CN116333559A - Preparation method of high-temperature-resistant CNPU@TEOS water-based intumescent fireproof coating - Google Patents
Preparation method of high-temperature-resistant CNPU@TEOS water-based intumescent fireproof coating Download PDFInfo
- Publication number
- CN116333559A CN116333559A CN202310263270.0A CN202310263270A CN116333559A CN 116333559 A CN116333559 A CN 116333559A CN 202310263270 A CN202310263270 A CN 202310263270A CN 116333559 A CN116333559 A CN 116333559A
- Authority
- CN
- China
- Prior art keywords
- cnpu
- teos
- temperature
- water
- resistant
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000000576 coating method Methods 0.000 title claims abstract description 49
- 239000011248 coating agent Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 40
- 239000003063 flame retardant Substances 0.000 claims abstract description 35
- 229910000831 Steel Inorganic materials 0.000 claims abstract description 21
- 239000010959 steel Substances 0.000 claims abstract description 21
- 239000003822 epoxy resin Substances 0.000 claims description 34
- 229920000647 polyepoxide Polymers 0.000 claims description 34
- 238000003756 stirring Methods 0.000 claims description 18
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 12
- 229920000877 Melamine resin Polymers 0.000 claims description 10
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 10
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 10
- 239000003973 paint Substances 0.000 claims description 9
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 8
- DUNKXUFBGCUVQW-UHFFFAOYSA-J zirconium tetrachloride Chemical compound Cl[Zr](Cl)(Cl)Cl DUNKXUFBGCUVQW-UHFFFAOYSA-J 0.000 claims description 8
- TXBCBTDQIULDIA-UHFFFAOYSA-N 2-[[3-hydroxy-2,2-bis(hydroxymethyl)propoxy]methyl]-2-(hydroxymethyl)propane-1,3-diol Chemical compound OCC(CO)(CO)COCC(CO)(CO)CO TXBCBTDQIULDIA-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- GPNNOCMCNFXRAO-UHFFFAOYSA-N 2-aminoterephthalic acid Chemical compound NC1=CC(C(O)=O)=CC=C1C(O)=O GPNNOCMCNFXRAO-UHFFFAOYSA-N 0.000 claims description 5
- 230000001680 brushing effect Effects 0.000 claims description 4
- 229920000388 Polyphosphate Polymers 0.000 claims description 3
- 229960000583 acetic acid Drugs 0.000 claims description 3
- 239000012362 glacial acetic acid Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000001205 polyphosphate Substances 0.000 claims description 3
- 235000011176 polyphosphates Nutrition 0.000 claims description 3
- 239000000725 suspension Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 21
- 229910052799 carbon Inorganic materials 0.000 abstract description 19
- 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 abstract description 7
- 230000003647 oxidation Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 230000007547 defect Effects 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 230000009545 invasion Effects 0.000 abstract description 3
- 238000012546 transfer Methods 0.000 abstract description 3
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 23
- 229920002873 Polyethylenimine Polymers 0.000 description 8
- 239000013207 UiO-66 Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 238000005187 foaming Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000779 smoke Substances 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000005260 alpha ray Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000013096 zirconium-based metal-organic framework Substances 0.000 description 1
Images
Classifications
-
- 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Paints Or Removers (AREA)
Abstract
The invention discloses a preparation method of a high-temperature-resistant CNPU@TEOS water-based intumescent fireproof coating, which comprises the following steps: (1) preparation of a base material; (2) preparation of CNPU nano hybrid material; (3) preparing CNPU@TEOS nano hybrid material; (4) And (3) preparing the high-temperature-resistant CNPU@TEOS water-based intumescent fireproof coating. The modified CNPU@TEOS nano hybrid material is combined with the water-based intumescent fireproof coating, so that the defects of low strength, poor oxidation resistance and insufficient flame retardant property of the conventional water-based fireproof coating are overcome, and the obtained nano water-based fireproof coating forms a high-strength carbon layer at high temperature, so that heat transfer can be effectively inhibited, and a protection effect is achieved. The invention is mainly used for protecting the fire disaster of the steel structure, resists flame invasion when the fire disaster occurs, prolongs the failure time of the steel structure, thereby striving for precious time for fire rescue and having wide industrial application value.
Description
Technical Field
The invention belongs to the field of preparation methods of epoxy composite coatings, and particularly relates to a preparation method and application of a high-temperature-resistant CNPU@TEOS water-based intumescent fireproof coating.
Background
The steel structure has the advantages of light weight, strong bearing capacity and easy decoration, is an important base material widely used in modern large-scale buildings, but if the exposed steel structure is affected by strong fire, the mechanical property of the exposed steel structure is rapidly deteriorated, so that the structure is instable and damaged, and the life and property safety of personnel in the fire environment is threatened. Therefore, it is an urgent necessity to solve the fatal disadvantage that the steel structure is not resistant to high temperature. Coating the surface of the steel substrate with the aqueous fire retardant coating (IFR) is an effective and environmentally friendly method to address the poor thermal stability. When the flame retardant principle is that under the action of high temperature, a fluffy molten carbon layer is rapidly formed on the surface of the coating, so that external heat and combustible gas are reduced, the heating rate of the steel structure is further delayed, the rapid damage of the performance of the steel structure is prevented, and time is striven for rescue. However, the existing water-based intumescent fire-retardant coating has low carbon layer strength and uneven foaming, so that the thermal stability of the coating is insufficient, and therefore, an effective strategy needs to be formulated to solve the defects of the water-based fire-retardant coating, and further application of the water-based fire-retardant coating is promoted. Research shows that the existing condition can be improved and the flame retardant property of the fireproof paint can be enhanced by adding inorganic nano-filler into an expansion system, such as black phosphorus, graphene, boron nitride and the like. Therefore, a zirconium-based metal organic framework (UiO-66) is loaded on the surface of graphite phase Carbon Nitride (CN) by using Polyethylenimine (PEI) as a connecting agent and combined with Tetraethoxysilane (TEOS) to form the multifunctional synergistic efficient flame retardant CNPU@TEOS. Wherein CN provides physical barrier function, and isolates heat and combustible gas; the UiO-66 not only can improve the dispersibility of CN in water, but also can endow the nano material with a catalytic function, so as to promote the formation of a tighter carbon layer; TEOS can form a hollow structure at high temperature to enhance thermal barrier and smoke adsorption, thereby further enhancing the thermal stability and smoke suppression performance of the fireproof coating. And then the high-efficiency flame retardant is utilized to improve the fireproof performance of the water-based intumescent fireproof coating, including the flame retardant performance, the heat stability performance and the strength of the carbon layer.
Disclosure of Invention
The invention provides a preparation method of a high-temperature-resistant CNPU@TEOS water-based intumescent fire-retardant coating, which aims at the defects of poor heat stability, low carbon layer strength, nonuniform foaming and the like of the water-based intumescent fire-retardant coating, and exploits the application of a CNPU@TEOS flame retardant in the field of fire-retardant coatings.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
the preparation method of the high-temperature-resistant CNPU@TEOS water-based intumescent fire-retardant coating is characterized by comprising the following steps of:
s1: preparation of base material: weighing epoxy resin, a curing agent and an expansion component (melamine polyphosphate (MPP), dipentaerythritol (DPER) and Melamine (MEL)), stirring for 3h at 300r/min, and stirring for 2h at 60r/min to obtain a uniformly mixed base material;
s2: preparing a CNPU nano hybrid material: uniformly dispersing a certain amount of CN in 200mL of deionized water, adding a certain amount of PEI, stirring at room temperature for 6h, washing with pure water for several times to obtain a hybrid material CNP, dissolving a certain amount of the obtained CNP in 80mL of N, N-Dimethylformamide (DMF), transferring the solution to a 250mL three-neck flask, and adding a certain amount of zirconium tetrachloride (ZrCl) 4 ) Stirring for 1h at room temperature, adding a certain amount of 2-amino terephthalic acid and 4mL glacial acetic acid into the mixture, continuously reacting for 24h at 120 ℃, and centrifuging and drying to obtain a CNPU nano hybrid material;
s3: preparing a CNPU@TEOS nano hybrid material: adding a certain amount of CNPU into 100mL of deionized water, stirring by using a constant-temperature magnetic stirrer to obtain a suspension, adding a certain amount of cetyltrimethylammonium bromide (CTAB) and 2mL of TEOS, reacting for 2 hours, washing for a plurality of times by using ethanol, and drying to obtain a CNPU@TEOS nano hybrid material;
s4: preparation of high-temperature-resistant CNPU@TEOS water-based intumescent fireproof paint: mechanically stirring the base material and the CNPU@TEOS nano hybrid material for 5 hours to form a uniform dispersion system, then brushing the uniform dispersion system on the surface of a steel sheet, and curing for 7 days at normal temperature after brushing to obtain a high-temperature-resistant CNPU@TEOS water-based intumescent fire-retardant coating;
further, in the step S1, the mass ratio of the epoxy resin to the curing agent is 2:1, a step of;
further, in the step S1, the mass ratio of the epoxy resin to the expansion component is 2-3:1, a step of;
further, in the step S1, the mass ratio of MPP, DPER, MEL is 5.4-6.6:2.6-3.4:1, a step of;
further, in step S2, the mass ratio of CN to PEI is 1:4-10;
further, CNP and ZrCl are added in step S2 4 The mass ratio of the 2-amino terephthalic acid is 1:1.5-1.7:1.1 to 1.4;
further, in step S3, the mass ratio of CNPU to CTAB is 1:1.5-2.5;
further, the CNPU@TEOS nano hybrid material in the step S4 accounts for 1% -5% of the total weight of the uniform dispersion system.
The beneficial effects are that:
compared with the prior art, the invention has the following beneficial effects:
the preparation method of the high-temperature-resistant CNPU@TEOS water-based intumescent fire-retardant coating provided by the invention solves the dangerous characteristics of low strength, poor oxidation resistance and uneven expansion of the existing water-based fire-retardant coating, the obtained nano water-based fire-retardant coating can form a high-strength carbon layer at high temperature, the flame retardance and oxidation resistance of the carbon layer are enhanced, the heat transfer can be effectively inhibited, and the protection effect is achieved. The invention is mainly used for protecting the fire disaster of the steel structure, resists flame invasion when the fire disaster occurs, prolongs the time of failure caused by the rise of the temperature of the steel structure, and thus strives for precious time for fire disaster rescue. The water-based fireproof paint has the advantages of easily available raw materials, simple preparation, low cost, environmental protection and wide industrial application value.
Drawings
FIG. 1 is an X-ray diffraction pattern of CN, CNP, uiO-66, CNPU, CNPU@TEOS.
FIG. 2 is a transmission electron microscope image of CN, CNP, uiO-66, CNPU, CNPU@TEOS, wherein A is CN, B is CNP, C is CNPU, and D is CNPU@TEOS.
FIG. 3 is a scanning electron microscope image of the sections of the EP, CN/EP, CNP/EP, CNPU/EP, CNPU@TEOS/EP coating, wherein A is EP, B is CN/EP, C is CNP/EP, D is CNPU/EP, E is CNPU@TEOS/EP.
FIG. 4 is a graph showing the temperature of the back surface of a steel sheet after the large plate test.
FIG. 5 is a scanning electron microscope image of the carbon layer after the large plate test, wherein A is EP, B is CN/EP, C is CNP/EP, D is CNPU/EP, and E is CNPU@TEOS/EP.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Examples:
a preparation method of a high-temperature-resistant CNPU@TEOS water-based intumescent fire-retardant coating specifically comprises the following steps:
s1: weighing 50g of epoxy resin, 25g of curing agent and 25g of expansion system (15 g of melamine polyphosphate, 7.5g of dipentaerythritol and 2.5g of melamine), mechanically stirring for 3 hours at 300r/min, and then stirring for 2 hours at 60r/min to obtain a uniformly mixed base material;
s2: preparing a CNPU nano hybrid material: uniformly dispersing 0.2g of CN in 200mL of deionized water, adding 1g of PEI, stirring at room temperature for 6 hours, washing with pure water several times to obtain a hybrid material CNP, then dissolving 0.2g of the obtained CNP in 80mL of N, N-Dimethylformamide (DMF), transferring the solution to a 250mL three-necked flask, and then adding 0.32g of zirconium tetrachloride (ZrCl) 4 ) Stirring for 1h at room temperature, adding 2-amino terephthalic acid (0.25 g) and 4mL glacial acetic acid into the mixture, continuously reacting for 24h at 120 ℃, and centrifugally drying to obtain a CNPU nano hybrid material;
s3: preparing a CNPU@TEOS nano hybrid material: adding 0.2g of CNPU into 100mL of deionized water, stirring by using a constant-temperature magnetic stirrer to obtain a suspension, adding 0.4g of Cetyl Trimethyl Ammonium Bromide (CTAB) and 2mL of TEOS, reacting for 2 hours, washing with ethanol for multiple times, and drying to obtain a CNPU@TEOS nano hybrid material;
s4: preparation of high-temperature-resistant CNPU@TEOS water-based intumescent fireproof paint: and mechanically stirring the base material (98 g) and the CNPU@TEOS nano hybrid material (2 g) for 5h to form a uniform dispersion system, then coating the uniform dispersion system on the surface of the steel sheet, and curing for 7 days at normal temperature after coating is finished to obtain the high-temperature-resistant CNPU@TEOS water-based intumescent fireproof coating.
The present example shows the experimental analysis results related to the preparation method of the high temperature resistant CNPU@TEOS water-based intumescent fire retardant coating provided herein.
CN/EP, CNP/EP, CNPU/EP and cnpu@teos/EP water-based intumescent fire-retardant coatings were prepared using 2g of CN, CNP, CNPU and cnpu@teos and 98g of binder, respectively, and the fire-retardant coatings were painted on the blasted steel sheet using pure epoxy resin (EP) as a control, and cured at room temperature for 7 days to obtain test samples.
(1) The crystal structures of CN, CNP, uiO-66, CNPU and CNPU@TEOS were characterized by X-ray diffraction (XRD, X Pert PROMPD, cu K alpha ray diffraction, 5-80 ℃). The results are shown in FIG. 1. As can be seen from FIG. 1, in the XRD spectrum of the CNPU@TEOS nano hybrid material, the characteristic diffraction peaks of CN and UiO-66 can be detected simultaneously, which indicates that the UiO-66 is successfully loaded on the surface of CN through PEI. After loading with TEOS, the XRD peak intensity was reduced due to the coverage of TEOS.
(2) The morphology of CN, CNP, CNPU and CNPU@TEOS nano hybrid materials is observed by adopting a JEOL JEM-2100 high-resolution transmission electron microscope (HR-TEM), and the result is shown in figure 2. As can be seen from fig. 2A, the CN is wide and large in lamellar structure; after being modified by PEI (figure 2B), a layer of PEI is uniformly loaded on the surface of CN; after loading UiO-66 (fig. 2C), regular octahedron UiO-66 with evenly distributed CN surface can be observed; when modified with TEOS (fig. 2D), the nanomaterial edges are capped with a thin TEOS layer. The result shows that the CNPU@TEOS nano hybrid material is successfully synthesized.
(3) The cross-sectional morphology of each coating was observed by a JSM-7500F scanning electron microscope, and the results are shown in FIG. 3. As can be seen from fig. 3A, the pure EP has a smooth cross-section, exhibiting typical brittle fracture. After the filler is added, the section of the coating presents the characteristic of toughness and fracture. As can be seen from fig. 3E, the cnpu@teos nano hybrid material is uniformly dispersed in the coating, and the cross section is rough, which indicates that the interaction force between the cnpu@teos and the resin is strong.
(4) And testing the temperature of the back surface of the steel plate by adopting a large plate method to detect the fireproof performance of the fireproof paint. The results are shown in FIG. 4. As can be seen from fig. 4, the temperature of the back surface of the steel plate of the water-based fireproof paint containing the nano hybrid material of cnpu@teos is the lowest, and compared with pure EP, the temperature is reduced by 38.2%, which indicates that the strength and the flame retardance of the carbon layer can be effectively improved by the cnpu@teos, the heat blocking is increased, the temperature rise of the back surface of the steel plate is further effectively slowed down, and the fireproof performance is improved.
(5) The structure of the carbon layer after the large plate test is tested by adopting a JSM-7500F scanning electron microscope, and the result is shown in figure 5. As can be seen from fig. 5, cracks are found in the carbon layers of EP, CN/EP, CNP/EP and CNPU/EP, after the cnpu@teos nano hybrid material is added (fig. 5E), the cracks on the carbon layer disappear, the carbon layer structure is compact and complete, and a typical carbon layer network structure is presented, which indicates that the strength of the carbon layer is increased, the structural stability is enhanced, and thus the heat blocking capability is enhanced, and the problems of low strength and insufficient flame retardance of the water-based fireproof paint carbon layer can be effectively improved by adding the cnpu@teos nano hybrid material.
The preparation method of the high-temperature-resistant CNPU@TEOS water-based intumescent fire-retardant coating provided by the invention solves the dangerous characteristics of low strength, poor oxidation resistance and uneven expansion of the existing water-based fire-retardant coating, the obtained nano water-based fire-retardant coating can form a high-strength carbon layer at high temperature, the flame retardance and oxidation resistance of the carbon layer are enhanced, the heat transfer can be effectively inhibited, and the protection effect is achieved. The invention is mainly used for protecting the fire disaster of the steel structure, resists flame invasion when the fire disaster occurs, prolongs the time of failure caused by the rise of the temperature of the steel structure, and thus strives for precious time for fire disaster rescue. The water-based fireproof paint has the advantages of easily available raw materials, simple preparation, low cost, environmental protection and wide industrial application value.
The present invention is not limited to the above-mentioned embodiments, but is not limited to the above-mentioned embodiments, and any person skilled in the art can make some changes or modifications to the equivalent embodiments without departing from the scope of the technical solution of the present invention, but any simple modification, equivalent changes and modifications to the above-mentioned embodiments according to the technical substance of the present invention are still within the scope of the technical solution of the present invention.
Claims (8)
1. The preparation method of the high-temperature-resistant CNPU@TEOS water-based intumescent fire-retardant coating is characterized by comprising the following steps of:
s1: preparation of base material: weighing epoxy resin, a curing agent and an expansion component (melamine polyphosphate (MPP), dipentaerythritol (DPER) and Melamine (MEL)), stirring for 3h at 300r/min, and stirring for 2h at 60r/min to obtain a uniformly mixed base material;
s2: preparing a CNPU nano hybrid material: uniformly dispersing a certain amount of CN in 200mL of deionized water, adding a certain amount of PEI, stirring at room temperature for 6h, washing with pure water for several times to obtain a hybrid material CNP, dissolving a certain amount of the obtained CNP in 80mL of N, N-Dimethylformamide (DMF), transferring the solution to a 250mL three-neck flask, and adding a certain amount of zirconium tetrachloride (ZrCl) 4 ) Stirring for 1h at room temperature, adding a certain amount of 2-amino terephthalic acid and 4mL glacial acetic acid into the mixture, continuously reacting for 24h at 120 ℃, and centrifuging and drying to obtain a CNPU nano hybrid material;
s3: preparing a CNPU@TEOS nano hybrid material: adding a certain amount of CNPU into 100mL of deionized water, stirring by using a constant-temperature magnetic stirrer to obtain a suspension, adding a certain amount of cetyltrimethylammonium bromide (CTAB) and 2mL of TEOS, reacting for 2 hours, washing for a plurality of times by using ethanol, and drying to obtain a CNPU@TEOS nano hybrid material;
s4: preparation of high-temperature-resistant CNPU@TEOS water-based intumescent fireproof paint: and mechanically stirring the base material and the CNPU@TEOS nano hybrid material for 5 hours to form a uniform dispersion system, then brushing the uniform dispersion system on the surface of the steel sheet, and curing for 7 days at normal temperature after brushing is finished to obtain the high-temperature-resistant CNPU@TEOS water-based intumescent fire-retardant coating.
2. The preparation method of the high-temperature-resistant CNPU@TEOS water-based intumescent fire-retardant coating as claimed in claim 1, wherein the mass ratio of epoxy resin to curing agent in the step S1 is 2:1.
3. the preparation method of the high-temperature-resistant CNPU@TEOS water-based intumescent fire-retardant coating as claimed in claim 1, wherein the mass ratio of epoxy resin to intumescent component in the step S1 is 2-3:1.
4. the method for preparing the high-temperature-resistant CNPU@TEOS water-based intumescent fire-retardant coating as claimed in claim 1, wherein the mass ratio of MPP, DPER, MEL in the step S1 is 5.4-6.6:2.6-3.4:1.
5. the method for preparing the high-temperature-resistant CNPU@TEOS water-based intumescent fire-retardant coating as claimed in claim 1, wherein in the step S2, the mass ratio of CN to PEI is 1:4-10.
6. The method for preparing the high-temperature-resistant CNPU@TEOS water-based intumescent fire retardant coating as claimed in claim 1, wherein in the step S2, CNP and ZrCl are prepared by the following steps 4 The mass ratio of the 2-amino terephthalic acid is 1:1.5-1.7:1.1-1.4.
7. The method for preparing the high-temperature-resistant CNPU@TEOS water-based intumescent fire-retardant coating as claimed in claim 1, wherein in the step S3, the mass ratio of CNPU to CTAB is 1:1.5-2.5.
8. The method for preparing the high-temperature-resistant CNPU@TEOS water-based intumescent fire-retardant coating according to claim 1, wherein the CNPU@TEOS nano hybrid material in the step S4 accounts for 1% -5% of the total weight of the uniform dispersion system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310263270.0A CN116333559B (en) | 2023-03-17 | 2023-03-17 | Preparation method of high-temperature-resistant CNPU@TEOS water-based intumescent fireproof coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202310263270.0A CN116333559B (en) | 2023-03-17 | 2023-03-17 | Preparation method of high-temperature-resistant CNPU@TEOS water-based intumescent fireproof coating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN116333559A true CN116333559A (en) | 2023-06-27 |
| CN116333559B CN116333559B (en) | 2024-03-01 |
Family
ID=86894239
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310263270.0A Active CN116333559B (en) | 2023-03-17 | 2023-03-17 | Preparation method of high-temperature-resistant CNPU@TEOS water-based intumescent fireproof coating |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN116333559B (en) |
Citations (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005119260A (en) * | 2003-09-26 | 2005-05-12 | Dainippon Printing Co Ltd | Fire retardant film, interior material for house using it, electric product or printing film |
| JP2009090632A (en) * | 2007-09-19 | 2009-04-30 | Fujifilm Corp | Laminated film and light emitting element or display element using the same |
| JP2011127252A (en) * | 2009-12-18 | 2011-06-30 | Kuraray Co Ltd | Heat and flame resistant paper |
| CN106833176A (en) * | 2017-03-03 | 2017-06-13 | 北京茂源防火材料厂 | Aqueous indoor thin section steel structure fire-resisting paint of energy decomposing formaldehyde and preparation method thereof |
| CN110591156A (en) * | 2019-09-20 | 2019-12-20 | 武汉工程大学 | Zirconium phosphate flame retardant modified based on graphitized carbon nitride composite intercalation and preparation method thereof |
| CN110591388A (en) * | 2019-08-22 | 2019-12-20 | 安徽建筑大学 | Flame-retardant smoke suppressant containing cobalt, nitrogen and silicon and preparation method thereof |
| CN112592492A (en) * | 2020-12-31 | 2021-04-02 | 河北大学 | Flame retardant, flame-retardant epoxy resin and preparation methods of flame retardant and flame-retardant epoxy resin |
| US20210108092A1 (en) * | 2019-10-15 | 2021-04-15 | Swimc, Llc | Intumescent coating compositions effective at low |
| CA3154766A1 (en) * | 2019-10-14 | 2021-04-22 | James M. Tour | Porous polymeric carbon sorbents for co2 capture and methods of making and using same |
| CN113980551A (en) * | 2021-11-15 | 2022-01-28 | 西南石油大学 | Hydrotalcite-based water-based epoxy resin intumescent fire-retardant coating |
| CN113998966A (en) * | 2020-07-27 | 2022-02-01 | 傅吾录 | Efficient multifunctional environment-friendly zeolite wall material and preparation method thereof |
| CN114450354A (en) * | 2019-10-15 | 2022-05-06 | Swimc有限公司 | Low temperature effective intumescent coating composition |
| WO2022099321A1 (en) * | 2020-11-09 | 2022-05-12 | Washington State University | Conversion of co-mingled waste plastics to monomers and fuels in sequential catalytic process |
| CN114672221A (en) * | 2022-04-07 | 2022-06-28 | 西南石油大学 | Preparation method of BP @ ZHS-based ultrathin water-based expansion fireproof coating |
| CN115304810A (en) * | 2022-09-02 | 2022-11-08 | 乌镇实验室 | Preparation method of PEI/MOF/PEI composite membrane material with sandwich structure |
-
2023
- 2023-03-17 CN CN202310263270.0A patent/CN116333559B/en active Active
Patent Citations (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005119260A (en) * | 2003-09-26 | 2005-05-12 | Dainippon Printing Co Ltd | Fire retardant film, interior material for house using it, electric product or printing film |
| JP2009090632A (en) * | 2007-09-19 | 2009-04-30 | Fujifilm Corp | Laminated film and light emitting element or display element using the same |
| JP2011127252A (en) * | 2009-12-18 | 2011-06-30 | Kuraray Co Ltd | Heat and flame resistant paper |
| CN106833176A (en) * | 2017-03-03 | 2017-06-13 | 北京茂源防火材料厂 | Aqueous indoor thin section steel structure fire-resisting paint of energy decomposing formaldehyde and preparation method thereof |
| CN110591388A (en) * | 2019-08-22 | 2019-12-20 | 安徽建筑大学 | Flame-retardant smoke suppressant containing cobalt, nitrogen and silicon and preparation method thereof |
| CN110591156A (en) * | 2019-09-20 | 2019-12-20 | 武汉工程大学 | Zirconium phosphate flame retardant modified based on graphitized carbon nitride composite intercalation and preparation method thereof |
| CA3154766A1 (en) * | 2019-10-14 | 2021-04-22 | James M. Tour | Porous polymeric carbon sorbents for co2 capture and methods of making and using same |
| CN114450354A (en) * | 2019-10-15 | 2022-05-06 | Swimc有限公司 | Low temperature effective intumescent coating composition |
| US20210108092A1 (en) * | 2019-10-15 | 2021-04-15 | Swimc, Llc | Intumescent coating compositions effective at low |
| CN113998966A (en) * | 2020-07-27 | 2022-02-01 | 傅吾录 | Efficient multifunctional environment-friendly zeolite wall material and preparation method thereof |
| WO2022099321A1 (en) * | 2020-11-09 | 2022-05-12 | Washington State University | Conversion of co-mingled waste plastics to monomers and fuels in sequential catalytic process |
| CN112592492A (en) * | 2020-12-31 | 2021-04-02 | 河北大学 | Flame retardant, flame-retardant epoxy resin and preparation methods of flame retardant and flame-retardant epoxy resin |
| CN113980551A (en) * | 2021-11-15 | 2022-01-28 | 西南石油大学 | Hydrotalcite-based water-based epoxy resin intumescent fire-retardant coating |
| CN114672221A (en) * | 2022-04-07 | 2022-06-28 | 西南石油大学 | Preparation method of BP @ ZHS-based ultrathin water-based expansion fireproof coating |
| CN115304810A (en) * | 2022-09-02 | 2022-11-08 | 乌镇实验室 | Preparation method of PEI/MOF/PEI composite membrane material with sandwich structure |
Non-Patent Citations (3)
| Title |
|---|
| MIN CAO等: "Synergetic modification of graphitic carbon nitride by Zr-based metal-organic framework and tetraethoxysilane for improving fire performance in composite coatings", 《PROGRESS IN ORGANIC COATINGS》, vol. 183 * |
| PING LYU等: "Composites Filled with Metal Organic Frameworks and Their Derivatives: Recent Developments in Flame Retardants", 《POLYMERS》, vol. 14, no. 23, pages 1 - 22 * |
| 张朝岭等: "新型金属-有机骨架/纤维素气凝胶杂化材料的研究进展", 《功能材料》, vol. 53, no. 06, pages 06049 - 06059 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN116333559B (en) | 2024-03-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101955710B (en) | Water-borne nano ultra-thin steel structure fire retardant coating and preparation method thereof | |
| CN111592813A (en) | Intumescent fire-retardant coating and preparation method thereof | |
| CN112322167A (en) | Intumescent steel structure fireproof coating | |
| KR20090116042A (en) | Fire resistive intumescent coatings and it's use | |
| CN110862748B (en) | Fireproof heat-insulating coating and preparation method and application thereof | |
| CN112940611B (en) | High-performance expansion type sandwich structure ultrathin steel structure fireproof and anticorrosive composite coating and preparation method thereof | |
| CN114539886B (en) | Fireproof coating for ships and marine facilities, preparation method and fireproof separation structure | |
| CN109627867B (en) | Graphene modified fireproof coating and preparation method thereof | |
| CN110607101B (en) | Water-based fireproof heat-insulating coating, fireproof material and preparation method thereof | |
| CN113980551A (en) | Hydrotalcite-based water-based epoxy resin intumescent fire-retardant coating | |
| CN111171657A (en) | Energy-saving environment-friendly fireproof coating and preparation method thereof | |
| CN116333559B (en) | Preparation method of high-temperature-resistant CNPU@TEOS water-based intumescent fireproof coating | |
| CN113493624B (en) | Biomass flame retardant, water-based flame retardant coating, and preparation method and application thereof | |
| CN108559359A (en) | A kind of fire-resistant coating for steel structure and preparation method thereof of decalescence, expandable flame retardant | |
| WO2021175065A1 (en) | Organic-inorganic hybrid fireproof coating and preparation method therefor | |
| CN105670356A (en) | Fireproof waterborne coating for steel structures | |
| CN112251052A (en) | High-temperature-resistant heat-preservation dry powder functional film | |
| CN116285478A (en) | Basalt inorganic long crystal flake fireproof paint and preparation method thereof | |
| CN113480928B (en) | Fireproof coating | |
| CN113321959B (en) | Epoxy expansion type steel structure fireproof paint for spraying fire scene | |
| CN113999583A (en) | Ultrathin flame-retardant water-based paint for manufacturing tank and preparation method thereof | |
| CN112175436B (en) | Inorganic expansion type fire-proof paint | |
| CN110256879B (en) | Environment-friendly water-based inorganic flame-retardant coating | |
| CN112662235A (en) | Water-based bio-based flame-retardant luminescent coating and preparation method and application thereof | |
| CN114517036A (en) | Functional heat-insulating fireproof waterproof anticorrosive paint |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |