CN113372715A - Red phosphorus flame-retardant reinforced nylon composite material and application thereof - Google Patents
Red phosphorus flame-retardant reinforced nylon composite material and application thereof Download PDFInfo
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- CN113372715A CN113372715A CN202110699465.0A CN202110699465A CN113372715A CN 113372715 A CN113372715 A CN 113372715A CN 202110699465 A CN202110699465 A CN 202110699465A CN 113372715 A CN113372715 A CN 113372715A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
- C08L77/06—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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K2003/026—Phosphorus
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The invention discloses a red phosphorus flame-retardant reinforced nylon composite material and application thereof, wherein the red phosphorus flame-retardant reinforced nylon composite material comprises the following components in parts by weight: 35-55 parts of nylon resin, 3-20 parts of thermoplastic polyester, 5-20 parts of red phosphorus flame retardant and 10-45 parts of reinforcing filler, wherein the thermoplastic polyester is selected from one or a compound of polyethylene terephthalate (PET) and polybutylene terephthalate (PBT). According to the invention, a certain amount of thermoplastic polyester is added into a red phosphorus flame-retardant reinforced nylon composite material system, so that the thermal forming processing process of the composite material can be effectively reduced, and particularly the PH value under the condition of higher thermal forming processing temperature3The gas release amount reduces the harm to the health of people, improves the use safety of materials, and is suitable for the fields of connectors, socket connectors, circuit breakers, low-voltage switches and the like in electronic appliances.
Description
Technical Field
The invention relates to the technical field of engineering plastic modification, and in particular relates to a red phosphorus flame-retardant reinforced nylon composite material.
Background
The red phosphorus flame retardant is a universal halogen-free flame retardant, has high flame retardant efficiency, small addition amount, low price and small influence on the physical property and the electrical property of a resin matrix, has less smoke generation amount in combustion than a halogen flame retardant, does not migrate to the surface, is greatly used for compounding with nylon resin, and the prepared flame-retardant reinforced nylon material has good flame retardant property and excellent mechanical property and electrical property, and is widely applied to the field of electronic and electrical appliances.
However, the defect in the art is that the red phosphorus flame-retardant reinforced nylon material is easy to release pH with pungent smell during melt extrusion production and high-temperature thermoforming processing3Gas, and PH3The gas release amount is increased along with the increase of the content of the red phosphorus flame retardant in the nylon material. In addition, with the complicated and thin wall structure of the molded product, the thermoforming processing temperature of the red phosphorus flame-retardant reinforced nylon composite material is higher and higher (above 280 ℃ and even 300 ℃) in the application process, and the severe high-temperature thermoforming processing condition can further cause the PH value of the red phosphorus flame-retardant reinforced nylon material during the molding of the molded product by the molded product3The amount of gas released is greatly increased, thereby causing air quality in a limited space to be deteriorated. PH value3The gas is a highly toxic gas, and the inhaled gas can affect the heart, respiratory system, kidney, intestines and stomach, nervous system and liver of a human body and cause great harm to the life health of a material forming person.
For reducing PH in red phosphorus flame-retardant reinforced nylon material3Release amount, US6645625 discloses a method for improving red phosphorus precipitation by using silver and tin oxide to substantially lower the pH3The release amount is increased, but the use of metal and metal oxide can greatly reduce the electrical property of the nylon material, especially the electrical property under a humid environment. Chinese patent CN104059358A discloses a flame retardant thermoplastic polyamide composition using nigrosine as an adsorbent to reduce the pH during injection molding3Gas release, but this physical adsorption is not permanent; in addition, nigrosine is a black organic dye, can only be used for preparing black materials, and greatly limits the application of red phosphorus flame-retardant materials in terms of color. Special for ChinaLi CN112608595A discloses a red phosphorus flame-retardant polyamide composition, which adopts polyamide 66 to be compounded with long carbon chain polyamide, and simultaneously adds hyperbranched resin and solvent black chromium complex to reduce PH3The release amount is reduced, but the flame retardant performance of the red phosphorus flame retardant PA66 is reduced due to the addition of the long carbon chain polyamide, and the solvent black chromium complex can only be used for preparing black materials, and the overall cost is relatively high.
According to the invention, through the research and the unexpected discovery, a certain amount of thermoplastic polyester is added into a red phosphorus flame-retardant reinforced nylon composite material system, so that the PH value of the composite material in the thermoforming processing process can be effectively reduced3The release amount of gas can improve the electrical insulation of the molded product in a humid environment.
Disclosure of Invention
The invention aims to overcome the defects of the existing red phosphorus flame-retardant reinforced nylon material and reduce the PH value of the material in the thermal forming processing process3The release amount of the gas reduces the harm to the health of the molding personnel of the material, simultaneously improves the use safety of the material in a humid environment and provides a low pH3The red phosphorus flame-retardant reinforced nylon composite material is released and has good electrical insulation property in a humid environment.
The above purpose of the invention is realized by the following technical scheme:
the red phosphorus flame-retardant reinforced nylon composite material comprises the following components in parts by weight:
35-55 parts of nylon resin;
3-20 parts of thermoplastic polyester;
5-20 parts of a red phosphorus flame retardant;
10-45 parts of a reinforcing filler;
wherein the thermoplastic polyester is selected from polyethylene terephthalate (PET) and polybutylene terephthalate
(PBT) or a compound of the two.
The invention can effectively reduce the PH of the composite material in the thermoforming processing process by introducing a certain amount of specific thermoplastic polyester into a nylon composite material system3The release amount of gas can be kept goodThe electrical property of the composite material, especially the electrical insulation property in a humid environment, improves the use safety of the composite material in the humid environment.
Preferably, the nylon resin is selected from one or more of aliphatic nylon, semi-aromatic nylon and copolymerized nylon; the aliphatic nylon is selected from at least one of PA6, PA66, PA46, PA56, PA12, PA1010, PA1012 and PA1212, the semi-aromatic nylon is selected from at least one of PA4T, PA6T, PA9T and PA10T, and the copolymerized nylon is selected from at least one of PA10T/PA1010, PA6T/PA610 and PA10T/PA 1012.
The red phosphorus flame retardant is red phosphorus powder or red phosphorus master batch, and the weight ratio of the red phosphorus component in the red phosphorus master batch is 40-85%.
The reinforcing filler is a fibrous filler or a compound of the fibrous filler and inorganic mineral powder; the fiber filler is selected from at least one of glass fiber, carbon fiber, quartz fiber, potassium titanate fiber, basalt fiber and aramid fiber; the inorganic mineral powder is selected from at least one of wollastonite, calcium carbonate, mica, talcum powder, quartz, feldspar, kaolin, calcium silicate and barium sulfate.
Preferably, the red phosphorus flame-retardant reinforced nylon composite material comprises the following components in parts by weight:
35-55 parts of nylon resin;
5-15 parts of thermoplastic polyester;
10-15 parts of a red phosphorus flame retardant;
25-45 parts of a reinforcing filler;
2-5 parts of a compatilizer;
the red phosphorus flame retardant is red phosphorus master batches with the red phosphorus content of 40-60%, and preferably the red phosphorus master batches with nylon as a carrier.
Preferably, the thermoplastic polyester is PET resin, and the reinforcing filler is glass fiber.
More preferably, the ratio of the nylon resin to the PET resin is 1-5: 1, and the nylon resin is preferably PA6, PA66 or a mixture of the two.
The compatilizer is one or more than two of maleic anhydride grafted polyolefin elastomer, ethylene-ethyl acrylate-maleic anhydride copolymer, acrylate-glycidyl ester-ethylene copolymer, methacrylate-styrene-butadiene rubber-styrene copolymer, ethylene-acrylate copolymer, ethylene-vinyl acetate copolymer, acrylonitrile-butadiene-styrene copolymer, block copolymer containing polyester hard segment and polyether soft segment, or acrylonitrile-ethylene-styrene copolymer.
The composition of the present invention may contain other additional components according to the actual performance requirements, and the additional components may include, but are not limited to, heat stabilizers, processing aids, lubricants, mold release agents, color additives, glass fiber exposure prevention agents, impact modifiers, antioxidants, and the like.
The invention also provides the application of the red phosphorus flame-retardant reinforced nylon composite material in electronic appliances.
The invention also provides the hot forming processing of the thermoplastic polyester in the red phosphorus reduction and flame retardation reinforced nylon composite material
pH in the middle of the process3The application of the gas release amount is characterized in that the thermoplastic polyester is selected from one or a compound of polyethylene terephthalate (PET) and polybutylene terephthalate (PBT), the content of the red phosphorus flame retardant is more than or equal to 5 percent, and the addition amount of the thermoplastic polyester is 3-20 percent based on the total weight of the red phosphorus flame retardant reinforced nylon composite material.
Thermoplastic polyester for reducing PH in thermoforming processing process of red phosphorus flame-retardant reinforced nylon composite material3When the amount of the gas released is too small, the pH is suppressed by adding the thermoplastic polyester in an amount of too small3The effect of gas release amount is not obvious, and if the addition amount is too much, the mechanical property, especially the shock resistance, of the composite material is reduced.
The thermoplastic polyester can reduce the PH value of the red phosphorus flame-retardant reinforced nylon composite material in the thermal forming processing process3In the application of the gas release amount, when the red phosphorus flame retardant is red phosphorus master batch with the red phosphorus content of 40-60%, the content of the red phosphorus flame retardant is more than or equal to 10% and the thermoplastic reinforced nylon composite material is in terms of the total weight of the red phosphorus flame retardant reinforced nylon composite materialThe PET resin is used as the sexual polyester, and the addition amount of the PET resin is 5% -15%.
The thermoplastic polyester can reduce the PH value of the red phosphorus flame-retardant reinforced nylon composite material in the thermal forming processing process3In the application of the gas release amount, the thermoforming processing temperature of the red phosphorus flame-retardant reinforced nylon composite material is 280-300 ℃. In the thermal forming temperature range, the PH value is higher in the process of forming and processing a molded product by adopting the red phosphorus flame-retardant reinforced nylon composite material prepared by the invention3The release amount of the gas can be reduced to be below 30ppm/Kg, and the air quality of the thermoforming processing workshop is greatly improved.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, a certain amount of specific thermoplastic polyester is added into the red phosphorus flame-retardant reinforced nylon composite material, so that the thermal forming processing process of the composite material can be effectively reduced, and particularly the PH value under the condition of higher thermal forming processing temperature3The release amount of gas reduces the harm to the health of people, improves the use safety of the material, and the PH value is higher in the process of molding and processing the molded product at the high temperature of 300 DEG C3The gas release amount can be reduced to below 30 ppm/kg; the molded product formed by the red phosphorus flame-retardant reinforced nylon composite material prepared by the invention is stored for 28 days in the environment with 85% humidity and 85 ℃ and the surface resistivity of the molded product can still be kept at 1010 Omega and above, greatly reduce the risk of electric leakage when the molded product is used as an electronic and electrical element in a humid environment, is very suitable for parts such as a connector, a connector assembly, a circuit breaker, a low-voltage switch and the like in the field of electronic and electrical appliances, and widens the application range of the parts; the raw materials of the red phosphorus flame-retardant reinforced nylon composite material prepared by the method are conventional materials, and compared with the existing red phosphorus flame-retardant reinforced nylon composite material, the PH value is increased in use3The gas release technology has more advantages in material cost.
Detailed Description
The invention will now be described in greater detail, clearly and completely, with reference to specific examples, which are given by way of illustration only and are not intended to limit the scope of the invention.
Materials used in examples and comparative examples:
PA66 resin: model EPR27, available from Hippocampus Hibiscus engineering plastics, Inc.;
PBT resin: brand 1090, available from Nantong star synthetic materials, Inc.;
PET resin: the trade mark PET FG600, purchased from China petrochemical certified chemical fiber GmbH;
red phosphorus flame retardant a: red phosphorus powder, MM-F1, sumamelocene new materials ltd;
red phosphorus flame retardant B: red phosphorus master batch, REDNIC 20450 (red phosphorus content 50%, nylon 6 carrier), south american specialty chemicals ltd;
reinforcing materials: glass fiber, having a designation of ECS10-03-568H, available from Jushi group, Inc.;
a compatilizer: POE-g-MAH, brand WEK-108, available from Wannapu New materials science and technology, Inc., Jiangsu;
other components: antioxidant 1098, available from basf; lubricant: polyethylene wax, designation A-C540A, available from Honeywell corporation.
The performance test method comprises the following steps:
(1) tensile strength: testing according to ISO527-1 standard at a test speed of 2 mm/min;
(2) unnotched impact strength: the test specimens were 55mm by 6mm by 4mm, measured according to ISO179 standard;
(3) flame retardant property: the thickness of the test sample is 1.6mm according to the UL-94 vertical combustion method;
(4) dry surface resistivity: according to the test of GB/T1410 standard, the test sample plate is naturally placed for 12 hours under the conditions of 23 ℃ and 50% humidity and then is tested;
(5) wet insulation resistivity: according to the test of GB/T1410 standard, the test sample plate is placed in a constant temperature and humidity box with the temperature of 85 ℃ and the humidity of 85 percent, after the humidity adjustment treatment is carried out for 28 days, the test sample plate is taken out and naturally placed for 12 hours under the conditions of 23 ℃ and 50 percent of humidity, and then the test is carried out;
（6）PH3the release amount is as follows: injection molding by an injection molding machine to form test sample strips with the dimensions of 120mm multiplied by 3mm (the injection temperature is 290 ℃ C. and 300 ℃ C.), and the mold temperature is 300 ℃ C80 ℃), placing the sample strip which is just injection molded into a drying dish with a phosphine detector, sealing the sample strip immediately, pressing a stopwatch to start timing, recording the reading of the phosphine detector when the stopwatch reads for 5 minutes, and calculating the PH3And (4) releasing the amount. PH value3Release = reading/bar mass (kg) in ppm.
Examples 1 to 9 and comparative examples 1 to 6
In each embodiment and comparative example, the raw material components are weighed according to the weight ratio in the table 1 and the table 2 respectively, the components except the glass fiber are premixed in a high-speed mixer to obtain a premix, then the premix is put into a double-screw extruder from a main feeding port, the glass fiber is put into a side feeding port, and the red phosphorus flame-retardant reinforced nylon composite material is obtained through melt blending, extrusion, cooling, air drying and granulation; the length-diameter ratio of a screw of the double-screw extruder is 36: 1-44: 1, the extrusion processing temperature is 200-250 ℃, and the screw rotating speed is 250-450 rpm.
The composite materials prepared in the above embodiments and comparative examples are respectively placed in an oven, dried at 120 ℃ for 4 hours, and then injection molding is adopted to prepare a standard sample strip for testing according to the dimension required by each performance testing method, wherein the injection molding temperature is 260 ℃ and the mold temperature is 80 ℃. The results of the performance tests on the samples are shown in tables 1 and 2.
Table 1 examples 1-9 formulation components and their performance test results
TABLE 2 comparative examples 1-6 formulation components and their performance test results
As can be seen from the performance test results in tables 1 and 2, a certain amount of PBT resin or PET resin is introduced into a red phosphorus flame-retardant reinforced nylon composite material system, and the composite material has PH in the high-temperature thermoforming process3The amount of the released gas is such that,far lower than that of red phosphorus flame-retardant reinforced nylon system without introducing thermoplastic polyester, improves the electrical insulation property of the composite material in a humid environment, and can keep the surface resistivity of the molded test sample plate at 10 after being stored for 28 days in an environment with 85% humidity and 85 DEG C10 Omega and above (surface resistivity of solid material is less than 10)10 Omega, the risk of leakage is greater when used as an electronic component).
Claims (15)
1. The red phosphorus flame-retardant reinforced nylon composite material is characterized by comprising the following components in parts by weight:
35-55 parts of nylon resin;
3-20 parts of thermoplastic polyester;
5-20 parts of a red phosphorus flame retardant;
10-45 parts of a reinforcing filler;
wherein the thermoplastic polyester is selected from one or a compound of polyethylene terephthalate (PET) and polybutylene terephthalate (PBT).
2. The red phosphorus flame-retardant reinforced nylon composite material as claimed in claim 1, wherein the nylon resin is selected from one or more of aliphatic nylon, semi-aromatic nylon and copolymerized nylon; the aliphatic nylon is selected from at least one of PA6, PA66, PA46, PA56, PA12, PA1010, PA1012 and PA1212, the semi-aromatic nylon is selected from at least one of PA4T, PA6T, PA9T and PA10T, and the copolymerized nylon is selected from at least one of PA10T/PA1010, PA6T/PA610 and PA10T/PA 1012.
3. The red phosphorus flame retardant reinforced nylon composite material of claim 1, wherein the red phosphorus flame retardant is red phosphorus powder or red phosphorus master batch.
4. The red phosphorus flame-retardant reinforced nylon composite material as claimed in claim 3, wherein the weight ratio of the red phosphorus component in the red phosphorus master batch is 40-85%.
5. The red phosphorus flame-retardant reinforced nylon composite material according to claim 1, wherein the reinforcing filler is a fibrous filler or a compound of the fibrous filler and inorganic mineral powder; the fiber filler is at least one of glass fiber, carbon fiber, quartz fiber, potassium titanate fiber, basalt fiber and aramid fiber; the inorganic mineral powder is at least one of wollastonite, calcium carbonate, mica, talcum powder, quartz, feldspar, kaolin, calcium silicate and barium sulfate.
6. The red phosphorus flame-retardant reinforced nylon composite material as claimed in claim 1, which comprises the following components in parts by weight:
35-55 parts of nylon resin;
5-15 parts of thermoplastic polyester;
10-15 parts of a red phosphorus flame retardant;
25-45 parts of a reinforcing filler;
2-5 parts of a compatilizer;
wherein the red phosphorus flame retardant is red phosphorus master batch with the red phosphorus content of 40-60%.
7. The red phosphorus flame retardant reinforced nylon composite material of claim 6, wherein the thermoplastic polyester is PET resin, and the reinforcing filler is glass fiber.
8. The red phosphorus flame-retardant reinforced nylon composite material as claimed in claim 7, wherein the ratio of the nylon resin to the PET resin is 1-5: 1.
9. The red phosphorus flame retardant reinforced nylon composite material of claim 6, wherein the compatibilizer is one or more of a maleic anhydride grafted polyolefin elastomer, an ethylene-ethyl acrylate-maleic anhydride copolymer, an acrylate-glycidyl ester-ethylene copolymer, a methacrylate-styrene butadiene rubber-styrene copolymer, an ethylene-acrylate copolymer, an ethylene-vinyl acetate copolymer, an acrylonitrile-butadiene-styrene copolymer, a block copolymer containing a polyester hard segment and a polyether soft segment, or an acrylonitrile-ethylene-styrene copolymer.
10. The red phosphorus flame-retardant reinforced nylon composite material according to any one of claims 1 to 9, wherein the polymer material further comprises other components, and the other components are one or more of an antioxidant, a lubricant, a colorant, a mold release agent, a glass fiber exposure inhibitor and a light stabilizer.
11. The use of the red phosphorus flame retardant reinforced nylon composite material according to any one of claims 1 to 10 in electronic and electric appliances.
12. PH of thermoplastic polyester in thermal forming process of red phosphorus-reducing flame-retardant reinforced nylon composite material3The thermoplastic polyester is one or a compound of polyethylene terephthalate (PET) and polybutylene terephthalate (PBT).
13. The use of claim 12, wherein the content of the red phosphorus flame retardant is greater than or equal to 5% and the thermoplastic polyester is added in an amount of 3% to 20% based on the total weight of the red phosphorus flame retardant reinforced nylon composite material.
14. The application of the composite material as claimed in claim 12, wherein the red phosphorus flame retardant is red phosphorus master batch with a red phosphorus content of 40% -60%, the content of the red phosphorus flame retardant is greater than or equal to 10% based on the total weight of the red phosphorus flame retardant reinforced nylon composite material, the thermoplastic polyester is PET resin, and the addition amount of the PET resin is 5% -15%.
15. The use of claim 12, wherein the red phosphorus flame retardant reinforced nylon composite material has a thermoforming processing temperature of 280 ℃ to 300 ℃.
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Cited By (1)
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| CN114921092A (en) * | 2022-03-23 | 2022-08-19 | 金发科技股份有限公司 | Nylon composition and preparation method and application thereof |
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| CN113372715B (en) | 2022-12-16 |
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