CN113912907B - 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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- CN113912907B CN113912907B CN202111158073.XA CN202111158073A CN113912907B CN 113912907 B CN113912907 B CN 113912907B CN 202111158073 A CN202111158073 A CN 202111158073A CN 113912907 B CN113912907 B CN 113912907B
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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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- 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
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- C08K2003/2224—Magnesium hydroxide
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- C08K2003/2296—Oxides; Hydroxides of metals of zinc
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- C08K2003/385—Binary compounds of nitrogen with boron
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Abstract
The invention relates to a boron nitride and zinc oxide nanocomposite flame retardant and a preparation method thereof, belonging to the technical field of nano materials. The nano composite flame retardant of the boron nitride and the zinc oxide is prepared from the boron nitride and the zinc oxide by a mechanochemical method; in the process of mixing and mechanochemical modification of boron nitride and zinc oxide, the zinc oxide particles and the stripped boron nitride sheets are subjected to mechanochemical reaction while physical adsorption is carried out, so that stable boron nitride-zinc oxide nano composite particles are formed, re-stacking of the boron nitride sheets and agglomeration of the zinc oxide particles are avoided, and a foundation is laid for further application of the nano flame retardant in polymers and preparation of polymer nano composite flame retardant materials.
Description
Technical Field
The invention relates to a boron nitride and zinc oxide nanocomposite flame retardant and a preparation method thereof, belonging to the technical field of nano materials.
Background
In order to improve the flame retardant efficiency of the flame retardant, different flame retardants can be compounded, wherein an in-situ growth method is an effective method for preparing the compound flame retardant, and the in-situ growth method is reported in literature to be capable of compounding a core-shell compound flame retardant Al (OH) consisting of an aluminum hydroxide core and an aluminum polyphosphate shell 3 @AlPO 4 However, the composite particle structure prepared by the method can only reach the micrometer scale, the post-treatment time consumption 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.
Mechanochemical is a widely used method for modifying inorganic particles, which uses mechanical energy generated between media to change the physical and chemical structures of inorganic particles. In the flame-retardant field, a mechanochemical method is also used for preparing a 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 of the substances is increased to enable the particles to be mutually adsorbed to form composite powder, and a specific structure can be introduced onto a nano material through mechanochemical reaction to prepare the nano composite flame retardant containing flame-retardant functional group modification.
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 are often agglomerated, the compatibility with a matrix is poor, the flame retardant performance of the composite materials is improved only when the composite materials are used independently, the self-extinguishing property is still poor, and the ideal UL-94 combustion level cannot be achieved, so that improvement is urgently needed, and the flame retardant can exert better flame retardant effect. The mechanochemical modification time required by preparing the composite flame retardant is long, the energy consumption is large, the preparation process is complex, the yield is low, and the preparation cannot be carried out in a large amount. The preparation method has the advantages of simple mechanochemical process, easy operation, higher preparation efficiency of the flame retardant and less addition amount in the preparation process of the composite material. At present, no document reports on a technology for realizing the nano 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 nanocomposite flame retardant and a preparation method thereof.
The aim of the invention is achieved 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; the mass of the boron nitride is 25-75% of the total mass. The total mass is the sum of the mass of boron nitride and 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.
The 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 then placing into a mechanochemical modification container; then putting the modified medium; after being modified for 1-5 h by omnibearing mechanochemical modification, sieving to obtain a faint yellow boron nitride zinc oxide nano composite flame retardant;
the mixture of the dried boron nitride and 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 used for preparing the powder is omnibearing mechanochemical modification equipment, and omnibearing modification process conditions are set:
the technique 1 is that the chassis revolves at intervals of 30-60 degrees, and the rotation process of the chassis is operated for 5-50 minutes after the rotation is finished;
the process 2 is that the chassis continuously revolves at an angular speed of 30 degrees/min-90 degrees/min, and the chassis autorotation process is operated during the revolution period;
process 3 is a mixed arrangement of process 1 and process 2 in any manner.
The chassis rotation process is that the chassis rotates clockwise for 1-4 minutes, stops for 1 minute, rotates anticlockwise for 1-4 minutes, stops for 1 minute as a cycle, and the rotating speed is 500-800 rpm.
Advantageous effects
1. The invention uses mechanochemical method to prepare boron nitride and zinc oxide nano composite flame retardant, uses mechanical energy to weaken interlayer acting force of boron nitride, makes boron nitride sheet gradually slip and peel off, and reduces particle size when zinc oxide is impacted and pressed, and makes physical adsorption between peeled boron nitride sheet and zinc oxide particles and mechanochemical reaction to form stable flame retardant with 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 nanometer composite flame retardant of boron nitride and zinc oxide prepared by the mechanochemical method can enhance the nanometer effect when being applied to a polymer nanometer composite material, can obviously improve the thermal stability and flame retardant property of the composite material, has excellent smoke suppression and toxicity reduction effects, and lays a foundation for further application of the flame retardant in the polymer and preparation of the polymer nanometer composite flame retardant.
Drawings
FIG. 1 is an XRD spectrum of a boron nitride, zinc oxide and boron nitride zinc oxide nanocomposite flame retardant;
fig. 2 is a TEM photograph of the prepared boron nitride zinc oxide nanocomposite flame retardant.
Detailed Description
The invention is further described in connection with the following drawings and examples, 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 mixing uniformly 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 is shown in figure 2, and is a stable embedded two-dimensional lamellar structure prepared by a mechanochemical method from nano hexagonal boron nitride and nano zinc oxide; 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 then placing into a modification container; 281.25g of modifying medium is placed in a modifying container, the mass ratio of modifying powder to modifying medium is controlled to be 1:15, and the modifying powder and modifying medium account for 25% of the volume of the modifying container; setting all-round 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 is that the chassis rotates clockwise for 4 minutes, stops for 1 minute, rotates anticlockwise for 4 minutes, stops for 1 minute as a cycle, and the rotation speed is 500rpm. And carrying out omnibearing modification for 3 hours, and sieving to obtain the boron nitride and zinc oxide nanocomposite flame retardant.
As shown in fig. 1, from the XRD spectrum of boron nitride, 2θ=26.7° is a (002) characteristic diffraction peak of boron nitride; from the XRD spectrum of the boron nitride zinc oxide nano composite flame retardant, the intensity of a diffraction peak at 2 theta=26.7 degrees is greatly reduced, which indicates that the lamellar structure of the boron nitride is destroyed in the modification process and the lamellar layer is peeled off; from the TEM photograph of the boron nitride zinc oxide nanocomposite flame retardant, the exfoliated boron nitride platelet and zinc oxide particles adsorbed 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 then placing into a modification container; 285.71g of modified medium is placed in a modified container, the mass ratio of the modified powder to the modified medium is 1:20, and the modified powder and the modified medium occupy 20% of the volume of the modified container; setting all-round modification process conditions: the chassis revolves at intervals of 45 degrees, and maintains for 6 minutes after the rotation is finished, and a chassis rotation process is operated during the maintenance period; the chassis rotation process is that the chassis rotates clockwise for 3 minutes, stops for 1 minute, rotates anticlockwise for 3 minutes, stops for 1 minute as a cycle, and the rotation speed is 800rpm. And carrying out omnibearing modification for 4 hours, 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 micron 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 then placing into a modification container; 363.63g of modified medium is placed in a modified container, the mass ratio of modified powder to the modified medium is 1:10, and the modified powder and the modified medium occupy 40% of the volume of the modified container; setting all-round 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 completion of the rotation, and the chassis rotation process is operated during the maintenance period; condition 2 is that the chassis continuously revolves at an angular velocity of 60 °/min, during which the chassis rotation process is operated; conditions 1 and 2 were each run for 20 minutes and then alternated; the chassis rotation process is that the chassis rotates clockwise for 4 minutes, stops for 1 minute, rotates anticlockwise for 4 minutes, stops for 1 minute as a cycle, and the rotation speed is 600rpm. And carrying out omnibearing modification for 4 hours, 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.
14.28g of unmodified synthetic boron nitride and 14.28g of zinc oxide (the mass ratio is 1:1) are dried in an oven, and the mixture is placed into a modification container after being uniformly mixed; 571.42g of modified medium is placed in a modified container, the mass ratio of modified powder to the modified medium is 1:20, and the modified powder and the modified medium occupy 40% of the volume of the modified container; setting all-round modification process conditions: the chassis continuously revolves at an angular speed of 45 DEG/min, and a chassis rotation process is operated during the revolution; the chassis rotation process is that the chassis rotates clockwise for 4 minutes, stops for 1 minute, rotates anticlockwise for 4 minutes, stops for 1 minute as a cycle, and the rotation speed is 800rpm. And carrying out omnibearing modification for 5 hours, and sieving to obtain the boron nitride zinc oxide nano composite flame retardant.
To test the flame retardant effect of the boron nitride zinc oxide nanocomposite flame retardant obtained in each example, the flame retardant nanocomposite was prepared from the boron nitride zinc oxide nanocomposite flame retardant, an ethylene-vinyl acetate copolymer and magnesium hydroxide, wherein the percentage of the flame retardant (magnesium hydroxide and boron nitride zinc oxide nanocomposite flame retardant) was 60%, and the percentage of the boron nitride zinc oxide nanocomposite flame retardant was 5%,5%,4%,3%, respectively. The prepared nanocomposite was subjected to limiting oxygen index LOI, UL-94 vertical burning, cone calorimeter and smoke density test, and the test results are as follows.
While the foregoing is directed to embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (4)
1. A boron nitride and zinc oxide nano composite flame retardant is characterized in that: is prepared from boron nitride and zinc oxide by a mechanochemical method, wherein the boron nitride accounts for 25-75% of the total mass of the boron nitride and the zinc oxide; the preparation method comprises the following specific steps:
drying boron nitride and zinc oxide in an oven, uniformly mixing, and then placing into a modification container; placing a modifying medium into a modifying container, wherein the mass ratio of the modifying powder to the modifying medium is 1:10-1:20, and the modifying powder and the modifying medium account for 20% -50% of the volume of the ball milling container; setting an omnibearing modification process, wherein the omnibearing modification process is divided into any one of three processes; the condition 1 is that the chassis revolves at intervals of 30-60 degrees, and the chassis autorotation process is operated in the maintenance period after the rotation is completed for 5-50 minutes; condition 2 is that the chassis continuously revolves at an angular speed of 30 DEG/min-90 DEG/min, and the chassis autorotation process is operated during the revolution period; condition 3 is that condition 1 and condition 2 are mixed and arranged in any mode; after being modified for 1-5 h in all directions, the boron nitride zinc oxide nano composite flame retardant is obtained through sieving.
2. A method for preparing the boron nitride and zinc oxide nano composite flame retardant according to claim 1, which is characterized in that: drying boron nitride and zinc oxide in an oven, uniformly mixing, and then placing into a modification container; placing a modifying medium into a modifying container, wherein the mass ratio of the modifying powder to the modifying medium is 1:10-1:20, and the modifying powder and the modifying medium account for 20% -50% of the volume of the ball milling container; setting an omnibearing modification process, wherein the omnibearing modification process is divided into any one of three processes; the condition 1 is that the chassis revolves at intervals of 30-60 degrees, and the chassis autorotation process is operated in the maintenance period after the rotation is completed for 5-50 minutes; condition 2 is that the chassis continuously revolves at an angular speed of 30 DEG/min-90 DEG/min, and the chassis autorotation process is operated during the revolution period; condition 3 is that condition 1 and condition 2 are mixed and arranged in any mode; after being modified for 1-5 h in all directions, the boron nitride zinc oxide nano composite flame retardant is obtained through sieving.
3. The method for preparing the boron nitride and zinc oxide nano-composite flame retardant according to claim 2, which is characterized in that: the chassis rotation process is 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 process as a cycle, and the rotating speed is 500-800 rpm.
4. The method for preparing the boron nitride and zinc oxide nano-composite flame retardant according to claim 2, which is characterized in that: the boron nitride in the above steps comprises hexagonal boron nitride and nano hexagonal boron nitride, and the zinc oxide comprises: micro zinc oxide or nano zinc oxide.
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| 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) |
| JP6421448B2 (en) * | 2014-05-09 | 2018-11-14 | Dic株式会社 | Composite particle, method for producing the same, and resin composition |
| 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 |
| 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 |
| 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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