CN112707376B - Preparation method of fire-fighting-grade superfine ammonium dihydrogen phosphate - Google Patents
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- CN112707376B CN112707376B CN202110109536.7A CN202110109536A CN112707376B CN 112707376 B CN112707376 B CN 112707376B CN 202110109536 A CN202110109536 A CN 202110109536A CN 112707376 B CN112707376 B CN 112707376B
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Abstract
The invention relates to a preparation method of fire-fighting-grade ultrafine ammonium dihydrogen phosphate. The method comprises the following steps: adding the obtained ammonium dihydrogen phosphate solution into the assistant solution, and performing ultrasonic dispersion at 5-50 deg.C and ultrasonic power of 60-200W for 2-12min to obtain solid-liquid mixture; wherein, the volume ratio is that the ammonium dihydrogen phosphate solution and the auxiliary agent solution = 1-12; then the solid-liquid mixture is centrifuged at high speed and dried for 10 to 15 hours at the temperature of between 50 and 90 ℃; finally cooling, grinding and screening to obtain the finished product of the fire-fighting-grade superfine ammonium dihydrogen phosphate. The invention has low production cost, and the finished product index is higher than that of the current commercial powdery ammonium dihydrogen phosphate product.
Description
Technical Field
The invention belongs to the field of fire extinguishing agents, and relates to a preparation method of fire-fighting-grade ultrafine ammonium dihydrogen phosphate.
Background
With the gradual elimination of the Halon fire extinguishing agent, the superfine dry powder fire extinguishing agent as a substitute of the Halon fire extinguishing agent has become a hot point of research. The superfine ammonium phosphate fire extinguishing agent has high fire extinguishing efficiency and is environment friendly, so that the superfine ammonium phosphate fire extinguishing agent becomes one of the most ideal substitutes of the Halon fire extinguishing agent.
The main fire extinguishing component in the superfine ammonium phosphate dry powder fire extinguishing agent is ammonium dihydrogen phosphate, the requirements on the quality and the granularity of the ammonium dihydrogen phosphate are higher, at present, the superfine ammonium dihydrogen phosphate is mainly produced by a physical crushing method, but the production cost is higher, the granularity distribution is not uniform, and the crystal structure of the ammonium dihydrogen phosphate is easy to damage.
Cinnabar and the like (superfine ammonium dihydrogen phosphate preparation new process research [ D ]. Nanjing: nanjing university of physical and chemical industries, 2009; zhang Xiaojing et al (preparation and application of ultrafine spherical hollow ammonium phosphate fire-extinguishing powder [ J ]. Chinese powder technology, 2010, 16 (2): 34-38.) adopt a spray drying device to prepare spherical hollow ultrafine ammonium dihydrogen phosphate powder by two spray drying methods of centrifugation and air flow, wherein the product prepared by the air flow spray drying method has small but poor uniformity, and the sample prepared by the centrifugal spraying method has uniform but large particle size.
Disclosure of Invention
The invention aims to provide a preparation method of fire-fighting-grade ultrafine ammonium dihydrogen phosphate aiming at the difficult problem of production of ultrafine ammonium dihydrogen phosphate in the prior art. The method adopts an anti-solvent ultrasonic method to prepare the superfine ammonium dihydrogen phosphate powder, and obtains the novel preparation method of the fire-fighting grade ammonium dihydrogen phosphate superfine powder by controlling the conditions of low ammonium dihydrogen phosphate concentration, solvent anti-solvent ratio (1. The invention has low production cost, and the finished product index is higher than that of the current commercial powdery ammonium dihydrogen phosphate product.
The technical scheme of the invention is as follows:
a preparation method of fire-fighting-grade ultrafine ammonium dihydrogen phosphate comprises the following steps:
a. adding ammonium dihydrogen phosphate with the purity of more than or equal to 99.0% into deionized water to obtain an ammonium dihydrogen phosphate solution; wherein the initial concentration of ammonium dihydrogen phosphate is 0.1-2.75mol/L;
b. adding the obtained ammonium dihydrogen phosphate solution into the assistant solution, and performing ultrasonic dispersion at 5-50 deg.C for 2-12min to obtain solid-liquid mixture;
wherein, the volume ratio is that the ammonium dihydrogen phosphate solution and the auxiliary agent solution = 1-12;
the solvent of the auxiliary agent solution is absolute ethyl alcohol, and the auxiliary agent is a crystal form control agent and a dispersing agent; the auxiliary agent is added in the form of aqueous solution, the concentration of the crystal form control agent solution is 1-3% by mass, and the concentration of the dispersing agent solution is 1-3 mL/100mL of water; adding 1mL of crystal form control agent solution and 1mL of dispersant solution into every 10-120mL of absolute ethyl alcohol; preferably, 1mL of crystal form control agent solution and 1mL of dispersant solution are added into every 60mL of absolute ethyl alcohol;
c. centrifuging the solid-liquid mixture at high speed, and drying at 50-90 ℃ for 10-15 hours;
d. and d, cooling, grinding and screening the dried material obtained in the step c to obtain the finished product of the fire-fighting-grade superfine ammonium dihydrogen phosphate.
In the step b, the ultrasonic power is 60-200W.
The crystal form control agent is sucrose; the dispersing agent is fatty alcohol-polyoxyethylene ether.
In the step c, the high-speed centrifugal rotating speed is 6000 to 12000r/min.
The granularity of the finished product of the fire-fighting ammonium dihydrogen phosphate is less than 0.006mm.
The finished product of the fire-fighting ammonium dihydrogen phosphate has the fluidity/s of less than 7.0 and the moisture content of less than 0.25 percent by mass.
The invention has the beneficial effects that:
in addition, a scanning electron microscope and laser granularity analysis are carried out on finished ammonium dihydrogen phosphate powder prepared by an ultrasonic anti-solvent crystallization method, and the result shows that the particle size is 6 mu m, and the particle size is smaller compared with the particle size obtained by methods such as spray drying; XRD test is carried out on the prepared product, and the result shows that the product has the same property with the raw material, and compared with a physical crushing method, the crystal structure of ammonium dihydrogen phosphate is not damaged. In addition, the invention has the important characteristics that the invention adopts low-temperature and ultrasonic operation, adds a certain amount of crystal form control agent and dispersant, and then creates unique conditions for preparing ammonium dihydrogen phosphate powder with fine granularity and lower water content through high-speed centrifugation and drying. The invention obtains a novel preparation method of fire-fighting-grade ammonium dihydrogen phosphate superfine powder through the design of the process and the control of the parameters, the method has low production cost, and the finished product index is higher than that of the current commercial powdery ammonium dihydrogen phosphate product (the powder granularity is less than 0.006mm, the fluidity/s is less than 7.0, and the moisture content is less than 0.25 percent), and the method has good market competitive advantage in the dry powder extinguishing agent and is worthy of popularization and application.
Drawings
FIG. 1 is a scanning electron micrograph of the product obtained in example 1; wherein FIG. 1a is a SEM of a product at a scale of 30 μm; FIG. 1b is a SEM of the product at 5 μm scale;
FIG. 2 is a laser particle size analysis chart of the product obtained in example 1;
FIG. 3 is the XRD pattern of the product obtained in example 3;
Detailed Description
The invention can be embodied in the following manner:
a preparation method of fire-fighting-grade superfine ammonium dihydrogen phosphate comprises the following steps:
a. dissolving ammonium dihydrogen phosphate raw material with the purity of more than or equal to 99.0 percent by using deionized water and preparing a series of ammonium dihydrogen phosphate solutions with different concentrations; the initial concentration of ammonium dihydrogen phosphate is 0.1-2.75mol/L;
b. preparing an auxiliary agent solution: adding 1mL of crystal form control agent solution and 1mL of dispersing agent solution into every 60mL of absolute ethyl alcohol; wherein, the volume percentage concentration of the dispersant solution is 1 to 3 percent, and the mass percentage concentration of the crystal form control agent solution is 1 to 3 percent;
c. b, adding a proper amount of the ammonium dihydrogen phosphate solution obtained in the step a into anhydrous ethanol with an anti-solvent ratio of 1-1; the reaction temperature is 5-50 ℃, the ultrasonic power is 60-200W, and the ultrasonic time is 2-12min;
d. centrifuging the crystallized mixture at high speed of 6000-12000r/min, and drying ammonium dihydrogen phosphate after centrifuging; the drying temperature is 50-90 ℃;
e. cooling, grinding and screening the dried material in the step c to obtain finished product fire-fighting-grade superfine ammonium dihydrogen phosphate; the granularity of the finished fire-fighting ammonium dihydrogen phosphate superfine powder is less than 0.01mm, the fluidity/s is less than 7.0, and the water content is 0.1-0.25 percent by mass.
The technical solution of the present invention is further illustrated by the following examples.
Example 1
1) Dissolving an ammonium dihydrogen phosphate raw material with the purity of more than or equal to 99.0 percent by using deionized water and preparing an ammonium dihydrogen phosphate solution with the initial concentration of 0.5 mol/L;
2) Adding 1mL of sucrose solution with the mass percentage concentration of 1% and 1mL of fatty alcohol-polyoxyethylene ether solution with the volume percentage concentration of 1% into 60mL of anhydrous ethanol, then adding 10mL of prepared ammonium dihydrogen phosphate solution into the 60mL of anhydrous ethanol (solvent-antisolvent ratio (1; obtaining a crystalline mixture;
3) Centrifuging the crystallized mixture at 6000r/min, and drying the ammonium dihydrogen phosphate after centrifuging at 80 deg.C;
4) And cooling the dried material to normal temperature, grinding and screening to obtain the finished product of the fire-fighting-grade superfine ammonium dihydrogen phosphate. The product index is shown in table 1:
the powder particle size is tested by using an Euramerican LS-POP6 laser particle size analyzer.
The fluidity test adopts a glass sand bell test method introduced in GB4066-2017, the dry powder extinguishing agent is allowed to fall under the action of gravity, and the time of the dry powder extinguishing agent passing through the middle of the neck opening of the glass sand bell is recorded, so that the fluidity of the dry powder extinguishing agent is measured.
The water content of the powder is tested by adopting a method for testing the water content in GA 578-2005 ultrafine dry powder extinguishing agent, and the method comprises the following steps: weighing 2g of superfine dry powder extinguishing agent sample in a weighing bottle with constant weight to be accurate to 0.2mg, putting the weighing bottle in a vacuum drying oven with the temperature (50 Shi 2) DEG C and the vacuum degree (O.095-0.096) MPa for 1h without a cover, taking out the weighing bottle, covering the weighing bottle, putting the weighing bottle in a drier, standing for 15min, weighing to be accurate to 0.2mg.
The water content x is calculated as follows,
x＝(m 1 -m 2 )/m 1 ×100％
in the formula:
m 1 -mass of the superfine dry powder extinguishing agent sample before drying in grams (g);
m 2 -the mass of the dried superfine dry powder extinguishing agent sample, in grams (g).
TABLE 1 example product index
| Number of | Particle size/mm | Fluidity/s | The water content is% |
| 1# product | 0.0062 | 6.5 | 0.18 |
| 2# finished product | 0.0061 | 6.6 | 0.20 |
| 3# finished product | 0.0058 | 6.6 | 0.21 |
Example 2
1) Dissolving an ammonium dihydrogen phosphate raw material with the purity of more than or equal to 99.0 percent by using deionized water and preparing an ammonium dihydrogen phosphate solution with the initial concentration of 1.5 mol/L;
2) Adding 1mL of sucrose solution with the mass percentage concentration of 2% and 1mL of fatty alcohol-polyoxyethylene ether solution with the volume percentage concentration of 1% into 70mL of absolute ethyl alcohol, then adding 10mL of prepared ammonium dihydrogen phosphate solution into the 70mL of absolute ethyl alcohol (solvent-antisolvent ratio (1; obtaining a solid-liquid mixture;
3) Centrifuging the solid-liquid mixture at 8000r/min at high speed, and oven drying ammonium dihydrogen phosphate after centrifuging at 65 deg.C;
4) And cooling, grinding and screening the dried material to obtain the finished product of the fire-fighting-grade superfine ammonium dihydrogen phosphate. The product index is shown in table 2:
TABLE 2 product index of example two
| Numbering | Particle size/mm | Fluidity/s | Has water content of% |
| 1# finished product | 0.0068 | 5.9 | 0.17 |
| 2# finished product | 0.0065 | 6.2 | 0.15 |
| 3# finished product | 0.0066 | 6.0 | 0.20 |
Example 3
1) Dissolving an ammonium dihydrogen phosphate raw material with the purity of more than or equal to 99.0 percent by using deionized water and preparing an ammonium dihydrogen phosphate solution with the initial concentration of 2.75mol/L;
2) Adding 1mL of sucrose solution with the mass percentage concentration of 2% and 1mL of fatty alcohol-polyoxyethylene ether solution with the volume percentage concentration of 2% into 30mL of absolute ethyl alcohol, then adding 10mL of prepared ammonium dihydrogen phosphate solution into the 30mL of absolute ethyl alcohol (solvent-antisolvent ratio (1: 3)), controlling the reaction temperature to be 25 ℃, starting ultrasonic reaction, wherein the ultrasonic power is 150W, and the ultrasonic time is 6min; obtaining a solid-liquid mixture;
3) Centrifuging the solid-liquid mixture at 10000r/min at high speed, and drying the ammonium dihydrogen phosphate after centrifuging at 90 ℃;
4) And cooling, grinding and screening the dried material to obtain the finished product of the fire-fighting-grade superfine ammonium dihydrogen phosphate. Product indices are shown in table 3:
table 3 example 3 product index
| Number of | Particle size/mm | Fluidity/s | The water content is% |
| 1# finished product | 0.0065 | 6.2 | 0.15 |
| 2# finished product | 0.0068 | 6.3 | 0.18 |
| 3# finished product | 0.0069 | 6.6 | 0.16 |
The invention is not the best known technology.
Claims (2)
1. A preparation method of fire-fighting-grade ultrafine ammonium dihydrogen phosphate is characterized by comprising the following steps:
a. adding ammonium dihydrogen phosphate with the purity of more than or equal to 99.0% into deionized water to obtain an ammonium dihydrogen phosphate solution; wherein the initial concentration of ammonium dihydrogen phosphate is 0.5-2.75mol/L;
b. adding the obtained ammonium dihydrogen phosphate solution into the assistant solution, and performing ultrasonic dispersion at 5-50 deg.C for 2-12min to obtain solid-liquid mixture;
wherein the volume ratio of the ammonium dihydrogen phosphate solution to the auxiliary agent solution is 1 to 12;
the solvent of the auxiliary agent solution is absolute ethyl alcohol, and the auxiliary agent is a crystal form control agent and a dispersing agent; the auxiliary agent is added in the form of aqueous solution, the concentration of the crystal form control agent solution is 1-3% by mass, and the concentration of the dispersing agent solution is 1-3mL/100 mL of water; adding 1mL of crystal form control agent solution and 1mL of dispersant solution into every 10-80mL of absolute ethanol;
c. centrifuging the solid-liquid mixture at a high speed, and drying for 10 to 15 hours at the temperature of 50-90 ℃;
d. cooling, grinding and screening the dried material in the step c to obtain finished product fire-fighting-grade superfine ammonium dihydrogen phosphate;
the crystal form control agent is sucrose; the dispersing agent is fatty alcohol-polyoxyethylene ether;
the granularity of the finished product of the fire-fighting ammonium dihydrogen phosphate is less than 0.006mm;
the fluidity/s of the finished product of the fire-fighting ammonium dihydrogen phosphate is less than 7.0, and the water content is less than 0.25 percent by mass;
in the step b, the ultrasonic power is 60-200W;
in the step c, the high-speed centrifugal rotating speed is 6000 to 12000r/min.
2. The method for preparing fire-fighting grade ultra-fine ammonium dihydrogen phosphate as claimed in claim 1, wherein 1mL of crystal form control agent solution and 1mL of dispersing agent solution are added per 60mL of absolute ethyl alcohol.
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