CN109437262B - Micro-nano basic magnesium carbonate flame retardant and preparation method thereof - Google Patents
Micro-nano basic magnesium carbonate flame retardant and preparation method thereof Download PDFInfo
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Abstract
The invention provides a micro-nano basic magnesium carbonate flame retardant and a preparation method thereof. The preparation method comprises the following steps: 1) dropwise adding a soluble carbonate aqueous solution with the concentration of 0.1-1.5 mol/L into a magnesium chloride hexahydrate aqueous solution with the concentration of 0.1-1.5 mol/L and uniformly stirring at the speed of 1-50 mL/min; 2) curing the mixed solution obtained in the step 1) in an oven at 50-90 ℃ for 0.5-5 h; and 3) further filtering and washing the mixed solution obtained in the step 2), and drying the mixed solution at the temperature of 30-100 ℃ for 30-60 min to obtain the micro-nano basic magnesium carbonate flame retardant with the chemical formula of Mg5(CO3)4(OH)2·4H2And O. According to the micro-nano basic magnesium carbonate flame retardant provided by the invention, the preparation process does not need to use an organic solvent, and the micro-nano basic magnesium carbonate flame retardant is green and environment-friendly, and has excellent flame retardant effect and good smoke suppression effect.
Description
Technical Field
The invention relates to the field of nano materials, and in particular relates to a micro-nano basic magnesium carbonate flame retardant and a preparation method thereof.
Background
With the development of modern industry, the application scale of high molecular polymers is continuously enlarged, the substances have flammable characteristics, the hidden danger of fire is increasingly highlighted, in recent years, large fire accidents occur frequently, and most of the lethal inducement of fire is suffocation caused by overlarge smoke quantity. Part of the accidents are caused by that metal melt splashed by electric welding ignites a large amount of flammable polyurethane insulation material fragments accumulated below, thereby causing fire disasters. Therefore, the suppression of fire is imminent. Starting from raw materials, the method for inhibiting combustion is mainly to add proper flame retardant so as to improve the heat resistance of the polymer.
The flame retardant is classified into halogen-based, phosphorus-based, halogen-phosphorus-based, nitrogen-based, silicon-based, aluminum-magnesium-based, and the like, and is classified into inorganic flame retardants, organic flame retardants, polymeric flame retardants, and the like according to the chemical structure. Among them, the halogen flame retardant and the phosphorus flame retardant are gradually eliminated due to the large smoke generation and the generation of harmful gases in the flame retardant process, so that how to obtain an environment-friendly flame retardant which has high-efficiency flame retardancy and does not generate a large amount of byproducts is very important.
Patent CN102583457A introduces a method for synthesizing a nano needle-like magnesium hydroxide flame retardant, which is obtained by taking bischofite, hydrated lime and calcium chloride dihydrate as raw materials, taking polyethylene glycol and sodium dodecyl sulfate as dispersing agents, performing ball milling by a ball mill, and performing heat treatment.
Patent CN106673027A describes a preparation method of hexagonal sheet magnesium hydroxide flame retardant, which is prepared by taking magnesium salt solution, structure directing agent, inorganic alkali solution and absolute ethyl alcohol as raw materials to carry out hydrothermal reaction, wherein most of the structure directing agent used in the method is organic matters such as organic alkali or surfactant, the preparation process is accompanied with the generation of organic waste liquid, and the method does not have the characteristic of environmental protection, and the patent does not specifically measure the flame retardant effect of the flame retardant.
Disclosure of Invention
The invention aims to provide a micro-nano basic magnesium carbonate flame retardant and a preparation method thereof, so as to solve the problems that the flame retardant in the prior art has large smoke generation amount and is accompanied with harmful gas generation in the flame retardant process.
In order to solve the technical problems, the invention adopts the following technical scheme:
according to a first aspect of the invention, a preparation method of a micro-nano basic magnesium carbonate flame retardant is provided, and the preparation method comprises the following steps: 1) dropwise adding a soluble carbonate aqueous solution with the concentration of 0.1-1.5 mol/L into a magnesium chloride hexahydrate aqueous solution with the concentration of 0.1-1.5 mol/L, which is stirred at a constant speed, at the rate of 1-50 mL/min; 2) curing the mixed solution obtained in the step 1) in an oven at 50-90 ℃ for 0.5-5 h; and 3) further filtering and washing the mixed solution obtained in the step 2), and drying the mixed solution at the temperature of 30-100 ℃ for 30-60 min to prepare the micro-nano basic magnesium carbonate flame retardant with the chemical formula of Mg5(CO3)4(OH)2·4H2O。
The soluble carbonate includes sodium carbonate, potassium carbonate, ammonium carbonate, sodium bicarbonate, potassium bicarbonate, and the like.
Preferably, the concentration of the soluble carbonate aqueous solution in the step 1) is 0.7-1.5 mol/L, and the concentration of the magnesium chloride hexahydrate aqueous solution is 0.7-1.5 mol/L.
Preferably, the speed of uniform stirring in the step 1) is 10-1000 rpm.
Preferably, the curing temperature in the step 2) is 50-80 ℃, and the curing time is 2-5 h.
Preferably, the drying condition in the step 3) is drying at 60-100 ℃ for 30-60 min.
According to a preferred embodiment of the present invention, the preparation method specifically comprises the steps of: 1) dripping 1-1.5 mol/L soluble carbonate aqueous solution into 1-1.5 mol/L magnesium chloride hexahydrate aqueous solution which is uniformly stirred at a constant speed at the speed of 1-50 mL/min; 2) curing the mixed solution obtained in the step 1) in an oven at 50-80 ℃ for 2-4 h; and 3) further filtering and washing the mixed solution obtained in the step 2), and drying at 60-100 ℃ for 30-60 min to obtain the micro-nano basic magnesium carbonate flame retardant.
According to a particularly preferred embodiment of the invention, the preparation process comprises in particular: 1) dropwise adding a sodium carbonate aqueous solution with the concentration of 1mol/L into a magnesium chloride hexahydrate aqueous solution with the concentration of 1mol/L and uniformly stirred at 800rpm at the speed of 10 mL/min; 2) curing the mixed solution obtained in the step 1) in an oven at 80 ℃ for 2 hours; and 3) further filtering and washing the mixed solution obtained in the step 2), and drying at 60 ℃ for 30min to obtain the micro-nano basic magnesium carbonate flame retardant.
According to a second aspect of the invention, the micro-nano basic magnesium carbonate flame retardant prepared by the preparation method is provided, and is a micron particle with a spherical structure, wherein the micron particle is formed by stacking multiple layers of petal-shaped nanosheets, and the size of the micron particle is 30-50 microns.
The micron particles of the micro-nano basic magnesium carbonate inorganic flame retardant prepared by the preparation method provided by the invention are spherical structures, are formed by stacking a plurality of layers of nano sheets, are similar to petals, have uniform particle size distribution and good shape stability, and are all 30-50 microns in size. Especially, according to the micro-nano basic magnesium carbonate flame retardant prepared in the embodiment 11, almost all basic magnesium carbonate forms petal-shaped microspheres as seen by an electron scanning microscope, and a small amount of incomplete nucleation exists in other ranges, so that the flame retardant effect is slightly reduced compared with that of the embodiment 11. The technical difficulty of the invention is mainly that the nucleation condition of the basic magnesium carbonate particle with the unique structure is extremely harsh, particularly the solution proportion, the control of the reaction rate, the curing time, the control of the curing temperature and the like, and the condition of each step determines whether the basic magnesium carbonate flame retardant with the unique structure can be formed.
Compared with the prior art, the micro-nano basic magnesium carbonate flame retardant and the preparation method thereof provided by the invention have the advantages that:
1) the micro-nano basic magnesium carbonate flame retardant provided by the invention has the advantages of wide raw material source, simple and clean preparation process, no need of organic solvent, environmental friendliness;
2) due to the unique multilayer sheet structure, the micro-nano basic magnesium carbonate flame retardant provided by the invention can effectively reduce the heat transfer effect, so that the flame retardant effect is superior to other flame retardants in the prior art;
3) the micro-nano basic magnesium carbonate flame retardant provided by the invention is thermally decomposed in the flame retardant process, and two effective flame retardant components, namely water and carbon dioxide, are released, so that a good smoke suppression effect is achieved.
Drawings
FIG. 1 is an electron microscope picture of a micro-nano basic magnesium carbonate flame retardant prepared according to example 1 of the present invention under an electron scanning microscope;
fig. 2 is an XRD chart of the micro-nano basic magnesium carbonate flame retardant prepared according to example 1 of the present invention.
Detailed Description
The present invention will be further described with reference to the following specific examples. It should be understood that the following examples are illustrative only and are not intended to limit the scope of the present invention.
Example 1:
the preparation method of the flame retardant comprises the following steps:
respectively preparing 200mL of sodium carbonate aqueous solution (0.1mol/L) and 200mL of magnesium chloride hexahydrate solution (0.1mol/L), and dropwise adding the sodium carbonate aqueous solution into the magnesium chloride hexahydrate solution which is uniformly stirred at 1000rpm at the speed of 50 mL/min; after the dropwise addition is finished, putting the mixed solution into a 90 ℃ oven for curing for 5 hours; after the curing is finished, filtering out precipitates, and drying for 60min at 30 ℃ after washing; and drying to obtain the petal-shaped micro-nano basic magnesium carbonate flame retardant.
The nanometer basic magnesium carbonate flame retardant is imaged by a scanning electron microscope, and as a result, as shown in figure 1, the nanometer particles are spherical structures and formed by stacking multiple layers of nanometer sheets, are similar to petals, are uniform in particle size distribution, are all located between 30 and 50 micrometers in size, and are good in shape stability. The XRD pattern of the product is shown in figure 2, and the product is further confirmed to be Mg by the diffraction pattern5(CO3)4(OH)2·4H2O, a basic magnesium carbonate flame retardant.
The flame retardant effect of the flame retardant is tested as follows:
the basic magnesium carbonate is doped into the electrospinning liquid of cellulose acetate by 5 wt% to spin a film with the width of 15mm and the thickness of 0.1mm, and the combustion rate of the composite film is measured to be 504.3 mm/min by adopting a horizontal combustion method, so that the smoke generation amount is extremely small, and the smoke suppression effect is obvious.
Example 2
The preparation method of the flame retardant comprises the following steps:
respectively preparing 200mL of sodium carbonate aqueous solution (0.1mol/L) and 200mL of magnesium chloride hexahydrate solution (0.1mol/L), and dropwise adding the sodium carbonate aqueous solution into the magnesium chloride hexahydrate solution which is uniformly stirred at 1000rpm at the speed of 1 mL/min; after the dropwise addition is finished, putting the mixed solution into a 50 ℃ oven for curing for 5 hours; after the curing is finished, filtering out precipitates, and drying for 60min at 100 ℃ after washing; and drying to obtain the petal-shaped micro-nano basic magnesium carbonate flame retardant.
The flame retardant effect of the flame retardant is tested as follows:
the basic magnesium carbonate is doped into the electrospinning liquid of cellulose acetate by 5 wt% to spin a film with the width of 15mm and the thickness of 0.1mm, and the combustion rate of the composite film is measured by adopting a horizontal combustion method to be 498.3 mm/min, the smoke generation amount is extremely small, and the smoke suppression effect is obvious.
Example 3
The preparation method of the flame retardant comprises the following steps:
respectively preparing 200mL of sodium carbonate aqueous solution (1.5mol/L) and 200mL of magnesium chloride hexahydrate solution (1.5mol/L), and dropwise adding the sodium carbonate aqueous solution into the magnesium chloride hexahydrate solution which is uniformly stirred at 1000rpm at the speed of 1 mL/min; after the dropwise addition is finished, putting the mixed solution into a 50 ℃ oven for curing for 0.5 h; after the curing is finished, filtering out precipitates, and drying for 60min at 30 ℃ after washing; and drying to obtain the petal-shaped micro-nano basic magnesium carbonate flame retardant.
The flame retardant effect of the flame retardant is tested as follows:
the basic magnesium carbonate is doped into the electrospinning liquid of cellulose acetate by 5 wt% to spin a film with the width of 15mm and the thickness of 0.1mm, and the combustion rate of the composite film is measured by a horizontal and vertical combustion method to be 508.8 mm/min, the smoke generation amount is extremely small, and the smoke suppression effect is obvious.
Example 4
The preparation method of the flame retardant comprises the following steps:
respectively preparing 200mL of potassium carbonate aqueous solution (0.1mol/L) and 200mL of magnesium chloride hexahydrate solution (0.1mol/L), and dropwise adding the potassium carbonate aqueous solution into the magnesium chloride hexahydrate solution which is stirred at a constant speed of 1000rpm at a speed of 50 mL/min; after the dropwise addition is finished, putting the mixed solution into a 90 ℃ oven for curing for 5 hours; after the curing is finished, filtering out precipitates, and drying for 60min at 100 ℃ after washing; and drying to obtain the petal-shaped micro-nano basic magnesium carbonate flame retardant.
The flame retardant effect of the flame retardant is tested as follows:
the basic magnesium carbonate is doped into the electrospinning liquid of cellulose acetate by 5 wt% to spin a film with the width of 15mm and the thickness of 0.1mm, and the combustion rate of the composite film is 475.2 mm/min by adopting a horizontal combustion method, so that the smoke generation amount is extremely small, and the smoke suppression effect is obvious.
Example 5
The preparation method of the flame retardant comprises the following steps:
respectively preparing 200mL of sodium bicarbonate aqueous solution (1.5mol/L) and 200mL of magnesium chloride hexahydrate solution (1.5mol/L), and dropwise adding the sodium carbonate aqueous solution into the magnesium chloride hexahydrate solution which is stirred at a constant speed of 1000rpm at the speed of 1 mL/min; after the dropwise addition is finished, putting the mixed solution into a 50 ℃ oven for curing for 5 hours; after the curing is finished, filtering out precipitates, and drying for 60min at 100 ℃ after washing; and drying to obtain the petal-shaped micro-nano basic magnesium carbonate flame retardant.
The flame retardant effect of the flame retardant is tested as follows:
the basic magnesium carbonate is doped into the electrospinning liquid of cellulose acetate by 5 wt% to spin a film with the width of 15mm and the thickness of 0.1mm, and the combustion rate of the composite film is measured by adopting a horizontal combustion method to be 484.3 mm/min, the smoke generation amount is extremely small, and the smoke suppression effect is obvious.
Example 6
The preparation method of the flame retardant comprises the following steps:
respectively preparing 200mL of potassium bicarbonate aqueous solution (0.1mol/L) and 200mL of magnesium chloride hexahydrate solution (1.5mol/L), and dropwise adding the sodium bicarbonate aqueous solution into the magnesium chloride hexahydrate solution which is stirred at a constant speed of 1000rpm at the speed of 1 mL/min; after the dropwise addition is finished, placing the mixed solution in a 50 ℃ oven for curing for 5 hours; after the curing is finished, filtering out precipitates, and drying for 60min at 100 ℃ after washing; and drying to obtain the petal-shaped micro-nano basic magnesium carbonate flame retardant.
The flame retardant effect of the flame retardant is tested as follows:
the basic magnesium carbonate is doped into the electrospinning liquid of cellulose acetate by 5 wt% to spin a film with the width of 15mm and the thickness of 0.1mm, and the combustion rate of the composite film is measured by adopting a horizontal combustion method to be 473.9 mm/min, the smoke generation amount is extremely small, and the smoke suppression effect is obvious.
Example 7
The preparation method of the flame retardant comprises the following steps:
respectively preparing 200mL of sodium carbonate aqueous solution (0.9mol/L) and 200mL of magnesium chloride hexahydrate solution (0.6mol/L), and dropwise adding the sodium carbonate aqueous solution into the magnesium chloride hexahydrate solution which is stirred at a constant speed of 1000rpm at a speed of 50 mL/min; after the dropwise addition is finished, putting the mixed solution into a 90 ℃ oven for curing for 5 hours; after the curing is finished, filtering out precipitates, and drying for 60min at 50 ℃ after washing; and drying to obtain the petal-shaped micro-nano basic magnesium carbonate flame retardant.
The flame retardant effect of the flame retardant is tested as follows:
the basic magnesium carbonate is doped into the electrospinning liquid of cellulose acetate by 5 wt% to spin a film with the width of 15mm and the thickness of 0.1mm, and the combustion rate of the composite film is measured by adopting a horizontal combustion method to be 468.3 mm/min, the smoke generation amount is extremely small, and the smoke suppression effect is obvious.
Example 8
The preparation method of the flame retardant comprises the following steps:
respectively preparing 200mL of sodium carbonate aqueous solution (1.3mol/L) and 200mL of magnesium chloride hexahydrate solution (0.7mol/L), and dropwise adding the sodium carbonate aqueous solution into the magnesium chloride hexahydrate solution which is stirred at a constant speed of 400rpm at a speed of 10 mL/min; after the dropwise addition is finished, putting the mixed solution into an oven at 80 ℃ for curing for 2 hours; after the curing is finished, filtering out precipitates, and drying at 80 ℃ for 60min after washing; and drying to obtain the petal-shaped micro-nano basic magnesium carbonate flame retardant.
The flame retardant effect of the flame retardant is tested as follows:
the basic magnesium carbonate is doped into the electrospinning liquid of cellulose acetate by 5 wt% to spin a film with the width of 15mm and the thickness of 0.1mm, and the combustion rate of the composite film is measured by adopting a horizontal combustion method to be 473.9 mm/min, the smoke generation amount is extremely small, and the smoke suppression effect is obvious.
Example 9
The preparation method of the flame retardant comprises the following steps:
respectively preparing 200mL of sodium carbonate aqueous solution (0.7mol/L) and 200mL of magnesium chloride hexahydrate solution (1.2mol/L), and dropwise adding the sodium carbonate aqueous solution into the magnesium chloride hexahydrate solution which is stirred at a constant speed of 500rpm at the speed of 10 mL/min; after the dropwise addition is finished, putting the mixed solution into a 70 ℃ oven for curing for 2 hours; after the curing is finished, filtering out precipitates, and drying for 60min at 70 ℃ after washing; and drying to obtain the petal-shaped micro-nano basic magnesium carbonate flame retardant.
The flame retardant effect of the flame retardant is tested as follows:
the basic magnesium carbonate is doped into the electrospinning liquid of cellulose acetate by 5 wt% to spin a film with the width of 15mm and the thickness of 0.1mm, and the combustion rate of the composite film is 486.1 mm/min by adopting a horizontal combustion method, so that the smoke generation amount is extremely small, and the smoke suppression effect is obvious.
Example 10
The preparation method of the flame retardant comprises the following steps:
respectively preparing 200mL of sodium carbonate aqueous solution (1mol/L) and 200mL of magnesium chloride hexahydrate solution (1.2mol/L), and dropwise adding the sodium carbonate aqueous solution into the magnesium chloride hexahydrate solution which is uniformly stirred at 700rpm at the speed of 30 mL/min; after the dropwise addition is finished, putting the mixed solution into a 60 ℃ oven for curing for 2 hours; after the curing is finished, filtering out precipitates, and drying for 30min at 60 ℃ after washing; and drying to obtain the petal-shaped micro-nano basic magnesium carbonate flame retardant.
The flame retardant effect of the flame retardant is tested as follows:
the basic magnesium carbonate is doped into the electrospinning liquid of cellulose acetate by 5 wt% to spin a film with the width of 15mm and the thickness of 0.1mm, and the combustion rate of the composite film is measured by adopting a horizontal combustion method to be 469.3 mm/min, the smoke generation amount is extremely small, and the smoke suppression effect is obvious.
Example 11
The preparation method of the flame retardant comprises the following steps:
respectively preparing 200mL of sodium carbonate aqueous solution (1mol/L) and 200mL of magnesium chloride hexahydrate solution (1mol/L), and dropwise adding the sodium carbonate aqueous solution into the magnesium chloride hexahydrate solution which is uniformly stirred at 800rpm at the speed of 10 mL/min; after the dropwise addition is finished, putting the mixed solution into an oven at 80 ℃ for curing for 2 hours; after the curing is finished, filtering out precipitates, and drying for 30min at 60 ℃ after washing; and drying to obtain the petal-shaped micro-nano basic magnesium carbonate flame retardant.
The flame retardant effect of the flame retardant is tested as follows:
the basic magnesium carbonate is doped with 5 wt% of cellulose acetate in electrospinning liquid to spin a film with the width of 15mm and the thickness of 0.1mm, and a horizontal combustion method is adopted to measure that the combustion rate of the composite film is 452.6 mm/min, the smoke generation amount is extremely small, the smoke suppression effect is obvious, and the flame retardant effect is best.
Comparative example 1:
a film having a width of 15mm and a thickness of 0.1mm was spun from an electrospinning solution of only cellulose acetate without adding a basic magnesium carbonate flame retardant, and the combustion rate of the film was measured by a horizontal combustion method to be 1464.8 mm/min, accompanied by the generation of a large amount of smoke.
Comparative example 2:
the injection rate of the sodium carbonate is increased to 100mL/min, the rest conditions are maintained to be the same as those of the example 1, the petal-shaped basic magnesium carbonate cannot be obtained, and the flame retardant test effect is poor.
Comparative example 3:
the aging temperature was lowered to 30 ℃ and the remaining conditions were maintained as in example 1, whereby petal-type basic magnesium carbonate could not be obtained and the flame retardant effect was not good.
Comparative example 4:
the aging time is reduced to 10min, and the rest conditions are maintained to be the same as those of the example 1, so that the petal-shaped basic magnesium carbonate cannot be obtained, and the flame retardant effect is poor.
The above embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and various changes may be made in the above embodiments of the present invention. All simple and equivalent changes and modifications made according to the claims and the content of the specification of the present application fall within the scope of the claims of the present patent application. The invention has not been described in detail in order to avoid obscuring the invention.
Claims (2)
1. A preparation method of a micro-nano basic magnesium carbonate flame retardant is characterized by comprising the following steps:
1) dropwise adding 1mol/L sodium carbonate aqueous solution into 1mol/L magnesium chloride hexahydrate aqueous solution which is uniformly stirred at 800rpm at the speed of 10 mL/min;
2) putting the mixed solution obtained in the step 1) into an oven at 80 ℃ for curing for 2 hours;
3) further filtering and washing the mixed solution obtained in the step 2), and drying for 30min at 60 ℃ to prepare the micro-nano basic magnesium carbonate flame retardant with the chemical formula of Mg5(CO3)4(OH)2·4H2O。
2. The micro-nano basic magnesium carbonate flame retardant prepared by the preparation method of claim 1 is a micro-particle with a petal-shaped spherical structure, and the micro-particle is formed by stacking multiple layers of petal-shaped nanosheets and has the size of 30-50 microns.
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