CN103319774A - Cross-linkable inorganic nano-LDPE (low-density polyethylene)/SiOx polymer composite material and preparation method thereof - Google Patents
Cross-linkable inorganic nano-LDPE (low-density polyethylene)/SiOx polymer composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a cross-linkable inorganic nano-LDPE (low-density polyethylene)/SiOx polymer composite material and a preparation method thereof. The cross-linkable inorganic nano-LDPE/SiOx polymer composite material comprises organic silicon sol, low-density polyethylene, a main antioxidant, an auxiliary antioxidant and a cross-linking agent, wherein the organic silicon sol is ethylene glycol silicon sol, the main antioxidant is pentaerythrite tetra (beta-(3,5-di-tert-butyl-4-hydroxyphenyl)-propionate), the auxiliary antioxidant is dilauryl thiodipropionate, and the cross-linking agent is dicumyl peroxide. The preparation method disclosed by the invention can solve the problems of poor dispersibility, serious particle agglomeration and the like of the existing preparation method of a polyolefin nano-composite material, a solvent-melt blending method is adopted for successfully preparing a cross-linkable SiOx/LDPE nano-cable material with the SiOx particle size of 55nm-100nm, the agglomeration of inorganic particles is effectively prevented, and the cross-linkable SiOx/LDPE nano-cable material is obviously better than a cross-linkable SiO2/LDPE nano-cable material as a control material.
Description
Technical field
The present invention relates to polymer inorganic nano composite material technical field, refer in particular to a kind of crosslinkable inorganic nano LDPE/ SiOx polymer composites and preparation method thereof.
Background technology
Compare with polyethylene, the crosslinkable polyethylene nano composite material has excellent electric property (high such as breaking down field strength, volume specific resistance is high) and mechanical property, has become one of focus of electric wire and cable material area research.Yet, inorganic nano-particle and polyethylene interfacial energy differ greatly, consistency is poor, easily produce secondary agglomeration, and, under high temperature fused state, mix the decomposition generation that easily causes linking agent crosslinked, be difficult to be prepared into the crosslinkable polyethylene nano composite material that nano level disperses, can not improve electric property and mechanical property.In order to make nano polythene composite material, usually adopt coupling agent that the inorganic nano-particle sub-surface is processed, to increase and poly consistency, melt blending, the preparation nano polythene composite material, because polyethylene viscosity is larger, the nanoparticle difficulties in dispersion, reunite more serious, easily the generation plumage is crosslinked when melting mixing to add simultaneously linking agent, affects performance, can not prepare crosslinkable Polyethylene Nanocomposites; Huang utilizes trimethoxy octane coupling agent treatment silicon-dioxide (SiO
2), then in the silicon oxide particle chloroform of toluene with processing, simultaneously, LLDPE is dissolved in 100 ℃ of xylene solvents, makes solution; Under 100 ℃, two kinds of solution mix, and use methanol extraction again, and 140 ℃, the nano polythene composite material of good dispersity is prepared in vacuum-drying, and disruptive strength and anti-electricity tree performance obviously improve.But should prepare complexity, can not prepare crosslinkable nano composite material, be difficult for realizing industrialization.
Summary of the invention
The purpose of this invention is to provide a kind of crosslinkable inorganic nano LDPE/ SiOx polymer composites and preparation method thereof.
The objective of the invention is to realize as follows: a kind of crosslinkable inorganic nano LDPE/ SiOx polymer composites and preparation method thereof, comprise organic silicon sol, Low Density Polyethylene, primary antioxidant, auxiliary antioxidant and linking agent, described organic silicon sol is the ethylene glycol silicon sol, primary antioxidant is four [β-(3,5-di-t-butyl 4-hydroxy phenyl) propionic acid] pentaerythritol ester, auxiliary antioxidant is the thio-2 acid dilaurate, and linking agent is dicumyl peroxide;
At first, be that the organic silicon sol of 5-15wt%, the Low Density Polyethylene that mass percent is 90-97wt%, the primary antioxidant of mass percent 0.1-0.4wt% and the auxiliary antioxidant of mass percent 0.2-0.8wt% mix in high-speed mixer with total mass percentage ratio;
Then, the material that mixes is adopted molten-molten blending method through the twin screw degassing extruder further heat up vacuum outgas, extrude, that melting enters in the single screw extrusion machine again is degassed, extrude, earnestly granulation, air-cooled, obtains LDPE/ SiO
xThe nano composite material particle;
At last, then with SiO
x/ LDPE nano composite material particle is that the 1.8-2.2wt% linking agent mixes infiltration 30min under 50-80 ℃ of temperature with mass percent, becomes crosslinkable SiO by the linking agent diffusion
x/ LDPE nano-cable material.
The invention has the beneficial effects as follows: the problems such as the present invention has overcome the bad dispersibility that existing preparation olefin polymerization nanometer composite material exists, and particle aggregation is serious have proposed a kind of novel method for preparing the crosslinkable polyolefin nano composite material simultaneously; Adopt the SiO that made of molten-molten blending method success
xSize of particles is the crosslinkable SiO of 55nm ~ 100nm
x/ LDPE nano-cable material has effectively prevented the reunion of inorganic particulate, significantly better than crosslinkable SiO
2The contrast of/LDPE nano-cable material.Add SiO
xNanoparticle energy Effective Raise electrical property; Work as SiO
xWhen addition was 1.5wt%, over-all properties was best, particle diameter 60-90nm, crosslinkable SiO
2/ LDPE nano-cable material has improved 82.6% with the volume specific resistance that pure LDPE compares, and the breaking down field strength of material, tensile strength, elongation at break and Young's modulus have improved respectively 14.3%, 12.5%, 35.2% and 23.8%.
Embodiment:
Crosslinkable inorganic nano LDPE/ SiOx polymer composites that following examples obtain and preparation method thereof, comprise organic silicon sol, Low Density Polyethylene, primary antioxidant, auxiliary antioxidant and linking agent, described organic silicon sol is the ethylene glycol silicon sol, primary antioxidant is four [β-(3,5-di-t-butyl 4-hydroxy phenyl) propionic acid] pentaerythritol ester, auxiliary antioxidant is the thio-2 acid dilaurate, and linking agent is dicumyl peroxide;
At first, be that the organic silicon sol of 5-15wt%, the Low Density Polyethylene that mass percent is 90-97wt%, the primary antioxidant of mass percent 0.1-0.4wt% and the auxiliary antioxidant of mass percent 0.2-0.8wt% mix in high-speed mixer with total mass percentage ratio;
Then, the material that mixes is adopted molten-molten blending method through the twin screw degassing extruder further heat up vacuum outgas, extrude, that melting enters in the single screw extrusion machine again is degassed, extrude, earnestly granulation, air-cooled, obtains LDPE/ SiO
xThe nano composite material particle;
At last, then with LDPE/ SiO
xThe nano composite material particle is that the 1.8-2.2wt% linking agent mixes infiltration 30min under 50-80 ℃ of temperature with mass percent, becomes crosslinkable SiO by the linking agent diffusion
x/ LDPE nano-cable material.
The preparation method of organic silicon sol: adopt in four-hole bottle, to add 50ml tetraethoxy (TEOS), be heated with stirring to 120-140 ℃, behind temperature-stable, in TEOS, drip Organic Alcohol with every 3-9s of rate of addition, the mol ratio of Organic Alcohol and TEOS is 1.9, reaction times 2-8h, obtaining boiling point 120-160 ℃, solids content is the 20-37wt% organic silicon sol.
Because the high boiling point silicon sol is close with the polyethylene melt temperature, favourable mixing each other in the degassed process that further heats up, has silicon sol to form homodisperse SiO in polyethylene melt
xNanoparticle, thereby will form the SiO that is evenly distributed
x/ LDPE nano composite material; Because the solid linking agent is melt into liquid more than 50 ℃, with nano composite material, the molecular diffusion effect crosslinked by liquid state infiltrates, and prepares crosslinkable SiO
x/ LDPE nano-cable material.
Embodiment 1
Take by weighing 192gLDPE, 10g solids content 20% organic silicon sol (actual solid SiO
xAccount for the mass percent 1.0% of whole matrix material), 0.6g primary antioxidant, 1.4g auxiliary antioxidant mix in mixing machine; With the principle of mixing through twin screw extruder melt extrude, after the exhaust, again through single screw rod exhaust, cool off, be a granulated into the nano composite material particle; This matrix material is mixed 30min with 80 ℃ of 4g linking agent intensifications in mixing machine, make crosslinkable SiO
x/ LDPE nano-cable material is sample 1.
To add the SiO of 50nm
2Inorganic nano SiOx/LDPE and LDPE prepare the crosslinkable CABLE MATERIALS in contrast.The SiO2 inorganic nano SiOx/LDPE, 0.6g primary antioxidant, the 1.4g auxiliary antioxidant that take by weighing 192gLDPE, 2g 50nm mix in mixing machine; With the principle of mixing through twin screw extruder melt extrude, after the exhaust, again through single screw rod exhaust, cool off, be a granulated into the nano composite material particle; This matrix material is mixed 30min with 80 ℃ of 4g linking agent intensifications in mixing machine, make crosslinkable SiO
2/ LDPE nano-cable material is sample 2.
With the crosslinkable CABLE MATERIALS of plus nano silicon oxide inorganic particulate not in contrast.Taking by weighing 192gLDPE, 0.6g primary antioxidant, 1.4g auxiliary antioxidant mixes in mixing machine; With the principle of mixing through twin screw extruder melt extrude, after the exhaust, again through single screw rod exhaust, cool off, be a granulated into the nano composite material particle; This matrix material is mixed 30min with 80 ℃ of 4g linking agent intensifications in mixing machine, making crosslinkable LDPE nano-cable material is sample 3.
HT-100 breakdown voltage testers that the voltage breakdown test adopts the Zhejiang Univ to make, sample: square sheet specimens, size 100mm * 100mm, thickness is 1mm approximately.Electrode: circular on-gauge plate-plate copper electrode, electrode diameter 25mm.Boosting mode: boost continuously.The rate of rise: 10kV/s.
ZC-36 meggers that the volume specific resistance test adopts Shanghai City the 6th ammeter factory to make.Test sample is of a size of 100mm * 100mm, and thickness is about the square plate tensile sample of 1mm.Electrode materials applies electric field 500V/mm for the annealing aluminium foil.Measure the volume specific resistance of sample according to GB 1410-89.
The AG-J10 KN electronic universal material testing machine that Mechanics Performance Testing adopts Japanese Shimadzu company to make; Material is hot pressed into the print of 10cm * 10cm * 1mm under vulcanizing press, dumbbell shape batten with reference to GB/ T1040-92 standard preparation standard, sample basic size is 100mm * 6mm * 1mm, maximum pull is 500N, draw speed is 200mm/min, the Young's modulus of test material, tensile strength and elongation at break.
Heat is extended the index of expression degree of crosslinking, the hot elongation test instrument of WSK-49b that its test adopts Jiangdu, Jiangsu experimental machine factory to make; Test after preparing sample and measure sectional area with reference to the GB/T2951.1 test method.The dumbbell thickness of test piece should be not less than 0.8mm, is not more than 2.0mm.
The FEI Sirion 200 scanning electron microscope analysis instrument (SEM) that the dispersion particle diameter test of inorganic particulate adopts Dutch PHILIPS Co. to make are observed the SiO of fracture
xSize of particles.At first with sample brittle failure in liquid nitrogen, the test after the brittle failure is fixed on the stainless steel sample table with conductive resin, utilizes the spraying plating instrument, at Fracture Profile in Metallic Materials place metal spraying.
The breaking down field strength of the crosslinkable polyethylene cable material for preparing, volume specific resistance and mechanical property and other performance number values see Table 1:
Table 1 breaking down field strength, volume specific resistance, mechanical property and other the performance test results
T
| Sample number into spectrum | Sample 1 | Sample 2 | Sample 3 |
| Breaking down field strength/kV/mm | 27.8 | 25.7 | 25.1 |
| Volume specific resistance/Ω m (* 10 15) | 2.64 | 2.22 | 1.95 |
| Tensile strength/MPa | 13.4 | 10.9 | 11.2 |
| Elongation at break/% | 889.4 | 592.1.4 | 634.8 |
| Young's modulus/Nmm -2 | 156.8 | 136.7 | 126.0 |
| Heat extension/% | 75 | 80 | 78 |
| The dispersion particle diameter (nm) of inorganic particulate | 55-96 | 80-180 | 0 |
Table 1
Embodiment 2:
Take by weighing 191gLDPE, 15g solids content 20% organic silicon sol (actual solid SiO
xAccount for the mass percent 1.5% of whole matrix material), 0.6g primary antioxidant, 1.4g auxiliary antioxidant mix in mixing machine; With the principle of mixing through twin screw extruder melt extrude, after the exhaust, again through single screw rod exhaust, cool off, be a granulated into the nano composite material particle; This matrix material is mixed 30min with 80 ℃ of 4g linking agent intensifications in mixing machine, make crosslinkable SiO
x/ LDPE nano-cable material is sample 4.
To add the SiO of 50nm
2Inorganic nano SiOx/LDPE and LDPE prepare the crosslinkable CABLE MATERIALS in contrast.The SiO2 inorganic nano SiOx/LDPE, 0.6g primary antioxidant, the 1.4g auxiliary antioxidant that take by weighing 192gLDPE, 3g 50nm mix in mixing machine; With the principle of mixing through twin screw extruder melt extrude, after the exhaust, again through single screw rod exhaust, cool off, be a granulated into the nano composite material particle; This matrix material is mixed 30min with 80 ℃ of 4g linking agent intensifications in mixing machine, make crosslinkable SiO
2/ LDPE nano-cable material is sample 5.
With the crosslinkable CABLE MATERIALS of plus nano silicon oxide inorganic particulate not in contrast.With sample 3.
HT-100 breakdown voltage testers that the voltage breakdown test adopts the Zhejiang Univ to make, sample: square sheet specimens, size 100mm * 100mm, thickness is 1mm approximately.Electrode: circular on-gauge plate-plate copper electrode, electrode diameter 25mm.Boosting mode: boost continuously.The rate of rise: 10kV/s.
ZC-36 meggers that the volume specific resistance test adopts Shanghai City the 6th ammeter factory to make.Test sample is of a size of 100mm * 100mm, and thickness is about the square plate tensile sample of 1mm.Electrode materials applies electric field 500V/mm for the annealing aluminium foil.Measure the volume specific resistance of sample according to GB 1410-89.
The AG-J10 KN electronic universal material testing machine that Mechanics Performance Testing adopts Japanese Shimadzu company to make; Material is hot pressed into the print of 10cm * 10cm * 1mm under vulcanizing press, dumbbell shape batten with reference to GB/ T1040-92 standard preparation standard, sample basic size is 100mm * 6mm * 1mm, maximum pull is 500N, draw speed is 200mm/min, the Young's modulus of test material, tensile strength and elongation at break.
Heat is extended the index of expression degree of crosslinking, the hot elongation test instrument of WSK-49b that its test adopts Jiangdu, Jiangsu experimental machine factory to make; Test after preparing sample and measure sectional area with reference to the GB/T2951.1 test method.The dumbbell thickness of test piece should be not less than 0.8mm, is not more than 2.0mm.
The FEI Sirion 200 scanning electron microscope analysis instrument (SEM) that the dispersion particle diameter test of inorganic particulate adopts Dutch PHILIPS Co. to make are observed the SiO of fracture
xSize of particles.At first with sample brittle failure in liquid nitrogen, the test after the brittle failure is fixed on the stainless steel sample table with conductive resin, utilizes the spraying plating instrument, at Fracture Profile in Metallic Materials place metal spraying.
The breaking down field strength of the crosslinkable polyethylene cable material for preparing, volume specific resistance and mechanical property and other performance number values see Table 2:
Table 2 breaking down field strength, volume specific resistance, mechanical property and other the performance test results
T
| Sample number into spectrum | Sample 4 | Sample 5 | Sample 3 |
| Breaking down field strength/kV/mm | 28.7 | 25.7 | 25.1 |
| Volume specific resistance/Ω m (* 10 15) | 3.56 | 2.22 | 1.95 |
| Tensile strength/MPa | 12.6 | 10.2 | 11.2 |
| Elongation at break/% | 858.5 | 508.2 | 634.8 |
| Young's modulus/Nmm -2 | 139.0 | 127.9 | 126.0 |
| Heat extension/% | 77 | 81 | 78 |
| The dispersion particle diameter (nm) of inorganic particulate | 55-90 | 80-180 | 0 |
Table 2
Embodiment 3:
Take by weighing 190gLDPE, 20g solids content 20% organic silicon sol (actual solid SiO
xAccount for the mass percent 1.5% of whole matrix material), 0.6g primary antioxidant, 1.4g auxiliary antioxidant mix in mixing machine; With the principle of mixing through twin screw extruder melt extrude, after the exhaust, again through single screw rod exhaust, cool off, be a granulated into the nano composite material particle; This matrix material is mixed 30min with 80 ℃ of 4g linking agent intensifications in mixing machine, make crosslinkable SiO
x/ LDPE nano-cable material is sample 6.
To add the SiO of 50nm
2Inorganic nano SiOx/LDPE and LDPE prepare the crosslinkable CABLE MATERIALS in contrast.The SiO2 inorganic nano SiOx/LDPE, 0.6g primary antioxidant, the 1.4g auxiliary antioxidant that take by weighing 190gLDPE, 4g 50nm mix in mixing machine; With the principle of mixing through twin screw extruder melt extrude, after the exhaust, again through single screw rod exhaust, cool off, be a granulated into the nano composite material particle; This matrix material is mixed 30min with 80 ℃ of 4g linking agent intensifications in mixing machine, make crosslinkable SiO
2/ LDPE nano-cable material is sample 7.
With the crosslinkable CABLE MATERIALS of plus nano silicon oxide inorganic particulate not in contrast.With sample 3.
HT-100 breakdown voltage testers that the voltage breakdown test adopts the Zhejiang Univ to make, sample: square sheet specimens, size 100mm * 100mm, thickness is 1mm approximately.Electrode: circular on-gauge plate-plate copper electrode, electrode diameter 25mm.Boosting mode: boost continuously.The rate of rise: 10kV/s.
ZC-36 meggers that the volume specific resistance test adopts Shanghai City the 6th ammeter factory to make.Test sample is of a size of 100mm * 100mm, and thickness is about the square plate tensile sample of 1mm.Electrode materials applies electric field 500V/mm for the annealing aluminium foil.Measure the volume specific resistance of sample according to GB 1410-89.
The AG-J10 KN electronic universal material testing machine that Mechanics Performance Testing adopts Japanese Shimadzu company to make; Material is hot pressed into the print of 10cm * 10cm * 1mm under vulcanizing press, dumbbell shape batten with reference to GB/ T1040-92 standard preparation standard, sample basic size is 100mm * 6mm * 1mm, maximum pull is 500N, draw speed is 200mm/min, the Young's modulus of test material, tensile strength and elongation at break.
Heat is extended the index of expression degree of crosslinking, the hot elongation test instrument of WSK-49b that its test adopts Jiangdu, Jiangsu experimental machine factory to make; Test after preparing sample and measure sectional area with reference to the GB/T2951.1 test method.The dumbbell thickness of test piece should be not less than 0.8mm, is not more than 2.0mm.
The FEI Sirion 200 scanning electron microscope analysis instrument (SEM) that the dispersion particle diameter test of inorganic particulate adopts Dutch PHILIPS Co. to make are observed the SiO of fracture
xSize of particles.At first with sample brittle failure in liquid nitrogen, the test after the brittle failure is fixed on the sample table (stainless steel) with conductive resin, utilizes the spraying plating instrument, at Fracture Profile in Metallic Materials place metal spraying.
The breaking down field strength of the crosslinkable polyethylene cable material for preparing, volume specific resistance and mechanical property and other performance number values see Table 3:
Table 3 breaking down field strength, volume specific resistance, mechanical property and other the performance test results
T
| Sample number into spectrum | Sample 6 | Sample 7 | Sample 3 |
| Breaking down field strength/kV/mm | 26.8 | 24.7 | 25.1 |
| Volume specific resistance/Ω m (* 10 15) | 3.35 | 2.64 | 1.95 |
| Tensile strength/MPa | 11.3 | 9.3 | 11.2 |
| Elongation at break/% | 692.6 | 504.4 | 634.8 |
| Young's modulus/Nmm -2 | 141.8 | 123.6 | 126.0 |
| Heat extension/% | 81 | 85 | 78 |
| The dispersion particle diameter (nm) of inorganic particulate | 60-100 | 80-200 | 0 |
Table 3
The breaking down field strength of crosslinkable polyethylene cable material, volume specific resistance and mechanical property and other performance brief summaries.
Claims (1)
1. crosslinkable inorganic nano LDPE/ SiOx polymer composites and preparation method thereof, it is characterized in that, comprise organic silicon sol, Low Density Polyethylene, primary antioxidant, auxiliary antioxidant and linking agent, described organic silicon sol is the ethylene glycol silicon sol, primary antioxidant is four [β-(3,5-di-t-butyl 4-hydroxy phenyl) propionic acid] pentaerythritol ester, auxiliary antioxidant is the thio-2 acid dilaurate, linking agent is dicumyl peroxide;
At first, be that the organic silicon sol of 5-15wt%, the Low Density Polyethylene that mass percent is 90-97wt%, the primary antioxidant of mass percent 0.1-0.4wt% and the auxiliary antioxidant of mass percent 0.2-0.8wt% mix in high-speed mixer with total mass percentage ratio;
Then, the material that mixes is adopted molten-molten blending method through the twin screw degassing extruder further heat up vacuum outgas, extrude, that melting enters in the single screw extrusion machine again is degassed, extrude, earnestly granulation, air-cooled, obtains LDPE/ SiO
xThe nano composite material particle;
At last, then with LDPE/ SiO
xThe nano composite material particle is that the 1.8-2.2wt% linking agent mixes infiltration 30min under 50-80 ℃ of temperature with mass percent, becomes crosslinkable LDPE/SiO by the linking agent diffusion
xThe nano-cable material.
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| CN101445627A (en) * | 2008-12-11 | 2009-06-03 | 上海交通大学 | High-voltage DC cable insulating material and a preparation method thereof |
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| CN101445627A (en) * | 2008-12-11 | 2009-06-03 | 上海交通大学 | High-voltage DC cable insulating material and a preparation method thereof |
| CN102276901A (en) * | 2011-07-19 | 2011-12-14 | 哈尔滨理工大学 | Method for preparing ultraclean crosslinkable polyethylene insulation material of high-voltage cable |
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