CN111689481A - Aluminum hypophosphite flame retardant ultrafine powder and preparation method and application thereof - Google Patents
Aluminum hypophosphite flame retardant ultrafine powder and preparation method and application thereof Download PDFInfo
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- CN111689481A CN111689481A CN202010596337.9A CN202010596337A CN111689481A CN 111689481 A CN111689481 A CN 111689481A CN 202010596337 A CN202010596337 A CN 202010596337A CN 111689481 A CN111689481 A CN 111689481A
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- 229910001377 aluminum hypophosphite Inorganic materials 0.000 title claims abstract description 81
- 239000003063 flame retardant Substances 0.000 title claims abstract description 35
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 239000000843 powder Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 36
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims abstract description 30
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims abstract description 26
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 13
- 230000004888 barrier function Effects 0.000 claims abstract description 11
- 239000002904 solvent Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- 239000005543 nano-size silicon particle Substances 0.000 claims abstract description 8
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 8
- 239000004033 plastic Substances 0.000 claims abstract description 6
- 229920003023 plastic Polymers 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 34
- 239000002002 slurry Substances 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 15
- 238000004321 preservation Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 7
- 238000003825 pressing Methods 0.000 claims description 4
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 11
- 238000005054 agglomeration Methods 0.000 abstract description 7
- 230000002776 aggregation Effects 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 5
- 230000000903 blocking effect Effects 0.000 abstract description 3
- 239000012752 auxiliary agent Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 32
- 230000000052 comparative effect Effects 0.000 description 8
- 239000003960 organic solvent Substances 0.000 description 4
- 238000011085 pressure filtration Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 229920001169 thermoplastic Polymers 0.000 description 2
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 239000003674 animal food additive Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- CQYBWJYIKCZXCN-UHFFFAOYSA-N diethylaluminum Chemical compound CC[Al]CC CQYBWJYIKCZXCN-UHFFFAOYSA-N 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012847 fine chemical Substances 0.000 description 1
- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000010137 moulding (plastic) Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000003444 phase transfer catalyst Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/165—Hypophosphorous acid; Salts thereof
-
- 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
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
-
- 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
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/16—Solid spheres
- C08K7/18—Solid spheres inorganic
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/32—Spheres
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- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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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
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K2201/003—Additives being defined by their diameter
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- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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Abstract
The invention discloses an aluminum hypophosphite fire retardant superfine powder, a preparation method and application thereof, wherein the fire retardant superfine powder adopts sodium hypophosphite and aluminum sulfate as raw materials, water is used as a solvent, nano silicon dioxide and/or nano titanium dioxide are added as a barrier medium before reaction, and the agglomeration of generated aluminum hypophosphite crystal particles is blocked, so that the particle size of synthesized aluminum hypophosphite reaches 0.5-5 mu m; the nanometer blocking material is adsorbed on the surface of aluminum hypophosphite crystal in the preparation process due to high surface activity, and the agglomeration of the aluminum hypophosphite flame retardant in the drying process is blocked, so that the superfine powder is obtained. The synthesized aluminum hypophosphite has the characteristics of small particle size, regular crystal form, no agglomeration and the like, the introduced nano barrier material is a rubber and plastic common auxiliary agent, the addition amount is very small, and the influence on the purity and the application of the aluminum hypophosphite can be almost ignored.
Description
Technical Field
The invention relates to preparation and application of ultrafine powder of an aluminum hypophosphite flame retardant, and belongs to the technical field of fine chemical engineering.
Background
The aluminum hypophosphite is a novel flame retardant, has good thermal stability, does not cause the decomposition of a polymer in processing, and does not influence a plastic molding composition; the aluminum hypophosphite-containing thermoplastic polymer is insoluble in water and nonvolatile under the common conditions for preparing and processing thermoplastic polymers, so that the application product has higher thermal stability and better mechanical properties in the processing process, and the polymer composition containing the aluminum hypophosphite has higher flame retardance.
Because the aluminum hypophosphite has high phosphorus content, has the advantages of small water solubility, large flame retardant effect and the like, when the aluminum hypophosphite is used on modified plastics such as PA6, PBT and the like, a very high flame retardant effect is obtained, when the aluminum hypophosphite is added into the PBT, the heat release rate and the heat generated during combustion are rapidly reduced, the char formation amount after combustion is increased, the flame retardant property reaches the UL94 standard V-0 level, and in addition, compared with the PBT flame retardant used at present in China, the flame retardant effect can be improved by 60 percent through experiments.
The synthesis of aluminum hypophosphite is now well established. The aluminum hypophosphite flame retardant can be synthesized by taking the sodium hypophosphite and the aluminum sulfate as raw materials under normal process conditions, but because the reaction is an inorganic double decomposition reaction, the produced aluminum hypophosphite crystal is easy to agglomerate to form irregular larger particles, so that the particle size is larger and the particle size distribution is wider.
Patent 201210302490.1 discloses a preparation scheme for synthesizing aluminum hypophosphite by using sodium hypophosphite and aluminum sulfate, but the aluminum hypophosphite prepared by the experimental scheme has the disadvantages of large particle size, irregular crystal form and the like. Patent 201710598598.2 discloses that uniform and stable nano aluminum hypophosphite is prepared by using a reverse microemulsion method, taking an organic solvent as a continuous phase, and forming a water-in-oil reverse phase solution of sodium hypophosphite, aluminum salt and a phase transfer catalyst aqueous solution in the organic phase. Patent 201811288251.9 and patent 201310601059.1 disclose that aluminum hypophosphite and a product are obtained by performing double decomposition reaction by using sodium hypophosphite and a water-soluble aluminum salt as raw materials, water as a solvent and diethyl aluminum hypophosphite and melamine cyanurate as seed crystals respectively.
In the process of synthesizing the aluminum hypophosphite superfine powder by taking the sodium hypophosphite and the water-soluble aluminum salt as raw materials, an organic solvent or a surfactant is introduced, so that the difficulty is caused in the separation and treatment of the byproduct water-soluble sodium salt in the preparation method; other substances are introduced as seed crystals, so that the problem of agglomeration of aluminum hypophosphite crystals cannot be solved, and the purity of the product is reduced. FIG. 6 is an electron microscope scan of a conventional aluminum hypophosphite flame retardant.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention adopts sodium hypophosphite and aluminum sulfate as raw materials, takes water as a solvent, adds nano silicon dioxide and nano titanium dioxide as a blocking medium before reaction, and blocks the agglomeration of generated aluminum hypophosphite crystal particles, so that the particle size of the synthesized aluminum hypophosphite reaches 0.5-5 mu m; the nanometer blocking material is adsorbed on the surface of aluminum hypophosphite crystal in the preparation process due to extremely high surface activity, and the agglomeration of the aluminum hypophosphite flame retardant in the drying process is blocked, so that the superfine powder is obtained.
The invention aims to provide an aluminum hypophosphite flame retardant ultrafine powder which is prepared from the following raw materials in parts by weight: 90-110 parts of sodium hypophosphite, 100 parts of aluminum sulfate, 300 parts of water and 200 parts of nano barrier material.
Wherein, the used sodium hypophosphite and aluminum sulfate are both industrial grade, the content of the sodium hypophosphite is more than 98.0 percent, and the content of the aluminum oxide of the aluminum sulfate is more than 16 percent.
The barrier material is any one or two of nano silicon dioxide and nano titanium dioxide.
Preferably, the feed additive is prepared from the following raw materials in parts by weight: 90 parts of sodium hypophosphite, 100 parts of aluminum sulfate, 200 parts of water and 0.4 part of nano barrier material.
The invention also aims to provide a preparation method of the aluminum hypophosphite flame retardant ultrafine powder, which comprises the following specific preparation steps:
(1) adding water serving as a solvent into a reaction container, starting stirring, adding a barrier material into a reaction kettle, uniformly stirring, adding aluminum sulfate, and heating to 60-80 ℃;
(2) adding sodium hypophosphite after aluminum sulfate is completely dissolved, stirring and heating to 80-100 ℃, then starting heat preservation, and continuously stirring and reacting for 4-6 h to generate aluminum hypophosphite slurry;
(3) and (3) carrying out filter pressing, washing and drying on the aluminum hypophosphite slurry to obtain the aluminum hypophosphite.
Preferably, the temperature in the step (1) is 60 ℃; the temperature in the step (2) is 100 ℃, and the stirring reaction time is 4 h.
The average particle size (D50) of the aluminum hypophosphite ultrafine powder is 0.5-5 mu m.
The invention further aims to provide the application of the aluminum hypophosphite flame retardant ultrafine powder as a flame retardant in rubber and plastic materials.
The invention has the beneficial effects that:
in the prior art, the synthesis process is simple, the particle size of the synthesized aluminum hypophosphite is large, the influence of the aluminum hypophosphite serving as a flame retardant on the mechanical property of plastics cannot be met, and a dispersing agent or an organic solvent is introduced, so that a byproduct sodium sulfate is polluted by the dispersing agent or the organic solvent and becomes dangerous waste. The synthesized aluminum hypophosphite has the characteristics of small particle size, regular crystal form, no agglomeration and the like, the introduced nano barrier material is a rubber and plastic common auxiliary agent, the addition amount is very small, and the influence on the purity and the application of the aluminum hypophosphite can be almost ignored.
Drawings
FIG. 1a is an electron microscope scan of an aluminum hypophosphite flame retardant of example 1 of the present invention;
FIG. 1b is a graph of particle size for the product of example 1 of the present invention;
FIG. 2 is a graph of particle size for the product of example 2 of the present invention;
FIG. 3 is a graph of particle size for the product of example 3 of the present invention;
FIG. 4 is a graph of particle size for the product of example 4 of the present invention;
FIG. 5 is a graph of particle size for the product of the comparative example;
FIG. 6 is an electron microscope scan of a conventional aluminum hypophosphite flame retardant.
Detailed Description
In order to better illustrate the technical solutions adopted by the present invention, the present invention is further described below with reference to the accompanying drawings and examples, but the embodiments of the present invention are not limited by the following examples.
The sodium hypophosphite and aluminum sulfate used in the examples are both technical grade.
EXAMPLE 1 preparation of Aluminohypophosphite ultrafine powder product A
90 parts of sodium hypophosphite, 100 parts of aluminum sulfate, 200 parts of water and 0.4 part of nano silicon dioxide.
The preparation method comprises the following steps: weighing the raw materials according to the specific weight, firstly adding 200 parts of water as a solvent into a reaction vessel, starting stirring, adding 0.4 part of nano silicon dioxide and 100 parts of aluminum sulfate into a reaction kettle, uniformly stirring, heating to 60 ℃, adding 90 parts of sodium hypophosphite after the aluminum sulfate is completely dissolved, stirring, heating to 100 ℃, then starting heat preservation, and continuously stirring for reaction for 4 hours to generate aluminum hypophosphite slurry. And (3) carrying out pressure filtration, washing and drying on the aluminum hypophosphite slurry to obtain spherical aluminum hypophosphite with the particle size of 3.8 microns. FIG. 1a is a scanning electron microscope image of the product of this example 1, and FIG. 1b is a particle size image of the product of this example 1.
EXAMPLE 2 preparation of Aluminohypophosphite ultrafine powder product B
100 parts of sodium hypophosphite, 120 parts of aluminum sulfate, 250 parts of water and 0.1 part of nano silicon dioxide.
The preparation method comprises the following steps: weighing the raw materials according to the specific weight, firstly adding 250 parts of water as a solvent into a reaction container, starting stirring, adding 0.1 part of nano silicon dioxide and 120 parts of aluminum sulfate into a reaction kettle, starting stirring, heating to 65 ℃, adding 100 parts of sodium hypophosphite after the aluminum sulfate is completely dissolved, stirring, heating to 90 ℃, starting heat preservation, and continuously stirring for reaction for 4.5 hours to generate aluminum hypophosphite slurry. And (3) carrying out pressure filtration, washing and drying on the aluminum hypophosphite slurry to obtain spherical aluminum hypophosphite with the particle size of 4.3 microns. FIG. 2 is a particle size diagram of the product of example 2.
EXAMPLE 3 preparation of Aluminohypophosphite ultrafine powder product C
105 parts of sodium hypophosphite, 115 parts of aluminum sulfate, 270 parts of water and 0.7 part of nano titanium dioxide.
The preparation method comprises the following steps: weighing the raw materials according to the proportion, firstly adding 270 parts of water as a solvent into a reaction container, starting stirring, adding 0.7 part of nano titanium dioxide and 115 parts of aluminum sulfate into a reaction kettle, starting stirring, heating to 75 ℃ until the aluminum sulfate is completely dissolved, adding sodium hypophosphite, stirring, heating to 95 ℃, starting heat preservation, and continuously stirring for reaction for 5 hours to generate aluminum hypophosphite slurry. And (3) carrying out filter pressing, washing and drying on the aluminum hypophosphite slurry to obtain spherical aluminum hypophosphite with the particle size of 4.6 microns. FIG. 3 is a particle size chart of the product of this example 3.
EXAMPLE 4 preparation of Aluminohypophosphite ultrafine powder product D
110 parts of sodium hypophosphite, 130 parts of aluminum sulfate, 300 parts of water and 1.0 part of nano titanium dioxide.
The preparation method comprises the following steps: weighing the raw materials according to the proportion, firstly adding 300 parts of water as a solvent into a reaction container, starting stirring, adding 1 part of nano titanium dioxide and 130 parts of aluminum sulfate into a reaction kettle, starting stirring, heating to 80 ℃, adding sodium hypophosphite after the aluminum sulfate is completely dissolved, stirring, heating to 80 ℃, starting heat preservation, and continuously stirring for reaction for 6 hours to generate aluminum hypophosphite slurry. And (3) carrying out pressure filtration, washing and drying on the aluminum hypophosphite slurry to obtain spherical aluminum hypophosphite with the particle size of 4.8 microns. FIG. 4 is a particle size chart of the product of this example 4.
EXAMPLE 5 preparation of comparative product (conventional preparation method)
The preparation method comprises the following steps: adding 250 parts of water as a solvent into a reaction vessel, starting stirring, adding 120 parts of aluminum sulfate into a reaction kettle, uniformly stirring, heating to 80 ℃, adding sodium hypophosphite, stirring, heating to 100 ℃, starting heat preservation, and continuously stirring for reaction for 4 hours to generate aluminum hypophosphite slurry. And (3) carrying out pressure filtration, washing and drying on the aluminum hypophosphite slurry to obtain spherical aluminum hypophosphite with the particle size of 11.15 microns. FIG. 5 is a graph showing the particle size of the comparative example.
Experimental examples comparative tests of products prepared according to the invention and comparative examples
1. The particle size of the aluminum hypophosphite superfine powder flame retardant prepared by the invention is tested with that of aluminum hypophosphite prepared by a comparison example, and the test data is shown in Table 1.
TABLE 1 comparison table of the application properties of the product of the present invention and the conventional products
| Test items | Product A | Product B | Product C | Product D | Comparative example | Test method |
| Particle size (50) μm | 2.278 | 3.618 | 4.288 | 4.605 | 11.15 | Laser particle size analyzer |
| Particle size (10) μm | 0.807 | 0.896 | 0.944 | 0.973 | 1.631 | Laser particle size analyzer |
| Particle size (100) μm | 23.37 | 27.47 | 31.55 | 20.73 | 53.12 | Laser particle size analyzer |
The data in Table 1 show that the aluminum hypophosphite ultrafine powder flame retardant prepared in the embodiment of the invention has smaller particle size and narrower distribution than the aluminum hypophosphite prepared in the comparative example.
2. Flame retardant performance test of aluminum hypophosphite superfine powder flame retardant prepared by the invention and aluminum hypophosphite prepared by a control example
The aluminum hypophosphite superfine powder obtained in the embodiments 1, 2, 3, 4 and 5 is respectively applied to TPU, the specific application proportion and the test result are shown in the following table, and it can be obtained from the table 2 that the flame retardant property of the product of the invention is obviously better than that of the product of the comparison example in the same formula system.
Table 2 comparison of the application properties of the products of examples 1, 2, 3, 4, 5 in TPU
| Product A | Product B | Product C | Product D | Comparative example | |
| TPU(2285)，％ | 90 | 90 | 90 | 90 | 90 |
| Aluminum hypophosphite ultrafine powder,% | 10 | 10 | 10 | 10 | 10 |
| UL94(1.6mm) | V-0 | V-0 | V-0 | V-0 | V-2 |
| LOI，％ | 30.5 | 30.2 | 30.4 | 30.2 | 29.5 |
Claims (9)
1. The aluminum hypophosphite flame retardant ultrafine powder is characterized by being prepared from the following raw materials in parts by weight:
the nano barrier material is one or two of nano silicon dioxide and nano titanium dioxide;
the preparation method comprises the following steps:
(1) adding water serving as a solvent into a reaction vessel, starting stirring, adding a barrier material into the reaction vessel, uniformly stirring, adding aluminum sulfate, and heating to 60-80 ℃;
(2) adding sodium hypophosphite after aluminum sulfate is completely dissolved, stirring and heating to 80-100 ℃, then starting heat preservation, and continuously stirring and reacting for 4-6 h to generate aluminum hypophosphite slurry;
(3) and (3) carrying out filter pressing, washing and drying on the aluminum hypophosphite slurry to obtain the aluminum hypophosphite.
2. The ultrafine powder as claimed in claim 1, wherein the sodium hypophosphite and the aluminum sulfate are both technical grade, the sodium hypophosphite content is greater than 98.0%, and the aluminum oxide content of the aluminum sulfate is greater than 16%.
3. The aluminum hypophosphite flame retardant ultrafine powder as claimed in claim 1, is prepared from the following raw materials in parts by weight:
4. the aluminum hypophosphite flame retardant ultrafine powder as recited in claim 1, wherein the nano barrier material is nano silica.
5. An aluminum hypophosphite flame retardant ultrafine powder as claimed in any one of claims 1 to 4, wherein the average particle size (D50) of the aluminum hypophosphite ultrafine powder is 0.5 to 5 μm.
6. The method for preparing the ultrafine powder of the aluminum hypophosphite flame retardant as set forth in any one of claims 1 to 5, characterized by comprising the following steps:
(1) adding water serving as a solvent into a reaction vessel, starting stirring, adding a barrier material into the reaction vessel, uniformly stirring, adding aluminum sulfate, and heating to 60-80 ℃;
(2) adding sodium hypophosphite after aluminum sulfate is completely dissolved, stirring and raising the temperature to 80-100 ℃, then starting heat preservation, and continuously stirring and reacting for 4-6 h to generate aluminum hypophosphite slurry;
(3) and (3) carrying out filter pressing, washing and drying on the aluminum hypophosphite slurry to obtain the aluminum hypophosphite.
7. The method as recited in claim 6, wherein the temperature in step (1) is 60 ℃.
8. The method for preparing the ultrafine powder of the aluminum hypophosphite flame retardant as recited in claim 6, wherein the temperature in the step (2) is 100 ℃, and the stirring reaction time is 4 hours.
9. The use of the aluminum hypophosphite flame retardant ultrafine powder as defined in any one of claims 1 to 5 as a flame retardant in rubber and plastic materials.
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