CN112341702A - Efficient smoke-suppression halogen-free flame-retardant polypropylene composite material and preparation method thereof - Google Patents
Efficient smoke-suppression halogen-free flame-retardant polypropylene composite material and preparation method thereof Download PDFInfo
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- 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
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Abstract
The invention discloses a halogen-free flame-retardant polypropylene composite material with efficient flame-retardant and smoke-suppression functions and a preparation method thereof. The material consists of the following components: 100 parts of polypropylene, 1-6 parts of silicon compatilizer, 15-30 parts of ammonium polyphosphate, 3-15 parts of pentaerythritol, 0.01-1 part of antioxidant and 1-20 parts of sodium oleate modified dodecyl sulfate radical calcium magnesium aluminum hydrotalcite. The polypropylene composite material has good flame retardant effect, does not contain harmful substances such as lead, mercury, cadmium, hexavalent chromium, polybrominated biphenyls and the like, has low smoke generation amount in the combustion process, has little harm to the environment and human bodies, and has good mechanical property.
Description
The technical field is as follows:
the invention relates to a polymer composite material with a novel flame-retardant function and a preparation method thereof, belonging to the technical field of polymer composite materials. In particular to a high-efficiency smoke-suppression halogen-free flame-retardant polypropylene composite material and a preparation method thereof.
Background art:
polypropylene (PP) has advantages of wide source, economical price, easy molding and processing, etc., and is widely used in the fields of household appliances, vehicle engineering, electronic equipment, etc. But the molecular chain only contains carbon and hydrogen, so the flame is easy to burn. The limit oxygen index of pure PP is only about 17 percent, and PP is non-char forming high polymer, almost all long chains are cracked into combustible gas during combustion, and no carbon residue is left. Generally, halogen-containing flame retardants have the characteristics of low cost, high flame retardant efficiency, good compatibility and the like, and have a large market in the current PP flame retardation. However, the halogen-containing flame-retardant PP material generates toxic gas when being burnt, pollutes the environment and causes secondary damage to human bodies, and is prohibited to be used in many fields. The halogen-free flame retardant has the characteristics of low smoke release, no corrosive gas generation and low toxicity, has attracted extensive attention of researchers, and becomes a hotspot of polymer flame retardant research.
The intumescent flame retardant material has certain defects, which are mainly reflected in the following points: when the IFR is used alone, the flame retardant efficiency is not high, so that the mechanical property of the system is reduced to a certain degree. The IFR has a large polarity difference with the polymer, so that the electrical property of the composite material is reduced. The ammonium polyphosphate and the polyhydric alcohol are easy to absorb moisture, and the water resistance of the system is poor; at the same time, IFR is easy to migrate to the surface of the polymer, and the appearance and physical properties of the system are weakened. Therefore, the introduction of the nano particles, the synergistic effect of the nano particles in an IFR system and the nano effect of the nano particles can improve the flame retardant property and obtain a composite material with excellent other properties. The intumescent flame retardant and the inorganic hydroxide are the most commonly used halogen-free flame retardant for PP, and a lot of flame retardants are available in the past years, for example, CN201210410894.2 discloses a composite environment-friendly flame retardant for polypropylene and a polypropylene flame-retardant plastic, and the flame-retardant modification of PP is realized mainly by compounding trimethylsilyl dimethyl methyl phosphate, melamine cyanurate and hydroxide; CN201310236034.6 discloses a high-efficiency halogen-free intumescent flame retardant polypropylene material, which is mainly characterized in that the flame retardant efficiency of an intumescent flame retardant to PP is improved through a char-forming catalyst; CN201310222303.3, CN201310121879.0 and the like all mention that an intumescent flame retardant and a hydroxide compound are used as flame retardants or are compounded to improve the flame retardant property of PP.
Hydrotalcite is an anionic layered inorganic functional material, also called Layered Double Hydroxides (LDHs), whose layered metal cations and interlayer anions can be adjusted within a certain range, and is widely used in catalysts, adsorbents, heat stabilizers, flame retardants, and the like. When used as a flame retardant, LDHs have not only high flame retardant efficiency, but also non-toxic, halogen-free and smoke-suppressing effects, compared with conventional inorganic flame retardants and halogenated flame retardants, and are also known as a new-generation environment-friendly flame retardant. The interlayer water, the bonding water and the laminate hydroxyl of the LDHs are dehydrated in the heating process to absorb heat and reduce the temperature, and H generated at the same time2O can dilute the flammable gas. The well-dispersed hydrotalcite can form an intercalation or stripping well-dispersed structure in the polymer, volatile products generated by decomposition at high temperature are not easy to diffuse, and the outside O is isolated2. The hydrotalcite laminate can absorb heat in the decomposition process of the metal hydroxide, and the temperature of the system is reduced. Ions intercalated into hydrotalcite layers can enable the material to show better flame retardant performance due to certain special properties of the ions, such as dehydration and charring property of phosphorus-containing groups and dispersibility promotion of organic groups. However, the LDHs type flame retardant generally has the defects of large addition amount and deterioration of the mechanical property of a polymer matrix, which greatly limits the popularization and the application of the type of flame retardant. Therefore, before being used as a flame retardant, LDHs are subjected to surface modification or other flame retardantsThe combustion system is formulated to be necessary.
The calcium magnesium aluminum hydrotalcite modified by sodium oleate is compounded with the intumescent flame retardant system, so that the calcium magnesium aluminum hydrotalcite has good flame retardant synergistic effect, is beneficial to catalytic carbonization of the system and smoke suppression, and effectively improves the flame retardant property of the PP composite material.
The invention content is as follows:
the invention aims to provide a halogen-free flame-retardant polypropylene composite material with efficient flame-retardant and smoke-suppression functions and a preparation method thereof. The adopted flame retardant does not contain halogen, and completely meets the requirements of low smoke and zero halogen.
The technical scheme adopted by the invention for realizing the purpose is as follows:
a halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppression functions is prepared from the following components in parts by weight:
100 parts of polypropylene, 1-6 parts of silicon compatilizer, 15-30 parts of ammonium polyphosphate, 3-15 parts of pentaerythritol, 0.01-1 part of antioxidant and 1-20 parts of sodium oleate modified dodecyl sulfate radical calcium magnesium aluminum hydrotalcite.
The silicon-containing compatilizer is a compound with a macromolecular structure and a silane side chain, and the molecular weight of the compound is 2000 g/mol-10000 g/mol.
The antioxidant is prepared by compounding beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl ester and tris [2, 4-di-tert-butylphenyl ] phosphite in a ratio of 1: 1.
The polypropylene is one or a mixture of homo-polypropylene or co-polypropylene.
The preparation method of the sodium oleate modified dodecyl sulfate radical calcium magnesium aluminum hydrotalcite comprises the following steps:
(1) taking Ca (NO) by coprecipitation method3)2·4H2O、Mg(NO3)2·6H2O and Al (NO)3)3·9H2Dissolving O in the carbon dioxide-removed water, marking as solution A, dissolving 0.5-2 mol of NaOH in the carbon dioxide-removed water, marking as solution B, respectively dripping the solution A, B into the flask,stirring at normal temperature, keeping the pH value between 9 and 11, continuing stirring for 1 to 5 hours after the dropwise addition is finished, crystallizing for 13 to 24 hours at the temperature of between 60 and 85 ℃, performing suction filtration, washing with carbon dioxide to be neutral, drying at the temperature of between 60 and 85 ℃, grinding, and sieving with a 60 to 80-mesh sieve (177 to 250 mu m), wherein the sieve is marked as CaMgAl-LDHs.
(2) Dissolving 15g of CaMgAl-LDHs and 16.2g of Sodium Dodecyl Sulfate (SDS) in carbon dioxide-removed water by adopting an ion exchange method, stirring for 13-24 h at normal temperature, carrying out suction filtration, washing to be neutral by using carbon dioxide, drying at 60-85 ℃, grinding, and sieving by using a 60-80-mesh sieve (177-250 mu m) to obtain SDS-LDHs.
(3) Dissolving 10g of SDS-LDHs in carbon dioxide-removed water, stirring at normal temperature, adding 0.2-1.2 g/L of sodium oleate, reacting for 13-24 h, performing suction filtration, drying, and sieving with a 60-80-mesh sieve (177-250 mu m) to obtain the sodium oleate modified dodecyl sulfate radical calcium magnesium aluminum hydrotalcite.
Wherein said Ca (NO)3)2·4H2O、Mg(NO3)2·6H2O and Al (NO)3)3·9H2The molar ratio of O is 1-3: 2-3: 1-2.
The preparation method of the halogen-free flame-retardant polypropylene composite material with the efficient flame-retardant and smoke-suppression functions comprises the following steps:
before ammonium polyphosphate, pentaerythritol, an antioxidant, polypropylene and sodium oleate modified dodecyl sulfate radical type calcium magnesium aluminum hydrotalcite are used, the dodecyl sulfate radical type calcium magnesium aluminum hydrotalcite is placed in an oven at the temperature of 60-80 ℃ for drying for 8-24 hours, and then the dodecyl sulfate radical type calcium magnesium aluminum hydrotalcite is weighed according to a research formula. Firstly, adding polypropylene into a torque rheometer (the set temperature and the set rotating speed are 160-190 ℃ and 50-80 r/min respectively) for heating and melting for 2-5 min, then adding a premixed flame retardant, and banburying for 12-15 min. And (3) placing the banburying sample into a mold with a test size specification, placing the banburying sample into a flat vulcanizing machine with a set temperature of 160-190 ℃ for preheating for 2-5 min, maintaining the pressure for 2-5 min, and naturally cooling to room temperature to obtain the halogen-free flame-retardant polypropylene composite material with the efficient flame-retardant and smoke-suppression functions required by analysis and test.
The invention has the following beneficial effects:
(1) the flame-retardant polypropylene composite material compounded by the hydrotalcite and the intumescent flame retardant adopts a halogen-free nontoxic composite flame-retardant system, does not contain harmful substances such as lead, mercury, hexavalent chromium and the like, does not release toxic and harmful gases in the combustion process, and has good environmental effect.
(2) The hydrotalcite can release a large amount of moisture on the surface and among layers in the temperature rising process of the material, plays a role in diluting combustible gas in a polypropylene thermal degradation product, delays the combustion process of the material, and can be matched with an intumescent flame retardant to retard the flame of the polypropylene material in the early combustion stage.
(3) The hydrotalcite of the present invention can be converted from lamellar crystals into metal oxides at high temperature, and these metal oxides can absorb part of the heat to limit the thermal degradation of polypropylene, thus having a unique effect of improving the thermal stability of polypropylene.
(4) The hydrotalcite provided by the invention has a large specific surface area, can block heat transfer in the combustion process of polypropylene, can assist the intumescent flame retardant to form a compact carbon layer, and can also play a good role in adsorbing smoke, so that the heating smoke generation amount in the combustion process is low, and the harm to the environment and human body is small.
(5) The hydrotalcite is dodecyl sulfate radical type hydrotalcite prepared by a coprecipitation method, and after the dodecyl sulfate radical type hydrotalcite is modified and compounded, the interlayer spacing of the hydrotalcite is enlarged, the dispersion of the hydrotalcite in a PP (polypropylene) matrix material is facilitated, and the flame retardant property of the material is further improved.
Description of the drawings:
in order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 is a schematic diagram of the flame retarding mechanism of intumescent flame retardants.
The specific implementation mode is as follows:
the present invention will be further described with reference to the following examples. It is to be understood that the following examples are illustrative only and are not intended to limit the scope of the invention, which is to be given numerous insubstantial modifications and adaptations by those skilled in the art based on the teachings set forth above.
The invention relates to a sodium oleate modified dodecyl sulfate calcium magnesium aluminum hydrotalcite, which is a flame retardant modified calcium magnesium aluminum hydroxide, and the preparation method comprises the following steps: 0.06mol of Ca (NO) is taken3)2·4H2O、0.06mol Mg(NO3)2·6H2O and 0.03mol Al (NO)3)3·9H2Dissolving O in carbon dioxide-removed water, marking as a solution A, dissolving 1mol of NaOH in the carbon dioxide-removed water, marking as a solution B, respectively dropwise adding the solution A, B into a flask, stirring at normal temperature, keeping the pH value between 11, continuously stirring for 5h after dropwise adding is finished, crystallizing at 85 ℃ for 24h, performing suction filtration, washing to be neutral by using carbon dioxide water, drying at 60-85 ℃, grinding, sieving by using a 60-80-mesh sieve (177-250 mu m), and marking as CaMgAl-LDHs.
Dissolving 15g of CaMgAl-LDHs and 16.2g of Sodium Dodecyl Sulfate (SDS) in decarbonated water, stirring for 24 hours at normal temperature, carrying out suction filtration, washing to be neutral by the decarbonated water, drying at 85 ℃, grinding, and sieving by a 60-80-mesh sieve (177-250 mu m) to obtain SDS-LDHs. Dissolving 10g of SDS-LDHs in carbon dioxide-removed water, stirring at normal temperature, adding 1.2g/L of sodium oleate, reacting for 24 hours, filtering, drying, and sieving with a 60-80 mesh sieve (177-250 mu m) to obtain sodium oleate modified dodecyl sulfate radical type calcium magnesium aluminum hydrotalcite, which is marked as O1-CaMgAl-SDS-LDHs。
The invention relates to a sodium oleate modified dodecyl sulfate calcium magnesium aluminum hydrotalcite, which is a flame retardant modified calcium magnesium aluminum hydroxide, and the preparation method comprises the following steps: 0.02mol of Ca (NO) is taken3)2·4H2O、0.06molMg(NO3)2·6H2O and 0.04mol Al (NO)3)3·9H2Dissolving O in carbon dioxide-removed water, marking as a solution A, dissolving 1mol of NaOH in the carbon dioxide-removed water, marking as a solution B, respectively dropwise adding the solution A, B into a flask, stirring at normal temperature, keeping the pH value between 11, continuously stirring for 5h after dropwise adding is finished, crystallizing at 85 ℃ for 24h, performing suction filtration, washing to be neutral by using carbon dioxide water, drying at 60-85 ℃, grinding, sieving by using a 60-80-mesh sieve (177-250 mu m), and marking as CaMgAl-LDHs.
Dissolving 15g of CaMgAl-LDHs and 16.2g of Sodium Dodecyl Sulfate (SDS) in decarbonated water, stirring for 24 hours at normal temperature, carrying out suction filtration, washing to be neutral by the decarbonated water, drying at 85 ℃, grinding, and sieving by a 60-80-mesh sieve (177-250 mu m) to obtain SDS-LDHs. Dissolving 10g of SDS-LDHs in carbon dioxide-removed water, stirring at normal temperature, adding 1.2g/L of sodium oleate, reacting for 24 hours, filtering, drying, and sieving with a 60-80 mesh sieve (177-250 mu m) to obtain sodium oleate modified dodecyl sulfate radical type calcium magnesium aluminum hydrotalcite, which is marked as O2-CaMgAl-SDS-LDHs。
The invention relates to a sodium oleate modified dodecyl sulfate calcium magnesium aluminum hydrotalcite, which is a flame retardant modified calcium magnesium aluminum hydroxide, and the preparation method comprises the following steps: 0.06mol of Ca (NO) is taken3)2·4H2O、0.06mol Mg(NO3)2·6H2O and 0.04mol Al (NO)3)3·9H2Dissolving O in carbon dioxide-removed water, marking as a solution A, dissolving 1mol of NaOH in the carbon dioxide-removed water, marking as a solution B, respectively dropwise adding the solution A, B into a flask, stirring at normal temperature, keeping the pH value between 11, continuously stirring for 5h after dropwise adding is finished, crystallizing at 85 ℃ for 24h, performing suction filtration, washing to be neutral by using carbon dioxide water, drying at 60-85 ℃, grinding, sieving by using a 60-80-mesh sieve (177-250 mu m), and marking as CaMgAl-LDHs.
Dissolving 15g of CaMgAl-LDHs and 16.2g of Sodium Dodecyl Sulfate (SDS) in decarbonated water, stirring for 24 hours at normal temperature, carrying out suction filtration, washing to be neutral by the decarbonated water, drying at 85 ℃, grinding, and sieving by a 60-80-mesh sieve (177-250 mu m) to obtain SDS-LDHs. Dissolving 10g of SDS-LDHs in carbon dioxide-removed water, stirring at normal temperature, adding 1.2g/L of sodium oleate, reacting for 24 hours, filtering, drying, and sieving with a 60-80 mesh sieve (177-250 mu m) to obtain sodium oleate modified dodecyl sulfate radical type calcium magnesium aluminum hydrotalcite, which is marked as O3-CaMgAl-SDS-LDHs。
The invention discloses a halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppressing functions and a preparation method thereof, wherein the composition is as follows: 100 parts of polypropylene, 1-6 parts of silicon compatilizer, 15-30 parts of ammonium polyphosphate, 3-15 parts of pentaerythritol, 0.01-1 part of antioxidant and 1-20 parts of sodium oleate modified dodecyl sulfate radical calcium magnesium aluminum hydrotalcite.
Example 1
A halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppression functions comprises the following components:
100 parts by mass of polypropylene
Silicon-containing compatibilizer 1 part by mass
Ammonium polyphosphate 18 parts by mass
Pentaerythritol 6 parts by mass
0.1 part by mass of an antioxidant
O1-CaMgAl-SDS-LDHs 2 parts by mass
A preparation method of a halogen-free flame-retardant polypropylene composite material with efficient flame-retardant and smoke-suppression functions comprises the following steps:
mixing ammonium polyphosphate, antioxidant, polypropylene and O1Before use, the-CaMgAl-SDS-LDHs is placed in an oven at 80 ℃ for drying for 24 hours and then weighed according to the research formula. Firstly, polypropylene is added into a torque rheometer (the set temperature and the set rotating speed are respectively 180 ℃ and 50r/min) to be heated and melted for 3min, and then premixed flame retardant is added to be banburied for 12 min. And (3) placing the banburying sample into a mold with a test size specification, placing the banburying sample into a flat vulcanizing machine with a set temperature of 180 ℃ for preheating for 3min, maintaining the pressure for 5min, and naturally cooling to room temperature to obtain the halogen-free flame-retardant polypropylene composite material with the efficient flame-retardant and smoke-suppression functions required by analysis and test.
Example 2
A halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppression functions comprises the following components:
100 parts by mass of polypropylene
Silicon-containing compatibilizer 1 part by mass
Ammonium polyphosphate 18 parts by mass
Pentaerythritol 6 parts by mass
0.1 part by mass of an antioxidant
O1-CaMgAl-SDS-LDHs 3 parts by mass
A preparation method of a halogen-free flame-retardant polypropylene composite material with efficient flame-retardant and smoke-suppression functions comprises the following steps:
mixing ammonium polyphosphate, antioxidant, polypropylene and O1Before use, the-CaMgAl-SDS-LDHs is placed in an oven at 80 ℃ for drying for 24 hours and then weighed according to the research formula. Firstly, polypropylene is added into a torque rheometer (the set temperature and the set rotating speed are respectively 180 ℃ and 50r/min) to be heated and melted for 3min, and then premixed flame retardant is added to be banburied for 12 min. And (3) placing the banburying sample into a mold with a test size specification, placing the banburying sample into a flat vulcanizing machine with a set temperature of 180 ℃ for preheating for 3min, maintaining the pressure for 5min, and naturally cooling to room temperature to obtain the halogen-free flame-retardant polypropylene composite material with the efficient flame-retardant and smoke-suppression functions required by analysis and test.
Example 3
A halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppression functions comprises the following components:
100 parts by mass of polypropylene
Silicon-containing compatibilizer 1 part by mass
Ammonium polyphosphate 18 parts by mass
Pentaerythritol 6 parts by mass
0.1 part by mass of an antioxidant
O1-CaMgAl-SDS-LDHs 4 parts by mass
A preparation method of a halogen-free flame-retardant polypropylene composite material with efficient flame-retardant and smoke-suppression functions comprises the following steps:
mixing ammonium polyphosphate, antioxidant, polypropylene and O1Before use, the-CaMgAl-SDS-LDHs is placed in an oven at 80 ℃ for drying for 24 hours and then weighed according to the research formula. Firstly, polypropylene is added into a torque rheometer (the set temperature and the set rotating speed are respectively 180 ℃ and 50r/min) to be heated and melted for 3min, and then premixed flame retardant is added to be banburied for 12 min. And (3) placing the banburying sample into a mold with a test size specification, placing the banburying sample into a flat vulcanizing machine with a set temperature of 180 ℃ for preheating for 3min, maintaining the pressure for 5min, and naturally cooling to room temperature to obtain the halogen-free flame-retardant polypropylene composite material with the efficient flame-retardant and smoke-suppression functions required by analysis and test.
Example 4
A halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppression functions comprises the following components:
100 parts by mass of polypropylene
Silicon-containing compatibilizer 1 part by mass
Ammonium polyphosphate 18 parts by mass
Pentaerythritol 6 parts by mass
0.1 part by mass of an antioxidant
O15 parts by mass of-CaMgAl-SDS-LDHs
A preparation method of a halogen-free flame-retardant polypropylene composite material with efficient flame-retardant and smoke-suppression functions comprises the following steps:
mixing ammonium polyphosphate, antioxidant, polypropylene and O1Before use, the-CaMgAl-SDS-LDHs is placed in an oven at 80 ℃ for drying for 24 hours and then weighed according to the research formula. Firstly, polypropylene is added into a torque rheometer (the set temperature and the set rotating speed are respectively 180 ℃ and 50r/min) to be heated and melted for 3min, and then premixed flame retardant is added to be banburied for 12 min. And (3) placing the banburying sample into a mold with a test size specification, placing the banburying sample into a flat vulcanizing machine with a set temperature of 180 ℃ for preheating for 3min, maintaining the pressure for 5min, and naturally cooling to room temperature to obtain the halogen-free flame-retardant polypropylene composite material with the efficient flame-retardant and smoke-suppression functions required by analysis and test.
Example 5
A halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppression functions comprises the following components:
100 parts by mass of polypropylene
Silicon-containing compatibilizer 1 part by mass
Ammonium polyphosphate 18 parts by mass
Pentaerythritol 6 parts by mass
0.1 part by mass of an antioxidant
O2-CaMgAl-SDS-LDHs 2 parts by mass
A preparation method of a halogen-free flame-retardant polypropylene composite material with efficient flame-retardant and smoke-suppression functions comprises the following steps:
mixing polyphosphoric acidAmmonium, antioxidant, polypropylene, O2Before use, the-CaMgAl-SDS-LDHs is placed in an oven at 80 ℃ for drying for 24 hours and then weighed according to the research formula. Firstly, polypropylene is added into a torque rheometer (the set temperature and the set rotating speed are respectively 180 ℃ and 50r/min) to be heated and melted for 3min, and then premixed flame retardant is added to be banburied for 12 min. And (3) placing the banburying sample into a mold with a test size specification, placing the banburying sample into a flat vulcanizing machine with a set temperature of 180 ℃ for preheating for 3min, maintaining the pressure for 5min, and naturally cooling to room temperature to obtain the halogen-free flame-retardant polypropylene composite material with the efficient flame-retardant and smoke-suppression functions required by analysis and test.
Example 6
A halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppression functions comprises the following components:
100 parts by mass of polypropylene
Silicon-containing compatibilizer 1 part by mass
Ammonium polyphosphate 18 parts by mass
Pentaerythritol 6 parts by mass
0.1 part by mass of an antioxidant
O2-CaMgAl-SDS-LDHs 3 parts by mass
A preparation method of a halogen-free flame-retardant polypropylene composite material with efficient flame-retardant and smoke-suppression functions comprises the following steps:
mixing ammonium polyphosphate, antioxidant, polypropylene and O2Before use, the-CaMgAl-SDS-LDHs is placed in an oven at 80 ℃ for drying for 24 hours and then weighed according to the research formula. Firstly, polypropylene is added into a torque rheometer (the set temperature and the set rotating speed are respectively 180 ℃ and 50r/min) to be heated and melted for 3min, and then premixed flame retardant is added to be banburied for 12 min. And (3) placing the banburying sample into a mold with a test size specification, placing the banburying sample into a flat vulcanizing machine with a set temperature of 180 ℃ for preheating for 3min, maintaining the pressure for 5min, and naturally cooling to room temperature to obtain the halogen-free flame-retardant polypropylene composite material with the efficient flame-retardant and smoke-suppression functions required by analysis and test.
Example 7
A halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppression functions comprises the following components:
100 parts by mass of polypropylene
Silicon-containing compatibilizer 1 part by mass
Ammonium polyphosphate 18 parts by mass
Pentaerythritol 6 parts by mass
0.1 part by mass of an antioxidant
O2-CaMgAl-SDS-LDHs 4 parts by mass
A preparation method of a halogen-free flame-retardant polypropylene composite material with efficient flame-retardant and smoke-suppression functions comprises the following steps:
mixing ammonium polyphosphate, antioxidant, polypropylene and O2Before use, the-CaMgAl-SDS-LDHs is placed in an oven at 80 ℃ for drying for 24 hours and then weighed according to the research formula. Firstly, polypropylene is added into a torque rheometer (the set temperature and the set rotating speed are respectively 180 ℃ and 50r/min) to be heated and melted for 3min, and then premixed flame retardant is added to be banburied for 12 min. And (3) placing the banburying sample into a mold with a test size specification, placing the banburying sample into a flat vulcanizing machine with a set temperature of 180 ℃ for preheating for 3min, maintaining the pressure for 5min, and naturally cooling to room temperature to obtain the halogen-free flame-retardant polypropylene composite material with the efficient flame-retardant and smoke-suppression functions required by analysis and test.
Example 8
A halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppression functions comprises the following components:
100 parts by mass of polypropylene
Silicon-containing compatibilizer 1 part by mass
Ammonium polyphosphate 18 parts by mass
Pentaerythritol 6 parts by mass
0.1 part by mass of an antioxidant
O25 parts by mass of-CaMgAl-SDS-LDHs
A preparation method of a halogen-free flame-retardant polypropylene composite material with efficient flame-retardant and smoke-suppression functions comprises the following steps:
mixing ammonium polyphosphate, antioxidant, polypropylene and O2Before use, the-CaMgAl-SDS-LDHs is placed in an oven at 80 ℃ for drying for 24 hours and then weighed according to the research formula. Firstly, the methodAdding polypropylene into a torque rheometer (the set temperature and the set rotating speed are 180 ℃ and 50r/min respectively) to heat and melt for 3min, then adding a premixed flame retardant and banburying for 12 min. And (3) placing the banburying sample into a mold with a test size specification, placing the banburying sample into a flat vulcanizing machine with a set temperature of 180 ℃ for preheating for 3min, maintaining the pressure for 5min, and naturally cooling to room temperature to obtain the halogen-free flame-retardant polypropylene composite material with the efficient flame-retardant and smoke-suppression functions required by analysis and test.
Example 9
A halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppression functions comprises the following components:
100 parts by mass of polypropylene
Silicon-containing compatibilizer 1 part by mass
Ammonium polyphosphate 18 parts by mass
Pentaerythritol 6 parts by mass
0.1 part by mass of an antioxidant
O3-CaMgAl-SDS-LDHs 2 parts by mass
A preparation method of a halogen-free flame-retardant polypropylene composite material with efficient flame-retardant and smoke-suppression functions comprises the following steps:
mixing ammonium polyphosphate, antioxidant, polypropylene and O3Before use, the-CaMgAl-SDS-LDHs is placed in an oven at 80 ℃ for drying for 24 hours and then weighed according to the research formula. Firstly, polypropylene is added into a torque rheometer (the set temperature and the set rotating speed are respectively 180 ℃ and 50r/min) to be heated and melted for 3min, and then premixed flame retardant is added to be banburied for 12 min. And (3) placing the banburying sample into a mold with a test size specification, placing the banburying sample into a flat vulcanizing machine with a set temperature of 180 ℃ for preheating for 3min, maintaining the pressure for 5min, and naturally cooling to room temperature to obtain the halogen-free flame-retardant polypropylene composite material with the efficient flame-retardant and smoke-suppression functions required by analysis and test.
Example 10
A halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppression functions comprises the following components:
100 parts by mass of polypropylene
Silicon-containing compatibilizer 1 part by mass
Ammonium polyphosphate 18 parts by mass
Pentaerythritol 6 parts by mass
0.1 part by mass of an antioxidant
O3-CaMgAl-SDS-LDHs 3 parts by mass
A preparation method of a halogen-free flame-retardant polypropylene composite material with efficient flame-retardant and smoke-suppression functions comprises the following steps:
mixing ammonium polyphosphate, antioxidant, polypropylene and O3Before use, the-CaMgAl-SDS-LDHs is placed in an oven at 80 ℃ for drying for 24 hours and then weighed according to the research formula. Firstly, polypropylene is added into a torque rheometer (the set temperature and the set rotating speed are respectively 180 ℃ and 50r/min) to be heated and melted for 3min, and then premixed flame retardant is added to be banburied for 12 min. And (3) placing the banburying sample into a mold with a test size specification, placing the banburying sample into a flat vulcanizing machine with a set temperature of 180 ℃ for preheating for 3min, maintaining the pressure for 5min, and naturally cooling to room temperature to obtain the halogen-free flame-retardant polypropylene composite material with the efficient flame-retardant and smoke-suppression functions required by analysis and test.
Example 11
A halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppression functions comprises the following components:
100 parts by mass of polypropylene
Silicon-containing compatibilizer 1 part by mass
Ammonium polyphosphate 18 parts by mass
Pentaerythritol 6 parts by mass
0.1 part by mass of an antioxidant
O3-CaMgAl-SDS-LDHs 4 parts by mass
A preparation method of a halogen-free flame-retardant polypropylene composite material with efficient flame-retardant and smoke-suppression functions comprises the following steps:
mixing ammonium polyphosphate, antioxidant, polypropylene and O3Before use, the-CaMgAl-SDS-LDHs is placed in an oven at 80 ℃ for drying for 24 hours and then weighed according to the research formula. First, polypropylene was heated and melted for 3min in a torque rheometer (set temperature and rotation speed 180 ℃ and 50r/min, respectively), and then a premixed resistor was addedAnd (5) burning the agent, and banburying for 12 min. And (3) placing the banburying sample into a mold with a test size specification, placing the banburying sample into a flat vulcanizing machine with a set temperature of 180 ℃ for preheating for 3min, maintaining the pressure for 5min, and naturally cooling to room temperature to obtain the halogen-free flame-retardant polypropylene composite material with the efficient flame-retardant and smoke-suppression functions required by analysis and test.
Example 12
A halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppression functions comprises the following components:
100 parts by mass of polypropylene
Silicon-containing compatibilizer 1 part by mass
Ammonium polyphosphate 18 parts by mass
Pentaerythritol 6 parts by mass
0.1 part by mass of an antioxidant
O35 parts by mass of-CaMgAl-SDS-LDHs
A preparation method of a halogen-free flame-retardant polypropylene composite material with efficient flame-retardant and smoke-suppression functions comprises the following steps:
mixing ammonium polyphosphate, antioxidant, polypropylene and O3Before use, the-CaMgAl-SDS-LDHs is placed in an oven at 80 ℃ for drying for 24 hours and then weighed according to the research formula. Firstly, polypropylene is added into a torque rheometer (the set temperature and the set rotating speed are respectively 180 ℃ and 50r/min) to be heated and melted for 3min, and then premixed flame retardant is added to be banburied for 12 min. And (3) placing the banburying sample into a mold with a test size specification, placing the banburying sample into a flat vulcanizing machine with a set temperature of 180 ℃ for preheating for 3min, maintaining the pressure for 5min, and naturally cooling to room temperature to obtain the halogen-free flame-retardant polypropylene composite material with the efficient flame-retardant and smoke-suppression functions required by analysis and test.
Example 13
A halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppression functions comprises the following components:
100 parts by mass of polypropylene
Silicon-containing compatilizer 2 parts by mass
Ammonium polyphosphate 18 parts by mass
Pentaerythritol 6 parts by mass
0.1 part by mass of an antioxidant
O3-CaMgAl-SDS-LDHs 2 parts by mass
A preparation method of a halogen-free flame-retardant polypropylene composite material with efficient flame-retardant and smoke-suppression functions comprises the following steps:
mixing ammonium polyphosphate, antioxidant, polypropylene and O3Before use, the-CaMgAl-SDS-LDHs is placed in an oven at 80 ℃ for drying for 24 hours and then weighed according to the research formula. Firstly, polypropylene is added into a torque rheometer (the set temperature and the set rotating speed are respectively 180 ℃ and 60r/min) to be heated and melted for 3min, and then premixed flame retardant is added to be banburied for 12 min. And (3) placing the banburying sample into a mold with a test size specification, placing the banburying sample into a flat vulcanizing machine with a set temperature of 180 ℃ for preheating for 3min, maintaining the pressure for 5min, and naturally cooling to room temperature to obtain the halogen-free flame-retardant polypropylene composite material with the efficient flame-retardant and smoke-suppression functions required by analysis and test.
Example 14
A halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppression functions comprises the following components:
100 parts by mass of polypropylene
Silicon-containing compatilizer 2 parts by mass
Ammonium polyphosphate 18 parts by mass
Pentaerythritol 6 parts by mass
0.1 part by mass of an antioxidant
O3-CaMgAl-SDS-LDHs 3 parts by mass
A preparation method of a halogen-free flame-retardant polypropylene composite material with efficient flame-retardant and smoke-suppression functions comprises the following steps: o is3Before use, the-CaMgAl-SDS-LDHs is placed in an oven at 80 ℃ for drying for 24 hours and then weighed according to the research formula. Firstly, polypropylene is added into a torque rheometer (the set temperature and the set rotating speed are respectively 180 ℃ and 60r/min) to be heated and melted for 3min, and then premixed flame retardant is added to be banburied for 12 min. Placing the internal mixed sample into a mold with a test size specification, placing the mold in a flat vulcanizing machine with a set temperature of 180 ℃ for preheating for 3min, maintaining the pressure for 5min, and naturally cooling to room temperature to obtain an analysis test instituteThe halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant smoke-suppressing function is needed.
Example 15
A halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppression functions comprises the following components:
100 parts by mass of polypropylene
Silicon-containing compatilizer 2 parts by mass
Ammonium polyphosphate 18 parts by mass
Pentaerythritol 6 parts by mass
0.1 part by mass of an antioxidant
O3-CaMgAl-SDS-LDHs 4 parts by mass
A preparation method of a halogen-free flame-retardant polypropylene composite material with efficient flame-retardant and smoke-suppression functions comprises the following steps:
mixing ammonium polyphosphate, antioxidant, polypropylene and O3Before use, the-CaMgAl-SDS-LDHs is placed in an oven at 80 ℃ for drying for 24 hours and then weighed according to the research formula. Firstly, polypropylene is added into a torque rheometer (the set temperature and the set rotating speed are respectively 180 ℃ and 60r/min) to be heated and melted for 3min, and then premixed flame retardant is added to be banburied for 12 min. And (3) placing the banburying sample into a mold with a test size specification, placing the banburying sample into a flat vulcanizing machine with a set temperature of 180 ℃ for preheating for 3min, maintaining the pressure for 5min, and naturally cooling to room temperature to obtain the halogen-free flame-retardant polypropylene composite material with the efficient flame-retardant and smoke-suppression functions required by analysis and test.
Example 16
A halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppression functions comprises the following components:
100 parts by mass of polypropylene
Silicon-containing compatilizer 2 parts by mass
Ammonium polyphosphate 18 parts by mass
Pentaerythritol 6 parts by mass
0.1 part by mass of an antioxidant
O35 parts by mass of-CaMgAl-SDS-LDHs
A preparation method of a halogen-free flame-retardant polypropylene composite material with efficient flame-retardant and smoke-suppression functions comprises the following steps:
mixing ammonium polyphosphate, antioxidant, polypropylene and O3Before use, the-CaMgAl-SDS-LDHs is placed in an oven at 80 ℃ for drying for 24 hours and then weighed according to the research formula. Firstly, polypropylene is added into a torque rheometer (the set temperature and the set rotating speed are respectively 180 ℃ and 60r/min) to be heated and melted for 3min, and then premixed flame retardant is added to be banburied for 12 min. And (3) placing the banburying sample into a mold with a test size specification, placing the banburying sample into a flat vulcanizing machine with a set temperature of 180 ℃ for preheating for 3min, maintaining the pressure for 5min, and naturally cooling to room temperature to obtain the halogen-free flame-retardant polypropylene composite material with the efficient flame-retardant and smoke-suppression functions required by analysis and test.
The application effect is as follows:
the performance tests were carried out on the flame retardant polypropylene materials prepared in the above examples 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16 according to the following criteria: the horizontal and vertical burning test GB/T2408-2008, the limit oxygen index test GB/T2406.2-2009, and the cone calorimetry test ISO 5660. The results of the UL-94, LOI and total cone calorimetry (TSP) measurements obtained for the standard samples are shown in Table 1.
TABLE 1 results of UL-94 and LOI tests on the standard test specimens of the examples
The performance tests were carried out on the flame retardant polypropylene materials prepared in the above examples 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16 according to the following criteria: the tensile test was carried out in accordance with GB/T1040.3-2006 and the bending test was carried out in accordance with GB/T9341-2008. The results of the mechanical property tests of the obtained standard samples are shown in table 2.
TABLE 2 mechanical property test results of the standard samples of the examples
The invention has many applications, and the above description is only a preferred embodiment of the invention. It should be noted that the above examples are only for illustrating the present invention, and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that various modifications can be made without departing from the principles of the invention and these modifications are to be considered within the scope of the invention.
Claims (7)
1. A halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppressing functions is characterized in that: comprises the following raw materials and components: 100 parts of polypropylene, 1-6 parts of silicon compatilizer, 15-30 parts of ammonium polyphosphate, 3-15 parts of pentaerythritol, 0.01-1 part of antioxidant and 1-20 parts of sodium oleate modified dodecyl sulfate radical calcium magnesium aluminum hydrotalcite.
2. The halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppression functions as claimed in claim 1, is characterized in that: the silicon-containing compatilizer is a compound with a macromolecular structure and a silane side chain, and the molecular weight of the compound is 2000 g/mol-10000 g/mol.
3. The halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppression functions as claimed in claim 1, is characterized in that: the antioxidant is a compound of beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl ester and tris [2, 4-di-tert-butylphenyl ] phosphite in a ratio of 1: 1.
4. The halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppression functions as claimed in claim 1, is characterized in that: the polypropylene is one or a mixture of homo-polypropylene or co-polypropylene.
5. The halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppression functions as claimed in claim 1, is characterized in that: the preparation method of the sodium oleate modified dodecyl sulfate radical calcium magnesium aluminum hydrotalcite comprises the following steps:
(1) taking Ca (NO) by coprecipitation method3)2·4H2O、Mg(NO3)2·6H2O and Al (NO)3)3·9H2Dissolving O in carbon dioxide-removed water, marking as a solution A, dissolving 0.5-2 mol of NaOH in the carbon dioxide-removed water, marking as a solution B, respectively dropwise adding the solution A, B into a flask, stirring at normal temperature, keeping the pH value between 9-11, continuously stirring for 1-5 h after dropwise adding is finished, crystallizing for 13-24 h at 60-85 ℃, performing suction filtration, washing with carbon dioxide water to be neutral, drying at 60-85 ℃, grinding, sieving with a 60-80-mesh sieve (177-250 mu m), and marking as CaMgAl-LDHs.
(2) Dissolving 15g of CaMgAl-LDHs and 16.2g of Sodium Dodecyl Sulfate (SDS) in carbon dioxide-removed water by adopting an ion exchange method, stirring for 13-24 h at normal temperature, carrying out suction filtration, washing to be neutral by using carbon dioxide, drying at 60-85 ℃, grinding, and sieving by using a 60-80-mesh sieve (177-250 mu m) to obtain SDS-LDHs.
(3) Dissolving 10g of SDS-LDHs in carbon dioxide-removed water, stirring at normal temperature, adding 0.2-1.2 g/L of sodium oleate, reacting for 13-24 h, performing suction filtration, drying, and sieving with a 60-80 mesh sieve (177-250 mu m) to obtain the sodium oleate modified dodecyl sulfate radical calcium magnesium aluminum hydrotalcite.
6. The halogen-free flame retardant polypropylene composite material with high-efficiency flame retardant and smoke suppression function according to claim 5,the method is characterized in that: ca (NO)3)2·4H2O、Mg(NO3)2·6H2O and Al (NO)3)3·9H2The molar ratio of O is 1-3: 2-3: 1-2.
7. The halogen-free flame-retardant polypropylene composite material with high-efficiency flame-retardant and smoke-suppression functions as claimed in claim 1, is characterized in that: the preparation method comprises the following steps:
before ammonium polyphosphate, pentaerythritol, an antioxidant, polypropylene and sodium oleate modified dodecyl sulfate radical type calcium magnesium aluminum hydrotalcite are used, the mixture is placed in an oven at the temperature of 60-80 ℃ for drying for 8-24 hours, and then the mixture is weighed according to a formula; firstly, adding polypropylene into a torque rheometer, heating and melting for 2-5 min, setting the temperature and the rotating speed to be 160-190 ℃ and 50-80 r/min respectively, then adding a premixed flame retardant, and banburying for 12-15 min; and (3) placing the internally mixed sample into a mold with a tested size specification, placing the mold into a flat vulcanizing machine with a set temperature of 160-190 ℃ for preheating for 2-5 min, maintaining the pressure for 2-5 min, and naturally cooling to room temperature to obtain the product.
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| CN117362805A (en) * | 2023-09-08 | 2024-01-09 | 金发科技股份有限公司 | Halogen-free flame-retardant crosslinked polyolefin composition and preparation method and application thereof |
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