CN115109404A - Phosphorus-nitrogen expansion type halogen-free cable material and preparation method thereof - Google Patents
Phosphorus-nitrogen expansion type halogen-free cable material and preparation method thereof Download PDFInfo
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- CN115109404A CN115109404A CN202210797598.6A CN202210797598A CN115109404A CN 115109404 A CN115109404 A CN 115109404A CN 202210797598 A CN202210797598 A CN 202210797598A CN 115109404 A CN115109404 A CN 115109404A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 10
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- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims abstract description 42
- 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 26
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
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- 229920002803 thermoplastic polyurethane Polymers 0.000 claims abstract description 15
- 229920006228 ethylene acrylate copolymer Polymers 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 229920001971 elastomer Polymers 0.000 claims abstract description 10
- 239000000806 elastomer Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
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- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 8
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- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- 239000000178 monomer Substances 0.000 claims description 15
- 238000003756 stirring Methods 0.000 claims description 15
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
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- 238000012545 processing Methods 0.000 claims description 10
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- 239000001913 cellulose Substances 0.000 claims description 8
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- 239000012752 auxiliary agent Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 7
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 6
- 239000004970 Chain extender Substances 0.000 claims description 6
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 6
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- 229920005862 polyol Polymers 0.000 claims description 5
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- 238000001914 filtration Methods 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- JIGUQPWFLRLWPJ-UHFFFAOYSA-N Ethyl acrylate Chemical compound CCOC(=O)C=C JIGUQPWFLRLWPJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000005977 Ethylene Substances 0.000 claims description 3
- CTKINSOISVBQLD-UHFFFAOYSA-N Glycidol Chemical compound OCC1CO1 CTKINSOISVBQLD-UHFFFAOYSA-N 0.000 claims description 3
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 claims description 3
- 238000004040 coloring Methods 0.000 claims description 3
- 239000007822 coupling agent Substances 0.000 claims description 3
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 229920001684 low density polyethylene Polymers 0.000 claims description 3
- 239000004702 low-density polyethylene Substances 0.000 claims description 3
- 229940050906 magnesium chloride hexahydrate Drugs 0.000 claims description 3
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
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- 150000005846 sugar alcohols Polymers 0.000 claims 1
- 239000003822 epoxy resin Substances 0.000 description 7
- 229920000647 polyepoxide Polymers 0.000 description 7
- 229910052736 halogen Inorganic materials 0.000 description 4
- 150000002367 halogens Chemical class 0.000 description 4
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 4
- 239000000779 smoke Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 2
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 2
- 229910052794 bromium Inorganic materials 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 231100000053 low toxicity Toxicity 0.000 description 2
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
-
- 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
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/22—Halogen free composition
-
- 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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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a phosphorus-nitrogen intumescent halogen-free cable material, which comprises thermoplastic polyurethane, a maleic anhydride grafted styrene elastomer, an ethylene acrylate copolymer, a flame retardant and an anti-hydrolysis agent, wherein the mass ratio of the thermoplastic polyurethane to the maleic anhydride grafted styrene elastomer to the ethylene acrylate copolymer to the flame retardant to the anti-hydrolysis agent is 5: 3: 2: 10: 1; the flame retardant is diethyl dichlorophosphamide (DPAD), 27.5mL of phosphorus oxychloride is added into a 250mL three-neck flask which is provided with a reflux condenser tube, a thermometer, a nitrogen inlet tube and magnetons during production, 60mL of dichloromethane is added as a solvent, 62.5mL of EDA is added into a constant-pressure dropping funnel, and 30mL of dichloromethane solvent is used for dilution; introducing nitrogen for protection, starting dropwise adding the EDA solution under ice bath for reaction, and naturally heating to room temperature for reaction for 8 hours after the EDA is dropwise added. The invention relates to a phosphorus-nitrogen expansion type halogen-free cable material and a preparation method thereof, belonging to the field of halogen-free cable materials.
Description
Technical Field
The invention relates to the field of halogen-free cable materials, in particular to a phosphorus-nitrogen expansion type halogen-free cable material and a preparation method thereof.
Background
Low smoke zero halogen is a material classification for wire jackets in the wire and cable industry. The low-smoke halogen-free wire sheath is composed of thermoplastic or thermosetting materials which are low in smoke discharge amount when heated and do not contain halogen.
Disclosure of Invention
The invention mainly aims to provide a phosphorus-nitrogen expansion type halogen-free cable material and a preparation method thereof, which can effectively solve the problems in the background technology. The most used flame-retardant epoxy resins at present are halogen-containing advanced epoxy resins, which have incomparable advantages in fire-resistance, heat-resistance and electrical conductivity of precision instruments, and particularly the advanced bromine-containing epoxy resins currently play a significant role in sheet lamination and as flame-retardant for microelectronic devices. However, studies have shown that higher bromine-containing epoxy resins release irritating, corrosive toxic gases such as hydrogen bromide, polybrominated dibenzoxanes (PBDDs) and polybrominated dibenzofurans (PBDFs) during combustion, and that polybromides are strong carcinogens. How to replace halogen, the research of high-efficiency, low-toxicity and low-smoke halogen-free environment-friendly flame retardant and novel flame-retardant epoxy resin materials becomes a research hotspot of scholars at home and abroad.
In order to achieve the purpose, the invention adopts the technical scheme that:
the phosphorus-nitrogen expansion type halogen-free cable material comprises thermoplastic polyurethane, a maleic anhydride grafted styrene elastomer, an ethylene acrylate copolymer, a flame retardant and an anti-hydrolysis agent, wherein the mass ratio of the thermoplastic polyurethane to the maleic anhydride grafted styrene elastomer to the ethylene acrylate copolymer to the flame retardant to the anti-hydrolysis agent is 5: 3: 2: 10: 1.
Further, the flame retardant is diethyl dichlorophosphamide (DPAD), 27.5mL of phosphorus oxychloride is added into a 250mL three-necked bottle provided with a reflux condenser tube, a thermometer, a nitrogen inlet tube and a magneton during production, 60mL of dichloromethane is added as a solvent, 62.5mL of EDA is added into a constant-pressure dropping funnel, and 30mL of dichloromethane solvent is diluted; introducing nitrogen for protection, starting dropwise adding an EDA solution under ice bath for reaction, and naturally heating to room temperature for reaction for 8 hours after EDA is dropwise added; obtaining light yellow liquid slurry after the reaction is finished, and filtering, washing, rotatably steaming and drying the liquid to obtain colorless and transparent liquid; the method is characterized by comprising the following steps: adding 24mL of glycidol into a 250mL three-neck flask provided with a magnetic stirring device, a dropping funnel and a thermometer, adding 60mL of dichloromethane as a solvent, adding DPAD18.6mL and 80mL of dichloromethane into the dropping funnel for dilution, starting dropwise adding in ice bath, naturally heating to room temperature after 2h of dropwise adding is finished, reacting until no HCl gas is discharged, finishing the reaction, and processing to obtain light yellow liquid.
Further, in the halogen-free cable material, the thermoplastic polyurethane is prepared from raw materials including diphenylmethane diisocyanate, polyol and a chain extender; wherein, based on the total weight of the thermoplastic polyurethane, the content of the diphenylmethane diisocyanate is 40%, the content of the polyol is 45%, and the content of the chain extender is 3%.
Further, the ethylene acrylate copolymer is obtained by polymerizing ethylene with at least one of ethyl acrylate, 2-ethyl methacrylate and butyl acrylate.
Further, the ethylene acrylate copolymer is prepared as follows:
the method comprises the following steps: adding cellulose and deionized water into a reactor provided with a reflux condensing device, heating in a water bath to 60-90 ℃, and stirring to dissolve the cellulose and the deionized water;
step two: weighing an initiator, placing the initiator in a clean and dry container, adding monomers of styrene and acrylic ester, dissolving, and adding the mixture into the reactor in the first step;
step three: controlling the stirring speed to be 200-500 r/min, and reacting for 2-12 hours at constant temperature to form copolymer beads;
step four: after the reaction was stopped, the copolymer beads were washed with water, filtered and dried to give styrene-acrylate copolymers in the form of transparent beads; in the first step, the dosage of the cellulose is 0.05-20% of the total mass of the monomer styrene and the acrylate, and the dosage of the deionized water is 2-10 times of the total mass of the monomer styrene and the acrylate; in the second step, the dosage of the initiator is 0.3 to 10 percent of the total mass of the monomer styrene and the acrylate; in the second step, the mass ratio of the monomer styrene to the acrylate is 1: 0.01-100.
A phosphorus-nitrogen expansion type halogen-free cable material and a preparation method thereof comprise the following steps:
the method comprises the following steps: preparing raw materials and processing equipment, preparing various materials for preparing the halogen-free cable, putting the materials into a storage device for standby, and preparing the equipment required during processing.
Step two: and (3) preparing a mixed material, namely after the step one is finished, putting the materials into a mixing and stirring device according to a ratio by a worker, sequentially adding a certain amount of LDPE material, magnesium chloride hexahydrate, medical stone powder and a coupling agent into the mixing and stirring device, and mixing for the first time by using the mixing and stirring device to prepare the mixed material.
Step three: adding a flame retardant and an auxiliary agent, transferring the mixed material into a temperature-adjusting mixing device after the mixed material is prepared, adding the flame retardant and the auxiliary agent into the temperature-adjusting mixing device, and mixing the materials by using the temperature-adjusting mixing device.
Step four: adding a proper amount of carbon black into a temperature-regulating mixing device, coloring the whole mixture by using the carbon black, transferring the obtained mixture into an internal mixer, carrying out internal mixing on the mixture by using the internal mixer to prepare an internal mixed material, putting the prepared internal mixed material into a drying chamber, drying the internal mixed material to prepare a finished product, adding the dried material into a screw extruder, and carrying out mixing and granulation by using the screw extruder to prepare the finished cable material.
Compared with the prior art, the invention has the following beneficial effects:
the halogen-free cable material has low hardness, slow crystallization speed and good flame retardance and physical properties, and meanwhile, the phosphorus-nitrogen intumescent epoxy resin flame retardant has the advantages of low toxicity, high efficiency and environmental protection, is beneficial to continuous development, can be used as an epoxy resin diluent, has a flame retardant effect, and simultaneously has good mechanical properties of a cured product.
Drawings
FIG. 1 is a flow chart of the preparation of the present invention;
Detailed Description
In order to make the technical means, the creation characteristics, the achievement purposes and the effects of the invention easy to understand, the invention is further described with the specific embodiments.
As shown in fig. 1, a phosphorus-nitrogen expansion type halogen-free cable material comprises thermoplastic polyurethane, maleic anhydride grafted styrene elastomer, ethylene acrylate copolymer, flame retardant and hydrolysis resistant agent, wherein the mass ratio of the thermoplastic polyurethane, the maleic anhydride grafted styrene elastomer, the ethylene acrylate copolymer, the flame retardant and the hydrolysis resistant agent is 5: 3: 2: 10: 1; the flame retardant is diethyl dichlorophosphamide (DPAD), 27.5mL of phosphorus oxychloride is added into a 250mL three-neck flask which is provided with a reflux condenser tube, a thermometer, a nitrogen inlet tube and a magneton during production, 60mL of dichloromethane is added as a solvent, 62.5mL of EDA is added into a constant-pressure dropping funnel, and 30mL of dichloromethane solvent is diluted; introducing nitrogen for protection, starting dropwise adding an EDA solution under ice bath for reaction, and naturally heating to room temperature for reaction for 8 hours after EDA is dropwise added; obtaining light yellow liquid slurry after the reaction is finished, and filtering, washing, rotatably steaming and drying the liquid to obtain colorless and transparent liquid; the method is characterized by comprising the following steps: adding 24mL of glycidol into a 250mL three-neck flask provided with a magnetic stirring device, a dropping funnel and a thermometer, adding 60mL of dichloromethane serving as a solvent, adding 18.6mL of DPAD18 and 80mL of dichloromethane into the dropping funnel for dilution, starting dropwise adding in ice bath, naturally heating to room temperature after 2h of dropwise adding, reacting until no HCl gas is discharged, finishing the reaction, and processing to obtain a light yellow liquid; in the halogen-free cable material, the thermoplastic polyurethane is prepared from raw materials comprising diphenylmethane diisocyanate, polyol and a chain extender; wherein, based on the total weight of the thermoplastic polyurethane, the content of the diphenylmethane diisocyanate is 40 percent, the content of the polyol is 45 percent, and the content of the chain extender is 3 percent; the ethylene acrylate copolymer is obtained by polymerizing at least one of ethyl acrylate, 2-ethyl methacrylate and butyl acrylate with ethylene; the selected flame retardant and other auxiliary agents are screened to ensure compatibility with thermoplastic polyurethane, maleic anhydride grafted styrene elastomer and amino grafted styrene elastomer. In addition, the halogen-free cable material has good processing performance, surface effect and oil resistance, can be repeatedly used, and can be widely applied to the fields of industrial control cables, electronic cables, optical cables and the like.
Adding cellulose and deionized water into a reactor provided with a reflux condensing device during preparation of the ethylene acrylate copolymer, heating in a water bath to 60-90 ℃, stirring to dissolve the mixture, weighing an initiator, placing the initiator into a clean and dry container, adding monomer styrene and acrylate, dissolving, adding the dissolved initiator into the reactor in the step one, controlling the stirring speed to be 200-500 r/min, reacting at constant temperature for 2-12 hours to form copolymer beads, finally stopping the reaction, washing the copolymer beads with water, filtering and drying to obtain transparent beaded styrene-acrylate copolymer; in the first step, the dosage of the cellulose is 0.05-20% of the total mass of the monomer styrene and the acrylate, and the dosage of the deionized water is 2-10 times of the total mass of the monomer styrene and the acrylate; in the second step, the dosage of the initiator is 0.3 to 10 percent of the total mass of the monomer styrene and the acrylate; in the second step, the mass ratio of the monomer styrene to the acrylate is 1: 0.01-100.
When the halogen-free cable material is prepared, firstly, raw materials and processing equipment are prepared, various materials of the halogen-free cable are prepared, the materials are placed in a storage device for standby, meanwhile, the equipment required during processing is prepared, then, the materials are prepared, after the first step is completed, workers place the materials into a mixing and stirring device according to a proportion, a certain amount of LDPE material, magnesium chloride hexahydrate, medical stone powder and coupling agent are sequentially added into the mixing and stirring device, and the mixing and stirring device is utilized for first mixing to prepare mixed materials; adding a flame retardant and an auxiliary agent, transferring the mixed material into a temperature-regulating mixing device after the mixed material is prepared, adding the flame retardant and the auxiliary agent into the temperature-regulating mixing device, mixing the materials by using the temperature-regulating mixing device, finally adding a proper amount of carbon black into the temperature-regulating mixing device, coloring the whole mixed material by using the carbon black, transferring the obtained mixed material into an internal mixer, internally mixing the mixed material by using the internal mixer to prepare an internal mixed material, putting the prepared internal mixed material into a drying chamber, drying the internal mixed material to prepare a finished product, adding the dried material into a screw extruder, mixing and granulating by using the screw extruder to prepare a finished cable material.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (6)
1. A phosphorus-nitrogen expansion type halogen-free cable material is characterized in that: the cable material comprises the following raw materials in formula: the flame retardant comprises thermoplastic polyurethane, a maleic anhydride grafted styrene elastomer, an ethylene acrylate copolymer, a flame retardant and an anti-hydrolysis agent, wherein the mass ratio of the thermoplastic polyurethane to the maleic anhydride grafted styrene elastomer to the ethylene acrylate copolymer to the flame retardant to the anti-hydrolysis agent is 5: 3: 2: 10: 1.
2. The phosphorus-nitrogen intumescent halogen-free cable material of claim 2, characterized in that: the thermoplastic polyurethane is prepared from raw materials of diphenylmethane diisocyanate, polyhydric alcohol and a chain extender; wherein, based on the total weight of the thermoplastic polyurethane, the content of the diphenylmethane diisocyanate is 40%, the content of the polyol is 45%, and the content of the chain extender is 3%.
3. The phosphorus-nitrogen intumescent halogen-free cable material of claim 3, characterized in that: the ethylene acrylate copolymer is obtained by polymerizing ethylene with at least one of ethyl acrylate, 2-ethyl methacrylate and butyl acrylate.
4. The phosphorus-nitrogen intumescent halogen-free cable material as claimed in claim 1, characterized in that: the flame retardant is diethyl dichlorophosphamide (DPAD), and the production steps are as follows: adding 27.5mL of phosphorus oxychloride into a 250mL three-necked flask provided with a reflux condenser tube, a thermometer, a nitrogen inlet tube and magnetons, then adding 60mL of dichloromethane serving as a solvent, and adding 62.5mL of EDA and 30mL of dichloromethane solvent into a constant-pressure dropping funnel for dilution; introducing nitrogen for protection, starting dropwise adding an EDA solution under ice bath for reaction, and naturally heating to room temperature for reaction for 8 hours after EDA is dropwise added; obtaining light yellow liquid slurry after the reaction is finished, and filtering, washing, rotatably steaming and drying the liquid to obtain colorless and transparent liquid; adding 24mL of glycidol into a 250mL three-neck flask provided with a magnetic stirring device, a dropping funnel and a thermometer, adding 60mL of dichloromethane as a solvent, adding DPAD18.6mL and 80mL of dichloromethane into the dropping funnel for dilution, starting dropwise adding in ice bath, naturally heating to room temperature after 2h of dropwise adding is finished, reacting until no HCl gas is discharged, finishing the reaction, and processing to obtain light yellow liquid.
5. The phosphorus-nitrogen intumescent halogen-free cable material of claim 4, characterized in that: the preparation method of the ethylene acrylate copolymer comprises the following steps:
the method comprises the following steps: adding cellulose and deionized water into a reactor provided with a reflux condensing device, heating in a water bath to 60-90 ℃, and stirring to dissolve the cellulose and the deionized water;
step two: weighing an initiator, placing the initiator in a clean and dry container, adding monomers of styrene and acrylic ester, dissolving, and adding the mixture into the reactor in the first step;
step three: controlling the stirring speed to be 200-500 r/min, and reacting for 2-12 hours at constant temperature to form copolymer beads;
step four: after the reaction was stopped, the copolymer beads were washed with water, filtered and dried to give styrene-acrylate copolymers in the form of transparent beads; in the first step, the dosage of the cellulose is 0.05-20% of the total mass of the monomer styrene and the acrylate, and the dosage of the deionized water is 2-10 times of the total mass of the monomer styrene and the acrylate; in the second step, the amount of the initiator is 0.3 to 10 percent of the total mass of the monomer styrene and the acrylate; in the second step, the mass ratio of the monomer styrene to the acrylate is 1: 0.01-100.
6. The preparation method of the phosphorus-nitrogen intumescent halogen-free cable material as claimed in claim 1, characterized in that: the method comprises the following steps:
the method comprises the following steps: preparing raw materials and processing equipment, preparing various materials for preparing the halogen-free cable, putting the materials into a storage device for standby, and preparing the equipment required during processing.
Step two: and (3) preparing a mixed material, namely after the step one is finished, putting the materials into a mixing and stirring device according to a ratio by a worker, sequentially adding a certain amount of LDPE material, magnesium chloride hexahydrate, medical stone powder and a coupling agent into the mixing and stirring device, and mixing for the first time by using the mixing and stirring device to prepare the mixed material.
Step three: adding a flame retardant and an auxiliary agent, transferring the mixed material into a temperature-adjusting mixing device after the mixed material is prepared, adding the flame retardant and the auxiliary agent into the temperature-adjusting mixing device, and mixing the materials by using the temperature-adjusting mixing device.
Step four: adding a proper amount of carbon black into a temperature-regulating mixing device, coloring the whole mixture by using the carbon black, transferring the obtained mixture into an internal mixer, carrying out internal mixing on the mixture by using the internal mixer to prepare an internal mixed material, putting the prepared internal mixed material into a drying chamber, drying the internal mixed material to prepare a finished product, adding the dried material into a screw extruder, and carrying out mixing and granulation by using the screw extruder to prepare the finished cable material.
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| CN113956597A (en) * | 2021-11-12 | 2022-01-21 | 绍兴市聚成新材料科技股份有限公司 | Nitrogen, phosphorus and silicon ternary halogen-free synergistic flame-retardant thermoplastic elastomer and preparation method thereof |
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Application publication date: 20220927 |