CN111661830A - Preparation method of aluminum phosphite - Google Patents
Preparation method of aluminum phosphite Download PDFInfo
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- CN111661830A CN111661830A CN202010688064.0A CN202010688064A CN111661830A CN 111661830 A CN111661830 A CN 111661830A CN 202010688064 A CN202010688064 A CN 202010688064A CN 111661830 A CN111661830 A CN 111661830A
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- 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
- C01B25/163—Phosphorous acid; Salts thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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Abstract
The invention provides a preparation method of aluminum phosphite. The method comprises the following steps: providing aluminum hydroxide or pseudo-boehmite powder, and drying the aluminum hydroxide or pseudo-boehmite powder; providing solid phosphorous acid, adding the solid phosphorous acid into a preheated kneading stirrer, and heating and stirring to obtain liquid phosphorous acid; adding the dried aluminum hydroxide or pseudo-boehmite powder into liquid phosphorous acid, heating and stirring to obtain the aluminum phosphite. The method has the advantages of simple process, low cost, high production efficiency and good environmental protection performance.
Description
Technical Field
The invention relates to the technical field of flame retardance, and particularly relates to a preparation method of aluminum phosphite.
Background
With the economic development, the application range and the use amount of new materials are continuously enlarged, the application of polymer materials is wider and wider, the flammability of the materials is widely concerned by people, and the effective prevention of the combustion of flammable polymer materials is of great importance to the wide popularization of the materials.
The phosphorus flame retardant has low smoke generation, and the development and application of the phosphorus flame retardant become hot spots in the flame retardant industry in recent years. The phosphorus flame retardant is divided into inorganic flame retardant and organic phosphorus flame retardant, and the inorganic phosphorus flame retardant has the advantages of good thermal stability, low smoke, no halogen, no toxicity, no corrosion, no volatilization or precipitation in the storage process, rich raw material sources, low price and the like, occupies more than half of the market of the flame retardant, and is the first of the flame retardants. Although the organic phosphorus flame retardant dialkyl phosphinate on the market at present has excellent comprehensive performance, the price is high, and the organic phosphorus flame retardant dialkyl phosphinate is difficult to occupy domestic and foreign markets on a large scale, and aluminum hypophosphite (AlHP) serving as an inorganic additive type flame retardant has the defects of excellent performance, low cost, common stability at high temperature, narrow processing application range, easy precipitation in nylon flame retardance, product color change caused by strong reducibility, reduced mechanical property of nylon and common processability.
The aluminum phosphite can be used as an inorganic additive type flame retardant, has excellent flame retardant performance, and has better thermal stability and nylon flame retardant addition using effect than aluminum hypophosphite. The prior preparation method of the aluminum phosphite mainly comprises a neutralization method, a double decomposition method and a template hydrothermal synthesis method; the method is divided into a solid phase method and a liquid phase method, so that the time consumption is long, the purity and the yield are low, and the production process is difficult to control; the double decomposition reaction produces more waste water, aluminum hydroxide byproducts are easily produced when the pH value is not well controlled, the yield is low, new negative and positive impurity ions are easily introduced, and the influence factors on the flame retardant effect of the prepared product are more.
As for the template hydrothermal synthesis method, the prior art has a technical scheme that pseudo-boehmite is used as an aluminum source, phosphorous acid is used as a phosphorus source, and a polynitrogen compound guanidine carbonate is used as a structure directing agent to prepare an aluminum phosphite single crystal by a hydrothermal method. However, in the method, the reactant needs to be placed in a high-pressure reaction kettle and then placed in a constant-temperature drying box for crystallization for several days, the production time is too long, the requirement of large-scale industrial production cannot be met, and the organic template agent is easily introduced into the product and has adverse effect when being applied to flame retardance.
In addition, the prior art also has a technical scheme that aluminum hydroxide is placed in a kneader, phosphorous acid is added in batches and heated to 120-220 ℃ for reaction for 2 hours, and a mixture of aluminum phosphite and aluminum hydrogen phosphite is generated by the reaction, but the scheme is easy to cause the solidification of feed liquid in stirring in the actual production to damage equipment. Therefore, the preparation method of the aluminum phosphite, which is suitable for industrial large-scale production, has the advantages of good stability, safety, environmental protection, wide application range and low cost, is urgently needed in the market at present.
Disclosure of Invention
The invention aims to provide a preparation method of aluminum phosphite, which has the advantages of simple process, low cost, high production efficiency, no waste water and waste residue and good environmental protection performance, and when the prepared product is used in a flame retardant and related synergists thereof, the addition amount is small and the flame retardant efficiency is high.
In order to achieve the above object, the present invention provides a method for preparing aluminum phosphite, comprising the steps of:
step S1, providing aluminum hydroxide or pseudo-boehmite powder, and drying the aluminum hydroxide or pseudo-boehmite powder;
step S2, providing solid phosphorous acid, adding the solid phosphorous acid into a preheated kneading and stirring machine, and heating and stirring to obtain liquid phosphorous acid;
and step S3, adding the dried aluminum hydroxide or pseudo-boehmite powder into the liquid phosphorous acid, heating and stirring to obtain the aluminum phosphite.
The preparation method of the aluminum phosphite also comprises the following steps:
step S4, stirring the aluminum phosphite and cooling to room temperature;
and step S5, placing the cooled aluminum phosphite in a powder surface modification high-speed mixer, spraying a coupling agent into the powder surface modification high-speed mixer for modification, discharging and sieving after stirring reaction to obtain the surface modified aluminum phosphite.
The step S1 specifically includes:
putting the aluminum hydroxide or pseudo-boehmite powder into an oven at 110-130 ℃ for drying for 4-8 hours;
in the step S1, the moisture content of the dried aluminum hydroxide or pseudo-boehmite powder is controlled to be 0.5% -1%.
The step S2 specifically includes:
and adding the solid phosphorous acid into a preheated kneading stirrer, heating and stirring to melt the solid phosphorous acid, continuing heating and stirring to raise the temperature to 100-120 ℃, and continuously stirring at the temperature of 100-120 ℃ for 30-60 min.
In the step S2, an anti-oxidation protective gas is also introduced into the kneading mixer during the heating and stirring process.
The step S3 specifically includes: adding the dried aluminum hydroxide or pseudo-boehmite powder into the liquid phosphorous acid in batches, heating, stirring and heating to 130-160 ℃, reacting for 2-6 hours to obtain a powdery product, then continuing heating, stirring and heating to 180-230 ℃, and continuing reacting for 2-8 hours to finally obtain powdery aluminum phosphite.
In the step S3, the stirring rotation speed before half of the aluminum hydroxide or pseudo-boehmite powder added to the liquid phosphorous acid is the first rotation speed;
the stirring rotating speed after the dried aluminum hydroxide or pseudo-boehmite powder added into the liquid phosphorous acid reaches one half and before the dried aluminum hydroxide or pseudo-boehmite powder reaches two thirds is the second rotating speed;
the stirring speed is the third speed after the dried aluminum hydroxide or pseudo-boehmite powder added into the liquid phosphorous acid reaches two thirds;
the first rotational speed and the third rotational speed are both less than the second rotational speed.
The first rotating speed and the third rotating speed are 20-30 revolutions per minute, the second rotating speed is 50-70 revolutions per minute, and the particle size of the powdery aluminum phosphite is 20-50 microns.
The stirring reaction time in the step S5 is 60-90 minutes, and the coupling agent is a phosphorus-titanate coupling agent or a phosphate coupling agent.
The mixture ratio of the aluminum hydroxide or the pseudo-boehmite powder, the solid phosphorous acid and the coupling agent is as follows: solid phosphorous acid: 50% -70%; aluminum hydroxide or pseudo-boehmite powder: 30% -40%; coupling agent: 0.1 to 5 percent.
The invention has the beneficial effects that: the invention provides a preparation method of aluminum phosphite, which comprises the following steps: step S1, providing aluminum hydroxide or pseudo-boehmite powder, and drying the aluminum hydroxide or pseudo-boehmite powder; step S2, providing solid phosphorous acid, adding the solid phosphorous acid into a preheated kneading and stirring machine, and heating and stirring to obtain liquid phosphorous acid; step S3, adding the dried aluminum hydroxide or pseudo-boehmite powder into the liquid phosphorous acid, heating and stirring to obtain aluminum phosphite, and modifying the surface of the aluminum phosphite powder material to increase the compatibility of the aluminum phosphite powder material with a high polymer material; the method has the advantages of simple process, low cost, high production efficiency and good environmental protection performance.
Drawings
For a better understanding of the nature and technical aspects of the present invention, reference should be made to the following detailed description of the invention, taken in conjunction with the accompanying drawings, which are provided for purposes of illustration and description and are not intended to limit the invention.
In the drawings, there is shown in the drawings,
FIG. 1 is a flow chart of a process for the preparation of aluminum phosphite according to the present invention;
FIG. 2 is a powder diffraction pattern of the product obtained by the process for the preparation of aluminum phosphite according to the present invention.
Detailed Description
To further illustrate the technical means and effects of the present invention, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Referring to fig. 1, the present invention provides a method for preparing aluminum phosphite, comprising the following steps:
step S1, providing aluminum hydroxide or pseudo-boehmite powder, and drying the aluminum hydroxide or pseudo-boehmite powder.
Specifically, the step S1 specifically includes: and (3) putting the aluminum hydroxide or pseudo-boehmite powder into an oven at 110-130 ℃ for drying for 4-8 hours.
Further, in the step S1, the moisture content of the dried aluminum hydroxide or pseudo-boehmite powder is controlled to be 0.5% to 1%.
And step S2, providing solid phosphorous acid, adding the solid phosphorous acid into a preheated kneading and stirring machine, and heating and stirring to obtain liquid phosphorous acid.
Specifically, the step S2 specifically includes: and adding the solid phosphorous acid into a preheated kneading stirrer, heating and stirring to melt the solid phosphorous acid, continuing heating and stirring to raise the temperature to 100-120 ℃, and continuously stirring at the temperature of 100-120 ℃ for 30-60 min.
Specifically, in step S2, an anti-oxidation protective gas is also introduced into the kneading mixer during the heating and stirring process.
Preferably, the protective gas is an inert protective gas such as nitrogen or argon.
And step S3, adding the dried aluminum hydroxide or pseudo-boehmite powder into the liquid phosphorous acid, heating and stirring to obtain the aluminum phosphite.
Specifically, the step S3 specifically includes: adding the dried aluminum hydroxide or pseudo-boehmite powder into the liquid phosphorous acid in batches, heating, stirring and heating to 130-160 ℃, reacting for 2-6 hours to obtain a powdery product, then continuously heating, stirring and heating to 180-230 ℃, and further reacting for 2-8 hours to finally obtain powdery aluminum phosphite.
Further, when the dried aluminum hydroxide or pseudo-boehmite powder is added into the liquid phosphorous acid in batches, a large amount of heat can be released in the reaction process, and when the material is added to 1/2-2/3, the viscosity of the reactant is high and the reactant is easy to expand and overflow, so that the stirring speed needs to be controlled in a slow-fast-slow rhythm in the feeding process.
In detail, in the step S3, the stirring rotation speed before half of the aluminum hydroxide or pseudo-boehmite powder added to the liquid phosphorous acid is the first rotation speed; the stirring rotating speed after the dried aluminum hydroxide or pseudo-boehmite powder added into the liquid phosphorous acid reaches one half and before the dried aluminum hydroxide or pseudo-boehmite powder reaches two thirds is the second rotating speed; the stirring speed is the third speed after the dried aluminum hydroxide or pseudo-boehmite powder added into the liquid phosphorous acid reaches two thirds; the first rotational speed and the third rotational speed are both less than the second rotational speed.
Preferably, the first rotating speed and the third rotating speed are 20-30 revolutions per minute, and the second rotating speed is 50-70 revolutions per minute. More preferably, the first rotational speed is the same as or similar to the third rotational speed.
Specifically, the particle size of the powdery aluminum phosphite is 20-50 microns.
Further, the powder aluminum phosphite is subjected to an X-Ray diffraction (XRD) test to obtain a diffraction pattern of the powder aluminum phosphite as shown in fig. 2, and a standard pattern is used to determine that the molecular formula of the final product powder aluminum phosphite is Al (HPO)3)3·4H2O。
And step S4, stirring the aluminum phosphite and cooling to room temperature.
And step S5, placing the cooled aluminum phosphite in a powder surface modification high-speed mixer, spraying a coupling agent into the powder surface modification high-speed mixer for modification, discharging and sieving after stirring reaction to obtain the surface modified aluminum phosphite.
Specifically, the stirring reaction time in the step S5 is 60 to 90 minutes.
Preferably, the coupling agent in step S5 is a phosphorus titanate coupling agent or a phosphate ester coupling agent.
Optionally, in the step S5, the coupling agent of the alkoxy phosphorus-containing titanate is diluted with a solvent No. 200 and then sprayed into the powder surface modification high-speed mixer.
Specifically, the ratio of the aluminum hydroxide or pseudo-boehmite powder, the solid phosphorous acid and the coupling agent is as follows: solid phosphorous acid: 50% -70%; aluminum hydroxide or pseudo-boehmite powder: 30% -40%; coupling agent: 0.1 to 5 percent.
Specific embodiments of the invention are described below:
example 1
1600g of aluminum hydroxide is weighed and placed in an oven for drying for 6 hours at 180 ℃, the water content of the aluminum hydroxide is 0.8 percent, and the aluminum hydroxide is cooled for standby.
2600g solid phosphorous acid is weighed and added into a preheated kneading mixer, the phosphorous acid is melted by heating and stirring, the stirring is continued and the temperature is raised to 130 ℃, and nitrogen is introduced for protection in the heating and stirring process to prevent oxidation.
Adding the dried aluminum hydroxide into phosphorous acid slowly in batches, heating to 150 ℃ while stirring, reacting for 3 hours to obtain a powdery product, heating to 200 ℃, continuing to stir for 2 hours, and generating powdery aluminum phosphite after the reaction is completed.
The aluminum phosphite powder produced by the reaction was slowly stirred and cooled to room temperature.
Putting aluminum phosphite powder into a powder surface modification high-speed mixer, diluting an alkoxy phosphorus-containing titanate coupling agent (1:1 dilution) by using a No. 200 solvent, spraying the diluted alkoxy phosphorus-containing titanate coupling agent into the powder surface modification high-speed mixer (the dosage of the phosphorus-containing titanate coupling agent accounts for 0.8 percent of the weight of the powder), stirring for reaction for 10 to 20 minutes, discharging, sieving, subpackaging, sealing and storing.
Example 2
1200g of pseudo-boehmite powder is weighed and placed in an oven for drying for 7 hours at the temperature of 120 ℃, the moisture content of the pseudo-boehmite powder is 0.7 percent, and the pseudo-boehmite powder is cooled for standby.
2000g of solid phosphorous acid is weighed and added into a kneading stirrer, the solid phosphorous acid is heated and stirred to melt the phosphorous acid, the stirring is continued to be heated to 130 ℃, and nitrogen is introduced for protection in the heating and stirring process to prevent oxidation.
Slowly adding the dried pseudo-boehmite powder into phosphorous acid in batches, heating to 140 ℃ while stirring, reacting for 4 hours to obtain a powdery product, heating to 185 ℃, continuously stirring and reacting for 3 hours to generate powdery aluminum phosphite after the reaction is completed, wherein the stirring speed in the feeding process needs to be controlled in a slow-fast-slow rhythm.
The aluminum phosphite powder produced by the reaction was slowly stirred and cooled to room temperature.
Putting the aluminum phosphite powder into a powder surface modification high-speed mixer, diluting a phosphate coupling agent (1.5:1 dilution) by using isopropanol, spraying the phosphate coupling agent into the powder surface modification high-speed mixer (the phosphate coupling agent accounts for 1.0 percent of the weight of the powder), stirring for reaction for 15 to 25 minutes, discharging, sieving, subpackaging, sealing and storing.
The modified aluminum phosphite is applied to nylon flame retardation, and 13 percent of diethyl aluminum hypophosphite and 6 percent of aluminum phosphite Al (HPO) are added3)3·4H250-60% of O, 50-60% of nylon PA6 and 20-30% of glass fiber, and the flame retardance can reach V0 level without affecting the appearance and mechanical property of the nylon product.
It should be noted that the preparation method of the aluminum phosphite of the present invention has the following advantages:
firstly, common industrial-grade aluminum hydroxide or pseudo-boehmite powder is taken as a reactant, neutralization reaction without solvent and water addition can be carried out only by simple drying pretreatment, raw materials are easy to obtain, and the cost is low;
secondly, no solvent, water and other reaction media are added in the production process of the method, the equipment is simple to operate, the energy consumption is low, byproducts are not generated basically in the production process, wastewater and waste residues are not generated, the environmental protection performance is good, and the influence on the environment and workers is low;
thirdly, the conversion rate of the product is high, the phosphorus content of the generated aluminum phosphite is high, and when the aluminum phosphite is applied to a flame retardant and a related synergist, the flame retardant has good flame retardant efficiency and small addition amount, is not precipitated and floated in nylon, has no influence on the mechanical properties and the like of the nylon, and has good compatibility;
finally, the coupling agent used in the method is a phosphorus-containing titanate coupling agent or a phosphate coupling agent, and because two different reactive groups exist in the molecules of the coupling agent, a powder-coupling molecule-organic phase bonding layer can be formed, so that the bonding interface strength of the polymer and the flame retardant powder is improved, and the blending compatibility and other properties are improved. The coupling agent has good thermal stability, flame retardance and coupling property, the addition mode adopts dry modification, the addition is simple and convenient to operate, after modification, the polarity of the product is reduced, the dispersibility is improved, the compatibility with the polymer is better, and the coupling agent has flame retardance, so that the flame retardance of the product can be further enhanced.
In summary, the present invention provides a method for preparing aluminum phosphite, comprising the following steps: step S1, providing aluminum hydroxide or pseudo-boehmite powder, and drying the aluminum hydroxide or pseudo-boehmite powder; step S2, providing solid phosphorous acid, adding the solid phosphorous acid into a preheated kneading and stirring machine, and heating and stirring to obtain liquid phosphorous acid; step S3, adding the dried aluminum hydroxide or pseudo-boehmite powder into the liquid phosphorous acid, heating and stirring to obtain aluminum phosphite; the method has the advantages of simple process, low cost, high production efficiency and good environmental protection performance.
As described above, it will be apparent to those skilled in the art that other various changes and modifications may be made based on the technical solution and concept of the present invention, and all such changes and modifications are intended to fall within the scope of the appended claims.
Claims (10)
1. A preparation method of aluminum phosphite is characterized by comprising the following steps:
step S1, providing aluminum hydroxide or pseudo-boehmite powder, and drying the aluminum hydroxide or pseudo-boehmite powder;
step S2, providing solid phosphorous acid, adding the solid phosphorous acid into a preheated kneading and stirring machine, and heating and stirring to obtain liquid phosphorous acid;
and step S3, adding the dried aluminum hydroxide or pseudo-boehmite powder into the liquid phosphorous acid, heating and stirring to obtain the aluminum phosphite.
2. The method of preparing aluminum phosphite of claim 1, further comprising:
step S4, stirring the aluminum phosphite and cooling to room temperature;
and step S5, placing the cooled aluminum phosphite in a powder surface modification high-speed mixer, spraying a coupling agent into the powder surface modification high-speed mixer for modification, discharging and sieving after stirring reaction to obtain the surface modified aluminum phosphite.
3. The method according to claim 1, wherein the step S1 specifically comprises:
putting the aluminum hydroxide or pseudo-boehmite powder into an oven at 110-130 ℃ for drying for 4-8 hours;
in the step S1, the moisture content of the dried aluminum hydroxide or pseudo-boehmite powder is controlled to be 0.5% -1%.
4. The method according to claim 1, wherein the step S2 specifically comprises:
and adding the solid phosphorous acid into a preheated kneading stirrer, heating and stirring to melt the solid phosphorous acid, continuing heating and stirring to raise the temperature to 100-120 ℃, and continuously stirring at the temperature of 100-120 ℃ for 30-60 min.
5. The process for producing aluminum phosphite as set forth in claim 1, wherein in step S2, an anti-oxidizing protective gas is further introduced into the kneader-mixer during the heating and stirring.
6. The method according to claim 1, wherein the step S3 specifically comprises: adding the dried aluminum hydroxide or pseudo-boehmite powder into the liquid phosphorous acid in batches, heating, stirring and heating to 130-160 ℃, reacting for 2-6 hours to obtain a powdery product, then continuing heating, stirring and heating to 180-230 ℃, and continuing reacting for 2-8 hours to finally obtain powdery aluminum phosphite.
7. The method according to claim 6, wherein in step S3, the stirring speed is a first speed until one-half of the aluminum hydroxide or pseudo-boehmite powder added to the liquid phosphorous acid is added;
the stirring rotating speed after the dried aluminum hydroxide or pseudo-boehmite powder added into the liquid phosphorous acid reaches one half and before the dried aluminum hydroxide or pseudo-boehmite powder reaches two thirds is the second rotating speed;
the stirring speed is the third speed after the dried aluminum hydroxide or pseudo-boehmite powder added into the liquid phosphorous acid reaches two thirds;
the first rotational speed and the third rotational speed are both less than the second rotational speed.
8. The method of claim 7, wherein the first and third rotational speeds are 20-30 rpm, the second rotational speed is 50-70 rpm, and the particle size of the powdered aluminum phosphite is 20-50 μm.
9. The method for preparing aluminum phosphite according to claim 2, wherein the stirring reaction time in step S5 is 60-90 minutes, and the coupling agent is a phosphorus-titanate coupling agent or a phosphate coupling agent.
10. The method for preparing aluminum phosphite according to claim 2, wherein the ratio of the aluminum hydroxide or pseudo-boehmite powder, the solid phosphorous acid and the coupling agent is as follows: solid phosphorous acid: 50% -70%; aluminum hydroxide or pseudo-boehmite powder: 30% -40%; coupling agent: 0.1 to 5 percent.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113308023A (en) * | 2021-06-22 | 2021-08-27 | 四川省蜀爱新材料有限公司 | High-dispersion and organic-affinity aluminum phosphite flame retardant and preparation method thereof |
| CN113321945A (en) * | 2021-06-22 | 2021-08-31 | 华南农业大学 | Preparation method and application of carbon quantum dot regulated aluminum phosphite crystal |
| CN113460984A (en) * | 2020-10-22 | 2021-10-01 | 江苏利思德新材料有限公司 | Crystalline aluminum phosphite and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104114485A (en) * | 2011-12-05 | 2014-10-22 | 科莱恩金融(Bvi)有限公司 | Mixtures of aluminium hydrogenphosphites with aluminium salts, process for the production thereof and the use thereof |
-
2020
- 2020-07-16 CN CN202010688064.0A patent/CN111661830A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104114485A (en) * | 2011-12-05 | 2014-10-22 | 科莱恩金融(Bvi)有限公司 | Mixtures of aluminium hydrogenphosphites with aluminium salts, process for the production thereof and the use thereof |
Non-Patent Citations (2)
| Title |
|---|
| 中国科学技术协会等: "《颗粒学学科发展报告2009-2010》", 30 April 2010, 中国科学技术出版社 * |
| 刘西文: "《塑料配混工（中、高级）培训教程》", 31 January 2017, 文化发展出版社 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113460984A (en) * | 2020-10-22 | 2021-10-01 | 江苏利思德新材料有限公司 | Crystalline aluminum phosphite and preparation method and application thereof |
| WO2022083032A1 (en) * | 2020-10-22 | 2022-04-28 | 江苏利思德新材料有限公司 | Crystalline aluminum phosphite, preparation method therefor, and use thereof |
| US20220127434A1 (en) * | 2020-10-22 | 2022-04-28 | Zhejiang University | Crystalline aluminum phosphite, preparation method and application thereof |
| JP2022068842A (en) * | 2020-10-22 | 2022-05-10 | ジィァンスー リースーデェァ ニュー マテリアル カンパニー リミテッド | Crystalline aluminum phosphite, preparation method and use thereof |
| JP7258295B2 (en) | 2020-10-22 | 2023-04-17 | ジィァンスー リースーデェァ ニュー マテリアル カンパニー リミテッド | Crystalline aluminum phosphite and method for producing and using the same |
| US11787921B2 (en) * | 2020-10-22 | 2023-10-17 | Jiangsu Liside New Material Co., Ltd. | Crystalline aluminum phosphite, preparation method and application thereof |
| CN113308023A (en) * | 2021-06-22 | 2021-08-27 | 四川省蜀爱新材料有限公司 | High-dispersion and organic-affinity aluminum phosphite flame retardant and preparation method thereof |
| CN113321945A (en) * | 2021-06-22 | 2021-08-31 | 华南农业大学 | Preparation method and application of carbon quantum dot regulated aluminum phosphite crystal |
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