CN107936489A - A kind of effective halogen-free flameproof PET composite material of heat shrinking sleeve and preparation method - Google Patents
A kind of effective halogen-free flameproof PET composite material of heat shrinking sleeve and preparation method Download PDFInfo
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- CN107936489A CN107936489A CN201711169776.6A CN201711169776A CN107936489A CN 107936489 A CN107936489 A CN 107936489A CN 201711169776 A CN201711169776 A CN 201711169776A CN 107936489 A CN107936489 A CN 107936489A
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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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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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
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
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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
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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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
- C08L2201/22—Halogen free composition
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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
- C08L2203/00—Applications
- C08L2203/18—Applications used for pipes
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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
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
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- 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
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Abstract
The invention discloses a kind of effective halogen-free flameproof PET composite material of heat shrinking sleeve and preparation method, the halogen-free flameproof PET composite material to include the formula composition of following percentage by weight:PET resin 75 85%;Organic fire-retardant 10 20%;Nano imvite 1 3%;Glass fibre 1 4%;Nano silicon dioxide 1.7 3.5%;Heat stabilizer 0.1 0.4%;Antioxidant 0.1 0.4%;Compatilizer 1 3%;Dispersant 0.1 0.5%;Anti-dripping agent 0 0.5%.Halogen-free flameproof PET composite material prepared by the present invention has excellent anti-flammability and toughness, and boiling water shrinkage reaches 45%.
Description
Technical field
The present invention relates to technical field of polymer materials, is specially a kind of effective halogen-free flameproof PET composite woods of heat shrinking sleeve
Material and preparation method.
Background technology
At present, realize that the fire-retardant fire retardant of PET resin mainly there are two classes:Halogen and non-halogen class.Halogen flame master
If chlorine, bromine, fluorine, iodine play main function, but the hydrogen chloride of halogen flame generation, hydrogen bromide etc. in processing and use
During can destroy human central nervous and produce the poisonous and harmful substances such as the carcinogenic substance such as dioxin, while produce in burning big
The poisonous black dense smoke of amount, erosion damage equipment and Environmental security health, extend with hindering fire-fighting and rescue work;Halogen fire retardant is main
It is made of inorganic metal compound, phosphorus system, nitrogen system, phosphorus nitrogen system, silicon systems, which does not contain evil adding in human health
Add agent, without some heavy metals, do not produce toxic gas and cause environmental pollution, when burning only produces a little light white cigarette, to the mankind
Health and Environmental security influence smaller.
The halogen-free flame retardants for PET resin is mainly the following currently on the market:Hypo-aluminum orthophosphate, diethyl hypophosphorous acid
Aluminium, phosphonitrile fire retardant.Hypo-aluminum orthophosphate category inorganic type filled-type fire retardant, temperature tolerance is poor, and additive amount is big, to the performance shadow of material
Ring big;Diethyl hypo-aluminum orthophosphate additive amount is larger, has a great influence to material property;Although phosphonitrile fire retardant additive amount is little,
Flame retardant effect is poor, it is impossible to fully meets the flame-retardancy requirements compared with thin product;
The material that traditional thermal contraction casing tube is selected has PVC and PET, and PVC is although fire-retardant, but because it changes the feature of environmental protection, using being limited
System, the effective materials most of PET heat shrinking sleeves is non-flame-retardant material, if fire proofing is made, the boiling water shrinkage of product also can be by
To influence, it can not meet the requirement of thermal contraction casing tube.
The content of the invention
It is an object of the invention to provide a kind of effective halogen-free flameproof PET composite material of heat shrinking sleeve and preparation method, with
Solve the problems, such as proposed in the above background technology.
To achieve the above object, the present invention provides following technical solution:A kind of effective halogen-free flameproof PET of heat shrinking sleeve is compound
Material, the halogen-free flameproof PET composite material include the formula composition of following percentage by weight:PET resin 75-85%;Organic resistance
Fire agent 10-20%;Nano imvite 1-3%;Glass fibre 1-4%;Nano silicon dioxide 1.7-3.5%;Heat stabilizer 0.1-0.4%;
Antioxidant 0.1-0.4%;Compatilizer 1-3%;Dispersant 0.1-0.5%;Anti-dripping agent 0-0.5%.
Preferably, the organic fire-retardant is phosphorus flame retardant, its phosphorus content is 10.8%.
Preferably, the heat stabilizer uses 1010.
Preferably, the antioxidant is phosphite ester system antioxidant, using in 168, S9228 or Revonox 608
One or more, wherein it is preferred that Revonox 608.
Preferably, the compatilizer is ethylene-methyl acrylate-glyceryl methacrylate.
Preferably, the dispersant is the one or more in PETS, montanin wax, microwax, wherein it is preferred that montanin wax.
Preferably, the anti-dripping agent is surface coated polytetrafluoroethylene (PTFE).
Preferably, its preparation method comprises the following steps:
A, PET resin is fully dried, ensures that moisture is less than 100ppm;
B, organic fire-retardant is fully dried, ensures that moisture is less than 100ppm;
C, by PET resin;Organic fire-retardant;Nano imvite;Glass fibre;Nano silicon dioxide;Heat stabilizer;Antioxidant;
Compatilizer;Dispersant;Anti-dripping agent is sufficiently mixed, will wherein organic fire-retardant after weightlessness claims metering by double screw extruder the
Add at five sections of side feedings or added from main feeding, wherein it is preferred that being added from side feeding, PET resin and other dispensings claim through weightlessness
Added by main feeding after metering, according to the expressing technique of setting, be then granulated through double screw extruder blending extrusion, obtained required
PET composite material.
Preferably, the expressing technique in the step C is specific as follows:One 160 ± 5 DEG C of area's temperature, two area's temperature 230 ± 5
DEG C, three 250 ± 5 DEG C of area's temperature, four 250 ± 5 DEG C of area's temperature, five 250 ± 5 DEG C of area's temperature, six 250 ± 5 DEG C of area's temperature, seven area's temperature
240 ± 5 DEG C of degree, eight 230 ± 5 DEG C of area's temperature, nine 230 ± 5 DEG C of area's temperature, 250 ± 5 DEG C of die head temperature, screw speed 360-
400r/min。
Compared with prior art, the beneficial effects of the invention are as follows:Halogen-free flameproof PET composite material prepared by the present invention has
Excellent anti-flammability and toughness, wherein, the nano imvite of addition has excellent high temperature resistant, fire resistance, further improves
The fire resistance of composite material;The glass fibre of addition can further improve the toughness and tensile property of composite material;Through
Overtesting obtains, and composite material boiling water shrinkage produced by the present invention reaches 45%.
Embodiment
The technical solution in the embodiment of the present invention is clearly and completely described below, it is clear that described embodiment
Only part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this area
Art personnel all other embodiments obtained without making creative work, belong to the model that the present invention protects
Enclose.
The present invention provides following technical solution:A kind of effective halogen-free flameproof PET composite material of heat shrinking sleeve, the Halogen resistance
Combustion PET composite material includes the formula composition of following percentage by weight:PET resin 75-85%;Organic fire-retardant 10-20%;Nanometer
Montmorillonite 1-3%;Glass fibre 1-4%;Nano silicon dioxide 1.7-3.5%;Heat stabilizer 0.1-0.4%;Antioxidant 0.1-0.4%;
Compatilizer 1-3%;Dispersant 0.1-0.5%;Anti-dripping agent 0-0.5%;Wherein, PET resin contains Third monomer, and inherent viscosity is
0.7dl/g;The boiling water shrinkage of PET resin is 45%;Organic fire-retardant is phosphorus flame retardant, its phosphorus content is 10.8%, glass
Change about 105 DEG C of transition temperature;Heat stabilizer uses 1010.
Embodiment one:
Halogen-free flameproof PET composite material includes the formula composition of following percentage by weight:PET resin 75%;Organic fire-retardant
19.7%;Nano imvite 1%;Glass fibre 1%;Nano silicon dioxide 2%;Heat stabilizer 0.1%;Antioxidant 0.1%;Compatilizer
1%;Dispersant 0.1%;Anti-dripping agent 0%.
In the present embodiment, antioxidant is phosphite ester system antioxidant, using 168, S9228 mixtures.
In the present embodiment, compatilizer is ethylene-methyl acrylate-glyceryl methacrylate.
In the present embodiment, dispersant PETS.
In the present embodiment, anti-dripping agent is surface coated polytetrafluoroethylene (PTFE).
The preparation method of the present embodiment comprises the following steps:
A, PET resin is fully dried, ensures that moisture is less than 100ppm;
B, organic fire-retardant is fully dried, ensures that moisture is less than 100ppm;
C, by PET resin;Organic fire-retardant;Nano imvite;Glass fibre;Nano silicon dioxide;Heat stabilizer;Antioxidant;
Compatilizer;Dispersant;Anti-dripping agent is sufficiently mixed, will wherein organic fire-retardant after weightlessness claims metering by double screw extruder the
Add at five sections of side feedings or added from main feeding, wherein it is preferred that being added from side feeding, PET resin and other dispensings claim through weightlessness
Added by main feeding after metering, according to the expressing technique of setting, be then granulated through double screw extruder blending extrusion, obtained required
PET composite material.
In the present embodiment, the expressing technique in step C is specific as follows:One 155 DEG C of area's temperature, two 225 DEG C of area's temperature, 3rd area
245 DEG C of temperature, four 245 DEG C of area's temperature, five 245 DEG C of area's temperature, six 245 DEG C of area's temperature, seven 235 DEG C of area's temperature, eight area's temperature 225
DEG C, nine 225 DEG C of area's temperature, 245 DEG C of die head temperature, screw speed 360r/min.
Embodiment two:
Halogen-free flameproof PET composite material includes the formula composition of following percentage by weight:PET resin 83%;Organic fire-retardant 10%;
Nano imvite 3%;Glass fibre 1%;Nano silicon dioxide 1.7%;Heat stabilizer 0.1%;Antioxidant 0.1%;Compatilizer 1%;Point
Powder 0.1%;Anti-dripping agent 0%.
In the present embodiment, antioxidant is phosphite ester system antioxidant, using Revonox 608.
In the present embodiment, compatilizer is ethylene-methyl acrylate-glyceryl methacrylate.
In the present embodiment, dispersant is microwax.
In the present embodiment, anti-dripping agent is surface coated polytetrafluoroethylene (PTFE).
The preparation method of the present embodiment comprises the following steps:
A, PET resin is fully dried, ensures that moisture is less than 100ppm;
B, organic fire-retardant is fully dried, ensures that moisture is less than 100ppm;
C, by PET resin;Organic fire-retardant;Nano imvite;Glass fibre;Nano silicon dioxide;Heat stabilizer;Antioxidant;
Compatilizer;Dispersant;Anti-dripping agent is sufficiently mixed, will wherein organic fire-retardant after weightlessness claims metering by double screw extruder the
Add at five sections of side feedings or added from main feeding, wherein it is preferred that being added from side feeding, PET resin and other dispensings claim through weightlessness
Added by main feeding after metering, according to the expressing technique of setting, be then granulated through double screw extruder blending extrusion, obtained required
PET composite material.
In the present embodiment, the expressing technique in step C is specific as follows:One 165 DEG C of area's temperature, two 235 DEG C of area's temperature, 3rd area
255 DEG C of temperature, four 255 DEG C of area's temperature, five 255 DEG C of area's temperature, six 255 DEG C of area's temperature, seven 245 DEG C of area's temperature, eight area's temperature 235
DEG C, nine 235 DEG C of area's temperature, 255 DEG C of die head temperature, screw speed 400r/min.
Embodiment three:
Halogen-free flameproof PET composite material includes the formula composition of following percentage by weight:PET resin 75;Organic fire-retardant 20%;
Nano imvite 1%;Glass fibre 1%;Nano silicon dioxide 1.7%;Heat stabilizer 0.1%;Antioxidant 0.1%;Compatilizer 1%;Point
Powder 0.1%;Anti-dripping agent 0%.
In the present embodiment, antioxidant is phosphite ester system antioxidant, using 168, Revonox, 608 mixtures.
In the present embodiment, compatilizer is ethylene-methyl acrylate-glyceryl methacrylate.
In the present embodiment, dispersant is montanin wax, crystallite wax mixture.
In the present embodiment, anti-dripping agent is surface coated polytetrafluoroethylene (PTFE).
The preparation method of the present embodiment comprises the following steps:
A, PET resin is fully dried, ensures that moisture is less than 100ppm;
B, organic fire-retardant is fully dried, ensures that moisture is less than 100ppm;
C, by PET resin;Organic fire-retardant;Nano imvite;Glass fibre;Nano silicon dioxide;Heat stabilizer;Antioxidant;
Compatilizer;Dispersant;Anti-dripping agent is sufficiently mixed, will wherein organic fire-retardant after weightlessness claims metering by double screw extruder the
Add at five sections of side feedings or added from main feeding, wherein it is preferred that being added from side feeding, PET resin and other dispensings claim through weightlessness
Added by main feeding after metering, according to the expressing technique of setting, be then granulated through double screw extruder blending extrusion, obtained required
PET composite material.
In the present embodiment, the expressing technique in step C is specific as follows:One 158 DEG C of area's temperature, two 228 DEG C of area's temperature, 3rd area
247 DEG C of temperature, four 252 DEG C of area's temperature, five 253 DEG C of area's temperature, six 252 DEG C of area's temperature, seven 238 DEG C of area's temperature, eight area's temperature 229
DEG C, nine 234 DEG C of area's temperature, 254 DEG C of die head temperature, screw speed 370r/min.
Example IV:
Halogen-free flameproof PET composite material includes the formula composition of following percentage by weight:PET resin 80%;Organic fire-retardant 10%;
Nano imvite 1%;Glass fibre 2%;Nano silicon dioxide 2.8%;Heat stabilizer 0.1%;Antioxidant 0.1%;Compatilizer 3%;Point
Powder 0.5%;Anti-dripping agent 0.5%.
In the present embodiment, antioxidant is phosphite ester system antioxidant, using Revonox 608.
In the present embodiment, compatilizer is ethylene-methyl acrylate-glyceryl methacrylate.
In the present embodiment, dispersant is montanin wax.
In the present embodiment, anti-dripping agent is surface coated polytetrafluoroethylene (PTFE).
The preparation method of the present embodiment comprises the following steps:
A, PET resin is fully dried, ensures that moisture is less than 100ppm;
B, organic fire-retardant is fully dried, ensures that moisture is less than 100ppm;
C, by PET resin;Organic fire-retardant;Nano imvite;Glass fibre;Nano silicon dioxide;Heat stabilizer;Antioxidant;
Compatilizer;Dispersant;Anti-dripping agent is sufficiently mixed, will wherein organic fire-retardant after weightlessness claims metering by double screw extruder the
Add at five sections of side feedings or added from main feeding, wherein it is preferred that being added from side feeding, PET resin and other dispensings claim through weightlessness
Added by main feeding after metering, according to the expressing technique of setting, be then granulated through double screw extruder blending extrusion, obtained required
PET composite material.
In the present embodiment, the expressing technique in step C is specific as follows:One 160 DEG C of area's temperature, two 230 DEG C of area's temperature, 3rd area
250 DEG C of temperature, four 250 DEG C of area's temperature, five 250 DEG C of area's temperature, six 250 DEG C of area's temperature, seven 240 DEG C of area's temperature, eight area's temperature 230
DEG C, nine 230 DEG C of area's temperature, 250 DEG C of die head temperature, screw speed 380r/min.
Experimental example:Tested using composite material made from various embodiments of the present invention, obtain data such as following table:
Halogen-free flameproof PET composite material prepared by the present invention has excellent anti-flammability and toughness, wherein, the nanometer of addition, which is covered, to be taken off
Soil has excellent high temperature resistant, fire resistance, further increases the fire resistance of composite material;The glass fibre of addition can
Further improve the toughness and tensile property of composite material;Obtained through overtesting, composite material boiling shrinkage produced by the present invention
Rate reaches 45%.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
Understanding without departing from the principles and spirit of the present invention can carry out these embodiments a variety of changes, modification, replace
And modification, the scope of the present invention is defined by the appended.
Claims (9)
- A kind of 1. effective halogen-free flameproof PET composite material of heat shrinking sleeve, it is characterised in that:The halogen-free flameproof PET composite material Include the formula composition of following percentage by weight:PET resin 75-85%;Organic fire-retardant 10-20%;Nano imvite 1-3%;Glass Glass fiber 1-4%;Nano silicon dioxide 1.7-3.5%;Heat stabilizer 0.1-0.4%;Antioxidant 0.1-0.4%;Compatilizer 1-3%;Point Powder 0.1-0.5%;Anti-dripping agent 0-0.5%.
- A kind of 2. effective halogen-free flameproof PET composite material of heat shrinking sleeve according to claim 1, it is characterised in that:It is described Organic fire-retardant is phosphorus flame retardant, its phosphorus content is 10.8%.
- A kind of 3. effective halogen-free flameproof PET composite material of heat shrinking sleeve according to claim 1, it is characterised in that:It is described Heat stabilizer uses 1010.
- A kind of 4. effective halogen-free flameproof PET composite material of heat shrinking sleeve according to claim 1, it is characterised in that:It is described Antioxidant is phosphite ester system antioxidant, using the one or more in 168, S9228 or Revonox 608, wherein it is preferred that Revonox 608。
- A kind of 5. effective halogen-free flameproof PET composite material of heat shrinking sleeve according to claim 1, it is characterised in that:It is described Compatilizer is ethylene-methyl acrylate-glyceryl methacrylate.
- A kind of 6. effective halogen-free flameproof PET composite material of heat shrinking sleeve according to claim 1, it is characterised in that:It is described Dispersant is PETS, the one or more in montanin wax, microwax, wherein it is preferred that montanin wax.
- A kind of 7. effective halogen-free flameproof PET composite material of heat shrinking sleeve according to claim 1, it is characterised in that:It is described Anti-dripping agent is surface coated polytetrafluoroethylene (PTFE).
- 8. realize a kind of preparation method of the effective halogen-free flameproof PET composite material of heat shrinking sleeve described in claim 1, its feature It is:Its preparation method comprises the following steps:A, PET resin is fully dried, ensures that moisture is less than 100ppm;B, organic fire-retardant is fully dried, ensures that moisture is less than 100ppm;C, by PET resin;Organic fire-retardant;Nano imvite;Glass fibre;Nano silicon dioxide;Heat stabilizer;Antioxidant; Compatilizer;Dispersant;Anti-dripping agent is sufficiently mixed, will wherein organic fire-retardant after weightlessness claims metering by double screw extruder the Add at five sections of side feedings or added from main feeding, wherein it is preferred that being added from side feeding, PET resin and other dispensings claim through weightlessness Added by main feeding after metering, according to the expressing technique of setting, be then granulated through double screw extruder blending extrusion, obtained required PET composite material.
- 9. a kind of preparation method of the effective halogen-free flameproof PET composite material of heat shrinking sleeve described in claim 8, its feature exist In:Expressing technique in the step C is specific as follows:One 160 ± 5 DEG C of area's temperature, two 230 ± 5 DEG C of area's temperature, three area's temperature 250 ± 5 DEG C, four 250 ± 5 DEG C of area's temperature, five 250 ± 5 DEG C of area's temperature, six 250 ± 5 DEG C of area's temperature, seven 240 ± 5 DEG C of area's temperature, Eight 230 ± 5 DEG C of area's temperature, nine 230 ± 5 DEG C of area's temperature, 250 ± 5 DEG C of die head temperature, screw speed 360-400r/min.
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CN201711169776.6A CN107936489A (en) | 2017-11-22 | 2017-11-22 | A kind of effective halogen-free flameproof PET composite material of heat shrinking sleeve and preparation method |
PCT/CN2018/098270 WO2019100747A1 (en) | 2017-11-22 | 2018-08-02 | Halogen-free flame retardant pet composite material for heat-shrinkable sleeve and preparation method therefor |
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CN112391037A (en) * | 2020-11-06 | 2021-02-23 | 顺鹏塑胶(苏州)有限公司 | Preparation method of PET (polyethylene terephthalate) sleeve material for easily-shrinkable batteries and capacitors |
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WO2019100747A1 (en) * | 2017-11-22 | 2019-05-31 | 南通市东方塑胶有限公司 | Halogen-free flame retardant pet composite material for heat-shrinkable sleeve and preparation method therefor |
CN112391037A (en) * | 2020-11-06 | 2021-02-23 | 顺鹏塑胶(苏州)有限公司 | Preparation method of PET (polyethylene terephthalate) sleeve material for easily-shrinkable batteries and capacitors |
CN115895206A (en) * | 2022-11-21 | 2023-04-04 | 盘锦海兴科技股份有限公司 | Flame-retardant PET material and preparation method thereof |
CN115895206B (en) * | 2022-11-21 | 2024-06-18 | 盘锦海兴科技股份有限公司 | Flame-retardant PET material and preparation method thereof |
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