CN110724371A - Flame retardant material for electric vehicle electrical contacts - Google Patents
Flame retardant material for electric vehicle electrical contacts Download PDFInfo
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- CN110724371A CN110724371A CN201911104719.9A CN201911104719A CN110724371A CN 110724371 A CN110724371 A CN 110724371A CN 201911104719 A CN201911104719 A CN 201911104719A CN 110724371 A CN110724371 A CN 110724371A
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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
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/02—Polyesters derived from dicarboxylic acids and dihydroxy compounds
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/08—Polymer mixtures characterised by other features containing additives to improve the compatibility between two polymers
Abstract
The invention belongs to the technical field of plastic processing, and relates to a flame-retardant material for an electric contact element of an electric vehicle. The flame-retardant polypropylene composite material comprises a component A and a component B in parts by weight, wherein the component A comprises 65-85 parts of polybutylene terephthalate, 15-35 parts of polypropylene, 7-15 parts of a graft copolymer compatibilizer, 5-12 parts of a flame retardant, 1-3 parts of a lubricant, 1-3 parts of an antioxidant, and the component B: 10-20 parts of a compatibilization flame-retardant synergist, wherein the compatibilization flame-retardant synergist is composed of alkylphenol polyoxybutylene and graphene according to the weight ratio of 6-15: 4-10. The invention greatly improves the compatibility of the polybutylene terephthalate and the polypropylene on the basis of the traditional graft copolymer compatibilizer through the self-made compatibilizer flame-retardant synergist, thereby improving the stability during production.
Description
Technical Field
The invention belongs to the technical field of plastic processing, and relates to a flame-retardant material for an electric contact element of an electric vehicle.
Background
GB17761-2018 "safety technical specification for electric bicycles" has been enforced, which standard places further demands on the flame retardant properties of electric bicycle electrical contacts. Therefore, the flame retardance of the electric contact element of the electric vehicle is the focus of research at present, and the PP/PBT alloy is one of the main raw materials used by the electric contact element of the electric vehicle at present due to the low price of the raw materials, rich raw materials, excellent processing performance, good heat resistance and good chemical corrosion resistance. Due to the difference of molecular polarity and molecular chain structure, the PP/PBT is easy to generate phase separation phenomenon when blended. The prior research mostly focuses on improving the compatibility of PP/PBT by using a compatibilizer, such as graft polymer, and the Chinese invention [ CN201410545559.2] discloses a halogen-free flame-retardant PBT/PP-based wood-plastic composite material which comprises the following raw materials in parts by weight: 20-30 parts of polybutylene terephthalate, 10-20 parts of polypropylene, 28-35 parts of melamine formaldehyde resin modified plant fiber, 18-23 parts of coated ammonium polyphosphate, 1-3 parts of 4A molecular sieve, 4-8 parts of maleic anhydride grafted polyolefin, 2-3 parts of lubricant, 0.2-0.5 part of antioxidant and 0.2-0.5 part of light stabilizer. However, due to the improvement of the performance requirement of the electric contact element of the electric bicycle, the flame retardant modification of the PP/PBT alloy may require the coordination of a plurality of flame retardants, the existing compatibilization method is difficult to ensure the stability of the PP/PBT alloy system, and the development of the flame retardant material for the electric contact element of the electric bicycle is limited.
Disclosure of Invention
The invention aims to solve the problems and provides a flame-retardant material for an electric contact of an electric vehicle.
In order to achieve the purpose, the invention adopts the following technical scheme:
the flame retardant material for the electric contact element of the electric vehicle comprises a component A and a component B, and is characterized by comprising the following components in parts by weight:
and (2) component A:
and (B) component:
10-20 parts of a compatibilization flame-retardant synergist,
the compatibilization flame-retardant synergist consists of alkylphenol polyoxybutylene ester and graphene according to the weight ratio of 6-15: 4-10.
In the flame retardant material for the electric contact of the electric vehicle, the grafted copolymer compatibilizer is one or more of polypropylene copolymer grafted maleic anhydride, ethylene-octene copolymer grafted glycidyl methacrylate, ethylene-vinyl acetate copolymer grafted maleic anhydride and ethylene-methyl acrylate-glycidyl methacrylate.
In the flame retardant material for the electric contact element of the electric vehicle, the grafting rate of the graft copolymer compatibilizer is more than or equal to 4 percent.
In the flame retardant material for the electric contact element of the electric vehicle, the flame retardant is at least one of pentaerythritol diphosphate melamine salt, melamine cyanurate, aluminum hypophosphite and triphenyl phosphate.
In the flame retardant material for the electric contact element of the electric vehicle, the compatibilization flame retardant synergist also comprises red phosphorus, and the compatibilization flame retardant synergist is composed of alkylphenol polyoxybutylene ester, graphene and red phosphorus according to the weight ratio of 6-15:1-3: 3-7.
In the flame retardant material for the electric contact element of the electric vehicle, the red phosphorus is nano red phosphorus, and the graphene and the red phosphorus are subjected to coupling treatment by alkylphenol polyoxybutylene ester.
In the flame retardant material for the electric contact of the electric vehicle, the lubricant is at least one of polysiloxane, dimethyl silicone oil, methyl phenyl silicone oil, polyethylene wax, stearic acid and stearic acid soap.
In the flame retardant material for the electric contact element of the electric vehicle, the antioxidant is one or more of triethylene glycol bis-3- (3-tert-butyl-4-hydroxy-5-toluene phenyl) acrylate, tetra [ methyl-beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] pentaerythritol ester, tert-butyl hydroquinone and tris (2, 4-di-tert-butylphenol) phosphite.
The preparation method of the flame retardant material for the electric contact element of the electric vehicle comprises the following steps:
a) preparing the alkylphenol polyoxybutylene ester,
b) the compatibilization flame-retardant synergist is prepared,
c) preparing the raw materials according to the parts by weight of the raw materials,
d) putting the raw materials into a high-speed mixer for mixing, cooling to room temperature after uniform mixing,
e) and (3) feeding the cooled mixed material into a double-screw extruder for melt extrusion, cooling the extruded strip material by a water tank, and drawing the cooled strip material into a granulator for granulation to obtain the flame retardant material for the electric contact of the electric vehicle.
In the preparation method of the flame retardant material for the electric contact of the electric vehicle, in the step d), only the raw materials of the component A are mixed, and in the step e), the component A is added into a double-screw extruder through a main feeding hopper for melt blending; injecting the component B through a side feeding port, extruding and granulating, and e) obtaining the flame retardant material for the electric contact of the electric vehicle.
Compared with the prior art, the invention has the advantages that:
1. the flame retardant material for the electric contact of the electric vehicle provided by the invention greatly improves the compatibility of polybutylene terephthalate and polypropylene on the basis of the traditional graft copolymer compatibilizer through the self-made compatibilization flame retardant synergist, thereby improving the stability during production. Meanwhile, the heat-conducting component is added on the basis of a single flame retardant, so that the flame retardant property of the material is further improved, and the material is more suitable for being used on an electric contact element of an electric vehicle compared with the existing material.
2. The self-made compatibilization flame-retardant synergist provided by the invention has the advantages of low raw material price, simple preparation method and low reaction cost, and has the possibility of large-scale application.
3. The self-made alkylphenol polyoxybutylene provided by the invention can not only increase the capacity of a mixed system of polybutylene terephthalate and polypropylene, but also carry out coupling treatment on heat-conducting components. And the material does not react with other components, so that the stability of the material is further enhanced, and the product quality is improved.
Additional advantages of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
Examples 1 to 5
Examples 1 to 5 in parts by weight (unit: Kg), the compositions are shown in Table 1
TABLE 1 EXAMPLES 1-5 compositional Table (units Kg)
Wherein the PBT is polybutylene terephthalate, and is selected from Kafen biological technology of Guangzhou; PP, i.e. polypropylene, selected from shanghai spectinographic organisms; the grafted copolymer compatibilizers of examples 1-3 were polypropylene copolymer grafted maleic anhydride (i.e., PP-g-MAH), selected from Shanghai Mitsui laboratories; examples 4-5 wherein the graft copolymer compatibilizer was ethylene-octene copolymer grafted glycidyl acrylate (i.e., POE-g-GMA) selected from Dingxin plastics materials, Inc., of Dongguan; the grafting rate of the graft copolymer compatibilizer is more than or equal to 4 percent; the flame retardant is triphenyl phosphate, and is selected from Zhonghua (Hangzhou) science and technology limited; the lubricant is polyethylene wax selected from Nanjing Bamuda Biotech limited; the antioxidant is tert-butylhydroquinone, and is selected from Zhonghua (Hangzhou) science and technology limited; the graphene is selected from Zhonghua (Hangzhou) science and technology limited.
The alkylphenol polyoxybutylene ester is prepared by self-preparation, and the preparation reaction is as follows:
as shown in the reaction formula, the raw material is 2-methyl butenoic acid methyl ester, and is selected from Zhonghua (Hangzhou) science and technology limited company. Preparation of intermediate 1 by hydrolysis of the starting material: namely, sulfuric acid is added into the raw material, and hydrolysis is carried out under the condition of 60 ℃ to obtain the intermediate 1 aqueous solution. Intermediate 1 intermediate 2 was prepared by an acylchlorination reaction: namely, adjusting the pH value of the aqueous solution of the intermediate 1 to be alkaline, cooling to zero, starting to dropwise add an acyl chlorination reagent, heating to room temperature, and stirring for 1.5-3 hours to obtain an intermediate 2. And (3) carrying out halogenation reaction on the intermediate 2 and alkylphenol to prepare alkylphenol polyoxybutylene ester: namely heating the alkylphenol to 50 ℃, dropwise adding the intermediate 2, recovering acid gas by a tail gas recovery device, and carrying out heat preservation reaction for 2-3h after dropwise adding. And pouring the reactant into a separating funnel, standing for layering, separating out lower-layer liquid, and washing the lower-layer liquid for 2 times by using an extracting agent to obtain the alkylphenol polyoxybutylene ester.
The preparation of examples 1 to 5 was as follows:
a) preparing alkylphenol polyoxybutylene ester according to the method,
b) preparing a compatibilization flame-retardant synergist: fully mixing alkylphenol polyoxyethylene and graphene,
c) preparing the raw materials according to the parts by weight of the raw materials, respectively drying PBT and PP in a vacuum drying oven for 6-10 hours,
d) the raw materials are put into a high-speed mixer for mixing at the rotating speed of 750-1000rpm, are cooled to room temperature after being uniformly mixed,
e) and (3) feeding the cooled mixed material into a double-screw extruder for melt extrusion, wherein the temperature of a material cylinder of the double-screw extruder is 210-240 ℃, the rotating speed of a screw is 180-220 r/min, and the extruded strip material is cooled by a water tank, pulled and fed into a granulator for granulation, so that the flame retardant material for the electric contact element of the electric vehicle is obtained.
Comparative example 1
The composition of the comparative example 1 is different from that of the example 3 in that alkylphenol polyoxybutylene ester in the compatibilization flame-retardant synergist is replaced by PP-g-MAH with equal mass, graphene in the compatibilization flame-retardant synergist is replaced by nano silicon dioxide with equal mass, and the rest is the same as the composition of the example 3.
Comparative example 1 was prepared as in example 3.
Comparative example 2
The composition of comparative example 2 is different from that of example 3 in that alkylphenol polyoxyethylene in the compatibilization flame-retardant synergist is replaced by alkylphenol polyoxyethylene with equal mass, and the rest is the same as the composition of example 3.
Comparative example 2 was prepared in the same manner as in example 3.
Comparative example 3
The composition of comparative example 3 differs from that of example 3 in that PP-g-MAH was replaced with an equal mass of alkylphenol polyoxybutylene ester, and the rest was the same as that of example 3.
Comparative example 3 was prepared in the same manner as in example 3.
Test example 1
Injecting the materials obtained in the examples 1-5 and the comparative examples 1-3 by an injection molding machine to prepare test samples, and carrying out performance test;
melt flow rate: tested according to ISO 1183, the test conditions were 230 ℃, 2.16 kg; flame retardant property: testing according to GB17761-2018, namely GB/T5196.16; shrinkage rate: testing according to ISO 294-4; hardness: testing according to ISO 868; tensile strength: testing according to ISO 527-2; flexural modulus: testing according to ISO 178; the heat distortion temperature was tested according to ISO75A-1, -2 under test conditions of 1.80MPa, unannealed.
The detection results are shown in Table 2
TABLE 2 results of Performance test of examples 1 to 5 and comparative examples 1 to 3
As can be seen from Table 2, the performances of the examples 1-5 are better than those of the comparative example 1, and all the performances meet the requirements of GB17761-2018 on the combustion type of the secondary circuit and the electrical components connected with the secondary circuit in the safety technical Specification of electric bicycles. Both comparative examples 1 and 2 are not satisfactory. Presumably, because the addition of the compatibilization flame-retardant synergist leads to higher compatibility between PBT and PP and better compatibilization effect than that of the conventional PP-g-MAH, the materials obtained in examples 1-5 have more stable structures, higher melt flow rate and better flame-retardant effect, and the heat deformation temperature is greatly improved, so that the heat resistance of the materials can be enhanced due to the addition of the heat-conducting component. Secondly, it can be seen from table 2 that each performance of comparative example 2 is poor, and alkylphenol ethoxylate added in comparative example 2 is an existing adhesive and is not suitable for preparing PBT/PP alloy. Finally, it can be seen from table 2 that the performances of comparative example 3 are not significantly improved, i.e., the compatibilization flame retardant effect of the PBT/PP alloy is limited by only adding alkylphenol polyoxybutylene without adding the compatibilization flame retardant synergist.
Example 6
The composition of example 6 differs from that of example 1 in that the components of the compatibilization flame retardant synergist were replaced by 6 parts by weight of alkylphenol polyoxybutylene ester, 1 part of graphene and 3 parts of red phosphorus. The rest is the same as the component of the example 1.
Example 6 was prepared according to the same method as example 1.
Example 7
The composition of example 7 differs from that of example 2 in that the components of the compatibilization flame retardant synergist were replaced by a composition of 15 parts by weight of alkylphenol polyoxybutylene ester, 1 part of graphene and 4 parts of red phosphorus. The rest is the same as the component of the example 2.
Example 7 was prepared according to the same method as example 2.
Example 8
The composition of example 8 differs from that of example 2 in that the components of the compatibilization flame retardant synergist were replaced by 10 parts by weight of alkylphenol polyoxybutylene ester, 3 parts of graphene and 7 parts of red phosphorus. The rest is the same as the component of the example 2.
Example 8 was prepared according to the same method as example 2.
Example 9
The composition of example 9 differs from that of example 2 in that the components of the compatibilization flame retardant synergist were replaced by 10 parts by weight of alkylphenol polyoxybutylene ester, 3 parts of graphene and 7 parts of nano-scale red phosphorus. The rest is the same as the component of the example 2.
Example 9 was prepared according to the same method as example 2.
Example 10
The composition of example 10 was the same as the composition of example 9. The difference is that the preparation method of example 10 is as follows:
a) preparing alkylphenol polyoxybutylene ester according to the method,
b) preparing a compatibilization flame-retardant synergist: graphene and nano red phosphorus are coupled by alkylphenol polyoxybutylene ester, namely, the graphene and the nano red phosphorus are fully mixed firstly, and then the mixture is put into the alkylphenol polyoxybutylene ester for coupling treatment for 1.5 to 3 hours.
c) Preparing the raw materials according to the parts by weight of the raw materials, respectively drying PBT and PP in a vacuum drying oven for 6-10 hours,
d) only mixing the raw materials of the component A at the rotation speed of 750-1000rpm, uniformly mixing, cooling to room temperature,
e) adding the component A into a double-screw extruder through a main feeding hopper for melt blending; and (3) injecting the component B through a side feeding port, wherein the temperature of a double-screw extruder barrel is 210-240 ℃, the rotating speed of a screw is 180-220 r/min, and the extruded strip material is cooled by a water tank, drawn and then enters a granulator for granulation, so that the flame retardant material for the electric contact of the electric vehicle is obtained.
Test example 2
The materials obtained in examples 6 to 10 were injection-molded by an injection-molding machine to prepare test specimens. The performance test was carried out in accordance with the method of test example 1, and the test results are shown in Table 3.
Table 3 results of performance tests of examples 6 to 10
As can be seen from the comparison of Table 3 and Table 2, the performance of the material added with red phosphorus is further improved, the flame retardant grade of the material reaches V0 grade, and the material meets the requirements of GB17761-2018 on the combustion type of the main circuit and the electric components connected with the main circuit in the safety technical specification of electric bicycles. Comparing example 9 with examples 6-8, it can be seen that the melt flow rate scale heat distortion temperature is increased after the addition of nanoscale red phosphorus. Compared with example 9, the preparation method of example 10 can compatibilize the PBT/PP system, and the material performance is more excellent.
The specific embodiments described herein are merely illustrative of the spirit of the invention. Various modifications or additions may be made to the described embodiments or alternatives may be employed by those skilled in the art without departing from the spirit or ambit of the invention as defined in the appended claims.
Claims (10)
1. The flame retardant material for the electric contact element of the electric vehicle comprises a component A and a component B, and is characterized by comprising the following components in parts by weight:
and (2) component A:
and (B) component:
10-20 parts of a compatibilization flame-retardant synergist,
the compatibilization flame-retardant synergist consists of alkylphenol polyoxybutylene ester and graphene according to the weight ratio of 6-15: 4-10.
2. The flame retardant material of claim 1 wherein the graft copolymer compatibilizer is one or more of polypropylene copolymer grafted maleic anhydride, ethylene-octene copolymer grafted glycidyl methacrylate, ethylene-vinyl acetate copolymer grafted maleic anhydride, and ethylene-methyl acrylate-glycidyl methacrylate.
3. The flame retardant material for electric vehicle contacts as claimed in claim 2, wherein the graft copolymer compatibilizer has a grafting ratio of 4% or more.
4. The flame retardant material of claim 1, wherein the flame retardant is at least one of pentaerythritol diphosphate melamine salt, melamine cyanurate, aluminum hypophosphite, and triphenyl phosphate.
5. The flame retardant material for the electric contact of the electric vehicle as claimed in claim 1, wherein the compatibilization flame retardant synergist further comprises red phosphorus, and the compatibilization flame retardant synergist is composed of alkylphenol polyoxybutylene ester, graphene and red phosphorus according to a weight ratio of 6-15:1-3: 3-7.
6. The flame retardant material of claim 5, wherein said red phosphorus is nanoscale red phosphorus, and said graphene and said red phosphorus are coupled by alkylphenol polyoxybutylene.
7. The flame retardant material for use in electrical contacts for electric vehicles of claim 1 wherein said lubricant is at least one of silicone, dimethicone, methylphenylsilicone, polyethylene wax, stearic acid and soap of stearic acid.
8. The flame retardant material of claim 1, wherein the antioxidant is one or more of triethylene glycol bis-3- (3-tert-butyl-4-hydroxy-5-methylphenyl) acrylate, tetrakis [ methyl-beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ] pentaerythritol ester, tert-butylhydroquinone, and tris (2, 4-di-tert-butylphenol) phosphite.
9. Method for the preparation of a fire retardant material for electric vehicle electrical contacts according to any of claims 1-8, characterized in that it comprises the following steps:
a) preparing the alkylphenol polyoxybutylene ester,
b) the compatibilization flame-retardant synergist is prepared,
c) preparing the raw materials according to the parts by weight of the raw materials,
d) putting the raw materials into a high-speed mixer for mixing, cooling to room temperature after uniform mixing,
e) and (3) feeding the cooled mixed material into a double-screw extruder for melt extrusion, cooling the extruded strip material by a water tank, and drawing the cooled strip material into a granulator for granulation to obtain the flame retardant material for the electric contact of the electric vehicle.
10. The method for preparing a flame retardant material for an electric contact element of an electric vehicle according to claim 9, wherein in the step d), only raw materials of the component A are mixed, and in the step e), the component A is added into a twin-screw extruder through a main feeding hopper for melt blending; and injecting the component B through a side feeding port, and extruding and granulating to obtain the flame retardant material for the electric contact of the electric vehicle.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080071038A1 (en) * | 2005-03-11 | 2008-03-20 | Fujitsu Limited | Plant resin composition and plant resin molded product |
| CN102329479A (en) * | 2011-05-31 | 2012-01-25 | 深圳市科聚新材料有限公司 | Glass fiber reinforced PBT (Poly Butylenes Terephthalate)/PP (Polypropylene) alloy material and preparation method thereof |
| CN103254590A (en) * | 2013-05-10 | 2013-08-21 | 常熟市协新冶金材料有限公司 | Preparation method of environment-friendly fire-retardant polybutylene terephthalate alloy composite material |
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2019
- 2019-11-13 CN CN201911104719.9A patent/CN110724371A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20080071038A1 (en) * | 2005-03-11 | 2008-03-20 | Fujitsu Limited | Plant resin composition and plant resin molded product |
| CN102329479A (en) * | 2011-05-31 | 2012-01-25 | 深圳市科聚新材料有限公司 | Glass fiber reinforced PBT (Poly Butylenes Terephthalate)/PP (Polypropylene) alloy material and preparation method thereof |
| CN103254590A (en) * | 2013-05-10 | 2013-08-21 | 常熟市协新冶金材料有限公司 | Preparation method of environment-friendly fire-retardant polybutylene terephthalate alloy composite material |
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