CN108102331B - Termite-proof low-temperature-resistant flame-retardant PC/PE alloy material and preparation method thereof - Google Patents
Termite-proof low-temperature-resistant flame-retardant PC/PE alloy material and preparation method thereof Download PDFInfo
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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
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
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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
- C08K2201/002—Physical properties
- C08K2201/003—Additives being defined by their diameter
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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
- C08K2201/002—Physical properties
- C08K2201/004—Additives being defined by their length
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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
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
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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
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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
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
Abstract
The invention discloses a termite-proof low-temperature-resistant flame-retardant PC/PE alloy material and a preparation method thereof, wherein the termite-proof low-temperature-resistant flame-retardant PC/PE alloy material comprises the following raw materials in parts by weight: 50-80 parts of PC resin, 5-20 parts of PE resin, 3-8 parts of low-temperature synergist, 10-20 parts of phosphorus flame retardant, 0.2-2.0 parts of flame retardant synergist, 0.4-1.0 part of anti-dripping agent, 1-10 parts of termite-proof master batch and 0.4-1.0 part of antioxidant. In a PC/PE alloy system, the PE resin is distributed in the PC resin in a dispersed phase, the active groups of the low-temperature synergist and the PC resin improve the two-phase interface of the PC and the PE through a grafting reaction in the process of melt blending, the low-temperature toughening effect of the PE resin is fully exerted, and the phosphorus flame retardant and the flame-retardant synergist are cooperatively matched to meet the flame-retardant requirement of large-scale thin-walled workpieces. According to the invention, the termite-proof master batch is prepared firstly and then is used for synthesizing the PC/PE alloy material, so that the obtained termite-proof low-temperature-resistant flame-retardant PC/PE alloy material has a long-acting termite-proof effect while maintaining good low-temperature-resistant and flame-retardant characteristics, and is suitable for optical fiber and cable junction boxes.
Description
Technical Field
The invention belongs to the technical field of alloy materials, relates to a termite-proof low-temperature-resistant flame-retardant PC/PE alloy material and a preparation method thereof, and particularly relates to a termite-proof low-temperature-resistant flame-retardant PC/PE alloy material for junction boxes of optical fibers, cables and the like and a preparation method thereof.
Background
Polycarbonate (PC) material has the characteristics of excellent impact resistance, creep resistance, good dimensional stability, heat resistance, no toxicity and the like, and becomes an engineering plastic with the fastest application amount in recent years. One type of high density polyethylene copolymer (HDPE) which is a general-purpose plastic has outstanding impact resistance, heat resistance, low temperature resistance, and also environmental stress cracking resistance, electrical properties, and processability.
At present, the society enters an information age with high-speed development, and all industries can not leave communication networks. In order to ensure the rapid and efficient transmission of information, the optical fiber communication technology plays a crucial role. The use environment of the optical fiber junction box as an important component in a signal transmission system is limited to the harsh environment such as indoor environment, outdoor environment, buried environment or seabed environment, and the like, so that the junction box material is required to have excellent flame-retardant and low-temperature resistance and to have the function of preventing termite decay. Therefore, the development of the termite-proof low-temperature-resistant flame-retardant PC/PE alloy material for the optical fiber junction box is of great significance.
The invention patent with application number 201210303299.9 discloses a special plastic for an optical fiber junction box, which is mainly prepared from modified polypropylene such as a toughening low-temperature synergist, an anti-ultraviolet agent and the like. The material can be used for the optical fiber junction box but does not fully consider the requirements of low temperature resistance and flame retardance under outdoor conditions; the special function of termite resistance, especially when buried underground, is not involved.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a termite-proof low-temperature-resistant flame-retardant PC/PE alloy material for a junction box of optical fibers, cables and the like and a preparation method thereof. The modified PC/PE alloy prepared by blending Polycarbonate (PC) and high density polyethylene copolymer (HDPE) according to different proportions greatly expands the application environment and application field of the PC/PE alloy.
The high-density polyethylene resin selected in the invention as one component of the alloy material not only improves the defects of poor fluidity and low temperature resistance of PC resin, but also can better disperse the termite-proof effective component in the PC base material as a carrier, thereby fully playing the role of termite prevention. The termite-proof low-temperature-resistant flame-retardant PC/PE alloy material not only has high strength and low-temperature resistance, but also has the termite-proof characteristic and can greatly prolong the service life of the material. In addition, the preparation method of the termite-proof low-temperature-resistant flame-retardant PC/PE alloy material provided by the invention has the advantages of common equipment and simplicity in operation, and can meet the requirement of large-scale batch production.
The technical scheme adopted by the invention is as follows:
a termite-proof low-temperature-resistant flame-retardant PC/PE alloy material comprises the following raw materials in parts by weight:
further, the PC resin is bisphenol A polycarbonate, the molecular weight is 17000-30000, and the melt index is 10g/10min-20g/10 min.
Furthermore, the PE resin is high-density polyethylene HDPE copolymerized by a low-pressure method, and the molecular weight of the high-density polyethylene HDPE is 60000-100000.
Further, the low-temperature synergist is at least one of glycidyl methacrylate copolymer, ethylene-methyl acrylate copolymer or maleic anhydride grafted copolymer with epoxy functional groups.
Furthermore, the maleic anhydride graft copolymer is an EVA copolymer with a grafting rate of 1-3%.
Further, the phosphorus flame retardant is at least one of a halogen-free hypophosphite flame retardant or a phosphate flame retardant with the phosphorus content of 10-20%.
Further, the flame-retardant synergist is silicon carbide whisker with the diameter of 0.5-3.0um and the length of 100-500 um.
Further, the termite-proof master batch is a bifenthrin and methyl carbamate grafted high-density polyethylene polymer.
A preparation method of a termite-proof low-temperature-resistant flame-retardant PC/PE alloy material specifically comprises the following steps:
(1) preparing the termite-proof master batch: weighing a certain amount of bifenthrin, methyl carbamate, maleic anhydride and an initiator DCP, putting the bifenthrin, the methyl carbamate, the maleic anhydride and the initiator DCP into a closed stirring pot, stirring for 1-2 minutes, adding a certain weight fraction of PE resin, continuing stirring for 1-2 minutes, and finally performing extrusion reaction by a double-screw extruder 1 at an extrusion temperature of 160-220 ℃ and a rotating speed of 40-60r/min to obtain the termite-proof master batch.
The termite-proof master batch comprises the following raw materials in parts by weight: 0.2-0.5 part of initiator DCP, 1-3 parts of maleic anhydride, 4-6 parts of bifenthrin, 8-12 parts of methyl carbamate and 80-100 parts of high-density polyethylene HDPE.
The bifenthrin and the methyl carbamate can be effectively grafted to the HDPE resin under the action of the maleic anhydride and the initiator, and the prepared termite-proof master batch can be uniformly distributed in the PC/PE alloy material in the later processing and using process, and the volatilization loss of termite-proof active ingredients in the processing process can be reduced.
(2) Preparing a PC/PE alloy material: uniformly mixing PC resin, PE resin, a low-temperature synergist, a phosphorus flame retardant, a flame-retardant synergist, an anti-dripping agent and an antioxidant, adding the mixture from a feeding port in one area of a double-screw extruder 2, respectively arranging two plasticizing dispersing sections in the front area and the rear area of a vacuum port of the double-screw extruder 2, metering and adding termite-proof master batches from the plasticizing dispersing section in the ninth area behind the vacuum port, and extruding and granulating the mixture by the double-screw extruder 2 to obtain the termite-proof low-temperature flame-retardant PC/PE alloy material. Wherein the special process of adding the termite-proof master batch from the ninth area can reduce the process loss of the termite-proof active ingredients to the maximum extent.
The PE resin in the step (1) is used as a carrier, bifenthrin and methyl carbamate are grafted to the PE resin through maleic anhydride and an initiator, and the addition amount of the PE resin accounts for 80-100 parts by weight of the termite-proof master batch; the PE resin in the step (2) is a dispersion phase for preparing the PC/PE alloy material, the PE resin is distributed in the PC resin in the dispersion phase, and the addition amount of the PE resin accounts for 50-80 parts by weight of the PC/PE alloy material.
Further, the double-screw extruder 1 for preparing the termite-proof master batch comprises 10 temperature control areas, wherein the temperature distribution is 160-180 ℃ in the first area, 180-200 ℃ in the second area, 180-200 ℃ in the third area, 200-220 ℃ in the fourth area, 200-220 ℃ in the fifth area, 180-200 ℃ in the sixth area, 180-200 ℃ in the seventh area, 180-200 ℃ in the eighth area, 180-200 ℃ in the ninth area, 160-180 ℃ in the die head temperature and 40-60r/min in the screw rotating speed.
Further, the double screw extruder 2 for the termite-proof, low temperature resistant and flame retardant PC/PE alloy material comprises 13 temperature control areas, wherein the temperature distribution is that the first area is 200-210 ℃, the second area is 220-235 ℃, the third area is 220-235 ℃, the fourth area is 240-255 ℃, the fifth area is 240-255 ℃, the sixth area is 240-255 ℃, the seventh area is 230-245 ℃, the eighth area is 230-245 ℃, the ninth area is 230-245 ℃, the tenth area is 230-245 ℃, the eleventh area is 220-235 ℃, the twelfth area is 220-235 ℃, the die head temperature is 230-245 ℃, and the screw rotating speed is 400-charge 600 r/min.
Furthermore, the double-screw extruder 2 is provided with two plasticizing dispersion sections which are respectively arranged in the front area and the rear area of the vacuum port so as to protect the functional characteristics of the termite-proof master batch to the maximum extent.
The invention has the beneficial effects that:
in the PC/PE alloy system, the PE resin is distributed in the PC resin in a dispersed phase. The addition of the low-temperature synergist can improve the compatibility of two-phase interfaces so as to fully play the role of the PE resin, effectively improve the defects of poor low-temperature resistance and poor fluidity of PC materials, and meet the more severe outdoor environment.
The phosphorus flame retardant and the flame-retardant synergist are cooperated during combustion, and the phosphorus flame retardant component improves the carbon forming efficiency of the PC/PE alloy material, so that a carbon layer is quickly formed on the surface of the material. When a trace amount of whisker components are matched, the whiskers can play a role in reinforcing a carbon layer, so that the PC/PE alloy material is endowed with a higher flame-retardant grade, and the flame-retardant requirement of a large-scale thin-walled workpiece is met.
The self-made termite-proof master batch is bifenthrin and methyl carbamate grafted high-density polyethylene polymer, and the termite-proof master batch can ensure that the effective ingredients of the termite-proof master batch are uniformly distributed in the PC/PE alloy material, and can reduce the volatilization loss of the effective ingredients in the processing process. Compared with the conventional PC/PE alloy material, the termite-proof master batch added in the invention solves the problem of termite corrosion when the material is buried underground, and prolongs the service life of the material.
The low-temperature synergist adopts the synergistic effect of an epoxy functional group graft and a maleic anhydride graft. The active groups of the two components improve the two-phase interface of the PC and the PE through a grafting reaction in the process of melt blending, and the low-temperature toughening effect of the PE is fully exerted.
The termite-proof low-temperature-resistant flame-retardant PC/PE alloy material is particularly suitable for the field of communication, and can completely meet the use requirement of an optical fiber junction box buried outdoors deeply.
Detailed Description
The termite resistant, low temperature resistant, flame retardant PC/PE alloy material is further detailed by the following examples. But the embodiments of the present invention are not limited thereto. Several variations and modifications are possible to those skilled in the art within the scope of the inventive concept. Such changes and modifications are intended to be included within the scope of the present invention.
The raw materials selected in the following comparative examples and examples include: the PC resin is bisphenol A PC polycarbonate with the molecular weight of 17000-30000, specifically 201-10 of Korean LG or S-1000 of Mitsubishi; the PE resin is high-density polyethylene HDPE copolymerized by a low-pressure method, and concretely selects FB3450 in northern Europe chemical industry; the low-temperature synergist is prepared by grafting ethylene-vinyl acetate copolymer (GMA) with 4-8% of epoxy functional Group (GMA) or maleic anhydride grafted EVA with grafting rate of 1-3%, specifically adopting AX8900 of Acoma France and maleic anhydride grafted EVA1803 of Exxon Mobil company of America; the phosphorus flame retardant is halogen-free aluminum hypophosphite or phosphate ester flame retardant with the phosphorus content of 10-20%, the halogen-free aluminum hypophosphite is FR-ADP01 product of Guangzhou tiger source new material, and the phosphate ester flame retardant is FP600 of Aidic; the flame-retardant synergist is an alpha-type silicon carbide whisker with the diameter of 0.2-3.0um and the length of 100-500um, and concretely selects Sinet HP-90 of Changshaitetai new material company; the anti-dripping agent is polytetrafluoroethylene coated by styrene-acrylonitrile, the molecular weight of the polytetrafluoroethylene is 400-550 ten thousand, the weight percentage is 40-60%, and the B449 of GE is specifically selected; the termite-proof functional agent is at least one of bifenthrin, carbamates and novel organophosphorus medicaments, and particularly selects bifenthrin and methyl carbamate compound auxiliary agent; maleic anhydride is synthesized by n-butane oxidation method, and has purity of above 99.5, specifically Mitsubishi chemical product; the peroxide initiator DCP is 14S-FL product of Acksu company; the antioxidant is Irganox168 and Irganox1076 from Pasteur.
Comparative examples 1 to 2
Weighing a certain amount of PC resin, high-density polyethylene HDPE, maleic anhydride grafted EVA, aluminum hypophosphite, an anti-dripping agent, bifenthrin, methyl carbamate and an antioxidant, adding into a high-speed mixer, stirring for 3min, and then adding into a double-screw extruder from a main feeding port for melting and granulating. The temperatures of the respective sections from the feed section to the head in the twin-screw extruder were 200 ℃, 220 ℃,230 ℃, 245 ℃, 235 ℃,230 ℃ and 230 ℃, respectively, and the die temperature was 230 ℃. The prepared termite-proof low-temperature-resistant flame-retardant PC/PE alloy granules are placed in a vacuum drying oven at the temperature of 80 ℃ for 3 hours and then are prepared into test sample strips by an injection molding machine.
The weight fractions of the starting materials described in comparative examples 1-2 are given in Table 1, and the test results after preparation of the bars are given in Table 2.
Example 1
The preparation method of the termite-proof master batch specifically comprises the following steps:
firstly, 0.2 part of initiator DCP, 2 parts of maleic anhydride, 5 parts of bifenthrin and 10 parts of methyl carbamate are respectively added into a closed stirring pot, premixed for 1 minute at a low speed, then added with 82.4 parts of high-density polyethylene HDPE, stirred and mixed for 2 minutes at a high speed, and added into a double-screw extruder for melt reaction and granulation. The temperatures of the sections of the double-screw extruder are respectively 160 ℃, 180 ℃, 200 ℃, 220 ℃, 200 ℃, 180 ℃, the die head temperature is 160 ℃ and the screw rotating speed is 50 r/min. The prepared termite-proof master batch is packaged by an aluminum foil packaging bag and is sealed in vacuum in time for standby.
Examples 2 to 8
Weighing a certain amount of PC resin, High Density Polyethylene (HDPE), a low-temperature synergist, a phosphorus flame retardant, a flame-retardant synergist, an anti-dripping agent, a termite-proof master batch and an antioxidant, adding into a high-speed mixer, and stirring for 3min to obtain a mixed material; and (3) adding the termite-proof master batches from the ninth area by using a weightless scale, and performing melt granulation by using a double-screw extruder. The temperatures of the respective sections from the feed section to the head in the twin-screw extruder were 200 ℃, 220 ℃,230 ℃, 245 ℃, 235 ℃,230 ℃ and 230 ℃, respectively, and the die temperature was 230 ℃. The prepared termite-proof low-temperature-resistant flame-retardant PC/PE alloy granules are placed in a vacuum drying oven at the temperature of 80 ℃ for 3 hours and then are prepared into test sample strips by an injection molding machine.
The weight fractions of the starting materials described in examples 2-8 are given in Table 1, and the test results after preparation of the bars are given in Table 2.
TABLE 1
TABLE 2
In conjunction with table 1, it can be found from the comparative example 1 and comparative example 2 test data of table 2 that: the PC/PE alloy material has low compatibility and poor impact strength in a low-temperature environment without the action of a low-temperature synergist or a single low-temperature synergist. Comparative example 2, after adding aluminum hypophosphite flame retardant and a certain amount of termite-proof auxiliary agent, the flame retardant grade of the alloy material is improved from V-2 grade to V-1 grade; termite resistance ratings also increased from the lowest rating of 4 to 3. Through the examples 2-8, it can be found that the alloy material shows higher impact strength under the action of two different low-temperature synergists under the low-temperature condition. When the aluminum hypophosphite flame retardant and the silicon carbide whiskers in the PC/PE alloy material are used simultaneously, more excellent flame retardant performance can be shown, and the flame retardant grade is also improved from V-1 grade to V-0 grade. In addition, compared with the comparative example 2, the termite-proof master batch used in the examples can be uniformly dispersed in the alloy material while protecting the efficacy of the termite-proof agent, so that the termite-proof grade of the material is further improved.
The above description is not meant to be limiting, it being noted that: it will be apparent to those skilled in the art that various changes, modifications, additions and substitutions can be made without departing from the true scope of the invention, and these improvements and modifications should also be construed as within the scope of the invention.
Claims (8)
1. The termite-proof low-temperature-resistant flame-retardant PC/PE alloy material is characterized by comprising the following raw materials in parts by weight:
the low-temperature synergist is at least one of glycidyl methacrylate copolymer, ethylene-methyl acrylate copolymer or maleic anhydride graft copolymer with epoxy functional groups;
the termite-proof master batch is a bifenthrin and methyl carbamate grafted high-density polyethylene polymer;
the preparation method of the termite-proof master batch comprises the following steps: weighing a certain amount of bifenthrin, methyl carbamate, maleic anhydride and an initiator DCP, putting into a closed stirring pot, uniformly stirring, adding PE resin, continuously uniformly stirring, and finally extruding by a double-screw extruder 1 to obtain the termite-proof master batch.
2. The termite-proof low-temperature-resistant flame-retardant PC/PE alloy material as claimed in claim 1, wherein the PC resin is bisphenol A polycarbonate, the molecular weight is 17000-30000, and the melt index is 10g/10min-20g/10 min.
3. The termite-proof low-temperature-resistant flame-retardant PC/PE alloy material as claimed in claim 1, wherein the PE resin is high-density polyethylene HDPE copolymerized by a low-pressure method, and the molecular weight of the high-density polyethylene is 60000-100000.
4. The termite-proof low-temperature-resistant flame-retardant PC/PE alloy material as claimed in claim 3, wherein the maleic anhydride graft copolymer is EVA copolymer with a grafting rate of 1% -3%.
5. The termite-proof low-temperature-resistant flame-retardant PC/PE alloy material as claimed in claim 1, wherein the phosphorus flame retardant is at least one of a halogen-free hypophosphite flame retardant or a phosphate flame retardant with a phosphorus content of 10-20%.
6. The termite-proof low temperature resistant flame retardant PC/PE alloy material as claimed in claim 1, wherein the flame retardant synergist is silicon carbide whisker with a diameter of 0.5-3.0um and a length of 100-500 um.
7. The preparation method of the termite-proof, low-temperature-resistant and flame-retardant PC/PE alloy material as claimed in claim 1, which is characterized by comprising the following steps:
(1) preparing the termite-proof master batch: weighing a certain amount of bifenthrin, methyl carbamate, maleic anhydride and an initiator DCP, putting into a closed stirring pot, uniformly stirring, adding PE resin, continuously uniformly stirring, and finally extruding by a double-screw extruder 1 to obtain termite-proof master batches;
(2) preparing a PC/PE alloy material: uniformly mixing PC resin, PE resin, a low-temperature synergist, a phosphorus flame retardant, a flame-retardant synergist, an anti-dripping agent and an antioxidant, adding the mixture from a feeding port in one area of a double-screw extruder 2, respectively arranging two plasticizing dispersion sections in the front area and the rear area of a vacuum port of the double-screw extruder 2, metering and adding termite-proof master batches from the plasticizing dispersion sections behind the vacuum port, and extruding and granulating the mixture by the double-screw extruder 2.
8. The preparation method of the termite-proof low-temperature-resistant flame-retardant PC/PE alloy material as claimed in claim 7, wherein the PE resin in the step (1) is used as a carrier, bifenthrin and methyl carbamate are grafted to the PE resin through maleic anhydride and an initiator, and the addition amount of the PE resin accounts for 80-100 parts by weight of the termite-proof master batch; the PE resin in the step (2) is a dispersion phase for preparing the PC/PE alloy material, the PE resin is distributed in the PC resin in the dispersion phase, and the addition amount of the PE resin accounts for 50-80 parts by weight of the PC/PE alloy material.
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| WO2007091494A1 (en) * | 2006-02-06 | 2007-08-16 | Nippon Soda Co., Ltd. | Pesticide-containing resin compositions controlled in dissolution, process for production thereof, and pesticide preparations |
| CN101798417B (en) * | 2010-03-26 | 2011-12-07 | 华南理工大学 | Anti-termite and coloring functional master batch for plastic and preparation method thereof |
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