CN105936717A - Aerogel modified flame-retardant optical cable material and preparation method thereof - Google Patents
Aerogel modified flame-retardant optical cable material and preparation method thereof Download PDFInfo
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- CN105936717A CN105936717A CN201610457200.9A CN201610457200A CN105936717A CN 105936717 A CN105936717 A CN 105936717A CN 201610457200 A CN201610457200 A CN 201610457200A CN 105936717 A CN105936717 A CN 105936717A
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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
- 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
- C08L2205/03—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 an aerogel modified flame-retardant optical cable material, which is composed of the following raw materials in parts by weight: 0.4 to 1 part of hexamethyl phosphoric triamide, 3 to 4 parts of polyamide wax micropowder, 0.3 to 0.5 part of lithium silicate, 0.1 to 0.2 part of trihydroxymethyl propane, 100 to 130 parts of polyvinyl chloride, 3 to 4 parts of polystyrene 20-2 sodium hypophosphite monohydrate, 2 to 3 parts of paraformaldehyde, 0.2 to 0.3 part of hydrochloric acid (35-37%), 4 to 6 parts of chlorinated spiro-phosphate, 5 to 7 parts of aluminum chloride hexahydrate, 0.1 to 0.2 part of triethylamine, 0.7 to 1 part of saturated stearamide, 3 to 4 parts of silicon dioxide aerogel, 8 to 10 parts of talcum powder, and 0.1 to 0.2 part of diamino diphenyl ether. The provided optical cable material can dilute the flame and reduce the temperature of combustion area; at the same time, phosphor and oxygen free radicals generated during the cracking process can capture free radicals that are generated by cracking polystyrene chain segments, thus the thermal stability of the optical cable 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 aeroge 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 aeroge modified flame-retardant mass and preparation method thereof.
The present invention is achieved by the following technical solutions:
A kind of aeroge modified flame-retardant mass, it is made up of the raw material of following weight parts:
HMPA 0.4-1, polyamide wax micropowder 3-4, Lithium metasilicate 0.3-0.5, trimethylolpropane 0.1-0.2, 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, saturated octadecanoyl amine 0.7-1, aerosil 3-4, Pulvis Talci 8-10, diaminodiphenyl ether 0.1-0.2.
The preparation method of a kind of described aeroge 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 saturated octadecanoyl amine is joined in the deionized water of its weight 27-30 times, stir, addition aerosil, ultrasonic 1-2 minute, gel dispersion liquid of bringing about the desired sensation；
(5) above-mentioned Aluminium chloride hexahydrate is joined in the deionized water of its weight 20-30 times, stir；
(6) 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, drip the aqueous solution of above-mentioned Aluminium chloride hexahydrate, after dropping, add above-mentioned Lithium metasilicate, insulated and stirred 6-7 hour, add above-mentioned aeroge dispersion liquid, 100-200 rev/min is stirred 4-7 minute, and filter cake is washed 3-4 time by sucking filtration, it is vacuum dried 30-40 minute at 50-60 DEG C, obtains organic layer phosphonic acids aluminum；
(7) above-mentioned polyamide wax micropowder is joined in the toluene of its weight 5-7 times, send in the oil bath of 110-120 DEG C, insulated and stirred 10-14 minute, discharging, mix with above-mentioned HMPA, stirring, to room temperature, obtains premix benzole soln；
(8) above-mentioned organic layer phosphonic acids aluminum is taken, join in the toluene of its weight 70-80 times, add above-mentioned premix benzole soln, ultrasonic 20-30 minute, add above-mentioned polystyrene, diaminodiphenyl ether, 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.Present invention adds aerosil, can effectively improve filler grain dispersibility in the polymer, and stability and the surface strength of finished product can be improved.
Detailed description of the invention
A kind of aeroge modified flame-retardant mass, it is made up of the raw material of following weight parts:
HMPA 0.4, polyamide wax micropowder 3, Lithium metasilicate 0.3, trimethylolpropane 0.1, 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, saturated octadecanoyl amine 0.7, aerosil 3, Pulvis Talci 8, diaminodiphenyl ether 0.1.
The preparation method of a kind of described aeroge 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) above-mentioned saturated octadecanoyl amine is joined in the deionized water of its weight 27 times, stir, addition aerosil, ultrasonic 1 minute, gel dispersion liquid of bringing about the desired sensation；
(5) above-mentioned Aluminium chloride hexahydrate is joined in the deionized water of its weight 20 times, stir；
(6) 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, drip the aqueous solution of above-mentioned Aluminium chloride hexahydrate, after dropping, add above-mentioned Lithium metasilicate, insulated and stirred 6 hours, add above-mentioned aeroge dispersion liquid, 100 revs/min are stirred 4 minutes, and filter cake is washed 3 times by sucking filtration, it is vacuum dried 30 minutes at 50 DEG C, obtains organic layer phosphonic acids aluminum；
(7) above-mentioned polyamide wax micropowder is joined in the toluene of its weight 5 times, send in the oil bath of 110 DEG C, insulated and stirred 10 minutes, discharging, mix with above-mentioned HMPA, stirring, to room temperature, obtains premix benzole soln；
(8) above-mentioned organic layer phosphonic acids aluminum is taken, join in the toluene of its weight 70 times, add above-mentioned premix benzole soln, ultrasonic 20 minutes, add above-mentioned polystyrene, diaminodiphenyl ether, 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. an aeroge modified flame-retardant mass, it is characterised in that it is made up of the raw material of following weight parts:
HMPA 0.4-1, polyamide wax micropowder 3-4, Lithium metasilicate 0.3-0.5, trimethylolpropane 0.1-0.2, 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, saturated octadecanoyl amine 0.7-1, aerosil 3-4, Pulvis Talci 8-10, diaminodiphenyl ether 0.1-0.2.
2. the preparation method of an aeroge 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 saturated octadecanoyl amine is joined in the deionized water of its weight 27-30 times, stir, addition aerosil, ultrasonic 1-2 minute, gel dispersion liquid of bringing about the desired sensation；
(5) above-mentioned Aluminium chloride hexahydrate is joined in the deionized water of its weight 20-30 times, stir；
(6) 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, drip the aqueous solution of above-mentioned Aluminium chloride hexahydrate, after dropping, add above-mentioned Lithium metasilicate, insulated and stirred 6-7 hour, add above-mentioned aeroge dispersion liquid, 100-200 rev/min is stirred 4-7 minute, and filter cake is washed 3-4 time by sucking filtration, it is vacuum dried 30-40 minute at 50-60 DEG C, obtains organic layer phosphonic acids aluminum；
(7) above-mentioned polyamide wax micropowder is joined in the toluene of its weight 5-7 times, send in the oil bath of 110-120 DEG C, insulated and stirred 10-14 minute, discharging, mix with above-mentioned HMPA, stirring, to room temperature, obtains premix benzole soln；
(8) above-mentioned organic layer phosphonic acids aluminum is taken, join in the toluene of its weight 70-80 times, add above-mentioned premix benzole soln, ultrasonic 20-30 minute, add above-mentioned polystyrene, diaminodiphenyl ether, 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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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107236287A (en) * | 2017-05-27 | 2017-10-10 | 清远初曲智能科技有限公司 | A kind of new aeroge enhancing nylon heat-insulation composite material and preparation method thereof |
| CN108676288A (en) * | 2018-06-05 | 2018-10-19 | 安徽艾伊德动力科技有限公司 | A kind of heat-resisting pdu wire harness sheaths material and preparation method thereof |
-
2016
- 2016-06-22 CN CN201610457200.9A patent/CN105936717A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107236287A (en) * | 2017-05-27 | 2017-10-10 | 清远初曲智能科技有限公司 | A kind of new aeroge enhancing nylon heat-insulation composite material and preparation method thereof |
| CN108676288A (en) * | 2018-06-05 | 2018-10-19 | 安徽艾伊德动力科技有限公司 | A kind of heat-resisting pdu wire harness sheaths material and preparation method thereof |
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Application publication date: 20160914 |