CN113150382B - Modified melamine phytate flame retardant and preparation method and application thereof - Google Patents

Modified melamine phytate flame retardant and preparation method and application thereof Download PDF

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CN113150382B
CN113150382B CN202110235327.7A CN202110235327A CN113150382B CN 113150382 B CN113150382 B CN 113150382B CN 202110235327 A CN202110235327 A CN 202110235327A CN 113150382 B CN113150382 B CN 113150382B
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flame retardant
phytate
melamine
modified melamine
metal
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CN113150382A (en
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史聪灵
钱小东
刘国林
井静云
杨兆春
车洪磊
李建
胥旋
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China Academy of Safety Science and Technology CASST
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    • 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
    • C08K5/34928Salts
    • 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
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20Oxides; Hydroxides
    • C08K3/22Oxides; Hydroxides of metals
    • C08K2003/2237Oxides; Hydroxides of metals of titanium
    • 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
    • C08K2003/2248Oxides; Hydroxides of metals of copper
    • 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
    • C08K2003/2265Oxides; Hydroxides of metals of iron
    • 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
    • C08K2003/2265Oxides; Hydroxides of metals of iron
    • C08K2003/2275Ferroso-ferric oxide (Fe3O4)
    • CCHEMISTRY; METALLURGY
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    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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    • C08L2201/02Flame or fire retardant/resistant

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Abstract

The invention provides a modified melamine phytate flame retardant and a preparation method and application thereof. The invention provides a modified melamine phytate flame retardant, which can play a role in lamellar blocking in the combustion process of a high polymer, thereby blocking mass and heat transfer, delaying the exchange of pyrolysis gas and the outside, has stronger selectivity and catalytic activity on toxic gas, effectively inhibits smoke and reduces toxicity in the combustion process of the high polymer, and can be applied to the flame retardance of polyester, polyurethane, polyamide, polyacrylate resin, polyolefin and rubber materials.

Description

Modified melamine phytate flame retardant and preparation method and application thereof
Technical Field
The invention relates to the field of flame retardants, in particular to a modified melamine phytate flame retardant and a preparation method and application thereof.
Background
Polymeric materials such as polyesters, polyurethanes, polyamides, polyacrylate resins, polyolefin materials or rubbers, etc., are not only prone to burn during a fire, but also release a significant amount of smoke during the combustion process. It is common practice to combine some phosphorus-containing compound, halogen-containing compound, or mixture thereof with the polymer to achieve flame retardancy of the polymer.
Melamine (MA) and its salts belong to nitrogen and nitrogen-phosphorus flame retardants, and melamine salts integrate an acid source and a gas source, have the characteristics of no halogen, low smoke, low toxicity, good intermiscibility with a base material, good thermal stability, small addition amount, small water solubility, excellent flame retardant property and the like, and are important components for forming the intumescent halogen-free flame retardant. Melamine and its salts are an environment-friendly halogen-free flame retardant, are usually white powder in appearance, are widely applied to thermoplastic and thermosetting plastics, and rubber, fiber and other products, and have a very good flame retardant effect on glass fiber reinforced nylon 6. The melamine and the salt thereof have better flame retardant effect as the intumescent halogen-free flame retardant, meet the requirements of green chemistry, but have the defects of low flame retardant efficiency, poor smoke suppression performance and the like, and seriously restrict the application thereof.
Therefore, the flame retardant is modified on the original basis, the flame retardant efficiency and the smoke suppression performance of the flame retardant are improved to the greatest extent, and the halogen-free flame retardant is the direction of important research for future development of the halogen-free flame retardant.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a modified melamine phytate flame retardant, and a preparation method and application thereof.
The invention adopts the following technical scheme:
the invention provides a modified melamine phytate flame retardant, which is nano-particle in appearance, has a microstructure of layered melamine phytate containing metal salt, and the metal salt is compounded in the melamine phytate.
After the melamine phytate composite metal salt is modified, due to the special structure of the melamine phytate composite metal salt, the melamine phytate composite metal salt can play a role in lamellar blocking in the combustion process of a high polymer, so that the quality and heat transfer are blocked, the exchange of pyrolysis gas and the outside is delayed, and the melamine phytate composite metal salt has stronger selectivity and catalytic activity on toxic gas, and effectively inhibits smoke and reduces toxicity in the combustion process of the high polymer. The nano flame retardant is added into a polymer matrix, has good dispersibility, and can achieve better flame-retardant and smoke-suppression effects under the condition of less consumption.
Preferably, the mass ratio of the melamine phytate to the metal salt is 5-50: 1.
preferably, the metal in the metal salt is one or more of magnesium, calcium, strontium, barium, aluminum, tin, cerium, and transition metals.
Further preferably, the metal in the metal salt is copper, iron or titanium.
The invention also provides a preparation method of the modified melamine phytate flame retardant.
The preparation method provided by the invention comprises the following steps: dispersing melamine and a metal-containing compound in water, adding phytic acid at 50-95 ℃ for reaction, adjusting the pH of the solution to 6.5-7.5 after the reaction, and then sequentially filtering, washing, drying and crushing. Wherein a metal-containing compound refers to a compound capable of reacting to form a corresponding metal salt.
The preparation method can simply and controllably obtain the modified melamine phytate flame retardant, and has high yield.
Preferably, the metal-containing compound is a metal oxide or metal hydroxide. Specifically, the metal oxide may be one or more of alumina hydrate, alumina, magnesia, zinc oxide, calcium oxide, cerium oxide, ferric oxide, ferroferric oxide, titanium dioxide, barium oxide, strontium oxide, osmium oxide, and osmium tetroxide; the hydroxide can be one or more of aluminum hydroxide, zinc hydroxide, cerium hydroxide, iron hydroxide, calcium hydroxide, strontium hydroxide, copper hydroxide, titanium hydroxide and tin hydroxide.
Preferably, the molar ratio of the phytic acid to the melamine is 1: 0.5-1.
Preferably, the molar ratio of the phytic acid to the metal-containing compound is 1: 0.01-0.2.
Preferably, the phytic acid is added dropwise in order to make the reaction more complete.
The invention also provides application of the modified melamine phytate flame retardant in improving flame retardant performance and smoke suppression and attenuation performance of polymer materials such as polyester, polyurethane, polyamide, polyacrylate resin, polyolefin and rubber.
Specifically, the flame retardant can be added into a polymer matrix independently, or can be compounded with other flame retardants for use. The modified melamine phytate flame retardant provided by the invention has good flame retardant effect and good dispersibility when being added into a polymer matrix, so that the melamine phytate flame retardant can be used independently and the addition amount is 1-30 wt.%.
Preferably, the modified melamine phytate flame retardant is added to the polyolefin in an amount of 15 wt.% to 30 wt.%.
Adding the modified melamine phytate flame retardant into epoxy resin in an amount of 5-20 wt.%.
Adding the modified melamine phytate flame retardant into a polyester or polyamide material in an amount of 10-30 wt.%.
The invention provides a modified melamine phytate flame retardant, which can play a role in lamellar blocking in the combustion process of a high polymer, thereby blocking mass and heat transfer, delaying the exchange of pyrolysis gas and the outside, has stronger selectivity and catalytic activity on toxic gas, effectively inhibits smoke and reduces toxicity in the combustion process of the high polymer, and can be applied to the flame retardance of polyester, polyurethane, polyamide, polyacrylate resin, polyolefin and rubber materials.
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FIG. 1 is a scanning electron microscope image of a modified melamine phytate flame retardant in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention are clearly and completely described below, and it is obvious that the described embodiments are a part of the embodiments of the present invention, but not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The embodiment provides a modified melamine phytate flame retardant, and the preparation method comprises the following steps:
adding 800ml of deionized water into a three-necked bottle with the capacity of 2L, heating the three-necked bottle in a mechanical stirrer in a water bath to 80 ℃, weighing 47.5g of melamine and 2.5g of copper hydroxide, adding the melamine and the copper hydroxide into the three-necked bottle, stirring, slowly dripping 82.5g of phytic acid solution (70%) into the three-necked bottle, keeping the temperature of a water bath kettle at 80 ℃, and continuously stirring for 1 hour to fully form suspension; the pH value of the whole system is controlled between 6.5 and 7.5 by dripping a proper amount of sodium hydroxide. After the reaction, the reaction mixture was cooled to room temperature, repeatedly filtered and washed several times by a buchner funnel and a circulating water type vacuum pump, and the obtained product was dried in a drying oven at 80 ℃ for 24 hours and then taken out. The yield was 87%.
The structure of the product is shown in fig. 1, and it can be seen from the figure that the microstructure is a layered structure, and the metal salt is compounded in the melamine phytate.
The results of the product's major elemental analysis are shown in table 1:
table 1 results of main element analysis of the product of example 1
Figure BDA0002959749820000041
Taking 15g of the prepared modified melamine phytate flame retardant and 80g of epoxy resin, uniformly stirring at 60 ℃, then adding 17.4g of 4, 4-diaminodiphenylmethane serving as a curing agent, pouring the flame-retardant resin liquid into a grinding tool with the length of 8cm, the width of 3cm and the thickness of 3cm, heating to 100 ℃, keeping for 2 hours, heating to 150 ℃, keeping for 2 hours, cooling to room temperature, and demolding to obtain a sample. The samples were subjected to the UL94 vertical burn test to achieve a V0 rating. The oxygen index of the sample is measured by an oxygen index meter, and the oxygen index reaches 33. UL-94 and oxygen index measurement show that the modified melamine phytate flame retardant prepared in the embodiment has good flame retardant effect on epoxy resin.
The smoke density can be reduced by 41% through smoke density test determination, and the modified melamine phytate flame retardant prepared in the embodiment has good smoke suppression and attenuation effects on epoxy resin.
Example 2
The embodiment provides a modified melamine phytate flame retardant, and the preparation method comprises the following steps:
adding 800ml of deionized water into a three-necked bottle with the volume of 2L, heating the three-necked bottle in a mechanical stirrer in a water bath to 90 ℃, weighing 47.5g of melamine and 3.5g of ferric hydroxide, adding the melamine and the ferric hydroxide into the three-necked bottle, stirring, slowly dripping 82.5g of phytic acid solution (70%) into the three-necked bottle, keeping the temperature of a water bath kettle at 90 ℃ and continuously stirring for 1 hour to fully form a suspension; the pH value of the whole system is controlled between 6.5 and 7.5 by dripping a proper amount of sodium hydroxide. After the reaction, the reaction mixture was cooled to room temperature, repeatedly filtered and washed several times by a buchner funnel and a circulating water type vacuum pump, and the obtained product was dried in a drying oven at 60 ℃ for 24 hours and then taken out. The yield was 91%.
And (3) uniformly mixing 140g of the prepared modified melamine phytate flame retardant and 860gPA6, adding the mixture into a double-screw extruder, extruding and granulating at the unit temperature of 220-. The samples were subjected to the UL94 vertical burn test to achieve a V0 rating. The oxygen index of the sample is measured by a limit oxygen index instrument, and the oxygen index reaches 30.5. The flame retardant has good flame retardant effect on PA6 as can be seen by UL-94 and oxygen index measurement.
The smoke density is reduced by 52% through smoke density test determination, and the modified melamine phytate flame retardant prepared in the embodiment has good smoke suppression and attenuation effects on PA 6.
Example 3
The embodiment provides a modified melamine phytate flame retardant, and the preparation method comprises the following steps:
adding 800ml of deionized water into a three-necked bottle with the capacity of 2L, heating the three-necked bottle in a mechanical stirrer in a water bath to 70 ℃, weighing 47.5g of melamine and 1.5g of ferroferric oxide, adding the melamine and the ferroferric oxide into the three-necked bottle, stirring, slowly dripping 82.5g of phytic acid solution (70%) into the three-necked bottle, keeping the temperature of a water bath kettle at 70 ℃ and continuously stirring for 1 hour to fully form suspension; the pH value of the whole system is controlled between 6.5 and 7.5 by dripping a proper amount of sodium hydroxide. After the reaction, the reaction mixture was cooled to room temperature, repeatedly filtered and washed several times by a buchner funnel and a circulating water type vacuum pump, and the obtained product was dried in a drying oven at 80 ℃ for 24 hours and then taken out. The yield was 91%.
And (3) uniformly mixing 250g of the prepared modified melamine phytate flame retardant and 750g of PP, adding the mixture into a double-screw extruder, extruding and granulating at the unit temperature of 180-. The samples were subjected to the UL94 vertical burn test to achieve a V0 rating. The oxygen index of the sample is measured by a limit oxygen index meter, and the oxygen index reaches 32.5. The UL-94 and oxygen index measurement shows that the flame retardant has good flame retardant effect on PP.
The smoke density can be reduced by 45% through smoke density test determination, and the modified melamine phytate flame retardant prepared in the embodiment has good smoke suppression and attenuation effects on PP.
Example 4
The embodiment provides a modified melamine phytate flame retardant, and the preparation method comprises the following steps:
adding 800ml of deionized water into a three-necked bottle with the capacity of 2L, heating the three-necked bottle in a mechanical stirrer in a water bath to 70 ℃, weighing 47.5g of melamine and 3.0g of titanium hydroxide, adding the melamine and the titanium hydroxide into the three-necked bottle, stirring, slowly dripping 82.5g of phytic acid solution (70%) into the three-necked bottle, keeping the temperature of a water bath kettle at 70 ℃ and continuously stirring for 1 hour to fully form a suspension; the pH value of the whole system is controlled between 6.5 and 7.5 by dripping a proper amount of sodium hydroxide. After the reaction, the reaction mixture was cooled to room temperature, repeatedly filtered and washed several times by a buchner funnel and a circulating water type vacuum pump, and the obtained product was dried in a drying oven at 80 ℃ for 24 hours and then taken out. The yield was 85%.
And (2) uniformly mixing 150g of the prepared modified melamine phytate flame retardant and 800gPA6, adding the mixture into a double-screw extruder after uniform mixing, extruding and granulating at the unit temperature of 220-240 ℃, the die head temperature of 230 ℃ and the screw rotating speed of 240rpm, drying and cooling to obtain the flame-retardant PA6 granular material. The samples were subjected to UL94 vertical burn test to achieve a V0 rating. The oxygen index of the sample is measured by a limit oxygen index meter, and the oxygen index reaches 32.0. The flame retardant has good flame retardant effect on PA6 as can be seen by UL-94 and oxygen index measurement.
The smoke density can be reduced by 64% through smoke density test determination, and the modified melamine phytate flame retardant prepared in the embodiment has good smoke suppression and attenuation effects on PA 6.
Comparative example 1
This comparative example provides an unmodified melamine phytate flame retardant prepared as follows:
adding 800ml of deionized water into a three-necked bottle with the volume of 2L, heating the three-necked bottle in a mechanical stirrer in a water bath to 80 ℃, weighing 47.5g of melamine, adding the melamine into the three-necked bottle, stirring, slowly dripping 47.5g of phytic acid solution (70%) into the three-necked bottle, keeping the temperature of a water bath kettle at 80 ℃, and continuously stirring for 1 hour to fully form a suspension; the pH value of the whole system is controlled between 6.5 and 7.5 by dripping a proper amount of sodium hydroxide. After the reaction, the reaction mixture was cooled to room temperature, repeatedly filtered and washed several times by a buchner funnel and a circulating water type vacuum pump, and the obtained product was dried in a drying oven at 80 ℃ for 24 hours and then taken out. The yield was 81%.
The flame retardant prepared above was subjected to UL-94 and oxygen index measurement in the same manner as in example 1, and UL94 was rated V1, and the limiting oxygen index LOI was 29. Therefore, the performance of the modified melamine phytate flame retardant is obviously better than that of the unmodified melamine phytate flame retardant.
Comparative example 2
4.42g of copper phytate was mechanically mixed with 113.10g of melamine phytate and used as a comparative flame retardant.
The comparative flame retardant was measured for properties in the same manner as in example 1, and found to have a V2 rating in UL94 and a limiting oxygen index LOI of 27. Therefore, the performance of the modified melamine phytate flame retardant is obviously better than that of the flame retardant in the comparative example.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.

Claims (10)

1. The modified melamine phytate flame retardant is characterized in that the appearance of the flame retardant is nano particles, the microstructure of the flame retardant is layered melamine phytate containing metal salt, and the metal salt is compounded in the melamine phytate;
the preparation method of the modified melamine phytate flame retardant comprises the following steps: dispersing melamine and a metal-containing compound in water, adding phytic acid at 50-95 ℃ for reaction, adjusting the pH of the solution to 6.5-7.5 after the reaction, and then sequentially filtering, washing, drying and crushing.
2. The modified melamine phytate flame retardant according to claim 1, wherein the mass ratio of the melamine phytate to the metal salt is 5-50: 1.
3. the modified melamine phytate flame retardant of claim 1 or 2, wherein the metal of the metal salt is one or more of magnesium, calcium, strontium, barium, aluminum, tin, cerium, transition metals.
4. A method for preparing a modified melamine phytate flame retardant according to any one of claims 1 to 3, comprising: dispersing melamine and a metal-containing compound in water, adding phytic acid at 50-95 ℃ for reaction, adjusting the pH of the solution to 6.5-7.5 after the reaction, and then sequentially filtering, washing, drying and crushing.
5. The method of claim 4, wherein the metal-containing compound is a metal oxide or metal hydroxide.
6. The preparation method of the modified melamine phytate flame retardant of claim 4, wherein the molar ratio of the phytic acid to the melamine is 1: 0.5-1.
7. The method for preparing the modified melamine phytate flame retardant of claim 4, wherein the molar ratio of the phytic acid to the metal-containing compound is 1: 0.01-0.2.
8. The method of claim 4, wherein the phytic acid is added dropwise.
9. Use of the modified melamine phytate flame retardant of any one of claims 1 to 3 for improving the flame retardant and smoke and toxicity inhibiting properties of polyesters, polyurethanes, polyamides, polyacrylate resins, polyolefins or rubbers.
10. The use according to claim 9, wherein the modified melamine phytate flame retardant is added to the polyolefin in an amount of 15 to 30 wt.%;
and/or adding the modified melamine phytate flame retardant into epoxy resin, wherein the addition amount is 5-20 wt.%;
and/or adding the modified melamine phytate flame retardant into a polyester or polyamide material in an amount of 10-30 wt.%.
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