CN114772568B - Method for preparing modified aluminum hypophosphite and product thereof - Google Patents
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- CN114772568B CN114772568B CN202111157033.3A CN202111157033A CN114772568B CN 114772568 B CN114772568 B CN 114772568B CN 202111157033 A CN202111157033 A CN 202111157033A CN 114772568 B CN114772568 B CN 114772568B
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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
- C01B25/26—Phosphates
- C01B25/36—Aluminium phosphates
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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
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
Abstract
The invention discloses a method for preparing modified aluminum hypophosphite and a product thereof, wherein a prepolymer solution with a modification effect on aluminum hypophosphite is synthesized firstly, and then aluminum hypophosphite is generated by reaction in the prepolymer solution, so that the generation and modification of aluminum hypophosphite are carried out simultaneously, thereby obviously shortening the production route of the modified aluminum hypophosphite, directly preparing the modified aluminum hypophosphite product, further obviously improving the yield of the modified aluminum hypophosphite, leading the performance stability of the modified aluminum hypophosphite product to be better, reducing the energy consumption, reducing the production cost and reducing the emission of waste gas and waste water; meanwhile, due to reasonable raw material proportion and reaction conditions, the prepared modified aluminum hypophosphite has better compatibility and dispersibility with organic polymers, narrower particle size distribution and better particle size uniformity, and has positive effects on the application of modified aluminum hypophosphite products in organic polymer materials.
Description
Technical Field
The invention relates to the field of flame-retardant materials, in particular to a method for preparing modified aluminum hypophosphite and a product thereof.
Background
Aluminum hypophosphite is a flame retardant with high phosphorus content, small water solubility and excellent flame retardant effect, and is used on modified plastics such as PA6, PBT and the like, so that good flame retardant performance is obtained, for example, when aluminum hypophosphite is added into PBT, the flame retardant performance of PBT can reach V-0 grade of UL94 standard; meanwhile, aluminum hypophosphite and MCA are compounded to serve as a flame retardant of the elastomer TPE, TPU, TPV, so that the flame retardant effect is good; the aluminum hypophosphite, the melamine hydrobromic acid, the combined flame retardant and the like are compounded in the PP with the flame retardant grade V-2, and good flame retardant property and mechanical property balance can be achieved under the condition of lower addition; thus, aluminum hypophosphite is used in large amounts as a flame retardant in organic polymeric material articles.
However, aluminum hypophosphite is an inorganic substance, and when added to an organic polymer material, the aluminum hypophosphite inevitably has the defects of poor compatibility with the organic polymer and poor dispersibility, so in order to overcome the defects of poor compatibility and poor dispersibility of aluminum hypophosphite and the organic polymer, the aluminum hypophosphite is mostly modified and then added in the prior art. The existing modified aluminum hypophosphite is obtained by synthesizing inorganic aluminum hypophosphite and then carrying out modification treatment, such as CN105037808A (a microencapsulated aluminum hypophosphite and a preparation method and application thereof), CN105457574A (a preparation method of a microencapsulated aluminum hypophosphite flame retardant), CN107936296A (a modified aluminum hypophosphite flame retardant and a preparation method thereof) and the like, which are all prepared by carrying out modification treatment on synthesized aluminum hypophosphite. Although the modified aluminum hypophosphite product with excellent performance can be obtained by carrying out the later modification treatment on the aluminum hypophosphite, the synthesis of the aluminum hypophosphite and the modification treatment of the aluminum hypophosphite are carried out separately and independently, and the modified aluminum hypophosphite product can be prepared through two different production process routes, so that the energy sources are wasted, and the production cost is increased; more waste water and waste gas are generated, and environmental pollution is aggravated; meanwhile, the yield of the finally obtained modified aluminum hypophosphite is reduced due to the prolonged production process route, the product performance difference of different production batches is increased, and the large-scale production and application of the modified aluminum hypophosphite product are seriously influenced.
Disclosure of Invention
The invention aims to overcome the defects of long production process route and low yield of the existing preparation method of modified aluminum hypophosphite, and provides a method for preparing the modified aluminum hypophosphite and a product thereof, wherein the method firstly synthesizes a prepolymer solution with a modification effect on the aluminum hypophosphite, and then reacts in the prepolymer solution to generate the aluminum hypophosphite, so that the generation and modification of the aluminum hypophosphite are carried out simultaneously, thereby obviously shortening the production route of the modified aluminum hypophosphite, directly preparing the modified aluminum hypophosphite product, further obviously improving the yield of the modified aluminum hypophosphite, leading the performance stability of the modified aluminum hypophosphite product to be better, reducing the energy consumption, reducing the production cost and reducing the emission of waste gas and waste water; meanwhile, due to reasonable raw material proportion and reaction conditions, the prepared modified aluminum hypophosphite has better compatibility and dispersibility with organic polymers, narrower particle size distribution and better particle size uniformity, and has positive effects on the application of modified aluminum hypophosphite products in organic polymer materials.
A method of preparing a modified aluminum hypophosphite comprising the steps of:
(1) Preparing a prepolymer solution; the prepolymer solution is melamine formaldehyde resin prepolymer solution or urea formaldehyde resin prepolymer solution;
(2) Adding sodium hypophosphite monohydrate and aluminum sulfate octadecanoate into the prepolymer solution, and reacting for 3-5 hours at the temperature of 80-95 ℃ to obtain modified aluminum hypophosphite slurry;
(3) And (3) separating, purifying and drying the modified aluminum hypophosphite slurry to obtain a modified aluminum hypophosphite powder product.
Preferably, in the step (1), the preparation method of the melamine formaldehyde resin prepolymer solution comprises the following steps: dissolving melamine and formaldehyde into water to form a mixed solution, adjusting the pH value of the mixed solution to 8-10, and then reacting for 2-4 hours at the temperature of 70-90 ℃ to obtain a melamine formaldehyde resin prepolymer solution; the preparation method of the melamine formaldehyde resin prepolymer solution is preferable, the molecular weight of the prepolymer is more suitable, the reaction time is shorter, and the modification of aluminum hypophosphite is more facilitated.
Preferably, the mass ratio of the melamine to the formaldehyde is 1:0.5-1; the preferred mass ratio of melamine to formaldehyde is more thorough, the yield of prepolymer is higher, and most preferably, the mass ratio of melamine to formaldehyde is 1:0.8.
Preferably, the total mass of the melamine and the formaldehyde in the mixed solution is 0.1-2 percent by mass; the preferable concentration of melamine and formaldehyde ensures that the molecular weight of the prepolymer is more uniform, the modification effect on aluminum hypophosphite is better, the particle size of the aluminum hypophosphite is more uniform, and the yield is higher; most preferably, the total mass of the melamine and the formaldehyde in the mixed solution is 0.5-1% by mass.
Preferably, in the step (1), the preparation method of the urea resin prepolymer solution comprises the following steps: dissolving urea and formaldehyde into water to form a mixed solution, adjusting the pH value of the mixed solution to 8-10, and reacting for 2-4 hours at the temperature of 70-90 ℃ to obtain urea-formaldehyde resin prepolymer solution; the preparation method of the preferable urea resin prepolymer solution has more proper molecular weight of the prepolymer and shorter reaction time, and is more beneficial to the modification of aluminum hypophosphite.
Preferably, the mass ratio of the urea to the formaldehyde is 1:0.75-1; the preferable mass ratio of urea to formaldehyde has more thorough polymerization reaction and higher yield of prepolymer; most preferably, the mass ratio of urea to formaldehyde is 1:1.
Preferably, the total mass of the urea and the formaldehyde in the mixed solution is 0.1-2 percent by mass; the preferable concentration of urea and formaldehyde is that the molecular weight of the prepolymer is more uniform, the modification effect on aluminum hypophosphite is better, the particle size of the aluminum hypophosphite is more uniform, and the yield is higher; most preferably, the total mass of urea and formaldehyde in the mixed solution is 0.5-1% by mass.
Preferably, in the step (1), in the preparation method of the prepolymer solution, sodium carbonate is adopted to adjust the pH value of the mixed solution; the preferred pH regulator does not adversely affect the polymerization of the prepolymer and does not affect the synthesis and modification of aluminum hypophosphite.
Wherein, preferably, the mass ratio of the aluminum sulfate octadecanoate to the sodium hypophosphite monohydrate in the step (2) is 1:0.8-1.2; the preferred mass ratio of the aluminum sulfate octadecanoate to the sodium hypophosphite monohydrate has more thorough reaction, higher yield of the aluminum hypophosphite and better performance after modification; most preferably, the mass ratio of aluminum sulfate octadecanoate to sodium hypophosphite monohydrate is 1:1.15.
Wherein, preferably, the mass ratio of the total mass of the aluminum sulfate octadecanoate and the sodium hypophosphite monohydrate added in the step (2) to the prepolymer solution is 5:4-10; the preferable mass ratio of the aluminum sulfate octadecanoate to the hypophosphorous acid to the prepolymer solution has more thorough reaction, higher yield of the aluminum hypophosphite and better performance after modification; most preferably, the ratio of the total mass of aluminum sulfate octadecanoate and sodium hypophosphite monohydrate to the mass of the prepolymer solution is 5:6.
Preferably, in the step (2), the addition sequence of the aluminum sulfate octadecanoate and the sodium hypophosphite monohydrate is as follows: if the prepolymer solution is melamine formaldehyde resin prepolymer solution, firstly adding aluminum sulfate octadecanoate, and then adding sodium hypophosphite monohydrate after the aluminum sulfate octadecanoate is completely dissolved; if the prepolymer solution is urea resin prepolymer solution, sodium hypophosphite monohydrate is added first, and aluminum sulfate octadecanoate is added after the sodium hypophosphite monohydrate is completely dissolved; the preferred order of addition of aluminum sulfate octadecanoate and sodium hypophosphite monohydrate can improve the performance and yield of the modified aluminum hypophosphite.
Wherein, the reaction temperature in the step (2) is preferably 85-90 ℃ and the reaction time is 3-4h; the preferable reaction temperature and time are more thorough, the yield is higher and the energy consumption is lower.
Wherein, preferably, the temperature of the drying treatment in the step (3) is 70-150 ℃ and the time is 4-5h; preferred drying temperatures and times are higher drying efficiency and lower energy consumption.
Furthermore, the invention also provides a modified aluminum hypophosphite product, which is prepared by the preparation method; the modified aluminum hypophosphite product is obtained through one-time synthesis modification, has the advantages of more stable product performance, lower cost, higher yield and narrower particle size distribution range, and has good compatibility with organic polymer materials due to the fact that a large amount of organic components are wrapped on the surface of the product, is easy to disperse in the organic polymer materials, and can be used as a flame retardant for a large amount of organic polymer material products, so that the flame retardance of the organic polymer materials is obviously improved.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the method for preparing the modified aluminum hypophosphite, disclosed by the invention, the production route of the modified aluminum hypophosphite is obviously shortened by utilizing the method for simultaneously carrying out generation and modification of the aluminum hypophosphite, and the modified aluminum hypophosphite product is directly prepared, so that the yield of the modified aluminum hypophosphite is obviously improved, the performance stability is better, the energy consumption is reduced, the production cost is reduced, and the emission of waste gas and waste water is reduced.
2. In the method for preparing the modified aluminum hypophosphite, the prepared modified aluminum hypophosphite has the advantages of narrower particle size distribution and better particle size uniformity while having better compatibility and dispersibility with organic polymers by reasonably adjusting the raw material proportion and the reaction condition.
3. The method for preparing the modified aluminum hypophosphite is simple and reliable, has high production efficiency and low energy consumption, and is suitable for large-scale industrial production and application of modified aluminum hypophosphite products.
4. The modified aluminum hypophosphite product is obtained through one-time synthesis modification, has the advantages of more stable product performance, lower cost, higher yield, narrower particle size distribution range, good compatibility with organic polymer materials, easy dispersion in the organic polymer materials and capability of being used as a flame retardant for a large amount of organic polymer material products.
Detailed Description
The present invention will be described in further detail with reference to test examples and specific embodiments. It should not be construed that the scope of the above subject matter of the present invention is limited to the following embodiments, and all techniques realized based on the present invention are within the scope of the present invention.
Drawings
FIG. 1 is an XPS chart of modified aluminum hypophosphite in example 1 of the present invention;
example 1
A method of preparing a modified aluminum hypophosphite comprising the steps of:
(1) Dissolving 3.0g of melamine and 2.4g of formaldehyde into 2L of water to form a mixed solution, adjusting the pH value of the mixed solution to 9 by using sodium carbonate, and reacting for 3 hours at the temperature of 80 ℃ to obtain a melamine formaldehyde resin prepolymer solution;
(2) Adding 900g of aluminum sulfate octadecanoate into the melamine formaldehyde resin prepolymer solution, adding 1080g of sodium hypophosphite monohydrate after the aluminum sulfate octadecanoate is completely dissolved, and reacting for 4 hours at the temperature of 85 ℃ to obtain modified aluminum hypophosphite slurry;
(3) And (3) separating, purifying and drying the modified aluminum hypophosphite slurry to obtain a modified aluminum hypophosphite powder product.
Example 2
A method of preparing a modified aluminum hypophosphite comprising the steps of:
(1) Dissolving 1.0g of melamine and 0.5g of formaldehyde into 0.5L of water to form a mixed solution, adjusting the pH value of the mixed solution to 10 by using sodium carbonate, and reacting for 2 hours at the temperature of 90 ℃ to obtain a melamine formaldehyde resin prepolymer solution;
(2) Adding 250g of aluminum sulfate octadecanoate into the melamine formaldehyde resin prepolymer solution, adding 250g of sodium hypophosphite monohydrate after the aluminum sulfate octadecanoate is completely dissolved, and reacting for 5 hours at the temperature of 80 ℃ to obtain modified aluminum hypophosphite slurry;
(3) And (3) separating, purifying and drying the modified aluminum hypophosphite slurry to obtain a modified aluminum hypophosphite powder product.
Example 3
A method of preparing a modified aluminum hypophosphite comprising the steps of:
(1) Dissolving 4.0g of melamine and 4.0g of formaldehyde into 2L of water to form a mixed solution, adjusting the pH value of the mixed solution to 8 by using sodium carbonate, and reacting for 4 hours at the temperature of 70 ℃ to obtain a melamine formaldehyde resin prepolymer solution;
(2) Adding 800g of aluminum sulfate octadecanoate into the melamine formaldehyde resin prepolymer solution, adding 900g of sodium hypophosphite monohydrate after the aluminum sulfate octadecanoate is completely dissolved, and reacting for 3 hours at the temperature of 95 ℃ to obtain modified aluminum hypophosphite slurry;
(3) And (3) separating, purifying and drying the modified aluminum hypophosphite slurry to obtain a modified aluminum hypophosphite powder product.
Example 4
A method of preparing a modified aluminum hypophosphite comprising the steps of:
(1) Dissolving 4.0g of urea and 4g of formaldehyde into 2L of water to form a mixed solution, adjusting the pH value of the mixed solution to 9 by using sodium carbonate, and reacting for 3 hours at the temperature of 80 ℃ to obtain urea-formaldehyde resin prepolymer solution;
(2) Adding 1080g of sodium hypophosphite monohydrate into the urea resin prepolymer solution, adding 1132g of aluminum sulfate octadecanoate after the sodium hypophosphite monohydrate is completely dissolved, and reacting for 4 hours at the temperature of 85 ℃ to obtain modified aluminum hypophosphite slurry;
(3) And (3) separating, purifying and drying the modified aluminum hypophosphite slurry to obtain a modified aluminum hypophosphite powder product.
Example 5
A method of preparing a modified aluminum hypophosphite comprising the steps of:
(1) Dissolving 1.0g of urea and 0.75g of formaldehyde into 1L of water to form a mixed solution, adjusting the pH value of the mixed solution to 10 by using sodium carbonate, and reacting for 4 hours at the temperature of 85 ℃ to obtain a urea-formaldehyde resin prepolymer solution;
(2) Adding 600g of sodium hypophosphite monohydrate into the urea resin prepolymer solution, adding 600g of aluminum sulfate octadecanoate after the sodium hypophosphite monohydrate is completely dissolved, and reacting for 3 hours at the temperature of 95 ℃ to obtain modified aluminum hypophosphite slurry;
(3) And (3) separating, purifying and drying the modified aluminum hypophosphite slurry to obtain a modified aluminum hypophosphite powder product. .
Comparative example 1
Preparation of aluminum hypophosphite: 150ml of sodium hypophosphite monohydrate solution with the concentration of 8mol/L is added into 1000ml of water, 200ml of aluminum sulfate octadecanoate solution with the concentration of 8mol/L is added, the mixture is heated at 90 ℃ for reaction for 3 hours to obtain white precipitate, and the white precipitate is filtered, washed and dried to obtain an aluminum hypophosphite product.
Comparative example 2
A method of preparing a modified aluminum hypophosphite comprising the steps of:
(1) Dissolving 2.0g of melamine and 1.6g of formaldehyde into 1L of water to form a mixed solution, adjusting the pH value of the mixed solution to 9 by using sodium carbonate, and reacting for 3 hours at the temperature of 80 ℃ to obtain a melamine formaldehyde resin prepolymer solution;
(2) 380g of aluminum hypophosphite is directly added into the melamine formaldehyde resin prepolymer solution, and the reaction is carried out for 4 hours at the temperature of 85 ℃ to obtain modified aluminum hypophosphite slurry; the aluminum hypophosphite is the aluminum hypophosphite product of comparative example 1;
(3) And (3) separating, purifying and drying the modified aluminum hypophosphite slurry to obtain a modified aluminum hypophosphite powder product.
Comparative example 3
The aluminum hypophosphite product of comparative example 1 was modified by the preparation method of example 1 of patent CN107936296a to prepare a modified aluminum hypophosphite product.
Comparative example 4
A method of preparing a modified aluminum hypophosphite comprising the steps of:
(1) Adding 900g of aluminum sulfate octadecanoate into 2L of water, adding 1080g of sodium hypophosphite monohydrate after the aluminum sulfate octadecanoate is completely dissolved, and reacting for 4 hours at the temperature of 85 ℃ to obtain aluminum hypophosphite slurry;
(2) Adding 2.0g of melamine and 1.6g of formaldehyde into the aluminum hypophosphite slurry, and reacting for 3 hours at the temperature of 80 ℃ to obtain modified aluminum hypophosphite slurry;
(3) And (3) separating, purifying and drying the modified aluminum hypophosphite slurry to obtain a modified aluminum hypophosphite powder product.
Experimental example 1:
x-ray photoelectron scanning is carried out on the modified aluminum hypophosphite product prepared in the example 1 to obtain X-ray photoelectron spectrum (XPS) of the modified aluminum hypophosphite product as shown in figure 1, and specific data are shown in the following table, and a large amount of organic groups are grafted on the surface of the modified aluminum hypophosphite product prepared in the example 1 through the energy spectrum; al according to aluminum hypophosphite: p: after O=1:3:6 is subjected to atomic ratio, about 5.8% of the rest oxygen atoms are oxygen atoms in the organic group, and about 35% of the oxygen atoms are melamine formaldehyde resin groups containing carbon, nitrogen and oxygen, so that the compatibility and the dispersibility of aluminum hypophosphite and the organic polymer material are remarkably improved.
| Name of the name | Peak value (eV) | Atomic percent% |
| C1s | 284.78 | 24.46 |
| C1sScanA | 286.18 | 3.27 |
| C1sScanB | 288.78 | 0.49 |
| N1s | 399.75 | 1.07 |
| O1s | 531.52 | 44.76 |
| P2p | 149.92 | 19.48 |
| Al2p | 103.7 | 6.47 |
Experimental example 2
The yields of the final products prepared in examples 1 to 5 and comparative examples 1 to 4 were modified (twin screw extrusion, injection molding machine spline molding) by adding (adding 25% by mass of aluminum hypophosphite or modified aluminum hypophosphite+5% by mass of Melamine Cyanurate (MCA)) to thermoplastic vulcanizate (mountain-Du TPV 110) materials, and the mechanical properties of the modified TPV were examined (GB/T1040-1992) and flame retardant tested (UL 94) as follows:
| sequence number | Final product yield (%) | Tensile Strength (MPa) | Elongation at break (%) | UL94 rating (3.2 mm) |
| Example 1 | 95.7 | 6.8 | 785 | V0 |
| Example 2 | 94.8 | 6.7 | 748 | V0 |
| Example 3 | 93.6 | 6.8 | 768 | V0 |
| Example 4 | 94.3 | 6.6 | 770 | V0 |
| Example 5 | 95.2 | 6.7 | 756 | V0 |
| Comparative example 1 | 96.4 | 6.1 | 590 | V0 |
| Comparative example 2 | 88.7 | 6.3 | 643 | V0 |
| Comparative example 3 | 90.1 | 6.9 | 776 | V0 |
| Comparative example 4 | 92.7 | 6.4 | 695 | V0 |
| Pure TPV | - | 5.8 | ＞1200 | Stepless arrangement |
As can be seen from the results of experimental example 2, the modified aluminum hypophosphite products prepared in examples 1-5 have better compatibility with TPV, have good tensile strength improving effect on TPV and small reduction effect on elongation at break, and the yield is obviously improved because the modified aluminum hypophosphite products are prepared directly at one time; the aluminum hypophosphite product prepared in the comparative example 1 is not modified, has large influence on the mechanical properties of TPV, and is not suitable for mass addition; in comparative example 2, aluminum hypophosphite was not synthesized in the modification process, but an aluminum hypophosphite product was directly added, resulting in a significant reduction in modification effect, a reduction in compatibility with TPV, a significant influence on mechanical properties of TPV, and a significant reduction in final product yield (plus yield of aluminum hypophosphite preparation); in comparative example 3, aluminum hypophosphite is modified by adopting a method in the prior art, the modification effect is good, but the yield of the final product is obviously reduced; in comparative example 4, the addition sequence of the raw materials was changed, resulting in that the synthesis and modification of aluminum hypophosphite were not performed simultaneously, the modification effect was significantly reduced, the compatibility with TPV was reduced, the mechanical properties of TPV was significantly affected, and the final product yield was also reduced.
Experimental example 3
The particle size distribution of the products prepared in examples 1 to 5 and comparative examples 1 to 4 was counted as follows:
| sequence number | 5 μm or less | 5-10μm | 10-20μm | 20-30μm |
| Example 1 | 2.70％ | 68.37％ | 28.83％ | 0.10％ |
| Example 2 | 5.45％ | 65.23％ | 29.12％ | 0.20％ |
| Example 3 | 2.55％ | 70.23％ | 27.12％ | 0.10％ |
| Example 4 | 2.20％ | 68.69％ | 28.91％ | 0.20％ |
| Example 5 | 2.49％ | 68.32％ | 28.88％ | 0.31％ |
| Comparative example 1 | 2.98％ | 62.21％ | 30.51％ | 4.30％ |
| Comparative example 2 | 3.30％ | 62.20％ | 30.20％ | 4.30％ |
| Comparative example 3 | 2.44％ | 62.32％ | 30.14％ | 5.10％ |
| Comparative example 4 | 3.37％ | 64.21％ | 28.32％ | 4.10％ |
As shown by the statistical results of the particle size distribution in example 3, the particle sizes of the modified aluminum hypophosphite products prepared in examples 1-4 of the present invention are all distributed below 20 μm, and the particle sizes are mainly concentrated at about 5-10 μm, so that the distribution is uniform, while the particle sizes of the modified aluminum hypophosphite products prepared in comparative examples 1-4 are also partially distributed within the range of 20-30 μm due to the different preparation methods and processes, so that the uniformity of the particle sizes is obviously reduced, i.e., the particle size distribution of the modified aluminum hypophosphite products prepared in examples 1-4 is obviously narrower and more uniform.
Claims (8)
1. A method of preparing a modified aluminum hypophosphite comprising the steps of:
preparing a prepolymer solution; the prepolymer solution is melamine formaldehyde resin prepolymer solution or urea formaldehyde resin prepolymer solution; the preparation method of the melamine formaldehyde resin prepolymer solution comprises the following steps: dissolving melamine and formaldehyde into water to form a mixed solution, adjusting the pH value of the mixed solution to 8-10, and then reacting for 2-4 hours at the temperature of 70-90 ℃ to obtain a melamine formaldehyde resin prepolymer solution; the preparation method of the urea resin prepolymer solution comprises the following steps: dissolving urea and formaldehyde into water to form a mixed solution, adjusting the pH value of the mixed solution to 8-10, and reacting for 2-4 hours at the temperature of 70-90 ℃ to obtain urea-formaldehyde resin prepolymer solution;
adding sodium hypophosphite monohydrate and aluminum sulfate octadecanoate into the prepolymer solution, and reacting for 3-5 hours at the temperature of 80-95 ℃ to obtain modified aluminum hypophosphite slurry;
and (3) separating, purifying and drying the modified aluminum hypophosphite slurry to obtain a modified aluminum hypophosphite powder product.
2. The method for preparing modified aluminum hypophosphite according to claim 1, wherein the mass ratio of melamine and formaldehyde is 1:0.5-1.
3. The method for preparing modified aluminum hypophosphite according to claim 1, wherein the total mass of melamine and formaldehyde in the mixed solution is 0.1-2% by mass.
4. The method for preparing modified aluminum hypophosphite according to claim 1, wherein the mass ratio of urea to formaldehyde is 1:0.75-1.
5. The method for preparing modified aluminum hypophosphite according to claim 1, wherein the total mass of urea and formaldehyde in the mixed solution is 0.1-2% by mass.
6. The method for producing modified aluminum hypophosphite according to claim 1, wherein the mass ratio of aluminum sulfate octadecanoate to sodium hypophosphite monohydrate in the step (2) is 1:0.8-1.2.
7. The method for producing modified aluminum hypophosphite according to claim 1, wherein the mass ratio of the total mass of aluminum sulfate octadecanoate and sodium hypophosphite monohydrate added in the step (2) to the prepolymer solution is 5:4-10.
8. A modified aluminum hypophosphite product prepared by the method of any one of claims 1-7.
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