CN110615969B - Anti-aging and flame-retardant epoxy resin cable insulating material and preparation thereof - Google Patents
Anti-aging and flame-retardant epoxy resin cable insulating material and preparation thereof Download PDFInfo
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- CN110615969B CN110615969B CN201910747321.0A CN201910747321A CN110615969B CN 110615969 B CN110615969 B CN 110615969B CN 201910747321 A CN201910747321 A CN 201910747321A CN 110615969 B CN110615969 B CN 110615969B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
- C07F9/02—Phosphorus compounds
- C07F9/547—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
- C07F9/6564—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms
- C07F9/6571—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms having phosphorus and oxygen atoms as the only ring hetero atoms
- C07F9/657163—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms having phosphorus and oxygen atoms as the only ring hetero atoms the ring phosphorus atom being bound to at least one carbon atom
- C07F9/657172—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms having phosphorus and oxygen atoms as the only ring hetero atoms the ring phosphorus atom being bound to at least one carbon atom the ring phosphorus atom and one oxygen atom being part of a (thio)phosphinic acid ester: (X = O, S)
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5033—Amines aromatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/504—Amines containing an atom other than nitrogen belonging to the amine group, carbon and hydrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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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
- H01B3/40—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 epoxy resins
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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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
- C08K3/30—Sulfur-, selenium- or tellurium-containing compounds
- C08K2003/3045—Sulfates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- 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
Abstract
The invention relates to the field of cable materials, in particular to an anti-aging and flame-retardant epoxy resin cable insulating material and a preparation method thereof, wherein the cable insulating material comprises the following components in parts by weight: 100-150 parts of epoxy resin composition, 50-70 parts of curing agent shown in formula (I), 20-30 parts of asbestos fiber, 20-25 parts of silicon dioxide, 10-20 parts of titanium dioxide, 10-20 parts of aluminum oxide, 4-7 parts of bentonite, 2-3 parts of talcum powder and 2-4 parts of barium sulfate, the cable insulation material has good mechanical property and excellent ageing resistance and flame retardant property,
Description
Technical Field
The invention relates to the field of cable materials, in particular to an anti-aging and flame-retardant epoxy resin cable insulating material and a preparation method thereof.
Technical Field
The cable insulation material is a necessary basic component for forming the cable, ensures that current or electromagnetic waves and light waves transmitted by the conductor wire core only flow along the lead and do not flow to the outside, and simultaneously ensures the safety of external objects and people. At present, the main materials used for preparing the cable insulating material are two main types of organic polymer materials, namely plastics and rubber, wherein the plastics such as polyvinyl chloride plastics and crosslinked polyethylene plastics have poor flame retardant property; the rubber such as ethylene propylene rubber material, silicon rubber material, etc. has general flame retardant and mechanical properties.
The epoxy resin is an important thermosetting resin, is a matrix resin which is most widely applied in polymer composite materials, and has the advantages of excellent wear resistance, mechanical property, electrical insulation property, chemical stability, high and low temperature resistance, low shrinkage, easiness in processing and forming, low cost and the like, so that the development of epoxy resin cable insulation materials has great application prospect.
Disclosure of Invention
The invention aims to provide an anti-aging flame-retardant epoxy resin cable insulation material which has good mechanical properties and excellent anti-aging flame-retardant properties.
The invention also aims to provide a preparation method of the anti-aging flame-retardant epoxy resin cable insulation material.
In order to achieve the purpose, the invention provides the following technical scheme:
on one hand, the invention provides an anti-aging and flame-retardant epoxy resin cable insulation material which comprises the following components in parts by weight: 100-150 parts of epoxy resin composition, 50-70 parts of curing agent shown in formula (I), 20-30 parts of asbestos fiber, 20-25 parts of silicon dioxide, 10-20 parts of titanium dioxide, 10-20 parts of aluminum oxide, 4-7 parts of bentonite, 2-3 parts of talcum powder and 2-4 parts of barium sulfate.
In some preferred embodiments, the anti-aging, flame retardant epoxy resin cable insulation material according to the present invention comprises, by weight: 100-120 parts of epoxy resin composition, 50-60 parts of curing agent shown in formula (I), 20-30 parts of asbestos fiber, 20-25 parts of silicon dioxide, 10-20 parts of titanium dioxide, 10-20 parts of aluminum oxide, 4-7 parts of bentonite, 2-3 parts of talcum powder and 2-4 parts of barium sulfate.
In other preferred embodiments, the anti-aging, flame retardant epoxy resin cable insulation according to the present invention comprises, by weight: 100 parts of epoxy resin composition, 50 parts of curing agent shown in formula (I), 30 parts of asbestos fiber, 20 parts of silicon dioxide, 15 parts of titanium dioxide, 15 parts of alumina, 4-7 parts of bentonite, 2-3 parts of talcum powder and 2-4 parts of barium sulfate.
According to the anti-aging flame-retardant epoxy resin cable insulating material, the epoxy resin composition is a composition of bisphenol A or bisphenol F epoxy resin and acrylic acid modified organosilicon epoxy resin; preferably, the epoxy resin composition is a composition of bisphenol A or bisphenol F epoxy resin and acrylic modified organic silicon epoxy resin, and the mass of the acrylic modified organic silicon epoxy resin accounts for 30-40% of the mass of the total epoxy resin composition; further preferably, the epoxy resin composition is a composition of bisphenol A or bisphenol F epoxy resin and acrylic modified silicone epoxy resin, and the mass of the acrylic modified silicone epoxy resin accounts for 30% of the total mass of the epoxy resin composition. The inventor finds that when the addition of the acrylic modified organic silicon epoxy resin in the matrix material is helpful for improving the flame retardant property of the insulating material, but the amount of the acrylic modified organic silicon epoxy resin is not more than 40 percent of the total mass of the epoxy resin composition, the impact strength of the prepared insulating material is not more than 20KJ/m2In order to obtain the best service performance, the mass of the acrylic modified organic silicon epoxy resin is preferably 30-40% of the total mass of the epoxy resin composition.
According to the anti-aging flame-retardant epoxy resin cable insulating material, the weight ratio of the epoxy resin composition to the curing agent shown in the formula I is 1: 1-3: 1; preferably, the weight ratio of the epoxy resin composition to the curing agent shown in formula I is 2: 1. The inventor also finds that when the weight ratio of the epoxy resin composition to the curing agent shown in the formula I is higher than 3:1, the flame retardant performance is not high, and the limiting oxygen index is not higher than 20, while when the weight ratio of the epoxy resin composition to the curing agent shown in the formula I is lower than 1:1, the tensile strength is not higher than 45MPa, and when the weight ratio of the epoxy resin composition to the curing agent shown in the formula I is 2: 1-3: 1, good flame retardant performance and good mechanical performance can be simultaneously obtained.
According to the anti-aging flame-retardant epoxy resin cable insulating material, the acrylic acid modified organic silicon epoxy resin is prepared by taking 1, 3-bis (3-glycidoxypropyl) -1,1,3, 3-tetramethyldisiloxane as a matrix, dripping 5-10% by mass of acrylic acid, and reacting at 100-110 ℃ until the acid value is less than or equal to 3 mgKOH/g.
The preparation method of the compound shown in the formula (I) of the anti-aging and flame-retardant epoxy resin cable insulation material comprises the following steps:
step (1): vinyl dimethylchlorosilane reacts with methyl 2-amino-5-nitrobenzoate to produce a compound of formula a;
step (2): reacting the compound of the formula a with DOPO to prepare a compound of a formula b;
and (3): hydrolyzing the compound of the formula b to obtain a compound of a formula c;
and (4): reacting the compound shown in the formula c with 2, 4-dihydroxy benzophenone to obtain a compound shown in a formula d;
and (5): reduction of a compound of formula d to produce a compound of formula I, the reaction equation is as follows:
in a second aspect, the invention provides a preparation method of the anti-aging flame-retardant epoxy resin cable insulation material, which comprises the following steps:
step (1): placing silicon dioxide, titanium dioxide, aluminum oxide, bentonite, talcum powder and barium sulfate with the formula ratio in a high-speed mixer, and stirring for 5min at the rotating speed of 800 r/min;
step (2): adding a curing agent shown in the formula (I), and continuously stirring and stirring at the rotating speed of 800r/min for 5 min;
and (3): placing the mixed material obtained in the step (2) in an internal mixer, carrying out internal mixing for 4-6 min at 115-135 ℃, then transferring the mixed material into an open mill, carrying out thin-passing for 5-6 times, rolling, and cooling for 7-9 h at room temperature to obtain a primary mixed material;
and (4): putting the primary mixed material obtained in the step (3) and the epoxy resin composition with the formula amount into an internal mixer, carrying out internal mixing at 95-105 ℃ for 2-3 min, then transferring into an open mill, thinly passing through the open mill for 5-6 times, and rolling to obtain a secondary mixed material;
and (5): and (3) pouring the secondary mixed material obtained in the step (4) into a sheath screw extruder for melt blending, and extruding the mixture on a cable core, wherein the extrusion temperature is 185-200 ℃.
According to the anti-aging and flame-retardant epoxy resin cable insulation material, on one hand, flame-retardant and anti-aging elements are uniformly introduced into matrix molecules, so that the use performance of the material is greatly improved, and on the other hand, a proper amount of silicon dioxide, titanium dioxide, aluminum oxide and the like are added by adopting a specific formula, so that the excellent mechanical properties of epoxy resin are kept, and meanwhile, the heat resistance and the flame retardance of the material are further improved.
Detailed Description
EXAMPLE 1 preparation of the curing agent of formula I
Step 1: weighing 11.30g of 2-amino-5-nitrobenzoic acid methyl ester into a reaction bottle, adding 60mL of tetrahydrofuran and 30mL of triethylamine to dissolve, dropwise adding 10mL of tetrahydrofuran solution dissolved with 12.05g of vinyl dimethylchlorosilane at room temperature, stirring at 45 ℃ overnight after completing the reaction, cooling to room temperature, adding 80mL of water, extracting with dichloromethane (3 x 50mL), combining dichloromethane layers, drying with anhydrous sodium sulfate, filtering, and evaporating the solvent under reduced pressure to obtain the compound shown in the formula a, wherein the compound is directly used in the next step, ES: M/Z281 [ M + H]+；
Step 2: weighing 5g of DOPO in a reaction bottle, adding 7.2g of the compound of the formula a obtained in the step 1 and 80ml of dioxane, carrying out reflux reaction for 10 hours under the protection of nitrogen, cooling to room temperature after the reaction is finished, evaporating the solvent under reduced pressure, and carrying out column chromatography purification to obtain a compound of the formula b, ES: M/Z497 [ M + H]+；1H NMR(600MHz,CDCl3)(δ,ppm):8.36～8.34(m,1H),8.24～8.22(m,1H),7.98～7.96(m,1H),7.80～7.79(m,1H),7.67～7.65(m,1H),7.55～7.53(m,1H),7.42～7.40(m,1H),7.25～7.24(m,1H),7.09～7.07(m,1H),7.01～7.00(m,2H),4.05(s,1H),3.90(s,3H),1.85～1.83(m,2H),1.05～1.04(m,2H),0.09(s,6H)；
Step 3, weighing 4.2g of the compound of the formula b obtained in the step 2, putting the compound into a reaction bottle, adding 20mL of 40% sodium hydroxide aqueous solution, stirring for 2h at 70 ℃, cooling to room temperature after the reaction is finished, adjusting the pH to about 7 by 1M hydrochloric acid, adding dichloromethane for extraction (3X 20mL), combining a plurality of layers, drying by anhydrous sodium sulfate, filtering, evaporating the solvent under reduced pressure, and weighting the residue by methanolCrystallizing to obtain the compound of formula c; ES: M/Z483 [ M + H]+；1H NMR(600MHz,CDCl3)(δ,ppm):11.88(br,1H),8.59～8.57(m,1H),8.38～8.37(m,1H),7.97～7.96(m,1H),7.83～7.81(m,1H),7.66～7.65(m,1H),7.55～7.53(m,1H),7.42～7.40(m,1H),7.25～7.24(m,1H),7.09～7.07(m,1H),7.01～7.00(m,2H),4.05(s,1H),1.88～1.86(m,2H),1.10～1.09(m,2H),0.09(s,6H)；
And 4, step 4: weighing 2g of the compound of the formula c obtained in the step 3, adding 30mL of thionyl chloride and 2mL of DMF (dimethyl formamide), heating and refluxing for 2h, and evaporating the solvent under reduced pressure for later use; weighing 3.5g of 2, 4-dihydroxy benzophenone in a reaction bottle, adding 3mL of triethylamine and 20mL of tetrahydrofuran, slowly dropwise adding 15mL of tetrahydrofuran solution dissolved with acyl chloride obtained in the previous step at 0-5 ℃, continuously stirring for 4h at 0-10 ℃, after the reaction is finished, adding 30mL of water, extracting with dichloromethane (3 x 50mL), drying with anhydrous sodium sulfate, and purifying by column chromatography to obtain a compound shown in the formula d; ES: M/Z679 [ M + H ]]+；1H NMR(600MHz,CDCl3)(δ,ppm):8.53～8.52(m,1H),8.28～8.26(m,1H),7.98～7.97(m,1H),7.80～7.78(m,1H),7.70～7.68(m,2H),7.65～7.63(m,1H),7.58～7.56(m,2H),7.52～7.50(m,3H),7.40～7.38(m,1H),7.24～7.22(m,1H),7.08～7.03(m,5H),5.36(s,1H),4.10(s,1H),1.84～1.82(m,2H),1.05～1.04(m,2H),0.09(s,6H)；
And 5: weighing 1.0g of the compound of the formula d obtained in example 4, adding 50ml of ethanol, 0.5g of reduced iron powder and 5ml of hydrochloric acid into a reaction bottle, carrying out reflux reaction for 2 hours, cooling to room temperature after the reaction is finished, pouring the reaction solution into ice water, adding sodium bicarbonate to adjust the pH value to be neutral, carrying out suction filtration, extracting the filtrate with dichloromethane (30ml × 3), drying with anhydrous sodium sulfate, filtering, and carrying out column chromatography purification to obtain a standard compound; ES: M/Z649 [ M + H ]]+；1H NMR(600MHz,CDCl3)(δ,ppm):7.96～7.95(m,1H),7.83～7.81(m,1H),7.78～7.77(m,2H),7.68～7.67(m,1H),7.64～7.62(m,2H),7.59～7.57(m,3H),7.40～7.39(m,1H),7.24～7.22(m,1H),7.08～7.03(m,51H),6.68～6.66(m,1H),6.55～6.54(m,1H),6.27(br,2H),5.35(s,1H),4.10(s,1H),1.84～1.82(m,2H),1.05～1.04(m,2H),0.09(s,6H)。
EXAMPLE 2 preparation of anti-aging, flame retardant insulation
Placing silicon dioxide, titanium dioxide, aluminum oxide, bentonite, talcum powder and barium sulfate in a table 1 in a high-speed mixer, stirring for 5min at the rotating speed of 800r/min, adding a curing agent shown in a formula (I) in the table 1 in a formula amount, and continuously stirring for 5min at the rotating speed of 800 r/min; placing the obtained mixed material into an internal mixer, carrying out internal mixing for 4-6 min at 115-135 ℃, then transferring into an open mill, carrying out thin-passing for 5-6 times of rolling, and cooling for 7-9 h at room temperature to obtain a primary mixed material; putting the obtained primary mixed material and the epoxy resin composition with the formula amount in the table 1 into an internal mixer, carrying out internal mixing at 95-105 ℃ for 2-3 min, then transferring into an open mill, thinly passing through the mixer for 5-6 times, and rolling to obtain a secondary mixed material; finally, pouring the obtained secondary mixed mixture into a sheath screw extruder for melt blending, extruding and molding on the cable core at the extrusion temperature of 185-200 ℃,
TABLE 1
The insulation materials of examples 2a-2f were tested for performance and the results are shown in table 2,
TABLE 2
| Examples | Impact Strength (KJ/m)2) | Tensile Strength (MPa) | UL-94 flame retardant rating | Oxygen index |
| Example 2a | 30 | 89 | V-0 | 37 |
| Example 2b | 28 | 85 | V-0 | 36 |
| Example 2c | 29 | 87 | V-0 | 39 |
| Example 2d | 28 | 88 | V-0 | 38 |
| Example 2e | 28 | 86 | V-0 | 37 |
| Example 2f | 29 | 89 | V-0 | 38 |
| Comparative example 1 | 26 | 85 | V-2 | 19 |
| Comparative example 2 | 13 | 46 | V-0 | 42 |
Claims (8)
1. An anti-aging flame-retardant epoxy resin cable insulation material comprises the following components in parts by weight: 100-150 parts of an epoxy resin composition, 50-70 parts of a curing agent shown in formula (I), 20-30 parts of asbestos fibers, 20-25 parts of silicon dioxide, 10-20 parts of titanium dioxide, 10-20 parts of aluminum oxide, 4-7 parts of bentonite, 2-3 parts of talcum powder and 2-4 parts of barium sulfate, wherein the epoxy resin composition is a composition of bisphenol A or bisphenol F epoxy resin and acrylic modified organic silicon epoxy resin, and the mass of the acrylic modified organic silicon epoxy resin accounts for 30-40% of the total mass of the epoxy resin composition;
2. the anti-aging flame retardant epoxy resin cable insulation material as claimed in claim 1, comprising by weight: 100-120 parts of epoxy resin composition, 50-60 parts of curing agent shown in formula (I), 20-30 parts of asbestos fiber, 20-25 parts of silicon dioxide, 10-20 parts of titanium dioxide, 10-20 parts of aluminum oxide, 4-7 parts of bentonite, 2-3 parts of talcum powder and 2-4 parts of barium sulfate.
3. The anti-aging flame retardant epoxy resin cable insulation material as claimed in claim 1, comprising by weight: 100 parts of epoxy resin composition, 50 parts of curing agent shown in formula (I), 30 parts of asbestos fiber, 20 parts of silicon dioxide, 15 parts of titanium dioxide, 15 parts of alumina, 4-7 parts of bentonite, 2-3 parts of talcum powder and 2-4 parts of barium sulfate.
4. The anti-aging flame-retardant epoxy resin cable insulation material according to any one of claims 1 to 3, wherein the epoxy resin composition is a composition of bisphenol A or bisphenol F epoxy resin and acrylic modified silicone epoxy resin, and the mass of the acrylic modified silicone epoxy resin accounts for 30% of the total mass of the epoxy resin composition.
5. The anti-aging flame-retardant epoxy resin cable insulation material as claimed in any one of claims 1 to 3, wherein the weight ratio of the epoxy resin composition to the curing agent represented by formula I is 1: 1-3: 1.
6. The anti-aging flame-retardant epoxy resin cable insulation material according to any one of claims 1 to 3, wherein the weight ratio of the epoxy resin composition to the curing agent represented by the formula I is 2: 1.
7. The aging-resistant flame-retardant epoxy resin cable insulation material according to any one of claims 1 to 3, wherein the preparation method of the compound of formula (I) comprises the following steps:
step (1): vinyl dimethylchlorosilane reacts with methyl 2-amino-5-nitrobenzoate to produce a compound of formula a;
step (2): reacting the compound of the formula a with DOPO to prepare a compound of a formula b;
and (3): hydrolyzing the compound of the formula b to obtain a compound of a formula c;
and (4): reacting the compound shown in the formula c with 2, 4-dihydroxy benzophenone to obtain a compound shown in a formula d;
and (5): reduction of a compound of formula d to produce a compound of formula I, the reaction equation is as follows:
8. the preparation method of the aging-resistant flame-retardant epoxy resin cable insulation material as claimed in any one of claims 1 to 3, comprising the steps of:
step (1): placing silicon dioxide, titanium dioxide, aluminum oxide, bentonite, talcum powder and barium sulfate with the formula ratio in a high-speed mixer, and stirring for 5min at the rotating speed of 800 r/min;
step (2): adding a curing agent shown in the formula (I), and continuously stirring and stirring at the rotating speed of 800r/min for 5 min;
and (3): placing the mixed material obtained in the step (2) in an internal mixer, carrying out internal mixing for 4-6 min at 115-135 ℃, then transferring the mixed material into an open mill, carrying out thin-passing for 5-6 times, rolling, and cooling for 7-9 h at room temperature to obtain a primary mixed material;
and (4): putting the primary mixed material obtained in the step (3) and the epoxy resin composition with the formula amount into an internal mixer, carrying out internal mixing at 95-105 ℃ for 2-3 min, then transferring into an open mill, thinly passing through the open mill for 5-6 times, and rolling to obtain a secondary mixed material;
and (5): and (3) pouring the secondary mixed material obtained in the step (4) into a sheath screw extruder for melt blending, and extruding the mixture on a cable core, wherein the extrusion temperature is 185-200 ℃.
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| CN103304962A (en) * | 2013-06-20 | 2013-09-18 | 天津市凯华绝缘材料有限公司 | Epoxy resin composition with excellent flexibility and flame retardance, and preparation method thereof |
| CN107828187A (en) * | 2017-11-29 | 2018-03-23 | 国网河南省电力公司南阳供电公司 | A kind of erosion resisting insulation material for buried cable and preparation method thereof |
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