CN108314063B - Preparation method of hydrophobic and oleophobic BC superfine dry powder extinguishing agent base material carbonate - Google Patents
Preparation method of hydrophobic and oleophobic BC superfine dry powder extinguishing agent base material carbonate Download PDFInfo
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- C—CHEMISTRY; METALLURGY
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- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
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- A62D1/00—Fire-extinguishing compositions; Use of chemical substances in extinguishing fires
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Abstract
The invention discloses a preparation method of hydrophobic and oleophobic BC superfine dry powder extinguishing agent base material carbonate. The method comprises the following steps: (1) crushing carbonate into 90% superfine powder with grain size not greater than 5 micron; (2) adding the superfine powder into an organic solution of a silane coupling agent at normal temperature for dipping treatment; (3) after the reaction is finished, carrying out suction filtration, washing, drying at high temperature, cooling, crushing and screening; (4) adding the treated dry superfine powder into fluorosilane organic solution for dipping treatment; (5) after the reaction is finished, performing suction filtration, washing, drying at high temperature, cooling, crushing and screening to obtain the hydrophobic and oleophobic superfine carbonate powder. The superfine powder prepared by the invention has excellent hydrophobic and oleophobic properties and high stability, can quickly extinguish oil fire when being used for preparing superfine dry powder extinguishing agent, and has the characteristics of high extinguishing efficiency and afterburning resistance.
Description
Technical Field
The invention relates to the field of dry powder extinguishing agents, in particular to a preparation method of hydrophobic and oleophobic BC type superfine dry powder extinguishing agent base material carbonate.
Background
With the gradual depletion of the halon fire extinguishing agent, the development of a clean and efficient and environment-friendly halon substitute fire extinguishing agent is urgently needed. Because the dry powder extinguishing agent has the advantages of high extinguishing efficiency, low toxicity, no pollution and the like, the dry powder extinguishing agent is one of the most ideal substitutes for the Halon extinguishing agent at present, wherein the BC dry powder extinguishing agent taking carbonate as a base material is widely applied to extinguishing liquid and gas fire, while the traditional carbonate dry powder extinguishing agent is easy to settle because most of the particle diameters are larger than the critical reaction particle diameter, the thermal decomposition speed of the traditional carbonate dry powder extinguishing agent is slow, the capacity of capturing free radicals is limited, the extinguishing efficiency is low, the fire extinguishing efficiency can be greatly improved by performing superfine treatment on the traditional carbonate dry powder extinguishing agent, but the carbonate is a substance which is particularly easy to absorb moisture and agglomerate, the refined powder is in an unstable state of energy because the specific surface area is increased, the surface energy is high, the powder is more easy to agglomerate to achieve a stable state, the agglomeration greatly reduces the fluidity of the powder, the fire extinguishing efficiency is seriously influenced by superfine treatment, so that the existing production process, namely the 'damp-proof' of carbonate, and the silicone oil hydrophobic film on the surface of the powder has strong lipophilicity, so that the powder is easy to sink into oil when extinguishing a B-type oil fire, the fire extinguishing effect is lost, and if residual flame exists near the oil surface, the whole oil surface can be immediately ignited, namely the're-ignition' phenomenon of the oil fire, so that the application range of the superfine dry powder fire extinguishing agent is limited. Therefore, the development of a novel superfine dry powder extinguishing agent with high extinguishing efficiency, namely, hydrophobic and oleophobic performance is a technical problem which is urgently needed to be solved at present, and the hydrophobic and oleophobic performance of the dry powder extinguishing agent substrate carbonate is the most key technical problem.
At present, the fluorocarbon surfactant is adopted at home and abroad to treat the dry powder fire extinguishing agent so as to achieve the purpose of afterburning resistance. For example, in the foreign patent US3553127, the dry powder extinguishing agent is immersed in the fluorocarbon surfactant organic solution, and the prepared carbonate dry powder extinguishing agent is insoluble in water, slightly soluble in oil, poor in anti-flammability, large in particle size and low in extinguishing efficiency. In addition, whether the method is suitable for BC type superfine dry powder extinguishing agents or not is not researched, so that the selection and treatment process of the surfactant are needed to be researched to realize the hydrophobic and oleophobic performance of the BC type superfine dry powder extinguishing agent.
Disclosure of Invention
The invention aims to provide a preparation method of hydrophobic and oleophobic BC type superfine dry powder extinguishing agent base material carbonate, and the prepared superfine carbonate powder has higher chemical stability and excellent hydrophobic and oleophobic properties.
The invention is realized by the following technical scheme:
a preparation method of hydrophobic and oleophobic BC superfine dry powder extinguishing agent base material carbonate comprises the following preparation steps:
(1) crushing carbonate into 90% superfine powder with grain size not greater than 5 micron;
(2) adding the superfine powder into an organic solution of a silane coupling agent at normal temperature for dipping treatment;
(3) after the reaction is finished, carrying out suction filtration, washing, drying at high temperature, cooling, crushing and screening;
(4) adding the treated dry superfine powder into fluorosilane organic solution for dipping treatment;
(5) after the reaction is finished, performing suction filtration, washing, drying at high temperature, cooling, crushing and screening to obtain the hydrophobic and oleophobic superfine carbonate powder.
The carbonate is sodium bicarbonate or potassium bicarbonate.
The silane coupling agent is polydimethylsiloxane, amino siloxane or epoxypropyl siloxane, the organic solvent of the silane coupling agent organic solution is any one or a mixture of more than two of acetone, normal hexane, isopropanol or methanol, and the weight percentage of each substance is 10-30% of superfine powder, 67-89% of organic solvent and 1-3% of silane coupling agent.
The fluorosilane is tridecafluorooctyltrimethoxysilane, heptadecafluorodecyltrimethoxysilane or perfluorodecyltriethoxysilane. The organic solvent of the fluorosilane organic solution is any one or a mixture of more than two of normal hexane, isopropanol, acetone or ethanol, and the weight percentage of each substance is 1-10% of the treated superfine powder, 89-98.9% of the organic solvent and 0.1-1% of fluorosilane.
The high-temperature drying temperature in the step (3) and the step (5) is 100-120 ℃.
In the step (2), the silane coupling agent organic solution is soaked and stirred for 1-2h at the speed of 1000rpm at normal temperature. And (4) dipping the fluorosilane organic solution at normal temperature at the speed of 1000rpm for 10-12 h.
Advantageous effects
Compared with the prior art, the preparation method of the hydrophobic and oleophobic BC superfine dry powder extinguishing agent base material carbonate has the following beneficial effects:
1. the invention adopts silane coupling agent to dip the superfine powder, which greatly improves the hydrophobicity of carbonate and the compatibility and dispersibility in organism system.
2. The fluorosilane adopted by the invention can be hydrolyzed to generate silicon hydroxyl which is subjected to dehydration condensation reaction with the hydroxyl on the surface of the powder and is bonded to the surface of the powder, the adhesive force is strong, and the adjacent hydroxyl among fluorosilane molecules are connected after water molecules are removed, so that a two-dimensional and three-dimensional net structure can be formed on the surface of the powder, and the chemical stability of the BC superfine dry powder extinguishing agent substrate carbonate powder after surface modification is good.
3. The method has the advantages of easily controlled process conditions, high repeatability, basically non-toxic volatile matters, safety, environmental protection and easy large-scale production.
4. The superfine powder prepared by the invention has excellent hydrophobic and oleophobic properties and high stability, can quickly extinguish oil fire when being used for preparing superfine dry powder extinguishing agent, and has the characteristics of high extinguishing efficiency and afterburning resistance.
Drawings
FIG. 1 is a schematic view showing the contact angle of ultra-fine sodium bicarbonate solution prepared in example 1;
FIG. 2 is a schematic view showing the contact angle of ultra-fine sodium bicarbonate oil prepared in example 1;
FIG. 3 is a schematic view showing the water contact angle of the ultra-fine potassium bicarbonate prepared in example 2;
FIG. 4 is a schematic drawing showing the contact angle of the ultra-fine potassium bicarbonate oil prepared in example 2;
FIG. 5 is a schematic view showing the contact angle of the ultra-fine sodium bicarbonate solution prepared in example 3;
fig. 6 is a schematic view of the contact angle of the ultra-fine sodium bicarbonate oil prepared in example 3.
Detailed Description
The present invention is further illustrated by the following examples, which are provided only for the purpose of illustration and are not intended to limit the scope of the invention.
Example 1 preparation of hydrophobic and oleophobic ultrafine sodium bicarbonate powder
(1) Crushing sodium bicarbonate into 90% superfine powder with particle size not greater than 5 μm by supersonic airflow pulverizer;
(2) adding the superfine powder into a methanol solution of gamma-aminopropyl triethoxysilane (KH550) at normal temperature for dipping treatment, and stirring at 1000rpm for 1h, wherein the weight percentage of each substance is that the superfine powder accounts for 10%, the methanol accounts for 89%, and the KH550 accounts for 1%;
(3) after the reaction is finished, performing suction filtration and washing, drying at the high temperature of 100 ℃, cooling, crushing, and sieving by a 400-target standard sample sieve;
(4) adding the treated superfine powder into acetone solution of tridecafluorooctyltriethoxysilane for dipping treatment, and stirring at the speed of 1000rpm for 10 hours, wherein the weight percentage of each substance is that the quantity of the superfine powder is 10 percent, the quantity of the acetone is 89 percent, and the quantity of the tridecafluorooctyltriethoxysilane is 1 percent;
(5) and after the reaction is finished, performing suction filtration, washing, drying at the high temperature of 100 ℃, cooling, crushing, screening and performance detection.
The performance of the prepared superfine powder is detected, and the characterization result is as follows:
(1) the powder contact angle was measured using an optical method contact angle/interfacial tension SL200KS contact angle tester, manufactured by co-industrial ltd, usa, wherein the contact angle was about 148 ° (see fig. 1) for water and about 139 ° (see fig. 2) for oil, which was RP-3 aviation kerosene.
(2) After the prepared superfine powder is respectively soaked in acid and alkali solutions with pH values of 2 and 12 for 48 hours, the contact angles of the powder, water and oil are kept unchanged.
(3) After the powder is respectively treated in a low-temperature air atmosphere at the temperature of minus 55 ℃ and a high-temperature air atmosphere at the temperature of 110 ℃ for 4 hours, the contact angles of the powder water and the oil are kept unchanged; the temperature impact test is carried out in a circulation mode from a low temperature section of minus 55 ℃ to a high temperature section of 70 ℃, the heat preservation time is 1h respectively, the conversion time is not more than 1min, the circulation frequency is 3 times, the water and oil contact angles are kept unchanged after the powder is treated, and the requirement of aviation environment can be met.
Example 2 preparation of hydrophobic and oleophobic ultra-fine Potassium bicarbonate powder
(1) Crushing potassium bicarbonate into 90% superfine powder with particle size not greater than 5 μm by supersonic airflow crusher;
(2) adding the superfine powder into acetone solution of gamma-glycidoxypropyltrimethoxysilane (KH560) at normal temperature for dipping treatment, and stirring at 1000rpm for 2h, wherein the weight percentage of each substance is that the superfine powder accounts for 10%, the acetone accounts for 67%, and the KH560 accounts for 3%;
(3) after the reaction is finished, performing suction filtration and washing, drying at the high temperature of 110 ℃, cooling, crushing, and screening by a 400-target standard sample sieve;
(4) adding the treated superfine powder into a normal hexane solution of heptadecafluorodecyltrimethoxysilane for dipping treatment, and stirring at the speed of 1000rpm for 12h, wherein the weight percentage of each substance is that the quantity of the superfine powder is 5%, the quantity of the normal hexane is 94.9%, and the quantity of the heptadecafluorodecyltrimethoxysilane is 0.1%;
(5) and after the reaction is finished, performing suction filtration, washing, drying at the high temperature of 110 ℃, cooling, crushing, screening and performance detection.
The performance of the prepared superfine powder is detected, and the characterization result is as follows:
(1) the powder contact angle was measured using an optical method contact angle/interfacial tension SL200KS contact angle tester, manufactured by co-industrial ltd, usa, wherein the contact angle was about 148 ° (see fig. 3) for water and about 136 ° (see fig. 4) for oil, which was RP-3 aviation kerosene.
(2) After the prepared superfine powder is respectively soaked in acid and alkali solutions with pH values of 2 and 12 for 48 hours, the contact angles of the powder, water and oil are kept unchanged.
(3) After the powder is respectively treated in a low-temperature air atmosphere at the temperature of minus 55 ℃ and a high-temperature air atmosphere at the temperature of 110 ℃ for 4 hours, the contact angles of the powder water and the oil are kept unchanged; the temperature impact test is carried out in a circulation mode from a low temperature section of minus 55 ℃ to a high temperature section of 70 ℃, the heat preservation time is 1h respectively, the conversion time is not more than 1min, the circulation frequency is 3 times, the water and oil contact angles are kept unchanged after the powder is treated, and the requirement of aviation environment can be met.
Example 3 preparation of hydrophobic and oleophobic ultrafine sodium bicarbonate powder
(1) Crushing sodium bicarbonate into 90% superfine powder with particle size not greater than 5 μm by supersonic airflow pulverizer;
(2) adding the superfine powder into a normal hexane solution of gamma-aminopropyl triethoxysilane (KH550) at normal temperature for dipping treatment, and stirring at 1000rpm for 2h, wherein the weight percentage of each substance is that the superfine powder amount is 30%, the normal hexane amount is 67%, and the KH550 amount is 3%.
(3) After the reaction is finished, performing suction filtration and washing, drying at the high temperature of 115 ℃, cooling, crushing, and screening by a 400-target standard sample sieve;
(4) adding the treated superfine powder into an ethanol solution of perfluorodecyl triethoxysilane for dipping treatment, and stirring at 1000rpm for 12h, wherein the weight percentage of each substance is that the superfine powder amount is 1%, the ethanol amount is 98.9%, and the perfluorodecyl triethoxysilane amount is 0.1%;
(5) and after the reaction is finished, performing suction filtration, washing, drying at the high temperature of 115 ℃, cooling, crushing, screening and performance detection.
The performance of the prepared superfine powder is detected, and the characterization result is as follows:
(1) the powder contact angle was measured using an optical method contact angle/interfacial tension SL200KS contact angle tester, manufactured by co-industrial ltd, usa, wherein the contact angle was about 140 ° (see fig. 5) for water and about 129 ° (see fig. 6) for oil, which was RP-3 aviation kerosene.
(2) After the prepared superfine powder is respectively soaked in acid and alkali solutions with pH values of 2 and 12 for 48 hours, the contact angles of the powder, water and oil are kept unchanged.
(3) After the powder is respectively treated in a low-temperature air atmosphere at the temperature of minus 55 ℃ and a high-temperature air atmosphere at the temperature of 110 ℃ for 4 hours, the contact angles of the powder water and the oil are kept unchanged; the temperature impact test is carried out in a circulation mode from a low temperature section of minus 55 ℃ to a high temperature section of 70 ℃, the heat preservation time is 1h respectively, the conversion time is not more than 1min, the circulation frequency is 3 times, the water and oil contact angles are kept unchanged after the powder is treated, and the requirement of aviation environment can be met.
Example 4 preparation of hydrophobic and oleophobic ultra-fine Potassium bicarbonate powder
(1) Crushing potassium bicarbonate into 90% superfine powder with particle size not greater than 5 μm by supersonic airflow crusher;
(2) adding the superfine powder into an isopropanol mixed solution of polydimethylsiloxane for dipping treatment at normal temperature, and stirring at the speed of 1000rpm for 1.5h, wherein the weight percentage of each substance is that the quantity of the superfine powder is 20%, the quantity of the isopropanol is 78%, and the quantity of the polydimethylsiloxane is 2%.
(3) After the reaction is finished, performing suction filtration and washing, drying at 120 ℃ in a high-temperature environment, cooling, crushing, and sieving by a 400-target standard sample sieve;
(4) adding the treated superfine powder into an isopropanol mixed solution of dodecafluoroheptyl propyl trimethoxy silane for dipping treatment, and stirring at the speed of 1000rpm for 11 hours, wherein the weight percentage of each substance is that the quantity of the superfine powder is 8 percent, the quantity of the isopropanol is 91.5 percent, and the quantity of the dodecafluoroheptyl propyl trimethoxy silane is 0.5 percent;
(5) and after the reaction is finished, performing suction filtration, washing, drying at 120 ℃ in a high-temperature environment, cooling, crushing, screening and performance detection.
The performance of the prepared superfine powder is detected, and the characterization result is as follows:
(1) the powder contact angle is tested by adopting an optical method contact angle/interfacial tension SL200KS contact angle tester manufactured by the United states Keno industry Co., Ltd, wherein the water contact angle and the oil contact angle both exceed 130 degrees (refer to figures 1-6), and the oil adopts RP-3 aviation kerosene.
(2) After the prepared superfine powder is respectively soaked in acid and alkali solutions with pH values of 2 and 12 for 48 hours, the contact angles of the powder, water and oil are kept unchanged.
(3) After the powder is respectively treated in a low-temperature air atmosphere at the temperature of minus 55 ℃ and a high-temperature air atmosphere at the temperature of 110 ℃ for 4 hours, the contact angles of the powder water and the oil are kept unchanged; the temperature impact test is carried out in a circulation mode from a low temperature section of minus 55 ℃ to a high temperature section of 70 ℃, the heat preservation time is 1h respectively, the conversion time is not more than 1min, the circulation frequency is 3 times, the water and oil contact angles are kept unchanged after the powder is treated, and the requirement of aviation environment can be met.
The embodiment shows that the superfine carbonate powder prepared by the method has good hydrophobic and oleophobic performances and high chemical stability.
The above description of the embodiments is only intended to facilitate the understanding of the method of the invention and its core idea. It should be noted that, for those skilled in the art, it is possible to make various improvements and modifications to the present invention without departing from the principle of the present invention, and those improvements and modifications also fall within the scope of the claims of the present invention.
Claims (9)
1. A preparation method of hydrophobic and oleophobic BC superfine dry powder extinguishing agent base material carbonate is characterized by comprising the following preparation steps:
(1) crushing carbonate into 90% superfine powder with grain size not greater than 5 micron;
(2) adding the superfine powder into an organic solution of a silane coupling agent at normal temperature for dipping treatment;
(3) after the reaction is finished, carrying out suction filtration, washing, drying at high temperature, cooling, crushing and screening;
(4) adding the treated dry superfine powder into fluorosilane organic solution for dipping treatment;
(5) after the reaction is finished, performing suction filtration, washing, drying at high temperature, cooling, crushing and screening to obtain hydrophobic and oleophobic superfine carbonate powder;
the fluorosilane in the step (4) is tridecafluorooctyltrimethoxysilane, tridecafluorooctyltriethoxysilane, heptadecafluorodecyltrimethoxysilane or perfluorodecyltriethoxysilane.
2. The preparation method of the hydrophobic and oleophobic BC superfine dry powder fire extinguishing agent substrate carbonate according to claim 1, characterized in that: the carbonate in the step (1) is sodium bicarbonate or potassium bicarbonate.
3. The preparation method of the hydrophobic and oleophobic BC superfine dry powder fire extinguishing agent substrate carbonate according to claim 1, characterized in that: in the step (2), the silane coupling agent is polydimethylsiloxane, aminosiloxane or epoxypropylsiloxane.
4. The preparation method of the hydrophobic and oleophobic BC superfine dry powder fire extinguishing agent substrate carbonate according to claim 1, characterized in that: the organic solvent of the silane coupling agent organic solution in the step (2) is any one or a mixture of more than two of acetone, normal hexane, isopropanol or methanol.
5. The preparation method of the hydrophobic and oleophobic BC superfine dry powder fire extinguishing agent substrate carbonate according to claim 1, characterized in that: in the step (2), the weight percentages of the substances are 10-30% of superfine powder, 67-89% of organic solvent and 1-3% of silane coupling agent.
6. The preparation method of the hydrophobic and oleophobic BC superfine dry powder fire extinguishing agent substrate carbonate according to claim 1, characterized in that: the organic solvent of the fluorosilane organic solution in the step (4) is any one or a mixture of more than two of n-hexane, isopropanol, acetone or ethanol.
7. The preparation method of the hydrophobic and oleophobic BC superfine dry powder fire extinguishing agent substrate carbonate according to claim 1, characterized in that: in the step (4), the weight percentages of all the substances are 1-10% of the treated superfine powder, 89-98.9% of the organic solvent and 0.1-1% of fluorosilane.
8. The preparation method of the hydrophobic and oleophobic BC superfine dry powder fire extinguishing agent substrate carbonate according to claim 1, characterized in that: the high-temperature drying temperature in the step (3) and the step (5) is 100-120 ℃.
9. The preparation method of the hydrophobic and oleophobic BC superfine dry powder fire extinguishing agent substrate carbonate according to claim 1, characterized in that: in the step (2), the silane coupling agent organic solution is soaked and stirred for 1-2h at the speed of 1000rpm at normal temperature; and (4) dipping the fluorosilane organic solution at normal temperature at the speed of 1000rpm for 10-12 h.
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| US3553127A (en) * | 1969-02-06 | 1971-01-05 | Ansul Co | Anti-reflash dry chemical agent |
| CN101434709A (en) * | 2008-12-09 | 2009-05-20 | 西安交通大学 | Preparation of silastic surface hydrophobic coating |
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| US3553127A (en) * | 1969-02-06 | 1971-01-05 | Ansul Co | Anti-reflash dry chemical agent |
| CN101434709A (en) * | 2008-12-09 | 2009-05-20 | 西安交通大学 | Preparation of silastic surface hydrophobic coating |
| CN103550901A (en) * | 2013-10-31 | 2014-02-05 | 中国科学技术大学苏州研究院 | Novel composite powdery fire extinguishing medium and preparation method thereof |
| CN104479172A (en) * | 2014-12-05 | 2015-04-01 | 黑龙江省润特科技有限公司 | Preparation method of ammonium polyphosphate wrapped with fluorine-containing silicone oil on surface |
| CN105780468A (en) * | 2016-03-28 | 2016-07-20 | 北京易净星科技有限公司 | Super-hydrophobic fabric and preparation method thereof |
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