CN117612784B - High-flame-retardance anti-dripping fireproof cable and preparation process thereof - Google Patents
High-flame-retardance anti-dripping fireproof cable and preparation process thereof Download PDFInfo
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- CN117612784B CN117612784B CN202311586423.1A CN202311586423A CN117612784B CN 117612784 B CN117612784 B CN 117612784B CN 202311586423 A CN202311586423 A CN 202311586423A CN 117612784 B CN117612784 B CN 117612784B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000003063 flame retardant Substances 0.000 claims abstract description 107
- 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 claims abstract description 99
- 239000003365 glass fiber Substances 0.000 claims abstract description 84
- -1 polyethylene Polymers 0.000 claims abstract description 44
- 239000004698 Polyethylene Substances 0.000 claims abstract description 43
- 229920000573 polyethylene Polymers 0.000 claims abstract description 43
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims abstract description 39
- 239000002131 composite material Substances 0.000 claims abstract description 25
- 229920001661 Chitosan Polymers 0.000 claims abstract description 23
- 239000001913 cellulose Substances 0.000 claims abstract description 23
- 229920002678 cellulose Polymers 0.000 claims abstract description 23
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 19
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000004202 carbamide Substances 0.000 claims abstract description 15
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims abstract description 13
- 229930006000 Sucrose Natural products 0.000 claims abstract description 13
- 239000005720 sucrose Substances 0.000 claims abstract description 13
- KKUKTXOBAWVSHC-UHFFFAOYSA-N Dimethylphosphate Chemical compound COP(O)(=O)OC KKUKTXOBAWVSHC-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 12
- 239000000945 filler Substances 0.000 claims abstract description 9
- 239000006185 dispersion Substances 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims description 48
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 42
- 238000003756 stirring Methods 0.000 claims description 35
- 238000010438 heat treatment Methods 0.000 claims description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 32
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 25
- 238000010992 reflux Methods 0.000 claims description 25
- 238000009210 therapy by ultrasound Methods 0.000 claims description 24
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 18
- 239000002245 particle Substances 0.000 claims description 18
- 229910052681 coesite Inorganic materials 0.000 claims description 16
- 229910052906 cristobalite Inorganic materials 0.000 claims description 16
- 239000000377 silicon dioxide Substances 0.000 claims description 16
- 229910052682 stishovite Inorganic materials 0.000 claims description 16
- 229910052905 tridymite Inorganic materials 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 229910019089 Mg-Fe Inorganic materials 0.000 claims description 15
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- 239000011259 mixed solution Substances 0.000 claims description 13
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 12
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 12
- 239000011777 magnesium Substances 0.000 claims description 12
- 229910052749 magnesium Inorganic materials 0.000 claims description 12
- 239000007787 solid Substances 0.000 claims description 12
- 238000001291 vacuum drying Methods 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 11
- 238000005303 weighing Methods 0.000 claims description 11
- FALRKNHUBBKYCC-UHFFFAOYSA-N 2-(chloromethyl)pyridine-3-carbonitrile Chemical compound ClCC1=NC=CC=C1C#N FALRKNHUBBKYCC-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 229940014800 succinic anhydride Drugs 0.000 claims description 10
- 229910052742 iron Inorganic materials 0.000 claims description 9
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 8
- 238000011049 filling Methods 0.000 claims description 8
- 229920013716 polyethylene resin Polymers 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 7
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 7
- 239000011248 coating agent Substances 0.000 claims description 7
- 238000000576 coating method Methods 0.000 claims description 7
- 239000004020 conductor Substances 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 125000003277 amino group Chemical group 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 6
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 6
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 239000008096 xylene Substances 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 230000006641 stabilisation Effects 0.000 claims description 5
- 238000011105 stabilization Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims 8
- 230000000694 effects Effects 0.000 abstract description 8
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 abstract description 6
- 229910052943 magnesium sulfate Inorganic materials 0.000 abstract description 3
- 235000019341 magnesium sulphate Nutrition 0.000 abstract description 3
- 230000004048 modification Effects 0.000 abstract description 3
- 238000012986 modification Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 abstract 2
- 238000005576 amination reaction Methods 0.000 abstract 1
- 230000021523 carboxylation Effects 0.000 abstract 1
- 238000006473 carboxylation reaction Methods 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 20
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 11
- 229910052760 oxygen Inorganic materials 0.000 description 11
- 239000001301 oxygen Substances 0.000 description 11
- 229920000642 polymer Polymers 0.000 description 9
- 238000002485 combustion reaction Methods 0.000 description 7
- 230000009970 fire resistant effect Effects 0.000 description 6
- 230000002195 synergetic effect Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 5
- 125000000524 functional group Chemical group 0.000 description 5
- 229910052736 halogen Inorganic materials 0.000 description 5
- 150000002367 halogens Chemical class 0.000 description 5
- 229910017604 nitric acid Inorganic materials 0.000 description 5
- 239000000779 smoke Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 238000001000 micrograph Methods 0.000 description 3
- 239000011574 phosphorus Substances 0.000 description 3
- 230000002349 favourable effect Effects 0.000 description 2
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 description 2
- 230000002045 lasting effect Effects 0.000 description 2
- 231100000053 low toxicity Toxicity 0.000 description 2
- 239000010445 mica Substances 0.000 description 2
- 229910052618 mica group Inorganic materials 0.000 description 2
- 231100000956 nontoxicity Toxicity 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 238000005979 thermal decomposition reaction Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 239000002341 toxic gas Substances 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000001934 delay Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000000635 electron micrograph Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000618 nitrogen fertilizer Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/15—Heterocyclic compounds having oxygen in the ring
- C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
- C08K5/1545—Six-membered rings
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/21—Urea; Derivatives thereof, e.g. biuret
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/521—Esters of phosphoric acids, e.g. of H3PO4
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/02—Cellulose; Modified cellulose
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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
- C08L5/00—Compositions of polysaccharides or of their derivatives not provided for in groups C08L1/00 or C08L3/00
- C08L5/08—Chitin; Chondroitin sulfate; Hyaluronic acid; Derivatives thereof
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
- H01B3/30—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes
- H01B3/44—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins
- H01B3/441—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins from alkenes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B7/00—Insulated conductors or cables characterised by their form
- H01B7/02—Disposition of insulation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B7/00—Insulated conductors or cables characterised by their form
- H01B7/17—Protection against damage caused by external factors, e.g. sheaths or armouring
- H01B7/18—Protection against damage caused by wear, mechanical force or pressure; Sheaths; Armouring
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B7/00—Insulated conductors or cables characterised by their form
- H01B7/17—Protection against damage caused by external factors, e.g. sheaths or armouring
- H01B7/29—Protection against damage caused by extremes of temperature or by flame
- H01B7/295—Protection against damage caused by extremes of temperature or by flame using material resistant to flame
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0856—Iron
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/20—Applications use in electrical or conductive gadgets
- C08L2203/202—Applications use in electrical or conductive gadgets use in electrical wires or wirecoating
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Abstract
The invention provides a high-flame-retardance anti-dripping fireproof cable and a preparation process thereof. Specifically, the magnesium sulfate and the ferric nitrate are selected to modify the aluminum silicate, so that the modified aluminum silicate with excellent flame retardant effect is obtained, and in addition, the specific surface area of the composite material is further increased, so that the composite material is beneficial to the dispersion of the composite material in polyethylene; then modifying the polyethylene by using the modified aluminum silicate to obtain modified polyethylene; on the other hand, dimethyl phosphate, sucrose and urea are selected to prepare a safe and environment-friendly halogen-free intumescent flame retardant containing N, P elements, and then the glass fiber is subjected to amination and carboxylation modification to obtain the glass fiber with multifunctional groups, and the glass fiber is compounded with cellulose and chitosan to be used as a filler in a cable to improve the corrosion resistance of the composite cable; and finally, the high-flame-retardance anti-dripping fireproof cable is obtained through a cable preparation process.
Description
Technical Field
The invention belongs to the technical field of materials, relates to preparation of a cable, and particularly relates to a preparation process of a high-flame-retardance anti-dripping fireproof cable.
Background
The cable is used as a material for transmitting electric energy, the consumption and the application range of the cable are large, for example, the cable exists in all parts inside a building, when a fire disaster occurs, the cable is easy to serve as a material for transmitting a fire source, the large fire can spread everywhere in the building along the direction of laying the cable, and other combustible materials are ignited, so that the further expansion of the fire disaster is caused, and smoke, toxic gas, high temperature and dripping matters and the like generated during the combustion of the cable can cause greater harm to the life safety of people, so that the requirements on the cable are further improved along with the development of social construction and the progress of scientific technology.
The flame retardant performance of the cable mainly depends on the coating material used by the cable, so that the cable material with high flame retardance is a key point of flame retardance of the cable. Currently, the fire-resistant cables used in the market are still mainly based on the traditional two-layer or multi-layer mica tape overlapping wrapping process. The main difference between the structure of the fire-resistant cable and the common plastic cable is that a fire-resistant layer is added between the conductor and the insulating layer, and the fire-resistant layer is formed by wrapping mica tapes. The insulating layer of the traditional flame-retardant fire-resistant cable adopts a flame-retardant material formed by mixing a halogen-containing polymer and a halogen-containing flame retardant, and smoke and toxic gas generated during fire disaster can obstruct the sight of people, thereby affecting escape. Thus, a high flame-retardant anti-dripping fire-resistant cable becomes a new subject to be solved.
Disclosure of Invention
Aiming at the problems, the invention selects aluminum silicate particles loaded with magnesium/iron to modify polyethylene, then prepares a safe and environment-friendly flame retardant with excellent performance, and then combines glass fiber after modification with cellulose and chitosan to improve the corrosion resistance of a composite cable, thereby preparing the high flame-retardant anti-dripping flame-retardant cable. The specific operation process of the invention is as follows:
s1, preparing modified aluminum silicate: 1-5g of aluminum silicate is weighed and added into 100mL of aluminum silicate, wherein the volume ratio of the aluminum silicate to the aluminum silicate is 1, and the concentration of the aluminum silicate is 0.1 mol/L: 1, stirring for 6-8 hours at room temperature, filtering and drying, placing the obtained solid in a tube furnace, calcining for 3 hours at 460-680 ℃ under nitrogen atmosphere at a heating rate of 10 ℃/min, preserving heat for 1 hour, cooling, and taking out the solid to obtain magnesium/iron-loaded aluminum silicate particles, namely Mg-Fe@Al 2O3·SiO2; the pellets prepared in this step are used for the step S2 modified polyethylene. The aluminum silicate has the main functions of increasing the thermal decomposition temperature of the polymer and delaying the combustion process of the polymer, so that the dripping of the material when the material catches fire is reduced; the introduction of the magnesium element and the iron element improves the flame retardant property of the material, and in addition, the specific surface area of the particles is further increased, and the dispersibility in other materials is also improved;
S2, preparing modified polyethylene: weighing 8-10 g of polyethylene particles and 0.6-0.9 g of Mg-Fe@Al 2O3·SiO2 prepared by S1, adding into 30-50 ml of dimethylbenzene, stirring at 1500-1600 r/min, performing ultrasonic treatment for 1-3 h, removing an ultrasonic device after the system is uniformly mixed, changing an oil bath for heating, and performing reduced pressure distillation for 30min after the temperature is raised to 120 ℃ for stabilization, so as to obtain modified polyethylene; the polyethylene has the advantages of low cost and good moisture resistance, and the insulation property and the thermal stability of the modified aluminum silicate particles loaded with magnesium/iron are obviously improved;
S3, preparation of an intumescent flame retardant: adding 7.5-35mL of dimethyl phosphate into a 250mL three-neck flask with a magnetic stirrer, a thermometer and a reflux condenser, heating in an oil bath, adding 15-20g of sucrose, adding 0.2-0.3g of anhydrous aluminum trichloride, gradually heating to 120 ℃ for reflux reaction for 3h, adding 5-8g of urea, continuously stirring, heating to 100 ℃ for reflux reaction for 4h, cooling to room temperature after the reaction, filtering, washing with ethanol for 3 times, and obtaining the halogen-free intumescent flame retardant containing N, P elements under vacuum drying; in the step, dimethyl phosphate is selected as an acid source, sucrose is selected as a carbon source, and urea is selected as a nitrogen source, so that the intumescent flame retardant is prepared. Sucrose is selected as a carbon source, so that the method has the advantages of rich sources, no toxicity and no harm, and the cost of the flame retardant is reduced; urea is often used as a nitrogen fertilizer in agriculture, and has a rich nitrogen content, so that the urea is used as a nitrogen source of a flame retardant. The flame retardant has the advantages of good thermal stability, small hygroscopicity, good compatibility with polymer base materials, low toxicity, lasting flame retardant effect and the like; the most important flame retardant is a flame retardant with synergistic action of phosphorus and nitrogen, and is halogen-free;
S4, preparing a filler: immersing 6-15g of glass fiber into acetone solution for ultrasonic treatment and soaking overnight to remove impurities on the surface of the glass fiber; after drying at room temperature, the prepared glass fiber is put into a glass fiber tube which is prepared by concentrated sulfuric acid and concentrated nitric acid according to the volume ratio of 7:3, stirring overnight in the prepared solvent; mixing 80-100ml of KH550, 20-50ml of toluene solution and 30-40ml of deionized water, adding the pretreated glass fibers into the mixture to disperse for 0.5-1h, and refluxing at 110 ℃ for 8-10 hours; after the reaction is finished, cleaning by toluene and absolute ethyl alcohol, and then drying under vacuum to obtain amino modified glass fiber; placing the aminated glass fiber in 45-55mL of DMF, carrying out ultrasonic treatment for 30min, adding 20-30mL of succinic anhydride with the concentration of 1mol/L, stirring at 60 ℃ for 24h, washing the glass fiber with DMF and absolute ethyl alcohol after the reaction is finished, and then carrying out vacuum drying to obtain the multifunctional glass fiber with amino groups and carboxyl groups; preparing 100ml of cellulose/chitosan mixed solution with the concentration of 15wt%, wherein the mass ratio of cellulose to chitosan is 1:1, introducing 5-10g of multifunctional glass fiber into the mixed solution, then performing ultrasonic treatment for 0.5-1h to eliminate air bubbles in the system, and heating the prepared modified glass fiber/cellulose/chitosan composite material at 50 ℃ to obtain composite gel; in the step, after the glass fiber is acidified and aminated, the compatibility of the glass fiber is greatly improved, and the abundant functional groups in the gel preparation process are more favorable for the combination with cellulose and chitosan, so that a three-dimensional network structure is formed in the gel, and the structure can improve the toughness of the cable and ensure that the cable has higher impact strength; the glass fiber has good chemical stability, high temperature resistance and fireproof performance, the heat resistance temperature can reach more than 600 ℃, harmful smoke is not generated after the glass fiber is heated, and the flame retardant effect is further enhanced;
S5, preparing a flame-retardant fireproof material: weighing 7-9 g of polyethylene resin, respectively adding 20-30 ml of distilled water and 3-5 g of flame retardant prepared by S3, performing ball milling dispersion treatment at 3000r/min, then adding 0.6-1.5 g of curing agent, and magnetically stirring to uniform liquid to prepare the flame-retardant fireproof material; the addition of the flame retardant in the step can not only enhance the heat resistance and ductility of the polyethylene, but also generate no toxic and harmful gas and is safer when burning because the added flame retardant does not contain halogen; in addition, the flame retardant with the synergistic effect of phosphorus and nitrogen also enhances the thermal stability of the polyethylene;
s6, coating a layer of the flame-retardant fireproof material prepared in the step S5 on the outer wall of the conductor, filling 0.5-1 g of the composite gel prepared in the step S4 in a sleeve gap, then wrapping the outer wall of the sheath with the modified polyethylene prepared in the step S2, and finally sleeving the extruded 0.9-1.2 mm sheath on the surface of the flame-retardant fireproof layer to obtain the high flame-retardant anti-dripping fireproof cable.
Preferably: in the step S1, 3g of aluminum silicate is weighed.
Preferably: in the step S2, 10g of polyethylene particles and 0.85g of Mg-Fe@Al 2O3·SiO2 are weighed and added into 50ml of xylene, and stirred at 1500r/min and sonicated for 2.5h.
Preferably: 30mL of dimethyl phosphate, 16.5g of sucrose, 0.23g of anhydrous aluminum trichloride and 6.6g of urea are weighed in the step S3.
Preferably: the glass fiber addition amount in the step S4 is 10g, and the mixed acid is 100ml.
Preferably: in the step S4, the KH550 is used in an amount of 90ml, toluene is used in an amount of 30ml, deionized water is used in an amount of 30ml, the dispersing time is 1h, and the reflux time is 8h.
Preferably: the addition amount of succinic anhydride in the step S4 is 25ml, and the addition amount of the multifunctional glass fiber is 5.6g.
Preferably: 8.6g of polyethylene resin, 30ml of distilled water and 3.7g of the flame retardant prepared in S3 are weighed in the step S5.
Preferably: the filling amount of the composite gel in the step S6 is 1g.
By adopting the technical scheme, the invention has the technical advantages that:
1. According to the invention, aluminum silicate is selected as a substrate, and then magnesium element and iron element are introduced to modify the aluminum silicate, so that the thermal decomposition temperature of the polymer is increased, the combustion process of the polymer is delayed, the flame retardant property of the material is improved, and meanwhile, the dripping of the material in the ignition process is reduced; in addition, the specific surface area of the particles is further increased, and the dispersibility in other materials is also improved.
2. According to the invention, polyethylene is modified, and two elements of magnesium and iron have synergistic effect, so that the insulativity and the thermal stability of the polyethylene are obviously improved.
3. According to the invention, the intumescent flame retardant is prepared by taking dimethyl phosphate as an acid source, sucrose as a carbon source and urea as a nitrogen source. Sucrose is selected as a carbon source, so that the method has the advantages of rich sources, no toxicity and no harm, and the cost of the flame retardant is reduced; urea is rich in nitrogen and therefore serves as a nitrogen source for the flame retardant. The flame retardant has the advantages of good thermal stability, small hygroscopicity, good compatibility with polymer base materials, low toxicity, lasting flame retardant effect and the like; the most important flame retardant is a flame retardant with the synergistic effect of phosphorus and nitrogen, and is free of halogen and safer.
4. The glass fiber prepared by the invention has good dispersibility, because the modified surface of the glass fiber contains amino, carboxyl and other functional groups, compared with pure glass fiber, the dispersibility of the glass fiber in other materials is greatly improved; in addition, the abundant functional groups are favorable for the combination with cellulose and chitosan, so that a three-dimensional network structure is formed inside the gel, and the structure can improve the toughness of the cable, so that the cable has higher impact strength.
5. The flame-retardant fireproof material prepared by the invention has better thermal stability, because the flame retardant is subjected to ball milling treatment in the preparation process, the flame retardant is dispersed in the polyethylene matrix more uniformly, the addition of the flame retardant can not only enhance the heat resistance and ductility of the polyethylene, but also can not generate toxic and harmful gas due to the fact that the added flame retardant does not contain halogen during combustion, and is safer.
6. The cable material prepared by the invention has excellent performance, the preparation process is environment-friendly, and the harm to the environment is small.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments or the description of the prior art will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph showing limiting oxygen index of example 2, comparative example 4, and comparative example 5.
FIG. 2 is an electron microscope image of example 3.
FIG. 3 is an electron micrograph of comparative example 6.
FIG. 4 is a graph of limiting oxygen index for example 4 and comparative example 7.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved by the present invention more clear, the present invention is further described in detail below with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the present patent.
Example 1
S1, preparing modified aluminum silicate: 3g of aluminum silicate was weighed and added to 100mL of aluminum silicate at a volume ratio of 0.1mol/L each: 1, stirring for 8 hours at room temperature, filtering and drying, placing the obtained solid in a tube furnace, calcining at a temperature of 10 ℃/min under a nitrogen atmosphere at 600 ℃ for 3 hours, preserving heat for 1 hour, cooling, and taking out the solid to obtain magnesium/iron-loaded aluminum silicate particles, namely Mg-Fe@Al 2O3·SiO2;
S2, preparing modified polyethylene: weighing 10g of polyethylene particles and 0.85g of Mg-Fe@Al 2O3·SiO2 prepared by S1 according to parts by mass, adding into 50ml of xylene, stirring at 1500r/min, performing ultrasonic treatment for 2.5 hours, removing an ultrasonic device after the system is uniformly mixed, changing an oil bath for heating, and performing reduced pressure distillation for 30 minutes after the temperature is increased to 120 ℃ for stabilization, so as to obtain modified polyethylene;
S3, preparation of an intumescent flame retardant: adding 30mL of dimethyl phosphate into a 250mL three-neck flask with a magnetic stirrer, a thermometer and a reflux condenser, heating in an oil bath, adding 16.5g of sucrose, adding 0.23g of anhydrous aluminum trichloride, gradually heating to 120 ℃ for reflux reaction for 3 hours, adding 6.6g of urea for continuous stirring, heating to 100 ℃ for reflux reaction for 4 hours, cooling to room temperature after the reaction is finished, filtering, washing with ethanol for 3 times, and vacuum drying to obtain the halogen-free intumescent flame retardant containing N, P elements;
s4, preparing a filler: immersing 10g of glass fiber in an acetone solution for ultrasonic treatment and soaking overnight to remove impurities on the surface of the glass fiber; after drying at room temperature, the prepared glass fiber is put into a glass fiber tube which is prepared by concentrated sulfuric acid and concentrated nitric acid according to the volume ratio of 7:3, stirring the mixture overnight in 100ml of solvent prepared by the method; mixing 90ml of KH550, 30ml of toluene solution and 30ml of deionized water, adding the pretreated glass fiber into the mixture to disperse for 1 hour, and refluxing at 110 ℃ for 8 hours; after the reaction is finished, cleaning by toluene and absolute ethyl alcohol, and then drying under vacuum to obtain amino modified glass fiber; placing the aminated glass fiber in 45mL of DMF, carrying out ultrasonic treatment for 30min, then adding 25mL of succinic anhydride with the concentration of 1mol/L, stirring for 24h at 60 ℃, washing the glass fiber with DMF and absolute ethyl alcohol after the reaction is finished, and then carrying out vacuum drying to obtain the multifunctional glass fiber with amino groups and carboxyl groups; preparing 100ml of cellulose/chitosan mixed solution with the concentration of 15wt%, wherein the mass ratio of cellulose to chitosan is 1:1, introducing 5.6g of multifunctional glass fiber into the mixed solution, then performing ultrasonic treatment for 1h to eliminate air bubbles in the system, and heating the prepared modified glass fiber/cellulose/chitosan composite material at 50 ℃ to obtain composite gel;
S5, preparing a flame-retardant fireproof material: weighing 8.6g of polyethylene resin, respectively adding 30ml of distilled water and 3.7g of flame retardant prepared by S3, performing ball milling dispersion treatment at 3000r/min, adding 0.6g of curing agent, and magnetically stirring to uniform liquid to prepare the flame-retardant fireproof material;
S6, coating a layer of the flame-retardant fireproof material prepared in the step S5 on the outer wall of the conductor, filling 1g of the composite gel prepared in the step S4 in a sleeve gap, then wrapping the outer wall of the sheath with the modified polyethylene prepared in the step S2, and finally sleeving the extruded 0.9-1.2 mm sheath on the surface of the flame-retardant fireproof layer to obtain the high flame-retardant anti-dripping fireproof cable.
Comparative example 1: the procedure of example 1 was repeated except that magnesium sulfate was not added in step S1.
Comparative example 2: the procedure of example 1 was repeated except that iron nitrate was not added in step S2.
Comparative example 3: the procedure of example 1 was repeated except that magnesium sulfate and iron nitrate were not added in step S1.
The fire resistance test of the cable was carried out according to GB/T19216 test for the line integrity of cables or optical cables under flame conditions. After the fire supply time is reached, the fuse of the test device is continuous and the indicator lamp is not extinguished to pass.
The oxygen index (O.I) is an important flame retardant index of nonmetallic materials used for flame-retardant cables, and refers to the oxygen concentration of a material sample for maintaining stable combustion in a mixed gas flow of oxygen and nitrogen under a specified condition. Expressed as a volume percentage of oxygen in the mixed stream. The oxygen index 22 and below are inflammable materials, the oxygen indices 22 to 27 are flame retardant materials, and the oxygen index 27 or above is high flame retardant material.
Because the cable can produce smog after burning, thereby influence personnel's sight, reduce the probability of fleing, therefore it is very necessary to test the fuming amount after the cable burns, and main test standard is GB/T17681-2021, selects a certain amount of finished products according to the standard, places on the burning dish and burns the sample, in the room of fixed volume, measures the luminousness, if the luminousness is less than 60%, this test is unqualified.
Table 1 is the flame retardant data for the cables prepared in example 1, comparative example 2, comparative example 3, and table 1 shows that the cables obtained in example 1 have the best flame retardant properties, and it can be found that by introducing a single component into aluminum silicate, the properties can be improved to a lesser extent, and that after introducing two components, the properties are significantly improved due to the synergistic effect between magnesium and aluminum.
Table 1 analysis of flame retardant properties and smoke generation amounts of examples and comparative examples
Example 2
S1, preparing modified aluminum silicate: 3.8g of aluminum silicate was weighed and added to 100mL of aluminum silicate at a volume ratio of 0.1mol/L each: 1, stirring for 8 hours at room temperature, filtering and drying, placing the obtained solid in a tube furnace, calcining at a heating rate of 10 ℃/min at 500 ℃ for 3 hours under nitrogen atmosphere, preserving heat for 1 hour, cooling, and taking out the solid to obtain magnesium/iron-loaded aluminum silicate particles, namely Mg-Fe@Al 2O3·SiO2;
S2, preparing modified polyethylene: weighing 8.2g of polyethylene particles and 0.86g of Mg-Fe@Al 2O3·SiO2 prepared by S1 according to parts by mass, adding into 50ml of dimethylbenzene, stirring at 1500r/min, performing ultrasonic treatment for 2.5 hours, removing an ultrasonic device after the system is uniformly mixed, changing an oil bath for heating, and performing reduced pressure distillation for 30 minutes after the temperature is increased to 120 ℃ for stabilization, so as to obtain modified polyethylene;
S3, preparation of an intumescent flame retardant: adding 30mL of dimethyl phosphate into a 250mL three-neck flask provided with a magnetic stirrer, a thermometer and a reflux condenser, heating in an oil bath, adding 15g of sucrose, adding 0.25g of anhydrous aluminum trichloride, gradually heating to 120 ℃ for reflux reaction for 3 hours, adding 5.2g of urea for continuous stirring, heating to 100 ℃ for reflux reaction for 4 hours, cooling to room temperature after the reaction is finished, carrying out suction filtration, washing with ethanol for 3 times, and obtaining the halogen-free intumescent flame retardant containing N, P elements under vacuum drying;
S4, preparing a filler: immersing 6g of glass fiber in an acetone solution for ultrasonic treatment and soaking overnight to remove impurities on the surface of the glass fiber; after drying at room temperature, the prepared glass fiber is put into a glass fiber tube which is prepared by concentrated sulfuric acid and concentrated nitric acid according to the volume ratio of 7:3, stirring the mixture overnight in 100ml of solvent prepared by the method; mixing 80ml of KH550, 30ml of toluene solution and 40ml of deionized water, adding the pretreated glass fiber into the mixture to disperse for 1 hour, and refluxing at 110 ℃ for 8 hours; after the reaction is finished, cleaning by toluene and absolute ethyl alcohol, and then drying under vacuum to obtain amino modified glass fiber; placing the aminated glass fiber in 50mL of DMF, carrying out ultrasonic treatment for 30min, then adding 25mL of succinic anhydride with the concentration of 1mol/L, stirring for 24h at 60 ℃, washing the glass fiber with DMF and absolute ethyl alcohol after the reaction is finished, and then carrying out vacuum drying to obtain the multifunctional glass fiber with amino groups and carboxyl groups; preparing 100ml of cellulose/chitosan mixed solution with the concentration of 15wt%, wherein the mass ratio of cellulose to chitosan is 1:1, introducing 6.5g of multifunctional glass fiber into the mixed solution, then performing ultrasonic treatment for 1h to eliminate air bubbles in the system, and heating the prepared modified glass fiber/cellulose/chitosan composite material at 50 ℃ to obtain composite gel;
S5, preparing a flame-retardant fireproof material: weighing 7.5g of polyethylene resin, respectively adding 30ml of distilled water and 3.5g of flame retardant prepared by S3, performing ball milling dispersion treatment at 3000r/min, adding 0.6g of curing agent, and magnetically stirring to uniform liquid to prepare the flame-retardant fireproof material;
S6, coating a layer of the flame-retardant fireproof material prepared in the step S5 on the outer wall of the conductor, filling 0.8g of the composite gel prepared in the step S4 in a sleeve gap, then wrapping the outer wall of the sheath with the modified polyethylene prepared in the step S2, and finally sleeving the extruded 0.9-1.2 mm sheath on the surface of the flame-retardant fireproof layer to obtain the high flame-retardant anti-dripping fireproof cable.
Comparative example 4: the procedure of example 2 was repeated except that dimethyl phosphate was not added in step S3.
Comparative example 5: the procedure of example 2 was repeated except that urea was not added in step S3.
FIG. 1 is a graph showing limiting oxygen index data of example 2, comparative example 4 and comparative example 5, and it can be seen from the graph that the flame retardant effect of example 2 is best because the flame retardant prepared by the method is an intumescent flame retardant simultaneously containing N, P elements, wherein N, P has a synergistic effect, and the flame retardant effect can be improved well.
Example 3
S1, preparing modified aluminum silicate: 4.2g of aluminum silicate was weighed and added to 100mL of aluminum silicate at a volume ratio of 0.1mol/L each: 1, stirring for 8 hours at room temperature, filtering and drying, placing the obtained solid in a tube furnace, calcining at a temperature rising rate of 10 ℃/min at 650 ℃ for 3 hours under nitrogen atmosphere, preserving heat for 1 hour, cooling, and taking out the solid to obtain magnesium/iron-loaded aluminum silicate particles, namely Mg-Fe@Al 2O3·SiO2;
S2, preparing modified polyethylene: weighing 8.9g of polyethylene particles and 0.75g of Mg-Fe@Al 2O3·SiO2 prepared by S1 according to parts by mass, adding into 50ml of xylene, stirring at 1500r/min, performing ultrasonic treatment for 2.5 hours, removing an ultrasonic device after the system is uniformly mixed, changing an oil bath for heating, and performing reduced pressure distillation for 30 minutes after the temperature is increased to 120 ℃ for stabilization, so as to obtain modified polyethylene;
S3, preparation of an intumescent flame retardant: adding 30mL of dimethyl phosphate into a 250mL three-neck flask with a magnetic stirrer, a thermometer and a reflux condenser, heating in an oil bath, adding 16.2g of sucrose, adding 0.26g of anhydrous aluminum trichloride, gradually heating to 120 ℃ for reflux reaction for 3 hours, adding 7.5g of urea for continuous stirring, heating to 100 ℃ for reflux reaction for 4 hours, cooling to room temperature after the reaction is finished, filtering, washing with ethanol for 3 times, and vacuum drying to obtain the halogen-free intumescent flame retardant containing N, P elements;
S4, preparing a filler: immersing 12g of glass fiber in an acetone solution for ultrasonic treatment and soaking overnight to remove impurities on the surface of the glass fiber; after drying at room temperature, the prepared glass fiber is put into a glass fiber tube which is prepared by concentrated sulfuric acid and concentrated nitric acid according to the volume ratio of 7:3, stirring the mixture overnight in 100ml of solvent prepared by the method; 85ml of KH550, 35ml of toluene solution and 30ml of deionized water were mixed, and then the pretreated glass fiber was added to the mixture to be dispersed for 1 hour, and then refluxed at 110℃for 8 hours; after the reaction is finished, cleaning by toluene and absolute ethyl alcohol, and then drying under vacuum to obtain amino modified glass fiber; placing the aminated glass fiber in 50mL of DMF, carrying out ultrasonic treatment for 30min, then adding 30mL of succinic anhydride with the concentration of 1mol/L, stirring for 24h at 60 ℃, washing the glass fiber with DMF and absolute ethyl alcohol after the reaction is finished, and then carrying out vacuum drying to obtain the multifunctional glass fiber with amino groups and carboxyl groups; preparing 100ml of cellulose/chitosan mixed solution with the concentration of 15wt%, wherein the mass ratio of cellulose to chitosan is 1:1, introducing 7.3g of multifunctional glass fiber into the mixed solution, then performing ultrasonic treatment for 1h to eliminate air bubbles in the system, and heating the prepared modified glass fiber/cellulose/chitosan composite material at 50 ℃ to obtain composite gel;
s5, preparing a flame-retardant fireproof material: weighing 8.3g of polyethylene resin, respectively adding 30ml of distilled water and 3.7g of flame retardant prepared by S3, performing ball milling dispersion treatment at 3000r/min, adding 0.6g of curing agent, and magnetically stirring to uniform liquid to prepare the flame-retardant fireproof material;
S6, coating a layer of the flame-retardant fireproof material prepared in the step S5 on the outer wall of the conductor, filling 0.5g of the composite gel prepared in the step S4 in a sleeve gap, then wrapping the outer wall of the sheath with the modified polyethylene prepared in the step S2, and finally sleeving the extruded 0.9-1.2 mm sheath on the surface of the flame-retardant fireproof layer to obtain the high flame-retardant anti-dripping fireproof cable.
Comparative example 6: the procedure of example 3 was repeated except that succinic anhydride was not added in step S4.
Fig. 2 is an electron microscope image of the filler in example 3, and fig. 3 is an electron microscope image of the filler in comparative example 6, from which it can be seen that the glass fiber in example 3 has better dispersibility because the succinic anhydride modified the glass fiber has carboxyl functional groups introduced thereon, which can better interact with the functional groups on cellulose and chitosan, thereby better dispersing in the matrix, and the compact network structure also improves the fire resistance of the material.
Example 4
S1, preparing modified aluminum silicate: 2.6g of aluminum silicate was weighed and added to 100mL of aluminum silicate at a volume ratio of 0.1mol/L each: 1, stirring for 8 hours at room temperature, filtering and drying, placing the obtained solid in a tube furnace, calcining at a temperature of 10 ℃/min under a nitrogen atmosphere at 550 ℃ for 3 hours, preserving heat for 1 hour, cooling, and taking out the solid to obtain magnesium/iron-loaded aluminum silicate particles, namely Mg-Fe@Al 2O3·SiO2;
S2, preparing modified polyethylene: 9.3g of polyethylene particles and 0.66g of Mg-Fe@Al 2O3·SiO2 prepared by S1 are weighed according to parts by mass, added into 50ml of dimethylbenzene, stirred at 1500r/min and subjected to ultrasonic treatment for 2.5 hours, after the system is uniformly mixed, an ultrasonic device is removed, an oil bath is used for heating, after the temperature is raised to 120 ℃ and stable, reduced pressure distillation is carried out for 30 minutes, and solvent dimethylbenzene is removed, so that modified polyethylene is obtained;
S3, preparation of an intumescent flame retardant: adding 30mL of dimethyl phosphate into a 250mL three-neck flask provided with a magnetic stirrer, a thermometer and a reflux condenser, heating in an oil bath, adding 18g of sucrose, adding 0.28g of anhydrous aluminum trichloride, gradually heating to 120 ℃ for reflux reaction for 3 hours, adding 7.6g of urea for continuous stirring, heating to 100 ℃ for reflux reaction for 4 hours, cooling to room temperature after the reaction is finished, carrying out suction filtration, washing with ethanol for 3 times, and obtaining the halogen-free intumescent flame retardant containing N, P elements under vacuum drying;
s4, preparing a filler: immersing 8g of glass fiber in an acetone solution for ultrasonic treatment and soaking overnight to remove impurities on the surface of the glass fiber; after drying at room temperature, the prepared glass fiber is put into a glass fiber tube which is prepared by concentrated sulfuric acid and concentrated nitric acid according to the volume ratio of 7:3, stirring the mixture overnight in 100ml of solvent prepared by the method; mixing 90ml of KH550, 20ml of toluene solution and 40ml of deionized water, adding the pretreated glass fiber into the mixture to disperse for 1 hour, and refluxing at 110 ℃ for 8 hours; after the reaction is finished, cleaning by toluene and absolute ethyl alcohol, and then drying under vacuum to obtain amino modified glass fiber; placing the aminated glass fiber in 50mL of DMF, carrying out ultrasonic treatment for 30min, then adding 30mL of succinic anhydride with the concentration of 1mol/L, stirring for 24h at 60 ℃, washing the glass fiber with DMF and absolute ethyl alcohol after the reaction is finished, and then carrying out vacuum drying to obtain the multifunctional glass fiber with amino groups and carboxyl groups; preparing 100ml of cellulose/chitosan mixed solution with the concentration of 15wt%, wherein the mass ratio of cellulose to chitosan is 1:1, introducing 8.2g of multifunctional glass fiber into the mixed solution, then performing ultrasonic treatment for 1h to eliminate air bubbles in the system, and heating the prepared modified glass fiber/cellulose/chitosan composite material at 50 ℃ to obtain composite gel;
s5, preparing a flame-retardant fireproof material: weighing 7.8g of polyethylene resin, respectively adding 30ml of distilled water and 3.2g of flame retardant prepared by S3, performing ball milling dispersion treatment at 3000r/min, adding 0.6g of curing agent, and magnetically stirring to uniform liquid to prepare the flame-retardant fireproof material;
S6, coating a layer of the flame-retardant fireproof material prepared in the step S5 on the outer wall of the conductor, filling 1g of the composite gel prepared in the step S4 in a sleeve gap, then wrapping the outer wall of the sheath with the modified polyethylene prepared in the step S2, and finally sleeving the extruded 0.9-1.2 mm sheath on the surface of the flame-retardant fireproof layer to obtain the high flame-retardant anti-dripping fireproof cable.
Comparative example 7: the procedure of example 4 was repeated except that the modified polyethylene of the present invention was replaced with the ordinary polyethylene in step S6.
FIG. 4 is a graph showing limiting oxygen index of example 4 and comparative example 7, and Table 2 shows time-to-drip and smoke-generating conditions of the materials prepared in example 4 and comparative example 7. As can be seen from FIG. 4, the flame retardant effect of the material prepared in example 4 is best, because the flame retardant component is added into the polyethylene, and the dispersibility of the modified Mg-Fe@Al 2O3·SiO2 in the polyethylene matrix is improved, so that the flame retardant effect of the material is better improved; from table 2 it can be seen that the material prepared in example 4 takes longer to produce drips after combustion, because Mg-fe@al 2O3·SiO2 increases the temperature at which the polymer thermally decomposes and delays the polymer combustion process, thereby reducing drips when the material fires.
Table 2 anti-drip property and smoke analysis of examples and comparative examples
The above embodiments are merely illustrative of the preparation process of the present invention, and not intended to limit the scope of the present invention, and various modifications and improvements made by those skilled in the art to the technical solution of the present invention should fall within the protection scope defined by the claims of the present invention without departing from the design spirit of the present invention.
Claims (9)
1. A preparation process of a high-flame-retardance anti-dripping fireproof cable is characterized by comprising the following steps of: the preparation method comprises the following specific steps:
S1, preparing modified aluminum silicate: 1-5 g aluminum silicate is weighed and added to 100mL, and the volume ratio of the aluminum silicate to the 100:0.1 mol/L aluminum silicate is 1:1, stirring the mixed solution of MgSO 4、Fe (NO3) 3 at room temperature for 6-8: 8 h, filtering and drying, placing the obtained solid in a tube furnace, calcining at a heating rate of 10 ℃/min under nitrogen atmosphere at 460-680 ℃ for 3: 3h, preserving heat for 1:1 h, cooling, and taking out the solid to obtain magnesium/iron-loaded aluminum silicate particles, namely Mg-Fe@Al 2O3• SiO2;
S2, preparing modified polyethylene: weighing 8-10 g of polyethylene particles and 0.6-0.9 g of Mg-Fe@Al 2O3• SiO2 prepared by S1 according to parts by mass, adding into 30-50 ml of xylene, stirring at 1500-1600 r/min, performing ultrasonic treatment for 1-3 hours, removing an ultrasonic device after the system is uniformly mixed, changing an oil bath for heating, and performing reduced pressure distillation for 30 min after the temperature is increased to 120 ℃ for stabilization, and removing solvent xylene to obtain modified polyethylene;
S3, preparation of an intumescent flame retardant: adding 7.5-35 dimethyl phosphate of mL into a 250 mL three-neck flask with a magnetic stirrer, a thermometer and a reflux condenser, heating in an oil bath, adding 15-20 g sucrose, adding 0.2-0.3 g anhydrous aluminum trichloride, gradually heating to 120 ℃ for reflux reaction 3 h, adding 5-8 g urea for continuous stirring, heating to 100 ℃ for reflux reaction 4h, cooling to room temperature after the reaction is finished, filtering, washing with ethanol for 3 times, and obtaining the halogen-free intumescent flame retardant containing N, P elements under vacuum drying;
S4, preparing a filler: immersing 6-15g of glass fiber into acetone solution for ultrasonic treatment and soaking overnight to remove impurities on the surface of the glass fiber; after drying at room temperature, putting the prepared glass fiber into mixed acid, and stirring overnight; mixing 80-100ml of KH550, 20-50ml of toluene solution and 30-40ml of deionized water, adding the pretreated glass fibers into the mixture to disperse for 0.5-1h, and refluxing at 110 ℃ for 8-10 hours; after the reaction is finished, cleaning by toluene and absolute ethyl alcohol, and then drying under vacuum to obtain amino modified glass fiber; placing the aminated glass fiber in 45-55 mL DMF, carrying out ultrasonic treatment on the aminated glass fiber for 30min, then adding 20-30ml of succinic anhydride with the concentration of 1mol/L, stirring the mixture at the temperature of 60 ℃ for 24 hours, washing the glass fiber with DMF and absolute ethyl alcohol after the reaction is finished, and then carrying out vacuum drying to obtain the multifunctional glass fiber with amino groups and carboxyl groups; preparing 100ml of cellulose/chitosan mixed solution with the concentration of 15wt%, wherein the mass ratio of cellulose to chitosan is 1:1, introducing 5-10g of multifunctional glass fiber into the mixed solution, then performing ultrasonic treatment for 0.5-1h to eliminate air bubbles in the system, and heating the prepared modified glass fiber/cellulose/chitosan composite material at 50 ℃ to obtain composite gel;
S5, preparing a flame-retardant fireproof material: weighing 7-9 g of polyethylene resin, respectively adding 20-30 ml of distilled water and 3-5 g of flame retardant prepared by S3, performing ball milling dispersion treatment at a speed of 3000 r/min, then adding 0.6-1.5 g of curing agent, and magnetically stirring to uniform liquid to prepare the flame-retardant fireproof material;
And S6, coating a layer of the flame-retardant fireproof material prepared in the step S5 on the outer wall of the conductor, filling 0.5-1 g of the composite gel prepared in the step S4 in a gap of a sheath tube, then wrapping the outer wall of the sheath tube with the modified polyethylene prepared in the step S2, and finally sleeving the extruded 0.9-1.2 mm sheath on the surface of the flame-retardant layer of the modified polyethylene to obtain the high flame-retardant anti-dripping fireproof cable.
2. The process for preparing the high-flame-retardant anti-dripping fireproof cable according to claim 1, wherein the process comprises the following steps of: in the step S1, aluminum silicate is weighed to obtain 3 g.
3. The process for preparing the high-flame-retardant anti-dripping fireproof cable according to claim 1, wherein the process comprises the following steps of: 10g polyethylene particles and 0.85 g Mg-Fe@Al 2O3• SiO2 were weighed into 50 ml xylene in step S2, and stirred at 1500r/min and sonicated for 2.5 h.
4. The process for preparing the high-flame-retardant anti-dripping fireproof cable according to claim 2, wherein the process comprises the following steps of: 30mL of dimethyl phosphate, 16.5. 16.5 g of sucrose, 0.23. 0.23 g of anhydrous aluminum trichloride and 6.6. 6.6 g of urea are weighed in the step S3.
5. The process for preparing the high-flame-retardant anti-dripping fireproof cable according to claim 1, wherein the process comprises the following steps of: the glass fiber addition amount in the step S4 is 10 g, and the mixed acid addition amount is 100 ml.
6. The process for preparing the high-flame-retardant anti-dripping fireproof cable according to claim 5, wherein the process comprises the following steps of: in the step S4, the use amount of KH550 is 90 ml, the use amount of toluene is 30 ml, the use amount of deionized water is 30 ml, the dispersing time is 1h, and the reflux time is 8 h.
7. The process for preparing the high-flame-retardant anti-dripping fireproof cable according to claim 6, wherein the process comprises the following steps of: the addition amount of succinic anhydride in the step S4 is 25 ml, and the addition amount of the multifunctional glass fiber is 5.6 g.
8. The process for preparing the high-flame-retardant anti-dripping fireproof cable according to claim 4, wherein the process comprises the following steps of: the step S5 is to weigh 8.6 g polyethylene resin, 30. 30 ml distilled water and 3.7 g of the flame retardant prepared by S3.
9. The process for preparing the high-flame-retardant anti-dripping fireproof cable according to claim 1, wherein the process comprises the following steps of: the filling amount of the composite gel in the step S6 is 1g.
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