CN116159275B - Carbon dioxide fire extinguishing microcapsule and preparation method thereof - Google Patents
Carbon dioxide fire extinguishing microcapsule and preparation method thereof Download PDFInfo
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- CN116159275B CN116159275B CN202310342668.3A CN202310342668A CN116159275B CN 116159275 B CN116159275 B CN 116159275B CN 202310342668 A CN202310342668 A CN 202310342668A CN 116159275 B CN116159275 B CN 116159275B
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 150
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 75
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 75
- 239000003094 microcapsule Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 43
- 239000007789 gas Substances 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 25
- 238000003756 stirring Methods 0.000 claims abstract description 23
- 239000000839 emulsion Substances 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 17
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 16
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 16
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 10
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 9
- 238000001914 filtration Methods 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 14
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 8
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 239000011162 core material Substances 0.000 claims description 6
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- LJKMCTWPOSTJHB-UHFFFAOYSA-N [Na].C(=CC1=CC=CC=C1)/C/1=C/C(=O)OC1=O Chemical compound [Na].C(=CC1=CC=CC=C1)/C/1=C/C(=O)OC1=O LJKMCTWPOSTJHB-UHFFFAOYSA-N 0.000 claims description 4
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 4
- 239000001099 ammonium carbonate Substances 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 3
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 3
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 3
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 claims description 3
- 239000001095 magnesium carbonate Substances 0.000 claims description 3
- 229910000021 magnesium carbonate Inorganic materials 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 3
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 2
- 235000012501 ammonium carbonate Nutrition 0.000 claims description 2
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 claims description 2
- NKWPZUCBCARRDP-UHFFFAOYSA-L calcium bicarbonate Chemical compound [Ca+2].OC([O-])=O.OC([O-])=O NKWPZUCBCARRDP-UHFFFAOYSA-L 0.000 claims description 2
- 229910000020 calcium bicarbonate Inorganic materials 0.000 claims description 2
- QWDJLDTYWNBUKE-UHFFFAOYSA-L magnesium bicarbonate Chemical compound [Mg+2].OC([O-])=O.OC([O-])=O QWDJLDTYWNBUKE-UHFFFAOYSA-L 0.000 claims description 2
- 239000002370 magnesium bicarbonate Substances 0.000 claims description 2
- 229910000022 magnesium bicarbonate Inorganic materials 0.000 claims description 2
- 235000014824 magnesium bicarbonate Nutrition 0.000 claims description 2
- 235000014380 magnesium carbonate Nutrition 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 2
- 229920000053 polysorbate 80 Polymers 0.000 claims description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 2
- 239000011736 potassium bicarbonate Substances 0.000 claims description 2
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 2
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 235000011181 potassium carbonates Nutrition 0.000 claims description 2
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 239000000126 substance Substances 0.000 abstract description 12
- 230000008569 process Effects 0.000 abstract description 10
- 230000001105 regulatory effect Effects 0.000 abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 16
- 239000000243 solution Substances 0.000 description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- 238000004321 preservation Methods 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 230000009471 action Effects 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000000576 coating method Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 239000003063 flame retardant Substances 0.000 description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 4
- 239000004640 Melamine resin Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 230000001804 emulsifying effect Effects 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 150000008282 halocarbons Chemical group 0.000 description 2
- 229910052736 halogen Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 239000011257 shell material Substances 0.000 description 2
- 229940083575 sodium dodecyl sulfate Drugs 0.000 description 2
- 235000019333 sodium laurylsulphate Nutrition 0.000 description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 210000000748 cardiovascular system Anatomy 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- RVHPJLCXULJZOU-UHFFFAOYSA-N furan-2,5-dione;sodium;styrene Chemical compound [Na].O=C1OC(=O)C=C1.C=CC1=CC=CC=C1 RVHPJLCXULJZOU-UHFFFAOYSA-N 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- -1 halogen hydride Chemical class 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 229940068984 polyvinyl alcohol Drugs 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D1/00—Fire-extinguishing compositions; Use of chemical substances in extinguishing fires
- A62D1/0092—Gaseous extinguishing substances, e.g. liquefied gases, carbon dioxide snow
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D1/00—Fire-extinguishing compositions; Use of chemical substances in extinguishing fires
- A62D1/0007—Solid extinguishing substances
- A62D1/0021—Microcapsules
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Business, Economics & Management (AREA)
- Emergency Management (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
The application relates to the technical field of fire extinguishing materials, in particular to a carbon dioxide fire extinguishing microcapsule and a preparation method thereof. The preparation method of the carbon dioxide fire-extinguishing microcapsule provided by the application comprises the following steps: mixing and stirring an emulsifier and an acid solution, heating under a nitrogen atmosphere, adding carbonate, stirring and dispersing when the reaction system is clear and transparent, and obtaining an emulsion containing carbon dioxide gas; adding melamine prepolymer into the emulsion, heating for reaction, regulating pH value, continuously heating for reaction, cooling, filtering, washing after the reaction is finished, and drying to obtain carbon dioxide fire-extinguishing microcapsule powder. The carbon dioxide fire-extinguishing microcapsule provided by the application can not generate substances harmful to human bodies in the fire-extinguishing process, and has excellent fire-extinguishing performance.
Description
Technical Field
The application relates to the technical field of fire extinguishing materials, in particular to a carbon dioxide fire extinguishing microcapsule and a preparation method thereof.
Background
Microcapsules refer to micro-containers or packages having polymeric or inorganic walls. Microcapsule granulation is a technique in which solid, liquid or gas is embedded and encapsulated in microcapsules to form a solid particulate product. The microcapsule granulating technology has remarkable effects in changing the material state so as to improve the service performance, protecting and isolating special functional materials, controlling the release of core materials and the like, so that the microcapsule granulating technology is widely applied to the field of fire extinguishment gradually.
The fireproof microcapsule technology is to wrap an impermeable film outside the fire extinguishing agent or the fire retardant, the fire extinguishing agent or the fire retardant can be gas, liquid or solid, and the film wrapping the fire extinguishing agent or the fire retardant has to play the following roles: when the microcapsule fireproof or flame-retardant substance is mixed with some substances or protects inflammable substances, the capsule wall must withstand a certain pressure and temperature without rupture, and when the mixture or the protected object is impacted by fire at high temperature, the film is immediately melted and ruptured to release the fire-extinguishing and flame-retardant substance. Patent CN109821181a discloses a fireproof and/or fire extinguishing microcapsule and its preparation method and application, the inner core of the microcapsule is halogenated hydrocarbon fire extinguishing agent, the wall material is polyurethane, when halogenated hydrocarbon contacts with high temperature surface or flame, active free radical is generated by decomposition, through negative chemical catalysis and chemical purification of halogen hydride such as bromine and fluorine, free radical generated in combustion chain reaction is largely captured and consumed, the combustion chain reaction is destroyed and inhibited, the flame is extinguished rapidly, however, the halogen acid and phosgene generated by decomposition in the fire extinguishing process will harm the central nervous system and cardiovascular system of human body and have great damage to environmental ozone layer.
Based on the above analysis, it is important to provide a fire extinguishing microcapsule that does not generate harmful substances during the fire extinguishing process.
Disclosure of Invention
The embodiment of the application provides a preparation method of a carbon dioxide fire-extinguishing microcapsule, which aims to solve the problem that the conventional fire-extinguishing microcapsule in the related art can produce harmful substances in the fire-extinguishing process.
In a first aspect, the present application provides a method for preparing a carbon dioxide fire-extinguishing microcapsule, comprising the steps of:
step S101, mixing and stirring an emulsifier and an acid solution, heating under a nitrogen atmosphere, adding carbonate, and stirring and dispersing when a reaction system is clear and transparent to obtain an emulsion containing carbon dioxide gas;
and S102, adding melamine prepolymer into the emulsion, heating for reaction, adjusting the pH value, continuing the heating for reaction, cooling, filtering, washing and drying after the reaction is finished to obtain the carbon dioxide fire extinguishing microcapsule powder.
In some embodiments, the emulsifier is one or more of styrene-maleic anhydride sodium salt, sodium dodecylbenzene sulfonate, sodium dodecylsulfate, polyvinyl alcohol, OP-10, tween-80.
In some embodiments, the acid solution is one or more of dilute hydrochloric acid, dilute sulfuric acid, dilute nitric acid, acetic acid, dilute phosphoric acid, oxalic acid, and citric acid. In some preferred embodiments, the mass concentration of the dilute hydrochloric acid and the dilute sulfuric acid is 10%.
In some embodiments, the carbonate is one or more of sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate, barium carbonate, calcium bicarbonate, magnesium carbonate, magnesium bicarbonate, ammonium carbonate, ammonium bicarbonate.
In some embodiments, the melamine prepolymer is a water soluble melamine prepolymer.
In some preferred embodiments, the melamine prepolymer is one or more of cyanogen 385, new chemical industry MF4750, shanghai Shuai Ke chemical industry SK 5710.
In some embodiments, the pH adjusting solution is one or more of citric acid, hydrochloric acid, sulfuric acid, acrylic acid, phosphoric acid, nitric acid.
In some embodiments, in step S101, the temperature of heating is 30-60 ℃.
In some embodiments, in step S101, the stirring speed is 1000-4000rpm and the dispersing time is 5-20min.
In some embodiments, in step S102, the pH is adjusted to 3-4.
In some embodiments, the emulsifier is added in an amount of 1-10% by mass of the carbon dioxide gas.
In some embodiments, the molar ratio of acid solution to carbonate is 1-4:1.
In a second aspect, the application also provides a carbon dioxide fire-extinguishing microcapsule prepared by the preparation method, wherein the carbon dioxide fire-extinguishing microcapsule takes carbon dioxide gas as a core material and melamine prepolymer as a wall material.
The carbon dioxide fire-extinguishing microcapsule prepared by the method can be directly used as a fire-extinguishing agent singly, can also be applied to fire-extinguishing equipment such as fire-extinguishing sheets and fire-extinguishing blankets, and can be used for preparing coatings, fibers, adhesives and the like with fire-extinguishing functions, and has wide application range and multiple application fields.
The method adopts the mode of firstly generating gas and then emulsifying in the process of preparing the carbon dioxide fire-extinguishing microcapsule, the generated carbon dioxide gas is isolated by liquid phase to form bubbles under the action of external force of mechanical stirring, emulsifier molecules have the characteristic of hydrophilic hydrophobic groups, a layer of emulsifying agent layer can be formed around the bubbles, one hydrophobic end faces the bubbles, and the other hydrophilic end faces water, so that the interfacial tension between the bubbles and liquid is reduced, the existence of carbon dioxide bubbles is stabilized, and the added melamine prepolymer has positive charges and can adsorb and deposit on the surfaces of the carbon dioxide bubbles of the emulsifier with anions around, thereby completing the coating of the bubbles.
The fire extinguishing mechanism of the carbon dioxide fire extinguishing microcapsule provided by the application is as follows: the application adopts melamine resin to carry out the cladding to the carbon dioxide gas that the reaction produced, utilizes melamine resin's excellent mechanical properties and heat resistance can seal gaseous inside, when external temperature reaches more than 150 ℃, and the shell begins to decompose, releases a large amount of carbon dioxide in the twinkling of an eye, and carbon dioxide has higher density, is about 1.5 times of air, therefore when putting out a fire, carbon dioxide gas can discharge the air and surround on the surface of burning object or distribute in more airtight space, reduces the oxygen concentration around the combustible material or in the guard space, produces the choking effect and puts out the fire.
The beneficial effects that technical scheme that this application provided brought include:
1. according to the method provided by the application, firstly, air in a mixed system of an emulsifier and an acid solution is removed by utilizing nitrogen, carbonate is added to generate carbon dioxide gas, stable carbon dioxide bubbles are generated under the action of stirring and the emulsifier, then wall materials are added to adsorb and deposit on the surfaces of the bubbles, a compact cross-linked network structure is formed by heating and solidifying to complete coating, and the coating rate of the carbon dioxide gas can be effectively improved by adopting a mode of generating gas first and then emulsifying;
2. the carbon dioxide fire-extinguishing microcapsule that this application provided is inside with carbon dioxide gas as the cladding of fire-extinguishing core material, and wall material breaks when the conflagration takes place, releases carbon dioxide gas and plays the effect of putting out a fire, low cost, can not produce the material harmful to the human body in the process of putting out a fire, shows excellent fire extinguishing performance, is applicable to multiple conflagration scene.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings that are needed in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is an optical microscopic view of the carbon dioxide fire-extinguishing microcapsule prepared in example 1 of the present application.
Description of the embodiments
For the purposes of making the objects, technical solutions and advantages of the embodiments of the present application more clear, the technical solutions of the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is apparent that the described embodiments are some embodiments of the present application, but not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art without undue burden from the present disclosure, are within the scope of the present application based on the embodiments herein.
The embodiment of the application provides a preparation method of a carbon dioxide fire-extinguishing microcapsule, which can solve the problem that the existing fire-extinguishing microcapsule can produce harmful substances in the fire-extinguishing process.
The preparation method of the carbon dioxide fire-extinguishing microcapsule provided by the application comprises the following steps:
step S101, mixing and stirring an emulsifier and an acid solution, introducing nitrogen to remove air in a reaction system, heating to 30-60 ℃, then adding carbonate, stirring the reaction system from turbid to clear and transparent at a rotating speed of 1000-4000rpm, and dispersing at a high speed for 5-20min to obtain an emulsion containing carbon dioxide gas;
and S102, adding a water-soluble melamine prepolymer into the emulsion, heating to 60-80 ℃, carrying out heat preservation reaction for 1-3h, regulating the pH value of the system to 3-4, heating to 70-90 ℃, continuing to carry out heat preservation for 1-2h, cooling to room temperature after the reaction is finished, filtering, repeatedly washing with deionized water, and placing in an oven for drying to obtain the carbon dioxide fire-extinguishing microcapsule powder.
The carbon dioxide fire-extinguishing microcapsules and the preparation method thereof provided in the present application are described in detail below with reference to examples and comparative examples.
Examples
Example 1 provides a method for preparing carbon dioxide fire-extinguishing microcapsules, which comprises the following steps:
(1) Weighing 0.7g of sodium dodecyl benzene sulfonate and 100g of dilute hydrochloric acid, mixing and stirring, introducing nitrogen to remove air, heating to 30 ℃, adding 11g of calcium carbonate, stirring at 2500rpm for 10min when the reaction system becomes clear and transparent from turbidity, and obtaining emulsion containing carbon dioxide gas;
(2) 15g of SK5710 is added into the emulsion, the temperature is raised to 60 ℃, the reaction is carried out for 2 hours while the heat is preserved, then the PH value of the citric acid regulating system is added to 3.4, the temperature is raised to 70 ℃, the heat is preserved for 2 hours continuously, the reaction is cooled to room temperature after the completion, the reaction is filtered, and the reaction is repeatedly washed by deionized water, and the carbon dioxide fire-extinguishing microcapsule powder is obtained after the reaction is placed in an oven for drying.
The optical microscopic view of the carbon dioxide fire-extinguishing microcapsule powder prepared in example 1 is shown in fig. 1, and as can be seen from fig. 1, the microcapsule is presented as small particles with core material inside, demonstrating that carbon dioxide gas is coated in the shell material.
Comparative example 1:
(1) Weighing 100g of dilute hydrochloric acid, stirring, introducing nitrogen to remove air, heating to 30 ℃, adding 11g of calcium carbonate, stirring at 2500rpm for high-speed dispersion for 10min when the reaction system becomes clear and transparent from turbidity, and obtaining a solution containing carbon dioxide gas;
(2) Adding 15g of SK5710 into the solution containing carbon dioxide gas, heating to 60 ℃, keeping the temperature for reaction for 2 hours, then adding citric acid to adjust the pH value of the system to 3.4, heating to 70 ℃, keeping the temperature for 2 hours, cooling to room temperature after the reaction is completed, filtering, repeatedly washing with deionized water, and placing the mixture in an oven for drying to obtain white powder.
The white powder after drying in comparative example 1 was a melamine resin self-polymerization crosslinked product, and microcapsule powder coated with carbon dioxide gas was not obtained, because the comparative example 1 did not introduce an emulsifier to stabilize carbon dioxide bubbles in the aqueous phase, and melamine prepolymer could not migrate to the surface of carbon dioxide bubbles under the attraction of positive and negative charges, so that a large amount of prepolymer self-polymerized into balls, and finally an ideal product was not obtained.
It is further illustrated by comparative example 1 that only the introduction of the emulsifier and the subsequent emulsification of the gas produced was used to successfully coat the carbon dioxide gas.
Examples
Example 2 provides a method for preparing carbon dioxide fire-extinguishing microcapsules, which comprises the following steps:
(1) Weighing 0.5g of sodium dodecyl sulfate and 150g of dilute sulfuric acid, mixing and stirring, introducing nitrogen to remove air, heating to 40 ℃, adding 13g of calcium carbonate, stirring at 3000rpm for 5min when the reaction system becomes clear and transparent from turbidity, and obtaining emulsion containing carbon dioxide gas;
(2) 22g of SK5710 is added into the emulsion, the temperature is raised to 70 ℃, the reaction is carried out for 1h while the temperature is kept, the pH value of the system is regulated to 3.8 by adding acetic acid, the temperature is raised to 85 ℃, the heat is kept for 2h, the reaction is cooled to room temperature after the completion, the reaction is filtered, and the reaction is repeatedly washed by deionized water, and the microcapsule powder for extinguishing carbon dioxide is obtained after the reaction is carried out, and the microcapsule powder is placed in an oven for drying.
Examples
Example 3 provides a method for preparing carbon dioxide fire-extinguishing microcapsules, comprising the following steps:
(1) Weighing 100g of styrene-sodium maleic anhydride salt water solution, mixing and stirring with 20g of acetic acid, introducing nitrogen to remove air, heating to 50 ℃, adding 15g of sodium carbonate, stirring at 4000rpm for 5min when the reaction system becomes clear and transparent from turbidity, and obtaining emulsion containing carbon dioxide gas;
(2) 20g of MF4750 is added into the emulsion, the temperature is raised to 60 ℃, the reaction is carried out for 3 hours while the temperature is kept, the PH value of the acrylic acid regulating system is added to 4, the temperature is raised to 80 ℃, the heat is kept for 1 hour, the reaction is cooled to room temperature after the completion, the filtration and the repeated washing with deionized water are carried out, and the carbon dioxide fire extinguishing microcapsule powder is obtained after the drying in a baking oven.
Examples
Example 4 provides a method for preparing a carbon dioxide fire-extinguishing microcapsule, comprising the following steps:
(1) Weighing 85g of styrene-maleic anhydride sodium salt aqueous solution, mixing and stirring with 110g of dilute sulfuric acid, introducing nitrogen to remove air, heating to 40 ℃, adding 9g of magnesium carbonate, stirring at 1500rpm for 20min when the reaction system becomes clear and transparent from turbidity, and obtaining emulsion containing carbon dioxide gas;
(2) Adding 10g of cyanogen 385 into the emulsion, heating to 80 ℃, carrying out heat preservation reaction for 2 hours, adding hydrochloric acid to adjust the pH value of the system to 3, heating to 90 ℃, continuously carrying out heat preservation for 1 hour, cooling to room temperature after the reaction is completed, filtering, repeatedly washing with deionized water, and placing in an oven for drying to obtain the carbon dioxide fire-extinguishing microcapsule powder.
Examples
Example 5 provides a method for preparing a carbon dioxide fire-extinguishing microcapsule, comprising the following steps:
(1) Weighing 130g of styrene-maleic anhydride sodium salt aqueous solution, mixing and stirring with 110g of dilute hydrochloric acid, introducing nitrogen to remove air, heating to 60 ℃, adding 11g of calcium carbonate, stirring at 4000rpm for high-speed dispersion for 10min when the reaction system becomes clear and transparent from turbidity, and obtaining emulsion containing carbon dioxide gas;
(2) 17g of MF4750 is added into the emulsion, the temperature is raised to 75 ℃, the heat preservation reaction is carried out for 3 hours, the citric acid is added to adjust the pH value of the system to 4, the temperature is raised to 85 ℃, the heat preservation is continued for 2 hours, the reaction is cooled to room temperature after the completion, the filtration and the repeated washing with deionized water are carried out, and the carbon dioxide fire extinguishing microcapsule powder is obtained after the drying in a drying oven.
The fire-extinguishing microcapsules prepared in examples 1-5 were subjected to fire-extinguishing tests, which were conducted as follows:
the carbon dioxide fire-extinguishing microcapsule powder prepared in the embodiment 1-5 with the same mass is respectively placed in a glass tube, a paper towel is placed at the bottom of the glass tube, the paper towel is ignited, the time from burning to extinguishing of the paper towel is recorded, experiments show that the flame is extinguished within 5-15s, the microcapsule powder has excellent fire-extinguishing effect, wherein the time used in the embodiment 1 is 5s, the time is shortest, when the flame contacts the microcapsule powder, the flame is extinguished immediately, because the foam stabilizing effect of the emulsifier used in the embodiment 1 is optimal, the obtained carbon dioxide coating rate is highest, and more carbon dioxide gas is contained in the microcapsule under the same mass, so the fire-extinguishing effect is best.
In the description of the present specification, reference to the terms "one embodiment/manner," "some embodiments/manner," "example," "a particular example," or "some examples," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment/manner or example is included in at least one embodiment/manner or example of the present application. In this specification, the schematic representations of the above terms are not necessarily for the same embodiment/manner or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments/modes or examples. Furthermore, the various embodiments/modes or examples described in this specification and the features of the various embodiments/modes or examples can be combined and combined by persons skilled in the art without contradiction.
It should be noted that in this application, relational terms such as "first" and "second" and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising one … …" does not exclude the presence of other like elements in a process, method, article, or apparatus that comprises the element. In the present application, the meaning of "plurality" means at least two, for example, two, three, etc., unless explicitly specified otherwise.
The foregoing is merely a specific embodiment of the application to enable one skilled in the art to understand or practice the application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the application. Thus, the present application is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (7)
1. A preparation method of a carbon dioxide fire-extinguishing microcapsule is characterized in that: the method comprises the following steps:
s101, mixing and stirring an emulsifier and an acid solution, heating under a nitrogen atmosphere, adding carbonate, and stirring and dispersing when a reaction system is clear and transparent to obtain an emulsion containing carbon dioxide gas;
s102, adding melamine prepolymer into the emulsion, heating for reaction, adjusting the pH value, continuing the heating for reaction, cooling, filtering, washing and drying after the reaction is finished to obtain carbon dioxide fire extinguishing microcapsule powder;
wherein the emulsifier is one or more of styrene-maleic anhydride sodium salt, sodium dodecyl benzene sulfonate, sodium dodecyl sulfate, polyvinyl alcohol, OP-10 and Tween-80; the acid solution is one or more of dilute hydrochloric acid, dilute sulfuric acid, dilute nitric acid, acetic acid, dilute phosphoric acid, oxalic acid and citric acid; the carbonate is one or more of sodium carbonate, sodium bicarbonate, potassium carbonate, potassium bicarbonate, barium carbonate, calcium bicarbonate, magnesium carbonate, magnesium bicarbonate, ammonium carbonate and ammonium bicarbonate; the mol ratio of the acid solution to the carbonate is 1-4:1; the addition amount of the emulsifier is 1-10% of the mass of the carbon dioxide gas.
2. The method for preparing carbon dioxide fire-extinguishing microcapsules according to claim 1, characterized in that: the melamine prepolymer is a water-soluble melamine prepolymer.
3. The method for preparing carbon dioxide fire-extinguishing microcapsules according to claim 1, characterized in that: the solution added for adjusting the pH value is one or more of citric acid, hydrochloric acid, sulfuric acid, acrylic acid, phosphoric acid and nitric acid.
4. The method for preparing carbon dioxide fire-extinguishing microcapsules according to claim 1, characterized in that: in step S101, the heating temperature is 30-60 ℃.
5. The method for preparing carbon dioxide fire-extinguishing microcapsules according to claim 1, characterized in that: in the step S101, the stirring speed is 1000-4000rpm, and the dispersing time is 5-20min.
6. The method for preparing carbon dioxide fire-extinguishing microcapsules according to claim 1, characterized in that: in step S102, the pH is adjusted to 3-4.
7. The carbon dioxide fire-extinguishing microcapsule prepared by the preparation method of any one of claims 1 to 6, wherein the core material of the fire-extinguishing microcapsule is carbon dioxide gas, and the wall material of the fire-extinguishing microcapsule is melamine prepolymer.
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| CN117919644B (en) * | 2023-12-15 | 2025-12-02 | 武汉中科先进技术科技服务有限公司 | A fire extinguishing microcapsule containing cis-hexafluorobutene, its preparation method and application |
| CN117797441A (en) * | 2023-12-20 | 2024-04-02 | 重庆渝捷消防设备有限责任公司 | Microcapsule fire extinguishing agent and its preparation method and application |
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