CN113476778B - High-stability fire-extinguishing microcapsule and preparation method thereof - Google Patents
High-stability fire-extinguishing microcapsule and preparation method thereof Download PDFInfo
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- CN113476778B CN113476778B CN202110685536.1A CN202110685536A CN113476778B CN 113476778 B CN113476778 B CN 113476778B CN 202110685536 A CN202110685536 A CN 202110685536A CN 113476778 B CN113476778 B CN 113476778B
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- diisocyanate
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- microcapsule
- fire extinguishing
- extinguishing agent
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- 239000003094 microcapsule Substances 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims description 15
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 72
- 238000006243 chemical reaction Methods 0.000 claims abstract description 34
- -1 trihydroxymethyl dodecane-diisocyanate Chemical compound 0.000 claims abstract description 33
- 108010010803 Gelatin Proteins 0.000 claims abstract description 25
- 229920000159 gelatin Polymers 0.000 claims abstract description 25
- 239000008273 gelatin Substances 0.000 claims abstract description 25
- 235000019322 gelatine Nutrition 0.000 claims abstract description 25
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 25
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 23
- 239000011162 core material Substances 0.000 claims abstract description 19
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 15
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000004202 carbamide Substances 0.000 claims abstract description 15
- 239000008098 formaldehyde solution Substances 0.000 claims abstract description 15
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229920005749 polyurethane resin Polymers 0.000 claims abstract description 10
- BFDRQZUBFIOWOF-UHFFFAOYSA-N tridecane-1,1,1-triol Chemical compound CCCCCCCCCCCCC(O)(O)O BFDRQZUBFIOWOF-UHFFFAOYSA-N 0.000 claims abstract description 6
- IVJISJACKSSFGE-UHFFFAOYSA-N formaldehyde;1,3,5-triazine-2,4,6-triamine Chemical class O=C.NC1=NC(N)=NC(N)=N1 IVJISJACKSSFGE-UHFFFAOYSA-N 0.000 claims abstract description 5
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229940018564 m-phenylenediamine Drugs 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 53
- 238000003756 stirring Methods 0.000 claims description 32
- 229920000642 polymer Polymers 0.000 claims description 28
- 239000000463 material Substances 0.000 claims description 26
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 239000000839 emulsion Substances 0.000 claims description 17
- 229910052799 carbon Inorganic materials 0.000 claims description 16
- 239000000725 suspension Substances 0.000 claims description 15
- 239000012153 distilled water Substances 0.000 claims description 13
- 239000007864 aqueous solution Substances 0.000 claims description 11
- 150000001875 compounds Chemical class 0.000 claims description 11
- ZAFNJMIOTHYJRJ-UHFFFAOYSA-N Diisopropyl ether Chemical compound CC(C)OC(C)C ZAFNJMIOTHYJRJ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 230000007935 neutral effect Effects 0.000 claims description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- MNFZXIVKYRSXEA-UHFFFAOYSA-N 2-(hydroxymethyl)-2-undecylpropane-1,3-diol Chemical compound CCCCCCCCCCCC(CO)(CO)CO MNFZXIVKYRSXEA-UHFFFAOYSA-N 0.000 claims description 7
- WVSNNWIIMPNRDB-UHFFFAOYSA-N 1,1,1,3,3,4,4,5,5,6,6,6-dodecafluorohexan-2-one Chemical compound FC(F)(F)C(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F WVSNNWIIMPNRDB-UHFFFAOYSA-N 0.000 claims description 6
- 239000004114 Ammonium polyphosphate Substances 0.000 claims description 6
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 6
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 6
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 6
- 235000019826 ammonium polyphosphate Nutrition 0.000 claims description 6
- 229920001276 ammonium polyphosphate Polymers 0.000 claims description 6
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 6
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 6
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 239000003995 emulsifying agent Substances 0.000 claims description 5
- 230000001804 emulsifying effect Effects 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- FDYWJVHETVDSRA-UHFFFAOYSA-N 1,1-diisocyanatobutane Chemical compound CCCC(N=C=O)N=C=O FDYWJVHETVDSRA-UHFFFAOYSA-N 0.000 claims description 4
- VKLNMSFSTCXMSB-UHFFFAOYSA-N 1,1-diisocyanatopentane Chemical compound CCCCC(N=C=O)N=C=O VKLNMSFSTCXMSB-UHFFFAOYSA-N 0.000 claims description 4
- BZQKBFHEWDPQHD-UHFFFAOYSA-N 1,2,3,4,5-pentabromo-6-[2-(2,3,4,5,6-pentabromophenyl)ethyl]benzene Chemical compound BrC1=C(Br)C(Br)=C(Br)C(Br)=C1CCC1=C(Br)C(Br)=C(Br)C(Br)=C1Br BZQKBFHEWDPQHD-UHFFFAOYSA-N 0.000 claims description 4
- NNOZGCICXAYKLW-UHFFFAOYSA-N 1,2-bis(2-isocyanatopropan-2-yl)benzene Chemical compound O=C=NC(C)(C)C1=CC=CC=C1C(C)(C)N=C=O NNOZGCICXAYKLW-UHFFFAOYSA-N 0.000 claims description 4
- FKTHNVSLHLHISI-UHFFFAOYSA-N 1,2-bis(isocyanatomethyl)benzene Chemical compound O=C=NCC1=CC=CC=C1CN=C=O FKTHNVSLHLHISI-UHFFFAOYSA-N 0.000 claims description 4
- MTZUIIAIAKMWLI-UHFFFAOYSA-N 1,2-diisocyanatobenzene Chemical compound O=C=NC1=CC=CC=C1N=C=O MTZUIIAIAKMWLI-UHFFFAOYSA-N 0.000 claims description 4
- RTTZISZSHSCFRH-UHFFFAOYSA-N 1,3-bis(isocyanatomethyl)benzene Chemical compound O=C=NCC1=CC=CC(CN=C=O)=C1 RTTZISZSHSCFRH-UHFFFAOYSA-N 0.000 claims description 4
- OHLKMGYGBHFODF-UHFFFAOYSA-N 1,4-bis(isocyanatomethyl)benzene Chemical compound O=C=NCC1=CC=C(CN=C=O)C=C1 OHLKMGYGBHFODF-UHFFFAOYSA-N 0.000 claims description 4
- CDMDQYCEEKCBGR-UHFFFAOYSA-N 1,4-diisocyanatocyclohexane Chemical compound O=C=NC1CCC(N=C=O)CC1 CDMDQYCEEKCBGR-UHFFFAOYSA-N 0.000 claims description 4
- SBJCUZQNHOLYMD-UHFFFAOYSA-N 1,5-Naphthalene diisocyanate Chemical compound C1=CC=C2C(N=C=O)=CC=CC2=C1N=C=O SBJCUZQNHOLYMD-UHFFFAOYSA-N 0.000 claims description 4
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical compound C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 claims description 4
- KEZMBAQUUXDDDQ-UHFFFAOYSA-N CCC.N=C=O.N=C=O Chemical compound CCC.N=C=O.N=C=O KEZMBAQUUXDDDQ-UHFFFAOYSA-N 0.000 claims description 4
- KYIMHWNKQXQBDG-UHFFFAOYSA-N N=C=O.N=C=O.CCCCCC Chemical compound N=C=O.N=C=O.CCCCCC KYIMHWNKQXQBDG-UHFFFAOYSA-N 0.000 claims description 4
- OHRVBDRGLIWLPA-UHFFFAOYSA-N [3-hydroxy-2,2-bis(hydroxymethyl)propyl] dihydrogen phosphate Chemical compound OCC(CO)(CO)COP(O)(O)=O OHRVBDRGLIWLPA-UHFFFAOYSA-N 0.000 claims description 4
- 239000003063 flame retardant Substances 0.000 claims description 4
- 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 claims description 3
- GNFTZDOKVXKIBK-UHFFFAOYSA-N 3-(2-methoxyethoxy)benzohydrazide Chemical compound COCCOC1=CC=CC(C(=O)NN)=C1 GNFTZDOKVXKIBK-UHFFFAOYSA-N 0.000 claims description 2
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 2
- 230000001737 promoting effect Effects 0.000 description 13
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 9
- 238000012360 testing method Methods 0.000 description 5
- PYSRRFNXTXNWCD-UHFFFAOYSA-N 3-(2-phenylethenyl)furan-2,5-dione Chemical compound O=C1OC(=O)C(C=CC=2C=CC=CC=2)=C1 PYSRRFNXTXNWCD-UHFFFAOYSA-N 0.000 description 3
- 229920000147 Styrene maleic anhydride Polymers 0.000 description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 239000008346 aqueous phase Substances 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 239000004970 Chain extender Substances 0.000 description 2
- 239000002390 adhesive tape Substances 0.000 description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 description 2
- 239000002775 capsule Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000004677 Nylon Substances 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001722 carbon compounds Chemical class 0.000 description 1
- 238000012669 compression test Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 239000012074 organic phase Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229920001059 synthetic polymer Polymers 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
- A62D1/0007—Solid extinguishing substances
- A62D1/0021—Microcapsules
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Business, Economics & Management (AREA)
- Emergency Management (AREA)
- Manufacturing Of Micro-Capsules (AREA)
Abstract
A high-stability fire-extinguishing microcapsule and its preparing process, wherein the fire-extinguishing microcapsule comprises a shell and a core material, the core material comprises fire-extinguishing agent, the shell comprises an inner layer, an outer layer and an air-tight promoter, the inner layer comprises modified melamine-formaldehyde resin generated by the reaction of melamine, m-phenylenediamine, urea and formaldehyde solution, the outer layer adopts modified polyurethane resin generated by the reaction of trihydroxymethyl dodecane-diisocyanate adduct and gelatin solution, and the trihydroxymethyl dodecane-diisocyanate adduct is generated by the reaction of trihydroxymethyl dodecane and diisocyanate compound. The shell of the fire-extinguishing microcapsule has the characteristics of high stability, high toughness and high air tightness, and can effectively reduce the leakage of the core material and prolong the service life of the fire-extinguishing microcapsule.
Description
Technical Field
The invention relates to the technical field of fire extinguishing products, in particular to a high-stability fire extinguishing microcapsule and a preparation method thereof.
Background
The fire extinguishing microcapsule is prepared through dispersing fire extinguishing agent in the state of particle or micro liquid drop and forming one inert protecting shell with natural or synthetic polymer material. When the burning happens, the protective film of the capsule is destroyed to release the fire extinguishing agent, thereby achieving the effect of fire extinguishing and fire retardation.
In the prior art, the fire extinguishing microcapsule has the technical problem of poor stability, and the shell of the fire extinguishing microcapsule is easy to leak in the processes of storage and use, so that the fire extinguishing microcapsule is difficult to store and has short service life.
Disclosure of Invention
In order to solve the technical problems, the invention provides a high-stability fire-extinguishing microcapsule and a preparation method thereof, wherein the shell of the fire-extinguishing microcapsule has the characteristics of high stability, high toughness and high air tightness, and can effectively reduce the leakage of a core material and prolong the service life of the fire-extinguishing microcapsule.
In order to realize the purpose, the invention adopts the technical scheme that:
provided is a high-stability fire-extinguishing microcapsule, which comprises a shell and a core material, wherein the core material comprises a fire-extinguishing agent, the shell comprises an inner layer, an outer layer and an air tightness improver, the inner layer comprises modified melamine-formaldehyde resin generated by the reaction of melamine, m-phenylenediamine, urea and formaldehyde solution, the outer layer adopts modified polyurethane resin generated by the reaction of a trimethyloldodecane diisocyanate adduct and a gelatin solution, and the trimethyloldodecane diisocyanate adduct is generated by the reaction of trimethyloldodecane and a diisocyanate compound.
The particle size of the fire-extinguishing microcapsule is in the range of 3-15 microns.
The fire extinguishing agent of the fire extinguishing microcapsule accounts for 75-95% of the total mass of the fire extinguishing microcapsule.
As a further improvement of the invention, the air tightness promoter adopts a compound of double isopropyl oxide and lamellar carbon; the fire extinguishing agent is an inorganic fire extinguishing agent or an organic fire extinguishing agent; the inorganic fire extinguishing agent adopts one or more of red phosphorus, Al (OH)3 and ammonium polyphosphate; the organic fire extinguishing agent adopts one or more of an intumescent flame retardant pentaerythritol phosphate, perfluorohexanone and decabromodiphenylethane.
As a further improvement of the invention, the core material also comprises a thermochromism material which generates color change at 100-150 ℃; the thermochromic material adopts BiV03 or leuco dye. The thermochromic material can generate color change at the temperature of 100-150 ℃, so that the occurrence of fire is warned for people, and the personal and property losses are reduced. The color change temperature of the thermochromic material cannot be too low, otherwise, the sunlight irradiation can also generate color change, so that a user is misled, the temperature cannot be too high, early warning can be delayed due to too high temperature, and the effect of timely early warning cannot be achieved.
As a further improvement of the invention, the diisocyanate compound is selected from one of the following compounds: propane diisocyanate, butane diisocyanate, pentane diisocyanate, hexane diisocyanate, methylhexane-1, 6-diisocyanate, 3-dimethylpentane-1, 5-diisocyanate, 1, 3-and 1, 4-cyclohexylene diisocyanate, isophorone diisocyanate, toluene diisocyanate, m-and p-xylylene diisocyanate, phenylene diisocyanate, naphthalene-1, 5-diisocyanate, xylylene diisocyanate, diphenylmethane-4, 4' -diisocyanate, tetramethylxylylene diisocyanate, hexamethylene diisocyanate.
The fire-extinguishing microcapsule can be used as a fire-extinguishing additive. The fire extinguishing microcapsule and the coating are uniformly mixed to prepare fire extinguishing coating, and the fire extinguishing coating is sprayed or roll-coated on important parts with fire hidden danger, such as the inner side wall of a distribution box, the interior of a motor vehicle, an explosion-proof cable joint protection box, the inner wall of a battery box and a cable bridge, and the like; or the fire extinguishing microcapsule and the double faced adhesive tape patch are made into a fire extinguishing patch which is fixed in a small space protection space; or the fire extinguishing microcapsule is combined with a nylon rope to prepare a fire extinguishing rope which is wound in the protection space; or the fire-extinguishing microcapsule is blended into high-voltage electrical tape to prepare fire-extinguishing adhesive tape which is wrapped on the cable joint.
The invention also provides a preparation method of the high-stability fire-extinguishing microcapsule, which comprises the following steps:
a) stirring the airtight improver at high speed by using a high-speed stirrer to form airtight improver suspension;
b) reacting melamine, formaldehyde solution, urea, resorcinol and distilled water, and then adding half of the airtight promoter suspension for mixing to obtain an inner shell polymer solution;
c) adding an emulsifier into the fire extinguishing agent, and then heating, emulsifying and stirring to form fire extinguishing agent emulsion;
d) dripping the inner shell polymer solution on the fire extinguishing agent emulsion, and then stirring;
e) solidifying the shell layer and forming a microcapsule water solution A;
f) reacting trihydroxymethyl dodecane with a diisocyanate compound to generate a trihydroxymethyl dodecane-diisocyanate adduct, reacting the trihydroxymethyl dodecane-diisocyanate adduct with a gelatin solution, and then adding the other half of the airtight improver suspension to obtain an outer shell polymer solution;
g) dripping microcapsule aqueous solution A into the outer shell polymer solution, and then stirring;
h) and curing the shell layer again to form a microcapsule aqueous solution B, and then drying to obtain microcapsule particles.
As a further improvement of the invention, in the step b), when the melamine, the formaldehyde solution, the urea, the resorcinol and the distilled water are reacted, the reaction temperature is controlled to be 60-80 ℃, the pH is adjusted to be 8.5-9.5, and the stirring is carried out for at least 1 hour.
As a further improvement of the invention, in the step c), a thermochromism material which generates color change at the temperature of 100-150 ℃ is also added into the fire extinguishing agent emulsion; the thermochromic material adopts BiV03 or leuco dye.
As a further improvement of the invention, in the step d), the inner shell polymer solution is dripped into the fire extinguishing agent emulsion by using a separating funnel, then the pH of the system is adjusted to be 3.5-4.5, the reaction temperature is controlled to be 65-85 ℃, the stirring is carried out for at least 3 hours, the pH of the system is adjusted to be neutral after the reaction is finished, and then the cooling is carried out.
As a further development of the invention, in step f) the trimethyloldodecane-diisocyanate adduct is formed by reacting trimethyloldodecane with a diisocyanate compound; the diisocyanate compound is selected from the following compounds: propane diisocyanate, butane diisocyanate, pentane diisocyanate, hexane diisocyanate, methylhexane-1, 6-diisocyanate, 3-dimethylpentane-1, 5-diisocyanate, 1, 3-and 1, 4-cyclohexylene diisocyanate, isophorone diisocyanate, toluene diisocyanate, m-and p-xylylene diisocyanate, phenylene diisocyanate, naphthalene-1, 5-diisocyanate, xylylene diisocyanate, diphenylmethane-4, 4' -diisocyanate, tetramethylxylylene diisocyanate, hexamethylene diisocyanate; the gelatin solution needs to be kept at a constant temperature of 30-40 ℃.
As a further improvement of the invention, in step g), the microcapsule aqueous solution a is added dropwise to the outer shell polymer solution by using a separating funnel, then the pH of the system is adjusted to 3.5-4.5, the reaction temperature is controlled to 65-85 ℃, stirring is carried out for at least 3 hours, the pH of the system is adjusted to be neutral after the reaction is finished, and then cooling is carried out.
As a further development of the invention, in steps e) and h), the shell is cured by maintaining the temperature at 40-50 ℃ and at this temperature for at least 3.5 hours.
As a further improvement of the invention, the air tightness promoter adopts a compound of double isopropyl oxide and lamellar carbon; the fire extinguishing agent is an inorganic fire extinguishing agent or an organic fire extinguishing agent; the inorganic fire extinguishing agent adopts one or more of red phosphorus, Al (OH)3 and ammonium polyphosphate; the organic fire extinguishing agent adopts one or more of an intumescent flame retardant pentaerythritol phosphate, perfluorohexanone and decabromodiphenylethane.
In the high-stability fire-extinguishing microcapsule and the preparation method thereof, the weight parts of the components are as follows:
3-7 parts of fire extinguishing agent, 1-3 parts of thermochromic material, 1-3 parts of melamine, 2-5 parts of formaldehyde solution, 0.1-0.8 part of urea, 1-4 parts of resorcinol, 3-7 parts of trimethyloldodecane, 8-12 parts of diisocyanate compound, 1-3 parts of gelatin and 2-5 parts of air tightness improver. Wherein the concentration of the formaldehyde solution is 1-12%.
The invention has the beneficial effects that:
in the invention, the modified melamine-formaldehyde resin added with urea is used in the inner layer, compared with the existing melamine-formaldehyde resin wall material, the strength of the wall material can be improved, the surface of the wall material is smoother, and the thermal stability of the wall material can be obviously improved due to the resorcinol containing a benzene ring rigid structure.
Compared with the existing polyurethane wall material, the capsule wall material in the organic phase is generated by the polymerization reaction of the trihydroxymethyl dodecane-diisocyanate adduct and active groups containing multi-meridian groups and multi-oxygen groups at the interface of two phases, the trihydroxymethyl long-chain alkane is used as a chain extender, the content of the trihydroxymethyl long-chain alkane in the adduct is reduced along with the increase of the molecular weight of the chain extender, the content of the hard segment is reduced, the strength of the polymer is reduced, the elasticity is increased, and the toughness of the wall material is improved.
In the invention, the modified melamine-formaldehyde resin of the inner layer can provide enough strength, while the modified polyurethane resin of the outer layer can provide enough toughness, and the two are combined, so that the shell can be broken at the temperature of 180-220 ℃, the breaking temperature is high, the fire-extinguishing microcapsule is easy to store, the leakage of the fire-extinguishing microcapsule caused by the change of the air temperature is avoided, and the stability is strong.
Meanwhile, the air tightness promoting agent can enhance the air tightness of the fire extinguishing microcapsule, and prevent the fire extinguishing agent from gasifying and overflowing the microcapsule at high temperature to cause the reduction of the concentration of the fire extinguishing agent and the reduction of repeated fire extinguishing effect.
In addition, because the fire-extinguishing microcapsule adopts a double-layer shell design, the outer shell is firstly broken in a fire disaster, and a part of fire extinguishing agent is released to extinguish the fire so as to quickly cool down, so that the unreleased inner layer is kept in the original state, and in the reburning fire disaster, the unbroken inner layer is released and broken again to play a role in extinguishing the secondary fire disaster.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1:
a high-stability fire-extinguishing microcapsule comprises a shell and a core material, wherein the core material comprises a fire-extinguishing agent and a thermochromic material which generates color change at the temperature of 100 ℃ and 150 ℃, and the shell comprises an inner layer, an outer layer and an air tightness promoter.
Wherein, 5 parts of perfluorohexanone is adopted as a fire extinguishing agent; 1 part of BiV03 is adopted as a thermochromic material; the inner layer is melamine-formaldehyde resin generated by the reaction of 2 parts of melamine, 3.86 parts of 2% formaldehyde solution, 0.2 part of urea and 2 parts of resorcinol; adopting modified polyurethane resin as an outer layer, wherein the modified polyurethane resin is prepared by reacting a trihydroxymethyl dodecane-diisocyanate adduct generated by reacting 5 parts of trihydroxymethyl dodecane with 10 parts of hexamethylene diisocyanate and 1 part of gelatin; 3 parts of a composite of the double isopropyl oxide and the lamellar carbon is used as the air tightness promoter.
The preparation steps of the fire-extinguishing microcapsule are as follows:
a) adding 3 parts of airtight promoting agent into a stirring tank, wherein the airtight promoting agent is a compound of double isopropyl oxide and lamellar carbon, and stirring the airtight promoting agent at high speed for 30 minutes by using a high-speed stirrer to form airtight promoting agent suspension;
b) putting 2 parts of melamine, 3.86 parts of 2% formaldehyde solution, 0.2 part of urea, 2 parts of resorcinol and a proper amount of distilled water into a three-neck flask, then putting the three-neck flask into a water bath kettle for reaction, controlling the temperature of the water bath kettle to be 70 ℃, adjusting the pH value of the solution to be 9.0 by using triethanolamine, stirring for at least one hour to obtain a transparent prepolymer solution, and mixing the prepolymer solution with half of the airtight promoter suspension to obtain an inner shell polymer solution;
c) dissolving 5 parts of perfluorohexanone serving as a fire extinguishing agent in distilled water, adding a styrene-maleic anhydride polymer serving as an emulsifier, heating, emulsifying and stirring for 15 minutes to form a fire extinguishing agent emulsion; 1 part of thermochromic material BiV03 is added into the fire extinguishing agent emulsion.
d) Dropwise adding the inner shell polymer solution onto the fire extinguishing agent emulsion by using a separating funnel, then adjusting the pH of the system to 4 by using citric acid, controlling the reaction temperature to be 75 ℃, stirring for at least 3 hours, adjusting the pH of the system to be neutral by using alkali after the reaction is finished, and then cooling;
e) then curing the shell layer by maintaining the temperature at 45 ℃ and at this temperature for at least 3.5 hours to form an aqueous microcapsule solution A;
f) 5 parts of trimethyloldodecane and 10 parts of hexamethylene diisocyanate were reacted to produce a trimethyloldodecane-diisocyanate adduct, 1 part of gelatin was added to 100 parts of distilled water, heated and stirred until the gelatin was completely dissolved to form a gelatin solution, and then kept at a constant temperature of 35 ℃ as an aqueous phase. The trihydroxymethyl dodecane-diisocyanate addition product reacts with the gelatin solution, and then the other half of the airtight promoter suspension is added to obtain an outer shell polymer solution;
g) dropwise adding the microcapsule aqueous solution A into the outer-layer shell polymer solution by using a separating funnel, then adjusting the pH of the system to 4, controlling the reaction temperature to be 75 ℃, stirring for at least 3 hours, adjusting the pH of the system to be neutral after the reaction is finished, and then cooling;
h) the solidification of the shell layer to form the microcapsule aqueous solution B is again carried out by maintaining the temperature at 45 ℃ and at this temperature for at least 3.5 hours, followed by drying to obtain microcapsule particles.
Example 2:
a high-stability fire-extinguishing microcapsule comprises a shell and a core material, wherein the core material comprises a fire-extinguishing agent and a thermochromic material which generates color change at the temperature of 100 ℃ and 150 ℃, and the shell comprises an inner layer, an outer layer and an air tightness promoter.
Wherein, 4 parts of red phosphorus and 3 parts of Al (OH)3 are adopted as fire extinguishing agents; 2 parts of leuco dye is adopted as a thermochromic material; the inner layer is melamine-formaldehyde resin generated by the reaction of 3 parts of melamine, 4 parts of 4% formaldehyde solution, 0.4 part of urea and 3 parts of resorcinol; adopting a modified polyurethane resin as an outer layer, wherein the modified polyurethane resin is prepared by reacting a trihydroxymethyl dodecane-diisocyanate adduct generated by reacting 4 parts of trihydroxymethyl dodecane with 11 parts of isophorone diisocyanate and 2 parts of gelatin; 4 parts of double isopropyl oxide and lamellar carbon compound are adopted as the air tightness promoter.
The preparation steps of the fire-extinguishing microcapsule are as follows:
a) adding 4 parts of airtight promoting agent into a stirring tank, wherein the airtight promoting agent is a compound of double isopropyl oxide and lamellar carbon, and stirring the airtight promoting agent at high speed for 30 minutes by using a high-speed stirrer to form airtight promoting agent suspension;
b) putting 3 parts of melamine, 4 parts of 4% formaldehyde solution, 0.4 part of urea, 3 parts of resorcinol and a proper amount of distilled water into a three-necked bottle, then putting the three-necked bottle into a water bath kettle for reaction, controlling the temperature of the water bath kettle to be 60 ℃, adjusting the pH value of the solution to be 8.5 by using triethanolamine, stirring for at least one hour to obtain a transparent prepolymer solution, and mixing the prepolymer solution with half of the airtight promoter suspension to obtain an inner shell polymer solution;
c) dissolving 4 parts of red phosphorus and 3 parts of Al (OH)3 serving as fire extinguishing agents in distilled water, adding a styrene-maleic anhydride polymer serving as an emulsifier, and heating, emulsifying and stirring for 15 minutes to form fire extinguishing agent emulsion; 2 parts of leuco dye is added into the fire extinguishing agent emulsion.
d) Dropwise adding the inner shell polymer solution onto the fire extinguishing agent emulsion by using a separating funnel, then adjusting the pH of the system to 4 by using citric acid, controlling the reaction temperature to be 80 ℃, stirring for at least 3 hours, adjusting the pH of the system to be neutral by using alkali after the reaction is finished, and then cooling;
e) then curing the shell layer by keeping the temperature at 50 ℃ and keeping at this temperature for at least 3.5 hours to form a microcapsule aqueous solution A;
f) 4 parts of trimethyloldodecane and 11 parts of isophorone diisocyanate are reacted to generate a trimethyloldodecane-diisocyanate adduct, 2 parts of gelatin is added into 100 parts of distilled water, heated and stirred until the gelatin is completely dissolved to form a gelatin solution, and then the gelatin solution is kept at a constant temperature of 40 ℃ to be an aqueous phase. The trihydroxymethyl dodecane-diisocyanate addition product reacts with the gelatin solution, and then the other half of the airtight promoter suspension is added to obtain an outer shell polymer solution;
g) dropwise adding the microcapsule aqueous solution A into the outer-layer shell polymer solution by using a separating funnel, then adjusting the pH of the system to 4, controlling the reaction temperature to be 80 ℃, stirring for at least 3 hours, adjusting the pH of the system to be neutral after the reaction is finished, and then cooling;
h) the solidification of the shell layer to form the microcapsule aqueous solution B is again carried out by maintaining the temperature at 50 ℃ and at this temperature for at least 3.5 hours, followed by drying to obtain microcapsule particles.
Example 3:
a high-stability fire-extinguishing microcapsule comprises a shell and a core material, wherein the core material comprises a fire-extinguishing agent and a thermochromic material which generates color change at the temperature of 100 ℃ and 150 ℃, and the shell comprises an inner layer, an outer layer and an air tightness promoter.
Wherein, 4 parts of ammonium polyphosphate is adopted as a fire extinguishing agent; 1 part of BiV03 is adopted as a thermochromic material; the inner layer is melamine-formaldehyde resin generated by the reaction of 3 parts of melamine, 4 parts of 6% formaldehyde solution, 0.8 part of urea and 3 parts of resorcinol; adopting modified polyurethane resin as an outer layer, wherein the modified polyurethane resin is prepared by reacting a trihydroxymethyl dodecane-diisocyanate adduct generated by reacting 7 parts of trihydroxymethyl dodecane with 12 parts of toluene diisocyanate and 3 parts of gelatin; 2 parts of a composite of the double isopropyl oxide and the lamellar carbon is used as the air tightness promoter.
The preparation steps of the fire-extinguishing microcapsule are as follows:
a) adding 2 parts of airtight promoting agent into a stirring tank, wherein the airtight promoting agent is a compound of double isopropyl oxide and lamellar carbon, and stirring the airtight promoting agent at high speed for 30 minutes by using a high-speed stirrer to form airtight promoting agent suspension;
b) putting 3 parts of melamine, 4 parts of 6% formaldehyde solution, 0.8 part of urea, 3 parts of resorcinol and a proper amount of distilled water into a three-necked bottle, then putting the three-necked bottle into a water bath kettle for reaction, controlling the temperature of the water bath kettle to be 80 ℃, adjusting the pH value of the solution to be 8.5 by using triethanolamine, stirring for at least one hour to obtain a transparent prepolymer solution, and mixing the prepolymer solution with half of the airtight promoter suspension to obtain an inner shell polymer solution;
c) dissolving 4 parts of ammonium polyphosphate serving as a fire extinguishing agent in distilled water, adding a styrene-maleic anhydride polymer serving as an emulsifier, heating, emulsifying and stirring for 15 minutes to form a fire extinguishing agent emulsion; 1 part of thermochromic material BiV03 is added into the fire extinguishing agent emulsion.
d) Dropwise adding the inner shell polymer solution onto the fire extinguishing agent emulsion by using a separating funnel, adjusting the pH of the system to 4.5 by using citric acid, controlling the reaction temperature to be 70 ℃, stirring for at least 3 hours, adjusting the pH of the system to be neutral by using alkali after the reaction is finished, and then cooling;
e) then curing the shell layer by maintaining the temperature at 40 ℃ and at this temperature for at least 3.5 hours to form an aqueous microcapsule solution A;
f) 7 parts of trimethyloldodecane and 12 parts of toluene diisocyanate are reacted to generate a trimethyloldodecane-diisocyanate adduct, 3 parts of gelatin is added into 100 parts of distilled water, heated and stirred until the gelatin is completely dissolved to form a gelatin solution, and then the gelatin solution is kept at a constant temperature of 30 ℃ to be an aqueous phase. The trihydroxymethyl dodecane-diisocyanate addition product reacts with the gelatin solution, and then the other half of the airtight promoter suspension is added to obtain an outer shell polymer solution;
g) dropwise adding the microcapsule aqueous solution A into the outer-layer shell polymer solution by using a separating funnel, then adjusting the pH of the system to 4.5, controlling the reaction temperature to be 70 ℃, stirring for at least 3 hours, adjusting the pH of the system to be neutral after the reaction is finished, and then cooling;
h) the solidification of the shell layer was again carried out by maintaining the temperature at 40 ℃ and at this temperature for at least 3.5 hours to form an aqueous microcapsule solution B, followed by drying to obtain microcapsule particles.
And (3) detecting property performance:
through detection, the average particle size of the fire-extinguishing microcapsule prepared in the embodiment 1-3 is 3-15 microns, the film thickness is 0.01-0.07 micron, the content of the effective fire-extinguishing agent in the obtained fire-extinguishing microcapsule is 90%, and effective fire extinguishing is completed within 13 seconds of fire.
Air tightness test
The conditions are that the fire extinguishing microcapsule is stored for about 24 hours at the temperature of 100 ℃, and the loss degree of the core material in the fire extinguishing microcapsule is measured. The test results show that the air tightness of the fire-extinguishing microcapsule prepared in examples 1-3 is less than 1%. In addition, the loss is less than 1% at the temperature of 100 ℃, which is equivalent to that in the daily temperature using environment, the fire-extinguishing microcapsule can stably store the fire-extinguishing core material coated in the fire-extinguishing microcapsule for more than 5 years.
Mechanical Strength test (pressure test)
The self-made thickness is 2mm, and the area is 5cm2The microcapsule accumulation body is subjected to compression test under the condition of applying the same external force, the loss degree of the core material in the fire extinguishing microcapsule is measured, and three grades are divided,>the content of the active ingredients is preferably 80%,>60% is normal, and the following are differences.
The performance of the three tests is shown in table 1, and table 1 is the performance test data of the examples.
TABLE 1
The above-mentioned embodiments are only for convenience of illustration and not intended to limit the invention in any way, and those skilled in the art will be able to make equivalents of the features of the invention without departing from the technical scope of the invention.
Claims (9)
1. A high-stability fire extinguishing microcapsule comprises a shell and a core material, wherein the core material comprises a fire extinguishing agent, and is characterized in that: the outer shell comprises an inner layer and an outer layer, the inner layer comprises an airtight promoter and a modified melamine-formaldehyde resin produced by reacting melamine, m-phenylenediamine, urea and a formaldehyde solution, the outer layer comprises an airtight promoter and a modified polyurethane resin produced by reacting a trimethyloldodecane-diisocyanate adduct produced by reacting trimethyloldodecane with a diisocyanate compound with a gelatin solution;the gas tightness promoter adopts a compound of double isopropyl oxide and lamellar carbon; the fire extinguishing agent is an inorganic fire extinguishing agent or an organic fire extinguishing agent; the inorganic fire extinguishing agent adopts red phosphorus, Al (OH)3And ammonium polyphosphate; the organic fire extinguishing agent adopts one or more of expansion type fire retardants pentaerythritol phosphate, perfluorohexanone and decabromodiphenylethane, and the addition amount of the air tightness promoter in the inner layer and the outer layer is equal.
2. A high-stability fire-extinguishing microcapsule according to claim 1, characterized in that: the diisocyanate compound is selected from the following compounds: propane diisocyanate, butane diisocyanate, pentane diisocyanate, hexane diisocyanate, methylhexane-1, 6-diisocyanate, 3-dimethylpentane-1, 5-diisocyanate, 1, 3-and 1, 4-cyclohexylene diisocyanate, isophorone diisocyanate, toluene diisocyanate, m-and p-xylylene diisocyanate, phenylene diisocyanate, naphthalene-1, 5-diisocyanate, xylylene diisocyanate, diphenylmethane-4, 4' -diisocyanate, tetramethylxylylene diisocyanate, hexamethylene diisocyanate.
3. A high-stability fire-extinguishing microcapsule according to claim 1, characterized in that: the core material also comprises a thermochromic material which generates color change at 100-150 ℃; the thermochromic material adopts BiVO3Or a leuco dye.
4. A preparation method of a high-stability fire-extinguishing microcapsule is characterized by comprising the following steps:
a) stirring the airtight improver at high speed by using a high-speed stirrer to form airtight improver suspension;
b) reacting melamine, formaldehyde solution, urea, resorcinol and distilled water, and then adding half of the airtight promoter suspension for mixing to obtain an inner shell polymer solution;
c) adding an emulsifier into the fire extinguishing agent, and then heating, emulsifying and stirring to form fire extinguishing agent emulsion;
d) dripping the inner shell polymer solution on the fire extinguishing agent emulsion, and then stirring;
e) solidifying the shell layer and forming a microcapsule water solution A;
f) reacting trihydroxymethyl dodecane with a diisocyanate compound to generate a trihydroxymethyl dodecane-diisocyanate adduct, reacting the trihydroxymethyl dodecane-diisocyanate adduct with a gelatin solution, and then adding the other half of the airtight improver suspension to obtain an outer shell polymer solution;
g) dripping microcapsule aqueous solution A into the outer shell polymer solution, and then stirring;
h) solidifying the shell layer again to form a microcapsule water solution B, and then drying to obtain microcapsule particles;
the gas tightness promoter adopts a compound of double isopropyl oxide and lamellar carbon; the fire extinguishing agent is an inorganic fire extinguishing agent or an organic fire extinguishing agent; the inorganic fire extinguishing agent adopts red phosphorus, Al (OH)3And ammonium polyphosphate; the organic fire extinguishing agent adopts one or more of an intumescent flame retardant pentaerythritol phosphate, perfluorohexanone and decabromodiphenylethane.
5. The preparation method of the high-stability fire-extinguishing microcapsule according to claim 4, wherein: in the step b), when the melamine, the formaldehyde solution, the urea, the resorcinol and the distilled water are reacted, the reaction temperature is controlled to be 60-80 ℃, the pH value is adjusted to be 8.5-9.5, and the stirring is carried out for at least 1 hour.
6. The preparation method of the high-stability fire-extinguishing microcapsule according to claim 4, wherein: in the step c), a thermochromism material which generates color change at 100-150 ℃ is also added into the fire extinguishing agent emulsion; the thermochromic material adopts BiVO3Or a leuco dye.
7. The preparation method of the high-stability fire-extinguishing microcapsule according to claim 4, wherein: in the step d), dropwise adding the inner shell polymer solution onto the fire extinguishing agent emulsion by using a separating funnel, then adjusting the pH of the system to 3.5-4.5, controlling the reaction temperature to 65-85 ℃, stirring for at least 3 hours, adjusting the pH of the system to be neutral after the reaction is finished, and then cooling; in the step g), the microcapsule aqueous solution A is dripped into the outer-layer shell polymer solution by using a separating funnel, then the pH of the system is adjusted to be 3.5-4.5, the reaction temperature is controlled to be 65-85 ℃, the stirring is carried out for at least 3 hours, the pH of the system is adjusted to be neutral after the reaction is finished, and then the cooling is carried out.
8. The preparation method of the high-stability fire-extinguishing microcapsule according to claim 4, wherein: in the step f), the diisocyanate compound is selected from one of the following compounds: propane diisocyanate, butane diisocyanate, pentane diisocyanate, hexane diisocyanate, methylhexane-1, 6-diisocyanate, 3-dimethylpentane-1, 5-diisocyanate, 1, 3-and 1, 4-cyclohexylene diisocyanate, isophorone diisocyanate, toluene diisocyanate, m-and p-xylylene diisocyanate, phenylene diisocyanate, naphthalene-1, 5-diisocyanate, xylylene diisocyanate, diphenylmethane-4, 4' -diisocyanate, tetramethylxylylene diisocyanate, hexamethylene diisocyanate; the gelatin solution needs to be kept at a constant temperature of 30-40 ℃.
9. The preparation method of the high-stability fire-extinguishing microcapsule according to claim 4, wherein: in steps e) and h), the curing of the shell is carried out by maintaining the temperature at 40-50 ℃ and at this temperature for at least 3.5 hours.
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