WO2012177181A1 - Agent d'extinction d'incendie micro-encapsulé et procédé de production correspondant - Google Patents

Agent d'extinction d'incendie micro-encapsulé et procédé de production correspondant Download PDF

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Publication number
WO2012177181A1
WO2012177181A1 PCT/RU2012/000477 RU2012000477W WO2012177181A1 WO 2012177181 A1 WO2012177181 A1 WO 2012177181A1 RU 2012000477 W RU2012000477 W RU 2012000477W WO 2012177181 A1 WO2012177181 A1 WO 2012177181A1
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Prior art keywords
extinguishing
shell
microcapsules
core
liquid
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Russian (ru)
Inventor
Александр Дмитриевич ВИЛЕСОВ
Марина Сергеевна ВИЛЕСОВА
Ольга Михайловна СУВОРОВА
Владимир Евгеньевич ЮДИН
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OBSCHESTVO S OGRANICHENNOI OTVETSTVENNOSTYU "DELSI"
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OBSCHESTVO S OGRANICHENNOI OTVETSTVENNOSTYU "DELSI"
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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
    • A62D1/0007—Solid extinguishing substances
    • A62D1/0021—Microcapsules
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/18—Fireproof paints including high temperature resistant paints
    • C09D5/185—Intumescent paints
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/60—Additives non-macromolecular
    • C09D7/61—Additives non-macromolecular inorganic
    • C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40—Additives
    • C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres

Definitions

  • the present invention relates to methods for creating microcapsules containing a core from a target liquid inside a spherical shell, in which a predetermined opening temperature of the microcapsule is provided to release the target liquid contained in the microcapsule in the intended environment for its use, having a certain elevated temperature.
  • a predetermined opening temperature of the microcapsule is provided to release the target liquid contained in the microcapsule in the intended environment for its use, having a certain elevated temperature.
  • microcapsules of an extinguishing agent effective in extinguishing fires of different nature and created using the specified extinguishing agent, an extinguishing composite material, an extinguishing coating and an extinguishing fabric.
  • the invention can also be used for any microcapsules containing low-boiling, not miscible with water, liquids and volatile substances contained in them, in order to increase the barrier properties of the shell and, accordingly, the stability of microcapsules during storage and operation.
  • microencapsulation of various target products with the creation of a microcapsule that is stable under certain environmental conditions and is provided with a shell that does not affect the properties of the target product contained in it and ensures the release of the target product under certain parameters of external influences leading to biodegradation, dissolution or rupture of the shell, are very relevant .
  • the most difficult problems are microencapsulation of the target products, which are volatile or gasified when heated, which is associated with the problem of creating shells having high strength and low permeability when heated and at the same time ensuring destruction or opening of the shell at a given temperature to ensure the most efficient use of microcapsule of the target product.
  • microcapsules with the content of essential oils in the spherical core are known forms with a shell in the form of a thin external polymer membrane polyurea or polyurethane film around droplets of the specified essential oil, which controls the release of the essential oil and protects it from oxidation and evaporation, and also provides the release of an effective dose of oils with a constant constant speed over a long period of time (RU , 2347608, C2).
  • Microcapsules can be used in the production of disinfectant and repellent compositions, indoor air fragrances.
  • Microcapsules are known for curing natural and synthetic rubbers (RU, 2376058, C2), comprising a core containing at least one rubber additive in the polymer wall of the capsule formed by the melamine-formaldehyde resin and polyurea resin and polyelectrolyte. Microcapsules are thermally and mechanically stable up to 120-140 ° ⁇ , however, at a higher temperature, the rate of destruction of the shells of microcapsules and the temperature of their destruction are not the same for all microcapsules, which can affect the rubber vulcanization process.
  • the most difficult to solve are the problems of the release of the contents of the microcapsules at the same time, for example, during the explosive destruction of the shells of the microcapsules at a certain ambient temperature.
  • gaseous or liquid halogen-substituted (fluoro, bromo, chloro, iodo-substituted) hydrocarbons are extremely effective.
  • a fire-suppressing agent As a fire extinguishing agent using fluorine-substituted hydrocarbons, a fire-suppressing agent is known, having in its composition a non-combustible partially or fully fluorine-substituted hydrocarbon with a boiling point above 0 ° C combined with a gas that creates pressure to release the agent in atomized form in the protected zone (GB, 2265309, A).
  • the effect of suppressing fire is due to the fact that a high-density fire-extinguishing gas creates a non-combustible atmosphere, which prevents air from entering the surface having a high temperature, and fluorine radicals generated as a result of decomposition of the fluorine-substituted hydrocarbon by a flame having a high temperature interrupt the kinetic combustion chain.
  • Tetrafluorodibromoethane under the trade name Freon 114B2 and a number of other bromofluorine-substituted hydrocarbons (Halogen-containing extinguishing agents, TEZA Publishing House, St. Russia, 1999) are widely known as a fire extinguisher (OG) for volumetric extinguishing.
  • OG fire extinguisher
  • Fire extinguishing agents containing halogenated hydrocarbons are suitable for extinguishing fire at structures on the seabed and offshore, on aircraft, in archives, at nuclear power plants, and other structures.
  • bromine-substituted hydrocarbons were proposed as liquid gasifying fire extinguishing agents that do not accumulate in the atmosphere (WO 98/15322; Fire Safety, N ° 4, 2005, pp. 79-82).
  • WO 98/15322 Fire Safety, N ° 4, 2005, pp. 79-82
  • most bromine-substituted hydrocarbons converted to gas are not used in fire extinguishing due to extremely high volatility. For this reason, when used in concentrations close to the concentrations needed to extinguish the fire with other extinguishing agents, the practical effectiveness of brominated hydrocarbons was lower.
  • perfluoroketone perfluoroethyl perfluoroisopropyl ketone
  • This extinguishing agent is completely safe for the ozone layer of the stratosphere, does not apply to "greenhouse gases" It is safe for people even in the conditions of extinguishing a fire, its effectiveness allows you to stop the fire until a dangerous concentration of combustion products is achieved, and there is no need for urgent evacuation of people from the premises.
  • the agent was introduced to the market of many countries under the trade name “Novec 1230” (S. Dauenhauer. “Comparison of fire extinguishing systems”, magazine “Security Algorithm”. ⁇ ° 3, 2009). However, this agent is offered in the form of a liquid, which significantly increases the cost and complicates its transportation and makes it necessary to use it under increased pressure in special fire extinguishing equipment.
  • microencapsulated powder extinguishing agents have been developed that automatically release the extinguishing gas at high temperatures and deliver gas to the combustion center to the maximum extent possible.
  • Microcapsules are opened in the temperature ranges 130-149 ° C and 166-190 ° C.
  • the achieved stability of the material, necessary for its practical application, was insufficient.
  • the indicated fluorine substituted hydrocarbons and fluorinated amines were banned for use by the Kyoto Agreement in 1997 due to the fact that they cause a “greenhouse effect”.
  • JP fire extinguishing foam plastic
  • JP 57-195128, A
  • very small polymer capsules containing liquid halogenated hydrocarbon are dispersed, and foaming is performed at a temperature lower than the temperature of the explosive fracture of these small polymer capsules.
  • a fire extinguishing oil or water based paint is proposed (JP, 58-132056, A), in which very small polymer capsules containing a halogen-substituted hydrocarbon are mixed.
  • dibromotetrafluoroethane, bromochloroethane and bromochlorodifluoromethane were used as halogenated hydrocarbons.
  • the aim of the present invention is to obtain a microencapsulated extinguishing agent containing microcapsules having a core of extinguishing liquid gasifying low boiling substances, in shells having enhanced barrier properties when using this agent as an effective reactive fire extinguishing filler for extinguishing structural polymer materials, and to increase extinguishing efficiency due to the safety of the liquid from evaporation and providing explosive destruction of microcapsules at a given temperature and providing, accordingly, high stability of microcapsules in storage and operation.
  • the task was to create a microencapsulated extinguishing agent containing microcapsules having a core of extinguishing liquid gasifying low-boiling substances in shells with enhanced barrier properties and explosive destruction at a certain temperature, due to the formation of frame structural elements associated with polymer binder and having a certain size, and forming a layered structure in a polymer base shell parallel to microcapsules of the nucleus, providing a substantial increase in the possible path of fluid through the diffusion core shell microcapsules and increase the packing density of the shell polymer chains.
  • starting polymers were used that have basic functional groups in the macromolecule or in its constituent components, which ensure the formation of a complex on the surface of a mineral nanoscale plate having acidic functional groups. Only under this condition it was possible to obtain the effect of involving nanoscale plates in a coacervate drop, together with polymer macromolecules, and then ensure their location in the shell material. It was shown in experiments that up to 90% of the mass of the mineral filler introduced into the initial reaction medium was able to be concentrated in coacervate drops and in the composition of the microcapsule shell.
  • Aluminosilicates were used as sources of such mineral plates: the natural mineral montmorillonite (MMT), contained in bentonite clays, and its synthetic analogues.
  • MMT was used in the form of nanosized plates for modifying the properties of polymers, for example, polyimides (V. E. Yudin, V. M. Svetlichny. The effect of the structure and shape of filler nanoparticles on the physical properties of polyimide composites. Russian Chemical Journal, 2009, vol. 53, N ° 4, C.75-85.
  • VE Yudin, GM Divoux, JU Otaigbe, VM Svetlichnyi were used as sources of such mineral plates: the natural mineral montmorillonite (MMT), contained in bentonite clays, and its synthetic analogues.
  • MMT was used in the form of nanosized plates for modifying the properties of polymers, for example, polyimides (V. E. Yudin, V. M. Svetlichny. The
  • MMT plates were used after special modification of their surface with organic compounds and their subsequent introduction into melts or polymer solutions, to obtain block systems.
  • MMT nanoparticles in the form of plates the authors subjected the powdery natural MMT to exfoliation - separation of the initial powder particle into elementary structural units - folies, which are nanosized particles in the form of plates having a thickness within 1-2 nm (during exfoliation) and up to 5 nm (in case of partial intercalation).
  • microencapsulated extinguishing agent containing microcapsules having a core of spatially crosslinked polymer material placed inside a spherical polymer shell, a core of fire-extinguishing liquid, characterized in that the polymer shell contains nanoparticles of a mineral filler in the form of plates having a thickness of 1- 5 nm, and has the ability of explosive destruction in the temperature range of 90-270 ° C.
  • the polymeric material of the shell is a complex of polyvinyl alcohol and urea-resorcinol-formaldehyde resin.
  • the polymer material of the shell is crosslinked gelatin.
  • the nanoparticles of the mineral filler were made in the form of nanoscale plates of natural aluminosilicate montmorillonite or its analogues in an exfoliated state.
  • the shell contains the indicated nanoparticles of the mineral filler in an amount of 1-5% by weight of the shell.
  • said microcapsule has an outer diameter in the range of 50-400 microns. Moreover, according to the invention, it is advisable that the core contains extinguishing fluid in an amount of 75-95% by weight of the microcapsule.
  • the core it is possible for the core to contain perfluoroethyl perfluoroisopropyl ketone.
  • the core contains dibromomethane.
  • the core it is possible for the core to contain a bromine-containing or fluorine-bromine-containing fire extinguishing liquid.
  • the core it is possible for the core to contain a mixture of extinguishing fluids selected from the group consisting of perfluoroethyl perfluoroisopropyl ketone, dibromomethane, brominated hydrocarbons and fluorinated brominated hydrocarbons in a liquid state.
  • the problem was also solved by the development of a method for producing a microencapsulated extinguishing agent containing microcapsules having a core of a spatially crosslinked polymer inside a spherical polymer shell, a core of fire extinguishing liquid, in which the polymer shell contains nanoparticles of a mineral filler in the form of plates having a thickness of 1- 5 nm, and has the ability of explosive destruction in the temperature range 90-270 ° C, in which they carry out:
  • stage c) stage-by-stage formation on the drops of the emulsion obtained in stage c), the shell by the method of coacervation, including drop separation of phases, sorption coacervate drops on the surface of the droplets of the extinguishing liquid emulsion and their coalescence to obtain liquid shells;
  • step g) it is possible in step g) to form the shell by adding a fire-extinguishing liquid to the emulsion in the solution of polyvinyl alcohol obtained in step c), a mixture of an aqueous solution of urea with resorcinol and formaldehyde and lowering the pH of the medium to 1, 2, and stage e) curing of the shells is carried out by raising the temperature to 45 ° C and holding at the indicated temperature for 3.5 hours.
  • crosslinked gelatin is used as the polymer material of the shell.
  • step g) when using crosslinked gelatin as a polymeric material, it is possible in step g) the formation of the shell is carried out by adding an extinguishing liquid to the emulsion in the gelatin solution obtained in step c), an aqueous solution of sodium polyphosphate, lowering the pH of the medium to 4.0 -4.5, subsequent cooling of the emulsion to 5-10 ° C, and at the stage d) curing of the shells is carried out by adding glutaraldehyde, holding at that temperature for at least 1.0 hour, raising the temperature to 20-25 ° C,transpose pH of the mixture to 1.0-2.0, adding resorcinol and formaldehyde, at temperature 30-35 ° C for 30-40 min.
  • step g) it is possible in step g) to form a shell by adding an extinguishing liquid to the emulsion in the gelatin solution obtained in step c), an aqueous solution of sodium polyphosphate, lowering the pH to 4.0-4.5, then cooling the emulsion up to 5-10 ° C, and at the stage d) curing of the shells is carried out by adding glutaraldehyde and holding at the indicated temperature for at least 5.0-6.0 hours.
  • nanoparticles made in the form of mineral filler nanoparticles nanosized plates of natural montmorillonite aluminosilicate or its analogues in an exfoliated state are used.
  • microcapsules having an outer diameter in the range of 50-400 microns it is possible to obtain microcapsules having an outer diameter in the range of 50-400 microns.
  • microcapsules in which the core contains fire extinguishing liquid in an amount of 75-95% by weight of the microcapsule.
  • fire-extinguishing liquids selected from the group consisting of: perfluoroethyl-perfluoroisopropyl-ketone, dibromomethane, bromo-substituted hydrocarbons, fluorobromo-substituted hydrocarbons in a liquid state as an extinguishing liquid.
  • the material was made in the form of foam.
  • the material was made in the form of a curable paste.
  • the material was made in the form of a structural element.
  • the material was made in the form of a film.
  • the material was made in the form of a fire extinguishing fabric, impregnated or coated with a cured paste, containing resin or rubber, including dispersed in them microencapsulated extinguishing agent, made according to the invention.
  • Figure 1 data on the loss of dibromomethane from the core of microcapsules of a microencapsulated extinguishing agent having a shell of gelatin: line 1-shell without filler; line 2 - by a shell with a filler in the form of nanoparticles - montmorillonite plates;
  • Figure 2 data on the loss of perfluoroketone from the core of microcapsules of a microencapsulated extinguishing agent having a shell of a mixture of polyvinyl alcohol with urea-resorcinol-formaldehyde resin: line 3-shell without filler; line 4 - by a shell with a filler in the form of nanoparticles of montmorillonite plates;
  • Fig. 3 data on the loss of perfluoroketone from the core of microcapsules of a microencapsulated extinguishing agent having a shell of gelatin: line 5th shell without a filler; line 6 - a shell with a filler in the form of nanoparticles of montmorillonite plates;
  • Figure 4 data of thermogravimetric analysis of microcapsules of a microencapsulated extinguishing agent with a core of Novec 1230 perfluoroketone and a shell of gelatin: line 7 - shell without filler; line 8 — with a shell with nanoparticles in the form of nanoscale plates of montmorillonite with a shell without filler.
  • a microencapsulated extinguishing agent according to the invention containing microcapsules having a core made of cured spatially crosslinked polymer material inside the spherical polymer shell, a core of fire extinguishing liquid, and in which the shell contains nanoparticles of a mineral filler in the form of nanoscale plates having a thickness of 1-5 nm, and the microcapsule shell has the ability to explosively destroy in the temperature range 90-270 ° C, can be obtained by the method according to the invention using various, water-insoluble, extinguishing liquids for the formation of the core, and various polymeric materials with a mineral filler in the form of nanoparticles in the form of plates for the formation of the shell.
  • stage c) the gradual formation on the droplets of the emulsion obtained in stage c), the shell by the coacervation method, including drop separation of phases, sorption of the coacervate droplets on the surface of the droplets of the extinguishing liquid emulsion and their coalescence to obtain liquid shells;
  • the operations c), d) and e) were performed as follows: - in the case of using a complex of polyvinyl alcohol and urea-resorcinol-formaldehyde resin as a polymer material for the shell, the formation of the shell was carried out by adding a fire-extinguishing liquid obtained in stage c) and heated to 35 ° C, a mixture of an aqueous solution of urea with resorcinol and formaldehyde, lowering the pH of the medium to 1.2.
  • microcapsule shells were carried out by sorption of coacervate microdrops on the surface of the emulsion droplets and their coalescence (fusion) with the formation of liquid shells.
  • a mixture of urea, formaldehyde, and resorcinol in the form of aqueous solutions was added, the nanoparticles of the mineral filler were mainly concentrated in microdroplets of the coacervate phase.
  • a temperature was raised to 45 ° C and kept at the indicated temperature for 3.5 hours, cooled to room temperature, the obtained microcapsules were washed with water, filtered and dried.
  • the formation of the shell was carried out by adding to the emulsion obtained in stage c), an aqueous solution of sodium polyphosphate, lowering the pH of the medium to 4.0-4.5.
  • the formation of microcapsule shells was carried out due to sorption of coacervate microdrops on the surface of the emulsion droplets and their coalescence (fusion) with the formation of liquid shells.
  • a sodium polyphosphate solution is added, the nanoparticles of the mineral filler are predominantly concentrated in microdroplets of the coacervate phase.
  • the emulsion was cooled to 5-10 ° C, glutaraldehyde was added, kept at this temperature for at least 1.0 hour, the temperature was raised to 20-25 ° C, the pH of the mixture was lowered to 1.0-2.0, resorcinol and formaldehyde were added, kept at a temperature of 30-35 ° C for 30-40 minutes, the microcapsules were washed with water, filtered and dried.
  • the proposed method for producing microcapsules of a microencapsulated extinguishing agent according to the invention does not require a special process step for modifying the surface of nanoparticles filler, as it is combined with the main process of microencapsulation in a single technological chain. This greatly simplifies and reduces the cost of the process of obtaining the shell of a microcapsule filled with MMT nanoparticles.
  • the microcapsules obtained by the method described above consist of a shell and a liquid core of the target liquid product.
  • the shell is made of a cured spatially crosslinked polymer material containing nanoparticles of a natural mineral filler or its natural or synthetic analogue.
  • the shell polymeric material may be spatially crosslinked gelatin cured with glutaraldehyde and formaldehyde resorcinol, or polyvinyl alcohol in combination with urea-formaldehyde resorcinol resin.
  • the outer diameter of the obtained microcapsules is 50-400 microns, the content of the extinguishing fluid is 75-95% by weight of the entire microcapsule.
  • the temperature of the explosive destruction of the microcapsule is in the range of 90-270 ° C, depending on the nature (including the boiling point) of the extinguishing liquid in the core. The temperature of explosive destruction is considered, respectively, a sharp inflection on the curve of mass loss during gravimetric investigation (hereinafter TGA) of microcapsules.
  • microencapsulated extinguishing agents according to the invention used mainly for extinguishing a fire, contain microcapsules, the core of which contains an extinguishing liquid and is surrounded by a shell. At elevated temperatures, the extinguishing fluid inside the shell overheats to temperatures well above its boiling point under normal conditions, to the critical point of explosive destruction of the shell. When the shell of the microcapsule is explosively destroyed by heat or flame, the agent releases a gasified fire extinguishing liquid in a gaseous state into the surrounding space.
  • the microencapsulated extinguishing agent can be used as a filler for the manufacture of structural composite materials, coatings, films and other materials, imparting fire-extinguishing properties to these materials due to explosive destruction of microcapsules contained in the material with increasing temperature to a certain level of destruction temperature.
  • microencapsulated extinguishing agent according to the present invention can be introduced as a filler in resins, liquid curable rubbers, latexes, curable foams, in fabrics and other materials and products.
  • the extinguishing composite material according to the present invention contains a cured resin or liquid cured rubber, or latex rubber, containing the microencapsulated extinguishing agent dispersed therein according to the invention.
  • the extinguishing coating according to the present invention is a paste comprising a curing polymer matrix and the above microencapsulated extinguishing agent according to the invention complete with a hardener.
  • the extinguishing foam (solid foam) according to the present invention contains a microencapsulated extinguishing agent according to the invention.
  • extinguishing fabric according to the present invention is impregnated or coated with resins or other other curable binders containing a dispersed microencapsulated extinguishing agent according to the invention.
  • Fire extinguishing paint according to the present invention contains the above fire extinguishing agent according to the invention.
  • liquids having a boiling point of 45-150 ° C have a thermal destruction range of 90-270 ° C.
  • the choice of the lower limit is mainly dictated by the microencapsulation conditions (at temperatures of 35-45 ° C), and the upper limit - by the thermal stability of the shell material.
  • the expansion of these limits is possible when creating special conditions for microencapsulation (for example, sealing the technological process of microencapsulation), and the use of additional curing of the shell.
  • the extinguishing liquid should preferably have a melting point of minus 50 ° C or lower to provide possible storage and operating conditions.
  • Example 1 Obtaining microcapsules containing the core of the fire extinguishing liquid of Novecl230 perfluoroketone in a shell of a complex of polyvinyl alcohol with urea-resorcinol-formaldehyde resin filled with montmorillonite nanoparticles in the form of nanoscale plates.
  • exfoliation occurred - separation of the initial particle of the powdered mineral filler into its elementary structural units - folia, which are micro-sized plates having a thickness of 1-5 nm and a plane size of about 100 nm x 200 nm.
  • the control of achieving exfoliation is the enlightenment (transparency) of the initial suspension, which retains slight opalescence.
  • 1st solution (for the coacervation process): 0.38 g of urea, 0.9 g of resorcinol and 2.25 ml of formalin (37% by weight aqueous formaldehyde solution) were dissolved in 5.25 ml of distilled water; 2nd solution (for the curing process of the shell): 0.38 g of urea, 1.28 g of resorcinol and 5.25 ml of formalin were dissolved in 7.5 ml of distilled water.
  • the temperature of the reaction mixture was increased to 45 ° C, a second solution was added and kept for 3.5 hours to cure the shell. After cooling to room temperature, the microcapsules were filtered off, washed with distilled water and dried.
  • a microencapsulated extinguishing agent according to the invention was obtained containing microcapsules with a diameter of 50-200 ⁇ m with a perfluoroketone content of 87% by weight of the microcapsule, the output of the microcapsules was 90%, the temperature of explosive destruction was 92 ° C.
  • Example 2 Obtaining microcapsules containing a core of dibromomethane in a shell from a complex of polyvinyl alcohol with a urea-resorcinol-formaldehyde resin filled with montmorillonite nanoparticles in the form of nanoscale plates.
  • the obtained microcapsules had a diameter of 50-200 ⁇ m, the content of dibromomethane was 92% by weight of the microcapsules, the output of the microcapsules was 93%, and the temperature of explosive destruction was 220 ° C.
  • Example 3 Obtaining microcapsules containing the core of Novecl230 perfluoroketone in a gelatin shell filled with montmorillonite nanoparticles in the form of nanoscale plates.
  • a suspension of montmorillonite nanoparticles was added to 2.0 g of gelatin, kept at room temperature for 20 minutes to swell, then heated at 50 ° C for 30 minutes.
  • resorcinol To prepare a 15% by weight aqueous solution of resorcinol, 15.0 g of resorcinol was added to 85.0 g of distilled water and stirred at room temperature for 30 minutes.
  • the obtained microcapsules had a diameter of 120-400 ⁇ m, the perfluoroketone content was 89% by weight of the microcapsule, the microcapsule yield was 92%, and the temperature of explosive destruction was 90 ° C.
  • the shell it was cured as follows: after adding glutaraldehyde and holding for one hour, 5.2 ml of a 15% by weight aqueous solution of resorcinol was added to the reaction mass, and the mixture was stirred for 15 minutes, after which was added a 10% by weight aqueous solution of sulfuric acid in order to lower the pH to 1.3-1.4.
  • Example 4 Obtaining microcapsules containing a core of dibromomethane in a shell of gelatin, filled with nanoparticles of montmorillonite in the form of nanoscale plates.
  • Microcapsules were obtained by a method similar to that described in example 3, by curing the shell of the microcapsule.
  • the obtained microcapsules had a diameter of 200-300 ⁇ m, the content of dibromomethane was 93% by weight of the microcapsules, the output of the microcapsules was 90%, and the temperature of explosive destruction was 220 ° C.
  • Example 5 Obtaining microcapsules containing the core of the extinguishing fluid - a mixture of 80 wt.%. perfluoroketone and 20 wt.% dibromotetrafluoroethane in a gelatin shell filled with montmorillonite nanoparticles in the form of nanoscale plates.
  • Microcapsules were obtained as described in example 4..
  • the obtained microcapsules had a diameter of 200-300 ⁇ m, the content of dibromomethane was 93% by weight of the microcapsules, the yield of microcapsules was 90%, and the temperature of explosive destruction was 100 ° C.
  • Example 6 Obtaining microcapsules containing the core of the extinguishing liquid of tetrafluorodibromoethane in a shell of gelatin filled with montmorillonite nanoparticles in the form of nanoscale plates.
  • Microcapsules were obtained as described in example 4.
  • the obtained microcapsules had a diameter of 200-300 ⁇ m, the content of the extinguishing liquid was 92% by weight of the microcapsules, and the temperature of explosive destruction was 120 ° C.
  • Example 7 Obtaining microcapsules containing the core of the extinguishing fluid - a mixture of 20 wt.%. tribromomethane and 80 wt.% dibromomethane in a gelatin shell filled with montmorillonite nanoparticles in the form of nanoscale plates.
  • Microcapsules were obtained as described in example 4.
  • the obtained microcapsules had a diameter of 200-350 ⁇ m, the content of the extinguishing liquid was 90% by weight of the microcapsules, and the temperature of explosive destruction was 270 ° C.
  • Example 8 Experimental confirmation of the concentration of montmorillonite nanoparticles in the form of nanoscale plates in the shell of a microcapsule (for example, a shell with gelatin as a polymer material).
  • a portion of 0.06 g of montmorillonite in 32 ml of distilled water was exfoliated in an ultrasonic bath at a frequency of 35 kHz for 1.5 hours to obtain a transparent, slightly opalescent suspension.
  • a suspension of montmorillonite nanoparticles was added to 2.0 g of gelatin, kept at room temperature for 20 minutes to swell, then heated at 50 ° C for 30 minutes.
  • the silicon content was determined (by atomic absorption analysis) and the gelatin content (by gravimetric method).
  • the dry residue of the coacervate phase (shell material) was found:
  • Example 9 The study of the stability of microcapsules with extinguishing liquids.
  • the stability of the microcapsule samples was evaluated by the loss of extinguishing fluid (weight loss) from the microcapsules during open storage in a layer with a thickness of 1-2 mm at a temperature of 25 ° C.
  • Figure 1 presents data on the loss of dibromomethane from microcapsules for two variants of microcapsules:
  • microcapsules with a core of dibromomethane and a shell of gelatin (without nanoparticles) -line 1;
  • Figure 2 presents data on the loss of perfluoroketone from microcapsules for two variants of microcapsules:
  • microcapsules with a core of perfluoroketone and a shell of a mixture of polyvinyl alcohol with urea-resorcinol-formaldehyde resin (without nanoparticles) - line 3;
  • microcapsules with a core of perfluoroketone and a shell of a mixture of polyvinyl alcohol with urea-resorcinol-formaldehyde resin with nanoparticles in the form of nanoscale plates of montmorillonite obtained as described in Example 1, line 4.
  • Fig.3 presents data on the loss of perfluoroketone from microcapsules for two options for microcapsules:
  • microcapsules with a core of perfluoroketone and a shell of gelatin (without nanoparticles) - line 5;
  • the research data indicate the production of microcapsules containing fire extinguishing liquids (perfluoroketone and dibromomethane) having stable properties necessary for their practical use, only upon receipt of them according to the present invention, with a shell containing nanoparticles of a mineral filler in the form of nanoscale plates.
  • Example 10 Carrying out thermogravimetric analysis (TGA) of microcapsules.
  • Figure 4 presents the TGA data of samples of microcapsules with a core of perfluoroketone (Novec 1230) and a shell of gelatin (without nanoparticles) - line 7, and microcapsules with a core of perfluoroketone (Novec 1230) and a shell of gelatin with nanoparticles in the form of nanoscale plates of montmorillonite obtained as described in Example 3, line 8.
  • TGA data also indicate the stabilization of microcapsules, the shell of which contains nanoparticles of a mineral filler in the form of nanosized plates, under thermal exposure and their cooperative explosive destruction at a temperature significantly higher than the boiling point of the extinguishing liquid contained in the core of the microcapsule. It is this type of destruction of microcapsules that is necessary for the active release of a fire extinguisher and extinguishing a fire.
  • the following examples 11 to 18 relate to fire tests of the resulting microcapsules and extinguishing materials.
  • Example 11 The use of microencapsulated extinguishing agent according to the invention for extinguishing fire.
  • the amount of spent microencapsulated extinguishing agent with a core of perfluoroketone and the extinguishing time were less than when using microcapsules with dibromomethane.
  • microencapsulated extinguishing agents are undoubtedly effective. Since they are explosively destroyed at different temperatures, differing by more than 100 ° C, they will find application for different fire extinguishing systems.
  • Example 12 Extinguishing material.
  • Example 12 The same paste from a mixture of liquid uncured epoxy resin, hardener and a microencapsulated extinguishing agent according to the invention, as in Example 12, was applied to the inner wall of the same experimental box used in Example 11, and kept at 20-25 ° C for 48 hours for curing. The resulting coating reached a thickness of 1-2 mm. Diesel fuel was put into the box and diesel fuel was set on fire. The fire was extinguished 1-2 seconds after its occurrence.
  • Example 14 Extinguishing material.
  • Example 15 Fire extinguishing fabric.
  • a mixture of silicone rubber with a hardener with an organotin K-18 catalyst and a microencapsulated extinguishing agent according to the invention described in Example 3 was used to impregnate technical fabric with subsequent curing.
  • the fabric was tested as in example 12. The fire was extinguished after 1-2 seconds. The fabric remained intact.
  • Example 16 Extinguishing material.
  • Example 17 Extinguishing foam.
  • ZOG water-based paint (based on polyvinyl acetate) was mixed with 20 g of microcapsules obtained as in example 4. The paint was applied to a sheet of cardboard 150x150x200 and dried. The tests were carried out as in Example 12. The fire was extinguished in 2-3 seconds. Cardboard is preserved, its edges are slightly burnt.
  • microencapsulated agents according to the present invention containing a powder of microcapsules according to the invention, having a polymer shell consisting of a polymeric material with nanoparticles of a mineral filler in the form of nanoscale plates that stably hold a liquid and gasified during heating in the core and provide the mandatory release of the target liquid product from the core at a certain temperature of destruction of the shell in the range not 90-270 ° C.
  • the microencapsulated extinguishing agent according to the present invention is a microcapsule containing a polymer shell consisting of a spatially crosslinked polymer binder and inlaid (filled) with nanoparticles of a mineral filler in the form of nanoscale plates and having an explosion temperature in the range of 90-270 ° C, and the core of the extinguishing liquid, it is adapted for explosive destruction under the influence of heat and flame with the release of a gasified fire extinguisher for fire, while its production and use are not limited to the Montreal Agreement and the Kyoto Protocol.
  • microencapsulated extinguishing agent according to the present invention is easily mixed with resins, liquid curable rubbers and other matrices and can be used as a filler in fire extinguishing composite materials, for example, in the form of pastes, plates, films, coatings, foams, industrial fabrics, shaped and other products.
  • microencapsulated extinguishing agents capable of ejecting the desired liquid product into the external environment at a certain temperature can be provided, for example, by selecting a specific fire extinguishing liquid and ensuring stability by introducing nanofillers into the composition of the shell.
  • extinguishing agents can be used in various industries and in various fire extinguishing systems for effective automatic inertia-free fire prevention both in the form of microcapsule powder and as part of fire-extinguishing composite materials - coatings, films, cambrices, fire extinguishing protective fabrics and others ..

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  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • General Chemical & Material Sciences (AREA)
  • Business, Economics & Management (AREA)
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  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing Of Micro-Capsules (AREA)
  • Fire-Extinguishing Compositions (AREA)

Abstract

L'invention concerne un agent d'extinction d'incendie micro-encapsulé comprenant une enveloppe polymère ayant une température de rupture explosive se situent dans une plage de 90-270°C, et un noyau fait d'un liquide d'extinction d'incendie contenant du perfluoroéthyl-perfluoroisopropylkétone (Novec 1230) ou du dibromométhane ou des mélanges avec d'autres liquides contenant un composé bromo-fluoro; l'enveloppe polymère est faite d'un complexe d'alcool de polyvinyle avec une résine à base d'urée-résorcine-formaldéhyde ou une gélatine réticulée, lesquels sont incrustés (remplis) de plaques minérales ayant une épaisseur de 1 à 5 nm (comme de la montmorillonite exfoliée). L'invention concerne également des matériaux composites d'extinction d'incendie se présentant sous forme de pâtes, de plaques, de pellicules, d'articles, de mousses solides, de tissus, ainsi que des revêtements d'extinction d'incendie comprenant dans leur composition ledit agent d'extinction d'incendie micro-encapsulé.
PCT/RU2012/000477 2011-06-23 2012-06-19 Agent d'extinction d'incendie micro-encapsulé et procédé de production correspondant Ceased WO2012177181A1 (fr)

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