CN113308023A - High-dispersion and organic-affinity aluminum phosphite flame retardant and preparation method thereof - Google Patents
High-dispersion and organic-affinity aluminum phosphite flame retardant and preparation method thereof Download PDFInfo
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- HJJOHHHEKFECQI-UHFFFAOYSA-N aluminum;phosphite Chemical compound [Al+3].[O-]P([O-])[O-] HJJOHHHEKFECQI-UHFFFAOYSA-N 0.000 title claims abstract description 25
- 239000003063 flame retardant Substances 0.000 title claims abstract description 24
- 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 23
- 239000006185 dispersion Substances 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000002245 particle Substances 0.000 claims abstract description 21
- 239000003607 modifier Substances 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 13
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000000243 solution Substances 0.000 claims abstract description 10
- -1 phosphorous acid compound Chemical class 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 150000003839 salts Chemical class 0.000 claims abstract description 4
- 229910000951 Aluminide Inorganic materials 0.000 claims abstract description 3
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 3
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
- 238000000967 suction filtration Methods 0.000 claims abstract description 3
- 230000002708 enhancing effect Effects 0.000 claims abstract 2
- 239000000203 mixture Substances 0.000 claims abstract 2
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 238000001291 vacuum drying Methods 0.000 claims description 6
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 5
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims description 4
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical group [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 3
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 3
- JDRJCBXXDRYVJC-UHFFFAOYSA-N OP(O)O.N.N.N Chemical compound OP(O)O.N.N.N JDRJCBXXDRYVJC-UHFFFAOYSA-N 0.000 claims description 2
- 229910019142 PO4 Inorganic materials 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- 235000021355 Stearic acid Nutrition 0.000 claims description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 2
- 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 description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 2
- 239000010452 phosphate Substances 0.000 claims description 2
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 2
- 229920000053 polysorbate 80 Polymers 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 230000008569 process Effects 0.000 claims description 2
- 239000008117 stearic acid Substances 0.000 claims description 2
- NCPXQVVMIXIKTN-UHFFFAOYSA-N trisodium;phosphite Chemical group [Na+].[Na+].[Na+].[O-]P([O-])[O-] NCPXQVVMIXIKTN-UHFFFAOYSA-N 0.000 claims description 2
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 8
- 239000011159 matrix material Substances 0.000 abstract description 8
- 239000013078 crystal Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000005054 agglomeration Methods 0.000 abstract description 2
- 230000002776 aggregation Effects 0.000 abstract description 2
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 10
- 239000000843 powder Substances 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- 238000010521 absorption reaction Methods 0.000 description 9
- 230000004048 modification Effects 0.000 description 8
- 238000012986 modification Methods 0.000 description 8
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 7
- 229910052698 phosphorus Inorganic materials 0.000 description 7
- 239000011574 phosphorus Substances 0.000 description 7
- 230000004913 activation Effects 0.000 description 5
- XSAOTYCWGCRGCP-UHFFFAOYSA-K aluminum;diethylphosphinate Chemical compound [Al+3].CCP([O-])(=O)CC.CCP([O-])(=O)CC.CCP([O-])(=O)CC XSAOTYCWGCRGCP-UHFFFAOYSA-K 0.000 description 5
- 230000007935 neutral effect Effects 0.000 description 5
- 238000001914 filtration Methods 0.000 description 4
- 239000011256 inorganic filler Substances 0.000 description 4
- 229910003475 inorganic filler Inorganic materials 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 239000002131 composite material Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 239000004677 Nylon Substances 0.000 description 2
- 229910001377 aluminum hypophosphite Inorganic materials 0.000 description 2
- 239000004359 castor oil Substances 0.000 description 2
- 235000019438 castor oil Nutrition 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 150000002367 halogens Chemical class 0.000 description 2
- 238000009775 high-speed stirring Methods 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 229920001778 nylon Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000009736 wetting Methods 0.000 description 2
- 229920002302 Nylon 6,6 Polymers 0.000 description 1
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- CQYBWJYIKCZXCN-UHFFFAOYSA-N diethylaluminum Chemical compound CC[Al]CC CQYBWJYIKCZXCN-UHFFFAOYSA-N 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- AQSJGOWTSHOLKH-UHFFFAOYSA-N phosphite(3-) Chemical class [O-]P([O-])[O-] AQSJGOWTSHOLKH-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
Images
Classifications
-
- 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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-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
- C08K3/32—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
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
Abstract
The invention discloses a high-dispersion and organic-affinity aluminum phosphite flame retardant and a preparation method thereof, relates to the technical field of materials, and aims to provide an aluminum phosphite flame retardant with controllable granularity and good dispersibility, wherein the technical scheme provided by the invention is as follows: (1) dissolving phosphorous acid or salt thereof in an aqueous solution at a concentration of 30-50 wt%; (2) adding a modifier in the step (1), and uniformly stirring to obtain a mixture with the concentration of 1-5 wt%; the modifier is used for adjusting the particle size and enhancing the dispersibility; (3) adding an aluminide into the solution in the step (2) according to a stoichiometric ratio, and starting heating and stirring until the reaction is finished; (4) and carrying out suction filtration, washing to neutrality and drying on the obtained solution to obtain a product. The invention has the beneficial effects that: the aluminum phosphite crystal is prepared by taking the phosphorous acid compound and the aluminum compound as raw materials, the modifier is added to reduce the particle size, improve the particle dispersion degree and organic compatibility, solve the problem of incompatibility of agglomeration of the aluminum phosphite in an organic matrix, and reduce the cost.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a high-dispersion and organic affinity anhydrous aluminum phosphite flame retardant and a preparation method thereof.
Background
The phosphorus flame retardant has the characteristics of low toxicity, low smoke, low halogen and even no halogen, and has high efficiency, small dosage, great attention in the field of flame retardants and large development space. The phosphorus flame retardant is divided into an organic phosphorus flame retardant and an inorganic phosphorus flame retardant, the organic phosphorus flame retardant has the disadvantages of complex preparation process, high cost, large part volatility, poor thermal stability and pungent and toxic odor, and the inorganic phosphorus flame retardant has the advantages of simple and environment-friendly process, low components, good stability, high single use or compound efficiency and small dosage, but has the disadvantages of poor dispersibility, incompatibility with organic organisms and serious influence on the overall mechanical property of the material. The aluminum phosphite is a new inorganic phosphorus flame retardant in China, has the advantages of stability and nonflammability, high expansion rate and better flame retardant effect compared with a flame retardant of aluminum hypophosphite, and has the advantages of excellent flame retardant property, good color compatibility, no precipitation and reduced cost when compounded with diethyl aluminum hypophosphite (ADP).
Aluminum phosphite (Al)2(HPO3)3) As a flame retardant, the particle sizes required in different fields are different, the traditional flame retardant particle size control is further optimized by firstly adjusting the reaction rotating speed and then additionally arranging a three-ring mill or an air flow mill, the adjustment of the reaction rotating speed is generally realized by adjusting the stirring rotating speed and the stirring mode, the production requirement cannot be met, the cost of additionally arranging a crushing device is high, the energy consumption is high, and the production and processing cost is high; on the other hand, the aluminum phosphite belongs to inorganic filler, has poor dispersibility and compatibility in an organic matrix, and seriously influences the application mechanical property of the material.
Regarding aluminum phosphite, the patents CN104093663B and CN104364305B describe the preparation and application thereof in detail, and the particle size and compatibility thereof are not optimized; patent JP6842692B controls the particle size by controlling the particle size of the raw material aluminum hydroxide and the amount of water added, and the cost thereof increases greatly as the particle size of the aluminum hydroxide becomes smaller.
The patent provides a preparation method of an aluminum phosphite flame retardant with adjustable particle size and affinity with an organic matrix, and the preparation method is simple in preparation process and low in cost. Firstly, the particle size is controlled, and products with corresponding particle sizes are provided according to different requirements; secondly, the inorganic material is subjected to surface modification to improve the physical and chemical properties of the surface of the inorganic material, enhance the compatibility with resin materials and the dispersibility in a matrix, and improve the mechanical property and the comprehensive property of the material.
Disclosure of Invention
The invention aims to provide an aluminum phosphite flame retardant with adjustable particle size and affinity with an organic matrix and a preparation method thereof.
(1) Dissolving phosphorous acid or (salt thereof) in a certain aqueous solution;
the phosphorous acid or (salt thereof) in the step (1) is phosphorous acid (H)3PO3) And various phosphites thereof, e.g. sodium phosphite (Na)2HPO3) Ammonium phosphite ((NH)4)2HPO3) The concentration of the phosphorous acid and the salt solution thereof is preferably 30 to 50 wt%.
(2) Adding a modifier in the step (1), and uniformly stirring;
the modifier in the step (2) has the effects of inhibiting crystal growth and reducing the particle size of the product on the one hand, and changing the physical and chemical properties of the surface of the material on the other hand, so as to enhance the compatibility with the surface of the organic polymer and the dispersibility in the organic matrix, the modifier is an organic surface modifier, such as a coupling agent, a surfactant, organosilicon, unsaturated organic acid, organic oligomer, an organic intercalation modifier and a water-soluble polymer, including but not limited to sodium dodecyl sulfate, stearic acid, a silane coupling agent, phosphate ester, tween-80, polyvinyl alcohol, urea and the like, and the modifier is added by at least 1, wherein the total concentration is 1-5 wt% (based on the weight of the product).
(3) Adding aluminide into the solution according to a stoichiometric ratio, and starting heating and stirring;
the aluminum oxide includes aluminum oxide, aluminum salt, aluminum hydroxide, such as aluminum hydroxide (Al (OH)3) Alumina (Al)2O3) Aluminum sulfate (Al)2(SO4)3) Aluminum chloride (AlCl)3) Oxides and aluminum salts are added, the heating temperature is 40-100 ℃, preferably 80 ℃.
(4) Stirring until the reaction is finished;
the reaction time is 1h to 4h, preferably 2 h.
(5) And carrying out suction filtration, washing (to be neutral) and drying on the obtained solution to obtain the optimized aluminum phosphite with small particle size, good dispersion and affinity with the organic matrix.
Vacuum drying is adopted to reduce or even remove the crystal water, and the drying temperature is 150 ℃ and 240 ℃, and the preferred temperature is 220 ℃.
The invention has the beneficial effects that:
(1) the particle size of the aluminum phosphite obtained by the invention can be adjusted by changing the type and the dosage of the modifier, so that the aluminum phosphite can be applied to different polymer fields.
2) The aluminum phosphite crystal is prepared by taking phosphorous acid compound and aluminum compound as raw materials, and modifier is added in the preparation process to reduce particle size, improve particle dispersion degree and organic compatibility, thus solving the problem of incompatibility of agglomeration of aluminum phosphite in organic matrix.
(3) The refining and modification of the aluminum phosphite are completed by a one-step method, the high-value and high-energy-consumption airflow crushing equipment and modification equipment are avoided, the production efficiency is high, and the cost is low.
Drawings
FIG. 1 is a phase diagram of examples 1-3, which corresponds to the standard spectrum of anhydrous aluminum phosphite phase (card: PDF82-0509), and shows example 1, example 2, and example 3 from the top.
Detailed Description
Comparative example 1
Weighing 200g of phosphorous acid, dissolving the phosphorous acid in 200g of water, stirring and dissolving, slowly adding 130g of aluminum hydroxide, starting heating after the adding is finished, controlling the heating temperature to be 80 ℃ (mechanically stirring at the rotating speed of 200n/min), reacting for 2 hours, filtering the obtained solution, washing to be neutral, and vacuum-drying at 220 ℃ for 8 hours.
Example 2
Weighing 200g of phosphorous acid, dissolving in 200g of water, stirring and dissolving, adding 3g of silane coupling agent, continuously stirring uniformly, slowly adding 130g of aluminum hydroxide, starting heating after the addition is finished, wherein the heating temperature is 80 ℃ (mechanical stirring, the rotating speed is 200n/min)), reacting for 2 hours, filtering the obtained solution, washing to be neutral, and vacuum drying for 8 hours at 220 ℃.
Comparative example 3
Weighing 200g of phosphorous acid, dissolving in 200g of water, continuously stirring uniformly, slowly adding 130g of aluminum hydroxide, starting heating after the addition is finished, wherein the heating temperature is 80 ℃ (high-speed stirring, the rotating speed is 2000n/min)), reacting for 2 hours, filtering the obtained solution, washing to be neutral, and vacuum drying for 8 hours at 220 ℃.
Example 4
Weighing 200g of phosphorous acid, dissolving in 200g of water, stirring and dissolving, then adding 3g of sodium dodecyl sulfate, continuously stirring uniformly, slowly adding 130g of aluminum hydroxide, starting heating after the addition is finished, wherein the heating temperature is 80 ℃ (high-speed stirring, the rotating speed is 2000n/min)), reacting for 2 hours, filtering the obtained solution, washing to be neutral, and vacuum drying for 8 hours at 220 ℃.
For comparison, the particle size, activation rate and oil absorption value of the first, second and third powders and the Aluminum Diethylphosphinate (ADP) powder serving as a flame retardant are detected; after compounding aluminum phosphite and ADP (total capacity of 18 wt%, mass ratio of 1: 2), mechanical properties were compared with those of nylon 66, and the results are shown in Table 1.
The aluminum phosphite can replace part of ADP to be applied in nylon, the flame retardant property reaches the standard, and the aluminum phosphite (example 2 and example 4) after process optimization improves the comprehensive mechanical property of the nylon due to smaller size and better affinity.
Note: the dispersion degree and the organic compatibility of the product are expressed in the activation rate and the oil absorption value of the powder, and the higher the activation rate and the lower the oil absorption value are, the better the dispersion degree and the better the organic compatibility of the powder are.
On the other hand, the dispersion degree and the organic compatibility are also shown in the aspect of mechanical property, the dispersion degree is good, the organic compatibility is excellent, and the mechanical property of the composite material is good.
Activation index: inorganic powder generally has a high relative density and naturally settles in water. Most of the organic surface modification is water insoluble or nonpolar, so the surface of the inorganic powder after organic modification has polarity and is changed into nonpolar, and the inorganic powder has strong non-wetting property to water. Such non-wetting finely divided particles float on the water surface like an oil film due to the hydrophobicity and surface tension. Based on this phenomenon, the concept of "activation index" is proposed, denoted by H, which is calculated by the formula:
h ═ 100% mass of the floating fraction in the sample (g)/total mass of the sample;
inorganic powder without organic surface modification, H is 0;
when the modification was complete, H was 100%.
Oil absorption value: the oil absorption value is the volume or mass of castor oil or dibutyl phthalate adsorbed by unit mass of powder. The oil absorption value is one of the most main direct characterization indexes of inorganic powder modification, and particularly for an inorganic filler applied to a high polymer base material, the processing performance and the filling amount of the composite material are directly influenced by the oil absorption value of the filler. Generally, for inorganic fillers in high polymer composites, especially ultra-fine inorganic fillers, the lower the oil absorption, the easier it is to mix with the resin system or the filler loading can be increased.
Oil absorption value calculation formula: a is M/M;
m: the quality of the castor oil used;
m is the mass of the sample.
Claims (8)
1. A preparation method of a high-dispersion and organic-affinity aluminum phosphite flame retardant is characterized by comprising the following steps:
(1) dissolving phosphorous acid or salt thereof in an aqueous solution at a concentration of 30-50 wt%;
(2) adding a modifier in the step (1), and uniformly stirring to obtain a mixture with the concentration of 1-5 wt%; the modifier is used for adjusting the particle size and enhancing the dispersibility;
(3) adding aluminide into the solution in the step (2) according to a stoichiometric ratio, starting heating and stirring until the reaction is finished, wherein the heating temperature is 40-100 ℃;
(4) and carrying out suction filtration, washing to neutrality and drying on the obtained solution to obtain a product.
2. The method of claim 1, wherein the phosphite is sodium phosphite and/or ammonium phosphite.
3. The method of claim 1, wherein the modifier is an organic surface modifier.
4. The method of claim 3, wherein the modifier is sodium dodecyl sulfate, stearic acid, a silane coupling agent, phosphate ester, tween-80, polyvinyl alcohol and/or urea.
5. The method of claim 1, wherein the aluminum oxide is aluminum oxide, aluminum salt and/or aluminum hydroxide.
6. The method of claim 5, wherein the aluminum compound is aluminum hydroxide, aluminum oxide, aluminum sulfate and/or aluminum chloride.
7. The method as claimed in claim 1, wherein the step (4) is vacuum drying at 150 ℃ and 240 ℃.
8. A highly dispersed and organophilic aluminum phosphite flame retardant prepared by the process of claims 1-7.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115073819A (en) * | 2022-06-15 | 2022-09-20 | 兰州瑞朴科技有限公司 | Aluminum phosphate salt flame retardant based on growth nucleus and preparation method and application thereof |
| CN115784183A (en) * | 2022-12-21 | 2023-03-14 | 襄阳汉伟化工科技有限公司 | Preparation process of high-yield and low-granularity aluminum phosphite |
| CN116254002A (en) * | 2023-02-23 | 2023-06-13 | 深圳市森日有机硅材料股份有限公司 | Liquid silicone rubber composition for coating air bags and preparation method thereof |
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| CN115073819A (en) * | 2022-06-15 | 2022-09-20 | 兰州瑞朴科技有限公司 | Aluminum phosphate salt flame retardant based on growth nucleus and preparation method and application thereof |
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| CN115784183A (en) * | 2022-12-21 | 2023-03-14 | 襄阳汉伟化工科技有限公司 | Preparation process of high-yield and low-granularity aluminum phosphite |
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| CN116254002A (en) * | 2023-02-23 | 2023-06-13 | 深圳市森日有机硅材料股份有限公司 | Liquid silicone rubber composition for coating air bags and preparation method thereof |
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