CN104861269A - Medium-voltage water-tree-retardant crosslinked polyethylene cable material and preparation method thereof - Google Patents
Medium-voltage water-tree-retardant crosslinked polyethylene cable material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a medium-voltage water-tree-retardant crosslinked polyethylene cable material and a preparation method thereof and belongs to the technical field of wire cable materials and preparation of the wire cable materials. The medium-voltage water-tree-retardant crosslinked polyethylene cable material is prepared from raw materials as follows: 60-75 parts of polyolefin composite resin, 15-25 parts of a polyethylene silane-grafting material, 5-10 parts of water-tree-retardant composite catalytic master batch and 2-5 parts of a cross-linking agent. The polyolefin composite resin comprises raw materials as follows: 60-80 parts of low-density polyethylene and 20-40 parts of ethylene vinyl acetate copolymer; the water-tree-retardant composite catalytic master batch comprises raw materials as follows: 70-80 parts of low-density polyethylene, 3-5 parts of a catalyst, 10-15 parts of a nucleating agent, 2-5 parts of an antioxidant, 0.1-0.2 parts of a crosslinking agent and 3-5 parts of an assistant crosslinking agent. Formation of a water tree is delayed, surrounding water can be dispersed to a certain extent, formation of the water tree can be effectively inhibited, the overall physical property of the material is improved, and the material has excellent mechanical and physical properties and is environment-friendly.
Description
Technical field
The invention belongs to electric wire and cable material and preparing technical field thereof, be specifically related in one, press water resistant to set cross-linked poly-ethylene cable material, and relate to its preparation method.
Background technology
The concept of aforesaid middle pressure is known by industry, refer to the proof voltage of cable or claim to be suitable for voltage range, such as 0.6 (line voltage)/1KV (phase voltage) and be low-voltage cable below, 3.6 (line voltage)/6KV (phase voltages) are midium voltage cable to 25KV, 35-110KV is high-tension cable, and more than 220KV is extra-high-tension cable.Above mentioned water tree refers in presence of water and under the effect of highfield, the cable insulation material be exposed in water forms dendritic defect, and this defect easily causes cable insulation disruptive strength to reduce and fault.
Peroxide crosslinked polyethylene material has good thermotolerance, excellent insulating property and the advantage such as easy to process because of it, is widely used in middle-high voltage power cable field.Cross-linked polyethylene insulated cable is pressed generally to adopt common cross-linked polyethylene insulating material as cable insulation for a long time in China, but according to State Grid's department statistics display in recent years, because it is laid in the wet environment of underground for a long time, thus pressure crosslinking polyethylene-insulated cable insulation layer in after more than 5 years is used just to start to occur water tree phenomenon, continuous increase (spreading) along with water tree can aggravate the rapid ageing of cable insulation, thus causes power failure to take place frequently.
In order to slow down or suppress the formation of cable water tree, domestic and international experts and scholars propose a lot of solution.Known technical scheme is mainly based on following two kinds of thinkings, first, from sub polyethylene minor structure, by grafting on molecular chain or some specific groups of copolymerization to stop the localized agglomeration of moisture content, and then play the effect suppressing water tree, " the having the preparation method of specific water tree growth rate multipolymer " of recommending as invention patent mandate notification number CN1078225C (patent No. is ZL90106964.7) discloses by ethene, the polymkeric substance of the monomer copolymerization such as 4-methyl-1-pentene and vinyl silanes compound are containing magnesium, titanium, the compound system of the catalyzer of halogen and electron donor(ED) has excellent water tree resistant property, second, select some to take into account and with base material, there is better consistency and there is the additive that excellent water resistant sets characteristic, this additive mostly is the polar material that some possess certain water-wet behavior, the effect of dispersion moisture content can be played, as US Patent No. 6828505B1 reports that the polyoxyethylene glycol additive of different molecular weight shows excellent water resistant tree function in crosslinked polyethylene system in whole system.The combination that China Patent Publication No. CN101367972 discloses aromaticity multipolymer and EVA can be used as the use that water sets inhibitor.
Although the research both at home and abroad for middle pressure water resistant tree crosslinked polyethylene has achieved certain achievement, but still fail to reach the degree that industry institute's phase gets, such as there is the technical barriers such as such as poor compatibility, cost be high, volatile and still annoying electric wire production firm.Substitute the constantly surging of the cry of common crosslinked material along with recent year uses water resistant to set crosslinked material comprehensively, if can not be broken through, so will certainly form restriction to China's electric wire towards domestic and international market.In view of this, the applicant has done useful exploration, and technical scheme described below produces under this background.
Summary of the invention
Task of the present invention is to provide a kind of and contributes to significantly improving water tree resistant property, be conducive to embodying desirable mechanical and physical performance and processability, being of value to the middle pressure water resistant tree cross-linked poly-ethylene cable material embodying excellent environmental protection effect.
Another task of the present invention is the preparation method providing a kind of middle pressure water resistant tree cross-linked poly-ethylene cable material, presses water resistant to set cross-linked poly-ethylene cable material can ensure excellent water tree resistant property, desirable mechanical and physical performance and processability and environmental protection by the method in being obtained.
Task of the present invention has been come like this, press water resistant to set cross-linked poly-ethylene cable material in one, it is made up of the raw material of following proportioning by weight: polyolefine compound resin 60-75 part, polyethylene-silane grafted material 15-25 part, water resistant tree composite catalyzing master batch 5-10 part and linking agent 2-5 part; Described polyolefine compound resin is made up of the raw material of following proportioning by weight: Low Density Polyethylene 60-80 part and ethylene vinyl acetate 20-40 part; Described water resistant tree composite catalyzing master batch is made up of the raw material of following proportioning by weight: Low Density Polyethylene 70-80 part, catalyzer 3-5 part, nucleator 10-15 part, oxidation inhibitor 2-5 part, linking agent 0.1-0.2 part and additional crosslinker 3-5 part.
In a specific embodiment of the present invention, the Low Density Polyethylene of described Low Density Polyethylene to be melting index be 1.8-2.2g/10min; Described ethylene vinyl acetate is the mass percentage of vinyl acetate between to for plastic (VA) is the ethylene vinyl acetate of 18-28%.
In another specific embodiment of the present invention, the melting index of described polyethylene-silane grafted material is 1.5-1.8g/min, and described silane is vinyl-three (2-methoxy ethoxy) silane.
In another specific embodiment of the present invention, described catalyzer is one or more the combination in dinonylnaphthalene sulfonic acid, dinonylnaphthalene disulfonic acid, Witco 1298 Soft Acid; Described nucleator is Zinic stearas or calcium stearate.
In another specific embodiment of the present invention, described oxidation inhibitor is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, 4,4'-thiobis (the 6-tertiary butyl-3-methylphenol), 2,6-di-tert-butyl methyl phenol, (2,4-di-tert-butyl-phenyl) one or more combination in tris phosphite, β-positive octadecanol ester of (3,5-di-tert-butyl-hydroxy phenyl) propionic acid and Tyox B.
Also have in a specific embodiment of the present invention, described linking agent is one or more the combination in dicumyl peroxide, the dibenzoyl peroxide tert-butyl ester, dual-tert-butyl dicumyl peroxide; Described additional crosslinker is one or more mixtures in iso-cyanuric acid triallyl ester, triallyl cyanurate, trimethylolpropane trimethacrylate and Viscoat 295.
A preparation method for middle pressure water resistant tree cross-linked poly-ethylene cable material, comprises the following steps:
A) polyethylene-silane grafted material is prepared, by the Low Density Polyethylene 80-90 part taken by weight, vinyl silanes 3-5 part, linking agent 0.1-0.2 part and oxidation inhibitor 2-4 part drop into pre-mixing in stirred vessel, and control rotating speed and the pre-mixing time of stirred vessel, obtain polyethylene silicon alkylating mixture, then this polyethylene silicon alkylating mixture is extruded by carrying out grafting in volume pump feeding to twin screw extruder, and control rotating speed that twin screw extruder grafting extrudes and extrusion temperature, through water ring pelletizing, dehydration and drying, obtain polyethylene-silane grafted material,
B) water resistant tree composite catalyzing master batch is prepared, the Low Density Polyethylene 70-80 part taken by weight, oxidation inhibitor 2-5 part, catalyzer 3-5 part, linking agent 0.1-0.2 part, additional crosslinker 3-5 part and nucleator 10-15 part drop into premix in whipping appts, and control stirring velocity and the premix time of whipping appts, obtain miscellany, then miscellany is extruded by carrying out plasticizing in volume pump feeding to twin screw extruder, what control twin screw extruder extrudes rotating speed and extrusion temperature, through water ring pelletizing, dehydration and drying, obtain water resistant tree composite catalyzing master batch,
C) finished product is prepared, by the polyolefine compound resin 60-75 part taken by weight, by steps A) polyethylene-silane grafted material 15-25 part of obtaining and by step B) water resistant tree composite catalyzing master batch 5-10 part of obtaining and linking agent 2-5 part drops in mixing machine and mixes, and control mixing velocity and the mixing time of mixing machine, obtain water resistant tree premixture, then this water resistant is set premixture by carrying out blending extrusion in volume pump feeding to twin screw extruder, control blending extrusion rotating speed and blending extrusion temperature, through water ring pelletizing, dehydration and drying, obtain middle pressure water resistant tree cross-linked poly-ethylene cable material, wherein: described polyolefine compound resin is made up of the Low Density Polyethylene 60-80 part taken by weight and ethylene vinyl acetate 20-40 part.
More of the present invention and in a specific embodiment, steps A) described in Low Density Polyethylene be melting index be 1.8-2.2g/10min; Described vinyl silanes is vinyl-three (2-methoxy ethoxy) silane; Described linking agent is one or more the combination in dicumyl peroxide, the dibenzoyl peroxide tert-butyl ester, dual-tert-butyl dicumyl peroxide; Described oxidation inhibitor is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, 4,4'-thiobis (the 6-tertiary butyl-3-methylphenol), 2,6-di-tert-butyl methyl phenol, (2,4-di-tert-butyl-phenyl) one or more combination in tris phosphite, β-positive octadecanol ester of (3,5-di-tert-butyl-hydroxy phenyl) propionic acid and Tyox B.
In an of the present invention and then specific embodiment, steps A) described in the rotating speed of control stirred vessel and the pre-mixing time be that the rotating speed of stirred vessel is controlled as 200-300r/min, be 5-8min by the time controling of pre-mixing, the rotating speed that described control twin screw extruder grafting is extruded is that rotating speed twin screw extruder grafting extruded controls as 215-245r/min; Step B) described in the stirring velocity of control whipping appts and the premix time be that the stirring velocity of whipping appts is controlled as 200-300r/min, be 5-8min by the time controling of premix, the rotating speed of extruding of described control twin screw extruder controls as 190-210r/min by the rotating speed of extruding of twin screw extruder; Step C) described in the mixing velocity of control mixing machine and mixing time be that mixing velocity is controlled as 300-350r/min, mixing time controlled as 3-5min, the rotating speed of described control blending extrusion controls the rotating speed of blending extrusion for 210-230r/min.
Of the present invention again more and in a specific embodiment, steps A) described in control extrusion temperature be that the temperature of a district of district to eight of twin screw extruder, machine neck and head is controlled as 120 DEG C, a district, two 135 DEG C, districts, three 145 DEG C, districts, four 155 DEG C, districts, five 165 DEG C, districts, six 178 DEG C, districts, seven 185 DEG C, districts, eight 190 DEG C, districts, 195 DEG C, machine neck, head 200 DEG C; Step B) described in control extrusion temperature be that the temperature of a district of district to eight of twin screw extruder, machine neck and head is controlled as 120 DEG C, a district, two 135 DEG C, districts, three 145 DEG C, districts, four 155 DEG C, districts, five 162 DEG C, districts, six 168 DEG C, districts, seven 175 DEG C, districts, eight 180 DEG C, districts, 185 DEG C, machine neck, head 190 DEG C; Step C) described in control blending extrusion temperature be that the temperature of a district of district to eight of twin screw extruder, machine neck and head is controlled as: 98 DEG C, a district, two 100 DEG C, districts, three 102 DEG C, districts, four 105 DEG C, districts, five 106 DEG C, districts, six 108 DEG C, districts, seven 110 DEG C, districts, eight 110 DEG C, districts, 112 DEG C, machine neck, head 112 DEG C.
One of technical scheme provided by the invention technique effect compared with the prior art, owing to introducing the good polyethylene-silane grafted material of graft polymerization preformer in system, again because silane has very strong hydrophilic, water absorbability, and be uniformly distributed in Insulation Material, thus moisture content is around dispersibled, effective suppression moisture content localized agglomeration, is extremely conducive to the formation delaying water tree; Two, the introducing of organic sulfonic acid catalyst has dual-use function, first, it can the hydrolysis of catalysis silane with crosslinked, the poly cross-linking density of further raising, prevent the too much infiltration of moisture content, secondly, sulfonic acid catalyst is because of its special chain alkyl structure, itself and polyolefine have good consistency, but its sulfonic acid group has again certain water absorbability, moisture content around can be disperseed to a certain extent, there is the function of excellent suppression water tree equally; Three, the introducing of organic nucleating agent can impel that polyethylene crystallization crystal grain is more regular, size is less, crystallization velocity is faster, degree of crystallinity is higher, can effectively suppress water to set the overall physical properties being formed and promote material; Four, due to each material choice in formula and reasonable ratio, thus there is excellent mechanical and physical performance; Five, because organic sulfonic acid catalyst can't harm environment, thus can embody environmental protection effect.
Embodiment
Embodiment 1:
A) polyethylene-silane grafted material is prepared, it is first the Low Density Polyethylene 80 parts of 1.8g/10min by the melting index taken by weight, 5 parts, vinyl-three (2-methoxy ethoxy) silane, dicumyl peroxide 0.1 part and 4, 4'-thiobis (the 6-tertiary butyl-3-methylphenol) 2 parts drops into pre-mixing in stirred vessel, the rotating speed of stirred vessel controls as 200r/min, the time controling of pre-mixing is 8min, obtain polyethylene silicon alkylating mixture, then this polyethylene silicon alkylating mixture is such as extruded by carrying out grafting in Brabender metering system feeding to (being namely fed to) twin screw extruder by volume pump that (said grafting is extruded and is plasticizing and extrudes here, the following examples 2 and 3 are with example), the rotating speed that twin screw extruder grafting is extruded controls as 245r/min, and by the extrusion temperature of twin screw extruder from a district of district to eight, the temperature of machine neck and head is controlled as 120 DEG C, a district, two 135 DEG C, districts, three 145 DEG C, districts, four 155 DEG C, districts, five 165 DEG C, districts, six 178 DEG C, districts, seven 185 DEG C, districts, eight 190 DEG C, districts, 195 DEG C, machine neck, head 200 DEG C, again successively through water ring pelletizing, dehydration and drying, obtain melting index and be 1.8g/10min and silane is the polyethylene-silane grafted material of vinyl-three (2-methoxy ethoxy) silane, stand-by,
B) water resistant tree composite catalyzing master batch is prepared, be first 2.2g/10min Low Density Polyethylene 70 parts by the melting index taken by weight, four [β-(3, 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 3.5 parts, dinonylnaphthalene disulfonic acid 3 parts, dicumyl peroxide 0.1 part, the dibenzoyl peroxide tert-butyl ester 0.1 part, different three cyanate 4 parts of triallyl and premix in calcium stearate 10 parts of input whipping apptss, the stirring velocity of whipping appts controls as 250r/min, premix time controling is 6.5min, obtain miscellany (miscellany is mixture), then miscellany is carried out plasticizing as passed through in Brabender metering system feeding to (being namely fed to) twin screw extruder by volume pump to extrude, the rotating speed of extruding of twin screw extruder controls as 190r/min, and by the extrusion temperature of twin screw extruder from a district of district to eight, the temperature of machine neck and head is controlled as: 120 DEG C, a district, two 130 DEG C, districts, three 145 DEG C, districts, four 155 DEG C, districts, five 162 DEG C, districts, six 168 DEG C, districts, seven 175 DEG C, districts, eight 180 DEG C, districts, 185 DEG C, machine neck, head 190 DEG C, again successively through water ring pelletizing, dehydration and drying, obtain water resistant tree composite catalyzing master batch, stand-by,
C) finished product is prepared, the polyolefine compound resin 65 parts first will taken by weight, by steps A) the polyethylene-silane grafted material 25 parts that obtains, by step B) mix in the water resistant that obtains tree composite catalyzing master batch 8 parts and dicumyl peroxide 2 parts of input mixing machines, the mixing velocity of mixing machine controls as 300r/min, mixing time controls as 5min, obtain water resistant tree premixture, then by this water resistant tree premixture by volume pump as by carrying out blending extrusion in Brabender metering system feeding to twin screw extruder, blending extrusion rotating speed controls as 220r/min, and by the blending extrusion temperature of twin screw extruder from a district of district to eight, the temperature of machine neck and head is controlled as: 98 DEG C, a district, two 100 DEG C, districts, three 102 DEG C, districts, four 105 DEG C, districts, five 106 DEG C, districts, six 108 DEG C, districts, seven 110 DEG C, districts, eight 110 DEG C, districts, 112 DEG C, machine neck, head 112 DEG C, again successively through water ring pelletizing, dehydration and drying, obtain middle pressure water resistant tree cross-linked poly-ethylene cable material, polyolefine compound resin described in this step is made up of the Low Density Polyethylene taken by weight 60 parts and ethylene vinyl acetate 40 parts, the melting index of this Low Density Polyethylene is 2.2g/10min, and the mass percentage that ethylene vinyl acetate is vinyl acetate between to for plastic (VA) is 18%.
Embodiment 2:
A) polyethylene-silane grafted material is prepared, it is first the Low Density Polyethylene 90 parts of 2.2g/10min by the melting index taken by weight, 3 parts, vinyl-three (2-methoxy ethoxy) silane, dicumyl peroxide 0.1 part, dual-tert-butyl dicumyl peroxide 0.1 part, four [β-(3, 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 1 part, β-(3, 5-di-tert-butyl-hydroxy phenyl) the positive octadecanol ester of propionic acid 0.5 part and Tyox B 0.5 part drop into pre-mixing in stirred vessel, the rotating speed of stirred vessel controls as 300r/min, the time controling of pre-mixing is 5min, obtain polyethylene silicon alkylating mixture, then this polyethylene silicon alkylating mixture is carried out grafting by volume pump as passed through in Brabender metering system feeding to (being namely fed to) twin screw extruder to squeeze, the rotating speed that twin screw extruder grafting is extruded controls as 215r/min, and by the extrusion temperature of twin screw extruder from a district of district to eight, the temperature of machine neck and head is controlled as 120 DEG C, a district, two 135 DEG C, districts, three 145 DEG C, districts, four 155 DEG C, districts, five 165 DEG C, districts, six 178 DEG C, districts, seven 185 DEG C, districts, eight 190 DEG C, districts, 195 DEG C, machine neck, head 200 DEG C, again successively through water ring pelletizing, dehydration and drying, obtain melting index and be 2.2g/10min and silane is the polyethylene-silane grafted material of vinyl-three (2-methoxy ethoxy) silane, stand-by,
B) water resistant tree composite catalyzing master batch is prepared, be first 2g/10min Low Density Polyethylene 75 parts by the melting index taken by weight, 4, 4'-thiobis (the 6-tertiary butyl-3-methylphenol) 2.5 parts, 2, 6-di-tert-butyl methyl phenol 2.5 parts, dinonylnaphthalene disulfonic acid 2.5 parts, dual-tert-butyl dicumyl peroxide 0.1 part, trimethylolpropane trimethacrylate 1.5 parts, Viscoat 295 1.5 parts and premix in Zinic stearas 15 parts of input whipping apptss, the stirring velocity of whipping appts controls as 200r/min, premix time controling is 8min, obtain miscellany (miscellany is mixture), then miscellany is carried out plasticizing as passed through in Brabender metering system feeding to (being namely fed to) twin screw extruder by volume pump to extrude, the rotating speed of extruding of twin screw extruder controls as 210r/min, and by the extrusion temperature of twin screw extruder from a district of district to eight, the temperature of machine neck and head is controlled as: 120 DEG C, a district, two 130 DEG C, districts, three 145 DEG C, districts, four 155 DEG C, districts, five 162 DEG C, districts, six 168 DEG C, districts, seven 175 DEG C, districts, eight 180 DEG C, districts, 185 DEG C, machine neck, head 190 DEG C, again successively through water ring pelletizing, dehydration and drying, obtain water resistant tree composite catalyzing master batch, stand-by,
C) finished product is prepared, the polyolefine compound resin 75 parts first will taken by weight, by steps A) the polyethylene-silane grafted material 15 parts that obtains, by step B) mix in the water resistant that obtains tree composite catalyzing master batch 5 parts and dicumyl peroxide 5 parts of input mixing machines, the mixing velocity of mixing machine controls as 350r/min, mixing time controls as 3min, obtain water resistant tree premixture, then by this water resistant tree premixture by volume pump as by carrying out blending extrusion in Brabender metering system feeding to twin screw extruder, blending extrusion rotating speed controls as 210r/min, and by the blending extrusion temperature of twin screw extruder from a district of district to eight, the temperature of machine neck and head is controlled as: 98 DEG C, a district, two 100 DEG C, districts, three 102 DEG C, districts, four 105 DEG C, districts, five 106 DEG C, districts, six 108 DEG C, districts, seven 110 DEG C, districts, eight 110 DEG C, districts, 112 DEG C, machine neck, head 112 DEG C, again successively through water ring pelletizing, dehydration and drying, obtain middle pressure water resistant tree cross-linked poly-ethylene cable material, polyolefine compound resin described in this step is made up of the Low Density Polyethylene taken by weight 80 parts and ethylene vinyl acetate 20 parts, the melting index of this Low Density Polyethylene is 2g/10min, and the mass percentage that ethylene vinyl acetate is vinyl acetate between to for plastic (VA) is 28%.
Embodiment 3:
A) polyethylene-silane grafted material is prepared, it is first the Low Density Polyethylene 85 parts of 2g/10min by the melting index taken by weight, 4 parts, vinyl-three (2-methoxy ethoxy) silane, the different benzene of peroxidation two 0.15 part and 4, 4'-thiobis (the 6-tertiary butyl-3-methylphenol) 3 parts drops into pre-mixing in stirred vessel, the rotating speed of stirred vessel controls as 250r/min, the time controling of pre-mixing is 6.5min, obtain polyethylene silicon alkylating mixture, then this polyethylene silicon alkylating mixture is carried out grafting by volume pump as passed through in Brabender metering system feeding to (being namely fed to) twin screw extruder to squeeze, the rotating speed that twin screw extruder grafting is extruded controls as 230r/min, and by the extrusion temperature of twin screw extruder from a district of district to eight, the temperature of machine neck and head is controlled as 120 DEG C, a district, two 135 DEG C, districts, three 145 DEG C, districts, four 155 DEG C, districts, five 165 DEG C, districts, six 178 DEG C, districts, seven 185 DEG C, districts, eight 190 DEG C, districts, 195 DEG C, machine neck, head 200 DEG C, again successively through water ring pelletizing, dehydration and drying, obtain melting index and be 2g/10min and silane is the polyethylene-silane grafted material of vinyl-three (2-methoxy ethoxy) silane, stand-by,
B) water resistant tree composite catalyzing master batch is prepared, be first 1.8g/10min Low Density Polyethylene 80 parts by the melting index taken by weight, four [β-(3, 5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester 2 parts, dinonylnaphthalene sulfonic acid 4 parts, dicumyl peroxide 0.15 part, cyanuric acid tripropylene 5 parts and premix in calcium stearate 12 parts of input whipping apptss, the stirring velocity of whipping appts controls as 300r/min, premix time controling is 5min, obtain miscellany (miscellany is mixture), then miscellany is carried out plasticizing as passed through in Brabender metering system feeding to (being namely fed to) twin screw extruder by volume pump to extrude, the rotating speed of extruding of twin screw extruder controls as 200r/min, and by the extrusion temperature of twin screw extruder from a district of district to eight, the temperature of machine neck and head is controlled as: 120 DEG C, a district, two 130 DEG C, districts, three 145 DEG C, districts, four 155 DEG C, districts, five 162 DEG C, districts, six 168 DEG C, districts, seven 175 DEG C, districts, eight 180 DEG C, districts, 185 DEG C, machine neck, head 190 DEG C, again successively through water ring pelletizing, dehydration and drying, obtain water resistant tree composite catalyzing master batch, stand-by,
C) finished product is prepared, the polyolefine compound resin 60 parts first will taken by weight, by steps A) the polyethylene-silane grafted material 20 parts that obtains, by step B) mix in the water resistant that obtains tree composite catalyzing master batch 10 parts and dicumyl peroxide 3.5 parts of input mixing machines, the mixing velocity of mixing machine controls as 325r/min, mixing time controls as 4min, obtain water resistant tree premixture, then by this water resistant tree premixture by volume pump as by carrying out blending extrusion in Brabender metering system feeding to twin screw extruder, blending extrusion rotating speed controls as 230r/min, and by the blending extrusion temperature of twin screw extruder from a district of district to eight, the temperature of machine neck and head is controlled as: 98 DEG C, a district, two 100 DEG C, districts, three 102 DEG C, districts, four 105 DEG C, districts, five 106 DEG C, districts, six 108 DEG C, districts, seven 110 DEG C, districts, eight 110 DEG C, districts, 112 DEG C, machine neck, head 112 DEG C, again successively through water ring pelletizing, dehydration and drying, obtain middle pressure water resistant tree cross-linked poly-ethylene cable material, polyolefine compound resin described in this step is made up of the Low Density Polyethylene taken by weight 70 parts and ethylene vinyl acetate 30 parts, the melting index of this Low Density Polyethylene is 1.8g/10min, and the mass percentage that ethylene vinyl acetate is vinyl acetate between to for plastic (VA) is 23%.
Comparative example:
Prepare 35KV that the trade mark is YJ-35 and following peroxide crosslinked polyethylene preparation method as follows: take Low Density Polyethylene 98 parts by weight, dicumyl peroxide 1.8 parts, 4, 4'-thiobis (the 6-tertiary butyl-3-methylphenol) 0.2 part drops into pre-mixing in stirred vessel, obtain mixture, then mixture is extruded by carrying out plasticizing in Brabender metering system feeding to twin screw extruder, it is 200r/min that rotating speed is extruded in control, the temperature of forcing machine is: 98 DEG C, a district, two 100 DEG C, districts, three 102 DEG C, districts, four 105 DEG C, districts, five 106 DEG C, districts, six 108 DEG C, districts, seven 110 DEG C, districts, eight 110 DEG C, districts, 112 DEG C, machine neck and head 112 DEG C, through water ring pelletizing, dehydration and drying obtain crosslinked polyethylene particle.
Press water resistant to set cross-linked poly-ethylene cable material in being obtained by above-described embodiment 1 to 3 and there is technical indicator shown in following table after tested:
As can be seen from the above table, every physical and mechanical properties and the electrical performance indexes of middle pressure water resistant tree cross-linked poly-ethylene cable material prepared according to the methods of the invention can reach JB/T10437-2004 necessary requirement, and comparative example and import material performance index close.But the length reduction more obvious than comparative example of water tree, reduction amplitude reaches 40%-50%, and this water tree resistant property of pressing water resistant to set cross-linked poly-ethylene cable material in showing to be prepared by the inventive method is very excellent.
Claims (10)
1. press water resistant to set a cross-linked poly-ethylene cable material in, it is characterized in that it is made up of the raw material of following proportioning by weight: polyolefine compound resin 60-75 part, polyethylene-silane grafted material 15-25 part, water resistant tree composite catalyzing master batch 5-10 part and linking agent 2-5 part; Described polyolefine compound resin is made up of the raw material of following proportioning by weight: Low Density Polyethylene 60-80 part and ethylene vinyl acetate 20-40 part; Described water resistant tree composite catalyzing master batch is made up of the raw material of following proportioning by weight: Low Density Polyethylene 70-80 part, catalyzer 3-5 part, nucleator 10-15 part, oxidation inhibitor 2-5 part, linking agent 0.1-0.2 part and additional crosslinker 3-5 part.
2. middle pressure water resistant tree cross-linked poly-ethylene cable material according to claim 1, is characterized in that described Low Density Polyethylene to be melting index is the Low Density Polyethylene of 1.8-2.2g/10min; Described ethylene vinyl acetate is the mass percentage of vinyl acetate between to for plastic is the ethylene vinyl acetate of 18-28%.
3. middle pressure water resistant tree cross-linked poly-ethylene cable material according to claim 1, it is characterized in that the melting index of described polyethylene-silane grafted material is 1.5-1.8g/min, and described silane is vinyl-three (2-methoxy ethoxy) silane.
4. middle pressure water resistant tree cross-linked poly-ethylene cable material according to claim 1, is characterized in that described catalyzer is one or more the combination in dinonylnaphthalene sulfonic acid, dinonylnaphthalene disulfonic acid, Witco 1298 Soft Acid; Described nucleator is Zinic stearas or calcium stearate.
5. middle pressure water resistant tree cross-linked poly-ethylene cable material according to claim 1, it is characterized in that described oxidation inhibitor is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, 4,4'-thiobis (the 6-tertiary butyl-3-methylphenol), 2,6-di-tert-butyl methyl phenol, (2,4-di-tert-butyl-phenyl) one or more combination in tris phosphite, β-positive octadecanol ester of (3,5-di-tert-butyl-hydroxy phenyl) propionic acid and Tyox B.
6. middle pressure water resistant tree cross-linked poly-ethylene cable material according to claim 1, is characterized in that described linking agent is one or more the combination in dicumyl peroxide, the dibenzoyl peroxide tert-butyl ester, dual-tert-butyl dicumyl peroxide; Described additional crosslinker is one or more mixtures in iso-cyanuric acid triallyl ester, triallyl cyanurate, trimethylolpropane trimethacrylate and Viscoat 295.
7. a preparation method for middle pressure water resistant tree cross-linked poly-ethylene cable material as claimed in claim 1, is characterized in that comprising the following steps:
A) polyethylene-silane grafted material is prepared, by the Low Density Polyethylene 80-90 part taken by weight, vinyl silanes 3-5 part, linking agent 0.1-0.2 part and oxidation inhibitor 2-4 part drop into pre-mixing in stirred vessel, and control rotating speed and the pre-mixing time of stirred vessel, obtain polyethylene silicon alkylating mixture, then this polyethylene silicon alkylating mixture is extruded by carrying out grafting in volume pump feeding to twin screw extruder, and control rotating speed that twin screw extruder grafting extrudes and extrusion temperature, through water ring pelletizing, dehydration and drying, obtain polyethylene-silane grafted material,
B) water resistant tree composite catalyzing master batch is prepared, the Low Density Polyethylene 70-80 part taken by weight, oxidation inhibitor 2-5 part, catalyzer 3-5 part, linking agent 0.1-0.2 part, additional crosslinker 3-5 part and nucleator 10-15 part drop into premix in whipping appts, and control stirring velocity and the premix time of whipping appts, obtain miscellany, then miscellany is extruded by carrying out plasticizing in volume pump feeding to twin screw extruder, what control twin screw extruder extrudes rotating speed and extrusion temperature, through water ring pelletizing, dehydration and drying, obtain water resistant tree composite catalyzing master batch,
C) finished product is prepared, by the polyolefine compound resin 60-75 part taken by weight, by steps A) polyethylene-silane grafted material 15-25 part of obtaining and by step B) water resistant tree composite catalyzing master batch 5-10 part of obtaining and linking agent 2-5 part drops in mixing machine and mixes, and control mixing velocity and the mixing time of mixing machine, obtain water resistant tree premixture, then this water resistant is set premixture by carrying out blending extrusion in volume pump feeding to twin screw extruder, control blending extrusion rotating speed and blending extrusion temperature, through water ring pelletizing, dehydration and drying, obtain middle pressure water resistant tree cross-linked poly-ethylene cable material, wherein: described polyolefine compound resin is made up of the Low Density Polyethylene 60-80 part taken by weight and ethylene vinyl acetate 20-40 part.
8. the preparation method of middle pressure water resistant tree cross-linked poly-ethylene cable material according to claim 7, is characterized in that steps A) described in Low Density Polyethylene be melting index be 1.8-2.2g/10min; Described vinyl silanes is vinyl-three (2-methoxy ethoxy) silane; Described linking agent is one or more the combination in dicumyl peroxide, the dibenzoyl peroxide tert-butyl ester, dual-tert-butyl dicumyl peroxide; Described oxidation inhibitor is four [β-(3,5-di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, 4,4'-thiobis (the 6-tertiary butyl-3-methylphenol), 2,6-di-tert-butyl methyl phenol, (2,4-di-tert-butyl-phenyl) one or more combination in tris phosphite, β-positive octadecanol ester of (3,5-di-tert-butyl-hydroxy phenyl) propionic acid and Tyox B.
9. the preparation method of middle pressure water resistant tree cross-linked poly-ethylene cable material according to claim 7, it is characterized in that steps A) described in the rotating speed of control stirred vessel and the pre-mixing time be that the rotating speed of stirred vessel is controlled as 200-300r/min, be 5-8min by the time controling of pre-mixing, the rotating speed that described control twin screw extruder grafting is extruded is that rotating speed twin screw extruder grafting extruded controls as 215-245r/min; Step B) described in the stirring velocity of control whipping appts and the premix time be that the stirring velocity of whipping appts is controlled as 200-300r/min, be 5-8min by the time controling of premix, the rotating speed of extruding of described control twin screw extruder controls as 190-210r/min by the rotating speed of extruding of twin screw extruder; Step C) described in the mixing velocity of control mixing machine and mixing time be that mixing velocity is controlled as 300-350r/min, mixing time controlled as 3-5min, the rotating speed of described control blending extrusion controls the rotating speed of blending extrusion for 210-230r/min.
10. the preparation method of middle pressure water resistant tree cross-linked poly-ethylene cable material according to claim 7, it is characterized in that steps A) described in control extrusion temperature be that the temperature of a district of district to eight of twin screw extruder, machine neck and head is controlled as 120 DEG C, a district, two 135 DEG C, districts, three 145 DEG C, districts, four 155 DEG C, districts, five 165 DEG C, districts, six 178 DEG C, districts, seven 185 DEG C, districts, eight 190 DEG C, districts, 195 DEG C, machine neck, head 200 DEG C; Step B) described in control extrusion temperature be that the temperature of a district of district to eight of twin screw extruder, machine neck and head is controlled as 120 DEG C, a district, two 135 DEG C, districts, three 145 DEG C, districts, four 155 DEG C, districts, five 162 DEG C, districts, six 168 DEG C, districts, seven 175 DEG C, districts, eight 180 DEG C, districts, 185 DEG C, machine neck, head 190 DEG C; Step C) described in control blending extrusion temperature be that the temperature of a district of district to eight of twin screw extruder, machine neck and head is controlled as: 98 DEG C, a district, two 100 DEG C, districts, three 102 DEG C, districts, four 105 DEG C, districts, five 106 DEG C, districts, six 108 DEG C, districts, seven 110 DEG C, districts, eight 110 DEG C, districts, 112 DEG C, machine neck, head 112 DEG C.
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