KR101733423B1 - Halogen-based gaseous fire extinguishing agent composition and manufacturing method thereof - Google Patents
Halogen-based gaseous fire extinguishing agent composition and manufacturing method thereof Download PDFInfo
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- KR101733423B1 KR101733423B1 KR1020160020693A KR20160020693A KR101733423B1 KR 101733423 B1 KR101733423 B1 KR 101733423B1 KR 1020160020693 A KR1020160020693 A KR 1020160020693A KR 20160020693 A KR20160020693 A KR 20160020693A KR 101733423 B1 KR101733423 B1 KR 101733423B1
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- extinguishing agent
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- halogen
- fire extinguishing
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- 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
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- 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
- A62D1/0028—Liquid extinguishing substances
- A62D1/005—Dispersions; Emulsions
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- 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
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- 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
- A62D1/06—Fire-extinguishing compositions; Use of chemical substances in extinguishing fires containing gas-producing, chemically-reactive components
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- Manufacturing Of Micro-Capsules (AREA)
Abstract
Description
The present invention relates to a halogen-based gas-extinguishing agent composition and a method for preparing the same, and more particularly, to a halogen-based gas-extinguishing agent composition which improves the digestion function of the halogen- Which is capable of improving the physicochemical properties of the extinguishing agent through a manufacturing process using the extinguishing agent, and a method for producing the extinguishing agent composition.
Water or powder fire extinguishing agents are commonly used for general fire. However, water fire extinguishing agents have a relatively high freezing point of 0 ° C, which makes them difficult to use in a cold place or outdoors where winter heating is not possible. In the case of powder fire extinguishing agents, The secondary damage caused by the fire extinguishing agent component is very large, and if it is not shaken once or more regularly during management and handling, it hardens easily and is not radiated when necessary, and there is a problem that it is difficult to keep it when moisture is large.
The composition and components of the polymer conjugate and the microencapsulated fire extinguishing agent which are automatically ejected at the time of the temperature rise due to fire to suppress the fire have already been disclosed.
For example, prior art patents Soviet patent USSR 1696446 discloses its manufacturing encapsulation compositions and methods.
According to this prior patent, the linking material and the microencapsulated halogen 114B are extinguishing agents, and the combination comprises an epoxy resin ED-20 and a polyoxyethylene polyamine and an epoxidized polyoxyethylene propylene epimer in a constant state, It can be obtained by the following method.
The epoxy resin ED-20 is completely mixed with the oxiridine extracted at a constant state, and then the polyethylene polyamine is added thereto. When the epoxy resin is mixed again, the microcapsule containing the halon-based 114B2 is gradually generated.
The product or surface obtained by solidifying the lumps (solution) obtained after thorough mixing and coating on the surface of the mold and for two days in the room at the normal temperature for two days shows that the capsules explode at a temperature of 150 to 165 ° C to eject Halon 114B2 .
At this time, only the capsules are blown out by 8 ~ 10%, and the capsule explodes and simultaneously releases a lot of freon, so that the fire can be suppressed within 3 ~ 20 seconds.
However, since the extinguishing agent has a small proportion of the extinguishing agent at a weight ratio of 60:40 of the polymer connecting substance and the extinguishing agent, the effective fire suppression can not be ensured. Besides, the epoxy resin ages and vaporizes over time, It is weak against atmospheric pressure, and has a weak problem particularly in ultraviolet rays.
Other prior patent documents US Pat. No. 4,138,356 discloses phenol polyurethanes encapsulating an extinguishing agent.
The walls of the capsules made of polyurethane are obtained by solidifying trimethylolpropane and isocyanate.
This prior patent, however, is structured such that the content only imparts flame retardant polyurethane blowing agent, which is either a liquefied or hot solid organic phosphate (e.g. 2,3-dibromopropyl ether) There is a problem that fire can not be suppressed.
The use of a liquid or solid at a high temperature as a fire retardant does not require a wall of a low temperature molten halogen carbon capsule which does not require particularly high durability.
In this prior patent, an extinguishing agent with a boiling point of 200 ° C or higher is used.
For example, halogen carbons such as Freon 114B2 produce a low pressure of about 13 to 14 atmospheres up to 130 ° C when heated, leading to the destruction of the capsule.
Another prior patent document Russian Patent RU No. 2161520 discloses an ozone protective polymer combination material containing a cooled solidified polymer conjugate, an encapsulated extinguishing agent and a method of obtaining the same.
(C 2 F 5 ) 2 N (C m F 2 m +1 ) and m = 1 to 2, with C 3 F 7 I or C n F2 n +2 as the extinguishing agent and n = 5-7, Lt; / RTI >
The composition comprises 40 to 51% of the components, microencapsulated fire extinguishing agent, polymeric binder and the remainder.
The cooled coagulated polymeric binder is selected from polyepoxy grades based on polyurethane, aliphatic epoxy resins.
An extinguishing agent is formed in the form of microcapsules microcapsules each consisting of an inner wall of a liquid extinguishing agent and a circular polymer wall and composed of gelatin having a diameter of 100 to 400 μm.
The capsules may be produced in the form of a molded article to be lined with the material of the mold or a sheet for a low temperature curable mastic which explodes at a temperature of 130 to 149 ° C and 166 to 190 ° C.
According to this prior patent, the strength of the microcapsule is determined according to the diameter, and the optimum diameter of the microcapsule is 100-400 탆.
This increases the content of the digestion agent in the capsule up to 94%, but the ratio of the weight ratio of the polymer conjugate to the digestion agent is 60:40, that is, less than 50% in the capsule.
In addition, the capsules have a sealing effect sufficient to store easily vaporized halogen carbons, and the resulting combination is capable of maintaining long-term performance as a result of the short time of presence of the conjugate in the form of a sticker and the difficulty of the method of acquisition.
Since an epoxy resin and a curing agent are used as raw materials for the coupling, the curing takes place for several hours and the constitution is immediately formed at the time of production.
Therefore, this material is not suitable for the production of paints, enamels and other construction materials that must be stored long before use.
As mentioned above, the disadvantage of the extinguishing composition and the method of obtaining according to the Russian patent RU 2161520 is that a lot of effort is required for the combination to be obtained, and the maintenance of the properties is short-term.
Despite this difficulty of manufacture, the extinguishing agent composition present in the capsule is small.
SUMMARY OF THE INVENTION [0005] The present invention has been made in order to solve the above-mentioned problems, and it is an object of the present invention to provide a microencapsulated fire extinguishing agent which simplifies the manufacturing method of a fire extinguishing agent and maintains a fire extinguishing agent for a long period, The microcapsules contain at least 80% of the extinguishing agent, and all the microcapsules are allowed to operate instantaneously at a predetermined temperature of 110 to 165 ° C, thereby reducing the manufacturing cost and enhancing the effect as a final product, A gas-extinguishing agent composition and a method for producing the same.
According to an aspect of the present invention, there is provided a halogen-based gas-extinguishing agent composition, which is a fire extinguishing agent composed of halogen carbon as a phase change material, capsule; And a polymer connected body in which the microcapsules are dispersed, wherein the shell is formed of at least one of polyurea and polyurethane based on a polyisocyanate prepolymer.
In this case, the diameter of the microcapsules is 10 to 50 μm.
The halogen carbon may be at least one selected from the group consisting of fluorine carbon, fluorine chlorine carbon, fluorine bromine carbon halocarbon, fluorine iodine carbon halogen carbon, 2-iodine-1,1,1,2,3,3,3-heptafluoropropane (HFC- 227ea) and Iodofluorocarbon (FIC-217I1 or FIC-13I1).
The polymer connecting body is characterized in that it is made of at least one of acrylic, alkyd, glyptal, latex, nitrocellulose, epoxy, polyvinyl chloride, polyurethane, polyurea, polyvinyl alcohol and polyvinyl acetate.
The content of the extinguishing agent is 80% or more.
According to the means for solving the above problems, a more effective and safe fire extinguishing device can be manufactured through a phase change process of the fire extinguishing agent by the microcapsule manufacturing method to improve the physicochemical characteristics of the halogen fire extinguishing device which is a liquefied gas.
DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, embodiments of the present invention will be described.
In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted when it may make the subject matter of the present invention rather unclear.
Also, when a part is referred to as "including " an element, it does not exclude other elements unless specifically stated otherwise.
In the production of microcapsules having a polymer shell and a fire extinguishing agent as nuclei, the resultant polymer obtained by polymerizing a polymeric linkage for producing capsules in a weight ratio of halogen carbon of 100: 1 to 100: 7 is first added in an amount of 0.1 to 3% 0.1 to 1 ml of water per second in aqueous surfactant and mix until a dropwise microemulsion.
At this time, the size of the droplet is equal to the size of the microphone capsule, and the ratio of the organic material to the aqueous solution is 1: 1 to 1: 5.
The aqueous surfactant used herein is polyvinyl alcohol and / or a derivative thereof and is stirred at 2500 to 3500 rpm.
The microemulsion is then mixed with a polyamine or polyalcohol solution at a concentration of 5 to 10% to make the envelope.
The reaction combination is then stored at a temperature of 20 to 60 ° C for 1 to 4 days to allow the shell to reach the required thickness.
Subsequently, the microcapsules are separated from the liquid (only a solid is left when the liquid is poured, a kind of water discarding) and used for the preparation of the extinguishing composition in the form of a binder.
The size of the microcapsules is 10 to 50 μm.
These extinguishing agents are halocarbon and fluorine iodine carbon halogens of various fluorine carbon, fluorine chlorine carbon, fluorine bromine carbon series, and 2-iodine-1, 1, 1, Extinguishing agents such as 2,3,3,3-heptafluoropropane can be used instead of halogen carbon.
Polymeric linkages include acrylic and / or alkyd and / or phenol and / or latex, and / or nitrocellulose and / or epoxy resin and / or polyvinyl chloride and / or polyurethane and / or polyurea and / or polyvinyl alcohol And / or polyvinyl acetate.
H 2 N (CH 2 CH 2 NH) n H, n = 1 ~ 5 in place of the polyamines (mono-, di-, tri-, tetra-, penta ethylene hexamine) and / or hexamethylenediamine and / or polyethylene Polyamines can be used.
Further, pentaerythritol can be used instead of the polyalcohol.
Instead of polyisocyanate, polyisocyanate based on methylene diisocyanate or toluene diisocyanate can be used as the shell material.
According to the present invention, it is possible to provide a highly efficient extinguishing agent that does not destroy the ozone layer, provides a large amount of rapid release of the extinguishing agent, substantially less manufacturing complexity than the previous patent, manufacture of the extinguishing agent composition and extinguishing agent, It is possible through the use of fundamentally different approaches to microencapsulation.
The extinguishing agents produced by the present invention can be used in the manufacture of paints, varnishes and other building materials, are transportable and maintain all basic physical and chemical properties for a minimum of 5 years.
In the present invention, polymeric microencapsulation methods are used at the interface to enable microencapsulation of volatile products at relatively low temperatures (below 20 DEG C) using simple hardware technology decorations.
The following items are possible by the manufacture of compositions which contain up to 90% of extinguishing agents and which last for long periods of time.
First, small size capsules can be placed between large size capsules, so that the maximum number of microcapsules can be packed in one unit so that the digestion component can occupy more than 80% of the extinguishing agent.
Second, the polyurethane and / or polyurea microcapsule sheath material obtained through polyisocyanate cooling with polyamines or polyvinyl alcohols ensures a thin sheath that can be broken at temperatures between 110 and 165 ° C.
In this case, the thin envelope maintains the integrity of the envelope over a long period of time, which allows for a loss of digestive medication of less than 10% over the years.
According to U.S. Patent No. 4,138,356, which is described in the background, polyurethane obtained using a diisocyanate does not guarantee the firmness of the shell wall since the tightness of the shell is insufficient.
The diisocyanate reacts only with a hydroxyl group or an amino group, and the obtained polyurethane has a structure close to a linear form, which has low density and high freon permeability.
However, the present invention uses polyisocyanates and polyamines and / or polyalcohols in the production of microcapsules because polyisocyanates react with thousands of hydroxyl groups or amino groups and therefore polyurethane and / Make it possible to
As a result of an experiment to obtain a microcapsule shell made of polyurea using the polyamine and the disocyanate, the rigidity of the capsule was very weak.
Moreover, the digestion agent evaporated from the capsule in a few days, which was due to the structure with a branched structure, high polymer permeability and low density.
Also, the microcapsules obtained by US Patent No. 4,138,356 are not destroyed due to a rapid temperature rise outside the capsule, but are destroyed when the temperature of the capsules melts.
Therefore, the fire extinguishing agent does not come out in the form of gas, but flows out to the surface of the phenol polyurethane, extinguishes only the substance, and does not extinguish the source of the fire.
In the past, the causal relationship of the capsule properties (robustness) of the method of obtaining structures (polyurea and / or polyurethane) materials has not been applied by anyone to obtain digestion compositions.
However, the connector according to the present invention allows to achieve a high level of composition charging and excludes the possibility of drying microcapsules in the manufacturing process.
This will eventually lower the cost of the final product and allow for a variety of polymer coatings with strong digestion effects on a variety of surfaces.
Unlike those used for conventional and epoxy resin curing agents, for example, water-insoluble and water-insoluble polymers or mixtures thereof (e.g., acrylic and / or alkyd and / or phenol and / or latex, and / or nitrocellulose and / The polymeric binder comprised of a polymeric binder consisting of polyvinyl chloride and / or polyurethane and / or polyurea and / or polyvinyl alcohol and / or polyvinyl acetate) is an environmentally-friendly curing agent and an epoxy resin, a heat- Only the materials resistant to ultraviolet rays are used to make the composition so that it can be maintained.
In addition, dispersing the microencapsulated component to 10-50 mu m enables the following.
First, the degree of density can be controlled according to the composition and filling of the active ingredient.
Second, the thickness of the microcapsule wall can be adjusted to pop up at the required temperature when the temperature rises.
Third, porosity can be adjusted to ensure a rapid temperature rise of the composition in order to ensure the destruction rate of the microcapsule.
In addition, the size of 10-50 μm microcapsules is guaranteed.
For example, 10-50 micron microcapsules and their properties can not be obtained from gelatin.
The most important parameters in temperature, digestion efficiency, product lifetime, etc. in microcapsule shell rupture depend on microcapsule and polymer connector.
The polymer matrix having a high content of epoxy resin of 60% is solid, and the capsules must have a size of 100 to 400 탆 in order to disintegrate the capsules at a required temperature. The microcapsules having a size of 10 to 50 탆, (Not destroyed) as indicated in Fig.
The fire extinguishing agent composition (including fire-extinguishing paint) according to the present invention can not be produced with microcapsules having a size of 100 mu m or more.
Because there is a visual difference in the surface and lack of mechanical properties, the smaller the size, the more pressure it can withstand.
In addition, capsules ranging in size from 10 to 50 microns can operate between 110 and 165 degrees Celsius and ensure the required mechanical and aesthetic properties.
The present invention relates to the production of microcapsules using the interfacial polycondensation method, and the extinguishing agent composition is prepared by the following procedure.
First, the polyisocyanate is mixed with the extinguishing agent in a weight ratio of 100: 1 to 100: 7. As the extinguishing agent, various fluorocarbons and / or fluorine bromine carbon series halocarbon, fluorine iodine carbon series halogen carbon Lt; / RTI >
The resulting mixture is then mixed with 0.1 to 3 ml of an aqueous surfactant solution (for example, a polyvinyl alcohol solution) in an amount of 0.1 to 1 ml / sec, with a special propeller agitator having a rotation speed of 2,500 to 3,500 revolutions per minute Until a microemulsion is formed, in which case the ratio of organic to liquid is 1: 5 to 1: 1.
The following microemulsion is mixed with 0.05 to 0.25 ml of a water-soluble polyamine or polyalcohol at a ratio of 1: 0.1 to 1: 1, based on the total amount of the polyisocyanate, until the shell composition is achieved.
Next, the reaction mixture is incubated at a temperature of 20 to 60 DEG C for 1 to 4 days to obtain a desired shell thickness (for example, 0.03 mm).
Then, the microcapsules are decanted and separated from the aqueous phase, and a binder or a chain reaction promoting material is added to prepare the extinguishing agent composition.
As a result, the extinguishing agent composition according to the present invention is a phase change material, wherein the nucleus is an extinguishing agent composed of two or more halogen carbons, and the envelope surrounding the nucleus is a micro- And the material of the shell is composed of at least one of polyurea and polyurethane based on polyisocyanate prepolymer, and the diameter of the microcapsules is 10 to 50 mu m.
An extinguishing agent composed of a mixture of 2-iodo-1,1,1,2,3,3,3-heptafluoropropane (HFC-227ea) and Iodofluorocarbon (FIC-217I1 or FIC-13I1) can be used instead of the halogen carbon .
In addition, at least 80% of the extinguishing agent is concentrated in the composition, and the size of the microcapsules is doubled so that small microcapsules can be positioned between large microcapsules for high concentration of the extinguishing agent.
In order to enhance the digestion function of the composition, ammonium perchlorate, ammonium dinitramide (ADN), dinitramide salt (N (NO 2 ) - ) which is a non - chlorine based oxidizing agent, (CDD: Copper diamine dinitrate) may be further added.
Here, a low-molecular, heat-resistant synthetic rubber can be added to bind and protect microcapsules.
The low-molecular-weight, heat-resistant synthetic rubber is made of at least one of polybutadiene, butadiene styrene rubber, butadiene acrylonitrile rubber, polychloroprene, polyisoprene, chlorosulfonated polyethylene, polyisobutylene, and isobutylene isoprene rubber.
[Confidentiality Test]
The thus-prepared microcapsules were dried and the dried microcapsule samples were stored at a temperature of 100 ° C. for 12 hours, and the airtightness was checked. As a result, the extinguishing agent loss was 0.5% or less.
This means that at regular temperatures, the digestive system maintains digestive drugs for five years.
[Definition of microcapsule size]
The distribution of the size of the microcapsules was observed using a 120x magnification microscope with a resolution of a digital camera of 800x600 pixels and microcapsules and microemulsions were photographed with the microscope using professional software, To determine the linear dimensions of the microcapsules, and to calculate the amount of microcapsules according to the ratio conversion size.
The correction of the linear dimensions of the microcapsules is carried out using a Goryaeva camera and the size of the microcapsules is determined as the ratio of the diameter of the microcapsules in the micrograph to the average total number.
The ability of the microcapsule to perform by rupturing the wall by thermogravimetry.
The weight of the sample is measured while heating the sample of the microcapsule to 10O < 0 > C per minute to 300 < 0 > C.
As a result, microcapsule rupture (abrupt loss of sample weight) was found to occur in the narrow temperature range between 110 and 165 ° C.
[Digestive capacity experiment]
For the digestibility test, an artificial digestion experiment was carried out. An iron plate with a size of 100 mm and a thickness of 1 mm, which was coated with a sample on the bottom, was placed on a cotton plate having a thickness of 2 mm and a size of 50 mm and 5 ml of gasoline was added. The time of post-digestion was measured.
[Example 1]
500 g of 1,1,2,2-tetrafluoro dibromethane was mixed with 35 g of a polyisocyanate based on methylene isocyanate, and the resulting mixture was poured into 2500 ml of a 3% aqueous solution of polyvinyl alcohol in an amount of 1.0 ml per second, Is stirred at a speed of 3500 rpm to produce a microemulsion having droplets of an average size of 20 mu m.
370 ml of a 10% aqueous solution of polyethylenepolyamine was added to the microemulsion in an amount of 0.25 ml per second and the resulting reaction mixture was kept at 20 캜 for 4 days to increase the shell thickness by 0.03 탆.
The following liquids were separated to obtain a highly concentrated suspension containing 550 g of microcapsules with an overall average size of 20 microns, with a size of 18 to 22 microns accounting for 81%, with a content of extinguishing agent of 88%.
10 g of aqueous solution polyvinyl alcohol was added to this suspension, and the resultant mixture was thoroughly mixed to obtain a 3 mm-thick material, which was then completely dried to complete the preparation of the extinguishing agent composition.
The extinguishing agent composition prepared in Example 1 was digested within 15 seconds as a result of the digestibility test described above, and the microcapsule was released at a temperature of 140 to 150 ° C.
[Example 2]
33 g of a polyisocyanate based on methylene diisocyanate was mixed with 450 g of 1,1,2-trifluorotrichloroethane as an extinguishing agent, and the resulting mixture was poured into 2200 ml of 3% aqueous polyvinyl alcohol in an amount of 1 ml per second. The propeller stirrer was rotated at a speed of 3500 rpm And stirred to produce a microemulsion having droplets of an average size of 10 mu m.
330 ml of a 10% aqueous solution of polyethylenepolyamine is added to the microemulsion in 0.25 ml per second and maintained at 20 캜 for 4 days to increase the shell thickness of the reaction mixture thus obtained by 0.03 탆.
The following liquids were separated to obtain a highly concentrated suspension containing 490 g of microcapsules having an overall average size of 10 mu m occupying 85% of the size of 8-12 mu m with a content of 85% extinguishing agent.
10 g of aqueous solution polyvinyl alcohol was added to this suspension, and the resultant mixture was thoroughly mixed to obtain a 3 mm-thick material, which was then completely dried to complete the preparation of the extinguishing agent composition.
The extinguishing agent composition prepared in Example 2 was digested within 15 seconds as a result of the digestibility test and the microcapsule was released at a temperature of 130 to 150 ° C.
[Example 3]
40 g of a polyisocyanate based on methylene diisocyanate is mixed with 600 g of the extinguishing agent 2-iodo-1,1,1,2,3,3,3-heptafluoropropane, and the resulting mixture is mixed with 2% aqueous poly The mixture is poured into 3000 ml of vinyl alcohol and the propeller stirrer is stirred at a speed of 3500 rpm to produce a microemulsion having droplets of an average size of 40 탆.
400 ml of a 5% polyethylenepolyamine aqueous solution is added to the microemulsion in 0.25 ml per second and maintained at 20 캜 for 4 days to increase the shell thickness of the reaction mixture thus obtained by 0.03 탆.
The following liquids were separated to obtain a highly concentrated suspension containing 660 g of microcapsules having a total average size of 40 탆, which accounted for 81% of the size of 35 to 45 탆, and the content of the extinguishing agent was 81%.
15 g of an aqueous solution of polyvinyl alcohol was added to this suspension, and the resultant mixture was thoroughly mixed to obtain a 2 mm-thick material, which was then completely dried to complete the preparation of the extinguishing agent composition.
The extinguishing agent composition prepared according to Example 3 was extinguished within 15 seconds as a result of the digestibility test and the microcapsule was released at a temperature of 140 to 150 ° C.
[Example 4]
700 g of an extinguishing agent consisting of 80% of 1,1,2-trifluorotrichloroethane and 20% of 2-iodo-1,1,1,2,3,3,3-heptafluoropropane was mixed with 45 g of polyisocyanate based on methylene diisocyanate , And the resulting mixture is poured into 4500 ml of 3% aqueous polyvinyl alcohol in an amount of 2 ml per second, and the propeller agitator is stirred at a speed of 3000 rpm to produce a microemulsion having droplets of an average size of 90 탆.
450 ml of a 10% aqueous solution of polyethylenepolyamine is added to the microemulsion in an amount of 0.25 ml per second and aged at 20 캜 for 4 days to increase the shell thickness of the reaction mixture thus obtained by 0.03-0.3 탆.
The following liquids were separated to obtain a highly concentrated suspension containing 780 g of microcapsules having an overall average size of 90 mu m occupying 90% of the size of 80 to 100 mu m, where the content of the extinguishing agent was 89%.
20 g of aqueous solution polyacrylic resin was added to the suspension, and the resultant mixture was thoroughly mixed to obtain a 0.5-mm-thick material, which was then completely dried to complete the preparation of the extinguishing agent composition.
The extinguishing agent composition prepared in Example 4 was digested within 10 seconds as a result of the digestibility test described above, and the microcapsule was released at a temperature of 110 to 125 ° C.
[Example 5]
1000 g of an extinguishing agent consisting of 80% of 1,1,2-trifluorotrichloroethane and 20% of 2-iodo-1,1,1,2,3,3,3-heptafluoropropane was mixed with 60 g of polyisocyanate based on methylene diisocyanate , The resulting mixture is poured into 5000 ml of 3% aqueous polyvinyl alcohol in an amount of 1 ml per second, and the propeller stirrer is agitated at a speed of 3500 rpm to produce a microemulsion having droplets of an average size of 50 탆.
700 ml of a 10% aqueous solution of polyethylenepolyamine is added to the microemulsion in an amount of 0.25 ml per second and aged at 60 ° C for 1 day to increase the shell thickness of the reaction mixture thus obtained by 0.03-0.3 μm.
The following liquids were separated to obtain a highly concentrated suspension containing 1120 g of microcapsules having a total average size of 50 mu m occupying 87% of the size of 45-55 mu m with an extinguishing agent content of 85%.
20 g of the aqueous solution latex resin was added to the suspension, and the resultant mixture was thoroughly mixed to obtain a 0.3 mm thick layer. The layer was completely dried to complete the preparation of the extinguishing agent composition.
The extinguishing agent composition prepared in Example 5 was digested within 10 seconds as a result of the digestibility test described above, and the microcapsule was released at 130 to 150 ° C.
[Example 6]
1000 g of 1,1,2,2-tetrafluoro dibromethane digesting agent was mixed with 60 g of toluene isocyanate polyisocyanate, and the resulting mixture was poured into 5000 ml of 3% aqueous polyvinyl alcohol in an amount of 1 ml per second, and the propeller stirrer was rotated at a rate of 3500 rpm To produce a microemulsion having droplets of an average size of 80 mu m.
400 ml of a 5% aqueous solution of polyethylenepolyamine is added to the microemulsion in an amount of 0.25 ml per second and aged at 60 ° C for 1 day to increase the shell thickness of the reaction mixture thus obtained by 0.03 to 0.3 탆.
The following liquids were separated to obtain a highly concentrated suspension containing 1100 g of microcapsules with an overall average size of 80 mu m occupying 81% of the size of 70-90 mu m with an extinguishing agent content of 85%.
30 g of aqueous alkyd varnish was added to the suspension, and the resultant mixture was thoroughly mixed. The resultant material was applied to a thickness of 0.2 mm and then completely dried to complete the preparation of the extinguishing agent composition.
The extinguishing agent composition prepared in Example 6 was digested within 12 seconds as a result of the digestibility test described above, and the microcapsule was released at 110 to 130 ° C.
[Example 7]
500 g of 1,1,2,2-tetrafluoro dibromethane digesting agent was mixed with 30 g of toluene isocyanate polyisocyanate, and the resulting mixture was poured into 2,000 ml of 3% aqueous polyvinyl alcohol in an amount of 1 ml per second, and the propeller stirrer was rotated at a speed of 3000 rpm To produce a microemulsion having droplets of an average size of 50 mu m.
200 ml of a 10% pentaerythritol aqueous solution is added to the microemulsion in 0.25 ml per second and aged at 75 캜 for 1 day to increase the shell thickness of the reaction mixture thus obtained by 0.05 to 0.2 탆.
The following liquids were separated to obtain a highly concentrated suspension containing 550 g of microcapsules having a total average size of 50 mu m occupying 83% of the size of 45-55 mu m, where the content of the extinguishing agent was 81%.
10 g of aqueous solution polyurethane varnish was added to this suspension and thoroughly mixed to obtain a 0.25-mm-thick material. The material was then completely dried to complete the preparation of the extinguishing agent composition.
The extinguishing agent composition prepared according to Example 7 was digested within 10 seconds as a result of the digestibility test described above and the microcapsule was released at 120 to 145 ° C.
Although the technical idea of the present invention has been described above, it is to be understood that the present invention is not limited thereto.
In addition, it is a matter of course that various modifications and variations are possible without departing from the scope of the technical idea of the present invention by anyone having ordinary skill in the art.
Claims (15)
Wherein the shell is made of at least one of polyurea and polyurethane based on polyisocyanate prepolymer,
At least 80% of the extinguishing agent is concentrated into the composition, the size of the microcapsule is doubled so that a small microcapsule can be positioned between the large microcapsules for high concentration of the extinguishing agent,
Wherein the composition is at least one chain selected from the group consisting of ammonium dinitramide (ADN), dinitramide salt (N (NO 2 ) - ) which is a non - chlorine based oxidizer, and diamine dihydrate (CDD) A reaction promoting material,
At least one low molecular weight material selected from the group consisting of polybutadiene, butadiene styrene rubber, butadiene acrylonitrile rubber, polychloroprene, polyisoprene, chlorosulfonated polyethylene, polyisobutylene, and isobutylene isoprene rubber, Wherein the halogen-based gas-extinguishing agent composition further comprises a halogen-based gas-extinguishing agent composition.
The halogen carbon may be at least one selected from the group consisting of fluorine carbon, fluorine chlorine carbon, fluorine bromine carbon halocarbon, fluorine iodine carbon halogen carbon, 2-iodine-1,1,1,2,3,3,3-heptafluoropropane (HFC- 227ea) and at least one of Iodofluorocarbon (FIC-217I1 or FIC-13I1).
Wherein the microcapsules have a diameter of 10 to 50 占 퐉.
Wherein the polymer connecting body is made of at least one material selected from the group consisting of acrylic, alkyd, glyptal, latex, nitrocellulose, epoxy, polyvinyl chloride, polyurethane, polyurea, polyvinyl alcohol, and polyvinyl acetate. Pharmaceutical composition.
(b) mixing a polyamine aqueous solution or pentaerythritol in the microemulsion at a weight ratio of 1: 0.1 to 1: 1 until a sheath is formed;
(c) aging the mixture obtained in step (b) at 20 to 60 ° C. for 1 to 4 days until the thickness of the outer skin reaches 0.03 to 0.3 μm; And
(d) separating the microcapsules obtained in the step (c) from water, and
(e) a group consisting of ammonium dinatraimide (ADN), dinitramide salt (N (NO 2 ) - ) which is a non - chlorine oxidizing agent, and copper diamine dinitrate (CDD) Is selected from the group consisting of polybutadiene, butadiene styrene rubber, butadiene acrylonitrile rubber, polychloroprene, polyisoprene, chlorosulfonated polyethylene, polyisobutylene, and isobutylene isoprene rubber. Heat-resistant synthetic rubber, wherein the low-
Wherein the method comprises the step of reducing the size of the microcapsules so that small microcapsules are located between large microcapsules for high concentration of the extinguishing agent.
Wherein at least one of polyvinyl alcohol and a derivative thereof is used as a surfactant in the step (a).
Wherein the size of the microcapsules obtained in step (d) is 10 to 50 占 퐉.
Wherein the mixture is stirred at a rate of 2,500 to 3,500 rpm in the step (a).
Wherein the polyisocyanate is replaced with at least one of toluene diisocyanate, methylene diisocyanate series or similar series polyisocyanate in the step (a).
In step (b), H 2 N (CH 2 CH 2 NH) n H, n = 1-5 (mono-, di-, tri-, tetra-, pentaethylene hexamines) Polyethylene polyamines, and polyethylene polyamines. ≪ RTI ID = 0.0 > 21. < / RTI >
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| CN108837367A (en) * | 2018-06-01 | 2018-11-20 | 潘洋 | A kind of preparation method and application of environment-friendly type aqueous film-forming foam extinguishing agent |
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