CN110229420A - A kind of polyacrylic preparation method of optical cable toughening flame-proof - Google Patents

A kind of polyacrylic preparation method of optical cable toughening flame-proof Download PDF

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CN110229420A
CN110229420A CN201910630487.4A CN201910630487A CN110229420A CN 110229420 A CN110229420 A CN 110229420A CN 201910630487 A CN201910630487 A CN 201910630487A CN 110229420 A CN110229420 A CN 110229420A
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parts
optical cable
fire
retardant
coupling agent
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张小敏
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Jinling Institute of Technology
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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
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/10—Homopolymers or copolymers of propene
    • C08L23/12—Polypropene
    • 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
    • C08K2003/2217—Oxides; Hydroxides of metals of magnesium
    • C08K2003/2224—Magnesium hydroxide
    • 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
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets
    • C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
    • 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
    • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend

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  • Health & Medical Sciences (AREA)
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  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
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  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The present invention relates to a kind of polyacrylic preparation methods of optical cable toughening flame-proof, Toughened PP resin particle, coupling agent modified fire-retardant filler, the preparation of fire-retardant PP particle are carried out, formulation optimization and performance improvement have been carried out, the PP composite material of high tenacity, flame retardant property is prepared.After the present invention is to PP toughening modifying, its flame retardant property and mechanical performance are effectively improved, preparation cost performance is high.Good reaction selectivity of the invention, process flow is simple, is a kind of preparation method of high financial profit.

Description

A kind of polyacrylic preparation method of optical cable toughening flame-proof
Technical field
The present invention relates to electronics industry fields, and in particular to a kind of polyacrylic preparation method of optical cable toughening flame-proof.
Background technique
Polypropylene (PP) is the plastics with excellent processability, mechanical property, and poor impact toughness, intensity are low.It is logical in light In letter field, core component of the Loose tube as layer-twisted type and central-beam tube type fiber optic cable, effect mainly protect optical fiber from Internal stress and external side pressure.In recent years, optic cable producer starts using raw material of the PP as Loose tube, but PP casing Toughness it is poor, be unable to satisfy its extensive engineer application.It is main at present that toughening is carried out to it by adding rubber elastomer, such as three First EP rubbers, EP rubbers, ethylene octene copolymer, but elastomer is added usually reduces polyacrylic intensity, and toughening Polypropylene belongs to inflammable high molecular material, and the application of the plastic products for there is flame retardant property to require is restricted.Therefore, it is desirable to Find a kind of method that strength reduction is reduced while tenacity-increased profax, and the polypropylene with flame retardant property.
The fire-retardant product of PP mainly has using containing halogen organic and antimony oxide compound flame retardant both at home and abroad at present.So And flue dust and corrosive gas are generated when fire-retardant high molecular material burning, it pollutes the environment.Fire-retardant PP's is inorganic fire-retarded Agent mainly has magnesium hydroxide and aluminium hydroxide, and the fire retardant is low in cost, nontoxic, suppression cigarette, but its dosage is larger, will significantly drop The mechanical property of low material.Phenyl-phosphonic acid metal salt can form fine dispersion layer in resin, and carbon-based material high temperature resistant can be Completely cut off extraneous oxygen and heat when burning, thulium can improve thermal stability and anti-flammability after resin burning Energy.
Summary of the invention
The object of the present invention is to provide a kind of optical cable toughening flame-proof polypropylene, have carried out formulation optimization and performance improvement, Prepare the PP composite material of high tenacity, flame retardant property.
To achieve the above object, present invention provide the technical scheme that
A kind of polyacrylic preparation method of optical cable toughening flame-proof, comprising the following steps:
1) by a certain amount of chlorinated scoline (CIIR), polyvinyl chloride (PVC), Dimeric Cyclopentadiene Carboxylic Acid sodium salt, antioxygen Agent, stabilizer, which are placed in mixer, carries out esterification realization crosslinking, obtains the crosslinking rubber with thermal reversibility；By the friendship Join rubber and PP, crosslinking agent, stabilizer blend kneading machine after mixing, mixed material is added twin-screw extrude Extruding pelletization obtains Toughened PP resin particle；
2) cerous nitrate aqueous solution, ultrasound point will be added after phenyl-phosphonic acid aqueous solution and graphene or carbon nanotube sonic oscillation It is transferred in autoclave after dissipating, carries out hydro-thermal reaction, obtain metal phosphonic acid cerium hydridization graphene or carbon nanotube, filtered, It is dried in vacuo after deionization washing；By a certain amount of metal phosphonic acid cerium hydridization graphene or carbon nanotube, mix inorganic fire-retarded fill out Material, coupling agent and spirit solvent are uniformly mixed, and certain time ultrasound point after mixing is blended by high speed shear dispersion machine It dissipates, evaporates solvent by air dry oven to obtain coupling agent modified fire-retardant filler；
3) Toughened PP for obtaining coupling agent modified fire-retardant filler, antioxidant and a certain amount of step 1) that step 2) obtains Resin particle mixing, by extruder, melting mixing obtains the fire-retardant PP particle for being uniformly mixed granulation at a certain temperature；
4) the fire-retardant PP particle by the uniformly mixed granulation that step 3) obtains is put into mold, is existed with hot press and injection molding machine It is molded under certain temperature and pressure, batten is obtained after held for some time；
5) color masterbatch and fire-retardant PP is added to go out head by 50 single screw extrusion machine of φ by batten is casing, after casing goes out head It quickly enters sink to be rapidly cooled, leads and be heat-treated subsequently into the first water-bath wheel, the second water-bath is entered after heat treatment Wheel lead and air-blowing it is air-cooled again cool down after enter admission machine.
In parts by mass, CIIR described in step 1) and PVC content are 100 parts altogether, and mass ratio is 80:20~90:10； Dimeric Cyclopentadiene Carboxylic Acid sodium salt mass content is the 1~8% of CIIR；Stabilizer is calcium stearate, content be CIIR 1~ 5%；Antioxidant is Phenyl Di-2-ethyl Hexyl Phosphite (DPP), and content is the 1~8% of CIIR；70~90 parts of PP, 10~30 parts of systems Standby crosslinking rubber.
In step 1), melting temperature is 140~190 DEG C, and 40~200r/min of revolving speed is kneaded 10~30min, extruder 140 ~180 DEG C of granulations.
In step 2), the phenyl-phosphonic acid aqueous solution is 1~5mmol, cerous nitrate 1~4mmol of aqueous solution, ultrasonic disperse 10~40min, 100~150 DEG C of hydro-thermal reactions 10~20h, 50~80 DEG C of 10~20h of vacuum drying.
Mixing inorganic fire-retarded filler described in step 2) is tetraphenyl diphenol A diphosphonate (BDP), graphene (GE), carbon Nanotube, phosphonic acids rare-earth salts modified graphene, phosphonic acids rare-earth salts modified carbon nano-tube, magnesium hydroxide (Mg (OH)2) and hydroxide Aluminium (Al (OH)3) in a variety of mixing；Coupling agent is titanate coupling agent, gamma-aminopropyl-triethoxy-silane, self-control rare earth titanium One or more of coupling agent.
In step 2), in parts by mass, 3~9 parts of BPD, 1~5 part of Mg (OH) are taken2, 1~5 part of Al (OH)3, 1~5 part of GE, 1 ~5 parts of carbon nanotubes, 1~4 part of titanate coupling agent, 1~4 part of gamma-aminopropyl-triethoxy-silane, 1~4 part of self-control rare earth titanium Coupling agent, 30~60 DEG C of 1~40min of magnetic agitation, 10~50min of ultrasound.
In step 3), by 1~10 part of coupling agent modified fire-retardant filler, 1~5 part of antioxidant four [β-(3,5- bis- tertiary fourths Base -4- hydroxy phenyl) propionic acid] pentaerythritol ester, 100 parts of Toughened PP resin particles, 130~180 DEG C of extruder.
In step 4), it is pressed and molded condition are as follows: be uniformly mixed the 10~30g of fire-retardant PP particle being granulated, upper and lower mould temperature 130~180 DEG C, 4~10Mpa.
The additive amount of the step 5) color masterbatch is the 1~4% of batten quality, 190~240 DEG C of extrusion trombone slides of extruder.
Further, by 1 part of lanthana and 5 parts of pyrophosphoric acid type titanate esters, it is added there-necked flask, and with magnetic force oil bath heating, In 130 DEG C of reaction 5h, self-control rare earth titanium coupling agent is prepared.
Compared with prior art, the beneficial effects of the present invention are:
A kind of polyacrylic preparation method of optical cable toughening flame-proof of the present invention effectively mentions after PP toughening modifying Its high flame retardant property and mechanical performance, preparation cost performance are high.Good reaction selectivity of the invention, process flow is simple, is a kind of The preparation method of high financial profit.
Specific embodiment
The present invention is further explained in the light of specific embodiments.
Embodiment 1 (preparation for being crosslinked rubber toughened PP):
By 90 parts of CIIR and 10 part of PVC, 5 parts of Dimeric Cyclopentadiene Carboxylic Acid sodium salts, 3 parts of calcium stearates, 4 parts of DPP, it is placed in close 180 DEG C of mixing 30min obtain crosslinking rubber in mill.By 10 parts of crosslinking rubber, 90 parts of PP, 0.1 part of DPP, 1 part of magnesia (MgO) blend in kneading machine 150 DEG C after mixing, material is added twin-screw extrude into extruding pelletization, squeezes out temperature Degree is 180 DEG C, and revolving speed is that 200r/min extruding pelletization obtains Toughened PP.It is 28MPa, elongation at break that test, which obtains tensile strength, It is 183%, impact strength 10kJ/m2, Vicat softening point is 99.5 DEG C.Toughened PP particle, which is placed in hopper, to be injection moulded, temperature 160 DEG C, injection pressure 5MPa, molding time 45s of degree prepares the batten of test oxygen index (OI).Limit oxygen index (LOI) is 18% It can burn with vertical combustion refining (UL-94) experiment display batten.
Comparative example 1 (preparation for being crosslinked rubber toughened PP):
By 90 parts of CIIR and 10 part of PVC, 5 parts of Dimeric Cyclopentadiene Carboxylic Acid sodium salts, 3 parts of calcium stearates, 4 parts of DPP, it is placed in close 180 DEG C of mixing 30min obtain crosslinking rubber in mill.By 30 parts of crosslinking rubber, 70 parts of PP, 0.1 part of DPP, 1 part of magnesia (MgO) blend in kneading machine 150 DEG C after mixing, material is added twin-screw extrude into extruding pelletization, squeezes out temperature Degree is 180 DEG C, and revolving speed is that 200r/min extruding pelletization obtains Toughened PP.It is 25MPa, elongation at break that test, which obtains tensile strength, It is 209%, impact strength 23kJ/m2, Vicat softening point is 92 DEG C.Toughened PP particle, which is placed in hopper, to be injection moulded, temperature 160 DEG C, injection pressure 5MPa, molding time 45s, prepare the batten of test oxygen index (OI).Limit oxygen index (LOI) is 15% He Vertical combustion refining (UL-94) experiment display batten can burn.
Comparative example 2 (preparation of no Toughened PP):
It by pure PP particle mold, is placed in hot press, 150 DEG C of upper and lower mould temperature, 5Mpa preheating 10min, pressurization is set To 10MP hot pressing 10min, leads to cooling water to room temperature, prepare tensile test batten.It is 32MPa that test, which obtains tensile strength, is broken Splitting elongation is 175%, impact strength 2kJ/m2, Vicat softening point is 72 DEG C.Toughened PP particle, which is placed in hopper, to be injected into Type, prepares the batten of test oxygen index (OI) by 160 DEG C of temperature, injection pressure 5MPa, molding time 45s.Limit oxygen index (LOI) It can burn for 14% and vertical combustion refining (UL-94) experiment display batten.
Embodiment 2 (modified containing graphene fire-retardant filler preparation):
Sonic oscillation 30min, solution A at 60 DEG C by 25 parts of phenyl-phosphonic acid aqueous solutions (5mmol) and 2 parts of graphenes.It will 25 parts of cerous nitrate aqueous solutions (3mmol) are added in solution A, and ultrasonic disperse 30min obtains being easy B.B solution is transferred to high pressure In reaction kettle, hydro-thermal reaction 20h is carried out at 100 DEG C.The filtering of metal phosphonic acid cerium hydridization graphene will be obtained, and uses deionized water It is washcoated multiple, 60 DEG C of vacuum drying 20h.
By 1 part of lanthana and 5 parts of pyrophosphoric acid type titanate esters, there-necked flask is added, and use magnetic force oil bath heating, instead at 130 DEG C 5h is answered, rare earth titanium coupling agent is prepared.
By 1 part of metal phosphonic acid cerium hydridization graphene, 5 parts of BDP, 3 parts of Mg (OH)2With 3 parts of Al (OH)3It is placed in alcoholic solution, 2 parts of rare earth titanium coupling agents, 1 part of gamma-aminopropyl-triethoxy-silane are added, ultrasound 30min after 50 DEG C of magnetic agitation 30min, drum It air-dries and dry volatilizees solvent to obtain modified flame-retardant filler.
Embodiment 3 (preparation of modified carbonaceous nanotube fire-retardant filler):
Sonic oscillation 30min, solution A at 60 DEG C by 25 parts of phenyl-phosphonic acid aqueous solutions (5mmol) and 1 part of carbon nanotube. 25 parts of cerous nitrate aqueous solutions (3mmol) are added in solution A, ultrasonic disperse 30min obtains being easy B.B solution is shifted supreme It presses in reaction kettle, hydro-thermal reaction 20h is carried out at 100 DEG C.To obtain metal phosphonic acid cerium hydridization carbon nanotube filtering, and spend from Son washing applies repeatedly, 60 DEG C of vacuum drying 20h.By 1 part of metal phosphonic acid cerium hydridization carbon nanotube, 4 parts of BDP, 2 parts of Mg (OH)2With 2 Part Al (OH)3It is placed in alcoholic solution, 2 parts of titanate coupling agents, 2 parts of gamma-aminopropyl-triethoxy-silanes, 50 DEG C of magnetic force is added Ultrasound 30min after stirring 30min, forced air drying volatilize solvent to obtain modified flame-retardant filler.
Embodiment 4 (fire-retardant PP preparation):
By the modified containing graphene fire-retardant filler of 2 parts of embodiments 2 and 4 parts of antioxidant four [β-(3,5- di-t-butyl -4- hydroxyls Base phenyl) propionic acid] the rubber toughened PP of crosslinking for preparing of pentaerythritol ester, 100 parts of embodiments 1 add twin-screw extrude by 150 DEG C of blendings prepare toughening flame-proof PP particle.Then, it is pressed and molded: appropriate toughening flame-proof PP particle is placed in dumbbell shape punching block It in tool, is placed in hot press, 160 DEG C of upper and lower mould temperature, 5Mpa preheating 10min is set, is pressurized to 10MP hot pressing 10min, leads to cold But water prepares tensile test batten to room temperature.Measure tensile strength be 19MPa, elongation at break 148%, impact strength, 12kJ/m2, Vicat softening point is 92 DEG C.Modified particle is placed in hopper and is injection moulded, and 160 DEG C of temperature, injection pressure 5MPa, at Type time 45s prepares the batten of test oxygen index (OI).Limit oxygen index (LOI) is 28% and vertical combustion refining (UL-94) reaches V- The test result of 2 ranks.
Comparative example 3 (fire-retardant PP preparation):
By the modified containing graphene fire-retardant filler of 2 parts of embodiments 2 and 4 parts of antioxidant four [β-(3,5- di-t-butyl -4- hydroxyls Base phenyl) propionic acid] the rubber toughened PP of crosslinking for preparing of pentaerythritol ester, 100 parts of comparative examples 1 add twin-screw extrude by 150 DEG C of blendings prepare toughening flame-proof PP particle.Then, it is pressed and molded: appropriate toughening flame-proof PP particle is placed in dumbbell shape punching block It in tool, is placed in hot press, 160 DEG C of upper and lower mould temperature, 5Mpa preheating 10min is set, is pressurized to 10MP hot pressing 10min, leads to cold But water prepares tensile test batten to room temperature.Measure tensile strength be 15MPa, elongation at break 163%, impact strength, 18kJ/m2, Vicat softening point is 90 DEG C.Modified particle is placed in hopper and is injection moulded, and 160 DEG C of temperature, injection pressure 5MPa, at Type time 45s prepares the batten of test oxygen index (OI).Limit oxygen index (LOI) is 28% and vertical combustion refining (UL-94) reaches V- The test result of 2 ranks.
Embodiment 5 (fire-retardant PP preparation):
4 parts of embodiments 3 are prepared into modified carbonaceous nanotube fire-retardant filler and 3 parts of antioxidant four [β-(3,5- bis- tertiary fourths Base -4- hydroxy phenyl) propionic acid] Toughened PP for preparing of pentaerythritol ester, 100 parts of embodiments 1 add twin-screw extrude by 150 DEG C of blendings prepare toughening flame-proof PP particle.Then, it is pressed and molded: appropriate toughening flame-proof PP particle is placed in dumbbell shape punching block It in tool, is placed in hot press, 160 DEG C of upper and lower mould temperature, 5Mpa preheating 10min is set, is pressurized to 10MP hot pressing 10min, leads to cold But water prepares tensile test batten to room temperature.Measuring tensile strength is 21MPa, elongation at break 157%, impact strength 16kJ/m2, Vicat softening point is 99 DEG C.Modified particle is placed in hopper and is injection moulded, and 160 DEG C of temperature, injection pressure 5MPa, at Type time 45s prepares the batten of test oxygen index (OI).Limit oxygen index (LOI) is 34% and vertical combustion refining (UL-94) reaches V- The test result of 1 rank.
Embodiment 6 (fire-retardant PP preparation):
2 parts of embodiments 2 are prepared into modified containing graphene fire-retardant filler, 2 parts of embodiments 3 are prepared into the resistance of modified carbonaceous nanotube Fire filler and 3 parts of antioxidant four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol ester, 100 parts of embodiments 1 The Toughened PP of preparation, which is added twin-screw extrude, prepares toughening flame-proof PP particle by 150 DEG C of blendings.Then, it is pressed and molded: Appropriate toughening flame-proof PP particle is placed in dumbbell shape steel mold, is placed in hot press, 160 DEG C of upper and lower mould temperature, 5Mpa are set 10min is preheated, 10MP hot pressing 10min is pressurized to, leads to cooling water to room temperature, prepares tensile test batten.Measure tensile strength For 16MPa, elongation at break 183%, impact strength 23kJ/m2, Vicat softening point is 102 DEG C.Modified particle is placed in hopper Middle injection moulding, prepares the batten of test oxygen index (OI) by 160 DEG C of temperature, injection pressure 5MPa, molding time 45s.Limit oxygen refers to Number (LOI) is 36% and vertical combustion refining (UL-94) reaches the test result of V-0 rank.
Embodiment 7 (preparation of toughening flame-proof PP casing):
2 parts of color masterbatch prepare PP with 98 parts of embodiments 6 and mix, through single screw extrusion machine melt production 2.3/1.6-12B1 specification Loose tube, the extruder body temperature are 190 DEG C, after trombone slide wears fibre, and high-speed production speed is that 200m/min enters cooling water Slot, sink length are 4m, and water temperature is 35 DEG C, subsequently enter heat treatment water-bath wheel and lead, and around full 5 circle, water temperature is 90 DEG C, after heat treatment Cooling is led into water-bath wheel, around full 5 circle, cooling temperature is 35 DEG C, and the laggard cold blowing-dry apparatus of inlet air, cooling temperature is 20 DEG C, with Enter admission machine drum afterwards.Optical fiber laying tension, casing drawing tension, casing takeup tension are respectively 100g, 600g, 1500g, Long 0.1-0.2 ‰ more than lateral pressure resistant value 1500N, 0h is measured, for 24 hours remaining long 0.2-0.3 ‰.
Comparative example 4 (pure PP casing preparation):
2 parts of color masterbatch are mixed with 98 parts of pure PP, through single screw extrusion machine melt production 2.3/1.6-12B1 specification Loose tube, institute Stating extruder body temperature is 190 DEG C, after trombone slide wears fibre, and high-speed production speed is that 200m/min enters cooling trough, and sink is long Degree is 4m, and water temperature is 35 DEG C, subsequently enters heat treatment water-bath wheel and leads, and around full 5 circle, water temperature is 90 DEG C, and water-bath is entered after heat treatment Wheel leads cooling, and around full 5 circle, cooling temperature is 35 DEG C, and the laggard cold blowing-dry apparatus of inlet air, cooling temperature is 20 DEG C, subsequently enters receipts Line machine drum.Optical fiber laying tension, casing drawing tension, casing takeup tension are respectively 100g, 600g, 1500g, measure anti-side Long 0.1-0.2 ‰ more than pressure value 753N, 0h, for 24 hours remaining long 0.2-0.3 ‰.
The above is only presently preferred embodiments of the present invention, is not intended to limit the present invention in any form, any ripe Professional and technical personnel is known, without departing from the scope of the present invention, according to the technical essence of the invention, to the above reality Any simple modifications, equivalent substitutions and improvements etc. made by example are applied, it is fallen within the scope of protection of the technical scheme of the present invention It is interior.

Claims (10)

1. a kind of polyacrylic preparation method of optical cable toughening flame-proof, it is characterised in that: the following steps are included:
1) by a certain amount of chlorinated scoline (CIIR), polyvinyl chloride (PVC), Dimeric Cyclopentadiene Carboxylic Acid sodium salt, antioxidant, Stabilizer, which is placed in mixer, carries out esterification realization crosslinking, obtains the crosslinking rubber with thermal reversibility；By the crosslinking rubber Glue and PP, crosslinking agent, stabilizer blend kneading machine after mixing, mixed material is added twin-screw extrude into extrusion Granulation obtains Toughened PP resin particle；
2) cerous nitrate aqueous solution will be added after phenyl-phosphonic acid aqueous solution and graphene or carbon nanotube sonic oscillation, after ultrasonic disperse Be transferred in autoclave, carry out hydro-thermal reaction, obtain metal phosphonic acid cerium hydridization graphene or carbon nanotube, filter, go from It is dried in vacuo after son washing；By a certain amount of metal phosphonic acid cerium hydridization graphene or carbon nanotube, mixing inorganic fire-retarded filler, idol Join agent and spirit solvent is uniformly mixed, and certain time ultrasonic disperse after mixing is blended by high speed shear dispersion machine, leads to Air dry oven is crossed to evaporate solvent to obtain coupling agent modified fire-retardant filler；
3) the Toughened PP resin for obtaining coupling agent modified fire-retardant filler, antioxidant and a certain amount of step 1) that step 2) obtains Particle mixing, by extruder, melting mixing obtains the fire-retardant PP particle for being uniformly mixed granulation at a certain temperature；
4) the fire-retardant PP particle by the uniformly mixed granulation that step 3) obtains is put into mold, with hot press and injection molding machine certain It is molded under temperature, pressure, batten is obtained after held for some time；
5) color masterbatch and fire-retardant PP is added to go out head by 50 single screw extrusion machine of φ by batten is casing, and casing goes out after head rapidly It is rapidly cooled into sink, leads and be heat-treated subsequently into the first water-bath wheel, the second water-bath wheel is entered after heat treatment and is led And air-blowing it is air-cooled again cool down after enter admission machine.
2. the polyacrylic preparation method of optical cable toughening flame-proof according to claim 1, it is characterised in that: press mass parts It counts, CIIR described in step 1) and PVC content are 100 parts altogether, and mass ratio is 80:20~90:10；Dimeric Cyclopentadiene Carboxylic Acid Sodium salt mass content is the 1~8% of CIIR；Stabilizer is calcium stearate, and content is the 1~5% of CIIR；Antioxidant is phosphorous Acid-benzene di-isooctyl (DPP), content are the 1~8% of CIIR；70~90 parts of PP, 10~30 parts of crosslinking rubber prepared.
3. the polyacrylic preparation method of optical cable toughening flame-proof according to claim 1, it is characterised in that: in step 1), Melting temperature is 140~190 DEG C, and 40~200r/min of revolving speed is kneaded 10~30min, 140~180 DEG C of extruder granulations.
4. the polyacrylic preparation method of optical cable toughening flame-proof according to claim 1, it is characterised in that: in step 2), The phenyl-phosphonic acid aqueous solution be 1~5mmol, cerous nitrate 1~4mmol of aqueous solution, ultrasonic disperse 10~40min, 100~ 150 DEG C of hydro-thermal reactions 10~20h, 50~80 DEG C of 10~20h of vacuum drying.
5. the polyacrylic preparation method of optical cable toughening flame-proof according to claim 1, it is characterised in that: step 2) is described Mixing inorganic fire-retarded filler be tetraphenyl diphenol A diphosphonate (BDP), graphene (GE), carbon nanotube, phosphonic acids rare-earth salts change Property graphene, phosphonic acids rare-earth salts modified carbon nano-tube, magnesium hydroxide (Mg (OH)2) and aluminium hydroxide (Al (OH)3) in it is a variety of mixed It closes；Coupling agent is one or more of titanate coupling agent, gamma-aminopropyl-triethoxy-silane, self-control rare earth titanium coupling agent.
6. the polyacrylic preparation method of optical cable toughening flame-proof according to claim 5, it is characterised in that: in step 2), In parts by mass, 3~9 parts of BPD, 1~5 part of Mg (OH) are taken2, 1~5 part of Al (OH)3, 1~5 part of GE, 1~5 part of carbon nanotube, 1~ 4 parts of titanate coupling agents, 1~4 part of gamma-aminopropyl-triethoxy-silane, 1~4 part of self-control rare earth titanium coupling agent, 30~60 DEG C of magnetic Power stirs 1~40min, 10~50min of ultrasound.
7. the polyacrylic preparation method of optical cable toughening flame-proof according to claim 1, it is characterised in that: in step 3), By 1~10 part of coupling agent modified fire-retardant filler, 1~5 part of antioxidant four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] Pentaerythritol ester, 100 parts of Toughened PP resin particles, 130~180 DEG C of extruder.
8. the polyacrylic preparation method of optical cable toughening flame-proof according to claim 1, it is characterised in that: in step 4), Compression molding condition are as follows: it is uniformly mixed the 10~30g of fire-retardant PP particle being granulated, 130~180 DEG C of upper and lower mould temperature, 4~ 10Mpa。
9. the polyacrylic preparation method of optical cable toughening flame-proof according to claim 1, it is characterised in that: step 5) is described The additive amount of color masterbatch is the 1~4% of batten quality, 190~240 DEG C of extrusion trombone slides of extruder.
10. the polyacrylic preparation method of optical cable toughening flame-proof according to claim 6, it is characterised in that: aoxidize 1 part Lanthanum and 5 parts of pyrophosphoric acid type titanate esters are added there-necked flask, and it is dilute to prepare self-control in 130 DEG C of reaction 5h with magnetic force oil bath heating Native titanium coupling agent.
CN201910630487.4A 2019-07-12 2019-07-12 A kind of polyacrylic preparation method of optical cable toughening flame-proof Pending CN110229420A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107383599A (en) * 2017-07-28 2017-11-24 江苏长海复合材料股份有限公司 A kind of environment protective and flame-retardant polypropelene material and preparation method thereof
CN107674275A (en) * 2017-11-01 2018-02-09 安徽美腾特种电缆材料有限公司 A kind of flame-proof anti-aging cable material
CN108503971A (en) * 2018-03-02 2018-09-07 上海利物盛企业集团有限公司 A kind of graphene conductive plastics and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107383599A (en) * 2017-07-28 2017-11-24 江苏长海复合材料股份有限公司 A kind of environment protective and flame-retardant polypropelene material and preparation method thereof
CN107674275A (en) * 2017-11-01 2018-02-09 安徽美腾特种电缆材料有限公司 A kind of flame-proof anti-aging cable material
CN108503971A (en) * 2018-03-02 2018-09-07 上海利物盛企业集团有限公司 A kind of graphene conductive plastics and preparation method thereof

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Application publication date: 20190913