CN113912907A - Boron nitride and zinc oxide nano composite flame retardant and preparation method thereof - Google Patents
Boron nitride and zinc oxide nano composite flame retardant and preparation method thereof Download PDFInfo
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- CN113912907A CN113912907A CN202111158073.XA CN202111158073A CN113912907A CN 113912907 A CN113912907 A CN 113912907A CN 202111158073 A CN202111158073 A CN 202111158073A CN 113912907 A CN113912907 A CN 113912907A
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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- C08K2003/2224—Magnesium hydroxide
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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- C08K3/00—Use of inorganic substances as compounding ingredients
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Abstract
The invention relates to a boron nitride and zinc oxide nano composite flame retardant and a preparation method thereof, belonging to the technical field of nano materials. The nanometer composite fire retardant of boron nitride and zinc oxide of the invention is prepared by boron nitride and zinc oxide with a mechanochemical method; in the process of mixed mechanochemical modification of boron nitride and zinc oxide, zinc oxide particles and the stripped boron nitride sheet layer are subjected to mechanochemical reaction while being subjected to physical adsorption, so that stable boron nitride-zinc oxide nano composite particles are formed, the boron nitride sheet layer is prevented from being stacked again and zinc oxide particles are prevented from agglomerating, and a foundation is laid for further application of a nano flame retardant in a polymer and preparation of a polymer nano composite flame retardant material.
Description
Technical Field
The invention relates to a boron nitride and zinc oxide nano composite flame retardant and a preparation method thereof, belonging to the technical field of nano materials.
Background
To improve flame retardanceThe flame retardant efficiency of the agent can be compounded with different flame retardants, wherein an in-situ growth method is an effective method for preparing the compound flame retardant, and the in-situ growth method can be used for preparing a core-shell type compound flame retardant Al (OH) consisting of an aluminum hydroxide core and an aluminum polyphosphate shell3@AlPO4However, the composite particle structure prepared by the method can only reach the micron scale, the post-treatment time of the preparation process is long, the preparation efficiency of the flame retardant is low, and the addition amount of the flame retardant is large when the flame retardant composite material is prepared.
The mechanochemical method is a method widely used for modifying inorganic particles, and changes the physical and chemical structures of the inorganic particles by using mechanical energy generated between media. In the flame retardant field, a mechanochemical method is also used for preparing novel nano composite flame retardant, two substances which do not react at normal temperature can be subjected to chemical action through mechanochemical action, the binding force is increased, the particles are mutually adsorbed to form composite powder, and a specific structure can be introduced onto a nano material through mechanochemical reaction to prepare the modified nano composite flame retardant containing the flame retardant functional group.
Boron nitride and zinc oxide are often used as flame-retardant synergists in halogen-free flame-retardant composite materials, the boron nitride can improve the thermal stability of the composite materials, the zinc oxide can improve the char formation of the composite materials, but unmodified boron nitride and zinc oxide often agglomerate and have poor compatibility with a matrix, the improvement of the flame-retardant property of the composite materials is limited when the boron nitride and the zinc oxide are used alone, the self-extinguishing property is still poor, and the ideal UL-94 combustion level cannot be reached, so that the improvement is urgently needed, and the flame retardant can exert a better flame-retardant effect. The mechanochemical modification time required for preparing the composite flame retardant is long, the energy consumption is high, the preparation process is complex, the yield is low, and the preparation of a large amount of the composite flame retardant cannot be carried out. The mechanochemical process in the invention is simple, the operation is easy, the preparation efficiency of the flame retardant is higher, and the addition amount in the preparation process of the composite material is less. At present, no literature reports a technology for realizing the nanometer composite flame retardant of boron nitride and zinc oxide by using a mechanochemical method.
Disclosure of Invention
The invention aims to solve the problem of low flame retardant efficiency of the existing inorganic flame retardant, and provides a boron nitride and zinc oxide nano composite flame retardant and a preparation method thereof.
The purpose of the invention is realized by the following technical scheme.
A boron nitride and zinc oxide nano composite flame retardant is a stable embedded two-dimensional lamellar structure prepared by a mechanochemical method from boron nitride and zinc oxide; the mass of the boron nitride accounts for 25-75% of the total mass. The total mass is the sum of the mass of boron nitride and the mass of zinc oxide;
the boron nitride comprises hexagonal boron nitride and nano hexagonal boron nitride, and the zinc oxide comprises micro zinc oxide and nano zinc oxide.
A preparation method of the boron nitride and zinc oxide nano composite flame retardant comprises the following steps: drying boron nitride and zinc oxide in an oven, uniformly mixing, and placing into a mechanochemical modification container; then putting the modified medium; after omnibearing mechanochemical modification is carried out for 1-5 hours, screening to obtain a faint yellow boron nitride zinc oxide nano composite flame retardant;
the mixture of the dried boron nitride and the dried zinc oxide is called modified powder; the mass ratio of the modified powder to the modified medium is 1: 10-1: 20, and the modified powder and the modified medium account for 20-40% of the volume of the modified container.
The process equipment for preparing the powder is omnibearing mechanochemical modification equipment, and the process conditions of omnibearing modification are set as follows:
the process 1 is that the chassis revolves at intervals of 30-60 degrees, the rotation is maintained for 5-50 minutes after the rotation is finished, and the chassis autorotation process is operated during the maintenance period;
the process 2 is that the chassis continuously revolves at an angular speed of 30-90 DEG/min, and the chassis autorotation process is operated in the period;
the process 3 is a mixed arrangement of the process 1 and the process 2 in any mode.
The chassis autorotation process comprises the steps that the chassis rotates clockwise for 1-4 minutes, stops for 1 minute, rotates anticlockwise for 1-4 minutes, stops for 1 minute and is a cycle, and the rotating speed is 500-800 rpm.
Advantageous effects
1. The invention uses a mechanochemical method to prepare the boron nitride and zinc oxide nano composite flame retardant, utilizes mechanical energy to weaken the interlayer acting force of the boron nitride, so that a boron nitride sheet layer gradually slides and peels, simultaneously, the particle size of zinc oxide is reduced when the zinc oxide is subjected to impact force and pressure, and the peeled boron nitride sheet layer and zinc oxide particles are subjected to physical adsorption and mechanochemical reaction to form the flame retardant with a stable nano composite structure.
2. The method has the advantages of simple process, easily obtained raw materials, low cost, suitability for industrial application, no organic solvent and environmental friendliness. The boron nitride and zinc oxide nano composite flame retardant prepared by a mechanochemical method can enhance the nano effect when being applied to a polymer nano composite material, can obviously improve the thermal stability and the flame retardant property of the composite material, has excellent smoke suppression and attenuation effects, and lays a foundation for further application of the flame retardant in a polymer and preparation of the polymer nano composite flame retardant.
Drawings
FIG. 1 is an XRD spectrogram of boron nitride, zinc oxide and boron nitride zinc oxide nano composite flame retardant;
FIG. 2 is a TEM picture of the prepared boron nitride zinc oxide nano composite flame retardant.
Detailed Description
The invention is further illustrated by the following examples in conjunction with the accompanying drawings, which are not intended to limit the scope of the invention.
Comparative example 1
The invention relates to a boron nitride zinc oxide nano composite flame retardant which is prepared by grinding and mixing boron nitride and zinc oxide, and comprises the following components in percentage by mass: 50% of boron nitride and 50% of zinc oxide.
Drying 9.37g of boron nitride and 9.37g of zinc oxide (the mass ratio is 1:1) in an oven, grinding and uniformly mixing in a mortar, and sieving to obtain the boron nitride and zinc oxide composite flame retardant.
Example 1
The boron nitride zinc oxide nano composite flame retardant disclosed by the invention is a stable embedded two-dimensional lamellar structure prepared from nano hexagonal boron nitride and nano zinc oxide by a mechanochemical method, as shown in figure 2; the mass percentage is as follows: 50% of boron nitride and 50% of zinc oxide.
The preparation method comprises the following steps: drying 9.37g of boron nitride and 9.37g of zinc oxide (the mass ratio is 1:1) in an oven, uniformly mixing, and placing into a modification container; 281.25g of modified medium is placed in a modification container, the mass ratio of the modified powder to the modified medium is controlled to be 1:15, and the modified powder and the modified medium account for 25% of the volume of the modification container; setting all-dimensional modification process conditions: the chassis continuously revolves at an angular speed of 90 DEG/min, and a chassis rotation process is operated during the revolution; the chassis rotation process comprises the steps of rotating the chassis clockwise for 4 minutes, stopping the rotation for 1 minute, rotating the chassis anticlockwise for 4 minutes, stopping the rotation for 1 minute to form a cycle, and enabling the rotation speed to be 500 rpm. And after omnibearing modification for 3 hours, sieving to obtain the boron nitride and zinc oxide nano composite flame retardant.
As shown in fig. 1, from the XRD spectrum of boron nitride, 2 θ ═ 26.7 ° is the (002) characteristic diffraction peak of boron nitride; from an XRD spectrogram of the boron nitride zinc oxide nano composite flame retardant, the intensity of a diffraction peak at 26.7 degrees 2 theta is greatly reduced, which indicates that the layered structure of boron nitride is damaged in the modification process and the lamella is stripped; from TEM photographs of the boron nitride zinc oxide nanocomposite flame retardant, it was found that the exfoliated boron nitride lamella and the zinc oxide particles were adsorbed to each other and formed stable nanocomposite particles.
Example 2
The invention relates to a boron nitride zinc oxide nano composite flame retardant which is prepared by a hexagonal boron nitride and nano zinc oxide mechanochemical method, and comprises the following components in percentage by mass: 75% of boron nitride and 25% of zinc oxide.
Drying 10.71g of boron nitride and 3.57g of zinc oxide (the mass ratio is 3:1) in an oven, uniformly mixing, and placing into a modification container; 285.71g of modified medium is placed in a modification container, the mass ratio of the modified powder to the modified medium is 1:20, and the modified powder and the modified medium together account for 20% of the volume of the modification container; setting all-dimensional modification process conditions: revolving the base plate at intervals of 45 degrees, maintaining for 6 minutes after the rotation is finished, and operating the base plate autorotation process during the maintenance period; the rotation process of the chassis comprises the steps of clockwise rotation of the chassis for 3 minutes, stopping for 1 minute, anticlockwise rotation for 3 minutes, stopping for 1 minute as a cycle, and the rotation speed of 800 rpm. And carrying out omnibearing modification for 4h, and sieving to obtain the boron nitride zinc oxide nano composite flame retardant.
Example 3
The invention relates to a boron nitride zinc oxide nano composite flame retardant which is prepared by a nano hexagonal boron nitride and micro zinc oxide mechanochemical method, and comprises the following components in percentage by mass: 25% of boron nitride and 75% of zinc oxide.
Drying 9.09g of boron nitride and 27.27g of zinc oxide (the mass ratio is 1:3) in an oven, uniformly mixing, and placing into a modification container; 363.63g of modified medium is placed in a modification container, the mass ratio of the modified powder to the modified medium is 1:10, and the modified powder and the modified medium together account for 40% of the volume of the modification container; setting all-dimensional modification process conditions: the condition 1 is that the chassis revolves at intervals of 30 degrees, the rotation is maintained for 10 minutes after the rotation is finished, and the chassis autorotation process is operated during the maintenance period; the condition 2 is that the chassis continuously revolves at an angular speed of 60 degrees/minute, and a chassis rotation process is operated during the revolution; the conditions 1 and 2 are alternated after running for 20 minutes; the chassis rotation process comprises the steps of rotating the chassis clockwise for 4 minutes, stopping the rotation for 1 minute, rotating the chassis anticlockwise for 4 minutes, stopping the rotation for 1 minute to form a cycle, and enabling the rotation speed to be 600 rpm. And carrying out omnibearing modification for 4h, and sieving to obtain the boron nitride zinc oxide nano composite flame retardant.
Example 4
The invention relates to a boron nitride zinc oxide nano composite flame retardant which is prepared by a nano hexagonal boron nitride and nano zinc oxide mechanochemical method, and comprises the following components in percentage by mass: 50% of boron nitride and 50% of zinc oxide.
Drying 14.28g of unmodified synthetic boron nitride and 14.28g of zinc oxide (the mass ratio is 1:1) in an oven, uniformly mixing, and placing into a modification container; 571.42g of modified medium is placed in a modification container, the mass ratio of the modified powder to the modified medium is 1:20, and the modified powder and the modified medium together account for 40% of the volume of the modification container; setting all-dimensional modification process conditions: the chassis continuously revolves at an angular speed of 45 degrees/minute, and a chassis rotation process is operated in the period; the rotation process of the chassis comprises the steps of clockwise rotation of the chassis for 4 minutes, stopping for 1 minute, anticlockwise rotation for 4 minutes, stopping for 1 minute to form a cycle, and the rotation speed is 800 rpm. And after omnibearing modification for 5 hours, sieving to obtain the boron nitride zinc oxide nano composite flame retardant.
In order to test the flame retardant effect of the boron nitride zinc oxide nano composite flame retardant obtained in each example, the boron nitride zinc oxide nano composite flame retardant, the ethylene-vinyl acetate copolymer and the magnesium hydroxide were prepared into a flame retardant nano composite material, wherein the percentage of the flame retardant (magnesium hydroxide and boron nitride zinc oxide nano composite flame retardant) was 60%, and the percentage of the boron nitride zinc oxide nano composite flame retardant was 5%, 5%, 4% and 3%, respectively. The prepared nanocomposite was subjected to limiting oxygen index LOI, UL-94 vertical combustion, cone calorimeter and smoke density tests, and the test results are as follows.
The above detailed description is intended to illustrate the objects, aspects and advantages of the present invention, and it should be understood that the above detailed description is only exemplary of the present invention and is not intended to limit the scope of the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (4)
1. A boron nitride and zinc oxide nanometer composite flame retardant and a preparation method thereof are characterized in that: is prepared from boron nitride and zinc oxide by mechanochemical method, wherein the boron nitride accounts for 25-75% of the total mass of the boron nitride and the zinc oxide.
2. The preparation method of the boron nitride and zinc oxide nano composite flame retardant of claim 1 is characterized by comprising the following steps: the method comprises the following specific steps:
drying boron nitride and zinc oxide in an oven, mixing uniformly and then placing into a modification container; putting a modified medium into a modification container, wherein the mass ratio of the modified powder to the modified medium is 1: 10-1: 20, and the modified powder and the modified medium account for 20-50% of the volume of the ball milling container; setting an omnibearing modification process which is divided into any one of three processes; the condition 1 is that the chassis revolves at intervals of 30-60 degrees, the rotation is maintained for 5-50 minutes after the rotation is finished, and the chassis autorotation process is operated during the maintenance period; the condition 2 is that the chassis continuously revolves at an angular speed of 30 DEG/min-90 DEG/min, and a chassis autorotation process is operated in the period; condition 3 is that condition 1 is mixed with condition 2 in an arbitrary manner; and after all-dimensional modification for 1-5 h, sieving to obtain the boron nitride zinc oxide nano composite flame retardant.
3. The method of claim 2, wherein: the chassis autorotation process comprises the steps that the chassis rotates clockwise for 1-4 minutes, stops for 1 minute, rotates anticlockwise for 1-4 minutes, stops for 1 minute, and takes the rotation as a cycle with the rotation speed of 500-800 rpm.
4. The method of claim 2, wherein: the boron nitride in the above steps comprises hexagonal boron nitride and nano hexagonal boron nitride, and the zinc oxide comprises: micron zinc oxide or nanometer zinc oxide.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20100114865A (en) * | 2010-09-28 | 2010-10-26 | 안승우 | Non-combustible inorganic materials are powdered or melted to nano size (10 ~ 20nm) standard, mixed with metasilicate and other optical thermoplastic resins (PMMA, PE, PS, PETG) and substituted (ionized) Design of technology to give permeability, high transparency and high strength nonflammable (flame retardant, flameproof) function (invention) |
| JP2015214639A (en) * | 2014-05-09 | 2015-12-03 | Dic株式会社 | Composite particle, method for producing the same and resin composition |
| CN111484670A (en) * | 2019-12-20 | 2020-08-04 | 四川鑫达企业集团有限公司 | Halogen-free flame-retardant low-floating-fiber reinforced polypropylene composite material and preparation method thereof |
| CN111484702A (en) * | 2019-12-20 | 2020-08-04 | 四川鑫达企业集团有限公司 | Low-shrinkage precipitation-resistant halogen-free flame-retardant ABS (acrylonitrile butadiene styrene) composite material and preparation method thereof |
| CN112029346A (en) * | 2020-07-31 | 2020-12-04 | 国网山东省电力公司电力科学研究院 | High-flame-retardance tracking-resistant and electric-corrosion-resistant fluorocarbon coating and preparation method and application thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20100114865A (en) * | 2010-09-28 | 2010-10-26 | 안승우 | Non-combustible inorganic materials are powdered or melted to nano size (10 ~ 20nm) standard, mixed with metasilicate and other optical thermoplastic resins (PMMA, PE, PS, PETG) and substituted (ionized) Design of technology to give permeability, high transparency and high strength nonflammable (flame retardant, flameproof) function (invention) |
| JP2015214639A (en) * | 2014-05-09 | 2015-12-03 | Dic株式会社 | Composite particle, method for producing the same and resin composition |
| CN111484670A (en) * | 2019-12-20 | 2020-08-04 | 四川鑫达企业集团有限公司 | Halogen-free flame-retardant low-floating-fiber reinforced polypropylene composite material and preparation method thereof |
| CN111484702A (en) * | 2019-12-20 | 2020-08-04 | 四川鑫达企业集团有限公司 | Low-shrinkage precipitation-resistant halogen-free flame-retardant ABS (acrylonitrile butadiene styrene) composite material and preparation method thereof |
| CN112029346A (en) * | 2020-07-31 | 2020-12-04 | 国网山东省电力公司电力科学研究院 | High-flame-retardance tracking-resistant and electric-corrosion-resistant fluorocarbon coating and preparation method and application thereof |
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