CN113754945B - PET (polyethylene terephthalate) fiber filling low-smoke halogen-free material and preparation method thereof - Google Patents
PET (polyethylene terephthalate) fiber filling low-smoke halogen-free material and preparation method thereof Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
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Abstract
The invention provides a PET fiber filling low-smoke halogen-free material and a preparation method thereof. The raw material composition of the PET cellosilk filled low-smoke halogen-free material comprises: 60-100 parts of polar copolymer resin, 10-50 parts of polyolefin resin, 0-40 parts of POE resin, 10-50 parts of compatilizer, 100-200 parts of inorganic flame retardant hydroxide, 10-40 parts of PET (polyethylene terephthalate) fiber, 0.5-2.5 parts of surface modifier, 1-5 parts of lubricant and 0.5-1.5 parts of antioxidant. The invention also provides a preparation method of the halogen-free material. The PET fiber filling low-smoke halogen-free material has good mechanical property, electrical property and flame retardant carbon forming property.
Description
Technical Field
The invention relates to a halogen-free material, in particular to a low-smoke halogen-free material filled with PET (polyethylene terephthalate) fiber yarns and a preparation method thereof, belonging to the technical field of polymer composite materials.
Background
The low-smoke halogen-free flame-retardant polyolefin cable material is widely applied and accepted as an environment-friendly material in the aspects of wires and cables, and the quantity and the type of the polyolefin cable material are rapidly developed along with the continuous development and the demand of the market.
The low-smoke halogen-free cable is an environment-friendly cable which is made of rubber materials which do not contain halogen (F, cl, br, I, at), lead, cadmium, chromium, mercury and other harmful environmental substances and can not emit toxic smoke during combustion. The volume resistance of the conventional low-smoke halogen-free material is 10 11 Omega cm or so, the high-resistance low-smoke halogen-free material cannot meet the requirement of high-power cables on high resistance of low-smoke halogen-free materials.
Due to the continuously expanded application range of the low-smoke halogen-free material, besides the requirements, a plurality of special requirements can be provided according to the difference of the use conditions, and along with the upgrade of products, higher technical requirements can be provided for the low-smoke halogen-free material.
At present, in the wire and cable industry, new products of low-smoke halogen-free flame retardant materials are continuously required and released in the wire and cable industry, and the research and development problems of low-smoke halogen-free flame retardant polyolefin cable materials with high resistance and high mechanical properties need to be solved urgently.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a low-smoke halogen-free material with good mechanical property, electrical property and flame-retardant char formation property and a preparation method thereof.
In order to achieve the technical purpose, the invention firstly provides a low-smoke halogen-free material filled with PET fiber yarns, and the raw material composition of the low-smoke halogen-free material filled with PET fiber yarns comprises the following components in parts by weight:
60-100 parts of polar copolymer resin, 10-50 parts of polyolefin resin, 0-40 parts of POE resin, 10-50 parts of compatilizer, 100-200 parts of inorganic flame retardant hydroxide, 10-40 parts of PET (polyethylene terephthalate) fiber, 0.5-2.5 parts of surface modifier, 1-5 parts of lubricant and 0.5-1.5 parts of antioxidant.
The PET fiber filament filling low-smoke halogen-free material has good mechanical property, electrical property and flame retardant carbon forming property, the processing temperature of the low-smoke halogen-free material is below 170 ℃, the processing temperature is far lower than the melting point of PET resin, the PET fiber filament always exists in the low-smoke halogen-free material in a fiber structure form, and the mechanical property of the low-smoke halogen-free material can be obviously improved due to the large rigidity and the good flame retardant carbon forming property of a PET benzene ring. Meanwhile, under the action of the compatilizer, the PET fibers and the polar copolymer resin can react, so that a net structure is formed, and the anti-cracking performance of the low-smoke halogen-free material is improved; and PET has polarity higher than that of polyethylene and better compatibility with inorganic flame retardant hydroxide.
In one embodiment of the present invention, the polar copolymer resin used is at least one of EVA (ethylene-vinyl acetate copolymer), EEA (ethylene-ethyl acrylate copolymer), and EBA (ethylene-butyl acrylate copolymer). Preferably, the polar copolymer resin is EVA (ethylene-vinyl acetate copolymer) with the melt index of 2.0-10.0g/10min, wherein the mass content of Vinyl Acetate (VA) is 17-40%.
In one embodiment of the present invention, the polyolefin resin used is Polyethylene (PE) and/or metallocene linear low density polyethylene (mLLDPE).
In one embodiment of the present invention, the POE resin used has a melt index of 0.5 to 5.0g/10min.
In one embodiment of the present invention, the compatibilizer used is one or a combination of Maleic Anhydride (MAH) grafted compatibilizer or Glycidyl Methacrylate (GMA) grafted compatibilizer grafted PE or POE. The preferred compatibilizer used is Maleic Anhydride (MAH) used in conjunction with a graft-type compatibilizer graft of Glycidyl Methacrylate (GMA), such as Surlyn resin.
In one embodiment of the present invention, the inorganic flame retardant hydroxide used is an aluminum hydroxide flame retardant and/or a magnesium hydroxide flame retardant.
In a specific embodiment of the invention, the adopted PET fiber yarns are PET fiber yarns obtained by (recycled) PET film, PET textile fabric and PET bottle filament blowing; preferably, the length of the PET fiber is less than or equal to 3mm.
In one embodiment of the present invention, the surface modifying agent used is a polysiloxane and/or a silane coupling agent.
In a specific embodiment of the present invention, the lubricant used is one or a combination of several of EVA wax (ethylene-vinyl acetate copolymer wax), PE wax (polyethylene wax), silicone oil, stearic acid, and stearate.
In one embodiment of the present invention, the antioxidant employed is selected from antioxidant 1010, i.e., the antioxidant tetrakis [ beta- (3,5-di-tert-butyl-4-hydroxyphenyl) propanoic acid ] pentaerythritol ester; antioxidant 1076, namely antioxidant beta- (3,5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl ester; antioxidant 168, namely the antioxidant tris (2,4-di-tert-butylphenyl) phosphite; antioxidant 300, antioxidant 4,4' -thiobis (6-tert-butyl-3-methylphenol); antioxidant DLTP, i.e., a combination of one or more of the antioxidants lauryl thiopropionate.
In order to achieve the purpose, the invention also provides a preparation method of the PET filament filled low-smoke halogen-free material, which comprises the following steps:
polar copolymer resin, polyolefin resin, POE resin, compatilizer, half part of inorganic flame retardant hydroxide, PET fiber yarns, surface modifier, lubricant and antioxidant are mixed at high speed, the mixture is discharged after being mixed uniformly, the mixture is fed into a first feeding port of a BUSS high-speed shearing machine, the other half part of inorganic flame retardant hydroxide is fed into a second feeding port of the BUSS high-speed shearing machine, and granules of the PET fiber yarns filled with the low-smoke halogen-free material are obtained after plasticization, single-screw granulation and drying.
In one embodiment of the invention, the parameters of high-speed mixing are 100-200rpm, and the material is discharged when the temperature is raised to 50 ℃;
BUSS host screw temperature: 130 +/-10 ℃;
temperature of the granulation screw: 160 +/-10 ℃;
temperature of the granulator: 165 +/-5 ℃;
the variation amplitude of the rotating speed/torque of the screw of the main machine is 300 +/-50/40-60;
the rotating speed/torque of the granulation screw is 40 +/-5/30-40;
the rotating speed of the granulator is 600 +/-100, the upper-stage material temperature is 150 +/-5 ℃, and the pressure of the vacuum pump is 0.5-1.0bar;
the water spraying pressure is 0-2bar.
The melting point of the PET resin of the low-smoke halogen-free material filled with the PET fiber yarns is higher than the processing temperature of the low-smoke halogen-free material, the PET fiber yarns always exist in the low-smoke halogen-free material in a fiber structure form, the rigidity of PET benzene rings is high, the flame-retardant carbonization property is good, and the mechanical property of the low-smoke halogen-free material can be obviously improved. Meanwhile, under the action of the compatilizer, the PET fibers and the polar copolymer resin can react, so that a net structure is formed, and the cracking resistance of the low-smoke halogen-free material is improved; and PET has polarity higher than that of polyethylene, and has better compatibility with inorganic flame retardant hydroxide.
The PET fiber filling low-smoke halogen-free material has good mechanical property, electrical property and flame retardant carbon forming property.
The preparation method of the PET fiber filling low-smoke halogen-free material has the advantages of stable process, high yield and high efficiency.
Detailed Description
The invention provides a PET (polyethylene terephthalate) fiber filling low-smoke halogen-free material which comprises the following components in parts by weight:
60-100 parts of polar copolymer resin;
10-50 parts of polyolefin resin;
0-40 parts of POE resin;
10-50 parts of a compatilizer;
100-200 parts of inorganic flame retardant hydroxide;
10-40 parts of PET fiber yarns;
0.5-2.5 parts of a surface modifier;
1-5 parts of a lubricant;
0.5-1.5 parts of antioxidant.
The PET filament is obtained by recovering and blowing PET films, PET textiles and PET bottles. Preferably, the length of the PET fiber is less than or equal to 3mm.
The polar copolymer resin is ethylene-vinyl acetate copolymer EVA with a melt index of 2.0-10.0g/10min and a vinyl acetate VA content of 17-40%.
The polyolefin resin is metallocene linear low density polyethylene mLLDPE with a melt index of 1.0-15.0g/10min.
The POE resin has a melt index of 0.5-5.0g/10min.
The compatilizer is Maleic Anhydride (MAH) and Glycidyl Methacrylate (GMA) graft type compatilizer graft, and Surlyn resin.
The inorganic flame retardant hydroxide is used together with an aluminum hydroxide flame retardant and a magnesium hydroxide flame retardant, wherein the aluminum hydroxide flame retardant accounts for 90-150 parts, and the magnesium hydroxide flame retardant accounts for 10-50 parts.
The surface modifier is polysiloxane, and the Dow Corning is 11-100.
The lubricant is polyethylene wax and silicone, wherein the polyethylene wax is 0.5-1.5 parts, and the silicone is 0.5-3.5 parts.
The antioxidant is selected from antioxidant 1010, namely antioxidant tetra [ beta- (3,5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester; the antioxidant 1076 is one or two of antioxidant beta- (3,5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl ester.
In the invention, the antioxidant is antioxidant 1010, namely antioxidant tetra [ beta- (3,5-di-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester and antioxidant 1076, namely a mixture of antioxidant beta- (3,5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl ester, wherein the weight of the antioxidant 1010 is 0.4-1.2 parts, and the weight of the antioxidant 1076 is 0.1-0.3 part.
The preparation method of the PET fiber yarn filled low-smoke halogen-free material comprises the following steps: the PET fiber filament filled low-smoke halogen-free material particles are produced by adopting a Swiss import BUSS line, the weighed polar copolymer resin, polyolefin resin, POE resin, compatilizer, half part of inorganic flame retardant hydroxide, PET fiber filaments, surface modifier, lubricant and antioxidant are mixed at high speed, the mixture is uniformly mixed and then discharged, the mixture is fed into a first feeding port of a BUSS high-speed shearing machine, the other half part of inorganic flame retardant hydroxide is fed into a second feeding port of the BUSS high-speed shearing machine, and the PET fiber filament filled low-smoke halogen-free material particles are obtained through plasticization, single-screw granulation and drying. The parameters are as follows: the parameters of the high-speed mixer are 100-200rpm, and the material is discharged when the temperature is raised to 50 ℃; BUSS host screw temperature: 130 +/-10 ℃; temperature of the granulation screw: 160 +/-10 ℃; temperature of the granulator: 165 +/-5 ℃; the variation amplitude of the rotation speed/torque of a screw of the host machine is 300 +/-50/40-60, the rotation speed/torque of a granulating screw is 40 +/-5/30-40, the rotation speed of a granulator is 600 +/-100, the temperature of the upper-stage material is 150 +/-5 ℃, and the pressure of a vacuum pump is 0.5-1.0bar; the water spraying pressure is 0-2bar.
The following provides a detailed description of preferred embodiments of the invention.
Example 1
The embodiment provides a low-smoke halogen-free material filled with PET (polyethylene terephthalate) fiber yarns, which comprises the following components in parts by weight:
80 parts of polar copolymer resin; (EVA)
30 parts of polyolefin resin; (mLLDPE)
20 parts of POE resin;
30 parts of a compatilizer; (Surlyn resin)
150 parts of inorganic flame retardant hydroxide; (aluminum hydroxide 120 parts, magnesium hydroxide 30 parts)
25 parts of PET fiber yarns;
1.5 parts of a surface modifier; (polysiloxanes)
3 parts of a lubricant; (polyethylene wax 1 part, silicone 2 parts)
1 part of an antioxidant; (antioxidant 1010)
The preparation method of the embodiment comprises the following steps: the PET fiber filament filled low-smoke halogen-free material particles are produced by adopting a Swiss import BUSS line, and the PET fiber filament filled low-smoke halogen-free material particles are obtained by mixing weighed polar copolymer resin, polyolefin resin, POE resin, compatilizer, half part of inorganic flame retardant hydroxide, PET fiber filaments, surface modifier, lubricant and antioxidant at high speed, uniformly mixing, discharging, feeding into a first feeding port of a BUSS high-speed shearing machine, feeding the other half part of inorganic flame retardant hydroxide into a second feeding port of the BUSS high-speed shearing machine, plasticizing, granulating by a single screw rod and drying;
wherein the parameter of the high-speed mixer is 100-200rpm, and the material is discharged when the temperature is raised to 50 ℃; BUSS host screw temperature: 130 +/-10 ℃; temperature of the granulation screw: 160 +/-10 ℃; temperature of the granulator: 165 +/-5 ℃; the variation amplitude of the rotation speed/torque of a screw of the host machine is 300 +/-50/40-60, the rotation speed/torque of a granulating screw is 40 +/-5/30-40, the rotation speed of a granulator is 600 +/-100, the temperature of the upper-stage material is 150 +/-5 ℃, and the pressure of a vacuum pump is 0.5-1.0bar; the water spraying pressure is 0-2bar.
Example 2
The embodiment provides a low-smoke halogen-free material filled with PET fiber yarns, the preparation method of which is completely the same as that of embodiment 1, except that the raw material components are different, and the low-smoke halogen-free material comprises the following components in parts by weight:
100 parts of polar copolymer resin; (EVA)
50 parts of polyolefin resin; (mLLDPE 40 parts, PE 10 parts)
40 parts of POE resin;
50 parts of a compatilizer; (GMA graft 37.5 parts, MAH graft 12.5 parts)
200 parts of inorganic flame retardant hydroxide; (aluminum hydroxide 150 parts, magnesium hydroxide 50 parts)
40 parts of PET fiber yarns;
2.5 parts of a surface modifier; (polysiloxanes)
5 parts of a lubricant; (polyethylene wax 1.5 parts, silicone 3.5 parts)
1.5 parts of an antioxidant; (antioxidant 1010.2 parts, antioxidant 1076.3 parts)
Example 3
The embodiment provides a low-smoke halogen-free material filled with PET fiber yarns, which has the same preparation method as that of embodiment 1, and is different from the raw material components in part by weight:
60 parts of polar copolymer resin; (EVA)
10 parts of polyolefin resin; (mLLDPE)
10 parts of a compatilizer; (Surlyn resin)
100 parts of inorganic flame retardant hydroxide; (aluminum hydroxide 90 parts, magnesium hydroxide 10 parts)
10 parts of PET fiber yarns;
0.5 part of a surface modifier; (polysiloxanes)
1 part of a lubricant; (polyethylene wax 0.5 part, silicone 0.5 part)
0.5 part of antioxidant; (antioxidant 1010 0.4 part, antioxidant 1076.1 parts)
Comparative example 1
The comparative example provides a PET fiber filled low-smoke halogen-free material, the formula components of which are basically the same as those in the example 1, and the preparation method is completely the same, and the difference is only that: no PET filament was added.
Comparative example 2
The comparative example provides a PET fiber filling low-smoke halogen-free material, the formula components of which are completely the same as those in example 1, and the preparation method is different from that in example 1: the production process of a conventional internal mixer is adopted.
Comparative example 3
The comparative example provides a halogen-free material, and the preparation method is completely the same, and the difference is only that:
20 parts of polar copolymer resin; (EVA)
60 parts of polyolefin resin; (mLLDPE)
50 parts of POE resin;
5 parts of a compatilizer; (Surlyn resin)
50 parts of inorganic flame retardant hydroxide; (aluminum hydroxide 20 parts, magnesium hydroxide 30 parts)
5 parts of PET fiber yarns;
1.5 parts of a surface modifier; (polysiloxanes)
3 parts of a lubricant; (polyethylene wax 1 part, silicone 2 parts)
1 part of an antioxidant; (antioxidant 1010)
TABLE 1 results of physical Property measurements of examples 1 to 3 and comparative examples 1 to 3 (GB/T32129-2015)
As can be seen from examples 1-3 and comparative example 1, the tensile strength, elongation at break and volume resistance at 20 ℃ of the material are only slightly higher than the standard requirements due to no addition of PET fiber yarns in the low-smoke halogen-free material, and the thermal shock resistance test is not qualified, mainly because the polar copolymer resin has low strength and is easy to excite under the action of an electric field due to the existence of the polar region of the resin, so that the volume resistance of the material is reduced; in order to improve the flame-retardant carbon formation property, a large amount of inorganic flame retardant must be added, and the inorganic flame retardant enters the resin amorphous region to reduce the creep of resin molecular chains and reduce the thermal shock resistance of the low-smoke halogen-free material, so that the material is easy to crack.
The above embodiments illustrate that the PET fiber filled low smoke and halogen-free material of the present invention, because the melting point of the PET resin is higher than the processing temperature of the low smoke and halogen-free material, the PET fiber can exist in the low smoke and halogen-free material in a fiber structure form, and because the rigidity of the PET benzene ring is large and the flame retardant carbon forming property is good, the mechanical properties of the low smoke and halogen-free material can be significantly improved. Meanwhile, under the action of the compatilizer, the PET fibers and the polar copolymer resin can react, so that a net structure is formed, and the cracking resistance of the low-smoke halogen-free material is improved; and the polarity of PET is greater than that of polyethylene, and the compatibility between the PET and inorganic flame retardant hydroxide is better, so that the oxygen index of the low-smoke halogen-free material is correspondingly improved.
As can be seen from examples 1-3 and comparative example 2, the productivity is greatly reduced by using the conventional internal mixer for melt-mixing granulation, and the production efficiency and the stability and consistency of the product are reduced due to the adoption of the manual operation mode.
As is clear from examples 1 to 3 and comparative example 3, since the proportion of the polar copolymer resin in the resin system is decreased, the amount of the inorganic flame retardant hydroxide which can be filled in the resin system is decreased; the excessive inorganic flame retardant hydroxide blocks the movement of resin molecular chains, so that the mechanical property of the low-smoke halogen-free material is reduced, and meanwhile, the inorganic flame retardant hydroxide cannot be effectively added into the low-smoke halogen-free material due to the reduced compatibility of the inorganic flame retardant hydroxide and a resin system, so that the oxygen index of the low-smoke halogen-free material is reduced, and more inorganic flame retardant hydroxide powder is separated out from the surfaces of particles of the low-smoke halogen-free material.
In summary, it can be known from the examples and comparative examples that the PET fiber filament filled low-smoke halogen-free material has good mechanical properties, electrical properties and flame retardant char formation properties, the processing temperature of the low-smoke halogen-free material is below 170 ℃, which is much lower than the melting point of the PET resin, the PET fiber filament always exists in the low-smoke halogen-free material in the form of fiber structure, and the mechanical properties of the low-smoke halogen-free material can be significantly improved due to the large rigidity of the PET benzene ring and the good flame retardant char formation properties. Meanwhile, under the action of the compatilizer, the PET fibers and the polar copolymer resin can react, so that a net structure is formed, and the cracking resistance of the low-smoke halogen-free material is improved; and PET has polarity higher than that of polyethylene and better compatibility with inorganic flame retardant hydroxide. The Swiss import BUSS production line can be used for greatly improving the yield and the production efficiency of materials, optimizing the uniformity and the stability of the materials and avoiding the hidden quality trouble caused by the fluctuation of the products.
According to the results in the table 1, the PET fiber yarn filled low-smoke halogen-free material has good mechanical property, electrical property and flame retardant carbon forming property, can meet the use requirement of the low-smoke halogen-free material, and has good economic benefit and social benefit; the preparation method adopts advanced Swiss BUSS line production, and has the advantages of stable process, large yield and high efficiency.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (5)
1. The raw material composition of the PET fiber filled low-smoke halogen-free material comprises the following components in parts by weight:
60-100 parts of polar copolymer resin, 10-50 parts of polyolefin resin, 0-40 parts of POE resin, 10-50 parts of compatilizer, 100-200 parts of inorganic flame retardant hydroxide, 10-40 parts of PET (polyethylene terephthalate) fiber, 0.5-2.5 parts of surface modifier, 1-5 parts of lubricant and 0.5-1.5 parts of antioxidant;
the polar copolymer resin is EVA, the polyolefin resin is polyethylene, and the compatilizer is one or two of maleic anhydride or glycidyl methacrylate grafted PE or POE;
the PET fiber yarns are obtained by blowing recycled PET films, PET textile fabrics and PET bottles;
the fiber length of the PET fiber filaments is less than or equal to 3mm.
2. The PET filament filled low smoke zero halogen material according to claim 1, wherein the inorganic flame retardant hydroxide is an aluminum hydroxide flame retardant and/or a magnesium hydroxide flame retardant.
3. The PET filament filled low smoke zero halogen material according to claim 1, wherein the surface modifier is polysiloxane and/or a silane coupling agent.
4. The PET filament filled low smoke and zero halogen material according to claim 1, wherein the lubricant is one or a combination of several of EVA wax, PE wax, silicone oil, stearic acid and stearate;
the antioxidant is selected from one or a combination of several of an antioxidant 1010, an antioxidant 1076, an antioxidant 168, an antioxidant 300 and an antioxidant DLTP.
5. A method for preparing the PET filament filled low smoke zero halogen material according to any one of claims 1 to 4, which comprises the following steps:
polar copolymer resin, polyolefin resin, POE resin, a compatilizer, half of inorganic flame retardant hydroxide, PET fiber filaments, a surface modifier, a lubricant and an antioxidant are mixed at a high speed, the mixture is discharged after being uniformly mixed, the mixture is fed into a first feeding port of a BUSS high-speed shearing machine, the other half of inorganic flame retardant hydroxide is fed into a second feeding port of the BUSS high-speed shearing machine, and the granules of the PET fiber filaments filled with the low-smoke halogen-free material are obtained after plasticization, single-screw granulation and drying.
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| CN102850659B (en) * | 2011-06-29 | 2016-02-03 | 合肥杰事杰新材料股份有限公司 | A kind of thermoplas tic resin composite for mine safety helmet |
| CN103013020A (en) * | 2012-12-25 | 2013-04-03 | 上海新上化高分子材料有限公司 | Natural silane cross-linking LSOH (Low Smoke Zero Halogen) flame-retardant polyolefin cable material and preparation method thereof |
| CN108047712A (en) * | 2017-12-14 | 2018-05-18 | 广东思汗新材料有限公司 | Fire-retardant Nylon 66 composite material and preparation method thereof |
| CN109627568B (en) * | 2018-12-29 | 2021-11-19 | 上海至正新材料有限公司 | Polyolefin cable sheath material and preparation method thereof |
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