CN114276608A - Halogen-free flame-retardant heat-resistant cable material and preparation method thereof - Google Patents
Halogen-free flame-retardant heat-resistant cable material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 83
- 239000003063 flame retardant Substances 0.000 title claims abstract description 58
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 86
- 229920001276 ammonium polyphosphate Polymers 0.000 claims abstract description 58
- 239000004114 Ammonium polyphosphate Substances 0.000 claims abstract description 53
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims abstract description 53
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 45
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 26
- 238000002156 mixing Methods 0.000 claims abstract description 17
- 239000005038 ethylene vinyl acetate Substances 0.000 claims abstract description 7
- 238000000465 moulding Methods 0.000 claims abstract description 7
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 229910052681 coesite Inorganic materials 0.000 claims description 15
- 229910052906 cristobalite Inorganic materials 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 15
- 239000008187 granular material Substances 0.000 claims description 15
- 229910052682 stishovite Inorganic materials 0.000 claims description 15
- 229910052905 tridymite Inorganic materials 0.000 claims description 15
- 239000002131 composite material Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 10
- 238000001125 extrusion Methods 0.000 claims description 10
- 238000001746 injection moulding Methods 0.000 claims description 10
- 239000004433 Thermoplastic polyurethane Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 229920002803 thermoplastic polyurethane Polymers 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000000314 lubricant Substances 0.000 claims description 7
- 230000004048 modification Effects 0.000 claims description 7
- 238000012986 modification Methods 0.000 claims description 7
- 229920001610 polycaprolactone Polymers 0.000 claims description 7
- 239000004632 polycaprolactone Substances 0.000 claims description 7
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 125000002924 primary amino group Chemical class [H]N([H])* 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 229920009204 Methacrylate-butadiene-styrene Polymers 0.000 claims description 2
- WWNGFHNQODFIEX-UHFFFAOYSA-N buta-1,3-diene;methyl 2-methylprop-2-enoate;styrene Chemical group C=CC=C.COC(=O)C(C)=C.C=CC1=CC=CC=C1 WWNGFHNQODFIEX-UHFFFAOYSA-N 0.000 claims description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 2
- RKISUIUJZGSLEV-UHFFFAOYSA-N n-[2-(octadecanoylamino)ethyl]octadecanamide Chemical group CCCCCCCCCCCCCCCCCC(=O)NCCNC(=O)CCCCCCCCCCCCCCCCC RKISUIUJZGSLEV-UHFFFAOYSA-N 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 229920001897 terpolymer Polymers 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 6
- 229920005989 resin Polymers 0.000 abstract description 5
- 239000011347 resin Substances 0.000 abstract description 5
- 230000007062 hydrolysis Effects 0.000 abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 3
- 239000011159 matrix material Substances 0.000 abstract description 3
- 230000005012 migration Effects 0.000 abstract description 2
- 238000013508 migration Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 10
- 239000012796 inorganic flame retardant Substances 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000012496 blank sample Substances 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000005543 nano-size silicon particle Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- 229920002943 EPDM rubber Polymers 0.000 description 2
- 239000004743 Polypropylene Substances 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- -1 polypropylene Polymers 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- HIVGXUNKSAJJDN-UHFFFAOYSA-N [Si].[P] Chemical compound [Si].[P] HIVGXUNKSAJJDN-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical group [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- 229940043315 aluminum hydroxide / magnesium hydroxide Drugs 0.000 description 1
- SXSTVPXRZQQBKQ-UHFFFAOYSA-M aluminum;magnesium;hydroxide;hydrate Chemical compound O.[OH-].[Mg].[Al] SXSTVPXRZQQBKQ-UHFFFAOYSA-M 0.000 description 1
- HHSPVTKDOHQBKF-UHFFFAOYSA-J calcium;magnesium;dicarbonate Chemical compound [Mg+2].[Ca+2].[O-]C([O-])=O.[O-]C([O-])=O HHSPVTKDOHQBKF-UHFFFAOYSA-J 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
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- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000011256 inorganic filler Substances 0.000 description 1
- 229910003475 inorganic filler Inorganic materials 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000002028 premature Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
- Insulated Conductors (AREA)
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Abstract
The invention relates to a halogen-free flame-retardant heat-resistant cable material and a preparation method thereof. Finally, mixing the ethylene-vinyl acetate copolymer with the flame retardant, and molding to obtain the halogen-free flame-retardant heat-resistant cable material product with excellent performance. The prepared cable material overcomes the defects of poor compatibility of common ammonium polyphosphate and a resin matrix and easy hydrolysis and migration; due to the addition of the silicon dioxide, the heat resistance of the cable material is further improved on the basis of improving the flame retardant property of the cable material.
Description
Technical Field
The invention relates to the technical field of flame-retardant materials, in particular to a halogen-free flame-retardant heat-resistant cable material and a preparation method thereof.
Background
In the development of insulating layers and sheathing materials of electric wires and cables, the early widely used halogen flame retardant has the remarkable advantages of high flame retardant efficiency, small using amount and low price, but the halogen flame retardant can release toxic gas when burning, thereby causing harm to human bodies. Therefore, it is very important to develop a high-performance halogen-free flame-retardant heat-resistant cable material.
At present, the main method for preparing the halogen-free flame-retardant heat-resistant cable material is to add inorganic flame retardants, such as aluminum hydroxide/magnesium hydroxide, ammonium polyphosphate, expanded graphite and the like. Chinese patent CN 110591213A discloses a low-smoke density high-flame-retardant halogen-free cable material and a preparation method thereof, wherein an inorganic flame retardant is aluminum hydroxide and calcium magnesium carbonate ore which are compounded for use, the surface of the inorganic flame retardant is subjected to surface treatment by using a silane coupling agent, and meanwhile, a nano flame-retardant technology is applied to the halogen-free cable material by adding a nano catalyst into resin, so that the cable material with excellent flame-retardant property is prepared. However, the use amount of the inorganic flame retardant is too large and even exceeds the use amount of the resin, so that the processing process is difficult to perform on one hand; on the other hand, too much inorganic filler can deteriorate the comprehensive properties, especially the mechanical properties, of the cable material. Chinese patent CN 106566097A discloses a high-temperature halogen-free flame-retardant polypropylene/ethylene propylene diene monomer cable material and a preparation method thereof, ammonium polyphosphate is added into ethylene propylene diene monomer and polypropylene as an inorganic flame retardant to prepare a flame-retardant cable material composite material with good comprehensive performance. Due to the existence of hydrogen bond action in the ammonium polyphosphate, the ammonium polyphosphate has the characteristic of high hygroscopicity, so that the permeability of the base material is changed, and under the condition of high humidity, water vapor often corrodes the material, so that the ammonium polyphosphate in the base material is dissolved and migrates outwards, and the performance of the material is reduced.
Disclosure of Invention
The invention aims to provide a halogen-free flame-retardant heat-resistant cable material and a preparation method thereof aiming at the defects of the prior art. The method is characterized in that silicon dioxide and thermoplastic polyurethane are used as shells, ammonium polyphosphate is used as a core, and the ammonium polyphosphate is modified in a micro-encapsulation mode through an ion exchange reaction of the ammonium polyphosphate. Finally, mixing the ethylene-vinyl acetate copolymer with the flame retardant, and molding to obtain the halogen-free flame-retardant heat-resistant cable material product with excellent performance. The prepared cable material overcomes the defects of poor compatibility of common ammonium polyphosphate and a resin matrix and easy hydrolysis and migration; due to the addition of the silicon dioxide, the heat resistance of the cable material is further improved on the basis of improving the flame retardant property of the cable material.
1. The invention provides a preparation method of a halogen-free flame-retardant heat-resistant cable material, which is characterized by comprising the following steps:
(1) microencapsulation modification of ammonium polyphosphate (APP): step 1, 20 g of silicon dioxide is added into 150ml of absolute ethyl alcohol and 40ml of deionized water, the mixture is moved into a three-neck flask after being subjected to ultrasonic treatment for 10 min, then 40 g of silane coupling agent KH 550 is slowly dripped into the three-neck flask, the mixture is heated to 75 ℃ and stirred for 24 h, and silicon dioxide (NH) with primary amine on the surface is prepared2-SiO2) (ii) a Step 2, 10 g of APP was added to a three-necked flask filled with ethanol, and then heated to 90 ℃ to add 48g of NH2-SiO2Adding into a three-neck bottle, reacting for 4h to obtain silicon dioxide coated ammonium polyphosphate (NH)2-SiO2-APP); step 3, adding 25 g of polycaprolactone into a three-neck flask, drying at 120 ℃ for 24 h, mixing with 12.8 g of 4, 4-diphenylmethane diisocyanate, heating to 85 ℃ for reaction, reacting for 2 h, adding 1, 4-butanediol and NH2-SiO2APP is placed into a 120 ℃ oven for drying and curing after being uniformly stirred to prepare microencapsulated ammonium polyphosphate with silicon dioxide and thermoplastic polyurethane as shells and ammonium polyphosphate as cores;
(2) the preparation method of the halogen-free flame-retardant heat-resistant cable material comprises the following steps: 100 parts of ethylene-vinyl acetate copolymer, 20-30 parts of microencapsulated ammonium polyphosphate, 0.5-1.5 parts of lubricant and 5-10 parts of compatilizer are mixed in a mixing cylinder for 3-5 min, the materials are fully mixed in the mixing cylinder and are mixed for 3-5 min at the rotating speed of 80-120 r/min to obtain a premixed material, the obtained premixed material is added into a double-screw extruder through a main feeding port, and the premixed material is subjected to melt extrusion, cooling, drying and grain cutting to obtain flame-retardant cable material composite material granules, the obtained granules are added into an injection molding machine, the temperature is 170-190 ℃, and the flame-retardant cable material composite material granules are subjected to heating melting, extrusion, injection molding and molding.
2. The halogen-free flame-retardant heat-resistant cable material and the preparation method thereof are characterized in that the silicon dioxide is nano silicon dioxide, the particle size range of the nano silicon dioxide is 300-500 nm, and the surface of the nano silicon dioxide is provided with hydroxyl.
3. The halogen-free flame-retardant heat-resistant cable material and the preparation method thereof are characterized in that the molecular weight of the polycaprolactone is 2000.
4. The halogen-free flame-retardant heat-resistant cable material and the preparation method thereof are characterized in that the molecular weight of the ammonium polyphosphate is more than 1000.
5. The halogen-free flame-retardant heat-resistant cable material and the preparation method thereof are characterized in that the compatilizer is methyl methacrylate-butadiene-styrene terpolymer (MBS).
6. The halogen-free flame-retardant heat-resistant cable material and the preparation method thereof are characterized in that the lubricant is N, N' -Ethylene Bis Stearamide (EBS).
Compared with the prior art, the invention has the following positive effects:
(1) silicon dioxide and thermoplastic polyurethane are used as shells, ammonium polyphosphate is used as a core, ammonium polyphosphate is subjected to microencapsulation modification by using the ion exchange reaction of the ammonium polyphosphate, and the obtained flame retardant does not contain halogen. Due to the existence of thermoplastic polyurethane, the prepared cable material overcomes the defect that the mechanical property of the cable material is reduced due to poor compatibility of common ammonium polyphosphate and a resin matrix;
(2) due to the addition of the silicon dioxide, a phosphorus-silicon synergistic flame retardant system is constructed in the cable material composite material, the defect that the thermal stability of the material is reduced due to premature decomposition of a phosphorus flame retardant is overcome, and the heat resistance of the cable material is greatly improved;
(3) the microencapsulation of the ammonium polyphosphate can also improve the defects of high hygroscopicity and easy hydrolysis of the ammonium polyphosphate, and greatly improve the comprehensive performance of the cable material.
Detailed Description
The present invention is described in detail by the following embodiments, it should be noted that the following embodiments are only used for further illustration of the present invention, and should not be construed as limiting the scope of the present invention, and those skilled in the art can make some insubstantial modifications and adaptations based on the above disclosure, and still fall within the scope of the present invention.
Example 1:
(1) microencapsulation modification of ammonium polyphosphate (APP): step 1, 20 g of silicon dioxide is added into 150ml of absolute ethyl alcohol and 40ml of deionized water, the mixture is moved into a three-neck flask after being subjected to ultrasonic treatment for 10 min, then 40 g of silane coupling agent KH 550 is slowly dripped into the three-neck flask, the mixture is heated to 75 ℃ and stirred for 24 h, and silicon dioxide (NH) with primary amine on the surface is prepared2-SiO2) (ii) a Step 2, 10 g of APP was added to a three-necked flask filled with ethanol, and then heated to 90 ℃ to add 48g of NH2-SiO2Adding into a three-neck bottle, reacting for 4h to obtain silicon dioxide coated ammonium polyphosphate (NH)2-SiO2-APP); step 3, adding 25 g of polycaprolactone into a three-neck flask, drying at 120 ℃ for 24 h, mixing with 12.8 g of 4, 4-diphenylmethane diisocyanate, heating to 85 ℃ for reaction, reacting for 2 h, adding 1, 4-butanediol and NH2-SiO2APP is placed into a 120 ℃ oven for drying and curing after being uniformly stirred to prepare microencapsulated ammonium polyphosphate with silicon dioxide and thermoplastic polyurethane as shells and ammonium polyphosphate as cores;
(2) the preparation method of the halogen-free flame-retardant heat-resistant cable material comprises the following steps: 100 parts of ethylene-vinyl acetate copolymer, 20 parts of microencapsulated ammonium polyphosphate, 0.5 part of lubricant and 5 parts of compatilizer are mixed in a mixing cylinder for 3 min, the mixture is fully mixed in the mixing cylinder and is mixed for 3 min at the rotating speed of 80 r/min to obtain a premixed material, the obtained premixed material is added into a double-screw extruder through a main feeding port, and is subjected to melt extrusion, cooling, drying and grain cutting to obtain a flame-retardant cable material composite material granule, the obtained granule is added into an injection molding machine, the temperature is 170 ℃, and the flame-retardant cable material composite material granule is subjected to heating melting, extrusion, injection molding and molding.
Compared with a blank sample (the cable material without the flame retardant), the Limit Oxygen Index (LOI) of the prepared halogen-free flame-retardant heat-resistant cable material is improved to 29.9% from 19.2%, the tensile strength is 16.6 MPa, and the retention rate of the mechanical property is more than 98.1% after the cable material is soaked in water for one week.
Example 2:
(1) microencapsulation modification of ammonium polyphosphate (APP): step 1, 20 g of silica was added to 150ml of absolute ethanol and 40ml of deionized waterIn the reaction solution, the mixture was sonicated for 10 min and then transferred into a three-necked flask, and then 40 g of KH 550, a silane coupling agent, was slowly dropped into the three-necked flask, heated to 75 ℃ and stirred for 24 hours to prepare silica (NH) having a primary amine surface2-SiO2) (ii) a Step 2, 10 g of APP was added to a three-necked flask filled with ethanol, and then heated to 90 ℃ to add 48g of NH2-SiO2Adding into a three-neck bottle, reacting for 4h to obtain silicon dioxide coated ammonium polyphosphate (NH)2-SiO2-APP); step 3, adding 25 g of polycaprolactone into a three-neck flask, drying at 120 ℃ for 24 h, mixing with 12.8 g of 4, 4-diphenylmethane diisocyanate, heating to 85 ℃ for reaction, reacting for 2 h, adding 1, 4-butanediol and NH2-SiO2APP is placed into a 120 ℃ oven for drying and curing after being uniformly stirred to prepare microencapsulated ammonium polyphosphate with silicon dioxide and thermoplastic polyurethane as shells and ammonium polyphosphate as cores;
(2) the preparation method of the halogen-free flame-retardant heat-resistant cable material comprises the following steps: 100 parts of ethylene-vinyl acetate copolymer, 25 parts of microencapsulated ammonium polyphosphate, 1 part of lubricant and 7.5 parts of compatilizer are mixed in a mixing cylinder for 4 min, the mixture is fully mixed in the mixing cylinder and is mixed for 4 min at the rotating speed of 100 r/min to obtain a premixed material, the obtained premixed material is added into a double-screw extruder through a main feeding port, and is subjected to melt extrusion, cooling, drying and grain cutting to obtain a flame-retardant cable material composite material granule, the obtained granule is added into an injection molding machine, the temperature is 180 ℃, and the flame-retardant cable material composite material granule is subjected to heating melting, extrusion, injection molding and molding.
Compared with a blank sample (the cable material without the flame retardant), the Limit Oxygen Index (LOI) of the prepared halogen-free flame-retardant heat-resistant cable material is improved to 30.1% from 19.2%, the tensile strength is 16.9 MPa, and the retention rate of the mechanical property is more than 98.4% after the cable material is soaked in water for one week.
Example 3:
(1) microencapsulation modification of ammonium polyphosphate (APP): step 1, 20 g of silicon dioxide is added into 150ml of absolute ethyl alcohol and 40ml of deionized water, the mixture is moved into a three-mouth flask after being subjected to ultrasonic treatment for 10 min, then 40 g of silane coupling agent KH 550 is slowly dripped into the three-mouth flask, and the mixture is heated to 75 DEG CAnd stirred for 24 hours to prepare silicon dioxide (NH) with primary amine on the surface2-SiO2) (ii) a Step 2, 10 g of APP was added to a three-necked flask filled with ethanol, and then heated to 90 ℃ to add 48g of NH2-SiO2Adding into a three-neck bottle, reacting for 4h to obtain silicon dioxide coated ammonium polyphosphate (NH)2-SiO2-APP); step 3, adding 25 g of polycaprolactone into a three-neck flask, drying at 120 ℃ for 24 h, mixing with 12.8 g of 4, 4-diphenylmethane diisocyanate, heating to 85 ℃ for reaction, reacting for 2 h, adding 1, 4-butanediol and NH2-SiO2APP is placed into a 120 ℃ oven for drying and curing after being uniformly stirred to prepare microencapsulated ammonium polyphosphate with silicon dioxide and thermoplastic polyurethane as shells and ammonium polyphosphate as cores;
(2) the preparation method of the halogen-free flame-retardant heat-resistant cable material comprises the following steps: 100 parts of ethylene-vinyl acetate copolymer, 30 parts of microencapsulated ammonium polyphosphate, 1.5 parts of lubricant and 10 parts of compatilizer are mixed in a mixing cylinder for 5 min, the mixture is fully mixed in the mixing cylinder and is mixed for 5 min at the rotating speed of 120 r/min to obtain a premixed material, the obtained premixed material is added into a double-screw extruder through a main feeding port, and is subjected to melt extrusion, cooling, drying and grain cutting to obtain a flame-retardant cable material composite material granule, the obtained granule is added into an injection molding machine, the temperature is 190 ℃, and the flame-retardant cable material composite material granule is subjected to heating melting, extrusion, injection molding and molding.
Compared with a blank sample (the cable material without the flame retardant), the Limit Oxygen Index (LOI) of the prepared halogen-free flame-retardant heat-resistant cable material is improved to 31.3% from 19.2%, the tensile strength is 17.1 MPa, and the retention rate of the mechanical property is more than 99% after the cable material is soaked in water for one week.
Claims (6)
1. The halogen-free flame-retardant heat-resistant cable material is characterized by comprising the following steps of:
microencapsulation modification of ammonium polyphosphate (APP): step 1, 20 g of silica was added to 150ml of absolute ethanol and 40ml of deionized water, sonicated for 10 min and then transferred to a three-necked flask, and then 40 g of a silane coupling agent KH 550 was addedSlowly dropwise adding into a three-neck flask, heating to 75 deg.C and stirring for 24 hr to obtain silicon dioxide (NH) with primary amine on surface2-SiO2) (ii) a Step 2, 10 g of APP was added to a three-necked flask filled with ethanol, and then heated to 90 ℃ to add 48g of NH2-SiO2Adding into a three-neck bottle, reacting for 4h to obtain silicon dioxide coated ammonium polyphosphate (NH)2-SiO2-APP); step 3, adding 25 g of polycaprolactone into a three-neck flask, drying at 120 ℃ for 24 h, mixing with 12.8 g of 4, 4-diphenylmethane diisocyanate, heating to 85 ℃ for reaction, reacting for 2 h, adding 1, 4-butanediol and NH2-SiO2APP is placed into a 120 ℃ oven for drying and curing after being uniformly stirred to prepare microencapsulated ammonium polyphosphate with silicon dioxide and thermoplastic polyurethane as shells and ammonium polyphosphate as cores;
the preparation method of the halogen-free flame-retardant heat-resistant cable material comprises the following steps: 100 parts of ethylene-vinyl acetate copolymer, 20-30 parts of microencapsulated ammonium polyphosphate, 0.5-1.5 parts of lubricant and 5-10 parts of compatilizer are mixed in a mixing cylinder for 3-5 min, the materials are fully mixed in the mixing cylinder and are mixed for 3-5 min at the rotating speed of 80-120 r/min to obtain a premixed material, the obtained premixed material is added into a double-screw extruder through a main feeding port, and the premixed material is subjected to melt extrusion, cooling, drying and grain cutting to obtain flame-retardant cable material composite material granules, the obtained granules are added into an injection molding machine, the temperature is 170-190 ℃, and the flame-retardant cable material composite material granules are subjected to heating melting, extrusion, injection molding and molding.
2. The halogen-free flame-retardant heat-resistant cable material and the preparation method thereof as claimed in claim 1, wherein the silica is nano silica, the particle size range of the nano silica is 300-500 nm, and the surface of the nano silica has hydroxyl groups.
3. The halogen-free flame-retardant heat-resistant cable material and the preparation method thereof as claimed in claim 1, wherein the molecular weight of the polycaprolactone is 2000.
4. The halogen-free flame-retardant heat-resistant cable material and the preparation method thereof as claimed in claim 1, wherein the molecular weight of the ammonium polyphosphate is more than 1000.
5. The halogen-free flame-retardant heat-resistant cable material and the preparation method thereof as claimed in claim 1, wherein the compatibilizer is methyl methacrylate-butadiene-styrene terpolymer (MBS).
6. The halogen-free flame-retardant heat-resistant cable material and the preparation method thereof according to claim 1, wherein the lubricant is N, N' -Ethylene Bis Stearamide (EBS).
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| CN115716985A (en) * | 2022-11-24 | 2023-02-28 | 上海皆利新材料科技有限公司 | Halogen-free flame-retardant polyurethane elastomer and preparation method thereof |
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| CN101608060A (en) * | 2009-07-09 | 2009-12-23 | 中国科学技术大学 | Core-shell type ammonium polyphosphate synergetic flame-retardant polyurethane elastic composite material and method for making thereof |
| CN103252200A (en) * | 2013-05-04 | 2013-08-21 | 辽宁恒星精细化工有限公司 | Microencapsulation ammonium polyphosphate fire retardant and preparation method thereof |
| CN106750708A (en) * | 2016-12-07 | 2017-05-31 | 安徽合聚阻燃新材料股份有限公司 | A kind of phosphorus nitrogen compounds flame resistance irradiation crosslinked halogen-free low smoke cables material |
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