CN106009382A - Phosphorous-modified flame-retardant optical cable material and preparation method thereof - Google Patents
Phosphorous-modified flame-retardant optical cable material and preparation method thereof Download PDFInfo
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- CN106009382A CN106009382A CN201610457164.6A CN201610457164A CN106009382A CN 106009382 A CN106009382 A CN 106009382A CN 201610457164 A CN201610457164 A CN 201610457164A CN 106009382 A CN106009382 A CN 106009382A
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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
- C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/04—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08L27/06—Homopolymers or copolymers of vinyl chloride
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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
- 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
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The invention discloses a phosphorous-modified flame-retardant optical cable material. The material is prepared from raw materials in parts by weight as follows: 2-3 parts of polyphenyl ether, 10-12 parts of wollastonite powder, 5-7 parts of tricresyl phosphate, 100-130 parts of polyvinyl chloride, 20-27 parts of polystyrene, 3-4 parts of sodium hypophosphite hydrate, 2-3 parts of paraformaldehyde, 0.2-0.3 parts of 35%-37% hydrochloric acid, 4-6 parts of dichloropentate, 5-7 parts of aluminium chloride hexahydrate, 0.1-0.2 parts of triethylamine, 1-2.3 parts of sodium butylnaphthylsulfonate, 2-4 parts of aluminium dihydrogen phosphate, 0.1-0.2 parts of butylmercaptooxo stannane, 0.3-1 part of N,N-diisopropylethanolamine, 0.7-1 part of polyimide and 0.1-0.2 parts of phytosterol. The material can realize effects of attenuating flames and reducing the temperature of a combustion zone and produces some phosphorus oxide radicals and the like which can capture radicals produced during splitting of polystyrene chain segments during splitting, the heat stability of the material is improved, and the heat release value of the material is reduced.
Description
Technical field
The present invention relates to mass technical field, particularly relate to a kind of phosphatization modified flame-retardant mass and preparation method thereof.
Background technology
In recent years, nanotechnology causes in flame retardant area and pays close attention to widely, and research shows that nano material only needs less addition (generally less than 5%), it becomes possible to reach flame retardant effect the most significantly.Therefore, the preparation of anti-flaming nano composite material is ingredient important in field of fire-proof technology, the green grass or young crops of the most vast research worker.Laminated inorganic matter nano material is one of packing material most effectively in anti-flaming nano composite material, when laminated inorganic matter nano material is that nanoscale is dispersed in macromolecular material matrix, and it can significantly improve the mechanical property of nano composite material, heat stability and fire resistance etc..
Conventional layered inorganic nanoparticle has: phyllosilicate (wearing soil, Muscovitum etc.), layered double-hydroxide (LDH), layered metal phosphates, GO and graphite are dilute.Its layered silicates and layered double-hydroxide are owing to easily being peeled off by intercalation, thus can improve its dispersion in macromolecule matrix, and the nano composite material preparing gained can significantly improve heat stability and the anti-flammability of material, has the highest application prospect.Layered metal phosphates also has relevant report in flame retardant area, main research bedded zirconium phosphate and the impact on nano composite material combination property of the stratiform titanium phosphate.
Simultaneously, hypo-aluminum orthophosphate is as one of more efficient fire retardant in engineering plastics in recent years, it can produce hydrogen phosphide and relatively stable pyrophosphate condensed phase residue when cracking, can remarkably promote macromolecule matrix becomes charcoal to stop the further burning of material, thus promotes the fire resistance of macromolecule matrix.Research shows, hypo-aluminum orthophosphate is widely used in the fire-retardant of the macromolecular materials such as ethylene glycol terephthalate, mutual-phenenyl two acid bromide two alcohol ester, polylactic acid, polyvinyl alcohol and polyamide, and can reach good effect in commercial Application.Therefore, the preparation organic trick of stratiform both can play the iris action of stratiform lamella, can produce, during its cracking, the compound promoting that polymer becomes charcoal simultaneously, and its resultant effect can be effectively improved fire resistance and the heat stability of nano composite material；
The more also material such as double-hydroxide (LDH) and graphite refining is studied in lamellar compound/flame-retardant polystyrene nano-composite material field.Research shows that the LDH of modification can be significantly increased the heat stability of composite with in good condition being dispersed in polystyrene matrix peeled off, and owing to lamella iris action can reduce peak heat release and the total heat release of material, improves the fire safety evaluating performance of material.
But substantial amounts of interpolation result in the phenomenon that modified particle occurs reuniting in matrix resin, can affect the combination property of polystyrene.In addition, the nano material such as carbon nanotube, metal oxide nano-wire and metal oxide nanoparticles can promote the polystyrene nano composite material catalysis carbon-forming when burning, thus improves the fire resistance of material.Therefore, research nanometer composite technology has important scientific meaning to impact and the fire retardant mechanism thereof of the fire resistance of polystyrene.
Summary of the invention
The object of the invention is contemplated to make up the defect of prior art, it is provided that a kind of phosphatization modified flame-retardant mass and preparation method thereof.
The present invention is achieved by the following technical solutions:
A kind of phosphatization modified flame-retardant mass, it is made up of the raw material of following weight parts:
Polyphenylene oxide 2-3, wollastonite in powder 10-12, tricresyl phosphate 5-7, polrvinyl chloride 100-130, polystyrene 20-2 mono-waterside sodium phosphate 3-4, the hydrochloric acid 0.2-0.3 of paraformaldehyde 2-3,35-37%, dichloropentate 4-6, Aluminium chloride hexahydrate 5-7, triethylamine 0.1-0.2, sodium butylnaphthalenesulfonate 1-2.3, aluminium dihydrogen phosphate 2-4, butanethiol stannum 0.1-0.2, diisopropyl ethanolamine 0.3-1, polyimides 0.7-1, plant sterol 0.1-0.2.
The preparation method of a kind of described phosphatization modified flame-retardant mass, comprises the following steps:
(1) an above-mentioned waterside sodium phosphate is taken; join in the deionized water of its weight 50-70 times; stir, send in the water bath with thermostatic control of 76-80 DEG C, be slowly added to above-mentioned paraformaldehyde; the hydrochloric acid of above-mentioned 35-37% is added under stirring condition; insulated and stirred 8-9 hour under nitrogen protection, discharging cools down, sucking filtration; it will be vacuum dried 10-12 hour at being deposited in 80-85 DEG C, obtains hydroxyalkylation phosphinic acid；
(2) above-mentioned hydroxyalkylation phosphinic acid are joined in the oxolane of its weight 40-50 times, stir, obtain the tetrahydrofuran solution of organic phosphoric acid；
(3) by above-mentioned dichloropentate, triethylamine mixing; join in the oxolane of compound weight 70-80 times; rise high-temperature and be 37-40 DEG C; insulated and stirred 20-30 minute, mixes with the tetrahydrofuran solution of above-mentioned organic phosphoric acid, rises high-temperature and is 60-65 DEG C; insulated and stirred 20-21 hour under nitrogen protection; it is filtered to remove precipitation, filtrate reduced in volume is removed oxolane, obtain polymerization organic phospho acid；
(4) above-mentioned tricresyl phosphate is joined in the toluene of its weight 3-5 times, stir, add butanethiol stannum, insulated and stirred 7-10 minute at 50-60 DEG C, obtain benzole soln；
(5) by above-mentioned aluminium dihydrogen phosphate, sodium butylnaphthalenesulfonate mixing, join in the deionized water of compound weight 5-7 times, stir, obtain saline solution；
(6) above-mentioned Aluminium chloride hexahydrate is joined in the deionized water of its weight 20-30 times, add plant sterol, stir, obtain aluminum dispersion liquid；
(7) take above-mentioned polymerization organic phospho acid, join in the deionized water of its weight 70-80 times, stir, dropping acetic acid or sodium hydroxide, regulation pH is 4-5, rises high-temperature and is 80-85 DEG C, it is slowly added to above-mentioned aluminum dispersion liquid, insulated and stirred 6-7 hour, adds above-mentioned saline solution, stirs, sucking filtration, filter cake is washed 3-4 time, is vacuum dried 30-40 minute at 50-60 DEG C, obtains organic layer phosphonic acids aluminum；
(8) above-mentioned organic layer phosphonic acids aluminum is taken, join in the toluene of its weight 70-80 times, add above-mentioned benzole soln, ultrasonic 20-30 minute, add above-mentioned polystyrene, polyimides, diisopropyl ethanolamine, continue ultrasonic 10-14 minute, rise high-temperature and be 57-60 DEG C, insulated and stirred 1.5-2 hour, drying under reduced pressure, obtain described compounded mix；
(9) above-mentioned compounded mix is mixed with remaining each raw material, stir, send into extruder, through melt extruding, cooling, pelletize, obtain described mass.
The invention have the advantage that to add the organic layer phosphonic acids aluminum of the present invention to and polystyrene is prepared fire proofing, due to special laminar structured of stratiform organic aluminum phosphate, it disperses in macromolecule matrix uniformly, lamella iris action is effectively played when burning occurs, stop the entrance of extraneous fuel, the chain degradation process of suppression macromolecule matrix, some components such as C02 produced when it is heated pyrolysis, CO, the gases such as phosphorus-containing compound, they can play dilution flame, reduce the effect of combustion zone temperature, and cracking time produce some phosphorus oxygen free radicals etc. can capture polystyrene segment cracking produce free radical,
Improve heat decomposition temperature and the neat coal amout of material, promote the heat stability of material, the continuation degraded of termination material, reduces the hot release value of material.Simultaneously, organic layer phosphonic acids aluminum also can promote, when degraded, the fine and close layer of charcoal that copolymer generating portion is stable, thus reduce the degradation rate of polymeric matrix and therefore inhibit the entrance of imflammable gas, slow down proceeding of burning, improve the fire safety of material.Optical cable material has good hydrophobicity, resistance to acids and bases, excellent storage stability, and service life is long.
Detailed description of the invention
A kind of phosphatization modified flame-retardant mass, it is made up of the raw material of following weight parts:
Polyphenylene oxide 2, wollastonite in powder 10, tricresyl phosphate 5, polrvinyl chloride 100, polystyrene 20 1 waterside sodium phosphate 3, the hydrochloric acid 0.2 of paraformaldehyde 2,35%, dichloropentate 4, Aluminium chloride hexahydrate 5, triethylamine 0.1, sodium butylnaphthalenesulfonate 1, aluminium dihydrogen phosphate 2, butanethiol stannum 0.1, diisopropyl ethanolamine 0.3, polyimides 0.7, plant sterol 0.1.
The preparation method of a kind of described phosphatization modified flame-retardant mass, comprises the following steps:
(1) an above-mentioned waterside sodium phosphate is taken; join in the deionized water of its weight 50 times; stir, send in the water bath with thermostatic control of 76 DEG C, be slowly added to above-mentioned paraformaldehyde; the hydrochloric acid of above-mentioned 35% is added under stirring condition; insulated and stirred 8 hours under nitrogen protection, discharging cools down, sucking filtration; vacuum drying 10 hours will be deposited at 80 DEG C, obtain hydroxyalkylation phosphinic acid；
(2) above-mentioned hydroxyalkylation phosphinic acid are joined in the oxolane of its weight 40 times, stir, obtain the tetrahydrofuran solution of organic phosphoric acid；
(3) by above-mentioned dichloropentate, triethylamine mixing; join in the oxolane of compound weight 70 times; rising high-temperature is 37 DEG C; insulated and stirred 20 minutes, mixes with the tetrahydrofuran solution of above-mentioned organic phosphoric acid, and rising high-temperature is 60 DEG C; insulated and stirred 20 hours under nitrogen protection; it is filtered to remove precipitation, filtrate reduced in volume is removed oxolane, obtain polymerization organic phospho acid；
(4) being joined by above-mentioned tricresyl phosphate in the toluene of its weight 3 times, stir, add butanethiol stannum, at 50 DEG C, insulated and stirred 7 minutes, obtain benzole soln；
(5) by above-mentioned aluminium dihydrogen phosphate, sodium butylnaphthalenesulfonate mixing, join in the deionized water of compound weight 5 times, stir, obtain saline solution；
(6) above-mentioned Aluminium chloride hexahydrate is joined in the deionized water of its weight 20 times, add plant sterol, stir, obtain aluminum dispersion liquid；
(7) take above-mentioned polymerization organic phospho acid, join in the deionized water of its weight 70 times, stir, dropping acetic acid or sodium hydroxide, regulation pH is 4, and rising high-temperature is 80 DEG C, it is slowly added to above-mentioned aluminum dispersion liquid, insulated and stirred 6 hours, adds above-mentioned saline solution, stirs, sucking filtration, filter cake is washed 3 times, is vacuum dried 30 minutes at 50 DEG C, obtains organic layer phosphonic acids aluminum；
(8) above-mentioned organic layer phosphonic acids aluminum is taken, join in the toluene of its weight 70 times, add above-mentioned benzole soln, ultrasonic 20 minutes, add above-mentioned polystyrene, polyimides, diisopropyl ethanolamine, continue ultrasonic 10 minutes, rising high-temperature is 57 DEG C, insulated and stirred 1.5 hours, drying under reduced pressure, obtain described compounded mix；
(9) above-mentioned compounded mix is mixed with remaining each raw material, stir, send into extruder, through melt extruding, cooling, pelletize, obtain described mass.
Performance test:
Hot strength: 19.6 MPa；
Low temperature brittleness impact temperature (DEG C) :-30 DEG C are passed through；
Fire-retardant rank: V-0；
After 100 DEG C × 240h hot air aging: hot strength rate of change (%)-7.6；
Extension at break rate of change (%)-8.0.
Claims (2)
1. a phosphatization modified flame-retardant mass, it is characterised in that it is made up of the raw material of following weight parts:
Polyphenylene oxide 2-3, wollastonite in powder 10-12, tricresyl phosphate 5-7, polrvinyl chloride 100-130, polystyrene 20-27, a waterside sodium phosphate 3-4, the hydrochloric acid 0.2-0.3 of paraformaldehyde 2-3,35-37%, dichloropentate 4-6, Aluminium chloride hexahydrate 5-7, triethylamine 0.1-0.2, sodium butylnaphthalenesulfonate 1-2.3, aluminium dihydrogen phosphate 2-4, butanethiol stannum 0.1-0.2, diisopropyl ethanolamine 0.3-1, polyimides 0.7-1, plant sterol 0.1-0.2.
2. the preparation method of a phosphatization modified flame-retardant mass as claimed in claim 1, it is characterised in that comprise the following steps:
(1) an above-mentioned waterside sodium phosphate is taken; join in the deionized water of its weight 50-70 times; stir, send in the water bath with thermostatic control of 76-80 DEG C, be slowly added to above-mentioned paraformaldehyde; the hydrochloric acid of above-mentioned 35-37% is added under stirring condition; insulated and stirred 8-9 hour under nitrogen protection, discharging cools down, sucking filtration; it will be vacuum dried 10-12 hour at being deposited in 80-85 DEG C, obtains hydroxyalkylation phosphinic acid；
(2) above-mentioned hydroxyalkylation phosphinic acid are joined in the oxolane of its weight 40-50 times, stir, obtain the tetrahydrofuran solution of organic phosphoric acid；
(3) by above-mentioned dichloropentate, triethylamine mixing; join in the oxolane of compound weight 70-80 times; rise high-temperature and be 37-40 DEG C; insulated and stirred 20-30 minute, mixes with the tetrahydrofuran solution of above-mentioned organic phosphoric acid, rises high-temperature and is 60-65 DEG C; insulated and stirred 20-21 hour under nitrogen protection; it is filtered to remove precipitation, filtrate reduced in volume is removed oxolane, obtain polymerization organic phospho acid；
(4) above-mentioned tricresyl phosphate is joined in the toluene of its weight 3-5 times, stir, add butanethiol stannum, insulated and stirred 7-10 minute at 50-60 DEG C, obtain benzole soln；
(5) by above-mentioned aluminium dihydrogen phosphate, sodium butylnaphthalenesulfonate mixing, join in the deionized water of compound weight 5-7 times, stir, obtain saline solution；
(6) above-mentioned Aluminium chloride hexahydrate is joined in the deionized water of its weight 20-30 times, add plant sterol, stir, obtain aluminum dispersion liquid；
(7) take above-mentioned polymerization organic phospho acid, join in the deionized water of its weight 70-80 times, stir, dropping acetic acid or sodium hydroxide, regulation pH is 4-5, rises high-temperature and is 80-85 DEG C, it is slowly added to above-mentioned aluminum dispersion liquid, insulated and stirred 6-7 hour, adds above-mentioned saline solution, stirs, sucking filtration, filter cake is washed 3-4 time, is vacuum dried 30-40 minute at 50-60 DEG C, obtains organic layer phosphonic acids aluminum；
(8) above-mentioned organic layer phosphonic acids aluminum is taken, join in the toluene of its weight 70-80 times, add above-mentioned benzole soln, ultrasonic 20-30 minute, add above-mentioned polystyrene, polyimides, diisopropyl ethanolamine, continue ultrasonic 10-14 minute, rise high-temperature and be 57-60 DEG C, insulated and stirred 1.5-2 hour, drying under reduced pressure, obtain described compounded mix；
(9) above-mentioned compounded mix is mixed with remaining each raw material, stir, send into extruder, through melt extruding, cooling, pelletize, obtain described mass.
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| CN201610457164.6A CN106009382A (en) | 2016-06-22 | 2016-06-22 | Phosphorous-modified flame-retardant optical cable material and preparation method thereof |
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| CN201610457164.6A CN106009382A (en) | 2016-06-22 | 2016-06-22 | Phosphorous-modified flame-retardant optical cable material and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108285560A (en) * | 2018-02-24 | 2018-07-17 | 四会市启德信息咨询服务有限公司 | A kind of phosphorylation is modified the preparation method of compound high ductility accumulator housing |
| CN108299770A (en) * | 2018-02-24 | 2018-07-20 | 四会市启德信息咨询服务有限公司 | A kind of compound high ductility accumulator housing of phosphorylation modification |
-
2016
- 2016-06-22 CN CN201610457164.6A patent/CN106009382A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108285560A (en) * | 2018-02-24 | 2018-07-17 | 四会市启德信息咨询服务有限公司 | A kind of phosphorylation is modified the preparation method of compound high ductility accumulator housing |
| CN108299770A (en) * | 2018-02-24 | 2018-07-20 | 四会市启德信息咨询服务有限公司 | A kind of compound high ductility accumulator housing of phosphorylation modification |
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