CN115505186A - g-C containing melamine indirect intercalation 3 N 4 Flame-retardant cable material and preparation method thereof - Google Patents

g-C containing melamine indirect intercalation 3 N 4 Flame-retardant cable material and preparation method thereof Download PDF

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Publication number
CN115505186A
CN115505186A CN202110700786.8A CN202110700786A CN115505186A CN 115505186 A CN115505186 A CN 115505186A CN 202110700786 A CN202110700786 A CN 202110700786A CN 115505186 A CN115505186 A CN 115505186A
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parts
melamine
indirect
intercalation
flame
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Inventor
张倩
李亮
杭祖圣
余慧丽
董铁男
沈磊
丰柳
谢静宜
徐伯强
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Nanjing Institute of Technology
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Nanjing Institute of Technology
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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
    • C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L23/04—Homopolymers or copolymers of ethene
    • C08L23/06—Polyethene
    • 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
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2207/00—Properties characterising the ingredient of the composition
    • C08L2207/06—Properties of polyethylene
    • C08L2207/062—HDPE

Abstract

The invention relates to the technical field of wire and cable material preparation, and discloses a melamine-containing indirect intercalation g-C 3 N 4 The flame-retardant cable material and the preparation method thereof are calculated according to the parts by massThe flame-retardant cable material is prepared from the following components: high density polyethylene: 90-100 parts; melamine indirect intercalation g-C 3 N 4 Flame retardant: 15-25 parts; tris (2-chloropropyl) phosphate (TCPP): 10 parts of (A); plasticizer: 10-30 parts; lubricant: 0.5-2.5 parts; a stabilizer: 4 parts of a mixture; an anti-aging agent: 1-3 parts; antioxidant: 1-2 parts; accelerator (b): 1-1.5 parts. The invention uses melamine and g-C through indirect intercalation 3 N 4 The flame retardant is prepared on the basis, is different from the traditional cable flame-retardant composition material, improves the flame retardant property, simultaneously reduces the filling amount of hydroxide, improves the overall processing property of the cable material, and has melamine and g-C after intercalation 3 N 4 The cable material has the advantages of improving the comprehensive use performance of the cable material, simplifying the whole production and preparation process of the material, reducing the manufacturing cost and improving the production efficiency of the material.

Description

g-C containing melamine indirect intercalation 3 N 4 Flame-retardant cable material and preparation method thereof
Technical Field
The invention relates to the technical field of wire and cable material preparation, in particular to a melamine-containing indirect intercalation g-C 3 N 4 The flame-retardant cable material and the preparation method thereof.
Background
In recent years, electricity is the leading cause of fire, electricity consumption in society declines in year, but with continuous production and repeated production of enterprises, electricity consumption rises rapidly, and electrical fires increase. From the fire investigation, a large fire of 31.9%, particularly 57.8%, caused by electricity is also caused electrically. The causes of these electrical fires are mainly three points: the reason is that long-term use causes the aging of wire and cable materials; the second reason is the electrical leakage phenomenon caused by the wire and cable materials with reduced mechanical properties; the third reason is that the material of the cable is flammable due to the low ignition point and poor flame retardance of the materials of the wire and the cable. The fire caused by the three main reasons accounts for more than 50 percent of the total number of the fire, and the development of novel flame-retardant cable materials is urgent.
Currently, the most common flame retardant material in wire and cable materials is the thermoplastic polymer material, low Density Polyethylene (LDPE). The LDPE material is very inflammable in high-temperature and high-heat environments, and in order to achieve the flame-retardant effect of the traditional flame-retardant cable, a halogen flame retardant is added into the LDPE material. But it will release a lot of poisonous and harmful gas when burning, which threatens people's life. Therefore, in order to change the flame retardancy of the material and meet the requirements of excellent flame retardancy and no toxicity and harm during combustion, a novel halogen-free efficient flame retardant must be developed.
The Chinese patent CN110294880A discloses a cable material formula added with an aluminum hydroxide flame retardant, but the flame retardant used in the formula is a hydroxide flame retardant, which can cause serious reduction of mechanical properties. Chinese patent
CN201610076944.6 discloses a flame-retardant impact-resistant modified linear low-density polyethylene cable sheath material, wherein montmorillonite and the like are added into a flame retardant to reduce the filling amount of hydroxide and improve the processability, but the montmorillonite modification process is complex and has high production cost, and the industrial large-scale production is difficult to realize. Therefore, the search for more environmentally friendly and more efficient flame retardants is urgently needed in the field of cable manufacturing.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides an indirect intercalation g-C containing melamine 3 N 4 The flame-retardant cable material has excellent flame-retardant performance by being combined with multi-component ingredients, so that the comprehensive performance requirement of the flame-retardant cable is met, and the problem that the comprehensive use performance of the cable is reduced by the ingredients of the conventional flame-retardant cable material is solved.
(II) technical scheme
1. In order to achieve the purpose of flame retardant property, the invention provides the following technical scheme: melamine-containing indirect intercalation g-C 3 N 4 The flame-retardant cable material comprises the following components in parts by mass: 90-100 parts; melamine indirect intercalation g-C 3 N 4 Flame retardant: 15-25 parts; phosphoric acid tris (2-chloro)Propyl) ester (TCPP): 10 parts of (A); plasticizer: 10-30 parts; lubricant: 0.5-2.5 parts; a stabilizer: 4 parts of a mixture; an anti-aging agent: 1-3 parts; antioxidant: 1-2 parts; accelerator (b): 1-1.5 parts.
Preferably, the plasticizer is dioctyl terephthalate.
Preferably, the lubricant is chlorinated paraffin.
Preferably, the stabilizer is one or more of dibutyltin dilaurate, zinc stearate and barium hyaluronate.
Preferably, the anti-aging agent is one or a combination of anti-aging agent RD, anti-aging agent AW and anti-aging agent 4010.
Preferably, the antioxidant is one or a combination of more of antioxidant 1076, antioxidant 1010 and antioxidant 168.
Preferably, the accelerator is one or a combination of an accelerator M and an accelerator DM.
Preferably, the melamine is indirectly intercalated into g-C 3 N 4 The flame retardant consists of melamine and g-C 3 N 4 Synthesized by an indirect intercalation method.
Preferably, the melamine-containing indirect intercalated g-C 3 N 4 The flame-retardant cable material and the preparation method thereof comprise the following steps:
s1, preparing melamine indirect intercalation g-C 3 N 4 Flame retardant, melamine indirect intercalation g-C 3 N 4 The flame retardant consists of melamine and g-C 3 N 4 Synthesized by an indirect intercalation method, firstly, 1 to 3 parts of g-C 3 N 4 Soaking the powder in saturated copper sulfate solution for 2 hr, stirring at 25 deg.C and stirring speed of 110-130r/min to obtain suspension, vacuum filtering the suspension to obtain solid powder, and drying at 80 deg.C for 10 hr to obtain Cu sample 2+ -g-C 3 N 4 (ii) a Adding 1-3 parts of melamine into 13-15 parts of hydrazine hydrate solution to disperse in a three-neck flask, placing the three-neck flask with the mixed raw materials into an oil bath kettle, and stirring for 30 minutes at the temperature of 80 ℃ and the stirring speed of 90-110 r/min; then, 1-3 parts of Cu 2+ -g-C 3 N 4 Adding into a three-neck flask, stirring at 110-130r/min, keeping the reaction at 80 deg.C, and stirring for 1 hr; finally, the obtained product is filtered and dried for 24 hours at 80 ℃ to obtain the melamine indirect intercalation g-C 3 N 4 The flame retardant is used as a raw material for preparing the flame-retardant cable material;
s2, proportioning raw materials in parts by mass: high density polyethylene: 90-100 parts; melamine indirect intercalation g-C 3 N 4 Flame retardant: 15-25 parts; tris (2-chloropropyl) phosphate (TCPP): 10 parts of a binder; plasticizer: 10-30 parts; lubricant: 0.5-2.5 parts; a stabilizer: 4 parts; an anti-aging agent: 1-3 parts; antioxidant: 1-2 parts; accelerator (b): 1-1.5 parts of the raw materials, namely introducing the proportioned raw materials into a high-speed mixer, starting the high-speed mixer to stir the mixture and start heating, wherein the stirring speed range of the high-speed mixer is 500-600r/min, and the stirring time range of the high-speed mixer is 15-20min;
s3, stopping mixing and stirring by the high-speed mixer when the temperature of the materials in the high-speed mixer reaches 100-110 ℃;
and S4, cooling the uniformly mixed materials to room temperature, and adding the materials into a double-screw extruder for melt extrusion and granulation.
Preferably, the rotating speed range of the main machine of the twin-screw extruder in the S4 is 25-30rpm, the blanking speed range is 5-10rpm, and the specific processing temperature parameters of the twin-screw extruder are as follows:
name of each processing mechanism of double-screw extruder Heating temperature (. Degree. C.) of processing mechanism
One zone of host 110
Host computer two zone 110
Three zones of the host 115
Four zones of host 115
Five zones of host 117
Host six-zone 117
Seven zones of the host 117
Head area 120
Second area of machine head 120
(III) advantageous effects
Compared with the prior art, the invention provides the g-C containing the melamine indirect intercalation 3 N 4 The flame-retardant cable material and the preparation method thereof have the following beneficial effects:
1. the melamine-containing indirect intercalation g-C 3 N 4 The flame-retardant cable material is prepared by using melamine and g-C through indirect intercalation 3 N 4 The flame retardant is prepared on the basis, is different from the traditional cable flame-retardant composition material, and is beneficial to expanding melamine and g-C 3 N 4 The application field of (2) has important significance.
2. The melamine-containing indirect intercalation g-C 3 N 4 Is flame-retardantCable material, g-C indirectly intercalated by melamine 3 N 4 The flame retardant and the flame retardant have synergistic effect, so that the flame retardant performance is improved, the filling amount of hydroxide is reduced, the overall processing performance of the cable material is improved, and the production of raw materials is facilitated.
3. The melamine-containing indirect intercalation g-C 3 N 4 The flame-retardant cable material is prepared by inserting melamine into g-C by an intercalation compounding method 3 N 4 Interlaminar formation of melamine-Cu 2+ -g-C 3 N 4 The flame retardant after intercalation has melamine and g-C 3 N 4 Thereby increasing the comprehensive use performance of the cable material.
4. The melamine-containing indirect intercalation g-C 3 N 4 In the raw material preparation and production process, the whole production and preparation process of the material is simple, the manufacturing cost is reduced, the material production efficiency is improved, and the economic benefit of the product is improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
3. The invention provides a technical scheme that: g-C containing melamine indirect intercalation 3 N 4 The flame-retardant cable material is prepared from the following components in parts by mass: high density polyethylene: 90-100 parts; melamine indirect intercalation g-C 3 N 4 Flame retardant: 15-25 parts; tris (2-chloropropyl) phosphate (TCPP): 10 parts of (A); plasticizer: 10-30 parts; lubricant: 0.5-2.5 parts; a stabilizer: 4 parts of a mixture; an anti-aging agent: 1-3 parts; antioxidant: 1-2 parts; accelerator (b): 1-1.5 parts. The plasticizer is dioctyl terephthalate.
The lubricant is chlorinated paraffin.
The stabilizer is one or more of dibutyl tin dilaurate, zinc stearate, and barium hyaluronate.
The anti-aging agent is one or a combination of anti-aging agent RD, anti-aging agent AW and anti-aging agent 4010.
The antioxidant is one or more of antioxidant 1076, antioxidant 1010 and antioxidant 168.
The accelerator is one or a combination of an accelerator M and an accelerator DM.
Melamine indirect intercalation g-C 3 N 4 The flame retardant consists of melamine and g-C 3 N 4 Synthesized by an indirect intercalation method.
The high density polyethylene had a particle size of 120 mesh and the tris (2-chloropropyl) phosphate (TCPP) had a particle size range of 250 mesh.
Melamine, hydrazine hydrate solution, copper sulfate solution and g-C 3 N 4 Reacting with each other, and reacting the solution of g-C through hydrazine hydrate and copper sulfate solution 3 N 4 Is increased to enable intercalation of melamine, hydrazine hydrate solution and g-C 3 N 4 After the end of the stirring, the mixed material reaction particles were examined by transmission electron microscopy, scanning electron microscopy or infrared microscopy.
Example 1
Melamine-containing indirect intercalation g-C 3 N 4 The flame-retardant cable material and the preparation method thereof comprise the following steps:
s1, preparing melamine indirect intercalation g-C 3 N 4 Flame retardant, melamine indirect intercalation g-C 3 N 4 The flame retardant consists of melamine and g-C 3 N 4 Synthesized by an indirect intercalation method; first, 1 part of g-C 3 N 4 Soaking the powder in saturated copper sulfate solution for 2 hr, stirring at 25 deg.C with stirring speed of 100r/min to obtain suspension, vacuum filtering the suspension to obtain solid powder, and drying at 80 deg.C for 10 hr to obtain Cu sample 2+ -g-C 3 N 4 (ii) a 1 part of melamine is added to 15 parts of hydrazine hydrate solution and dispersed in a three-neck flask,placing the three-necked flask mixed with the raw materials into an oil bath kettle, wherein the placing temperature is 80 ℃, the stirring speed range is 100r/min, and the stirring is carried out for 30 minutes; then, 1 part of Cu 2+ -g-C 3 N 4 Adding into a three-neck flask, stirring at 120r/min, keeping the reaction at 80 ℃ and stirring for 1 hour; finally, the obtained product is filtered and dried for 24 hours at 80 ℃ to obtain the melamine indirect intercalated g-C 3 N 4 The flame retardant is used as a raw material for preparing the flame-retardant cable material;
s2, mixing the following raw materials in parts by mass: 100 parts of high-density polyethylene and melamine indirect intercalation g-C 3 N 4 Flame retardant: 15 parts of a mixture; tris (2-chloropropyl) phosphate (TCPP): 10 parts of (A); plasticizer: 10 parts of (A); lubricant: 0.5 part; a stabilizer: 4 parts; an anti-aging agent: 3 parts of a mixture; antioxidant: 1 part; accelerator (b): 1.5 parts.
5. Melamine indirect intercalation g-C 3 N 4 15 parts of flame retardant, 50 parts of magnesium hydroxide, 10 parts of plasticizer, 0.5 part of lubricant, 1.5 parts of stabilizer, 3 parts of anti-aging agent, 1 part of antioxidant and 1.5 parts of accelerator, introducing the proportioned raw materials into a high-speed mixer, starting the high-speed mixer to stir the mixture and start heating, wherein the stirring speed of the high-speed mixer is 524r/min, and the stirring time range of the high-speed mixer is 15-20min;
s3, stopping mixing and stirring by the high-speed mixer when the temperature of the materials in the high-speed mixer reaches 105 ℃;
and S4, cooling the uniformly mixed materials to room temperature, and adding the materials into a double-screw extruder for melt extrusion and granulation.
The rotating speed of the main machine of the double-screw extruder is 30rpm, the blanking speed is 10rpm, and the processing temperature parameters of the double-screw extruder are as follows:
name of each processing mechanism of double-screw extruder Heating temperature of processing mechanism(℃)
One zone of host 110
Host computer two zone 110
Three zones of the main machine 115
Four zones of host 115
Five zones of host 117
Six zones of host 117
Seven zones of the host 117
Head area 120
Second area of machine head 120
Example 2
Melamine-containing indirect intercalation g-C 3 N 4 The flame-retardant cable material and the preparation method thereof comprise the following steps:
s1, preparing melamine indirect intercalation g-C 3 N 4 Flame retardant, melamine indirect intercalation g-C 3 N 4 The flame retardant consists of melamine and g-C 3 N 4 Synthesized by an indirect intercalation method, firstly, 1 part of g-C 3 N 4 Soaking the powder in saturated copper sulfate solution for 2 hr, stirring at 25 deg.C with stirring speed of 100r/min to obtain suspension, vacuum filtering the suspension to obtain solid powder, and drying at 80 deg.C for 10 hr to obtain Cu sample 2+ -g-C 3 N 4 . 1 part of melamine is added into 15 parts of hydrazine hydrate solution to be dispersed in a three-neck flask, the three-neck flask with the mixed raw materials is placed in an oil bath pot, the placing temperature is 80 ℃, the stirring speed range is 100r/min, and the stirring is carried out for 30 minutes. Then, 1 part of Cu 2+ -g-C 3 N 4 The mixture was charged into a three-necked flask, stirred at a rate in the range of 120r/min, and the reaction was maintained at 80 ℃ and stirred for 1 hour. Finally, the obtained product is filtered and dried for 24 hours at 80 ℃ to obtain the melamine indirect intercalated g-C 3 N 4 The flame retardant is used as a raw material for preparing the flame-retardant cable material;
s2, mixing the following raw materials in parts by mass: 98 portions of high-density polyethylene and g-C of melamine indirect intercalation 3 N 4 Flame retardant: 17 parts of a solvent; tris (2-chloropropyl) phosphate (TCPP): 9 parts of (1); plasticizer: 14 parts of a binder; lubricant: 0.5 part; a stabilizer: 4. preparing; an anti-aging agent: 3 parts of a mixture; antioxidant: 1 part; accelerator (b): 1.5 parts, introducing the proportioned raw materials into a high-speed mixer, starting the high-speed mixer to stir the mixture and start heating, wherein the stirring speed of the high-speed mixer is 524r/min, and the stirring time of the high-speed mixer is 15-20min;
s3, stopping mixing and stirring by the high-speed mixer when the temperature of the materials in the high-speed mixer reaches 105 ℃;
and S4, cooling the uniformly mixed materials to room temperature, and adding the materials into a double-screw extruder for melt extrusion and granulation.
The rotating speed of the main machine of the double-screw extruder is 30rpm, the blanking speed is 10rpm, and the processing temperature parameters of the double-screw extruder are as follows:
name of each processing mechanism of double-screw extruder Heating temperature (. Degree. C.) of processing mechanism
One zone of host 110
Host computer two area 110
Three zones of the main machine 115
Four zones of host 115
Five zones of host 117
Host six-zone 117
Seven zones of the host 117
Head area 120
Second area of machine head 120
Example 3
Melamine-containing indirect intercalation g-C 3 N 4 The flame-retardant cable material and the preparation method thereof comprise the following steps:
s1, preparingg-C of indirect insertion layer of polycyanum amine 3 N 4 Fire retardant, melamine indirect intercalation g-C 3 N 4 The flame retardant consists of melamine and g-C 3 N 4 Synthesized by an indirect intercalation method, firstly, 1 part of g-C 3 N 4 Soaking the powder in saturated copper sulfate solution for 2 hr, stirring at 25 deg.C with stirring speed of 100r/min to obtain suspension, vacuum filtering the suspension to obtain solid powder, and drying at 80 deg.C for 10 hr to obtain Cu sample 2+ -g-C 3 N 4 . 1 part of melamine is added into 15 parts of hydrazine hydrate solution to be dispersed in a three-neck flask, the three-neck flask with the mixed raw materials is placed in an oil bath pot, the placing temperature is 80 ℃, the stirring speed range is 100r/min, and the stirring is carried out for 30 minutes. Then, 1 part of Cu 2+ -g-C 3 N 4 The mixture was charged into a three-necked flask, stirred at a rate in the range of 120r/min, and the reaction was maintained at 80 ℃ and stirred for 1 hour. Finally, the obtained product is filtered and dried for 24 hours at 80 ℃ to obtain the melamine indirect intercalated g-C 3 N 4 The flame retardant is used as a raw material for preparing the flame-retardant cable material;
s2, proportioning the following raw materials in parts by mass: 96 parts of high-density polyethylene and melamine indirect intercalation g-C 3 N 4 Flame retardant: 19 parts of: tris (2-chloropropyl) phosphate (TCPP): 8 parts of a mixture; plasticizer: 18 parts of a mixture; lubricant: 1.5 parts; a stabilizer: 4. preparing; an anti-aging agent: 3 parts of a mixture; antioxidant: 1 part; accelerator (b): 1.5 parts, introducing the proportioned raw materials into a high-speed mixer, starting the high-speed mixer to stir the mixture and start heating, wherein the stirring speed of the high-speed mixer is 524r/min, and the stirring time range of the high-speed mixer is 15-20min;
s3, stopping mixing and stirring by the high-speed mixer when the temperature of the materials in the high-speed mixer reaches 105 ℃;
and S4, cooling the uniformly mixed materials to room temperature, and adding the materials into a double-screw extruder for melt extrusion and granulation.
The rotating speed of the main machine of the double-screw extruder is 30rpm, the blanking speed is 10rpm, and the processing temperature parameters of the double-screw extruder are as follows:
name of each processing mechanism of double-screw extruder Heating temperature (. Degree. C.) of processing mechanism
One zone of host 110
Host computer two area 110
Three zones of the main machine 115
Four zones of host 115
Five zones of host 117
Six zones of host 117
Seven zones of the host 117
First zone of machine head 120
Second area of machine head 120
Example 4
A kind ofg-C containing melamine indirect intercalation 3 N 4 The flame-retardant cable material and the preparation method thereof comprise the following steps:
s1, preparing melamine indirect intercalation g-C 3 N 4 Fire retardant, melamine indirect intercalation g-C 3 N 4 The flame retardant consists of melamine and g-C 3 N 4 Synthesized by an indirect intercalation method, firstly, 1 part of g-C is added 3 N 4 Soaking the powder in saturated copper sulfate solution for 2 hr, stirring at 25 deg.C and stirring speed of 100r/min to obtain suspension, vacuum filtering the suspension to obtain solid powder, and drying at 80 deg.C for 10 hr to obtain Cu sample 2+ -g-C 3 N 4 . 1 part of melamine is added into 15 parts of hydrazine hydrate solution to be dispersed in a three-neck flask, the three-neck flask with the mixed raw materials is placed in an oil bath pot, the placing temperature is 80 ℃, the stirring speed range is 100r/min, and the stirring is carried out for 30 minutes. Then, 1 part of Cu 2+ -g-C 3 N 4 The mixture was charged into a three-necked flask, stirred at a rate in the range of 120r/min, and the reaction was maintained at 80 ℃ and stirred for 1 hour. Finally, the obtained product is filtered and dried for 24 hours at 80 ℃ to obtain the melamine indirect intercalation g-C 3 N 4 The flame retardant is used as a raw material for preparing the flame-retardant cable material;
s2, mixing the following raw materials in parts by mass: 94 parts of high-density polyethylene and g-C of melamine indirect intercalation 3 N 4 Flame retardant: 21 parts of (1); tris (2-chloropropyl) phosphate (TCPP): 7 parts; plasticizer: 22 parts of a binder; lubricant: 1.5 parts; a stabilizer: 4. preparing; an anti-aging agent: 3 parts of a mixture; antioxidant: 1 part; accelerator (b): 1.5 parts, introducing the proportioned raw materials into a high-speed mixer, starting the high-speed mixer to stir the mixture and start heating, wherein the stirring speed of the high-speed mixer is 524r/min, and the stirring time range of the high-speed mixer is 15-20min;
s3, stopping mixing and stirring by the high-speed mixer when the temperature of the materials in the high-speed mixer reaches 105 ℃;
and S4, cooling the uniformly mixed materials to room temperature, and adding the materials into a double-screw extruder for melt extrusion and granulation.
The rotating speed of the main machine of the double-screw extruder is 30rpm, the blanking speed is 10rpm, and the processing temperature parameters of the double-screw extruder body are as follows:
name of each processing mechanism of double-screw extruder Heating temperature (. Degree. C.) of processing mechanism
One zone of host 110
Host computer two zone 110
Three zones of the host 115
Four zones of host 115
Five zones of the host 117
Host six-zone 117
Seven zones of the host 117
Head area 120
Second zone of machine head 120
Example 5
Melamine-containing indirect intercalation g-C 3 N 4 The flame-retardant cable material and the preparation method thereof comprise the following steps:
s1, preparing melamine indirect intercalation g-C 3 N 4 Flame retardant, melamine indirect intercalation g-C 3 N 4 The flame retardant consists of melamine and g-C 3 N 4 Synthesized by an indirect intercalation method, firstly, 1 part of g-C 3 N 4 Soaking the powder in saturated copper sulfate solution for 2 hr, stirring at 25 deg.C and stirring speed of 100r/min to obtain suspension, vacuum filtering the suspension to obtain solid powder, and drying at 80 deg.C for 10 hr to obtain Cu sample 2+ -g-C 3 N 4 . 1 part of melamine is added into 15 parts of hydrazine hydrate solution to be dispersed in a three-neck flask, the three-neck flask with the mixed raw materials is placed in an oil bath pot, the placing temperature is 80 ℃, the stirring speed range is 100r/min, and the stirring is carried out for 30 minutes. Then, 1 part of Cu 2+ -g-C 3 N 4 The mixture was charged into a three-necked flask, stirred at a rate in the range of 120r/min, and the reaction was maintained at 80 ℃ and stirred for 1 hour. Finally, the obtained product is filtered and dried for 24 hours at 80 ℃ to obtain the melamine indirect intercalated g-C 3 N 4 The flame retardant is used as a raw material for preparing the flame-retardant cable material;
s2, mixing the following raw materials in parts by mass: 92 parts of high-density polyethylene and melamine indirect intercalation g-C 3 N 4 Flame retardant: 23 parts; tris (2-chloropropyl) phosphate (TCPP): 6 parts; plasticizer: 26 parts of (a); lubricant: 2.5 parts; a stabilizer: 4. preparing; an anti-aging agent: 1 part; antioxidant: 2 parts of (1); accelerator (b): 1 part, introducing the proportioned raw materials into a high-speed mixer, starting the high-speed mixer to stir the mixture and start heating, wherein the stirring speed of the high-speed mixer is 524r/min, and the stirring time of the high-speed mixer is 15-20min;
s3, stopping mixing and stirring by the high-speed mixer when the temperature of the materials in the high-speed mixer reaches 105 ℃;
and S4, cooling the uniformly mixed materials to room temperature, and adding the materials into a double-screw extruder for melt extrusion and granulation.
The rotating speed of the main machine of the double-screw extruder is 30rpm, the blanking speed is 10rpm, and the processing temperature parameters of the double-screw extruder body are as follows:
name of each processing mechanism of double-screw extruder Heating temperature (. Degree. C.) of processing mechanism
One zone of host 110
Host computer two area 110
Three zones of the main machine 115
Four zones of the host 115
Five zones of host 117
Six zones of host 117
Seven zones of the host 117
First zone of machine head 120
Second area of machine head 120
Example 6
Melamine-containing indirect intercalation g-C 3 N 4 The flame-retardant cable material and the preparation method thereof comprise the following steps:
s1, preparing melamine indirect intercalation g-C 3 N 4 Flame retardant, melamine indirect intercalation g-C 3 N 4 The flame retardant consists of melamine and g-C 3 N 4 Synthesized by an indirect intercalation method, firstly, 1 part of g-C 3 N 4 Soaking the powder in saturated copper sulfate solution for 2 hr, stirring at 25 deg.C with stirring speed of 100r/min to obtain suspension, vacuum filtering the suspension to obtain solid powder, and drying at 80 deg.C for 10 hr to obtain Cu sample 2+ -g-C 3 N 4 . 1 part of melamine is added into 15 parts of hydrazine hydrate solution to be dispersed in a three-neck flask, the three-neck flask with the mixed raw materials is placed in an oil bath pot, the placing temperature is 80 ℃, the stirring speed range is 100r/min, and the stirring is carried out for 30 minutes. Then, 1 part of Cu 2+ -g-C 3 N 4 The mixture was charged into a three-necked flask, stirred at a rate in the range of 120r/min, and the reaction was maintained at 80 ℃ and stirred for 1 hour. Finally, the obtained product is filtered and dried for 24 hours at 80 ℃ to obtain the melamine indirect intercalated g-C 3 N 4 The flame retardant is used as a raw material for preparing the flame-retardant cable material;
s2, mixing the following raw materials in parts by mass: 90 parts of high-density polyethylene and g-C of melamine indirect intercalation 3 N 4 Flame retardant: 25 parts of (1); tris (2-chloropropyl) phosphate (TCPP): 5 parts of a mixture; plasticizer: 30 parts of (1); lubricant: 2.5 parts; a stabilizer: 4. preparing; an anti-aging agent: 1 part; antioxidant: 2 parts of a mixture; accelerator (b): 1 part, guiding the proportioned raw materials into a high-speed mixer, starting the high-speed mixer to stir the mixture and start heating, wherein the stirring speed of the high-speed mixer is 524r/min, and the stirring time range of the high-speed mixer is 524r/min15-20min；
S3, stopping mixing and stirring by the high-speed mixer when the temperature of the materials in the high-speed mixer reaches 105 ℃;
and S4, cooling the uniformly mixed materials to room temperature, and adding the materials into a double-screw extruder for melt extrusion and granulation.
The rotating speed of the main machine of the double-screw extruder is 30rpm, the blanking speed is 10rpm, and the processing temperature parameters of the double-screw extruder are as follows:
name of each processing mechanism of double-screw extruder Heating temperature (. Degree. C.) of processing mechanism
One zone of host 110
Host computer two zone 110
Three zones of the host 115
Four zones of the host 115
Five zones of host 117
Host six-zone 117
Seven zones of the host 117
First zone of machine head 120
Second area of machine head 120
Comparative example 1
A preparation method of a flame-retardant cable material comprises the following steps:
s1, mixing the following raw materials in parts by mass: 90 parts of high-density polyethylene, 12.5 parts of melamine, g-C3N412.5 parts of tris (2-chloropropyl) phosphate (TCPP): 5 parts of plasticizer, 30 parts of plasticizer, 2.5 parts of lubricant, 4 parts of stabilizer, 1 part of anti-aging agent, 2 parts of antioxidant and 1 part of accelerator, the proportioned raw materials are introduced into a high-speed mixer, and the high-speed mixer is started to stir the mixture and start to heat the mixture;
s2, stopping mixing and stirring by the high-speed mixer when the temperature of the materials in the high-speed mixer reaches 105 ℃;
and S3, cooling the uniformly mixed materials to room temperature, and adding the materials into a double-screw extruder for melt extrusion and granulation.
The rotating speed of the main machine of the double-screw extruder is 30rpm, the blanking speed is 10rpm, and the processing temperature parameters of the double-screw extruder are as follows:
Figure BSA0000245468450000101
Figure BSA0000245468450000111
comparative example 2
A preparation method of a flame-retardant cable material comprises the following steps:
s1, mixing the following raw materials in parts by mass: 90 parts of high-density polyethylene, 30 parts of magnesium hydroxide, 30 parts of plasticizer, 2.5 parts of lubricant, 4 parts of stabilizer, 1 part of anti-aging agent, 2 parts of antioxidant and 1 part of accelerator, introducing the proportioned raw materials into a high-speed mixer, starting the high-speed mixer to stir the mixture and start heating;
s2, stopping mixing and stirring by the high-speed mixer when the temperature of the materials in the high-speed mixer reaches 105 ℃;
and S3, cooling the uniformly mixed materials to room temperature, and adding the materials into a double-screw extruder for melt extrusion and granulation.
The rotating speed of the main machine of the double-screw extruder is 30rpm, the blanking speed is 10rpm, and the processing temperature parameters of the double-screw extruder are as follows:
name of each processing mechanism of double-screw extruder Heating temperature (. Degree. C.) of processing mechanism
One zone of host 110
Host computer two area 110
Three zones of the main machine 115
Four zones of host 115
Five zones of host 117
Six zones of host 117
Seven zones of the host 117
Head area 120
Second area of machine head 120
The cable materials prepared in examples 1 to 6 and comparative examples 1 to 2 were tested for their properties, and the results are shown in the following table. Wherein the tensile test method is according to ASTM D-638 standard; the flame retardant property is subjected to a combustion test according to a method of UL94-2012, and the combustion characteristic of the polymer material is evaluated according to an oxygen index method of GB/T2406-93.
(1) Tensile properties test results:
Figure BSA0000245468450000112
Figure BSA0000245468450000121
(2) UL94 vertical burn test results:
Figure BSA0000245468450000122
by combining the various examples with comparative examples, it can be seen that melamine is indirectly intercalated into g-C 3 N 4 The flame retardant is added into the high-density polyethylene cable sheath formula material, so that the flame retardant property of the cable sheath is effectively improved.
The beneficial effects of the invention are: by indirect intercalation with melamine and g-C 3 N 4 The flame retardant is prepared on the basis, is different from the traditional cable flame-retardant composition material,the flame retardant property is improved, the filling amount of hydroxide is reduced, the integral processing property of the cable material is improved, and the flame retardant after intercalation has melamine and g-C 3 N 4 The cable material has the advantages of improving the comprehensive use performance of the cable material, simplifying the whole production and preparation process of the material, reducing the manufacturing cost and improving the production efficiency of the material.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (10)

1. Melamine-containing indirect intercalation g-C 3 N 4 The flame-retardant cable material is prepared from the following components in parts by mass: high density polyethylene: 90-100 parts; melamine indirect intercalation g-C 3 N 4 Flame retardant: 15-25 parts; tris (2-chloropropyl) phosphate (TCPP): 10 parts of a binder; plasticizer: 10-30 parts; lubricant: 0.5-2.5 parts; a stabilizer: 4 parts; an anti-aging agent: 1-3 parts; antioxidant: 1-2 parts; accelerator (b): 1-1.5 parts.
2. The indirectly intercalated g-C containing melamine as claimed in claim 1 3 N 4 The plasticizer is dioctyl terephthalate.
3. The claim 1 of a melamine-containing indirect intercalated g-C 3 N 4 The lubricant is chlorinated paraffin.
4. The indirectly intercalated g-C containing melamine as claimed in claim 1 3 N 4 The stabilizer is one or a combination of more of dibutyltin dilaurate, zinc stearate and barium hyaluronate.
5. The claim 1 of a melamine-containing indirect intercalated g-C 3 N 4 The anti-aging agent is one or a combination of an anti-aging agent RD, an anti-aging agent AW and an anti-aging agent 4010.
6. The indirectly intercalated g-C containing melamine as claimed in claim 1 3 N 4 The antioxidant is one or a combination of more of antioxidant 1076, antioxidant 1010 and antioxidant 168.
7. The indirectly intercalated g-C containing melamine as claimed in claim 1 3 N 4 The accelerant is one or a combination of accelerant M and accelerant DM.
8. The indirectly intercalated g-C containing melamine as claimed in claim 1 3 N 4 The melamine indirect intercalation g-C 3 N 4 The flame retardant consists of melamine and g-C 3 N 4 Synthesized by an indirect intercalation method.
9. The claim 1 of a melamine-containing indirect intercalated g-C 3 N 4 The flame-retardant cable material and the preparation method thereof comprise the following steps:
s1, preparing melamine indirect intercalation g-C 3 N 4 Flame retardant, melamine indirect intercalation g-C 3 N 4 The flame retardant consists of melamine and g-C 3 N 4 Synthesized by an indirect intercalation method; first, 1-3 parts of g-C 3 N 4 Soaking the powder in saturated copper sulfate solution for 2 hr, stirring at 25 deg.C at 110-130r/min to obtain suspension; drying the solid powder obtained after the suspension is subjected to suction filtration at the temperature of 80 ℃ for 10 hours to obtain a sample Cu 2+ -g-C 3 N 4 (ii) a Adding 1-3 parts of melamine into 13-15 parts of hydrazine hydrate solution to be dispersed in a three-neck flask, and placing the three-neck flask with mixed raw materials into the three-neck flaskThe mixture is put into an oil bath kettle, the temperature is 80 ℃, the stirring speed range is 90-110r/min, and the stirring is carried out for 30 minutes; then, 1-3 parts of Cu 2+ -g-C 3 N 4 Adding into a three-neck flask, stirring at 110-130r/min, keeping the reaction at 80 deg.C, and stirring for 1 hr; finally, the obtained product is filtered and dried for 24 hours at 80 ℃ to obtain the melamine indirect intercalation g-C 3 N 4 The flame retardant is used as a raw material for preparing the flame-retardant cable material;
s2, mixing the following raw materials in parts by mass: high density polyethylene: 90-100 parts; melamine indirect intercalation g-C 3 N 4 Flame retardant: 15-25 parts; tris (2-chloropropyl) phosphate (TCPP): 10 parts of a binder; plasticizer: 10-30 parts; lubricant: 0.5-2.5 parts; a stabilizer: 4 parts of a mixture; an anti-aging agent: 1-3 parts; antioxidant: 1-2 parts; accelerator (b): 1-1.5 parts of the raw materials, namely, introducing the proportioned raw materials into a high-speed mixer, starting the high-speed mixer to stir the mixture and start heating, wherein the stirring speed range of the high-speed mixer is 500-600r/min, and the stirring time range of the high-speed mixer is 15-20min;
s3, stopping mixing and stirring by the high-speed mixer when the temperature of the materials in the high-speed mixer reaches 100-110 ℃;
and S4, cooling the uniformly mixed materials to room temperature, and adding the materials into a double-screw extruder for melt extrusion and granulation.
10. The claim 9 of a melamine-containing indirect intercalated g-C 3 N 4 The rotation speed range of the host machine of the double-screw extruder in S4 is 25-30rpm, the blanking speed range is 5-10rpm, and the specific processing temperature parameters of the double-screw extruder are as follows:
name of each processing mechanism of double-screw extruder Heating temperature (deg.C) of processing mechanism) One zone of host 110 Host computer two area 110 Three zones of the main machine 115 Four zones of host 115 Five zones of host 117 Six zones of host 117 Seven zones of the host 117 Head area 120 Second area of machine head 120
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