CN109957169A - A kind of flame-retardant organosilane cross-linked poly-ethylene Insulation Material and its preparation method and application - Google Patents
A kind of flame-retardant organosilane cross-linked poly-ethylene Insulation Material and its preparation method and application Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/25—Component parts, details or accessories; Auxiliary operations
- B29C48/92—Measuring, controlling or regulating
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- 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
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
- C08L23/0807—Copolymers of ethene with unsaturated hydrocarbons only containing more than three carbon atoms
- C08L23/0815—Copolymers of ethene with aliphatic 1-olefins
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/44—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins
- H01B3/441—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins from alkenes
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- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29C2948/00—Indexing scheme relating to extrusion moulding
- B29C2948/92—Measuring, controlling or regulating
- B29C2948/92504—Controlled parameter
- B29C2948/92704—Temperature
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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
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K2003/026—Phosphorus
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- C08L2203/00—Applications
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- C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
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- 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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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2312/00—Crosslinking
- C08L2312/08—Crosslinking by silane
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Abstract
The invention belongs to CABLE MATERIALS technical fields, and in particular to a kind of flame-retardant organosilane cross-linked poly-ethylene Insulation Material and its preparation method and application, raw material include A material and B material, and the weight ratio of A material and B material is (75-85): (15-25)；Wherein, A material includes following parts by weight of component: 65-80 parts of LLDPE resin a；10-25 parts of LLDPE resin b；4-6 parts of processing aid；1.5-2.7 parts of silane；0.01-0.1 parts of initiator；0.1-0.3 parts of antioxidant；B material includes following parts by weight of component: 45-65 parts of LLDPE resin a；1.5-2.6 parts of catalyst；2-6 parts of antioxidant；10-20 parts of carbon black；20-30 parts of red phosphorus masterbatch.Flame-retardant organosilane cross-linked poly-ethylene Insulation Material of the invention is added in catalyst masterbatch using the good flame-retardance energy of red phosphorus masterbatch, so that resulting organosilane crosslinked polyethylene insulation material passes through the horizontal firing performance in UL44 standard well.
Description
Technical field
The invention belongs to CABLE MATERIALS technical fields, and in particular to a kind of flame-retardant organosilane cross-linked poly-ethylene Insulation Material and its preparation
Method and purposes.
Background technique
Mating industry of the wires and cables industry as the power industry of one of pillars of the national economy industry, in national economy
With extremely important effect and status.Poly-ethylene cable material is because of its light weight, mechanical property is good, it is very good also to have simultaneously
The outstanding properties such as resistance to low temperature, good environmental stress cracking resistance, good processability, outstanding electrical insulation capability
Feature has a very wide range of applications in wire and cable field.Poly-ethylene cable material is indispensable important in CABLE MATERIALS
One of component part.
With the increase of wire and cable export enterprise order, due to the difference of geographical environment, identical is using field pair
Also different in the requirement of cable, the export order of American Standard generally requires the horizontal firing that can be crossed in UL44.The present invention utilizes
The good flame-retardance of red phosphorus masterbatch can make originally the organosilane crosslinked polyethylene insulation material of not flame retardant property pass through the water in UL44
Flat burning, has expanded the use scope of organosilane crosslinked polyethylene insulation material significantly, has improved organosilane crosslinked polyethylene insulation material
Flame retardant property can also meet external standard.Therefore, it is necessary to targetedly further be changed to insulating material of polyethylene
Into.
Summary of the invention
In view of the foregoing deficiencies of prior art, the purpose of the present invention is to provide a kind of flame-retardant organosilane cross-linked poly-ethylenes
Insulation Material and its preparation method and application.The flame-retardant organosilane cross-linked poly-ethylene Insulation Material that the present invention obtains is marked by UL44 well
Horizontal firing performance in standard, and have extruded velocity fast, squeeze out the excellent characteristics such as the smooth exquisiteness in wire and cable surface.
In order to achieve the above objects and other related objects, the present invention adopts the following technical scheme that.
In a first aspect, the present invention provides a kind of flame-retardant organosilane cross-linked poly-ethylene Insulation Material, raw material includes A material and B material, institute
The weight ratio for stating A material and B material is (78-82): (22-18).
Wherein, the A material includes following parts by weight of component: 65-80 parts of LLDPE resin a；10-25 parts of LLDPE resin b；
4-6 parts of processing aid；1.5-2.7 parts of silane；0.01-0.2 parts of initiator；0.1-0.3 parts of antioxidant；The B material includes following
Parts by weight of component: 45-65 parts of LLDPE resin a；1.5-2.6 parts of catalyst；2-6 parts of antioxidant；10-20 parts of carbon black；Red phosphorus is female
20-30 parts of material.
Preferably, the A material includes following parts by weight of component: 65-75 parts of LLDPE resin a；LLDPE resin b 10-20
Part；4.8-5.2 parts of processing aid；1.9-2.1 parts of silane；0.095-0.105 parts of initiator；0.19-0.21 parts of antioxidant；It is described
B material includes following parts by weight of component: 50-60 parts of LLDPE resin a；1.95-2.05 parts of catalyst；3-5 parts of antioxidant；Carbon black
12-15 parts；22-27 parts of red phosphorus masterbatch.
It is highly preferred that the A material includes following parts by weight of component: 75 parts of LLDPE resin a；20 parts of LLDPE resin b；Add
5 parts of work auxiliary agent；2 parts of silane；0.1 part of initiator；0.2 part of antioxidant；The B material includes following parts by weight of component: LLDPE resin
55 parts of a；2 parts of catalyst；2.9 parts of antioxidant；13-14 parts of carbon black；25 parts of red phosphorus masterbatch.
Preferably, the melt index of the A material and LLDPE resin a in B material is 2.0 at 190 DEG C of load 2.16kg
±0.2g/10min.The melt index is measured using Melt Flow Rate Measurer.
Preferably, the degree of polymerization of the A material and LLDPE resin a in B material is 1000~10000.
It is highly preferred that the A material and coal LLDPE DFDA-7042 in LLDPE resin a model in B material.
Preferably, the melt index of the LLDPE resin b is 8-10g/10min at 150 DEG C of load 2.16kg.It is described
Melt index is measured using Melt Flow Rate Measurer.
Preferably, the degree of polymerization of the LLDPE resin b is 1000~10000.
It is highly preferred that model Zhenghai LLDPE M2320 of the LLDPE resin b.
Preferably, the processing aid is fire retardant.
It is highly preferred that the model FR-1 of the processing aid, originates from Haikang Bang get Industrial Co., Ltd..
Preferably, the silane is vinyltrimethoxysilane.
It is highly preferred that the model LT-171 of the silane, originates from Hubei.
Preferably, the initiator is cumyl peroxide (abbreviation DCP), originates from Aksu.
Preferably, the catalyst is dibutyl tin dilaurate.
Preferably, the model QY166 of the carbon black.
Preferably, the red phosphorus masterbatch is encapsulated red phosphorus flame-retardant master batch.
It is highly preferred that the model YT70 of the red phosphorus masterbatch.
Preferably, the A material and antioxidant in B material are 2,2'- thiobis [3- (3,5- di-t-butyl -4- hydroxy benzenes
Base) ethyl propionate].
Second aspect, the present invention provide a kind of side for preparing flame-retardant organosilane cross-linked poly-ethylene Insulation Material as described above
Method, comprising the following steps: preparation A material；Prepare B material；According to the weight ratio after evenly mixing by A material and B material, flame-proof silicone hydride is obtained
Cross-linked polyethylene insulating material.
Preferably, preparation A material the following steps are included:
(a) the LLDPE resin a and the LLDPE resin b are mixed and is dried according to parts by weight, according still further to weight
The processing aid is added in number, is uniformly mixed, obtains mixture；
(b) in a heated state, the silane, the initiator and the antioxidant are added to step according to parts by weight
Suddenly it in the mixture that (a) is obtained and is uniformly mixed, then through double screw extruder extruding pelletization, obtains pellet；
(c) for the pellet for obtaining step (b) successively after heated-air drying, cold air drying, vacuum packaging prepares institute
State A material.
Preferably, in step (a), the drying temperature of the LLDPE resin a and the LLDPE resin b are 75-85 DEG C,
Drying time is 1.5-2.5h.
Preferably, it in step (b), is heated by the way of the heating of kneading pot pot wall, heating temperature 45-55
℃。
Preferably, in step (b), the mixed revolving speed is 450-550rpm, and the mixed time is 2-5min.
It is highly preferred that the mixed revolving speed is 475-525rpm in step (b), the mixed time is 2.5-
3.5min。
Preferably, in step (b), the double screw extruder is feeding extruding pelletization mixed milling type double-screw extruding pelletizing
Machine.
Preferably, in step (b), the double screw extruder includes ten temperature sections, and one to nine area's temperature is respectively
148-152℃、118-122℃、158-162℃、158-162℃、158-162℃、158-162℃、178-182℃、188-192
DEG C, 198-202 DEG C, head temperature be 228-232 DEG C.
It is highly preferred that the double screw extruder includes ten temperature sections, one to nine area's temperature difference in step (b)
For 150 DEG C, 120 DEG C, 160 DEG C, 160 DEG C, 160 DEG C, 160 DEG C, 180 DEG C, 190 DEG C, 200 DEG C, head temperature is 230 DEG C.
Preferably, in step (b), the mode of the granulation is tie rod pelletizing.
Preferably, in step (c), the temperature of the heated-air drying is 50-70 DEG C, and the time of the heated-air drying is
0.5-2h。
It is highly preferred that in step (c), the temperature of the heated-air drying is 55-65 DEG C, and the time of the heated-air drying is
1-1.5h。
Preferably, in step (c), the temperature of the cold air drying is room temperature, and the time of the cold air drying is 0.5-
1.5h。
Preferably, in step (c), after heated-air drying, cold air drying, A material in moisture weight percentage≤
0.2%.
Moisture in pellet is taken away by hot wind, the material temperature of pellet is reduced and be further dried by cold wind, can be thorough by moisture
The moisture weight percentage composition of bottom removal, finally obtained A material can be down to 0.2%.
Preferably, preparation B material the following steps are included:
(A) LLDPE resin a is weighed according to parts by weight and is dried, and the catalyst, described is added according still further to parts by weight
Antioxidant, the carbon black, the red phosphorus masterbatch are simultaneously uniformly mixed, then through double screw extruder extruding pelletization, obtain pellet；
(B) for the pellet for obtaining step (A) successively after heated-air drying, cold air drying, vacuum packaging prepares institute
State B material.
Preferably, in step (A), the drying temperature of the LLDPE resin a is 80-90 DEG C, drying time 1.5-
2.5h。
Preferably, in step (A), the double screw extruder is feeding extruding pelletization mixed milling type double-screw extruding pelletizing
Machine.
Preferably, in step (A), the double screw extruder includes nine temperature sections, and one to eight area's temperature is respectively
138-142℃、153-157℃、162-167℃、168-172℃、172-178℃、172-178℃、178-183℃、182-187
DEG C, head temperature is 192-198 DEG C.
It is highly preferred that the double screw extruder includes nine temperature sections, one to eight area's temperature difference in step (A)
For 140 DEG C, 155 DEG C, 165 DEG C, 170 DEG C, 175 DEG C, 175 DEG C, 180 DEG C, 185 DEG C, head temperature is 195 DEG C.
Preferably, in step (A), the mode of the granulation is tie rod pelletizing.
Preferably, in step (B), the temperature of the heated-air drying is 50-70 DEG C, and the time of the heated-air drying is
0.5-2h。
It is highly preferred that in step (B), the temperature of the heated-air drying is 55-65 DEG C, and the time of the heated-air drying is
1-1.5h。
Preferably, in step (B), the temperature of the cold air drying is room temperature, and the time of the cold air drying is 0.5-
1.5h。
Preferably, in step (B), after heated-air drying, cold air drying, B material in moisture weight percentage≤
0.2%.
Moisture in pellet is taken away by hot wind, the material temperature of pellet is reduced and be further dried by cold wind, can be thorough by moisture
The moisture weight percentage composition of bottom removal, finally obtained B material can be down to 0.2%.
The third aspect, the present invention provide flame-retardant organosilane cross-linked poly-ethylene Insulation Material as described above and prepare in wire and cable
In purposes.
As described above, a kind of flame-retardant organosilane cross-linked poly-ethylene Insulation Material and its preparation method and application of the invention, this hair
It is bright to have the advantages that
Flame-retardant organosilane cross-linked poly-ethylene Insulation Material of the invention is added using the good flame-retardance energy of red phosphorus masterbatch
In catalyst masterbatch B material, the neither conventional production of influence A material, moreover it is possible to so that resulting organosilane crosslinked polyethylene is exhausted after squeezing out
Edge material can be good at through the horizontal firing performance in UL44 standard.Flame-retardant organosilane cross-linked poly-ethylene Insulation Material tool of the invention
Have that extruded velocity is fast, squeezes out the excellent characteristics such as the smooth exquisiteness in wire and cable surface, cable process velocity prepared by the present invention is more
Fastly, production efficiency is improved, energy consumption and cost are reduced, the use of import CABLE MATERIALS is reduced, is remarkably contributing to save the cost and increase
Benefit.
Specific embodiment
The present invention is further explained combined with specific embodiments below, it should be appreciated that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.
Illustrate embodiments of the present invention below by way of specific specific example, those skilled in the art can be by this specification
Other advantages and efficacy of the present invention can be easily understood for disclosed content.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints and application, without departing from
Various modifications or alterations are carried out under spirit of the invention.
Coal LLDPE DFDA-7042 in LLDPE resin a model employed in the embodiment of the present invention and comparative example,
Model Zhenghai LLDPE M2320 of LLDPE resin b, processing aid model FR-1, silane model LT-171, antioxidant
Model 1035.
Embodiment 1
The raw material of organosilane crosslinked polyethylene insulation material includes A material and B material, and A expects and the weight ratio of B material is 80:20.
A material includes following parts by weight of component: 70 parts of LLDPE resin a；25 parts of LLDPE resin b；5 parts of processing aid；Silicon
2 parts of alkane；0.1 part of initiator；0.1 part of antioxidant.
B material includes following parts by weight of component: 55 parts of LLDPE resin a；2 parts of catalyst；3 parts of antioxidant；15 parts of carbon black；It is red
25 parts of phosphorus masterbatch.
The preparation method of organosilane crosslinked polyethylene insulation material the following steps are included:
1) preparation A material:
LLDPE resin a and LLDPE resin b is dried into 2h under the conditions of 90 DEG C by the above proportion, then with processing aid FR-1
It is uniformly mixed, then mixed at high speed in the state that kneading pot is heated to 50 DEG C, while silane LT-171 is added, initiator DCP, resists
Oxygen agent 1035, mixed at high speed 3min, then blanking, into double screw extruder, extrusion temperature is as shown in table 1.
Table 1
| Heating zone | Ⅰ | Ⅱ | Ⅲ | Ⅳ | Ⅴ | Ⅵ | Ⅶ | Ⅷ | Ⅸ | Head |
| Temperature (DEG C) | 150 | 120 | 160 | 160 | 160 | 160 | 180 | 190 | 200 | 230 |
For the strip of extrusion through water-carrying groove tie rod pelletizing, particle is first pumped into the dry 1h of 60 DEG C of air driers, then is evacuated to cold wind
Drying machine dries 1h, then vacuumizes Aluminum-plastic composite bag and packs to obtain the final product.
2) preparation B material:
LLDPE resin a is first dried into 2h in 80 DEG C of condition, then with dibutyl tin dilaurate, antioxidant, carbon black and red
After mixing, then blanking, into double screw extruder, extrusion temperature is as shown in table 2 for phosphorus masterbatch.
Table 2
| Heating zone | Ⅰ | Ⅱ | Ⅲ | Ⅳ | Ⅴ | Ⅵ | Ⅶ | Ⅷ | Head |
| Temperature (DEG C) | 140 | 155 | 165 | 170 | 175 | 175 | 180 | 185 | 195 |
For the strip of extrusion through water-carrying groove tie rod pelletizing, it is 1 hour dry that particle is first pumped into 60 DEG C of air driers, then is evacuated to cold
Wind drying machine dries 1h, then vacuumizes Aluminum-plastic composite bag and packs to obtain the final product.
3) A material and B are expected according to weight ratio 80:20 after evenly mixing, and puts into and squeezes piece in flow instrument, through natural friendship
Connection, obtains insulating material of polyethylene.
Embodiment 2
The raw material of organosilane crosslinked polyethylene insulation material includes A material and B material, and A expects and the weight ratio of B material is 80:20.
A material includes following parts by weight of component: 65 parts of LLDPE resin a；20 parts of LLDPE resin b；4 parts of processing aid；Silicon
1.8 parts of alkane；0.08 part of initiator；0.19 part of antioxidant.
B material includes following parts by weight of component: 50 parts of LLDPE resin a；1.5 parts of catalyst；2 parts of antioxidant；18 parts of carbon black；
27 parts of red phosphorus masterbatch.
The preparation method of organosilane crosslinked polyethylene insulation material the following steps are included:
2) preparation A material:
LLDPE resin a and LLDPE resin b is dried into 2h under the conditions of 90 DEG C by the above proportion, then with processing aid FR-1
It is uniformly mixed, then mixed at high speed in the state that kneading pot is heated to 50 DEG C, while silane LT-171 is added, initiator DCP, resists
Oxygen agent 1035, mixed at high speed 3min, then blanking, into double screw extruder, extrusion temperature is as shown in table 3.
Table 3
| Heating zone | Ⅰ | Ⅱ | Ⅲ | Ⅳ | Ⅴ | Ⅵ | Ⅶ | Ⅷ | Ⅸ | Head |
| Temperature (DEG C) | 150 | 120 | 160 | 160 | 160 | 160 | 180 | 190 | 200 | 230 |
For the strip of extrusion through water-carrying groove tie rod pelletizing, particle is first pumped into the dry 1h of 60 DEG C of air driers, then is evacuated to cold wind
Drying machine dries 1h, then vacuumizes Aluminum-plastic composite bag and packs to obtain the final product.
2) preparation B material:
LLDPE resin a is first dried into 2h in 80 DEG C of condition, then with dibutyl tin dilaurate, antioxidant, carbon black and red
After mixing, then blanking, into double screw extruder, extrusion temperature is as shown in table 4 for phosphorus masterbatch.
Table 4
| Heating zone | Ⅰ | Ⅱ | Ⅲ | Ⅳ | Ⅴ | Ⅵ | Ⅶ | Ⅷ | Head |
| Temperature (DEG C) | 140 | 155 | 165 | 170 | 175 | 175 | 180 | 185 | 195 |
For the strip of extrusion through water-carrying groove tie rod pelletizing, it is 1 hour dry that particle is first pumped into 60 DEG C of air driers, then is evacuated to cold
Wind drying machine dries 1h, then vacuumizes Aluminum-plastic composite bag and packs to obtain the final product.
3) A material and B are expected according to weight ratio 80:20 after evenly mixing, and puts into and squeezes piece in flow instrument, through natural friendship
Connection, obtains insulating material of polyethylene.
Embodiment 3
The raw material of organosilane crosslinked polyethylene insulation material includes A material and B material, and A expects and the weight ratio of B material is 80:20.
A material includes following parts by weight of component: 80 parts of LLDPE resin a；15 parts of LLDPE resin b；6 parts of processing aid；Silicon
2.5 parts of alkane；0.12 part of initiator；0.21 part of antioxidant.
B material includes following parts by weight of component: 65 parts of LLDPE resin a；2.2 parts of catalyst；5 parts of antioxidant；12 parts of carbon black；
24 parts of red phosphorus masterbatch.
The preparation method of organosilane crosslinked polyethylene insulation material the following steps are included:
3) preparation A material:
LLDPE resin a and LLDPE resin b is dried into 2h under the conditions of 90 DEG C by the above proportion, then with processing aid FR-1
It is uniformly mixed, then mixed at high speed in the state that kneading pot is heated to 50 DEG C, while silane LT-171 is added, initiator DCP, resists
Oxygen agent 1035, mixed at high speed 3min, then blanking, into double screw extruder, extrusion temperature is as shown in table 5.
Table 5
| Heating zone | Ⅰ | Ⅱ | Ⅲ | Ⅳ | Ⅴ | Ⅵ | Ⅶ | Ⅷ | Ⅸ | Head |
| Temperature (DEG C) | 150 | 120 | 160 | 160 | 160 | 160 | 180 | 190 | 200 | 230 |
For the strip of extrusion through water-carrying groove tie rod pelletizing, particle is first pumped into the dry 1h of 60 DEG C of air driers, then is evacuated to cold wind
Drying machine dries 1h, then vacuumizes Aluminum-plastic composite bag and packs to obtain the final product.
2) preparation B material:
LLDPE resin a is first dried into 2h in 80 DEG C of condition, then with dibutyl tin dilaurate, antioxidant, carbon black and red
After mixing, then blanking, into double screw extruder, extrusion temperature is as shown in table 6 for phosphorus masterbatch.
Table 6
| Heating zone | Ⅰ | Ⅱ | Ⅲ | Ⅳ | Ⅴ | Ⅵ | Ⅶ | Ⅷ | Head |
| Temperature (DEG C) | 140 | 155 | 165 | 170 | 175 | 175 | 180 | 185 | 195 |
For the strip of extrusion through water-carrying groove tie rod pelletizing, it is 1 hour dry that particle is first pumped into 60 DEG C of air driers, then is evacuated to cold
Wind drying machine dries 1h, then vacuumizes Aluminum-plastic composite bag and packs to obtain the final product.
3) A material and B are expected according to weight ratio 80:20 after evenly mixing, and puts into and squeezes piece in flow instrument, through natural friendship
Connection, obtains insulating material of polyethylene.
Comparative example 1
The raw material of organosilane crosslinked polyethylene insulation material includes A material and B material, and the weight ratio of the A material and B material is 80:
20。
A material includes following parts by weight of component: 70 parts of LLDPE resin a；25 parts of LLDPE resin b；5 parts of processing aid；Silicon
2 parts of alkane；0.1 part of initiator；0.1 part of antioxidant.
B material includes following parts by weight of component: 80 parts of LLDPE resin a；2 parts of catalyst；3 parts of antioxidant；15 parts of carbon black.
The preparation method of organosilane crosslinked polyethylene insulation material the following steps are included:
1) preparation A material:
LLDPE resin a and LLDPE resin b is dried into 2h under the conditions of 90 DEG C by the above proportion, then with processing aid FR-1
It is uniformly mixed, then mixed at high speed in the state that kneading pot is heated to 50 DEG C, while silane LT-171, initiator DCP is added, resist
Oxygen agent 1035, mixed at high speed 3min, then blanking, into double screw extruder, extrusion temperature is as shown in table 7.
Table 7
| Heating zone | Ⅰ | Ⅱ | Ⅲ | Ⅳ | Ⅴ | Ⅵ | Ⅶ | Ⅷ | Ⅸ | Head |
| Temperature (DEG C) | 150 | 120 | 160 | 160 | 160 | 160 | 180 | 190 | 200 | 230 |
For the strip of extrusion through water-carrying groove tie rod pelletizing, particle is first pumped into the dry 1h of 60 DEG C of air driers, then is evacuated to cold wind
Drying machine dries 1h, then vacuumizes Aluminum-plastic composite bag and packs to obtain the final product.
2) preparation B material:
LLDPE DFDA-7042 is first dried into 2h under the conditions of 80 DEG C, then with dibutyl tin dilaurate, antioxidant and carbon
It is black after mixing, then blanking, into double screw extruder, extrusion temperature is as shown in table 8.
Table 8
| Heating zone | Ⅰ | Ⅱ | Ⅲ | Ⅳ | Ⅴ | Ⅵ | Ⅶ | Ⅷ | Head |
| Temperature (DEG C) | 140 | 155 | 165 | 170 | 175 | 175 | 180 | 185 | 195 |
For the strip of extrusion through water-carrying groove tie rod pelletizing, it is 1 hour dry that particle is first pumped into 60 DEG C of air driers, then is evacuated to cold
Wind drying machine dries 1h, then vacuumizes Aluminum-plastic composite bag and packs to obtain the final product.
3) A material and B are expected according to weight ratio 80:20 after evenly mixing, and puts into and squeezes piece in flow instrument, through natural friendship
Connection, obtains insulating material of polyethylene.
Comparative example 2
The raw material of organosilane crosslinked polyethylene insulation material includes A material and B material, and the weight ratio of the A material and B material is 80:
20。
A material includes following parts by weight of component: 70 parts of LLDPE resin a；25 parts of LLDPE resin b；5 parts of processing aid；Silicon
2 parts of alkane；0.1 part of initiator；0.1 part of antioxidant.
B material includes following parts by weight of component: 60 parts of LLDPE resin a；2 parts of catalyst；3 parts of antioxidant；15 parts of carbon black；Ten
15 parts of bromine；5 parts of antimony oxide.
The preparation method of organosilane crosslinked polyethylene insulation material the following steps are included:
1) preparation A material:
Resin LLDPE DFDA-7042 and LLDPE M2320 is dried into 2h under the conditions of 90 DEG C by the above proportion, then with add
Work auxiliary agent FR-1 is uniformly mixed, then mixed at high speed in the state that kneading pot is heated to 50 DEG C, while silane LT-171 is added, draws
Agent DCP, antioxidant 1035, mixed at high speed 3min are sent out, then blanking, into double screw extruder, extrusion temperature is as shown in table 9.
Table 9
| Heating zone | Ⅰ | Ⅱ | Ⅲ | Ⅳ | Ⅴ | Ⅵ | Ⅶ | Ⅷ | Ⅸ | Head |
| Temperature (DEG C) | 150 | 120 | 160 | 160 | 160 | 160 | 180 | 190 | 200 | 230 |
For the strip of extrusion through water-carrying groove tie rod pelletizing, particle is first pumped into the dry 1h of 60 DEG C of air driers, then is evacuated to cold wind
Drying machine dries 1h, then vacuumizes Aluminum-plastic composite bag and packs to obtain the final product.
2) preparation B material:
LLDPE DFDA-7042 first dried to the condition of 2h under the conditions of 80 DEG C, then with dibutyl tin dilaurate, antioxygen
After mixing, then blanking, into double screw extruder, extrusion temperature is as shown in table 10 for agent, carbon black, ten bromines, antimony oxide.
Table 10
| Heating zone | Ⅰ | Ⅱ | Ⅲ | Ⅳ | Ⅴ | Ⅵ | Ⅶ | Ⅷ | Head |
| Temperature (DEG C) | 140 | 155 | 165 | 170 | 175 | 175 | 180 | 185 | 195 |
For the strip of extrusion through water-carrying groove tie rod pelletizing, it is 1 hour dry that particle is first pumped into 60 DEG C of air driers, then is evacuated to cold
Wind drying machine dries 1h, then vacuumizes Aluminum-plastic composite bag and packs to obtain the final product.
3) A material and B are expected according to weight ratio 80:20 after evenly mixing, and puts into and squeezes piece in flow instrument, through natural friendship
Connection, obtains insulating material of polyethylene.
Comparative example 3
The raw material of organosilane crosslinked polyethylene insulation material includes A material and B material, and the weight ratio of the A material and B material is 80:
20。
A material includes following parts by weight of component: 70 parts of LLDPE resin a；25 parts of LLDPE resin b；5 parts of processing aid；Silicon
2 parts of alkane；0.1 part of initiator；0.1 part of antioxidant.
B material includes following parts by weight of component: 55 parts of LLDPE resin a；2 parts of catalyst；3 parts of antioxidant；15 parts of carbon black；Hydrogen
25 parts of magnesia.
The preparation method of organosilane crosslinked polyethylene insulation material, comprising the following steps:
1) preparation A material: resin LLDPE DFDA-7042 and LLDPE M2320 is dried in 90 DEG C of conditions by the above proportion
2h, then be uniformly mixed with processing aid FR-1, then mixed at high speed in the state that kneading pot is heated to 50 DEG C, while silane is added
LT-171, initiator DCP and antioxidant 1035, mixed at high speed 3min, then blanking are into double screw extruder, extrusion temperature such as table
Shown in 11.
Table 11
For the strip of extrusion through water-carrying groove tie rod pelletizing, particle is first pumped into the dry 1h of 60 DEG C of air driers, then is evacuated to cold wind
Drying machine dries 1h, then vacuumizes Aluminum-plastic composite bag and packs to obtain the final product.
4) preparation B material:
First LLDPE DFDA-7042 is dried into 2h under the conditions of 80 DEG C, then is mixed with dibutyl tin dilaurate, antioxidant
After uniformly, then blanking, into double screw extruder, extrusion temperature is as shown in table 12.
Table 12
| Heating zone | Ⅰ | Ⅱ | Ⅲ | Ⅳ | Ⅴ | Ⅵ | Ⅶ | Ⅷ | Head |
| Temperature (DEG C) | 140 | 155 | 165 | 170 | 175 | 175 | 180 | 185 | 195 |
For the strip of extrusion through water-carrying groove tie rod pelletizing, it is 1 hour dry that particle is first pumped into 60 DEG C of air driers, then is evacuated to cold
Wind drying machine dries 1h, then vacuumizes Aluminum-plastic composite bag and packs to obtain the final product.
3) A material and B are expected according to weight ratio 80:20 after evenly mixing, and puts into and squeezes piece in flow instrument, through natural friendship
Connection, obtains insulating material of polyethylene.
Test result:
Insulating material of polyethylene made from embodiment 1 to 3 and comparative example 1 to 3 is existedElectric wire is squeezed out on machine, by embodiment
1, the resulting electric wire of comparative example 1 to 3 carries out surface comparison and performance test respectively, and performance test results are as shown in table 13,14.
Table 13
Table 14
By the performance test results of embodiment 1 to 3 in table 13, table 14 and comparative example 1 to 3 and to engineer testing scene table
Face observation result can be seen that after UL baking oven heat ageing, and the electric wire of embodiment 1 to 3 stretches change rate of strength and extension at break
Rate change rate is below the electric wire of comparative example 1 to 3.Embodiment 1 to 3 existsWire surface smooth exquisiteness when machine unwrapping wire, better than pair
The surface appearance of the electric wire of ratio 2 and comparative example 3.Embodiment 1 to 3 obtains cable and passes through the horizontal firing performance in UL44 standard
Test, and 1 to 3 horizontal firing of comparative example cannot be tested by the horizontal firing performance in UL44 standard.Illustrate embodiment 1 to
3 enable the electric wire obtained to have good flame-retardance, the neither conventional production of influence A material using addition red phosphorus masterbatch into B material,
Resulting organosilane crosslinked polyethylene insulation material after squeezing out can also be made to can be good at through the horizontal flammability in UL44 standard
Energy.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (10)
1. a kind of flame-retardant organosilane cross-linked poly-ethylene Insulation Material, which is characterized in that its raw material includes A material and B material, and the A expects and institute
The weight ratio for stating B material is (75-85): (15-25)；
Wherein, the A material includes following parts by weight of component:
The B material includes following parts by weight of component:
2. flame-retardant organosilane cross-linked poly-ethylene Insulation Material as described in claim 1, which is characterized in that in the A material and B material
Melt index of the LLDPE resin a at 190 DEG C of load 2.16kg is (1.8-2.2) g/10min.
3. flame-retardant organosilane cross-linked poly-ethylene Insulation Material as described in claim 1, which is characterized in that the LLDPE resin b exists
Melt index under 150 DEG C of load 2.16kg is (8-10) g/10min.
4. flame-retardant organosilane cross-linked poly-ethylene Insulation Material as described in claim 1, which is characterized in that the processing aid is fire-retardant
Agent；
And/or the silane is vinyltrimethoxysilane；
And/or the initiator is cumyl peroxide；
And/or the catalyst is dibutyl tin dilaurate；
And/or the red phosphorus masterbatch is encapsulated red phosphorus flame-retardant master batch；
And/or antioxidant is 2,2'- thiobis [3- (3,5- di-tert-butyl-hydroxy phenyl) third in the A material and B material
Acetoacetic ester].
5. a kind of prepare the method such as the described in any item flame-retardant organosilane cross-linked poly-ethylene Insulation Materials of Claims 1-4, feature
It is, comprising the following steps: preparation A material；Prepare B material；According to the weight ratio after evenly mixing by A material and B material, fire-retardant silicon is obtained
Alkane cross-linked polyethylene insulating material.
6. the preparation method of flame-retardant organosilane cross-linked poly-ethylene Insulation Material as claimed in claim 5, which is characterized in that the preparation
A material the following steps are included:
(a) the LLDPE resin a and the LLDPE resin b are mixed and is dried according to parts by weight, according still further to parts by weight
The processing aid is added, is uniformly mixed, obtains mixture；
(b) in a heated state, the silane, the initiator and the antioxidant are added to step according to parts by weight
(a) it in the mixture obtained and is uniformly mixed, then squeezes out, is granulated through double screw extruder, obtain pellet；
(c) for the pellet for obtaining step (b) successively after heated-air drying, cold air drying, vacuum packaging prepares the A
Material.
7. the preparation method of flame-retardant organosilane cross-linked poly-ethylene Insulation Material as claimed in claim 6, which is characterized in that in step
(a) in, the drying temperature of the LLDPE resin a and the LLDPE resin b are 75-85 DEG C, drying time 1.5-2.5h；
And/or in step (b), heated by the way of the heating of kneading pot pot wall, heating temperature is 45-55 DEG C；
And/or in step (b), the mixed revolving speed is 450-550rpm, and the mixed time is 2-5min；
And/or in step (b), the double screw extruder includes ten temperature sections, and one to ten area's temperature is respectively 148-
152℃、118-122℃、158-162℃、158-162℃、158-162℃、158-162℃、178-182℃、188-192℃、
198-202℃,228-232℃；
And/or in step (b), the mode of the granulation is tie rod pelletizing；
And/or in step (c), the temperature of the heated-air drying is 60-70 DEG C, and the time of heated-air drying is 1-2h；
And/or in step (c), the temperature of the cold air drying is room temperature, and the time of the cold air drying is 0.5-1.5h.
8. the preparation method of flame-retardant organosilane cross-linked poly-ethylene Insulation Material as claimed in claim 5, which is characterized in that the preparation
B material the following steps are included:
(A) LLDPE resin a is weighed according to parts by weight and is dried, and the catalyst, the antioxygen is added according still further to parts by weight
Agent, the carbon black, the red phosphorus masterbatch are simultaneously uniformly mixed, then are squeezed out, are granulated through double screw extruder, and pellet is obtained；
(B) for the pellet for obtaining step (A) successively after heated-air drying, cold air drying, vacuum packaging prepares the B
Material.
9. the preparation method of flame-retardant organosilane cross-linked poly-ethylene Insulation Material as claimed in claim 8, which is characterized in that in step
(A) in, the drying temperature of the LLDPE resin a is 75-85 DEG C, drying time 1.5-2.5h；
And/or in step (A), the double screw extruder includes nine temperature sections, and one to nine area's temperature is respectively 138-
142℃、153-157℃、162-167℃、168-172℃、172-178℃、172-178℃、178-183℃、182-187℃、
192-198℃；
And/or in step (A), the mode of the granulation is tie rod pelletizing；
And/or in step (B), the temperature of the heated-air drying is 60-70 DEG C, and the time of the heated-air drying is 1-2h；
And/or in step (B), the temperature of the cold air drying is room temperature, and the time of the cold air drying is 0.5-1.5h.
10. the flame-retardant organosilane cross-linked poly-ethylene Insulation Material as described in any one of claim 1-4 claim is in wire and cable system
Purposes in standby.
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| CN110760123A (en) * | 2019-12-11 | 2020-02-07 | 上海凯波特种电缆料厂有限公司 | High-carbon-black tracking-resistant silane crosslinked polyethylene insulating material and preparation method thereof |
| CN112480523A (en) * | 2020-11-27 | 2021-03-12 | 无锡鸿仪新材料科技有限公司 | Silane crosslinked polyethylene insulating material for overhead cable and preparation process thereof |
| CN113736167A (en) * | 2021-09-30 | 2021-12-03 | 苏州亨利通信材料有限公司 | Weather-resistant silane crosslinked polyethylene overhead insulating material and preparation method thereof |
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| CN116262845A (en) * | 2022-11-15 | 2023-06-16 | 浙江万马高分子材料集团有限公司 | Weather-proof and tracking-resistant silane crosslinked polyethylene insulating material and preparation method thereof |
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| CN112480523A (en) * | 2020-11-27 | 2021-03-12 | 无锡鸿仪新材料科技有限公司 | Silane crosslinked polyethylene insulating material for overhead cable and preparation process thereof |
| CN113736167A (en) * | 2021-09-30 | 2021-12-03 | 苏州亨利通信材料有限公司 | Weather-resistant silane crosslinked polyethylene overhead insulating material and preparation method thereof |
| CN114426729A (en) * | 2021-11-19 | 2022-05-03 | 浙江万马高分子材料集团有限公司 | Low-precipitation silane crosslinked polyethylene insulating material and preparation method thereof |
| CN115010864A (en) * | 2022-06-17 | 2022-09-06 | 浙江太湖远大新材料股份有限公司 | Preparation of special silane crosslinked polyethylene insulating material for thin-wall wire |
| CN115926299A (en) * | 2022-10-31 | 2023-04-07 | 上海凯波电缆特材股份有限公司 | Silane crosslinking halogen-free flame-retardant polyolefin material for photovoltaic cable and preparation method thereof |
| CN116262845A (en) * | 2022-11-15 | 2023-06-16 | 浙江万马高分子材料集团有限公司 | Weather-proof and tracking-resistant silane crosslinked polyethylene insulating material and preparation method thereof |
| CN116262845B (en) * | 2022-11-15 | 2024-11-05 | 浙江万马高分子材料集团有限公司 | Weather-proof and tracking-resistant silane crosslinked polyethylene insulating material and preparation method thereof |
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