the content of the melamine polyphosphate is low, a proper amount of polyvinylpyrrolidone is introduced, and the vertical combustion performance of the halogen-free flame-retardant polyamide can still reach 0.8 mmV-0.
Secondly, on the one hand, the existence of the polyvinylpyrrolidone can reduce the using amount of the melamine derivative, thereby reducing the precipitation amount of the flame retardant; on the other hand, polyvinylpyrrolidone in a certain molecular weight range can reduce the precipitation of melamine derivatives.
Thirdly, the carbonyl group of the polyvinylpyrrolidone reduces the crystallization speed of the polyamide by forming a hydrogen bond with the polyamide molecule, thereby further improving the appearance of the product.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The raw material sources used in the examples and comparative examples are as follows:
PA66, designation PA66 EP-158, Huafeng group;
PA6, trademark PA6 HY-2800, Sun chemical fibers Inc.;
PA56, designation 1270W, Kaiser Co., Ltd;
PA66/6T, designation C1504T, Franks boundless company;
glass fiber, mark ECS10-3.0-568H, china boulder gmbh;
diethyl aluminum hypophosphite, designation OP 1230, clariant corporation;
aluminum hypophosphite: M-116S, Shanghai dynasty, New materials science and technology, Inc.
Melamine polyphosphate-1, designation MPP-1, degree of polymerization 50, Budenheim Iberica, Germany;
melamine polyphosphate-2, designation MPP-2, Polymer 100, Budenheim Iberica, Germany;
melamine polyphosphate-3, trade designation MPP-3, degree of polymerization 300, Budenheim Iberica, Germany;
melamine polyphosphate-4, designation MPP-4, degree of polymerization 400, Budenheim Iberica, Germany;
zinc borate, brand No. ZB-503, anshui yishitong ltd;
polyvinylpyrrolidone A, number average molecular weight 12000g/mol, Shanghai Korea;
polyvinylpyrrolidone B, number average molecular weight 40000g/mol, Shanghai Korea;
polyvinylpyrrolidone C: number average molecular weight 220000g/mol, Shanghai Korea company;
polyvinylpyrrolidone D: number average molecular weight 600000g/mol, Shanghai Korea;
antioxidant: antioxidant 1010, commercially available.
The performance test method comprises the following steps:
(1) flame retardant property: carrying out flame retardant property test on the sample strip according to the relevant standard of UL 94-2013, wherein the thickness of the sample is 0.8 mm; the flame retardant property has great significance for electrical safety, and the UL94 flame retardant grade can meet the application requirement only when reaching V-0.
(2) Appearance: and (3) injection molding a color plate (84 × 54 × 2.0 mm), observing floating fibers on the surface of the color plate, and evaluating according to the condition of the floating fibers on the surface of the color plate, wherein the color plate is divided into 4 grades, namely no floating fibers, no obvious floating fibers (the number of the fiber-shaped protrusions is less than 5, the protrusions are shallow, the appearance of the surface of the color plate is not influenced), obvious floating fibers (the number of the fiber-shaped protrusions is about 5-10, the protrusions are high, only good appearance can be kept), and more floating fibers (the number of the protrusions on the surface of the color plate is more than 10, and the appearance of the surface of the color plate is already obviously influenced).
(3) Precipitation performance: and (3) injection molding of the color plate, treating the color plate in a double 85-wet heat aging box for 168 hours, observing whether white precipitates exist on the surface of the color plate, and according to precipitation conditions, respectively carrying out 4 grades of no precipitation, no obvious precipitation (less than 4 pale white spots exist on the color plate), obvious precipitation (the pale white spots on the color plate are large, and partial spots are connected with each other), and more precipitation (white precipitates on the color plate are flaky).
Table 1: EXAMPLES 1-6 flame-retardant Polyamide composite Material content (parts by weight) and test results
Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | |
PA66 | 60 | 60 | 60 | |||
PA6 | 60 | |||||
PA56 | 60 | |||||
PA66/6T | 60 | |||||
Glass fiber | 30 | 30 | 30 | 30 | 10 | 40 |
Diethyl aluminium hypophosphite | 15 | 15 | 15 | 15 | 30 | 8 |
Melamine polyphosphate-2 | 1 | 1 | 1 | 1 | 0.5 | 2 |
Zinc borate | 2 | 2 | 2 | 2 | 1.5 | 3 |
Polyvinylpyrrolidone B | 3 | 3 | 3 | 3 | 6 | 1 |
Vertical combustion performance | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 |
Appearance of the product | Without floating fiber | Without floating fiber | Without floating fiber | Without floating fiber | Without floating fiber | The floating fiber is not obvious |
Precipitation out of | Without precipitation | Without precipitation | Without precipitation | Without precipitation | Without precipitation | Without precipitation |
From example 5, it is understood that when the amount of diethyl aluminum hypophosphite added is 30 parts, precipitation thereof can be suppressed.
From example 6, it can be seen that, even in the formulation of the present invention, the amount of glass fiber added is 40 parts, and the floating of the fiber can be controlled in a very small range.
Table 2: examples 7-13 flame retardant polyamide composite materials content by weight of each component and test results
Example 7 | Example 8 | Example 9 | Example 10 | Example 11 | Example 12 | Example 13 | |
PA66 | 60 | 60 | 60 | 60 | 60 | 60 | 60 |
Glass fiber | 30 | 30 | 30 | 30 | 30 | 30 | 30 |
Diethyl aluminium hypophosphite | 12 | 20 | 8 | 30 | 15 | 15 | 15 |
Melamine polyphosphate-2 | 1.5 | 0.8 | 2 | 0.5 | |||
Melamine polyphosphate-1 | 1 | ||||||
Melamine polyphosphate-3 | 1 | ||||||
Melamine polyphosphate-4 | 1 | ||||||
Zinc borate | 3 | 1.5 | 5 | 1 | 2 | 2 | 2 |
Polyvinylpyrrolidone B | 4 | 2 | 1 | 6 | 3 | 3 | 3 |
Vertical combustion performance | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 | V-0 |
Appearance of the product | Without floating fiber | Without floating fiber | Without floating fiber | The floating fiber is not obvious | Without floating fiber | Without floating fiber | The floating fiber is not obvious |
Precipitation out of | Without precipitation | Without precipitation | No obvious precipitation | Without precipitation | No obvious precipitation | Without precipitation | Without precipitation |
From examples 1/7 to 10, it is clear that the preferable range of the compounding ratio is more excellent in appearance.
From examples 1/11-13, it is preferable that the melamine polyphosphate has an average degree of polymerization of 100-300.
Table 3: EXAMPLES 14-16 flame-retardant Polyamide composite Material content by weight and test results
Example 14 | Example 15 | Example 16 | Example 17 | Example 18 | |
PA66 | 60 | 60 | 60 | 60 | 60 |
Glass fiber | 30 | 30 | 30 | 30 | 30 |
Diethyl aluminium hypophosphite | 15 | 15 | 15 | 15 | |
Aluminum hypophosphite | 15 | ||||
Melamine polyphosphate-2 | 1 | 1 | 1 | 1 | 1 |
Zinc borate | 2 | 2 | 2 | 2 | 2 |
Polyvinylpyrrolidone A | 3 | 3 | 3 | ||
Polyvinylpyrrolidone C | 3 | ||||
Polyvinylpyrrolidone D | 3 | ||||
Flame retardant | |||||
Vertical combustion performance | V-0 | V-0 | V-0 | V-0 | V-0 |
Appearance of the product | Without floating fiber | Without floating fiber | The floating fiber is not obvious | Without floating fiber | Without floating fiber |
Precipitation out of | Without precipitation | Without precipitation | Without precipitation | Without precipitation | Without precipitation |
From examples 1/14-16, the number average molecular weight is preferably 12000-220000 g/mol.
Table 4: comparative example flame-retardant polyamide composite Material content (parts by weight) of Each component and test results
Comparative example 1 | Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | Comparative example 6 | |
PA66 | 60 | 60 | 60 | 60 | 60 | 60 |
Glass fiber | 30 | 30 | 30 | 30 | 30 | 30 |
Diethyl aluminium hypophosphite | 15 | 15 | 15 | 15 | 15 | 15 |
Melamine polyphosphate-2 | 1 | 1 | 0.1 | 2.5 | 1 | 1 |
Zinc borate | 2 | 2 | 2 | 2 | 0.5 | 6 |
Polyvinylpyrrolidone A | 0.5 | 8 | 3 | 3 | 3 | 3 |
Vertical combustion performance | V-1 | V-0 | V-1 | V-0 | V-1 | V-0 |
Appearance of the product | Much floating fiber | Much floating fiber | Without floating fiber | The floating fiber is not obvious | Without floating fiber | Much floating fiber |
Precipitation out of | Without precipitation | Without precipitation | Without precipitation | Obvious precipitation | Without precipitation | Without precipitation |
As shown in the comparative example 1/2, when the amount of polyvinylpyrrolidone added was too low, the flame retardant property of the halogen-free flame retardant polyamide composite could not reach V-0 and the surface fiber floating was large; when the amount of the polyvinylpyrrolidone is large, the flame retardant property of the halogen-free flame retardant polyamide compound can reach V-0, but the surface of the compound has a large amount of floating fibers, probably because the thermal stability is poor, so that the material has a large amount of gas in the injection molding process, and a melt cannot be well copied into a mold.
As shown in the comparative example 3/4, the addition amount of melamine polyphosphate is too low, and the flame retardant property of the halogen-free flame retardant polyamide composite can not reach V-0; the addition amount of the melamine polyphosphate is too high, and the surface of the halogen-free flame-retardant polyamide compound has obvious precipitation, because the melamine polyphosphate has poor compatibility with polyamide and is easy to migrate outwards when the content exceeds a certain amount.
As shown in the comparative example 5/6, the addition amount of the borate flame-retardant synergist is too low, and the flame-retardant performance of the halogen-free flame-retardant polyamide composite can not reach V-0; the addition amount of the borate flame-retardant synergist is too high, and the surface of the halogen-free flame-retardant polyamide composite has more floating fibers, because the viscosity of the melt is reduced due to the too high addition amount of the borate flame-retardant synergist, the melt cannot be well copied into a mold and coated with surface glass fibers.
Claims (10)
1. The flame-retardant polyamide composite material is characterized by comprising the following components in parts by weight:
60 parts of polyamide resin;
1-6 parts of polyvinylpyrrolidone;
8-30 parts of a hypophosphite flame retardant;
0.5-2 parts of melamine polyphosphate;
1-5 parts of borate flame-retardant synergist;
10-40 parts of glass fiber.
2. The flame-retardant polyamide composite material as claimed in claim 1, which comprises the following components in parts by weight:
60 parts of polyamide resin;
2-4 parts of polyvinylpyrrolidone;
12-20 parts of a hypophosphite flame retardant;
0.8-1.5 parts of melamine polyphosphate;
1.5-3 parts of borate flame-retardant synergist;
10-40 parts of glass fiber.
3. The flame retardant polyamide composite material according to claim 1, wherein the polyamide resin is at least one selected from the group consisting of PA6, PA56, PA66, PA6/66, PA66/6, PA66/6T, PA6T/66, MXD 6.
4. The flame retardant polyamide composite material as claimed in claim 1, wherein the polyvinylpyrrolidone has a number average molecular weight of 8000-; the number average molecular weight is preferably 12000-220000 g/mol.
5. The flame retardant polyamide composite material of claim 1, wherein the hypophosphite flame retardant is selected from at least one of aluminum hypophosphite and diethyl aluminum hypophosphite.
6. The flame retardant polyamide composite material as claimed in claim 1, wherein the melamine polyphosphate has an average degree of polymerization of 100-300.
7. The flame retardant polyamide composite material of claim 1, wherein the borate flame retardant synergist is at least one selected from the group consisting of zinc borate, magnesium borate, and aluminum borate.
8. The flame retardant polyamide composite material according to claim 1, further comprising 0 to 1 part by weight of an antioxidant.
9. A process for the preparation of a flame retardant polyamide composite material according to any of claims 1 to 8, characterized in that it comprises the following steps: according to the proportion, the components are uniformly mixed and then extruded and granulated by a double-screw extruder, the temperature range of the screw is 200-280 ℃, and the rotating speed range is 250-350rpm, so as to obtain the flame-retardant polyamide composite material.
10. Use of the flame retardant polyamide composite material according to any one of claims 1 to 8 for the manufacture of housings for electronic and electrical appliances.
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CN115058116A (en) * | 2022-04-14 | 2022-09-16 | 万华化学(宁波)有限公司 | Halogen-free flame-retardant corrugated pipe material and preparation method thereof |
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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 |
CN116731421A (en) * | 2023-07-03 | 2023-09-12 | 郑州峰泰纳米材料有限公司 | Noise-reduction composite cotton material for aircraft passenger cabin and preparation method and application thereof |
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CN116731421A (en) * | 2023-07-03 | 2023-09-12 | 郑州峰泰纳米材料有限公司 | Noise-reduction composite cotton material for aircraft passenger cabin and preparation method and application thereof |
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