CN117720789B - Low-smoke halogen-free fireproof flame-retardant power cable and preparation method thereof - Google Patents
Low-smoke halogen-free fireproof flame-retardant power cable and preparation method thereof Download PDFInfo
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- CN117720789B CN117720789B CN202410172606.7A CN202410172606A CN117720789B CN 117720789 B CN117720789 B CN 117720789B CN 202410172606 A CN202410172606 A CN 202410172606A CN 117720789 B CN117720789 B CN 117720789B
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 90
- 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 78
- 239000000779 smoke Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000002131 composite material Substances 0.000 claims abstract description 49
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical class [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 claims abstract description 38
- 239000001508 potassium citrate Substances 0.000 claims abstract description 23
- 229960002635 potassium citrate Drugs 0.000 claims abstract description 23
- 235000011082 potassium citrates Nutrition 0.000 claims abstract description 23
- 229910052588 hydroxylapatite Inorganic materials 0.000 claims abstract description 14
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 13
- 150000002367 halogens Chemical class 0.000 claims abstract description 13
- UBIJTWDKTYCPMQ-UHFFFAOYSA-N hexachlorophosphazene Chemical compound ClP1(Cl)=NP(Cl)(Cl)=NP(Cl)(Cl)=N1 UBIJTWDKTYCPMQ-UHFFFAOYSA-N 0.000 claims abstract description 13
- QEEAPRPFLLJWCF-UHFFFAOYSA-K potassium citrate (anhydrous) Chemical compound [K+].[K+].[K+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O QEEAPRPFLLJWCF-UHFFFAOYSA-K 0.000 claims abstract description 13
- 239000004246 zinc acetate Substances 0.000 claims abstract description 13
- 239000010410 layer Substances 0.000 claims description 104
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 30
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 30
- 238000002156 mixing Methods 0.000 claims description 24
- 238000006243 chemical reaction Methods 0.000 claims description 23
- 238000010438 heat treatment Methods 0.000 claims description 20
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 19
- 238000011049 filling Methods 0.000 claims description 19
- 238000001035 drying Methods 0.000 claims description 16
- RYHBNJHYFVUHQT-UHFFFAOYSA-N 1,4-Dioxane Chemical compound C1COCCO1 RYHBNJHYFVUHQT-UHFFFAOYSA-N 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000000706 filtrate Substances 0.000 claims description 15
- 238000001914 filtration Methods 0.000 claims description 15
- 229920002379 silicone rubber Polymers 0.000 claims description 15
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 15
- 239000004020 conductor Substances 0.000 claims description 14
- 239000011241 protective layer Substances 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- -1 potassium citrate modified hydroxyapatite Chemical class 0.000 claims description 11
- URYJRUOOVOCDLA-UHFFFAOYSA-N 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzene-1,2-dicarbonitrile Chemical compound O1C(C)(C)C(C)(C)OB1C1=CC=C(C#N)C(C#N)=C1 URYJRUOOVOCDLA-UHFFFAOYSA-N 0.000 claims description 10
- JRRAUWWVBVECPY-UHFFFAOYSA-N 4-(tetrazol-1-yl)aniline Chemical compound C1=CC(N)=CC=C1N1N=NN=C1 JRRAUWWVBVECPY-UHFFFAOYSA-N 0.000 claims description 10
- 239000004793 Polystyrene Substances 0.000 claims description 10
- 239000004699 Ultra-high molecular weight polyethylene Substances 0.000 claims description 10
- 239000003153 chemical reaction reagent Substances 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- HIHIPCDUFKZOSL-UHFFFAOYSA-N ethenyl(methyl)silicon Chemical compound C[Si]C=C HIHIPCDUFKZOSL-UHFFFAOYSA-N 0.000 claims description 10
- 238000001125 extrusion Methods 0.000 claims description 10
- QWXYZCJEXYQNEI-OSZHWHEXSA-N intermediate I Chemical compound COC(=O)[C@@]1(C=O)[C@H]2CC=[N+](C\C2=C\C)CCc2c1[nH]c1ccccc21 QWXYZCJEXYQNEI-OSZHWHEXSA-N 0.000 claims description 10
- YIOFGHHAURBGSJ-UHFFFAOYSA-N isoquinoline-1,3,4-trione Chemical compound C1=CC=C2C(=O)C(=O)NC(=O)C2=C1 YIOFGHHAURBGSJ-UHFFFAOYSA-N 0.000 claims description 10
- 229920002223 polystyrene Polymers 0.000 claims description 10
- 239000004945 silicone rubber Substances 0.000 claims description 10
- 238000009210 therapy by ultrasound Methods 0.000 claims description 10
- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 9
- 229920001971 elastomer Polymers 0.000 claims description 9
- 239000005060 rubber Substances 0.000 claims description 9
- 238000010025 steaming Methods 0.000 claims description 8
- 238000002390 rotary evaporation Methods 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 5
- 229910052782 aluminium Inorganic materials 0.000 claims description 5
- 239000000919 ceramic Substances 0.000 claims description 5
- 239000011888 foil Substances 0.000 claims description 5
- 239000003365 glass fiber Substances 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 239000011347 resin Substances 0.000 claims description 5
- 229920005989 resin Polymers 0.000 claims description 5
- 238000009941 weaving Methods 0.000 claims description 5
- 230000002265 prevention Effects 0.000 claims description 3
- 229920000800 acrylic rubber Polymers 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 229920000058 polyacrylate Polymers 0.000 claims 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 11
- 229910052799 carbon Inorganic materials 0.000 abstract description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 4
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 4
- 239000011574 phosphorus Substances 0.000 abstract description 4
- 230000002829 reductive effect Effects 0.000 abstract description 4
- 230000002195 synergetic effect Effects 0.000 abstract description 4
- 230000009471 action Effects 0.000 abstract description 3
- 230000008901 benefit Effects 0.000 abstract description 3
- JYEUMXHLPRZUAT-UHFFFAOYSA-N 1,2,3-triazine Chemical compound C1=CN=NN=C1 JYEUMXHLPRZUAT-UHFFFAOYSA-N 0.000 abstract description 2
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 abstract description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract description 2
- 229910052796 boron Inorganic materials 0.000 abstract description 2
- 125000000623 heterocyclic group Chemical group 0.000 abstract description 2
- IEQIEDJGQAUEQZ-UHFFFAOYSA-N phthalocyanine Chemical group N1C(N=C2C3=CC=CC=C3C(N=C3C4=CC=CC=C4C(=N4)N3)=N2)=C(C=CC=C2)C2=C1N=C1C2=CC=CC=C2C4=N1 IEQIEDJGQAUEQZ-UHFFFAOYSA-N 0.000 abstract description 2
- 125000003003 spiro group Chemical group 0.000 abstract description 2
- 229910052717 sulfur Inorganic materials 0.000 abstract description 2
- 239000011593 sulfur Substances 0.000 abstract description 2
- VLLMWSRANPNYQX-UHFFFAOYSA-N thiadiazole Chemical compound C1=CSN=N1.C1=CSN=N1 VLLMWSRANPNYQX-UHFFFAOYSA-N 0.000 abstract description 2
- 238000003763 carbonization Methods 0.000 abstract 1
- 238000004132 cross linking Methods 0.000 abstract 1
- 238000009792 diffusion process Methods 0.000 abstract 1
- 238000009413 insulation Methods 0.000 abstract 1
- 229920000642 polymer Polymers 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 11
- 238000012360 testing method Methods 0.000 description 7
- 238000002485 combustion reaction Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 230000000670 limiting effect Effects 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 206010000369 Accident Diseases 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- MPNNOLHYOHFJKL-UHFFFAOYSA-N peroxyphosphoric acid Chemical compound OOP(O)(O)=O MPNNOLHYOHFJKL-UHFFFAOYSA-N 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A30/00—Adapting or protecting infrastructure or their operation
- Y02A30/14—Extreme weather resilient electric power supply systems, e.g. strengthening power lines or underground power cables
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a low-smoke halogen-free fireproof flame-retardant power cable and a preparation method thereof, belonging to the technical field of power cable preparation. The invention adopts hexachlorocyclotriphosphazene as a mother nucleus to prepare the composite flame retardant, has the synergistic flame retardant property of nitrogen, phosphorus, boron, nitrogen, phosphorus and sulfur, and is interacted with the composite modified hydroxyapatite to rapidly expand to form a carbon layer at high temperature, thereby realizing fireproof heat insulation. The fused heterocyclic structures such as spiro and thiadiazole in the flame retardant molecule enhance the molecular rigidity, improve the thermal stability and mechanical strength of the cable material, and the contained o-cyano group can be self-crosslinked under the action of heat to generate triazine and phthalocyanine structures, so that the thermal stability of the cable material is improved, the viscosity is increased, and the risk of molten drops is reduced. The hydroxyapatite is modified by the potassium citrate and the zinc acetate, so that the expansion of the flame-retardant layer can be promoted, the cross-linking of the polymer is catalyzed, the carbonization of the flame-retardant layer is accelerated, and the diffusion of smoke is effectively controlled. The cable material prepared by the invention has the advantages of low smoke, no halogen, quick char formation, fire resistance and flame retardance.
Description
Technical Field
The invention belongs to the technical field of power cable preparation, and particularly relates to a low-smoke halogen-free fireproof flame-retardant power cable and a preparation method thereof.
Background
A power cable is a wire or cable that is specially used for transmitting and distributing electrical energy. They are widely used in electrical power systems, including power plants, transmission systems, distribution systems and ultimately electrical terminals. The power cable is capable of carrying currents of different voltage levels, from low voltage household cables to high voltage long distance transmission cables. Along with frequent fire accidents, people increasingly raise awareness of fire safety, flame retardation of wires and cables gradually attracts attention, the existing power cables often release harmful gases such as chlorine and toxic smoke during combustion, the health of evacuees and firefighters is endangered, and pollution is caused to the environment, a large amount of generated thick smoke seriously influences vision, people evacuation and firefighting rescue are hindered, the power cables cannot quickly char and can further cause melt dripping, other inflammables nearby the cables are ignited, and the addition of flame retardants often further causes the decline of mechanical properties of the cables. Therefore, development of a low-smoke halogen-free fireproof flame-retardant power cable is important for reducing the risk of electric fire accidents and protecting the life safety and property safety of people.
Disclosure of Invention
Aiming at the situation, the invention provides a low-smoke halogen-free fireproof flame-retardant power cable and a preparation method thereof for overcoming the existing power cable.
In order to achieve the above purpose, the following technical scheme is adopted: the utility model provides a low smoke and zero halogen fire prevention fire-retardant power cable and preparation method thereof, power cable includes cable core and external layer, the external layer comprises fire-retardant layer and the protective layer from inside to outside in proper order, four cable cores of mutual interval and parallel arrangement in the fire-retardant layer, the cable core comprises copper core conductor, insulating layer, the shielding layer from inside to outside in proper order, be provided with the filling layer between cable core and the external layer.
Further, the flame-retardant layer comprises the following components in parts by weight: 80-100 parts of polystyrene, 30-40 parts of methyl vinyl silicone rubber, 20-25 parts of acrylate rubber, 12-18 parts of ultra-high molecular weight polyethylene, 7-10 parts of composite flame retardant and 5-8 parts of composite modified hydroxyapatite.
Further, the composite flame retardant is prepared by the steps of:
s1, dissolving hexachlorocyclotriphosphazene in tetrahydrofuran at room temperature, slowly adding 4- (1H-tetrazole-1-yl) aniline and triethylamine under the nitrogen atmosphere, heating to 60-75 ℃ after the addition is completed for 0.5H, continuing to react for 5-8H, filtering after the reaction is finished, and removing tetrahydrofuran by rotary evaporation of filtrate to obtain an intermediate I;
s2, adding isoquinoline-1, 3, 4-trione into a reaction kettle, adding 1, 4-dioxane and Lawson reagent, heating to reflux, reacting for 1-2h, cooling to room temperature, adding the intermediate I, heating to 65-80 ℃ for continuing to react for 2-5h, filtering with diatomite, and removing the 1, 4-dioxane by rotary evaporation of filtrate to obtain the intermediate II;
s3, adding 3, 4-dicyano phenylboronic acid pinacol ester into an ethanol solution of sodium hydroxide with the concentration of 1.5mol/L, adding the intermediate II after 0.5h, uniformly mixing, reacting for 5-8h at the temperature of 60-100 ℃, filtering, steaming filtrate in a rotary way, removing ethanol, and drying in a vacuum oven at the temperature of 80-120 ℃ for 1-2h to obtain the composite flame retardant.
The reaction equation for preparing the composite flame retardant is as follows:
further, the dosage proportions of hexachlorocyclotriphosphazene, 4- (1H-tetrazol-1-yl) aniline, triethylamine, isoquinoline-1, 3, 4-trione, lawson reagent, 3, 4-dicyanophenylboronic acid pinacol ester, tetrahydrofuran, 1, 4-dioxane and ethanol are as follows: (0.95-1) mol: (6-6.05) mol: (6-6.1) mol: (1.45-1.5) mol: (4.5-5) mol: (1.2-1.3) mol: (180-200) mL: (200-250) mL: (250-300) mL.
Further, the composite modified hydroxyapatite is prepared by the steps of:
A. adding hydroxyapatite into a reaction device, adding 1.5mol/L potassium citrate solution, performing ultrasonic treatment for 30-60min, standing for 10-15h, washing with deionized water for 3 times, and drying in an oven at 60-80 ℃ for 12-24h to obtain potassium citrate modified hydroxyapatite;
B. adding the potassium citrate modified hydroxyapatite into a reaction device, adding 1.5mol/L zinc acetate solution, performing ultrasonic treatment for 30-60min, standing for 12-18h, taking out, washing with deionized water for 3 times, and drying in an oven at 40-50 ℃ for 24-48h to obtain the composite modified hydroxyapatite.
Further, the dosage proportion of the hydroxyapatite, the potassium citrate solution and the zinc acetate solution is (5-8) g: (40-60) mL: (50-80) mL.
Further, the copper core conductor is a nickel-plated copper core with the diameter of 10-15 mm; the insulating layer is made of ceramic silicon rubber; the shielding layer is tinned aluminum foil with the thickness of 0.5-1.0 mm; the protective layer is PFA resin; the filling layer is made of glass fiber.
Further, the preparation method of the power cable comprises the following steps: extruding the insulating layer on the surface of a copper core conductor in an extrusion mode, weaving a shielding layer outside the insulating layer to obtain the cable core, wrapping a filling layer outside the cable core, mixing polystyrene, methyl vinyl silicone rubber, acrylate rubber, ultra-high molecular weight polyethylene and composite modified hydroxyapatite in a mixing machine at 180-200 ℃ for 40-60min, cooling to 100-105 ℃, adding a composite flame retardant, continuously mixing for 10min, heating to 180-200 ℃ for 40-60min, extruding and wrapping the shielding layer outside the filling layer to form a flame-retardant layer, and extruding and wrapping the protective layer outside the flame-retardant layer in an extrusion mode to obtain the low-smoke halogen-free fireproof flame-retardant power cable.
The beneficial effects of the invention are as follows:
(1) According to the invention, hexachlorocyclotriphosphazene is used as a parent nucleus to prepare a star-shaped composite flame retardant, and the flame retardant has synergistic flame retardant effect of nitrogen, phosphorus, boron, nitrogen, phosphorus and sulfur in molecules, and is combined with composite modified hydroxyapatite to be rapidly expanded into carbon to form a compact carbon layer, so that the flame retardant has the effects of fire prevention and flame retardance, and a plurality of fused heterocyclic structures such as a spiro structure and thiadiazole in a flame retardant molecule are used to increase the rigidity of the molecule, improve the thermal stability and mechanical property of a cable, avoid the decrease of the mechanical property of the cable caused by the addition of the flame retardant, and contain two adjacent cyano groups in the molecule, and can be self-crosslinked after being heated to generate triazine and phthalocyanine structures, so that the thermal stability of the cable is further enhanced, the viscosity of the cable after melting is increased, and the risk of molten drops is greatly reduced;
(2) The invention modifies the hydroxyapatite by potassium citrate and zinc acetate, K + Ion-exchange inserted between layers of hydroxyapatite in ionized waterUnder the chemical action, the balance of the hydroxyl phosphate gray layer and interlayer cations is destroyed, so that interlayer bonding water is quickly evaporated after being heated at high temperature, the potassium citrate is quickly decomposed to generate carbon dioxide and water, the expansion of the flame-retardant layer is further promoted, zinc acetate can catalyze the compounds in the flame-retardant layer to crosslink, the flame-retardant layer is quickly carbonized, and the smoke is effectively prevented from being scattered;
(3) The power cable prepared by the invention has the advantages of low smoke, no halogen, quick char formation, fire resistance and flame retardance, and has little environmental pollution after combustion.
Drawings
FIG. 1 is a cross-sectional view of a low smoke zero halogen fire-retardant power cable of the present invention;
FIG. 2 is a schematic diagram of a low smoke zero halogen fire-retardant power cable according to the present invention;
FIG. 3 is a graph of the release heat of the flame retardant layer of the power cable prepared in each of the examples and comparative examples;
fig. 4 is an SEM image of the carbon layer formed after combustion of each example and comparative example.
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention.
Legend: 1. a cable core; 11. a copper core conductor; 12. an insulating layer; 13. a shielding layer; 2. a filling layer; 3. an outer layer; 31. a flame retardant layer; 32. and (3) a protective layer.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and all other embodiments obtained by those skilled in the art based on the embodiments of the present invention without making any inventive effort are within the scope of the present invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition, any methods and materials similar or equivalent to those described herein can be used in the present invention. The preferred methods and materials described herein are illustrative only and should not be construed as limiting the scope of the present application.
The experimental methods in the following examples are conventional methods unless otherwise specified, and the experimental materials used in the following examples are commercially available unless otherwise specified.
Example 1
A low smoke zero halogen fireproof flame-retardant power cable and a preparation method thereof.
According to fig. 1-2, the power cable comprises a cable core and an outer layer, wherein the outer layer consists of a flame-retardant layer and a protective layer which are sequentially arranged from inside to outside, four cable cores are arranged in the flame-retardant layer at intervals in parallel, each cable core consists of a copper core conductor, an insulating layer and a shielding layer which are sequentially arranged from inside to outside, and a filling layer is arranged between each cable core and the outer layer.
The flame-retardant layer comprises the following components in parts by weight: 80 parts of polystyrene, 30 parts of methyl vinyl silicone rubber, 20 parts of acrylate rubber, 12 parts of ultra-high molecular weight polyethylene, 7 parts of composite flame retardant and 5 parts of composite modified hydroxyapatite.
The composite flame retardant is prepared by the following steps:
s1, dissolving hexachlorocyclotriphosphazene in tetrahydrofuran at room temperature, slowly adding 4- (1H-tetrazole-1-yl) aniline and triethylamine under the nitrogen atmosphere, heating to 60 ℃ after the addition is completed for 0.5H, continuing to react for 5H, filtering after the reaction is finished, steaming filtrate in a rotary way, and removing tetrahydrofuran to obtain an intermediate I;
s2, adding isoquinoline-1, 3, 4-trione into a reaction kettle, adding 1, 4-dioxane and Lawson reagent, heating to reflux, reacting for 1h, cooling to room temperature, adding the intermediate I, heating to 65 ℃ for continuous reaction for 2h, filtering with diatomite, and removing the 1, 4-dioxane by rotary evaporation of filtrate to obtain the intermediate II;
s3, adding 3, 4-dicyano phenylboronic acid pinacol ester into an ethanol solution of sodium hydroxide with the concentration of 1.5mol/L, adding the intermediate II after 0.5h, uniformly mixing, reacting at 60 ℃ for 5h, filtering, steaming filtrate in a rotary way, removing ethanol, and drying in a vacuum oven at 80 ℃ for 1h to obtain the composite flame retardant.
The dosage proportions of the hexachlorocyclotriphosphazene, 4- (1H-tetrazol-1-yl) aniline, triethylamine, isoquinoline-1, 3, 4-trione, lawson reagent, 3, 4-dicyanophenylboronic acid pinacol ester, tetrahydrofuran, 1, 4-dioxane and ethanol are as follows: 0.95mol:6mol:6mol:1.45mol:4.5mol:1.2mol:180mL:200mL:250mL.
The composite modified hydroxyapatite is prepared by the following steps:
A. adding hydroxyapatite into a reaction device, adding 1.5mol/L potassium citrate solution, performing ultrasonic treatment for 30min, standing for 10h, washing with deionized water for 3 times, and drying in a 60 ℃ oven for 12h to obtain potassium citrate modified hydroxyapatite;
B. adding the potassium citrate modified hydroxyapatite into a reaction device, adding 1.5mol/L zinc acetate solution, performing ultrasonic treatment for 30min, standing for 12h, taking out, washing with deionized water for 3 times, and drying in a baking oven at 40 ℃ for 24h to obtain the composite modified hydroxyapatite.
The dosage proportion of the hydroxyapatite, the potassium citrate solution and the zinc acetate solution is 5g:40mL:50mL.
The copper core conductor is a nickel-plated copper core with the diameter of 10 mm; the insulating layer is made of ceramic silicon rubber; the shielding layer is tinned aluminum foil with the thickness of 0.5 mm; the protective layer is PFA resin; the filling layer is made of glass fiber.
The preparation method of the power cable comprises the following steps: extruding the insulating layer on the surface of a copper core conductor in an extrusion mode, weaving a shielding layer outside the insulating layer to obtain the cable core, wrapping a filling layer outside the cable core, mixing polystyrene, methyl vinyl silicone rubber, acrylate rubber, ultra-high molecular weight polyethylene and composite modified hydroxyapatite in a mixing machine at 180 ℃ for 40min, cooling to 100 ℃, adding a composite flame retardant, continuing mixing for 10min, heating to 180 ℃ for mixing for 40min, extruding and wrapping the shielding layer outside the filling layer to form a flame-retardant layer, extruding and wrapping the protective layer outside the flame-retardant layer in an extrusion mode to obtain the low-smoke halogen-free fireproof flame-retardant power cable.
Example 2
A low smoke zero halogen fireproof flame-retardant power cable and a preparation method thereof.
The structure of the power cable is the same as that of embodiment 1.
The flame-retardant layer comprises the following components in parts by weight: 100 parts of polystyrene, 40 parts of methyl vinyl silicone rubber, 25 parts of acrylate rubber, 18 parts of ultra-high molecular weight polyethylene, 10 parts of composite flame retardant and 8 parts of composite modified hydroxyapatite.
The composite flame retardant is prepared by the following steps:
s1, dissolving hexachlorocyclotriphosphazene in tetrahydrofuran at room temperature, slowly adding 4- (1H-tetrazole-1-yl) aniline and triethylamine under the nitrogen atmosphere, heating to 75 ℃ after the addition is completed for 0.5H, continuing to react for 8H, filtering after the reaction is finished, steaming filtrate in a rotary way, and removing tetrahydrofuran to obtain an intermediate I;
s2, adding isoquinoline-1, 3, 4-trione into a reaction kettle, adding 1, 4-dioxane and Lawson reagent, heating to reflux, reacting for 2 hours, cooling to room temperature, adding the intermediate I, heating to 80 ℃ for continuous reaction for 5 hours, filtering with diatomite, and removing the 1, 4-dioxane by rotary evaporation of filtrate to obtain the intermediate II;
s3, adding 3, 4-dicyano phenylboronic acid pinacol ester into an ethanol solution of sodium hydroxide with the concentration of 1.5mol/L, adding the intermediate II after 0.5h, uniformly mixing, reacting at 100 ℃ for 8h, filtering, steaming filtrate in a rotary way, removing ethanol, and drying in a vacuum oven at 120 ℃ for 2h to obtain the composite flame retardant.
The dosage proportions of the hexachlorocyclotriphosphazene, 4- (1H-tetrazol-1-yl) aniline, triethylamine, isoquinoline-1, 3, 4-trione, lawson reagent, 3, 4-dicyanophenylboronic acid pinacol ester, tetrahydrofuran, 1, 4-dioxane and ethanol are as follows: 1mol:6.05mol:6.1mol:1.5mol:5mol:1.3mol:200mL:250mL:300mL.
The composite modified hydroxyapatite is prepared by the following steps:
A. adding hydroxyapatite into a reaction device, adding 1.5mol/L potassium citrate solution, performing ultrasonic treatment for 60min, standing for 15h, washing with deionized water for 3 times, and drying in an oven at 80 ℃ for 24h to obtain potassium citrate modified hydroxyapatite;
B. adding the potassium citrate modified hydroxyapatite into a reaction device, adding 1.5mol/L zinc acetate solution, performing ultrasonic treatment for 60min, standing for 18h, taking out, washing with deionized water for 3 times, and drying in a 50 ℃ oven for 48h to obtain the composite modified hydroxyapatite.
The dosage proportion of the hydroxyapatite, the potassium citrate solution and the zinc acetate solution is 8g:60mL:80mL.
The copper core conductor is a nickel-plated copper core with the diameter of 15 mm; the insulating layer is made of ceramic silicon rubber; the shielding layer is tinned aluminum foil with the thickness of 1.0 mm; the protective layer is PFA resin; the filling layer is made of glass fiber.
The preparation method of the power cable comprises the following steps: extruding the insulating layer on the surface of a copper core conductor in an extrusion mode, weaving a shielding layer outside the insulating layer to obtain the cable core, wrapping a filling layer outside the cable core, mixing polystyrene, methyl vinyl silicone rubber, acrylate rubber, ultra-high molecular weight polyethylene and composite modified hydroxyapatite in a mixing machine for 60min at 200 ℃, cooling to 105 ℃, adding a composite flame retardant, continuing mixing for 10min, heating to 200 ℃ for mixing for 60min, extruding and wrapping the shielding layer outside the filling layer to form a flame-retardant layer, extruding and wrapping the protective layer outside the flame-retardant layer in an extrusion mode to obtain the low-smoke halogen-free fireproof flame-retardant power cable.
Example 3
A low smoke zero halogen fireproof flame-retardant power cable and a preparation method thereof.
The structure of the power cable is the same as that of embodiment 1.
The flame-retardant layer comprises the following components in parts by weight: 90 parts of polystyrene, 35 parts of methyl vinyl silicone rubber, 24 parts of acrylate rubber, 15 parts of ultra-high molecular weight polyethylene, 8 parts of composite flame retardant and 6 parts of composite modified hydroxyapatite.
The composite flame retardant is prepared by the following steps:
s1, dissolving hexachlorocyclotriphosphazene in tetrahydrofuran at room temperature, slowly adding 4- (1H-tetrazole-1-yl) aniline and triethylamine under the nitrogen atmosphere, heating to 70 ℃ after the addition is completed for 0.5H, continuing to react for 6H, filtering after the reaction is finished, steaming filtrate in a rotary way, and removing tetrahydrofuran to obtain an intermediate I;
s2, adding isoquinoline-1, 3, 4-trione into a reaction kettle, adding 1, 4-dioxane and Lawson reagent, heating to reflux, reacting for 1.5 hours, cooling to room temperature, adding the intermediate I, heating to 70 ℃ for continuing to react for 3 hours, filtering with diatomite, and removing the 1, 4-dioxane by rotary evaporation of filtrate to obtain the intermediate II;
s3, adding 3, 4-dicyano phenylboronic acid pinacol ester into an ethanol solution of sodium hydroxide with the concentration of 1.5mol/L, adding the intermediate II after 0.5h, uniformly mixing, reacting at 80 ℃ for 6h, filtering, steaming filtrate in a rotary way, removing ethanol, and drying in a vacuum oven at 100 ℃ for 1.5h to obtain the composite flame retardant.
The dosage proportions of the hexachlorocyclotriphosphazene, 4- (1H-tetrazol-1-yl) aniline, triethylamine, isoquinoline-1, 3, 4-trione, lawson reagent, 3, 4-dicyanophenylboronic acid pinacol ester, tetrahydrofuran, 1, 4-dioxane and ethanol are as follows: 0.98mol:6.02mol:6.05mol:1.47mol:4.8mol:1.25mol:185mL:220mL:270mL.
The composite modified hydroxyapatite is prepared by the following steps:
A. adding hydroxyapatite into a reaction device, adding 1.5mol/L potassium citrate solution, performing ultrasonic treatment for 40min, standing for 12h, washing with deionized water for 3 times, and drying in a 70 ℃ oven for 15h to obtain potassium citrate modified hydroxyapatite;
B. adding the potassium citrate modified hydroxyapatite into a reaction device, adding 1.5mol/L zinc acetate solution, performing ultrasonic treatment for 50min, standing for 15h, taking out, washing with deionized water for 3 times, and drying in a drying oven at 45 ℃ for 30h to obtain the composite modified hydroxyapatite.
The dosage proportion of the hydroxyapatite, the potassium citrate solution and the zinc acetate solution is 6g:50mL:75mL.
The copper core conductor is a nickel-plated copper core with the diameter of 12 mm; the insulating layer is made of ceramic silicon rubber; the shielding layer is tinned aluminum foil with the thickness of 0.6 mm; the protective layer is PFA resin; the filling layer is made of glass fiber.
The preparation method of the power cable comprises the following steps: extruding the insulating layer on the surface of a copper core conductor in an extrusion mode, weaving a shielding layer outside the insulating layer to obtain the cable core, wrapping a filling layer outside the cable core, mixing polystyrene, methyl vinyl silicone rubber, acrylate rubber, ultra-high molecular weight polyethylene and composite modified hydroxyapatite in a mixing machine for 50min at 190 ℃, cooling to 105 ℃, adding a composite flame retardant, continuing mixing for 10min, heating to 190 ℃ for mixing for 50min, extruding and wrapping the shielding layer outside the filling layer to form a flame-retardant layer, extruding and wrapping the protective layer outside the flame-retardant layer in an extrusion mode to obtain the low-smoke halogen-free fireproof flame-retardant power cable.
Comparative example 1
Low-smoke halogen-free fireproof flame-retardant power cable and preparation method thereof
This comparative example differs from example 1 in that the composite flame retardant was replaced by an equivalent amount of hexachlorocyclotriphosphazene in the power cable, and the remaining components and the content of the components were the same as in example 1.
Comparative example 2
Low-smoke halogen-free fireproof flame-retardant power cable and preparation method thereof
This comparative example differs from example 1 in that the composite modified hydroxyapatite was replaced with equal amounts of hydroxyapatite, and the remaining components and component contents were the same as in example 1.
Analysis of results
The flame retardant layer of the power cable prepared in each example and comparative example was tested for heat release using an IMZLY-01 cone calorimeter, and the result is shown in fig. 3, with a set heat radiation power of 60kW/m 2 The sample sizes were 100mm by 10mm by 3mm.
SEM pictures of the carbon layers formed in the examples and comparative examples after testing using a cone calorimeter are shown in fig. 4.
The flame retardant layers of the power cables prepared in each of the examples and comparative examples were tested for limiting oxygen index, tensile strength, UL94 vertical burn, smoke density and melt drop resistance, and the test results are shown in table 1. Limiting oxygen index test using an HC-2CZ oxygen index tester, the sample size was 100mm by 10mm by 3mm; the tensile strength test adopts a WDW-100 universal material testing machine, and the tensile speed is 500mm/min; UL94 vertical burn test using CZF-4 horizontal vertical burn tester with sample dimensions of 100mm x 13mm x 3mm; smoke density testing using a JCY-3 smoke density meter, the sample sizes were 25mm x 3mm.
Table 1 results table for testing flame-retardant smoke-suppressing and mechanical properties of power cable
As can be seen from fig. 3, the heat released after the combustion of each embodiment is lower than that of the comparative example, which indicates that the power cable prepared by the invention rapidly expands to form a carbon layer after being heated, thereby preventing the transfer of external heat, reducing the heat release, and having obvious synergistic flame retardant effect, and as can be seen from fig. 4, the continuity and compactness of the carbon layer formed after the combustion of each embodiment are obviously higher than those of each comparative example, the carbon particles are visible on the surface of the carbon layer, the number of pores of the carbon layer is obviously reduced, which indicates that the gas overflow is effectively inhibited, and the invention has better effects of forming carbon and inhibiting smoke.
From Table 1, it is clear that the limiting oxygen index of the power cable is increased and the smoke density is reduced by the synergistic flame retardance of the composite flame retardant and the action of the composite modified hydroxyapatite, the single vertical combustion reaches the UL94V-0 level, the anti-dripping effect is obvious, and the mechanical property is not affected.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
The invention and its embodiments have been described above with no limitation, and the invention is illustrated in the figures of the accompanying drawings as one of its embodiments, without limitation in practice. In summary, those skilled in the art, having benefit of this disclosure, will appreciate that the invention can be practiced without the specific details disclosed herein.
Claims (6)
1. The utility model provides a low smoke and zero halogen fire prevention fire-retardant power cable which characterized in that: the cable comprises a cable core and an outer layer, wherein the outer layer consists of a flame-retardant layer and a protective layer which are sequentially arranged from inside to outside, four cable cores are arranged in the flame-retardant layer at intervals in parallel, the cable core consists of a copper core conductor, an insulating layer and a shielding layer which are sequentially arranged from inside to outside, and a filling layer is arranged between the cable core and the outer layer; the flame-retardant layer comprises the following components in parts by weight: 80-100 parts of polystyrene, 30-40 parts of methyl vinyl silicone rubber, 20-25 parts of acrylate rubber, 12-18 parts of ultra-high molecular weight polyethylene, 7-10 parts of composite flame retardant and 5-8 parts of composite modified hydroxyapatite;
the composite flame retardant is prepared by the following steps:
s1, dissolving hexachlorocyclotriphosphazene in tetrahydrofuran at room temperature, slowly adding 4- (1H-tetrazole-1-yl) aniline and triethylamine under the nitrogen atmosphere, heating to 60-75 ℃ after the addition is completed for 0.5H, continuing to react for 5-8H, filtering after the reaction is finished, and removing tetrahydrofuran by rotary evaporation of filtrate to obtain an intermediate I;
s2, adding isoquinoline-1, 3, 4-trione into a reaction kettle, adding 1, 4-dioxane and Lawson reagent, heating to reflux, reacting for 1-2h, cooling to room temperature, adding the intermediate I, heating to 65-80 ℃ for continuing to react for 2-5h, filtering with diatomite, and removing the 1, 4-dioxane by rotary evaporation of filtrate to obtain the intermediate II;
s3, adding 3, 4-dicyano phenylboronic acid pinacol ester into an ethanol solution of sodium hydroxide with the concentration of 1.5mol/L, adding the intermediate II after 0.5h, uniformly mixing, reacting for 5-8h at 60-100 ℃, filtering, steaming filtrate in a rotary way, removing ethanol, and drying in a vacuum oven at 80-120 ℃ for 1-2h to obtain the composite flame retardant;
the dosage proportions of the hexachlorocyclotriphosphazene, 4- (1H-tetrazol-1-yl) aniline, triethylamine, isoquinoline-1, 3, 4-trione, lawson reagent, 3, 4-dicyanophenylboronic acid pinacol ester, tetrahydrofuran, 1, 4-dioxane and ethanol are as follows: (0.95-1) mol: (6-6.05) mol: (6-6.1) mol: (1.45-1.5) mol: (4.5-5) mol: (1.2-1.3) mol: (180-200) mL: (200-250) mL: (250-300) mL;
the composite modified hydroxyapatite is prepared by the following steps:
A. adding hydroxyapatite into a reaction device, adding 1.5mol/L potassium citrate solution, performing ultrasonic treatment for 30-60min, standing for 10-15h, washing with deionized water for 3 times, and drying in an oven at 60-80 ℃ for 12-24h to obtain potassium citrate modified hydroxyapatite;
B. adding the potassium citrate modified hydroxyapatite into a reaction device, adding 1.5mol/L zinc acetate solution, carrying out ultrasonic treatment for 30-60min, standing for 12-18h, taking out, washing with deionized water for 3 times, and drying in a baking oven at 40-50 ℃ for 24-48h to obtain the composite modified hydroxyapatite;
the dosage proportion of the hydroxyapatite, the potassium citrate solution and the zinc acetate solution is (5-8) g: (40-60) mL: (50-80) mL.
2. A low smoke zero halogen fire-retardant power cable according to claim 1, wherein: the copper core conductor is a nickel-plated copper core with the diameter of 10-15mm, and the insulating layer is ceramic silicon rubber.
3. A low smoke zero halogen fire-retardant power cable according to claim 2, wherein: the shielding layer is tinned aluminum foil with the thickness of 0.5-1.0 mm.
4. A low smoke zero halogen fire-retardant power cable according to claim 3, wherein: the protective layer is PFA resin.
5. A low smoke zero halogen fire-retardant power cable according to claim 4, wherein: the filling layer is made of glass fiber.
6. A method of making a low smoke, halogen-free, fire-retardant power cable according to any one of claims 1 to 5, characterized by: the preparation method comprises the following steps: extruding the insulating layer on the surface of a copper core conductor in an extrusion mode, weaving a shielding layer outside the insulating layer to obtain the cable core, wrapping a filling layer outside the cable core, mixing the polystyrene, the methyl vinyl silicone rubber, the acrylic rubber, the ultra-high molecular weight polyethylene and the composite modified hydroxyapatite in a mixing machine at 180-200 ℃ for 40-60min, cooling to 100-105 ℃, adding the composite flame retardant, continuing mixing for 10min, heating to 180-200 ℃ for mixing for 40-60min, extruding and wrapping the shielding layer outside the filling layer to form a flame-retardant layer, extruding and wrapping the protective layer outside the flame-retardant layer in an extrusion mode to obtain the low-smoke halogen-free fireproof flame-retardant power cable.
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