CN107434878B - High glow wire, boiling-resistant and flame-retardant polypropylene composite material and preparation method thereof - Google Patents

High glow wire, boiling-resistant and flame-retardant polypropylene composite material and preparation method thereof Download PDF

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CN107434878B
CN107434878B CN201710709168.3A CN201710709168A CN107434878B CN 107434878 B CN107434878 B CN 107434878B CN 201710709168 A CN201710709168 A CN 201710709168A CN 107434878 B CN107434878 B CN 107434878B
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flame
boiling
resistant
retardant
wire
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CN107434878A (en
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吕志勇
邢纪普
任东方
李荣群
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Orinko Advanced Plastics Co Ltd
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Orinko Advanced Plastics Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L23/00Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/02Compositions 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
    • C08L23/10Homopolymers or copolymers of propene
    • C08L23/12Polypropene
    • 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
    • C08K3/32Phosphorus-containing compounds
    • C08K2003/321Phosphates
    • C08K2003/322Ammonium phosphate
    • C08K2003/323Ammonium polyphosphate
    • CCHEMISTRY; METALLURGY
    • 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
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

Abstract

The invention provides a high glow wire and boiling-resistant flame-retardant polypropylene composite material and a preparation method thereof, wherein the high glow wire and boiling-resistant flame-retardant polypropylene composite material consists of 72-76 parts of PP resin, 24-28 parts of nitrogen-phosphorus intumescent flame retardant, 0.1-0.2 part of anti-dripping agent, 0.2-0.3 part of antioxidant, 0.4-0.6 part of lubricant and 0.1-0.2 part of high-efficiency synergist.

Description

High glow wire, boiling-resistant and flame-retardant polypropylene composite material and preparation method thereof
Technical Field
The invention relates to the technical field of high polymers, and particularly relates to a high glow wire, boiling-resistant and flame-retardant polypropylene composite material and a preparation method thereof.
Background
The polypropylene has rich raw material sources, low price, easy processing and forming and excellent comprehensive performance of products, is widely applied to industries such as automobiles, household appliances, electronic appliances and the like, and becomes the fastest-developing variety in general resin. However, polypropylene is a flammable material, the oxygen index of the polypropylene is only 17.4-18.5%, the char formation rate is low, molten drops are generated during combustion, and flame is easily spread to cause fire. With the rapid development of social economy, the application of polypropylene is deepened more and more, and the flame-retardant polypropylene is developed greatly, particularly in the fields of electricians, electronics, low-voltage electrical appliances and the like, the flame-retardant polypropylene is not limited to the flame-retardant grade per se, but has stricter and more rigorous requirements, so as to prevent surrounding parts, especially high-power electrical appliances such as: the safety performance of extension socket, fan heater and the like is the most concerned problem of people, so the development of high glow wire materials is very important, and the novel flame retardant in the 21 st century is a multifunctional composite flame retardant with no halogen, high efficiency, low smoke, low toxicity and low toxicity.
In the long-term use process of the material, the commonly used flame retardant is easy to precipitate in strict environments such as high temperature, high humidity and the like, the precipitation of the flame retardant not only influences the normal work of electrical components, but also significantly reduces or even loses the flame retardant property and glow wire ignition temperature of the material. Therefore, for the flame-retardant polypropylene electrical appliance components applied to special high-end environments, the more special the environments are, the more strict the requirements are, and the requirements on the performances of the flame-retardant polypropylene, such as high glow wire, precipitation resistance and the like, are also higher.
Disclosure of Invention
The invention discloses a high glow wire, boiling-resistant and flame-retardant polypropylene composite material and a preparation method thereof, aiming at overcoming the problems that the ignition temperature of a common flame-retardant polypropylene glow wire is low, precipitation is easy to occur in a specific environment and the like.
The high glow wire and boiling-resistant flame-retardant polypropylene composite material prepared by the method improves the flame-retardant and char-forming efficiency by using the self-prepared intumescent flame retardant, and on the one hand, can obtain the high glow wire grade (875 ℃ and GWIT) and on the other hand effectively solves the serious problem of precipitation of the flame retardant in the using process.
The technical scheme of the invention is as follows: a high glow wire, boiling-resistant and flame-retardant polypropylene composite material comprises the following raw materials in parts by weight:
further, the polypropylene is at least one of isotactic polypropylene, syndiotactic polypropylene and atactic polypropylene.
Further, the flame retardant is a nitrogen-phosphorus intumescent flame retardant, and is prepared from ammonium polyphosphate (APP): the triazine charring agent is compounded according to the mass ratio of 5: 1.
Further, the antioxidant is at least one of hindered phenol, thioester and phosphite antioxidants.
Further, the hindered phenol is pentaerythritol tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], the thioester is distearyl thiodipropionate, and the phosphite is tris (2, 4-di-tert-butylphenyl) phosphite.
Further, the lubricant is selected from at least one of polyethylene wax, stearate, ethylene bis stearamide and grafted ethylene bis stearamide.
Further, the anti-dripping agent is pure powder type 100% PTFE.
Further, the high-efficiency synergist is octaphenyl cage type polysilsesquioxane.
The flame retardant is self-compounded and is prepared according to the following formula: the triazine charring agent is compounded by 5:1, and is not sold in the market at present.
The invention also aims to provide a preparation method of the high glow-wire, boiling-resistant and flame-retardant polypropylene composite material, which comprises the following steps:
(1) weighing the polypropylene, the flame retardant, the anti-dripping agent, the antioxidant, the lubricant and the high-efficiency synergist according to the proportion, adding the weighed materials into a mixer filled with inert gas for high-speed mixing for 2-10 minutes;
(2) and (2) under the protection of inert gas, putting the mixed material prepared in the step (1) into a parallel double-screw extruder for melting, and granulating to obtain the high glow-wire, boiling-resistant and flame-retardant polypropylene composite material.
Preferably, the barrel temperature of the extruder is 180-110 ℃, the screw rotation speed is 400-500r/min, and the vacuum degree is-0.04 to-0.1 MPa.
Compared with the prior art, the high glow wire, boiling-resistant and flame-retardant polypropylene composite material has the following beneficial effects:
1. the flame retardant has high flame retardant efficiency, the halogen-free flame retardant is prepared by compounding ammonium polyphosphate and triazine charring agent, and has the characteristics of high charring rate, rapid expansion and the like, on one hand, ammonia and water vapor generated by the decomposition of ammonium polyphosphate under heating can dilute the concentration of combustible gas, on the other hand, the phosphorus oxygen free radical generated by the decomposition of ammonium polyphosphate can block chain type combustion reaction, so that the combustion heat release can be reduced, and the material can easily meet the requirement of U L-1.6 mm V0.
2. High glow wire: the flame-retardant system adopted by the invention can promote expansion into carbon at the instant of contact of a glow wire at 850 ℃, the generated gas can quickly dilute the surrounding oxygen concentration, and meanwhile, the expanded carbon layer can timely cover the vicinity of a contact point, thereby achieving the purpose of preventing contact fire.
3. Resisting thermo-oxidative aging and discoloration: the material is characterized by most obvious aging, and the halogen-free flame retardant compounded by the ammonium polyphosphate and the triazine charring agent has extremely strong heat resistance, so that the material can still keep excellent thermal stability under continuous high-temperature thermal-oxidative aging without influencing the flame retardant property of the material.
4. Precipitation resistance: PP is a semi-crystalline substance and has a lower glass transition temperature, and when the ambient temperature is higher than the glass transition temperature, the thermal motion of an amorphous chain segment is accelerated along with the increase of the temperature, so that the micromolecule flame retardant with poor compatibility with PP resin can easily overcome resistance and migrate to the surface. The triazine charring agent has the advantages that strong polar group amino is introduced, so that the interface effect of the flame retardant and PP is enhanced, and the problem of flame retardant precipitation is effectively reduced in a high-temperature and high-humidity environment.
Drawings
FIG. 1 is a 875 ℃ GWIT glow wire contact ignition test plot for example 3, comparative examples 1 and 2;
FIG. 2 is a graph showing the results of the boiled-out test (100 ℃ C., 4 hours) for example 3 and comparative examples 1 and 2;
FIG. 3 is a graph showing the results before (top) and after (bottom) of the thermal oxidative aging resistance tests (150 ℃, 4d) of example 3 and comparative examples 1 and 2;
wherein, a is example 3, b is comparative example 1, and c is comparative example 2.
Detailed Description
The invention will now be further described with reference to the following examples, which are intended to illustrate, but not limit the invention.
Example 1:
the high glow wire, boiling-resistant and flame-retardant polypropylene composite material in the embodiment is prepared from the following raw materials in parts by weight:
the preparation method comprises the following steps:
(1) adding 72 parts of isotactic polypropylene, 28 parts of self-prepared intumescent halogen-free flame retardant (23.3 parts of ammonium polyphosphate and 4.7 parts of triazine charring agent), 0.1 part of PTFE anti-dripping agent, 0.1 part of hindered phenol antioxidant, 0.1 part of phosphite antioxidant, 0.2 part of PE wax, 0.2 part of bright lubricant and 0.1 part of octaphenyl cage polysilsesquioxane into a mixer with nitrogen protection, and mixing at high speed for 10 minutes;
(2) under the protection of nitrogen, putting the mixed material obtained in the step (1) into a parallel double-screw extruder for melting, and extruding and granulating to obtain the reinforced polypropylene composite material; wherein the temperature of each cylinder of the extruder is 180-110 ℃, the rotating speed of the screw is 450r/min, and the vacuum degree is-0.04 MPa, thus obtaining the high glow-wire, boiling-resistant and flame-retardant polypropylene composite material.
Example 2:
the high glow wire, boiling-resistant and flame-retardant polypropylene composite material in the embodiment is prepared from the following raw materials in parts by weight:
the preparation method comprises the following steps:
(1) adding 50 parts of isotactic polypropylene, 25 parts of random copolymerization polypropylene, 25 parts of self-prepared intumescent halogen-free flame retardant (20.8 parts of ammonium polyphosphate and 4.2 parts of triazine charring agent), 0.15 part of PTFE anti-dripping agent, 0.15 part of hindered phenol antioxidant, 0.1 part of phosphite antioxidant, 0.25 part of PE wax, 0.25 part of bright lubricant and 0.15 part of octaphenyl cage polysilsesquioxane into a mixer with nitrogen protection for high-speed mixing for 10 minutes;
(2) under the protection of nitrogen, putting the mixed material obtained in the step (1) into a parallel double-screw extruder for melting, and extruding and granulating to obtain the reinforced polypropylene composite material; wherein the temperature of a machine barrel of the extruder is 180-.
Example 3:
the high glow wire and boiling-resistant flame-retardant polypropylene composite material in the embodiment is prepared from the following raw materials in parts by weight: the triazine charring agent is compounded according to the mass ratio of 5: 1:
the preparation method comprises the following steps:
(1) adding 20 parts of ammonium polyphosphate and 4 parts of triazine charring agent into a high-speed stirring machine, and stirring at a high speed for 5 min.
(2) Adding the 24 parts of the compound, 76 parts of isotactic polypropylene, 0.2 part of PTFE anti-dripping agent, 0.15 part of hindered phenol antioxidant, 0.15 part of phosphite antioxidant, 0.3 part of PE wax, 0.3 part of bright lubricant and 0.2 part of octaphenyl cage polysilsesquioxane into a mixer which is communicated with nitrogen for high-speed mixing for 10 minutes;
(3) under the protection of nitrogen, putting the mixed material obtained in the step (2) into a parallel double-screw extruder for melting, and performing extrusion and granulation to obtain the reinforced polypropylene composite material; wherein the temperature of a machine barrel of the extruder is 180-.
Comparative example 1:
the polypropylene composite material in the comparative example is prepared from the following raw materials in parts by weight, wherein the raw materials comprise ammonium polyphosphate (APP): the triazine charring agent is compounded according to the mass ratio of 4: 1:
the preparation method comprises the following steps:
(1) adding 11.2 parts of ammonium polyphosphate and 4.8 parts of triazine charring agent into a high-speed stirrer, and stirring at a high speed for 5 min.
(2) Adding the 24 parts of the compound, 76 parts of isotactic polypropylene, 0.2 part of PTFE anti-dripping agent, 0.15 part of hindered phenol antioxidant, 0.15 part of phosphite antioxidant, 0.3 part of PE wax, 0.3 part of bright lubricant and 0.2 part of octaphenyl cage polysilsesquioxane into a mixer which is communicated with nitrogen for high-speed mixing for 10 minutes;
(3) under the protection of nitrogen, putting the mixed material obtained in the step (2) into a parallel double-screw extruder for melting, and performing extrusion and granulation to obtain the reinforced polypropylene composite material; wherein the temperature of a machine barrel of the extruder is 180-.
Comparative example 2:
the polypropylene composite material in the comparative example is prepared from the following raw materials in parts by weight, wherein the raw materials comprise ammonium polyphosphate (APP): the triazine charring agent is compounded according to the mass ratio of 6: 1:
the preparation method comprises the following steps:
(1) adding 20.5 parts of ammonium polyphosphate and 3.5 parts of triazine charring agent into a high-speed stirrer, and stirring at a high speed for 5 min.
(2) Adding the 24 parts of the compound, 76 parts of isotactic polypropylene, 0.2 part of PTFE anti-dripping agent, 0.15 part of hindered phenol antioxidant, 0.15 part of phosphite antioxidant, 0.3 part of PE wax, 0.3 part of bright lubricant and 0.2 part of octaphenyl cage polysilsesquioxane into a mixer which is communicated with nitrogen for high-speed mixing for 10 minutes;
(3) under the protection of nitrogen, putting the mixed material obtained in the step (2) into a parallel double-screw extruder for melting, and performing extrusion and granulation to obtain the reinforced polypropylene composite material; wherein the temperature of a machine barrel of the extruder is 180-.
The high glow wire, boiling-resistant flame-retardant polypropylene composite material and the common halogen-free flame-retardant polypropylene prepared in the above examples 1 to 3 were tested for tensile strength, elongation at break, bending strength, bending modulus, notched izod impact strength, flame-retardant property, glow wire, boiling-resistant property, and thermal oxidation aging discoloration resistance according to the relevant test standards, which are shown in the following table 1:
table 1: main physical property indexes of the high glow wire, boiling-resistant and flame-retardant polypropylene composite material and the common halogen-free flame-retardant polypropylene of the embodiments 1 to 3
It can be seen from table 1 that the high glow wire, boiling resistant and flame retardant polypropylene composite material prepared by the invention uses the polypropylene copolymer as the base material, and the rigidity and toughness of the prepared composite material are well balanced through reactive extrusion under the protection of nitrogen, and the composite material fully exerts the high glow wire, boiling resistant, low precipitation, thermal oxidation aging resistant and discoloration resistant properties of the compound flame retardant while ensuring the mechanical strength, can replace the existing halogen-free flame retardant material, and meets the requirements of the halogen-free flame retardant polypropylene for the modern electronic and electric appliances under the environments of high temperature, high humidity and the like.
The high glow wire and boiling-resistant flame-retardant polypropylene composite material prepared in the embodiment 3 and the comparative examples 1-2 are tested for glow wire, boiling-resistant performance and thermal-oxidative aging-resistant discoloration performance according to related test standards, and the test results are shown in figures 1-3:
as can be seen from fig. 1, in the case of ammonium polyphosphate (APP): when the triazine charring agent is compounded in a mass ratio of 5:1, the glow wire can be completely nonflammable at 875 ℃ and GWIT contact, and no open fire is generated after the glow wire leaves. It can be seen from fig. 2 that in ammonium polyphosphate (APP): when the triazine charring agent is compounded according to the mass ratio of 5:1, the boiling precipitation resistance of the material is obviously better than that of the formula according to the mass ratio of 4:1 and 6:1 (both have different precipitation degrees). It can be seen from fig. 3 that in ammonium polyphosphate (APP): when the triazine charring agent is compounded according to the mass ratio of 5:1, the material has the most excellent thermal oxidation aging resistance and discoloration resistance, and the color difference change is obviously lower than that of the formulas with the mass ratios of 4:1 and 6:1 (both have obvious yellowing phenomenon).
From fig. 1-3, it can be seen that the high glow-wire, boiling-resistant and flame-retardant polypropylene composite material prepared by the invention is prepared by mixing the following components in parts by weight of ammonium polyphosphate (APP): when the triazine charring agent is compounded in a mass ratio of 5:1, the glow wire, the boiling resistance and the anti-thermal-oxidative aging discoloration resistance of the material are all optimal, and the mechanical property of the material can be ensured not to be affected.
If functional additives such as ultraviolet light absorbers, light stabilizers, antistatic agents, coloring agents and the like are added into the preparation components, the composite material has corresponding characteristics and is also protected by the invention.
The embodiments described above are intended to facilitate one of ordinary skill in the art in understanding and using the present invention. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the embodiments described herein, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.

Claims (8)

1. A high glow wire, boiling-resistant and flame-retardant polypropylene composite material is characterized in that: the composition comprises the following raw materials in parts by weight:
the flame retardant is a nitrogen-phosphorus intumescent flame retardant, and is prepared by mixing the following components in percentage by weight: compounding triazine charring agents according to the mass ratio of 5: 1;
the high-efficiency synergist is octaphenyl cage type polysilsesquioxane.
2. The high glow-wire, boiling-resistant, flame-retardant polypropylene composite of claim 1, wherein: the polypropylene is at least one of isotactic polypropylene, syndiotactic polypropylene and atactic polypropylene.
3. The high glow-wire, boiling-resistant, flame-retardant polypropylene composite of claim 1, wherein: the antioxidant is at least one of hindered phenol, thioester and phosphite antioxidant.
4. The high glow-wire, boiling-resistant and flame-retardant polypropylene composite material according to claim 3, wherein the hindered phenol antioxidant is pentaerythritol tetrakis [ β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ], the thioester antioxidant is distearyl thiodipropionate, and the phosphite antioxidant is tris (2, 4-di-tert-butylphenyl) phosphite.
5. The high glow-wire, boiling-resistant, flame-retardant polypropylene composite of claim 1, wherein: the lubricant is selected from at least one of polyethylene wax, stearate and ethylene bis-stearamide.
6. The high glow-wire, boiling-resistant, flame-retardant polypropylene composite of claim 1, wherein: the anti-dripping agent is pure powder type 100% PTFE anti-dripping agent.
7. A method of making the high glow-wire, boiling-resistant, flame-retardant polypropylene composite of claim 1, wherein: the method comprises the following steps:
(1) weighing the polypropylene, the flame retardant, the anti-dripping agent, the antioxidant, the lubricant and the high-efficiency synergist according to the proportion, adding the weighed materials into a mixer filled with inert gas for high-speed mixing for 2-10 minutes;
(2) and (2) under the protection of inert gas, putting the mixed material obtained in the step (1) into a parallel double-screw extruder for melting, and granulating to obtain the high glow-wire, boiling-resistant and flame-retardant polypropylene composite material.
8. The preparation method of the high glow-wire, boiling-resistant and flame-retardant polypropylene composite material according to claim 7, wherein the preparation method comprises the following steps: the temperature of the cylinder of the extruder in the step (2) is 190 ℃, the rotating speed of the screw is 400-500r/min, and the vacuum degree is-0.04 to-0.1 MPa.
CN201710709168.3A 2017-08-17 2017-08-17 High glow wire, boiling-resistant and flame-retardant polypropylene composite material and preparation method thereof Active CN107434878B (en)

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CN109233126A (en) * 2018-07-05 2019-01-18 何亚龙 A kind of flame-retardant expanded plate of polystyrene and preparation method
CN109705462B (en) * 2018-12-25 2021-08-24 广东聚石化学股份有限公司 V0-grade halogen-free flame-retardant polypropylene material special for extrusion and plastic uptake and preparation method thereof
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CN110372956B (en) * 2019-07-09 2022-05-13 广东奇德新材料股份有限公司 Halogen-free flame-retardant polypropylene composite with high glow wire
CN111057316B (en) * 2019-12-23 2022-03-29 清远市普塞呋磷化学有限公司 Non-sticking ammonium polyphosphate flame-retardant modified polypropylene material and preparation method thereof
CN112321945A (en) * 2020-11-23 2021-02-05 江苏金发科技新材料有限公司 Precipitation-resistant halogen-free flame-retardant polypropylene composite material and preparation method thereof
CN112590051A (en) * 2020-12-27 2021-04-02 南京天诗新材料科技有限公司 Production method and device of polypropylene anti-dripping master batch
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