CN109825093A - A kind of fire retardant insulating cable material and preparation method thereof - Google Patents
A kind of fire retardant insulating cable material and preparation method thereof Download PDFInfo
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Abstract
The present invention provides a kind of preparation method of fire retardant insulating cable material, including the following steps: (one) 3,3', pure and mild 2, the 3- of 5,5'- tetra isopropyl biphenyl -4,4- bis- is bis--(4- chlorphenyl) -5- tetraphenylphosphonium chloride tetrazole polycondensation；(2) penta ring -4S, 5S- dicarboxyl bis- (dimethylamino compounds) of 2- butyl -1,3,2- dioxy boron and bis- (3- chloropropyl) four (trimethylsiloxy group) the disiloxane polycondensations of 1,3-；(3) molding of cable material；(4) ion exchange.The invention also discloses the fire retardant insulating cable materials being prepared according to the preparation method of the fire retardant insulating cable material.Fire retardant insulating cable material flame retardant effect disclosed by the invention is significant, and insulating properties is good, and stability is good, and weatherability, corrosion resistance, mechanical property, heat resistance and machining property are excellent, and preparation cost is cheap, uses safety and environmental protection.
Description
Technical field
The present invention relates to cable material technical fields, and in particular to a kind of fire retardant insulating cable material and preparation method thereof.
Background technique
With the rapid development of social economy, wire and cable in all trades and professions using more and more extensive, for electric wire
The requirement of cable is also higher and higher, does not require nothing more than it with excellent corrosion resistance, mechanical mechanics property and insulating properties, also needs
Want it when wire and cable and ambient enviroment catch fire, propagation of flame can be prevented by having, and maintain wire and cable transmission electric energy and communication
The flame retardant properties such as signal, also require its burning when smoke amount it is low, generate gas attack it is small, use safety and environmental protection.
Insulated cable material in the prior art is mainly using synthetic resin as substrate, then adds filler, plasticizer, stabilization
The additives such as agent, lubricant, colorant and be made, this kind of insulated cable material has certain insulation performance, but mechanical performance,
Expected requirement is often not achieved in thermal stability and flame retardant property.In addition, in the long-term use, the additive largely added is easy
It is oozed out from material, so that material property stability is poor, service life is short.
But it is added to a large amount of inorganic fire retardants in existing conventional cable material, while with high flame-retardant property
The mechanical performance of material, the flexibility of electric property and material, low-temperature resistance cracking behavior are largely had lost, and it cannot
High temperature is born, and easily releases the poisonous and hazardous gas such as dioxin in burning, pollutes environment, and threaten human health, from
And it limits product and widely uses.
Chinese invention patent CN201210277279 discloses a kind of high-strength highly-conductive heat insulator, and the machinery of the material is strong
Degree is inadequate, and higher cost, is unfavorable for promoting the use of.Application publication number is that the Chinese invention patent of CN1557867A discloses
A kind of halogen free nanometer fire retardant polyolefin flame retardant, it is total come flame-proof polyethylene-vinylacetate using red phosphorus and nano-sized magnesium hydroxide
Polymers, the composite materials property and excellent flame retardancy of preparation, but the fire-resistant cable material containing red phosphorus in process of production and
Burning Shi Douhui releases penetrating odor in large quantities and smoke amount is very big, pollutes environment.
Therefore, it needs in the industry to develop a kind of environmentally friendly fire retardant insulating cable material, to meet modern wire and cable
Performance requirement.
Summary of the invention
In order to overcome the defects of the prior art, the present invention is intended to provide a kind of fire retardant insulating cable material and its preparation side
Method, preparation method is simple for this, and raw material is easy to get, and preparation cost is cheap, small to device dependence, and application value is high；It is logical
Cross that the fire retardant insulating cable material flame retardant effect that the preparation method is prepared is significant, and insulating properties is good, and stability is good, resistance to
Hou Xing, corrosion resistance, mechanical property, heat resistance and machining property are excellent, and preparation cost is cheap, use safety and environmental protection.
The invention is realized by the following technical scheme: a kind of preparation method of fire retardant insulating cable material, including walks as follows
It is rapid:
Two pure and mild 2,3- of I 3,3', 5,5'- tetra isopropyl biphenyl -4,4- are bis--(4- chlorphenyl) -5- tetraphenylphosphonium chloride tetrazole
Polycondensation: by 3,3', 5,5'- tetra isopropyl biphenyl -4,4- glycol, 2,3- be bis--(4- chlorphenyl) -5- tetraphenylphosphonium chloride tetrazole, alkali
Property catalyst is added in the there-necked flask for being connected to water segregator, then increases boiling point solvent and toluene, and reaction system is heated to 100-110
DEG C, it is stirred to react under nitrogen or inert gas shielding 4-6 hours, the Shui Hejia generated in reaction process is removed by water segregator
Benzene eliminates water and reaction temperature is slowly increased to 140-150 DEG C later, continues return stirring reaction 15-20 hours, after reaction
Reaction system is cooled to room temperature, is precipitated in water, by the polymer of precipitation with ethanol washing 4-7 times, is placed on vacuum drying
It dries at 80-90 DEG C of case to constant weight, obtains the first condensation polymer；
II 2- butyl -1,3,2- dioxy boron, penta ring -4S, 5S- dicarboxyl bis- (dimethylamino compounds) and bis- (the 3- chlorine of 1,3-
Propyl) four (trimethylsiloxy group) disiloxane polycondensations: the penta bis- (diformazans of ring -4S, 5S- dicarboxyl of 2- butyl -1,3,2- dioxy boron
Amino-compound), bis- (3- chloropropyl) four (trimethylsiloxy group) disiloxane of 1,3- be dissolved in ethyl alcohol, stirred at 40-60 DEG C
Mix reaction 10-12 hours, after rotate removing ethyl alcohol again, obtain the second condensation polymer；
The molding of III cable material: it is prepared by the first condensation polymer being prepared by step I, by step II
Second condensation polymer, nano mica powder, nanometer boron fibre, coupling agent are put into and mix extrusion molding in double screw extruder, obtain
Cable material；
IV ion exchange: it is 10- that the cable material being prepared by step III, which is immersed in mass fraction at 50-60 DEG C,
It is rear to take out 20-30 hours in the aqueous solution of 20% three sulfonate sodiums of triphenylphosphine, then it is placed in a vacuum drying oven 95-105
It dries at DEG C to constant weight, obtains fire retardant insulating cable material.
Further, 3,3', 5,5'- tetra isopropyl biphenyl -4,4- glycol, 2,3- described in step I it is bis--(4- chlorobenzene
Base) -5- tetraphenylphosphonium chloride tetrazole, basic catalyst, high boiling solvent, toluene mass ratio be 1:1.14:(0.8-1.2):
(10-15):(4-6)。
Preferably, the basic catalyst is selected from one of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate or several
Kind.
Preferably, the high boiling solvent be selected from dimethyl sulfoxide, n,N-Dimethylformamide, n,N-dimethylacetamide,
One or more of N-Methyl pyrrolidone.
Preferably, the inert gas is selected from one of helium, neon, argon gas.
Further, 2- butyl -1,3 described in step II, the penta bis- (dimethylaminos of ring -4S, 5S- dicarboxyl of 2- dioxy boron
Compound), bis- (3- chloropropyl) four (trimethylsiloxy group) disiloxane of 1,3-, ethyl alcohol mass ratio be 2.16:1:(10-
15)。
Further, the first condensation polymer described in step III, the second condensation polymer, nano mica powder, nanometer boron fibre, coupling
The mass ratio of agent is 1:0.3:0.1:0.05:(0.01-0.03).
Preferably, the coupling agent is selected from silane coupling agent KH560, silane coupling agent KH570, Silane coupling agent KH550
One or more of.
Preferably, the extrusion molding process parameter are as follows: screw slenderness ratio 20:1-30:1 squeezes temperature, the firstth area
185-195 DEG C, the second 200-210 DEG C of area, 215-220 DEG C of third area, the 4th 225-235 DEG C of area；Screw pressure 0.5-1.0Mpa；
Screw speed 180-220rpm.
Further, cable material described in step IV, three sulfonate sodiums of triphenylphosphine the mass ratio of aqueous solution be
1:(5-10)。
A kind of fire retardant insulating cable material is prepared using a kind of above-mentioned preparation method of fire retardant insulating cable material.
The beneficial effects of adopting the technical scheme are that
(1) a kind of fire retardant insulating cable material provided by the invention, preparation method is simple, and raw material is easy to get, and is prepared into
This is cheap, small to device dependence, and application value is high.
(2) a kind of fire retardant insulating cable material provided by the invention overcomes and is added in conventional cable material greatly
The inorganic fire retardants of amount largely has lost the mechanical performance of material, electric property while with high flame-retardant property
And the flexibility of material, low-temperature resistance cracking behavior, and it cannot bear high temperature, easily release that dioxin etc. is toxic to be had in burning
Harmful gas pollutes environment, and threatens human health, to limit the technological deficiency that product widely uses, has resistance
Significant effect is fired, insulating properties is good, and stability is good, weatherability, corrosion resistance, mechanical property, heat resistance and machining property
Can be excellent, preparation cost is cheap, uses safety and environmental protection.
(3) a kind of fire retardant insulating cable material provided by the invention, by introducing isopropyl biphenyl knot on molecular backbone
Structure improves insulation performance on the basis of guaranteeing very good mechanical properties；Nitrogen azoles structure is introduced, flame retardant property is improved and is resisted
Ultraviolet ageing performance；Ionic group is introduced, as crosslink sites, three-dimensional net structure is formed, improves the comprehensive performance of material；
Introduce boron, phosphorus, silicon, N structure simultaneously on molecular backbone, synergistic effect improves the anti-flammability of material；First condensation polymer and
Two condensation polymer compatibilities are good, and the material obtained after blending combines the advantage of the two, so that cable material excellent combination property.
(4) a kind of fire retardant insulating cable material provided by the invention, not adding a large amount of functional additive can but reach
Tradition adds the technical effect of a large amount of functional additives, effectively prevents the addition of a large amount of additives to material mechanical processing performance
And it is influenced caused by long-term behaviour stability；The nano mica powder and nanometer boron fibre of addition have preferable enhancing to material
Effect.
Specific embodiment
In order to make those skilled in the art more fully understand technical solution of the present invention, and make features described above of the invention,
Purpose and advantage are more clear understandable, and the present invention will be further explained with reference to the examples below.Embodiment is only used for
It is bright the present invention rather than limit the scope of the invention.
Present invention raw material as used in the following examples is commercially available.
Embodiment 1
A kind of preparation method of fire retardant insulating cable material, includes the following steps:
Two pure and mild 2,3- of I 3,3', 5,5'- tetra isopropyl biphenyl -4,4- are bis--(4- chlorphenyl) -5- tetraphenylphosphonium chloride tetrazole
Polycondensation: by 3,3', 5,5'- tetra isopropyl biphenyl -4,4- glycol 1kg, 2,3- be bis--(4- chlorphenyl) -5- tetraphenylphosphonium chloride tetrazole
1.14kg, sodium hydroxide 0.8kg are added in the there-necked flask for being connected to water segregator, then plus dimethyl sulfoxide 10kg and toluene 4kg, will react
System is heated to 100 DEG C, and stirred under nitrogen atmosphere reacts 4 hours, removes the Shui Hejia generated in reaction process by water segregator
Benzene eliminates water and reaction temperature is slowly increased to 140 DEG C later, continues return stirring and reacts 15 hours, after reaction will reaction
System is cooled to room temperature, and is precipitated in water, by the polymer of precipitation with ethanol washing 4 times, is placed at 80 DEG C of vacuum oven
Drying obtains the first condensation polymer to constant weight；
II 2- butyl -1,3,2- dioxy boron, penta ring -4S, 5S- dicarboxyl bis- (dimethylamino compounds) and bis- (the 3- chlorine of 1,3-
Propyl) four (trimethylsiloxy group) disiloxane polycondensations: the penta bis- (diformazans of ring -4S, 5S- dicarboxyl of 2- butyl -1,3,2- dioxy boron
Amino-compound) 2.16kg, 1,3- bis- (3- chloropropyls) four (trimethylsiloxy group) disiloxane 1kg be dissolved in ethyl alcohol 10kg,
Be stirred to react at 40 DEG C 10 hours, after rotate removing ethyl alcohol again, obtain the second condensation polymer；
The molding of III cable material: it is prepared by the first condensation polymer 1kg being prepared by step I, by step II
The second condensation polymer 0.3kg, nano mica powder 0.1kg, nanometer boron fibre 0.05kg, the silane coupling agent KH5600.01kg arrived is thrown
Enter and mix extrusion molding into double screw extruder, obtains cable material；The extrusion molding process parameter are as follows: screw slenderness ratio
For 20:1, temperature, the first 185 DEG C of area, the second 200 DEG C of area, 215 DEG C of third area, the 4th 225 DEG C of area are squeezed；Screw pressure
0.5Mpa；Screw speed 180rpm；
IV ion exchange: the cable material 1kg being prepared by step III, which is immersed in mass fraction at 50 DEG C, is
It is rear to take out 20 hours in the aqueous solution 5kg of 10% three sulfonate sodiums of triphenylphosphine, then be placed in a vacuum drying oven at 95 DEG C
Drying obtains fire retardant insulating cable material to constant weight.
A kind of fire retardant insulating cable material is prepared using a kind of above-mentioned preparation method of fire retardant insulating cable material.
Embodiment 2
A kind of preparation method of fire retardant insulating cable material, includes the following steps:
Two pure and mild 2,3- of I 3,3', 5,5'- tetra isopropyl biphenyl -4,4- are bis--(4- chlorphenyl) -5- tetraphenylphosphonium chloride tetrazole
Polycondensation: by 3,3', 5,5'- tetra isopropyl biphenyl -4,4- glycol 1kg, 2,3- be bis--(4- chlorphenyl) -5- tetraphenylphosphonium chloride tetrazole
1.14kg, potassium hydroxide 0.9kg are added in the there-necked flask for being connected to water segregator, then plus n,N-Dimethylformamide 11kg and toluene
Reaction system is heated to 103 DEG C, is stirred to react 4.5 hours under helium protection, removes reaction process by water segregator by 4.5kg
The water and toluene of middle generation eliminate water and reaction temperature are slowly increased to 143 DEG C later, continue return stirring and react 16.5 hours,
Reaction system is cooled to room temperature after reaction, is precipitated in water, by the polymer of precipitation with ethanol washing 5 times, is placed on
It dries at 83 DEG C of vacuum oven to constant weight, obtains the first condensation polymer；
II 2- butyl -1,3,2- dioxy boron, penta ring -4S, 5S- dicarboxyl bis- (dimethylamino compounds) and bis- (the 3- chlorine of 1,3-
Propyl) four (trimethylsiloxy group) disiloxane polycondensations: the penta bis- (diformazans of ring -4S, 5S- dicarboxyl of 2- butyl -1,3,2- dioxy boron
Amino-compound) 2.16kg, 1,3- bis- (3- chloropropyls) four (trimethylsiloxy group) disiloxane 1kg be dissolved in ethyl alcohol 11.5kg
In, be stirred to react at 45 DEG C 10.5 hours, after rotate removing ethyl alcohol again, obtain the second condensation polymer；
The molding of III cable material: it is prepared by the first condensation polymer 1kg being prepared by step I, by step II
The second condensation polymer 0.3kg, nano mica powder 0.1kg, nanometer boron fibre 0.05kg, the silane coupling agent KH5700.015kg arrived is thrown
Enter and mix extrusion molding into double screw extruder, obtains cable material；The extrusion molding process parameter are as follows: screw slenderness ratio
For 23:1, temperature, the first 188 DEG C of area, the second 203 DEG C of area, 217 DEG C of third area, the 4th 229 DEG C of area are squeezed；Screw pressure
0.7Mpa；Screw speed 195rpm；
IV ion exchange: the cable material 1kg being prepared by step III, which is immersed in mass fraction at 53 DEG C, is
It is rear to take out 24 hours in the aqueous solution 6.5kg of 13% three sulfonate sodiums of triphenylphosphine, then it is placed in a vacuum drying oven 98 DEG C
Lower drying obtains fire retardant insulating cable material to constant weight.
A kind of fire retardant insulating cable material is prepared using a kind of above-mentioned preparation method of fire retardant insulating cable material.
Embodiment 3
A kind of preparation method of fire retardant insulating cable material, includes the following steps:
Two pure and mild 2,3- of I 3,3', 5,5'- tetra isopropyl biphenyl -4,4- are bis--(4- chlorphenyl) -5- tetraphenylphosphonium chloride tetrazole
Polycondensation: by 3,3', 5,5'- tetra isopropyl biphenyl -4,4- glycol 1kg, 2,3- be bis--(4- chlorphenyl) -5- tetraphenylphosphonium chloride tetrazole
1.14kg, sodium carbonate 1kg are added in the there-necked flask for being connected to water segregator, then plus n,N-dimethylacetamide 13kg and toluene 5kg, will
Reaction system is heated to 106 DEG C, is stirred to react 5 hours under neon protection, removes the water generated in reaction process by water segregator
And toluene, it eliminates water and reaction temperature is slowly increased to 146 DEG C later, continue return stirring and react 18 hours, after reaction will
Reaction system is cooled to room temperature, and is precipitated in water, by the polymer of precipitation with ethanol washing 6 times, is placed on vacuum oven 85
It dries at DEG C to constant weight, obtains the first condensation polymer；
II 2- butyl -1,3,2- dioxy boron, penta ring -4S, 5S- dicarboxyl bis- (dimethylamino compounds) and bis- (the 3- chlorine of 1,3-
Propyl) four (trimethylsiloxy group) disiloxane polycondensations: the penta bis- (diformazans of ring -4S, 5S- dicarboxyl of 2- butyl -1,3,2- dioxy boron
Amino-compound) 2.16kg, 1,3- bis- (3- chloropropyls) four (trimethylsiloxy group) disiloxane 1kg be dissolved in ethyl alcohol 13kg,
Be stirred to react at 50 DEG C 11 hours, after rotate removing ethyl alcohol again, obtain the second condensation polymer；
The molding of III cable material: it is prepared by the first condensation polymer 1kg being prepared by step I, by step II
The second condensation polymer 0.3kg, nano mica powder 0.1kg, nanometer boron fibre 0.05kg, the Silane coupling agent KH550 0.02kg arrived is thrown
Enter and mix extrusion molding into double screw extruder, obtains cable material；The extrusion molding process parameter are as follows: screw slenderness ratio
For 26:1, temperature, the first 190 DEG C of area, the second 206 DEG C of area, 218 DEG C of third area, the 4th 230 DEG C of area are squeezed；Screw pressure
0.8Mpa；Screw speed 200rpm.
IV ion exchange: the cable material 1kg being prepared by step III, which is immersed in mass fraction at 58 DEG C, is
It is rear to take out 27 hours in the aqueous solution 8kg of 17% three sulfonate sodiums of triphenylphosphine, then it is placed in a vacuum drying oven 100 DEG C
Lower drying obtains fire retardant insulating cable material to constant weight.
A kind of fire retardant insulating cable material is prepared using a kind of above-mentioned preparation method of fire retardant insulating cable material.
Embodiment 4
A kind of preparation method of fire retardant insulating cable material, includes the following steps:
Two pure and mild 2,3- of I 3,3', 5,5'- tetra isopropyl biphenyl -4,4- are bis--(4- chlorphenyl) -5- tetraphenylphosphonium chloride tetrazole
Polycondensation: by 3,3', 5,5'- tetra isopropyl biphenyl -4,4- glycol 1kg, 2,3- be bis--(4- chlorphenyl) -5- tetraphenylphosphonium chloride tetrazole
1.14kg, basic catalyst 1.1kg are added in the there-necked flask for being connected to water segregator, then increase boiling point solvent 14kg and toluene 5.5kg,
Reaction system is heated to 109 DEG C, is stirred to react 5.5 hours under argon gas protection, is removed in reaction process and generated by water segregator
Water and toluene, eliminate and reaction temperature be slowly increased to 148 DEG C after water, continue return stirring and react 19 hours, reaction terminates
Reaction system is cooled to room temperature afterwards, is precipitated in water, by the polymer of precipitation with ethanol washing 6 times, is placed on vacuum drying
It dries at 88 DEG C of case to constant weight, obtains the first condensation polymer；The basic catalyst is sodium hydroxide, potassium hydroxide, sodium carbonate, carbon
The mixture that sour potassium 2:1:2:1 in mass ratio is mixed；The high boiling solvent is dimethyl sulfoxide, N, N- dimethyl formyl
The mixture that amine, DMAC N,N' dimethyl acetamide, N-Methyl pyrrolidone 1:2:3:2 in mass ratio are mixed；
II 2- butyl -1,3,2- dioxy boron, penta ring -4S, 5S- dicarboxyl bis- (dimethylamino compounds) and bis- (the 3- chlorine of 1,3-
Propyl) four (trimethylsiloxy group) disiloxane polycondensations: the penta bis- (diformazans of ring -4S, 5S- dicarboxyl of 2- butyl -1,3,2- dioxy boron
Amino-compound) 2.16kg, 1,3- bis- (3- chloropropyls) four (trimethylsiloxy group) disiloxane 1kg be dissolved in ethyl alcohol 14.5kg
In, be stirred to react at 55 DEG C 11.5 hours, after rotate removing ethyl alcohol again, obtain the second condensation polymer；
The molding of III cable material: it is prepared by the first condensation polymer 1kg being prepared by step I, by step II
To the second condensation polymer 0.3kg, nano mica powder 0.1kg, nanometer boron fibre 0.05kg, coupling agent 0.025kg put into double spiral shells
Extrusion molding is mixed in bar extruder, obtains cable material；The coupling agent is silane coupling agent KH560, silane coupling agent
The mixture that KH570, Silane coupling agent KH550 2:4:5 in mass ratio are mixed；The extrusion molding process parameter are as follows: spiral shell
Bar draw ratio is 29:1, squeezes temperature, the first 194 DEG C of area, the second 209 DEG C of area, 219 DEG C of third area, the 4th 234 DEG C of area；Screw rod
Pressure 0.9Mpa；Screw speed 210rpm.
IV ion exchange: the cable material 1kg being prepared by step III, which is immersed in mass fraction at 58 DEG C, is
It is rear to take out 29 hours in the aqueous solution 9.5kg of 19% three sulfonate sodiums of triphenylphosphine, then it is placed in a vacuum drying oven 104
It dries at DEG C to constant weight, obtains fire retardant insulating cable material.
A kind of fire retardant insulating cable material is prepared using a kind of above-mentioned preparation method of fire retardant insulating cable material.
Embodiment 5
A kind of preparation method of fire retardant insulating cable material, includes the following steps:
Two pure and mild 2,3- of I 3,3', 5,5'- tetra isopropyl biphenyl -4,4- are bis--(4- chlorphenyl) -5- tetraphenylphosphonium chloride tetrazole
Polycondensation: by 3,3', 5,5'- tetra isopropyl biphenyl -4,4- glycol 1kg, 2,3- be bis--(4- chlorphenyl) -5- tetraphenylphosphonium chloride tetrazole
1.14kg, potassium carbonate 1.2kg are added in the there-necked flask for being connected to water segregator, then plus N-Methyl pyrrolidone 15kg and toluene 6kg, will
Reaction system is heated to 110 DEG C, and stirred under nitrogen atmosphere reacts 6 hours, removes the water generated in reaction process by water segregator
And toluene, it eliminates water and reaction temperature is slowly increased to 150 DEG C later, continue return stirring and react 20 hours, after reaction will
Reaction system is cooled to room temperature, and is precipitated in water, by the polymer of precipitation with ethanol washing 7 times, is placed on vacuum oven 90
It dries at DEG C to constant weight, obtains the first condensation polymer；
II 2- butyl -1,3,2- dioxy boron, penta ring -4S, 5S- dicarboxyl bis- (dimethylamino compounds) and bis- (the 3- chlorine of 1,3-
Propyl) four (trimethylsiloxy group) disiloxane polycondensations: the penta bis- (diformazans of ring -4S, 5S- dicarboxyl of 2- butyl -1,3,2- dioxy boron
Amino-compound) 2.16kg, 1,3- bis- (3- chloropropyls) four (trimethylsiloxy group) disiloxane 1kg be dissolved in ethyl alcohol 15kg,
Be stirred to react at 60 DEG C 12 hours, after rotate removing ethyl alcohol again, obtain the second condensation polymer；
The molding of III cable material: it is prepared by the first condensation polymer 1kg being prepared by step I, by step II
The second condensation polymer 0.3kg, nano mica powder 0.1kg, nanometer boron fibre 0.05kg, the silane coupling agent KH5600.03kg arrived is thrown
Enter and mix extrusion molding into double screw extruder, obtains cable material；The extrusion molding process parameter are as follows: screw slenderness ratio
For 30:1, temperature, the first 195 DEG C of area, the second 210 DEG C of area, 220 DEG C of third area, the 4th 235 DEG C of area are squeezed；Screw pressure
1.0Mpa；Screw speed 220rpm；
IV ion exchange: the cable material 1kg being prepared by step III, which is immersed in mass fraction at 60 DEG C, is
It is rear to take out 30 hours in the aqueous solution 10kg of 20% three sulfonate sodiums of triphenylphosphine, then it is placed in a vacuum drying oven 105 DEG C
Lower drying obtains fire retardant insulating cable material to constant weight.
A kind of fire retardant insulating cable material is prepared using a kind of above-mentioned preparation method of fire retardant insulating cable material.
Comparative example
A kind of cable material is prepared according to the formula of 103087394 B embodiment 1 of Chinese invention patent CN.
Cable material sample obtained by above-described embodiment 1-5 and comparative example is tested, test result and test method
It is shown in Table 1.
Table 1
As can be seen from the above table, fire retardant insulating cable material disclosed by the embodiments of the present invention, tensile strength 26.5-
32.0MPa, elongation at break 285-327%, limit oxygen index 44-50%, 20 DEG C of volume resistivities 6.2 × 1013-9.0×
1013Ω .m, and the cable material in comparative example, tensile strength only 12.2MPa, elongation at break 185%, limit oxygen index
41%, 20 DEG C of volume resistivities 0.60 × 1013Ω.m.As it can be seen that fire retardant insulating cable material disclosed by the embodiments of the present invention has
Excellent mechanical mechanics property, fire protection flame retarding and insulating properties.
The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and what is described in the above embodiment and the description is only the present invention
Principle, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these variation and
Improvement is both fallen in the range of claimed invention.The present invention claims protection scope by appended claims and its
Equivalent defines.
Claims (10)
1. a kind of preparation method of fire retardant insulating cable material, which comprises the steps of:
Two pure and mild 2,3- of I 3,3', 5,5'- tetra isopropyl biphenyl -4,4- are bis--(4- chlorphenyl) -5- tetraphenylphosphonium chloride tetrazole polycondensation:
By 3,3', 5,5'- tetra isopropyl biphenyl -4,4- glycol, 2,3- be bis--(4- chlorphenyl) -5- tetraphenylphosphonium chloride tetrazole, base catalysis
Agent is added in the there-necked flask for being connected to water segregator, then increases boiling point solvent and toluene, reaction system is heated to 100-110 DEG C, nitrogen
It is stirred to react under gas or inert gas shielding 4-6 hours, the water and toluene that generate in reaction process is removed by water segregator, eliminated
Reaction temperature is slowly increased to 140-150 DEG C after water, continues return stirring and reacts 15-20 hours, it after reaction will reaction
System is cooled to room temperature, and is precipitated in water, by the polymer of precipitation with ethanol washing 4-7 times, is placed on vacuum oven 80-90
It dries at DEG C to constant weight, obtains the first condensation polymer；
II 2- butyl -1,3,2- dioxy boron, penta ring -4S, 5S- dicarboxyl bis- (dimethylamino compounds) and bis- (the 3- chlorine third of 1,3-
Base) four (trimethylsiloxy group) disiloxane polycondensations: penta bis- (the diformazan ammonia of ring -4S, 5S- dicarboxyl of 2- butyl -1,3,2- dioxy boron
Based compound), bis- (3- chloropropyl) four (trimethylsiloxy group) disiloxane of 1,3- be dissolved in ethyl alcohol, stirred at 40-60 DEG C
Reaction 10-12 hours, after rotate removing ethyl alcohol again, obtain the second condensation polymer；
The molding of III cable material: the first condensation polymer that step I is prepared, be prepared by step II second will be passed through
Condensation polymer, nano mica powder, nanometer boron fibre, coupling agent are put into and mix extrusion molding in double screw extruder, and cable is obtained
Material；
IV ion exchange: it is 10-20% that the cable material being prepared by step III, which is immersed in mass fraction at 50-60 DEG C,
Three sulfonate sodiums of triphenylphosphine aqueous solution in 20-30 hours, it is rear to take out, then be placed in a vacuum drying oven at 95-105 DEG C
Drying obtains fire retardant insulating cable material to constant weight.
2. a kind of preparation method of fire retardant insulating cable material according to claim 1, which is characterized in that institute in step I
Stating 3,3', 5,5'- tetra isopropyl biphenyl -4,4- glycol, 2,3- be bis--(4- chlorphenyl) -5- tetraphenylphosphonium chloride tetrazole, base catalysis
Agent, high boiling solvent, toluene mass ratio be 1:1.14:(0.8-1.2): (10-15): (4-6).
3. a kind of preparation method of fire retardant insulating cable material according to claim 1, which is characterized in that the alkalinity is urged
Agent is selected from one or more of sodium hydroxide, potassium hydroxide, sodium carbonate, potassium carbonate.
4. a kind of preparation method of fire retardant insulating cable material according to claim 1, which is characterized in that the higher boiling
Solvent is selected from one of dimethyl sulfoxide, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, N-Methyl pyrrolidone or several
Kind；The inert gas is selected from one of helium, neon, argon gas.
5. a kind of preparation method of fire retardant insulating cable material according to claim 1, which is characterized in that institute in step II
State penta ring -4S, 5S- dicarboxyl bis- (dimethylamino compounds) of 2- butyl -1,3,2- dioxy boron, bis- (the 3- chloropropyls) four of 1,3-
(trimethylsiloxy group) disiloxane, ethyl alcohol mass ratio be 2.16:1:(10-15).
6. a kind of preparation method of fire retardant insulating cable material according to claim 1, which is characterized in that institute in step III
State the first condensation polymer, the second condensation polymer, nano mica powder, nanometer boron fibre, coupling agent mass ratio be 1:0.3:0.1:0.05:
(0.01-0.03)。
7. a kind of preparation method of fire retardant insulating cable material according to claim 1, which is characterized in that the coupling agent
Selected from one or more of silane coupling agent KH560, silane coupling agent KH570, Silane coupling agent KH550.
8. a kind of preparation method of fire retardant insulating cable material according to claim 1, which is characterized in that described to be extruded into
Type technological parameter are as follows: screw slenderness ratio 20:1-30:1, extruding temperature, the first 185-195 DEG C of area, the second 200-210 DEG C of area,
215-220 DEG C of third area, the 4th 225-235 DEG C of area；Screw pressure 0.5-1.0Mpa；Screw speed 180-220rpm.
9. a kind of preparation method of fire retardant insulating cable material according to claim 1, which is characterized in that institute in step IV
State cable material, three sulfonate sodiums of triphenylphosphine aqueous solution mass ratio be 1:(5-10).
10. a kind of be prepared using a kind of described in any item preparation methods of fire retardant insulating cable material of claim 1-9
Fire retardant insulating cable material.
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Citations (3)
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|---|---|---|---|---|
| CN85101465A (en) * | 1984-08-14 | 1987-01-17 | 藤电线株式会社 | Flame-retardant composition and the anti-flammability cable that uses said composition to make |
| CN103881166A (en) * | 2014-03-26 | 2014-06-25 | 苏州红麒麟塑胶有限公司 | Low smoke halogen-free flame retardant material applicable to photovoltaic cable and manufacturing method thereof |
| CN105175905A (en) * | 2015-09-10 | 2015-12-23 | 上海大学 | Preparation method of tear-resistant halogen-free flame retardant polymer cover insulating material for cables |
-
2019
- 2019-03-12 CN CN201910185680.1A patent/CN109825093A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN85101465A (en) * | 1984-08-14 | 1987-01-17 | 藤电线株式会社 | Flame-retardant composition and the anti-flammability cable that uses said composition to make |
| CN103881166A (en) * | 2014-03-26 | 2014-06-25 | 苏州红麒麟塑胶有限公司 | Low smoke halogen-free flame retardant material applicable to photovoltaic cable and manufacturing method thereof |
| CN105175905A (en) * | 2015-09-10 | 2015-12-23 | 上海大学 | Preparation method of tear-resistant halogen-free flame retardant polymer cover insulating material for cables |
Non-Patent Citations (1)
| Title |
|---|
| 陈龙: "电线电缆用高强度低烟无卤阻燃硅橡胶材料的制备与应用研究", 《广东化工》 * |
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