CN110951191A - Cable material containing supramolecular self-assembly flame retardant and preparation method thereof - Google Patents

Cable material containing supramolecular self-assembly flame retardant and preparation method thereof Download PDF

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CN110951191A
CN110951191A CN201911291617.2A CN201911291617A CN110951191A CN 110951191 A CN110951191 A CN 110951191A CN 201911291617 A CN201911291617 A CN 201911291617A CN 110951191 A CN110951191 A CN 110951191A
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parts
flame retardant
melamine
phytic acid
cable material
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程斌
张林锐
杭祖圣
余慧丽
潘飞雄
王经逸
诸亚红
朱伟曦
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Wuxi Huamei Cable Co ltd
Nanjing Institute of Technology
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Wuxi Huamei Cable Co ltd
Nanjing Institute of Technology
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/04Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
    • C08L27/06Homopolymers or copolymers of vinyl chloride
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K13/00Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
    • C08K13/02Organic and inorganic ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/16Nitrogen-containing compounds
    • C08K5/34Heterocyclic compounds having nitrogen in the ring
    • C08K5/3467Heterocyclic compounds having nitrogen in the ring having more than two nitrogen atoms in the ring
    • C08K5/3477Six-membered rings
    • C08K5/3492Triazines
    • C08K5/34922Melamine; Derivatives thereof
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/49Phosphorus-containing compounds
    • C08K5/51Phosphorus bound to oxygen
    • C08K5/52Phosphorus bound to oxygen only
    • C08K5/521Esters of phosphoric acids, e.g. of H3PO4
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01BCABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/18Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
    • H01B3/30Insulators 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
    • H01B3/44Insulators 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
    • H01B3/443Insulators 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 vinylhalogenides or other halogenoethylenic compounds
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2227Oxides; Hydroxides of metals of aluminium
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/02Flame or fire retardant/resistant
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • C08L2203/202Applications use in electrical or conductive gadgets use in electrical wires or wirecoating

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Abstract

The invention relates to a cable material containing a supermolecule self-assembly flame retardant and a preparation method thereof, belonging to the field of manufacturing of wire and cable materials; the flame-retardant cable material is prepared from the following raw materials in parts by weight: polyvinyl chloride: 90-110 parts; melamine phytic acid flame retardant: 1-5 parts; plasticizer: 30-50 parts; lubricant: 1-3 parts; a stabilizer: 28-48 parts; 4-6 parts of an antioxidant; the cable material containing the supermolecule self-assembly flame retardant prepared by the invention has excellent thermal stability and flame retardant property, and meets the performance requirement of the cable.

Description

Cable material containing supramolecular self-assembly flame retardant and preparation method thereof
Technical Field
The invention relates to the field of manufacturing of wire and cable materials, in particular to a cable material containing a supermolecule self-assembly flame retardant and a preparation method thereof.
Background
Polyvinyl chloride, one of the most widely used plastics in the modern world, plays an important role in many consumer fields, such as automobiles, electronic materials, power cables, and the like. However, polyvinyl chloride, which is a polymer material, is easily decomposed and aged by light, heat, oxygen, or the like, and the cable is finally aged to cause a fire accident. Therefore, it is very necessary to improve the flame retardancy. Halogenated flame retardants are no longer acceptable because they generate a large amount of toxic fumes during combustion. Compared with halogenated flame retardants, the halogen-free flame retardants are hot spots in related fields due to the outstanding advantages of no toxicity, drip resistance, environmental protection and the like. However, in order to obtain the desired properties, high doses of conventional halogen-free flame retardants are required. This inevitably leads to a reduction in the thermal stability and mechanical properties of the cable.
Chinese patent CN103232631A discloses a halogen-free low-smoke flame-retardant cable sheath material and a preparation method thereof, but most of the flame retardant used in the cable sheath material is hydroxide flame retardant, which causes serious reduction of mechanical properties. Chinese patent CN101012326A discloses a halogen-free flame-retardant cable sheath material, wherein montmorillonite is added into a flame retardant to reduce the filling amount of hydroxide and improve the processing performance, but the montmorillonite modification mostly adopts intercalation compound type, the process is complex, the production cost is high, 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
The invention discloses a cable material containing a supermolecule self-assembly flame retardant and a preparation method thereof, aiming at the problems in the prior art.
The invention is realized by the following steps:
the cable material containing the supermolecule self-assembly flame retardant is prepared from the following components in parts by mass: polyvinyl chloride: 90-110 parts; melamine phytic acid flame retardant: 1-5 parts; aluminum hydroxide: 52-67 parts; plasticizer: 30-50 parts; lubricant: 1-3 parts; a stabilizer: 28-48 parts; 4-6 parts of an antioxidant.
Further, the melamine phytic acid flame retardant is prepared by synthesizing melamine and phytic acid through a supermolecule self-assembly technology, wherein 4-6 parts of melamine and 5-7 parts of phytic acid are aqueous solutions in parts by mass.
Further, the supramolecular self-assembly technology specifically comprises the following steps: firstly, dispersing 4-6 parts of melamine in a three-neck flask through deionized water, putting the three-neck flask into an oil bath kettle at the temperature of 80 ℃, and stirring for 10 minutes; secondly, 5-7 parts of phytic acid aqueous solution is dripped into a three-neck flask through a funnel, the reaction is kept at 80 ℃ and stirred for 0.5 h; finally, the obtained product is filtered and washed 5-6 times by deionized water at 60 ℃, and dried for 24 hours at 80 ℃ to obtain the melamine phytic acid flame retardant.
Further, the plasticizer is dioctyl phthalate.
Further, the lubricant is one or a combination of stearic acid and polyethylene wax.
Further, the stabilizer is one or a combination of more of calcium stearate, zinc stearate, barium stearate and Ca-Zn hydrotalcite.
Further, the antioxidant is one or a combination of more of an antioxidant 1076, an antioxidant 1010 and an antioxidant 168.
The invention also discloses a preparation method of the flame-retardant cable material prepared by supermolecule self-assembly, which is characterized by comprising the following steps:
step one, weighing according to actual needs, and mixing polyvinyl chloride: 90-110 parts; melamine phytic acid flame retardant: 1-5 parts; aluminum hydroxide: 52-67 parts; plasticizer: 30-50 parts; lubricant: 1-3 parts; a stabilizer: 28-48 parts; 4-6 parts of antioxidant are added into a high-speed mixer;
step two, stopping mixing when the temperature of the materials in the high-speed mixer reaches 100-;
and step three, cooling the materials to room temperature, adding the cooled materials into a double-screw extruder, and performing melt extrusion granulation.
Further, the melamine phytic acid flame retardant is prepared by a supermolecule self-assembly technology, and specifically, firstly, 4-6 parts of melamine are dispersed in a three-neck flask through deionized water, and are put into an oil bath kettle at 80 ℃ and stirred for 10 minutes; next, 5 to 7 parts of an aqueous phytic acid solution was dropped into the three-necked flask through a funnel. The reaction was maintained at 80 ℃ and stirred for 0.5 h; finally, the obtained product is filtered and washed 5-6 times by deionized water at 60 ℃, and dried for 24 hours at 80 ℃ to obtain the melamine phytic acid flame retardant.
Further, the temperature parameters of the twin-screw extruder in the third step are as follows: granulation temperature of the twin-screw extruder: the temperatures of a first host machine area, a second host machine area, a third host machine area, a fourth host machine area, a fifth host machine area, a sixth host machine area, a seventh host machine area, a first handpiece area and a second handpiece area are respectively 110 ℃, 113 ℃, 115 ℃, 120 ℃ and 120 ℃; the rotating speed of the main machine of the double-screw extruder is 25-30rpm, and the blanking speed is 5-10 rpm.
Compared with the prior art, the invention has the beneficial effects that:
1. in the invention, the flame retardant is prepared on the basis of melamine and phytic acid by a supramolecular self-assembly technology, which is beneficial to expanding the application fields of the melamine and the phytic acid and has important significance, and the application of the supramolecular self-assembly technology is an introduction to the preparation of the cable material of the flame retardant;
2. in the invention, the melamine phytic acid flame retardant has high phosphorus and nitrogen element contents, and the phosphorus and nitrogen element contents synergistically act to improve the flame retardant property. Meanwhile, the filling amount of the hydroxide is reduced, and the processing performance is improved.
3. In the invention, the two-dimensional melamine phytic acid prepared by supermolecule self-assembly plays a role of a barrier, the formation of carbon is promoted when the carbon is heated and decomposed, the carbon further resists heat transfer, the thermal decomposition of polyvinyl chloride can be relieved, and the thermal stability at high temperature is improved;
4. the performance index of the cable material containing the supermolecule self-assembly flame retardant prepared by the invention meets the relevant standard specification, the whole production and preparation process of the product is simple, the manufacturing cost is reduced, the production efficiency is improved, and the economic benefit is improved.
Detailed Description
In order to better illustrate the invention, the following examples are given. It should be emphasized that the examples are not meant to limit the scope of the invention to the conditions described in the examples, which are intended to further illustrate the content of the invention and its feasibility.
Example 1
The cable material containing the supramolecular self-assembly flame retardant in the embodiment 1 is characterized in that the flame retardant cable material is prepared from the following components in parts by mass: 90 parts of polyvinyl chloride; 1 part of melamine phytic acid flame retardant; aluminum hydroxide: 67 parts; 30 parts of a plasticizer; 1 part of a lubricant; 48 parts of a stabilizer; and 7 parts of an antioxidant.
Wherein, the melamine phytic acid flame retardant is synthesized by melamine and phytic acid through a supermolecular self-assembly technology. First, 4 parts of melamine were dispersed in a three-necked flask by deionized water and placed in an oil bath pan at 80 ℃ and stirred for 10 minutes. Next, 7 parts of an aqueous phytic acid solution was dropped into a three-necked flask through a funnel. The reaction was kept at 80 ℃ and stirred for 0.5 h. Finally, the obtained product was filtered and washed 6 times with deionized water at 60 ℃ and dried at 80 ℃ for 24 hours to obtain the melamine phytic acid flame retardant.
Wherein the plasticizer is dioctyl phthalate; the lubricant is one or a combination of stearic acid and polyethylene wax; the stabilizer is one or a combination of more of calcium stearate, zinc stearate, barium stearate and Ca-Zn hydrotalcite; the antioxidant is one or a combination of more of antioxidant 1076, antioxidant 1010 and antioxidant 168.
The preparation method comprises the following steps:
step one, weighing 90 parts of polyvinyl chloride according to actual needs; 1 part of melamine phytic acid flame retardant; aluminum hydroxide: 67 parts; 30 parts of a plasticizer; 1 part of a lubricant; 48 parts of a stabilizer; adding 7 parts of antioxidant into a high-speed mixer;
step two, stopping mixing when the temperature of the materials in the high-speed mixer reaches 110 ℃;
and step three, cooling the materials to room temperature, adding the cooled materials into a double-screw extruder, and performing melt extrusion granulation.
Wherein, the temperature parameters of the twin-screw extruder in the third step are as follows: granulation temperature of the twin-screw extruder: the temperatures of a first host machine area, a second host machine area, a third host machine area, a fourth host machine area, a fifth host machine area, a sixth host machine area, a seventh host machine area, a first handpiece area and a second handpiece area are respectively 110 ℃, 113 ℃, 115 ℃, 120 ℃ and 120 ℃; the rotating speed of the main machine of the double-screw extruder is 30rpm, and the blanking speed is 10 rpm.
Example 2
The cable material containing the supramolecular self-assembly flame retardant in the embodiment 2 is characterized in that the flame retardant cable material is prepared from the following components in parts by mass: 94 parts of polyvinyl chloride; 2 parts of melamine phytic acid flame retardant; aluminum hydroxide: 64 parts; 34 parts of a plasticizer; 1 part of a lubricant; 44 parts of a stabilizer; and 4 parts of an antioxidant.
Wherein, the melamine phytic acid flame retardant is synthesized by melamine and phytic acid through a supermolecular self-assembly technology. First, 4 parts of melamine were dispersed in a three-necked flask by deionized water and placed in an oil bath pan at 80 ℃ and stirred for 10 minutes. Next, 7 parts of an aqueous phytic acid solution was dropped into a three-necked flask through a funnel. The reaction was kept at 80 ℃ and stirred for 0.5 h. Finally, the obtained product was filtered and washed 6 times with deionized water at 60 ℃ and dried at 80 ℃ for 24 hours to obtain the melamine phytic acid flame retardant.
Wherein the plasticizer is dioctyl phthalate; the lubricant is one or a combination of stearic acid and polyethylene wax; the stabilizer is one or a combination of more of calcium stearate, zinc stearate, barium stearate and Ca-Zn hydrotalcite; the antioxidant is one or a combination of more of antioxidant 1076, antioxidant 1010 and antioxidant 168.
The preparation method comprises the following steps:
step one, weighing 94 parts of polyvinyl chloride according to actual requirements; 2 parts of melamine phytic acid flame retardant; aluminum hydroxide: 64 parts; 34 parts of a plasticizer; 1 part of a lubricant; 44 parts of a stabilizer; adding 4 parts of antioxidant into a high-speed mixer;
step two, stopping mixing when the temperature of the materials in the high-speed mixer reaches 110 ℃;
and step three, cooling the materials to room temperature, adding the cooled materials into a double-screw extruder, and performing melt extrusion granulation.
Wherein, the temperature parameters of the twin-screw extruder in the third step are as follows: granulation temperature of the twin-screw extruder: the temperatures of a first host machine area, a second host machine area, a third host machine area, a fourth host machine area, a fifth host machine area, a sixth host machine area, a seventh host machine area, a first handpiece area and a second handpiece area are respectively 110 ℃, 113 ℃, 115 ℃, 120 ℃ and 120 ℃; the rotating speed of the main machine of the double-screw extruder is 30rpm, and the blanking speed is 10 rpm.
Example 3
The cable material containing the supramolecular self-assembly flame retardant in the embodiment 3 is characterized in that the flame retardant cable material is prepared from the following components in parts by mass: 98 parts of polyvinyl chloride; 3 parts of melamine phytic acid flame retardant; aluminum hydroxide: 61 parts; 38 parts of a plasticizer; 2 parts of a lubricant; 40 parts of a stabilizer; and 5 parts of an antioxidant.
Wherein, the melamine phytic acid flame retardant is synthesized by melamine and phytic acid through a supermolecular self-assembly technology. First, 5 parts of melamine were dispersed in a three-necked flask by deionized water and placed in an oil bath pan at 80 ℃ and stirred for 10 minutes. Next, 6 parts of an aqueous phytic acid solution was dropped into a three-necked flask through a funnel. The reaction was kept at 80 ℃ and stirred for 0.5 h. Finally, the obtained product was filtered and washed 6 times with deionized water at 60 ℃ and dried at 80 ℃ for 24 hours to obtain the melamine phytic acid flame retardant.
Wherein the plasticizer is dioctyl phthalate; the lubricant is one or a combination of stearic acid and polyethylene wax; the stabilizer is one or a combination of more of calcium stearate, zinc stearate, barium stearate and Ca-Zn hydrotalcite; the antioxidant is one or a combination of more of antioxidant 1076, antioxidant 1010 and antioxidant 168.
The preparation method comprises the following steps:
step one, weighing 98 parts of polyvinyl chloride according to actual needs; 3 parts of melamine phytic acid flame retardant; aluminum hydroxide: 61 parts; 38 parts of a plasticizer; 2 parts of a lubricant; 40 parts of a stabilizer; adding 5 parts of antioxidant into a high-speed mixer;
step two, stopping mixing when the temperature of the materials in the high-speed mixer reaches 110 ℃;
and step three, cooling the materials to room temperature, adding the cooled materials into a double-screw extruder, and performing melt extrusion granulation.
Wherein, the temperature parameters of the twin-screw extruder in the third step are as follows: granulation temperature of the twin-screw extruder: the temperatures of a first host machine area, a second host machine area, a third host machine area, a fourth host machine area, a fifth host machine area, a sixth host machine area, a seventh host machine area, a first handpiece area and a second handpiece area are respectively 110 ℃, 113 ℃, 115 ℃, 120 ℃ and 120 ℃; the rotating speed of the main machine of the double-screw extruder is 30rpm, and the blanking speed is 10 rpm.
Example 4
The cable material containing the supramolecular self-assembly flame retardant in the embodiment 4 is characterized in that the flame retardant cable material is prepared from the following components in parts by mass: 102 parts of polyvinyl chloride; 3 parts of melamine phytic acid flame retardant; aluminum hydroxide: 58 parts of a mixture; 42 parts of a plasticizer; 2 parts of a lubricant; 36 parts of a stabilizer; and 5 parts of an antioxidant.
Wherein, the melamine phytic acid flame retardant is synthesized by melamine and phytic acid through a supermolecular self-assembly technology. First, 5 parts of melamine were dispersed in a three-necked flask by deionized water and placed in an oil bath pan at 80 ℃ and stirred for 10 minutes. Next, 6 parts of an aqueous phytic acid solution was dropped into a three-necked flask through a funnel. The reaction was kept at 80 ℃ and stirred for 0.5 h. Finally, the obtained product was filtered and washed 6 times with deionized water at 60 ℃ and dried at 80 ℃ for 24 hours to obtain the melamine phytic acid flame retardant.
Wherein the plasticizer is dioctyl phthalate; the lubricant is one or a combination of stearic acid and polyethylene wax; the stabilizer is one or a combination of more of calcium stearate, zinc stearate, barium stearate and Ca-Zn hydrotalcite; the antioxidant is one or a combination of more of antioxidant 1076, antioxidant 1010 and antioxidant 168.
The preparation method comprises the following steps:
step one, weighing 98 parts of polyvinyl chloride according to actual needs; 3 parts of melamine phytic acid flame retardant; aluminum hydroxide: 58 parts of a mixture; 38 parts of a plasticizer; 2 parts of a lubricant; 40 parts of a stabilizer; adding 5 parts of antioxidant into a high-speed mixer;
step two, stopping mixing when the temperature of the materials in the high-speed mixer reaches 110 ℃;
and step three, cooling the materials to room temperature, adding the cooled materials into a double-screw extruder, and performing melt extrusion granulation.
Wherein, the temperature parameters of the twin-screw extruder in the third step are as follows: granulation temperature of the twin-screw extruder: the temperatures of a first host machine area, a second host machine area, a third host machine area, a fourth host machine area, a fifth host machine area, a sixth host machine area, a seventh host machine area, a first handpiece area and a second handpiece area are respectively 110 ℃, 113 ℃, 115 ℃, 120 ℃ and 120 ℃; the rotating speed of the main machine of the double-screw extruder is 30rpm, and the blanking speed is 10 rpm.
Example 5
The cable material containing the supramolecular self-assembly flame retardant in the embodiment 5 is characterized in that the flame retardant cable material is prepared from the following components in parts by mass: 106 parts of polyvinyl chloride; 4 parts of melamine phytic acid flame retardant; aluminum hydroxide: 55 parts of (1); 46 parts of a plasticizer; 3 parts of a lubricant; 32 parts of a stabilizer; 6 parts of an antioxidant.
Wherein, the melamine phytic acid flame retardant is synthesized by melamine and phytic acid through a supermolecular self-assembly technology. First, 6 parts of melamine were dispersed in a three-necked flask by deionized water and placed in an oil bath pan at 80 ℃ and stirred for 10 minutes. Next, 5 parts of an aqueous phytic acid solution was dropped into a three-necked flask through a funnel. The reaction was kept at 80 ℃ and stirred for 0.5 h. Finally, the obtained product was filtered and washed 6 times with deionized water at 60 ℃ and dried at 80 ℃ for 24 hours to obtain the melamine phytic acid flame retardant.
Wherein the plasticizer is dioctyl phthalate; the lubricant is one or a combination of stearic acid and polyethylene wax; the stabilizer is one or a combination of more of calcium stearate, zinc stearate, barium stearate and Ca-Zn hydrotalcite; the antioxidant is one or a combination of more of antioxidant 1076, antioxidant 1010 and antioxidant 168.
The preparation method comprises the following steps:
step one, weighing 106 parts of polyvinyl chloride according to actual requirements; 4 parts of melamine phytic acid flame retardant; aluminum hydroxide: 55 parts of (1); 46 parts of a plasticizer; 3 parts of a lubricant; 32 parts of a stabilizer; adding 6 parts of antioxidant into a high-speed mixer;
step two, stopping mixing when the temperature of the materials in the high-speed mixer reaches 110 ℃;
and step three, cooling the materials to room temperature, adding the cooled materials into a double-screw extruder, and performing melt extrusion granulation.
Wherein, the temperature parameters of the twin-screw extruder in the third step are as follows: granulation temperature of the twin-screw extruder: the temperatures of a first host machine area, a second host machine area, a third host machine area, a fourth host machine area, a fifth host machine area, a sixth host machine area, a seventh host machine area, a first handpiece area and a second handpiece area are respectively 110 ℃, 113 ℃, 115 ℃, 120 ℃ and 120 ℃; the rotating speed of the main machine of the double-screw extruder is 30rpm, and the blanking speed is 10 rpm.
Example 6
The cable material containing the supramolecular self-assembly flame retardant in the embodiment 6 is characterized in that the flame retardant cable material is prepared from the following components in parts by mass: 110 parts of polyvinyl chloride; 5 parts of melamine phytic acid flame retardant; aluminum hydroxide: 52 parts of (1); 50 parts of a plasticizer; 3 parts of a lubricant; 28 parts of a stabilizer; 6 parts of an antioxidant.
Wherein, the melamine phytic acid flame retardant is synthesized by melamine and phytic acid through a supermolecular self-assembly technology. First, 6 parts of melamine were dispersed in a three-necked flask by deionized water and placed in an oil bath pan at 80 ℃ and stirred for 10 minutes. Next, 5 parts of an aqueous phytic acid solution was dropped into a three-necked flask through a funnel. The reaction was kept at 80 ℃ and stirred for 0.5 h. Finally, the obtained product was filtered and washed 6 times with deionized water at 60 ℃ and dried at 80 ℃ for 24 hours to obtain the melamine phytic acid flame retardant.
Wherein the plasticizer is dioctyl phthalate; the lubricant is one or a combination of stearic acid and polyethylene wax; the stabilizer is one or a combination of more of calcium stearate, zinc stearate, barium stearate and Ca-Zn hydrotalcite; the antioxidant is one or a combination of more of antioxidant 1076, antioxidant 1010 and antioxidant 168.
The preparation method comprises the following steps:
step one, weighing 106 parts of polyvinyl chloride according to actual requirements; 4 parts of melamine phytic acid flame retardant; aluminum hydroxide: 52 parts of (1); 46 parts of a plasticizer; 3 parts of a lubricant; 32 parts of a stabilizer; adding 6 parts of antioxidant into a high-speed mixer;
step two, stopping mixing when the temperature of the materials in the high-speed mixer reaches 110 ℃;
and step three, cooling the materials to room temperature, adding the cooled materials into a double-screw extruder, and performing melt extrusion granulation.
Wherein, the temperature parameters of the twin-screw extruder in the third step are as follows: granulation temperature of the twin-screw extruder: the temperatures of a first host machine area, a second host machine area, a third host machine area, a fourth host machine area, a fifth host machine area, a sixth host machine area, a seventh host machine area, a first handpiece area and a second handpiece area are respectively 110 ℃, 113 ℃, 115 ℃, 120 ℃ and 120 ℃; the rotating speed of the main machine of the double-screw extruder is 30rpm, and the blanking speed is 10 rpm.
Comparative example
The cable material containing the supermolecule self-assembly flame retardant in the comparative example is characterized by being prepared from the following components in parts by mass: 100 parts of polyvinyl chloride; aluminum hydroxide: 60 parts; 40 parts of a plasticizer; 2 parts of a lubricant; 38 parts of a stabilizer; and 5 parts of an antioxidant.
Wherein the plasticizer is dioctyl phthalate; the lubricant is one or a combination of stearic acid and polyethylene wax; the stabilizer is one or a combination of more of calcium stearate, zinc stearate, barium stearate and Ca-Zn hydrotalcite; the antioxidant is one or a combination of more of antioxidant 1076, antioxidant 1010 and antioxidant 168.
The preparation method comprises the following steps:
step one, weighing 106 parts of polyvinyl chloride according to actual requirements; 46 parts of a plasticizer; 3 parts of a lubricant; 32 parts of a stabilizer; adding 6 parts of antioxidant into a high-speed mixer;
step two, stopping mixing when the temperature of the materials in the high-speed mixer reaches 110 ℃;
and step three, cooling the materials to room temperature, adding the cooled materials into a double-screw extruder, and performing melt extrusion granulation.
Wherein, the temperature parameters of the twin-screw extruder in the third step are as follows: granulation temperature of the twin-screw extruder: the temperatures of a first host machine area, a second host machine area, a third host machine area, a fourth host machine area, a fifth host machine area, a sixth host machine area, a seventh host machine area, a first handpiece area and a second handpiece area are respectively 110 ℃, 113 ℃, 115 ℃, 120 ℃ and 120 ℃; the rotating speed of the main machine of the double-screw extruder is 30rpm, and the blanking speed is 10 rpm.
The cable materials prepared in the above examples 1 to 6 and comparative example were subjected to performance tests, and the test results are shown in the following table. Wherein the tensile test method is according to ASTM D-638 standard; the flame retardant properties were tested according to method UL 94-2012.
(1) Tensile properties test results:
Figure BDA0002319290900000091
(2) UL94 vertical burn test results
Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Comparative example
Flame retardancy V-0 V-0 V-0 V-0 V-0 V-0 V-0
The above table shows that the melamine phytic acid flame retardant prepared by the supermolecule self-assembly technology is added into the polyvinyl chloride cable sheath formula material, so that the thermal stability and the flame retardant property of the cable sheath are effectively improved.
The above description is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, several modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.

Claims (10)

1. The cable material containing the supermolecule self-assembly flame retardant is characterized by being prepared from the following components in parts by mass: polyvinyl chloride: 90-110 parts; melamine phytic acid flame retardant: 1-5 parts; aluminum hydroxide: 52-67 parts; plasticizer: 30-50 parts; lubricant: 1-3 parts; a stabilizer: 28-48 parts; 4-6 parts of an antioxidant.
2. The cable material containing the supramolecular self-assembly flame retardant as claimed in claim 1, wherein the melamine phytic acid flame retardant is prepared by synthesizing melamine and phytic acid through a supramolecular self-assembly technology, and the melamine phytic acid flame retardant comprises 4-6 parts by mass and the phytic acid is an aqueous solution and comprises 5-7 parts by mass.
3. The cable material containing the supramolecular self-assembly flame retardant as claimed in claim 2, wherein the supramolecular self-assembly technology is specifically as follows:
firstly, dispersing 4-6 parts of melamine in a three-neck flask through deionized water, putting the three-neck flask into an oil bath kettle at the temperature of 80 ℃, and stirring for 10 minutes; secondly, 5-7 parts of phytic acid aqueous solution is dripped into a three-neck flask through a funnel, the reaction is kept at 80 ℃ and stirred for 0.5 h; finally, the obtained product is filtered and washed 5-6 times by deionized water at 60 ℃, and dried for 24 hours at 80 ℃ to obtain the melamine phytic acid flame retardant.
4. The cable material containing supramolecular self-assembled flame retardant as claimed in claim 1, wherein said plasticizer is dioctyl phthalate.
5. The cable material containing supramolecular self-assembled flame retardant as claimed in claim 1, wherein said lubricant is one or a combination of stearic acid and polyethylene wax.
6. The cable material of claim 1, wherein the stabilizer is one or more selected from the group consisting of calcium stearate, zinc stearate, barium stearate, and Ca-Zn hydrotalcite.
7. The cable material containing the supramolecular self-assembled flame retardant as claimed in claim 1, wherein the antioxidant is one or more of antioxidant 1076, antioxidant 1010 and antioxidant 168.
8. The preparation method of the supramolecular self-assembly prepared flame-retardant cable material as claimed in any one of claims 1 to 7, characterized in that the method comprises the following steps:
step one, weighing according to actual needs, and mixing polyvinyl chloride: 90-110 parts; melamine phytic acid flame retardant: 1-5 parts; aluminum hydroxide: 52-67 parts; plasticizer: 30-50 parts; lubricant: 1-3 parts; a stabilizer: 28-48 parts; 4-6 parts of antioxidant are added into a high-speed mixer;
step two, stopping mixing when the temperature of the materials in the high-speed mixer reaches 100-;
and step three, cooling the materials to room temperature, adding the cooled materials into a double-screw extruder, and performing melt extrusion granulation.
9. The preparation method of the low temperature resistant flame retardant cable material according to claim 8, wherein the melamine phytic acid flame retardant is prepared by a supramolecular self-assembly technology, specifically, firstly, 4-6 parts of melamine is dispersed in a three-neck flask by deionized water, and is put into an oil bath pan at 80 ℃ to be stirred for 10 minutes; secondly, 5-7 parts of phytic acid aqueous solution is dripped into a three-neck flask through a funnel, the reaction is kept at 80 ℃ and stirred for 0.5 h; finally, the obtained product is filtered and washed 5-6 times by deionized water at 60 ℃, and dried for 24 hours at 80 ℃ to obtain the melamine phytic acid flame retardant.
10. The method for preparing a low temperature resistant flame retardant cable material as claimed in claim 8, wherein the temperature parameters of the twin-screw extruder in the third step are as follows: granulation temperature of the twin-screw extruder: the temperatures of a first host machine area, a second host machine area, a third host machine area, a fourth host machine area, a fifth host machine area, a sixth host machine area, a seventh host machine area, a first handpiece area and a second handpiece area are respectively 110 ℃, 113 ℃, 115 ℃, 120 ℃ and 120 ℃; the rotating speed of the main machine of the double-screw extruder is 25-30rpm, and the blanking speed is 5-10 rpm.
CN201911291617.2A 2019-12-16 2019-12-16 Cable material containing supramolecular self-assembly flame retardant and preparation method thereof Pending CN110951191A (en)

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CN115232359A (en) * 2022-08-19 2022-10-25 南京工程学院 Nitrogen-phosphorus multi-element synergistic flame retardant and preparation method thereof
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CN111690197A (en) * 2020-07-02 2020-09-22 南京工程学院 Melamine-containing direct intercalation g-C3N4Flame-retardant cable material and preparation method thereof
CN111690197B (en) * 2020-07-02 2022-09-13 南京工程学院 Melamine-containing direct intercalation g-C 3 N 4 Flame-retardant cable material and preparation method thereof
CN112300517A (en) * 2020-11-10 2021-02-02 安徽扬子美家新材料科技有限公司 Wallboard surface paving material and preparation method thereof
CN112812371A (en) * 2021-01-05 2021-05-18 湘潭大学 Nitrogen-phosphorus-containing hydrotalcite-based flame retardant and preparation method thereof
CN113150382A (en) * 2021-03-03 2021-07-23 中国安全生产科学研究院 Modified melamine phytate flame retardant and preparation method and application thereof
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CN115232359A (en) * 2022-08-19 2022-10-25 南京工程学院 Nitrogen-phosphorus multi-element synergistic flame retardant and preparation method thereof
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CN116120640B (en) * 2023-01-10 2024-03-22 东北林业大学 Expansion type nano composite flame retardant, preparation method thereof and application thereof in wood-plastic composite material

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