CN110591299A - Halogen-free flame-retardant cable material for new energy automobile charging cable and preparation method - Google Patents
Halogen-free flame-retardant cable material for new energy automobile charging cable and preparation method Download PDFInfo
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Abstract
The invention relates to a halogen-free flame-retardant cable material for a new energy automobile charging cable and a preparation method thereof, wherein the halogen-free flame-retardant cable material comprises 50-80 wt% of thermoplastic polyester elastomer serving as a resin base material, 20-50 wt% of halogen-free flame retardant and 0-2 wt% of processing aid. Adopting a double-screw extruder for direct processing, mixing all the components except the synergist, and feeding through a feeding port; the synergist is fed through the side feeding of the middle section of the equipment, and the processing temperature of the double-screw extruder is 170-220 ℃. Compared with the prior art, the halogen-free flame retardant cable material has good balance between halogen-free flame retardant and high-performance cable material, and effectively solves the problem that the charging cable cannot realize high-efficiency halogen-free flame retardant while considering mechanical properties.
Description
Technical Field
The invention relates to a cable for a new energy automobile, in particular to a halogen-free flame-retardant cable material for a charging cable of the new energy automobile and a preparation method thereof.
Background
New energy automobile charging cable is the basic component part of new energy automobile charging circuit and the electric pile facility of filling, and its performance has important influence to whole charging process. The main raw materials of the outer sleeve protection material of the automobile charging cable comprise a PVC (polyvinyl chloride) cable, a cross-linked polyolefin cable and a TPE cable. The PVC cable is low in price, and the branch structure contains chlorine atoms, so that the PVC cable has good flame retardant property. However, since the conventional PVC electric wires and cables release a great amount of smoke and toxic hydrogen chloride gas during the burning process, the usage amount of the PVC electric wires and cables has been reduced in recent years, and although it is unlikely that the PVC electric wires and cables disappear completely, the market occupation amount and the reduction of the usage amount have become an irreversible trend. The crosslinked polyolefin cable refers to a cable in which polyethylene is subjected to high-energy radiation and can be converted from a linear molecular structure into a three-dimensional structure of a body type under a certain condition. The cross-linked polyolefin cable has the advantages of corrosion resistance, acid and alkali resistance and excellent mechanical property due to the structure. However, the development of the method is severely limited by the defects of complicated process and easy deformation at high temperature.
Many studies on domestic and foreign halogen-free flame-retardant cable materials are made, and patents CN103788442A, CN103724783A, CN103571008A and CN103450551A indicate some novel high-performance flame-retardant polyolefin cable materials and preparation methods thereof, however, in the field of halogen-free flame-retardant cables, main studies still mainly use inorganic flame retardants such as magnesium hydroxide and aluminum hydroxide as main materials. Although inorganic flame retardants are inexpensive, their disadvantages are likewise quite evident. The product can only be used in the low-end field due to the large addition amount of the inorganic flame retardant, the serious damage to the matrix structure, the poor compatibility, the easy precipitation and easy migration, the easy aging and peeling of the cable, the short service life and the like, and the use safety is also obviously reduced along with the aging of the cable, so that the product can not meet the requirements of the field with high flame-retardant requirement. With the improvement of environmental protection consciousness and fire safety consciousness and the increasingly severe requirements of the market on the flame-retardant cable, the development of high-performance flame-retardant cable materials has been widely regarded in the professional field.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a halogen-free flame-retardant cable material for a new energy automobile charging cable with mechanical property, processability and flame retardance and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme: the halogen-free flame-retardant cable material for the new energy automobile charging cable is characterized in that a thermoplastic polyester elastomer (TPEE) is used as a resin base material, and a halogen-free flame retardant is used for endowing the resin base material with flame retardant performance, and specifically comprises 50-80 wt% of the thermoplastic polyester elastomer used as the resin base material, 20-50 wt% of the halogen-free flame retardant and 0-2 wt% of a processing aid.
The halogen-free flame retardant comprises the following components in percentage by weight: 30-70 wt% of main flame retardant, 10-50 wt% of auxiliary flame retardant, 0-30 wt% of synergist and 0-10 wt% of synergist.
The halogen-free flame retardant comprises the following components in percentage by weight: 40-60 wt% of main flame retardant, 20-40 wt% of auxiliary flame retardant, 10-20 wt% of synergist and 2-5 wt% of synergist.
The main flame retardant is piperazine pyrophosphate and/or a coating treatment product thereof; the material coated by the piperazine pyrophosphate can be one or more of hydrogen-containing silicone oil, methyl silicone oil, silane coupling agent, titanate coupling agent, epoxy resin, melamine resin and the like; the coating method may be a conventional coating method disclosed in the art, such as dry coating using high-speed stirring, wet coating using solvent dispersion, resin melt coating, and the like.
The secondary flame retardant is at least one of piperazine phosphate, piperazine diphosphate, melamine phosphate, melamine polyphosphate, dimelamine pyrophosphate, melamine cyanurate and ammonium polyphosphate;
the synergist is a halogen-free phosphate compound, and comprises one or more of methyl dimethyl phosphate, ethyl diethyl phosphate, triphenyl phosphate, triisopropylbenzene phosphate, resorcinol bis (diphenyl) phosphate and resorcinol bis (2, 6-dimethylphenyl) phosphate;
the synergist is one or more of zinc oxide, titanium dioxide, aluminum oxide, magnesium oxide, zinc borate, zinc stannate and lead stannate.
The particle size of the halogen-free flame retardant in the cable material is D50<10 microns, and the preferred particle size is D50<8 microns.
The hard segment of the thermoplastic polyester elastomer is polybutylene terephthalate (PBT), the soft segment of the thermoplastic polyester elastomer is polyether or polyester, wherein the polyether is polyether such as polyethylene glycol ether, polypropylene glycol ether or polybutylene glycol ether; the polyester is polylactide, polyglycolide or polycaprolactone.
The auxiliary agent comprises one or more of polyethylene wax, stearic acid, butyl stearate, oleamide, ethylene bis stearamide, 1, 3-tri (2-methyl-4-hydroxy-5-tert-butyl phenyl) butane, 1, 3-tri (2-methyl-4-hydroxy-5-tert-butyl phenol), 3, 5-dibutyl-4-hydroxy octadecyl phenylpropionate, 2 '-methylene bis (4-methyl-6-tert-butyl) phenol and 4, 4' -thiobis (3-methyl-6-tert-butyl) phenol.
A preparation method of a halogen-free flame-retardant cable material for a new energy automobile charging cable is characterized in that a double-screw extruder is adopted for direct processing, all components except a synergist are mixed and then fed through a feeding port; the synergist is fed through the side feeding of the middle section of the equipment, and the processing temperature of the double-screw extruder is 170-220 ℃.
The double-screw extruder is a 65-type double-screw extruder, and the processing temperature is 180-200 ℃.
Compared with the prior art, the modified cable material provided by the invention has excellent flame retardant property, and has the same excellent electrical breakdown and bending resistance, tensile strength, oil resistance and other properties as a charging cable. The invention provides a novel thermoplastic polyester elastomer (TPEE) halogen-free flame-retardant cable material, which well balances halogen-free flame retardance and high-performance cable materials, and effectively solves the problem that the charging cable cannot realize high-efficiency halogen-free flame retardance while taking mechanical properties into consideration.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1:
6.9kg of TPEE, 1.5kg of piperazine pyrophosphate, 0.8kg of melamine polyphosphate, 0.2kg of zinc oxide, 0.05kg of white carbon black and 0.05kg of butyl stearate are added into a 50L high-speed mixer to be mixed for 3 minutes at the rotating speed of 800 revolutions per minute. The mixed material was fed at constant speed through the main feed port of a type 65 extruder. 0.5kg of dimethyl methyl phosphate is synchronously fed through an auxiliary feeding port in the middle of the extruder, and when the feeding of the main feeding port is finished, the feeding of the materials of the auxiliary feeding port is also finished just by adjusting the feeding speed. The processing temperature of the type 65 extruder was 190 ℃. The obtained modified material can pass the UL94V-1(1.6mm) grade and cannot pass the VW-1 single vertical combustion test by a performance test; the tensile strength is 20.2MPa, and the elongation at break is 657%.
Example 2:
6.9kg of TPEE, 1.5kg of piperazine pyrophosphate, 0.8kg of melamine polyphosphate, 0.2kg of zinc oxide, 0.05kg of white carbon black and 0.05kg of butyl stearate are added into a 50L high-speed mixer to be mixed for 3 minutes at the rotating speed of 800 revolutions per minute. The mixed material was fed at constant speed through the main feed port of a type 65 extruder. 0.5kg of dimethyl methyl phosphate is synchronously fed through an auxiliary feeding port in the middle of the extruder, and when the feeding of the main feeding port is finished, the feeding of the materials of the auxiliary feeding port is also finished just by adjusting the feeding speed. The processing temperature of the type 65 extruder was 190 ℃. The obtained modified material can pass the UL94V-1(1.6mm) grade and cannot pass the VW-1 single vertical combustion test by a performance test; tensile strength 21.5MPa, elongation at break 655%.
Example 3:
6.9kg of TPEE, 1.5kg of piperazine pyrophosphate, 0.8kg of melamine polyphosphate, 0.2kg of zinc oxide, 0.05kg of white carbon black and 0.05kg of butyl stearate are added into a 50L high-speed mixer to be mixed for 3 minutes at the rotating speed of 800 revolutions per minute. The mixed material was fed at constant speed through the main feed port of a type 65 extruder. 0.5kg of dimethyl methyl phosphate is synchronously fed through an auxiliary feeding port in the middle of the extruder, and when the feeding of the main feeding port is finished, the feeding of the materials of the auxiliary feeding port is also finished just by adjusting the feeding speed. The processing temperature of the type 65 extruder was 190 ℃. The obtained modified material is subjected to a performance test, and can pass a UL94V-0(1.6mm) grade and a VW-1 single vertical combustion test; the tensile strength is 21.8MPa, and the elongation at break is 668%.
Example 4:
6.9kg of TPEE, 1.5kg of piperazine pyrophosphate, 0.8kg of melamine polyphosphate, 0.2kg of zinc oxide, 0.05kg of white carbon black and 0.05kg of butyl stearate are added into a 50L high-speed mixer to be mixed for 3 minutes at the rotating speed of 800 revolutions per minute. The mixed material was fed at constant speed through the main feed port of a type 65 extruder. 0.5kg of dimethyl methyl phosphate is synchronously fed through an auxiliary feeding port in the middle of the extruder, and when the feeding of the main feeding port is finished, the feeding of the materials of the auxiliary feeding port is also finished just by adjusting the feeding speed. The processing temperature of the type 65 extruder was 190 ℃. The obtained modified material is subjected to a performance test, and can pass a UL94V-0(1.6mm) grade and a VW-1 single vertical combustion test; the tensile strength is 17.7MPa, and the elongation at break is 610%.
Example 5:
6.9kg of TPEE, 1.5kg of piperazine pyrophosphate, 0.8kg of melamine polyphosphate, 0.2kg of zinc oxide, 0.05kg of white carbon black and 0.05kg of butyl stearate are added into a 50L high-speed mixer to be mixed for 3 minutes at the rotating speed of 800 revolutions per minute. The mixed material was fed at constant speed through the main feed port of a type 65 extruder. 0.5kg of dimethyl methyl phosphate is synchronously fed through an auxiliary feeding port in the middle of the extruder, and when the feeding of the main feeding port is finished, the feeding of the materials of the auxiliary feeding port is also finished just by adjusting the feeding speed. The processing temperature of the type 65 extruder was 190 ℃. The obtained modified material is subjected to a performance test, and can pass a UL94V-0(1.6mm) grade and a VW-1 single vertical combustion test; the tensile strength is 18.3MPa, and the elongation at break is 635%.
Example 6:
6.9kg of TPEE, 1.5kg of piperazine pyrophosphate, 0.8kg of melamine polyphosphate, 0.2kg of zinc oxide, 0.05kg of white carbon black and 0.05kg of butyl stearate are added into a 50L high-speed mixer to be mixed for 3 minutes at the rotating speed of 800 revolutions per minute. The mixed material was fed at constant speed through the main feed port of a type 65 extruder. 0.5kg of dimethyl methyl phosphate is synchronously fed through an auxiliary feeding port in the middle of the extruder, and when the feeding of the main feeding port is finished, the feeding of the materials of the auxiliary feeding port is also finished just by adjusting the feeding speed. The processing temperature of the type 65 extruder was 190 ℃. The obtained modified material is subjected to a performance test, and can pass a UL94V-0(1.6mm) grade and a VW-1 single vertical combustion test; the tensile strength is 17.1MPa, and the elongation at break is 622%.
Example 7:
6.9kg of TPEE, 1.5kg of piperazine pyrophosphate, 0.8kg of melamine polyphosphate, 0.2kg of zinc oxide, 0.05kg of white carbon black and 0.05kg of butyl stearate are added into a 50L high-speed mixer to be mixed for 3 minutes at the rotating speed of 800 revolutions per minute. The mixed material was fed at constant speed through the main feed port of a type 65 extruder. 0.5kg of dimethyl methyl phosphate is synchronously fed through an auxiliary feeding port in the middle of the extruder, and when the feeding of the main feeding port is finished, the feeding of the materials of the auxiliary feeding port is also finished just by adjusting the feeding speed. The processing temperature of the type 65 extruder was 190 ℃. The obtained modified material is subjected to a performance test, and can pass a UL94V-0(1.6mm) grade and a VW-1 single vertical combustion test; the tensile strength is 14.8MPa, and the elongation at break is 589%.
Example 8:
6.9kg of TPEE, 1.5kg of piperazine pyrophosphate, 0.8kg of melamine polyphosphate, 0.2kg of zinc oxide, 0.05kg of white carbon black and 0.05kg of butyl stearate are added into a 50L high-speed mixer to be mixed for 3 minutes at the rotating speed of 800 revolutions per minute. The mixed material was fed at constant speed through the main feed port of a type 65 extruder. 0.5kg of dimethyl methyl phosphate is synchronously fed through an auxiliary feeding port in the middle of the extruder, and when the feeding of the main feeding port is finished, the feeding of the materials of the auxiliary feeding port is also finished just by adjusting the feeding speed. The processing temperature of the type 65 extruder was 190 ℃. The obtained modified material is subjected to a performance test, and can pass a UL94V-0(1.6mm) grade and a VW-1 single vertical combustion test; the tensile strength is 15.8MPa, and the elongation at break is 612 percent.
Example 9:
6.9kg of TPEE, 1.5kg of piperazine pyrophosphate, 0.8kg of melamine polyphosphate, 0.2kg of zinc oxide, 0.05kg of white carbon black and 0.05kg of butyl stearate are added into a 50L high-speed mixer to be mixed for 3 minutes at the rotating speed of 800 revolutions per minute. The mixed material was fed at constant speed through the main feed port of a type 65 extruder. 0.5kg of dimethyl methyl phosphate is synchronously fed through an auxiliary feeding port in the middle of the extruder, and when the feeding of the main feeding port is finished, the feeding of the materials of the auxiliary feeding port is also finished just by adjusting the feeding speed. The processing temperature of the type 65 extruder was 190 ℃. The obtained modified material is subjected to a performance test, and can pass a UL94V-0(1.6mm) grade and a VW-1 single vertical combustion test; the tensile strength is 16.6MPa, and the elongation at break is 622%.
Comparative example 1:
6.9kg of TPEE, 3.0kg of piperazine pyrophosphate, 0.05kg of white carbon black and 0.05kg of butyl stearate are added into a 50L high-speed mixer and mixed for 3 minutes at the rotating speed of 800 rpm. The mixed material was fed at constant speed through the main feed port of a type 65 extruder. The processing temperature of the type 65 extruder was 190 ℃. The obtained modified material is subjected to a performance test, passes the UL94V-2(1.6mm) grade and cannot pass a VW-1 single vertical combustion test; the tensile strength is 20.2MPa, and the elongation at break is 612 percent.
Comparative example 2:
the TPEE is directly tested, cannot pass UL94 without grade, and cannot pass a VW-1 single vertical combustion test; the tensile strength is 26.3MPa, and the elongation at break is 710%.
Compared with the comparative example, the TPEE material has high-efficiency flame retardant property, mechanical property and electrical property, is halogen-free and flame retardant, is green and environment-friendly, and can be applied to the charging line of new energy vehicles.
Example 10
The halogen-free flame-retardant cable material for the new energy automobile charging cable specifically comprises 50 wt% of thermoplastic polyester elastomer serving as a resin base material, 48 wt% of halogen-free flame retardant and 2 wt% of processing aid.
The halogen-free flame retardant comprises the following components in percentage by weight: 30-70 wt% of main flame retardant piperazine pyrophosphate, 10-50 wt% of auxiliary flame retardant piperazine phosphate, 0-30 wt% of synergist dimethyl methyl phosphate and 0-10 wt% of synergist zinc oxide.
The hard segment of the thermoplastic polyester elastomer is polybutylene terephthalate (PBT), and the soft segment of the thermoplastic polyester elastomer is polyethylene glycol ether. The chemical auxiliary agent is polyethylene wax.
According to the preparation method of the halogen-free flame-retardant cable material for the new energy automobile charging cable, a double-screw extruder is adopted for direct processing, and all components except the synergist are mixed and then fed through a feeding port; the synergist is fed through the side feeding of the middle section of the equipment, and the processing temperature of the double-screw extruder is 170 ℃.
The obtained modified material is subjected to a performance test, and can pass a UL94V-0(1.6mm) grade and a VW-1 single vertical combustion test; the tensile strength is 19.8MPa, and the elongation at break is 672 percent.
Example 11
A halogen-free flame-retardant cable material for a new energy automobile charging cable specifically comprises 80 wt% of a thermoplastic polyester elastomer serving as a resin base material and 20 wt% of a halogen-free flame retardant.
The halogen-free flame retardant comprises the following components in percentage by weight: 30-70 wt% of main flame retardant piperazine pyrophosphate, 10-50 wt% of secondary flame retardant ammonium polyphosphate, 0-30 wt% of synergist triisopropylbenzene phosphate and 0-10 wt% of synergist titanium dioxide.
The hard segment of the thermoplastic polyester elastomer is polybutylene terephthalate (PBT), and the soft segment of the thermoplastic polyester elastomer is polycaprolactone.
According to the preparation method of the halogen-free flame-retardant cable material for the new energy automobile charging cable, a double-screw extruder is adopted for direct processing, and all components except the synergist are mixed and then fed through a feeding port; the synergist is fed through the side feeding of the middle section of the equipment, and the processing temperature of the double-screw extruder is 220 ℃.
The obtained modified material is subjected to a performance test, and can pass a UL94V-0(1.6mm) grade and a VW-1 single vertical combustion test; the tensile strength is 17.8MPa, and the elongation at break is 666%.
Claims (9)
1. The halogen-free flame-retardant cable material for the new energy automobile charging cable is characterized by comprising 50-80 wt% of thermoplastic polyester elastomer serving as a resin base material, 20-50 wt% of halogen-free flame retardant and 0-2 wt% of processing aid.
2. The halogen-free flame-retardant cable material for the new energy automobile charging cable according to claim 1, wherein the halogen-free flame retardant comprises the following components in percentage by weight: 30-70 wt% of main flame retardant, 10-50 wt% of auxiliary flame retardant, 0-30 wt% of synergist and 0-10 wt% of synergist.
3. The halogen-free flame-retardant cable material for the new energy automobile charging cable according to claim 2, wherein the halogen-free flame retardant comprises the following components in percentage by weight: 40-60 wt% of main flame retardant, 20-40 wt% of auxiliary flame retardant, 10-20 wt% of synergist and 2-5 wt% of synergist.
4. The halogen-free flame-retardant cable material for the charging cable of the new energy automobile as claimed in claim 2 or 3, wherein the main flame retardant is piperazine pyrophosphate and/or a coating treatment product thereof;
the secondary flame retardant is at least one of piperazine phosphate, piperazine diphosphate, melamine phosphate, melamine polyphosphate, dimelamine pyrophosphate, melamine cyanurate and ammonium polyphosphate;
the synergist is a halogen-free phosphate compound, and comprises one or more of methyl dimethyl phosphate, ethyl diethyl phosphate, triphenyl phosphate, triisopropylbenzene phosphate, resorcinol bis (diphenyl) phosphate and resorcinol bis (2, 6-dimethylphenyl) phosphate;
the synergist is one or more of zinc oxide, titanium dioxide, aluminum oxide, magnesium oxide, zinc borate, zinc stannate and lead stannate.
5. The halogen-free flame-retardant cable material for the charging cable of the new energy automobile as claimed in claim 1, wherein the particle size of the halogen-free flame retardant in the cable material is D50<10 microns, preferably D50<8 microns.
6. The halogen-free flame-retardant cable material for the new energy automobile charging cable according to claim 1, wherein the hard segment of the thermoplastic polyester elastomer is polybutylene terephthalate (PBT), and the soft segment of the thermoplastic polyester elastomer is polyether or polyester, wherein the polyether is polyether such as polyethylene glycol ether, polypropylene glycol ether or polybutylene glycol ether; the polyester is polylactide, polyglycolide or polycaprolactone.
7. The halogen-free flame-retardant cable material for the new energy automobile charging cable according to claim 1, wherein the processing aid comprises one or more of polyethylene wax, stearic acid, butyl stearate, oleamide, ethylene bis stearamide, 1, 3-tris (2-methyl-4-hydroxy-5-tert-butylphenyl) butane, 1, 3-tris (2-methyl-4-hydroxy-5-tert-butylphenol), 3, 5-dibutyl-4-hydroxy octadecyl phenylpropionate, 2 '-methylene bis (4-methyl-6-tert-butyl) phenol, and 4, 4' -thiobis (3-methyl-6-tert-butyl) phenol.
8. The preparation method of the halogen-free flame-retardant cable material for the charging cable of the new energy automobile as claimed in claim 1, characterized in that the direct processing is carried out by adopting a double-screw extruder, and all the components except the synergist are mixed and then fed through a feeding port; the synergist is fed through the side feeding of the middle section of the equipment, and the processing temperature of the double-screw extruder is 170-220 ℃.
9. The preparation method of the halogen-free flame-retardant cable material for the charging cable of the new energy automobile as claimed in claim 8, wherein the twin-screw extruder is a 65-type twin-screw extruder, and the processing temperature is 180-200 ℃.
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Application publication date: 20191220 |