CN112619020B - Method for preparing rare earth element composite high-efficiency superfine powder fire extinguishing agent by spray drying method - Google Patents

Method for preparing rare earth element composite high-efficiency superfine powder fire extinguishing agent by spray drying method Download PDF

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CN112619020B
CN112619020B CN202011511208.1A CN202011511208A CN112619020B CN 112619020 B CN112619020 B CN 112619020B CN 202011511208 A CN202011511208 A CN 202011511208A CN 112619020 B CN112619020 B CN 112619020B
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extinguishing agent
fire extinguishing
rare earth
earth element
powder
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CN112619020A (en
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周晓猛
李秀涛
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Tianjin Hangda Yian Technology Development Co ltd
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Civil Aviation University of China
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    • AHUMAN NECESSITIES
    • A62LIFE-SAVING; FIRE-FIGHTING
    • A62DCHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
    • A62D1/00Fire-extinguishing compositions; Use of chemical substances in extinguishing fires
    • A62D1/0007Solid extinguishing substances
    • A62D1/0014Powders; Granules

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  • General Chemical & Material Sciences (AREA)
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Abstract

A method for preparing rare earth element composite high-efficiency superfine powder fire extinguishing agent by a spray drying method. The method comprises the steps of refining and mixing a rare earth element compound and a powdery fire extinguishing agent base material by a spray drying and crushing method, adding fire extinguishing agent auxiliary materials, and then carrying out surface modification by using emulsified silicone oil to obtain the high-efficiency superfine powdery fire extinguishing agent; meanwhile, in order to solve the problem of hollow structure of the powder particles, the invention adopts the rare earth element compound which has smaller particle size and is insoluble in water, and can form solid composite particles of the powder extinguishing agent base material coated with the rare earth element compound in the spray drying process. The method further improves the fire extinguishing performance of the composite fire extinguishing agent by utilizing the high-efficiency fire extinguishing performance of the rare earth element, and forms solid powder particles of the powder fire extinguishing agent base material coated with the rare earth element compound by utilizing a spray drying and crushing method, so that the particle size of the raw materials can be reduced, the fire extinguishing agent raw materials are mixed more uniformly, and the problem of low bulk density of the powder material prepared by the traditional spray drying method can be solved.

Description

Method for preparing rare earth element composite high-efficiency superfine powder fire extinguishing agent by spray drying method
Technical Field
The invention belongs to the technical field of preparation of superfine powder fire extinguishing agents, and particularly relates to a method for preparing a rare earth element composite efficient superfine powder fire extinguishing agent by a spray drying method.
Background
The powder fire extinguishing agent is considered to be one of potential substitutes of a 'Halon' fire extinguishing agent due to the excellent characteristics of high fire extinguishing efficiency and low ODP and GWP values. The effective components of the existing powder fire extinguishing agent are mainly phosphate and carbonate, although the fire extinguishing performance of the fire extinguishing agent can be improved to a certain extent by refining the particle size of the fire extinguishing agent, the fire extinguishing performance of the superfine powder fire extinguishing agent (particularly the particle size of the superfine powder fire extinguishing agent is smaller than the limit particle size of the fire extinguishing agent) reaches the limit basically. Therefore, it is necessary to develop a new method for further improving the fire extinguishing performance of the ultrafine powder fire extinguishing agent.
The rare earth compound is a good flame-retardant heat-insulating material, and meanwhile, the rare earth (particularly lanthanum, cerium, yttrium, praseodymium, neodymium and the like) in China has the advantages of large reserves, large yield and low price. If the rare earth compound is compounded with the traditional powder extinguishing agent, the extinguishing performance of the powder extinguishing agent can be further improved through the synergistic extinguishing effect, the production cost of the powder extinguishing agent can not be obviously increased, and the powder extinguishing agent is convenient for industrial production and market popularization. Therefore, how to compound the rare earth compound with the traditional powder extinguishing agent to prepare the rare earth element compounded superfine powder extinguishing agent is the key for further improving the fire extinguishing performance of the existing powder extinguishing agent.
The spray drying method is a common method for preparing powder materials, but as the droplet particles are firstly carried out from outside to inside in the drying process, a hollow structure or a porous structure is often formed by using solution for spray drying, so that the bulk density of the powder materials is greatly reduced, and the performance of the dry powder extinguishing agent is influenced.
Disclosure of Invention
In order to solve the problems, the invention aims to provide a method for preparing a rare earth element composite high-efficiency superfine powder fire extinguishing agent by a spray drying method.
In order to achieve the aim, the method for preparing the rare earth element composite high-efficiency superfine powder fire extinguishing agent by the spray drying method provided by the invention comprises the following steps in sequence:
(1) adding the powder fire extinguishing agent base material and the rare earth element compound into water according to a certain proportion to prepare a mixed solution, adding a dispersing agent, fully stirring, and performing spray drying on the mixed solution by using a spray dryer to prepare powder;
(2) uniformly mixing the powder and fire extinguishing agent auxiliary materials in proportion to prepare a mixture, then adding emulsified silicone oil and uniformly mixing, then carrying out surface hydrophobic treatment at the temperature of 40-70 ℃ for 5-10 hours, and finally drying at the temperature of 80-100 ℃ for 1-2 hours to obtain the high-efficiency superfine powder fire extinguishing agent.
In the step (1), the powder fire extinguishing agent base material is selected from at least one of ammonium monohydrogen phosphate, ammonium dihydrogen phosphate, potassium dihydrogen phosphate, sodium bicarbonate and potassium bicarbonate.
In the step (1), the rare earth element compound is at least one selected from lanthanum carbonate, lanthanum phosphate, lanthanum oxide, cerium carbonate, cerium phosphate, cerium oxide, yttrium carbonate, yttrium phosphate, yttrium oxide, praseodymium carbonate, praseodymium phosphate, praseodymium oxide, neodymium carbonate, neodymium phosphate and neodymium oxide, and the average particle size of the rare earth element compound is less than or equal to 1 μm.
In the step (1), the dispersant is at least one selected from propylene glycol methyl ether, dipropylene glycol methyl ether, polypropylene pyrrolidone and sodium dodecyl benzene sulfonate.
In the step (1), the mass ratio of the powder fire extinguishing agent base material to the rare earth element compound is 80-99: 1-20; the total mass of the powder extinguishing agent base material and the rare earth element compound accounts for 20-60% of the total mass of the mixed solution; the addition amount of the dispersing agent accounts for 1-3% of the total mass of the mixed solution; wherein the outlet temperature of the spray dryer is 70-110 ℃.
In the step (2), the fire extinguishing agent auxiliary material is selected from at least one of zeolite, perlite, magnesite, mica powder, talcum powder, bentonite and hydrophobic white carbon black.
In the step (2), the mass ratio of the powder to the fire extinguishing agent auxiliary material is 80-90: 10-20; the addition amount of the emulsified silicone oil accounts for 0.1-2% of the total mass of the mixture.
The invention provides a method for preparing a rare earth element composite high-efficiency superfine powder extinguishing agent by a spray drying method, which mainly adopts the technical principle that: the rare earth element compound and the powder fire extinguishing agent base material are finely mixed by a spray drying and crushing method, and are added with fire extinguishing agent auxiliary materials and then are subjected to surface modification by emulsified silicone oil, so that the high-efficiency superfine powder fire extinguishing agent is obtained; meanwhile, in order to solve the problem of hollow structure of the powder particles, the invention adopts the rare earth element compound which has smaller particle size and is insoluble in water, and can form solid composite particles of the powder extinguishing agent base material coated with the rare earth element compound in the spray drying process. The method further improves the fire extinguishing performance of the composite fire extinguishing agent by utilizing the high-efficiency fire extinguishing performance of the rare earth element, and forms solid powder particles of the powder fire extinguishing agent base material coated with the rare earth element compound by utilizing a spray drying and crushing method, so that the particle size of the raw materials can be reduced, the fire extinguishing agent raw materials are mixed more uniformly, and the problem of low bulk density of the powder material prepared by the traditional spray drying method can be solved.
Compared with the prior art, the method for preparing the rare earth element composite high-efficiency superfine powder fire extinguishing agent by the spray drying method has the following effects: (1) the superfine powder fire extinguishing agent prepared by the invention contains rare earth elements, and the fire extinguishing efficiency of the fire extinguishing agent can be effectively improved through the synergistic fire extinguishing effect; (2) the superfine fire extinguishing composite particles with the fire extinguishing agent main material wrapped by the rare earth compound are prepared by a spray drying method, so that the rare earth element and the fire extinguishing agent main material are more tightly compounded, and the particle size is smaller; (3) the invention has simple operation method, low cost of raw materials and high fire extinguishing performance of the fire extinguishing agent, and can realize large-scale industrial production.
Detailed Description
The present invention is further described in the following description of the specific embodiments, which is not intended to limit the invention, but various modifications and improvements can be made by those skilled in the art according to the basic idea of the invention, within the scope of the invention, as long as they do not depart from the basic idea of the invention.
Example 1
The method for preparing the rare earth element composite high-efficiency superfine powder fire extinguishing agent by the spray drying method provided by the embodiment comprises the following steps in sequence:
(1) adding ammonium dihydrogen phosphate and lanthanum phosphate into water according to a mass ratio of 93:5 to prepare a mixed solution, wherein the total mass of the ammonium dihydrogen phosphate and the lanthanum phosphate accounts for 55% of the total mass of the mixed solution, adding sodium dodecyl benzene sulfonate accounting for 1.2% of the total mass of the mixed solution as a dispersing agent, fully stirring, and performing spray drying on the mixed solution by using a spray dryer to prepare powder; wherein the outlet temperature of the spray dryer is 100 ℃;
(2) uniformly mixing the powder and bentonite according to the mass ratio of 85:15 to prepare a mixture, then adding emulsified silicone oil accounting for 1% of the total mass of the mixture, uniformly mixing, performing surface hydrophobic treatment at 55 ℃ for 8, and finally drying at 100 ℃ for 2 hours to obtain the high-efficiency superfine powder extinguishing agent.
Through particle size analysis and test, the particle size of the high-efficiency superfine powder extinguishing agent provided by the embodiment is 2 μm; through the test of a Cup-type burner (Cup-burner), the fire extinguishing concentration of the high-efficiency superfine powder fire extinguishing agent to standard methane fire is 61g/m-3. Under the same experimental conditions, the fire extinguishing concentration of the superfine dry powder extinguishing agent without the rare earth compound to the standard methane fire is 146g/m-3
Example 2
The method for preparing the rare earth element composite high-efficiency superfine powder fire extinguishing agent by the spray drying method provided by the embodiment comprises the following steps in sequence:
(1) adding ammonium monohydrogen phosphate and cerium oxide into water according to a mass ratio of 93:7 to prepare a mixed solution, wherein the total mass of the ammonium monohydrogen phosphate and the cerium phosphate accounts for 50% of the total mass of the mixed solution, adding polypropylene pyrrolidone accounting for 1% of the total mass of the mixed solution as a dispersing agent, fully stirring, and performing spray drying on the mixed solution by using a spray dryer to prepare powder; wherein the outlet temperature of the spray dryer is 100 ℃;
(2) uniformly mixing the powder and zeolite according to a mass ratio of 85:15 to prepare a mixture, then adding emulsified silicone oil accounting for 1% of the total mass of the mixture, uniformly mixing, performing surface hydrophobic treatment at 55 ℃ for 8, and finally drying at 100 ℃ for 2 hours to obtain the high-efficiency superfine powder extinguishing agent.
Through particle size analysis and test, the particle size of the high-efficiency superfine powder extinguishing agent provided by the embodiment is 2.6 mu m; through the test of a Cup-type burner (Cup-burner), the fire extinguishing concentration of the high-efficiency superfine powder fire extinguishing agent to standard methane fire is 55g/m-3. Under the same experimental conditions, the fire extinguishing concentration of the superfine dry powder extinguishing agent without the rare earth compound to the standard methane fire is 146g/m-3
Example 3
The method for preparing the rare earth element composite high-efficiency superfine powder fire extinguishing agent by the spray drying method provided by the embodiment comprises the following steps in sequence:
(1) adding potassium dihydrogen phosphate and yttrium oxide into water according to the mass ratio of 93:6 to prepare a mixed solution, wherein the total mass of the potassium dihydrogen phosphate and the yttrium oxide accounts for 50% of the total mass of the mixed solution, adding dipropylene glycol methyl ether accounting for 1% of the total mass of the mixed solution as a dispersing agent, fully stirring, and performing spray drying on the mixed solution by using a spray dryer to prepare powder; wherein the outlet temperature of the spray dryer is 100 ℃;
(2) uniformly mixing the powder and perlite according to the mass ratio of 85:15 to prepare a mixture, then adding emulsified silicone oil accounting for 1% of the total mass of the mixture, uniformly mixing, performing surface hydrophobic treatment at 55 ℃ for 8, and finally drying at 100 ℃ for 2 hours to obtain the high-efficiency superfine powder extinguishing agent.
Through particle size analysis and test, the particle size of the high-efficiency superfine powder extinguishing agent provided by the embodiment is 3 μm; through the test of a Cup-type burner (Cup-burner), the fire extinguishing concentration of the high-efficiency superfine powder fire extinguishing agent to standard methane fire is 55g/m-3. Under the same experimental conditions, the fire extinguishing concentration of the superfine dry powder extinguishing agent without the rare earth compound to the standard methane fire is 146g/m-3
Example 4
The method for preparing the rare earth element composite high-efficiency superfine powder fire extinguishing agent by the spray drying method provided by the embodiment comprises the following steps in sequence:
(1) adding sodium bicarbonate and praseodymium phosphate into water according to a mass ratio of 93:7 to prepare a mixed solution, wherein the total mass of the sodium bicarbonate and the praseodymium phosphate accounts for 50% of the total mass of the mixed solution, adding polypropylene pyrrolidone accounting for 1% of the total mass of the mixed solution as a dispersing agent, fully stirring, and performing spray drying on the mixed solution by using a spray dryer to prepare powder; wherein the outlet temperature of the spray dryer is 100 ℃;
(2) uniformly mixing the powder and mica powder according to the mass ratio of 85:15 to prepare a mixture, then adding emulsified silicone oil accounting for 1% of the total mass of the mixture, uniformly mixing, performing surface hydrophobic treatment at 55 ℃ for 8, and finally drying at 100 ℃ for 2 hours to obtain the high-efficiency superfine powder extinguishing agent.
Through particle size analysis and test, the particle size of the high-efficiency superfine powder extinguishing agent provided by the embodiment is 2.1 mu m; through the test of a Cup-type burner (Cup-burner), the fire extinguishing concentration of the high-efficiency superfine powder fire extinguishing agent to standard methane fire is 51g/m-3. Under the same experimental conditions, the fire extinguishing concentration of the superfine dry powder extinguishing agent without the rare earth compound to the standard methane fire is 146g/m-3
Example 5
The method for preparing the rare earth element composite high-efficiency superfine powder fire extinguishing agent by the spray drying method provided by the embodiment comprises the following steps in sequence:
(1) adding potassium bicarbonate and neodymium carbonate into water according to the mass ratio of 93:7 to prepare a mixed solution, wherein the total mass of the potassium bicarbonate and the neodymium carbonate accounts for 50% of the total mass of the mixed solution, adding propylene glycol methyl ether accounting for 1% of the total mass of the mixed solution as a dispersing agent, fully stirring, and performing spray drying on the mixed solution by using a spray dryer to prepare powder; wherein the outlet temperature of the spray dryer is 100 ℃;
(2) uniformly mixing the powder and mica powder according to the mass ratio of 85:15 to prepare a mixture, then adding emulsified silicone oil accounting for 1% of the total mass of the mixture, uniformly mixing, performing surface hydrophobic treatment at 55 ℃ for 8, and finally drying at 100 ℃ for 2 hours to obtain the high-efficiency superfine powder extinguishing agent.
Through particle size analysis and test, the particle size of the high-efficiency superfine powder extinguishing agent provided by the embodiment is 1.9 mu m; through the test of a Cup-type burner (Cup-burner), the fire extinguishing concentration of the high-efficiency superfine powder fire extinguishing agent to standard methane fire is 62g/m-3. Under the same experimental conditions, the fire extinguishing concentration of the superfine dry powder extinguishing agent without the rare earth compound to the standard methane fire is 146g/m-3

Claims (6)

1. A method for preparing a rare earth element composite high-efficiency superfine powder extinguishing agent by a spray drying method is characterized by comprising the following steps: the method comprises the following steps which are carried out in sequence:
(1) adding the powder fire extinguishing agent base material and the rare earth element compound into water according to a certain proportion to prepare a mixed solution, adding a dispersing agent, fully stirring, and performing spray drying on the mixed solution by using a spray dryer to prepare powder;
(2) uniformly mixing the powder and fire extinguishing agent auxiliary materials in proportion to prepare a mixture, then adding emulsified silicone oil and uniformly mixing, then performing surface hydrophobic treatment at the temperature of 40-70 ℃ for 5-10 hours, and finally drying at the temperature of 80-100 ℃ for 1-2 hours to obtain the high-efficiency superfine powder fire extinguishing agent;
in the step (1), the rare earth element compound is at least one selected from lanthanum carbonate, lanthanum phosphate, lanthanum oxide, cerium carbonate, cerium phosphate, cerium oxide, yttrium carbonate, yttrium phosphate, yttrium oxide, praseodymium carbonate, praseodymium phosphate, praseodymium oxide, neodymium carbonate, neodymium phosphate and neodymium oxide, and the average particle size of the rare earth element compound is less than or equal to 1 μm.
2. The method for preparing the rare earth element compounded high-efficiency superfine powder fire extinguishing agent by the spray drying method according to claim 1, which is characterized in that: in the step (1), the powder fire extinguishing agent base material is selected from at least one of ammonium monohydrogen phosphate, ammonium dihydrogen phosphate, potassium dihydrogen phosphate, sodium bicarbonate and potassium bicarbonate.
3. The method for preparing the rare earth element compounded high-efficiency superfine powder fire extinguishing agent by the spray drying method according to claim 1, which is characterized in that: in the step (1), the dispersant is at least one selected from propylene glycol methyl ether, dipropylene glycol methyl ether, polypropylene pyrrolidone and sodium dodecyl benzene sulfonate.
4. The method for preparing the rare earth element compounded high-efficiency superfine powder fire extinguishing agent by the spray drying method according to claim 1, which is characterized in that: in the step (1), the mass ratio of the powder fire extinguishing agent base material to the rare earth element compound is 80-99: 1-20; the total mass of the powder extinguishing agent base material and the rare earth element compound accounts for 20-60% of the total mass of the mixed solution; the addition amount of the dispersing agent accounts for 1-3% of the total mass of the mixed solution; wherein the outlet temperature of the spray dryer is 70-110 ℃.
5. The method for preparing the rare earth element compounded high-efficiency superfine powder fire extinguishing agent by the spray drying method according to claim 1, which is characterized in that: in the step (2), the fire extinguishing agent auxiliary material is selected from at least one of zeolite, perlite, magnesite, mica powder, talcum powder, bentonite and hydrophobic white carbon black.
6. The method for preparing the rare earth element compounded high-efficiency superfine powder fire extinguishing agent by the spray drying method according to claim 1, which is characterized in that: in the step (2), the mass ratio of the powder to the fire extinguishing agent auxiliary material is 80-90: 10-20; the addition amount of the emulsified silicone oil accounts for 0.1-2% of the total mass of the mixture.
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