CN114874541A - Flame-retardant smoke-suppressing polymer composite material and preparation method thereof - Google Patents
Flame-retardant smoke-suppressing polymer composite material and preparation method thereof Download PDFInfo
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- CN114874541A CN114874541A CN202210392561.5A CN202210392561A CN114874541A CN 114874541 A CN114874541 A CN 114874541A CN 202210392561 A CN202210392561 A CN 202210392561A CN 114874541 A CN114874541 A CN 114874541A
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- 239000002131 composite material Substances 0.000 title claims abstract description 109
- 239000003063 flame retardant Substances 0.000 title claims abstract description 89
- 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 title claims abstract description 85
- 229920000642 polymer Polymers 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 142
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 142
- BNEMLSQAJOPTGK-UHFFFAOYSA-N zinc;dioxido(oxo)tin Chemical compound [Zn+2].[O-][Sn]([O-])=O BNEMLSQAJOPTGK-UHFFFAOYSA-N 0.000 claims abstract description 91
- 229920005989 resin Polymers 0.000 claims abstract description 71
- 239000011347 resin Substances 0.000 claims abstract description 71
- 238000000034 method Methods 0.000 claims abstract description 56
- 239000011159 matrix material Substances 0.000 claims abstract description 45
- 239000000779 smoke Substances 0.000 claims abstract description 33
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 29
- 238000011065 in-situ storage Methods 0.000 claims abstract description 20
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- BHTBHKFULNTCHQ-UHFFFAOYSA-H zinc;tin(4+);hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Zn+2].[Sn+4] BHTBHKFULNTCHQ-UHFFFAOYSA-H 0.000 claims description 18
- 230000002401 inhibitory effect Effects 0.000 claims description 17
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 15
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- 238000001027 hydrothermal synthesis Methods 0.000 claims description 13
- 239000000178 monomer Substances 0.000 claims description 13
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 239000003999 initiator Substances 0.000 claims description 12
- 238000001556 precipitation Methods 0.000 claims description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000008096 xylene Substances 0.000 claims description 8
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 239000004642 Polyimide Substances 0.000 claims description 5
- 239000012752 auxiliary agent Substances 0.000 claims description 5
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 5
- 229920001721 polyimide Polymers 0.000 claims description 5
- 239000012763 reinforcing filler Substances 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 4
- 229920000297 Rayon Polymers 0.000 claims description 4
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 4
- 239000002134 carbon nanofiber Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 4
- 230000005494 condensation Effects 0.000 claims description 4
- 238000005520 cutting process Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 4
- 239000002270 dispersing agent Substances 0.000 claims description 4
- 239000006185 dispersion Substances 0.000 claims description 4
- 238000007731 hot pressing Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 238000010992 reflux Methods 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 238000005470 impregnation Methods 0.000 claims description 3
- 239000011301 petroleum pitch Substances 0.000 claims description 3
- 238000001338 self-assembly Methods 0.000 claims description 3
- 230000001629 suppression Effects 0.000 abstract description 9
- 238000009755 vacuum infusion Methods 0.000 abstract description 6
- 238000007598 dipping method Methods 0.000 abstract description 3
- 239000004743 Polypropylene Substances 0.000 description 36
- 229920001155 polypropylene Polymers 0.000 description 36
- 239000004793 Polystyrene Substances 0.000 description 16
- 239000002861 polymer material Substances 0.000 description 15
- 239000004800 polyvinyl chloride Substances 0.000 description 15
- 229920002223 polystyrene Polymers 0.000 description 14
- 229920000915 polyvinyl chloride Polymers 0.000 description 13
- 239000000463 material Substances 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 5
- 238000002485 combustion reaction Methods 0.000 description 5
- 229910052760 oxygen Inorganic materials 0.000 description 5
- 239000001301 oxygen Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000012796 inorganic flame retardant Substances 0.000 description 4
- 230000003993 interaction Effects 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 229910052599 brucite Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003517 fume Substances 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 2
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 2
- 239000000347 magnesium hydroxide Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- -1 polypropylene Polymers 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 229920002994 synthetic fiber Polymers 0.000 description 2
- 230000037303 wrinkles Effects 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000010426 asphalt Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000002952 polymeric resin Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- DXZMANYCMVCPIM-UHFFFAOYSA-L zinc;diethylphosphinate Chemical compound [Zn+2].CCP([O-])(=O)CC.CCP([O-])(=O)CC DXZMANYCMVCPIM-UHFFFAOYSA-L 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Reinforced Plastic Materials (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a flame-retardant smoke-suppressing polymer composite material and a preparation method thereof, wherein the method comprises the following steps: s1: the raw materials are prepared according to the following mass percentages: 10-15% of three-dimensional carbon felt, 5-10% of zinc stannate and 75-85% of matrix resin; s2: loading zinc stannate on the three-dimensional carbon felt to prepare a three-dimensional zinc stannate-loaded carbon felt preform; s3: and (3) pouring or in-situ polymerizing matrix resin into the three-dimensional zinc stannate-loaded carbon felt preform in vacuum to prepare the flame-retardant smoke-suppressing polymer composite material with the three-dimensional zinc stannate-loaded carbon felt. The invention applies the structural characteristic that fibers in a three-dimensional carbon felt preform are mutually overlapped to form the carbon felt, introduces zinc stannate by dipping, coating, evaporating and self-assembling, constructs a three-dimensional flame-retardant and smoke-suppression network framework, and prepares the composite material by in-situ vacuum infusion or in-situ polymerization of matrix resin. The composite material prepared by the invention has excellent flame retardance, smoke suppression and mechanical properties, and can be widely applied to the field of flame retardance.
Description
Technical Field
The invention belongs to the technical field of high polymer flame retardant materials, and particularly relates to a flame retardant and smoke suppression high polymer composite material and a preparation method thereof.
Background
The polymer material is a long-chain molecule composed of repeating units, and is considered as a novel material for promoting social development together with steel, wood and cement. The polymer material has the characteristics of easy processability, flexibility, fatigue resistance, light weight, low production cost, high dielectric constant, high mechanical strength and the like, is widely applied to the industries of aerospace, electronic industry, biomedicine, automobiles and the like, but most of the polymer materials have inflammability and have fire hazard. The flame retardant can endow the synthetic material with self-extinguishing property, flame retardance and smoke abatement property, thereby becoming one of important auxiliary agents for the development and application of polymer synthetic materials
The halogen-containing flame retardant has high flame retardant efficiency, and can play a role in inhibiting ignition and slowing down flame spread. However, halogen-containing flame retardants tend to emit toxic gases and fumes during combustion, releasing acidic fumes. Therefore, there is a need to develop halogen-free flame retardants to replace current halogen-containing flame retardants. Zinc Hydroxystannate (ZHS) and Zinc Stannate (ZS) are novel inorganic flame-retardant and smoke-suppressant agents, have the advantages of environmental protection, no toxicity and the like, are widely applied to the field of high polymer materials, and are considered to be one of novel, stable, efficient and green flame retardants. However, the inorganic flame retardants such as Zinc Hydroxystannate (ZHS) and Zinc Stannate (ZS) have poor dispersibility (difficult uniform dispersion) in the polymer composite material, so that the flame retardant performance is greatly limited and complete release is difficult to achieve. Meanwhile, the interface compatibility between Zinc Hydroxystannate (ZHS) and Zinc Stannate (ZS) and the organic polymer material is poor, so that the problems of difficult dispersion and uneven dispersion exist in the polymer material, and the two problems can influence the performance of the polymer material, such as the mechanical property, tensile strength and toughness of the polymer material are obviously reduced.
In addition, the existing flame-retardant smoke-inhibiting polymer composite material also has the defects of complex preparation process, large addition amount of the flame-retardant smoke inhibitor, low flame-retardant smoke-inhibiting efficiency, obviously poor mechanical properties and decorative effect of the material and the like.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the flame-retardant smoke-inhibiting polymer composite material and the preparation method thereof, the addition amount of the flame-retardant smoke inhibitor can be greatly reduced, the preparation process is simplified by introducing the three-dimensional carbon felt and synchronously improving the preparation method, the adopted components and the proportion, and the prepared composite material can continuously maintain the excellent mechanical property and the decorative effect of the polymer material on the basis of having excellent flame-retardant and smoke-inhibiting properties.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the preparation method of the flame-retardant smoke-inhibiting polymer composite material is characterized by comprising the following steps of:
s1: the raw materials are prepared according to the following mass percentages: 10-15% of three-dimensional carbon felt, 5-10% of zinc stannate and 75-85% of matrix resin;
s2: loading zinc stannate on the three-dimensional carbon felt by a coprecipitation method, a hydrothermal synthesis method or a homogeneous precipitation method to prepare a three-dimensional zinc stannate-loaded carbon felt preform, wherein the three-dimensional zinc stannate-loaded carbon felt preform accounts for 15-25% of the total weight of the final composite material;
s3: vacuum infusion or in-situ polymerization of matrix resin is carried out on the three-dimensional carbon felt loaded with zinc stannate to prepare the flame-retardant smoke-suppressing polymer composite material loaded with zinc stannate by the three-dimensional carbon felt;
s4: and further cutting or hot-pressing the prepared flame-retardant smoke-inhibiting polymer composite material to finally prepare the flame-retardant smoke-inhibiting polymer composite material.
The S2 specifically includes the following steps:
s21: ultrasonically soaking the three-dimensional carbon felt in a mixed solution of ethanol and acetone for 40min, taking out and drying to obtain a three-dimensional carbon felt A with a clean surface and active groups;
s22: and adding the three-dimensional carbon felt A into a solution system of zinc stannate prepared in advance, preparing a three-dimensional zinc stannate loaded carbon felt preform by adopting a coprecipitation method, a hydrothermal synthesis method or a homogeneous precipitation method, taking out and drying for later use.
The matrix resin is one of PP, PVC, PS resin or monomers thereof.
The matrix resin is one of polypropylene (PP), polyvinyl chloride (PVC) and Polystyrene (PS).
The S3, the matrix resin is PP resin, which comprises the following steps:
s31: adding xylene with the volume three times that of PP resin into a beaker, gradually adding the PP resin, heating and stirring, controlling the heating temperature to be 120-140 ℃, and adding a three-dimensional zinc stannate loaded carbon felt into the dissolved PP resin after the PP resin is dissolved; and then drying the xylene solvent to obtain the three-dimensional zinc stannate loaded carbon felt PP system composite material, namely the flame-retardant smoke-suppressing polymer composite material.
The S3, the matrix resin is PVC, which comprises the following steps:
s32: adding a proper amount of deionized water, a proper amount of dispersing agent, initiator and other auxiliary agents, PVC monomers and the three-dimensional loaded zinc stannate carbon felt into a polymerization reaction kettle, controlling the reaction temperature to be 60 ℃, adding a terminator when the reaction pressure is reduced to a specified pressure, discharging, cleaning and drying to obtain the three-dimensional loaded zinc stannate carbon felt PVC system composite material, namely the flame-retardant smoke-suppression high polymer composite material.
The S3, the matrix resin being PS, specifically includes the following steps:
s33: mixing a three-dimensional zinc stannate-loaded carbon felt with a styrene PS monomer, magnetically stirring for a period of time at room temperature, adding a certain amount of dibenzoyl peroxide as an initiator into the mixed solution, pouring the mixture into a three-neck flask after the initiator is stirred and dissolved, stirring at 90 ℃, and carrying out condensation reflux to initiate polymerization; when the polymerization is viscous, taking down the condenser pipe and stirring slowly for a period of time to discharge non-polymerized styrene monomer; and then taking off the three-mouth bottle, quickly pouring out the primary polymerization product, putting the primary polymerization product into a container, putting the container into a drying oven at 90 ℃, and continuously polymerizing until the reaction is complete to obtain the three-dimensional zinc stannate loaded carbon felt PS composite material, namely the flame-retardant smoke-suppressing polymer composite material. .
The three-dimensional carbon felt is one or more of polyacrylonitrile carbon fiber, petroleum pitch-based carbon fiber, viscose-based carbon fiber, vapor-grown carbon fiber, polyimide-based carbon fiber and various carbonized fibers, the surfaces of which are provided with carboxyl or hydroxyl active groups; the fibers are mutually overlapped in a three-dimensional space to form a carbon felt, and the diameter of the fibers is 5-20 mu m.
The zinc stannate is one of zinc stannate or zinc hydroxystannate or a compound of the two, and is prepared by adopting a coprecipitation method, a hydrothermal synthesis method or a homogeneous precipitation method.
The flame-retardant smoke-suppressing polymer composite material prepared by the method is characterized in that a three-dimensional carbon felt is used as a dispersing template, impregnation coating evaporation self-assembly is utilized, zinc stannate is uniformly dispersed and loaded in a three-dimensional structure of the three-dimensional carbon felt, a three-dimensional carbon felt prefabricated body with a flame-retardant smoke-suppressing network framework which is mutually overlapped to form the carbon felt is constructed, then a resin matrix is poured into the three-dimensional network framework in a vacuum mode in situ, and a composite material system with the three-dimensional carbon felt prefabricated body as a framework and matrix resin as reinforcing filler is obtained.
Compared with the prior art, the invention has the following advantages and beneficial effects:
1. according to the flame-retardant smoke-suppressing polymer composite material and the preparation method provided by the invention, the three-dimensional carbon felt is introduced, the preparation method, the adopted components and the proportion are synchronously improved, the addition amount of the flame-retardant smoke-suppressing agent can be greatly reduced, the preparation process is simplified, and the prepared composite material continuously keeps the excellent mechanical property and the decorative effect of the polymer material on the basis of excellent flame-retardant and smoke-suppressing properties.
2. According to the flame-retardant smoke-suppressing polymer composite material and the preparation method thereof provided by the invention, the introduced three-dimensional carbon felt has a good three-dimensional network, and can contain a large number of groups on the fiber, provide enough active sites, and form good interface combination with an inorganic flame retardant, so that the three-dimensional structure of the three-dimensional carbon felt can be used as a template to impregnate polymer resin, the inorganic flame retardant can be well dispersed in the composite material, and the flame-retardant performance of the composite material can be fully exerted; the three-dimensional carbon felt has a good flame-retardant effect as an inorganic carbon material, and the composite material with the three-dimensional structure has excellent mechanical properties, flame retardance and smoke suppression, and is a polymer flame-retardant composite material with great prospect and a preparation method thereof.
3. The compatibility of the matrix resin and the zinc stannate interface is improved through the mutual synergistic effect of the three-dimensional carbon felt and the zinc stannate; the preparation method provided by the invention can skillfully and uniformly disperse the zinc stannate/zinc hydroxystannate in the three-dimensional carbon felt structure, and further enhance the original performance of the zinc stannate/zinc hydroxystannate in the matrix resin, so that the mechanical property, the flame retardant property and the smoke suppression property of the composite material system are remarkably and synchronously improved.
4. The flame-retardant smoke-inhibiting polymer composite material prepared by the invention has excellent flame-retardant and smoke-inhibiting properties, and simultaneously better maintains the excellent mechanical and solvent resistance properties of the polymer material. Meanwhile, the preparation method provided by the invention has the advantages of short time, easily controlled process, low manufacturing cost, capability of producing composite material systems based on different resins and easiness in industrialization.
Drawings
FIG. 1: SEM structural diagram of raw materials and intermediate materials adopted in embodiment 1 of the invention;
FIG. 2 is a schematic diagram: SEM structural drawings of the raw material and the intermediate material used in example 3 of the present invention.
Detailed Description
The present invention will be further described with reference to the accompanying drawings and examples, which are provided for the purpose of further illustrating the principles and operation of the present invention.
The preparation method of the flame-retardant smoke-suppressing polymer composite material provided by the invention comprises the following steps:
s1: the raw materials are prepared according to the following mass percentages: 10-15% of three-dimensional carbon felt, 5-10% of zinc stannate and 75-85% of matrix resin;
s2: loading zinc stannate on the three-dimensional carbon felt by a coprecipitation method, a hydrothermal synthesis method or a homogeneous precipitation method to prepare a three-dimensional zinc stannate-loaded carbon felt preform, wherein the three-dimensional zinc stannate-loaded carbon felt preform accounts for 15-25% of the total weight of the final composite material; the method specifically comprises the following steps:
s21: ultrasonically soaking the three-dimensional carbon felt in a solution of ethanol and acetone for 40min, taking out and drying to obtain a three-dimensional carbon felt A with a clean surface and active groups;
s22: adding the three-dimensional carbon felt A into a solution system of zinc stannate prepared in advance, preparing a three-dimensional zinc stannate loaded carbon felt preform by adopting a coprecipitation method, a hydrothermal synthesis method or a homogeneous precipitation method, taking out and drying for later use;
s3: vacuum infusion or in-situ polymerization of matrix resin is carried out on the three-dimensional carbon felt loaded with zinc stannate to prepare the flame-retardant smoke-suppressing polymer composite material loaded with zinc stannate by the three-dimensional carbon felt;
the matrix resin is one of polypropylene (PP), polyvinyl chloride (PVC), Polystyrene (PS) resin or monomers thereof; the PP/PVC/PS can also be a modified resin matrix which is properly filled with aluminum hydroxide and magnesium hydroxide (brucite powder) and has good flame retardant property.
When the matrix resin is PP, PVC, PS, respectively, the steps S31, S32, S33 are selected to be performed: one of them is:
when the matrix resin is a PP resin, the S3 specifically includes the following steps:
s31: adding xylene with the volume three times that of PP resin into a beaker, gradually adding the PP resin, heating and stirring, controlling the heating temperature to be 120-140 ℃, and adding a three-dimensional zinc stannate loaded carbon felt into the dissolved PP resin after the PP resin is dissolved; and then drying the xylene solvent to obtain the three-dimensional zinc stannate loaded carbon felt PP system composite material, namely the flame-retardant smoke-suppressing polymer composite material.
When the matrix resin is PVC, the S3 specifically includes the following steps:
s32: adding a proper amount of deionized water, a proper amount of dispersing agent, initiator and other auxiliary agents, PVC monomers and the three-dimensional loaded zinc stannate carbon felt into a polymerization reaction kettle, controlling the reaction temperature to be 60 ℃, adding a terminator when the reaction pressure is reduced to a specified pressure, discharging, cleaning and drying to obtain the three-dimensional loaded zinc stannate carbon felt PVC system composite material, namely the flame-retardant smoke-suppression high polymer composite material.
When the matrix resin is PS, the step S3 specifically includes the following steps:
s33: mixing a three-dimensional zinc stannate-loaded carbon felt with a styrene PS monomer, magnetically stirring for a period of time at room temperature, adding a certain amount of dibenzoyl peroxide as an initiator into the mixed solution, pouring the mixture into a three-neck flask after the initiator is stirred and dissolved, stirring at 90 ℃, and carrying out condensation reflux to initiate polymerization; when the polymerization is viscous, taking down the condenser pipe and stirring slowly for a period of time to discharge non-polymerized styrene monomer; then taking off the three-mouth bottle, quickly pouring out the primary polymerization product, putting the primary polymerization product into a container, putting the container into a drying oven at 90 ℃, and continuously polymerizing until the reaction is complete to obtain a three-dimensional zinc stannate-loaded carbon felt PS composite material, namely a flame-retardant smoke-suppressing high-molecular composite material;
s4: and further cutting or hot-pressing the prepared flame-retardant smoke-inhibiting polymer composite material to finally prepare the flame-retardant smoke-inhibiting polymer composite material.
The three-dimensional carbon felt is one or more of polyacrylonitrile carbon fiber, petroleum pitch-based carbon fiber, viscose-based carbon fiber, vapor-grown carbon fiber, polyimide-based carbon fiber and various carbonized fibers, the surfaces of which are provided with carboxyl or hydroxyl active groups; the fibers are mutually overlapped in a three-dimensional space to form a carbon felt, and the diameter of the fibers is 5-20 mu m.
The zinc stannate is one of zinc stannate or zinc hydroxystannate or a compound of the two, and is prepared by adopting a coprecipitation method, a hydrothermal synthesis method or a homogeneous precipitation method.
The flame-retardant smoke-suppressing polymer composite material prepared by the method is a composite material system which takes a three-dimensional carbon felt as a dispersing template, is self-assembled by dipping, coating, evaporating and self-assembling, so that zinc stannate is uniformly dispersed and loaded in a three-dimensional structure of the three-dimensional carbon felt to construct a three-dimensional carbon felt preform with a flame-retardant smoke-suppressing network framework which is mutually overlapped to form the carbon felt, and then matrix resin is poured into the three-dimensional network framework in a vacuum mode or polymerized in situ to obtain the matrix resin which takes the three-dimensional carbon felt preform as a framework and takes the matrix resin as reinforcing filler.
Example 1
Referring to the attached drawing 1, the flame-retardant smoke-suppressing polymer composite material provided by the embodiment is prepared from a three-dimensional carbon felt, zinc stannate and PP, and the preparation method specifically comprises the following steps:
s1: preparing raw materials:
respectively preparing three-dimensional carbon felt, zinc stannate and matrix resin PP, wherein the three components are sequentially in percentage by weight: 10%, 5% and 85%; the three-dimensional zinc stannate loaded carbon felt is 15%, the zinc stannate loaded amount is 5%, and the PP resin or monomer is 85%;
the three-dimensional carbon felt in the embodiment is polyimide-based carbon fiber, all fibers are mutually overlapped in a three-dimensional space to form the carbon felt, and the diameter of the fibers is 10-20 mu m.
The PP in the embodiment is a modified resin matrix which is modified by filling a proper amount of aluminum hydroxide and magnesium hydroxide (brucite powder) and has good flame retardant property, and is beneficial to the finally prepared polymer composite material to achieve the triple effects of structure enhancement, flame retardance and smoke abatement;
s2: loading zinc stannate on the three-dimensional carbon felt by a coprecipitation method, a hydrothermal synthesis method or a homogeneous precipitation method to prepare a three-dimensional zinc stannate-loaded carbon felt preform, wherein the three-dimensional zinc stannate-loaded carbon felt preform accounts for 15% of the total weight of the final composite material; the method specifically comprises the following steps:
s21: ultrasonically soaking the three-dimensional carbon felt in a mixed solution of ethanol and acetone for 40min, taking out and drying to obtain a three-dimensional carbon felt A with a clean surface and active groups;
s22: adding the three-dimensional carbon felt A into a solution system of zinc stannate prepared in advance, preparing a three-dimensional zinc stannate loaded carbon felt preform by adopting a coprecipitation method, a hydrothermal synthesis method or a homogeneous precipitation method, taking out and drying for later use;
s3: vacuum-infusing matrix resin PP into the three-dimensional zinc stannate-loaded carbon felt preform to prepare the flame-retardant smoke-suppressing polymer composite material with the three-dimensional carbon felt loaded with zinc stannate; when in-situ vacuum infusion is adopted, the interfacial interaction between the three-dimensional carbon felt and the resin is generated in the in-situ vacuum infusion process, so that the wettability of the three-dimensional carbon felt is improved, the compatibility of the three-dimensional structure and the interface of the high polymer material is enhanced, and the prepared composite material has excellent mechanical and flame retardant properties and smoke suppression properties.
The method comprises the following specific steps: adding xylene with the volume three times that of PP resin into a beaker, gradually adding the PP resin, heating and stirring, controlling the heating temperature to be 120-140 ℃, and adding the three-dimensional zinc stannate loaded carbon felt into the dissolved PP resin after the PP resin is dissolved (a large amount of bubbles are generated); and then drying the xylene solvent to obtain the three-dimensional zinc stannate-loaded carbon felt PP system composite material, namely the flame-retardant smoke-suppressing polymer composite material.
S4: and further cutting or hot-pressing the flame-retardant smoke-inhibiting polymer composite material to finally prepare the three-dimensional zinc stannate-loaded carbon felt PP composite material, namely a finished product of the flame-retardant smoke-inhibiting polymer composite material.
The flame-retardant smoke-suppressing polymer composite material prepared by the method is characterized in that a three-dimensional carbon felt is used as a dispersing template, impregnation coating evaporation self-assembly is utilized, zinc stannate is uniformly dispersed and loaded in a three-dimensional structure of the three-dimensional carbon felt, a three-dimensional carbon felt prefabricated body with a flame-retardant smoke-suppressing network framework and a carbon felt formed by mutual lap joint is constructed, matrix resin PP is poured into the three-dimensional network framework in situ in a vacuum mode, and a composite material system with the three-dimensional carbon felt prefabricated body as a framework and the matrix resin PP as a reinforcing filler is obtained.
Reference is made to fig. 1, which is an SEM representation of the skeleton and matrix of the raw and intermediate materials used in this example to illustrate the microstructure of the final composite material. The SEM image on the left shows the matrix resin, and it can be seen that regular wrinkles appear on the surface, which are caused by liquid nitrogen embrittlement; the middle part is an SEM image of the three-dimensional carbon felt, and polyimide-based carbon fibers in the three-dimensional carbon felt are staggered to form a three-dimensional network structure with smooth surface; the right picture is a three-dimensional carbon felt loaded with zinc stannate by adopting a coprecipitation method, and the zinc stannate is loaded on the surface of the fiber and forms a flame-retardant smoke-suppression three-dimensional network together with the three-dimensional carbon felt. As can be seen from the right figure, the three-dimensional zinc stannate-loaded carbon felt PP composite material prepared in this embodiment is a composite material system in which a three-dimensional carbon felt preform is used as a framework, matrix resin PP is used as a reinforcing filler, and zinc stannate is uniformly distributed in each position of a three-dimensional framework.
The flame-retardant smoke-suppressing polymer PP composite material sample prepared in the embodiment is subjected to mechanical property test, limited oxygen index test, UL-94 vertical combustion test and smoke density test, and the combustion and mechanical test results of the composite material are shown in Table 1.
Example 2
The flame-retardant smoke-suppressing polymer composite material and the preparation method thereof provided by the embodiment are basically the same as those of the embodiment 1, and the differences are as follows:
the composite material is prepared from a three-dimensional carbon felt, zinc hydroxystannate and a PP monomer, wherein the three components are sequentially in percentage by mass: 15%, 10% and 75%.
The samples are subjected to mechanical property test, limited oxygen index test, UL-94 vertical combustion test, smoke density test and SEM characterization, and the results are shown in the table.
According to the embodiment of the invention, the interfacial interaction between the three-dimensional carbon felt and the resin is generated in the in-situ polymerization process, so that the wettability of the three-dimensional carbon felt is improved, the compatibility of the three-dimensional structure and the interface of the high polymer material is enhanced, and the prepared composite material has excellent mechanical and flame retardant properties and smoke suppression properties.
Example 3
The flame-retardant smoke-suppressing polymer composite material and the preparation method thereof provided by the embodiment of the invention are basically the same as the embodiments 1 and 2, and the difference is that:
the composite material is prepared from three-dimensional carbon felt, zinc stannate and PS, wherein the three components are sequentially in percentage by mass: 12.5%, 8.5% and 79%.
The three-dimensional carbon felt is polyacrylonitrile carbon fiber with carboxyl or hydroxyl active groups on the surface, all fibers are mutually overlapped in a three-dimensional space to form the carbon felt, and the fiber diameter is 15-20 mu m.
Step S2, preparing a three-dimensional zinc stannate-loaded carbon felt preform by adopting a coprecipitation method;
in the step S3, the preparation process of the three-dimensional zinc stannate-loaded carbon felt PS composite material is to prepare the three-dimensional zinc stannate-loaded carbon felt PS system composite material by in-situ polymerization of PS. The method specifically comprises the following steps:
mixing a three-dimensional zinc stannate-loaded carbon felt with a styrene monomer, magnetically stirring for a period of time at room temperature, adding a certain amount of dibenzoyl peroxide as an initiator into the mixed solution, pouring the mixture into a three-neck flask after the initiator is stirred and dissolved, stirring at 90 ℃, and carrying out condensation reflux to initiate polymerization; when the polymerization became viscous, the condenser tube was removed and stirred slowly for a while to discharge the non-polymerized styrene monomer. And then taking off the three-neck bottle, quickly pouring out the primary polymerization product, putting the primary polymerization product into a container, putting the container into a drying oven at 90 ℃, and continuously polymerizing until the reaction is complete, thereby finally obtaining the three-dimensional zinc stannate-loaded carbon felt PS composite material.
In the embodiment, the interfacial interaction between the three-dimensional carbon felt and the resin is generated in the in-situ polymerization process, so that the wettability of the three-dimensional carbon felt is improved, the compatibility of the three-dimensional structure and the interface of the high polymer material is enhanced, and the prepared composite material has excellent mechanical and flame-retardant performances and smoke suppression performances.
Referring to fig. 2: the SEM image on the left shows the matrix resin, and it can be seen that regular wrinkles appear on the surface, which are caused by liquid nitrogen embrittlement; the middle part is an SEM image of the three-dimensional carbon felt, so that polyacrylonitrile carbon fibers in the three-dimensional carbon felt are staggered to form a three-dimensional network structure, and the surface is smooth; the right picture is a three-dimensional carbon felt loaded with zinc hydroxystannate by adopting a hydrothermal synthesis method, and the zinc hydroxystannate is loaded on the surface of the fiber and forms a flame-retardant smoke-suppression three-dimensional network together with the three-dimensional carbon felt.
The samples of the composite material of this example were subjected to mechanical property test, limiting oxygen index test, UL-94 vertical burning test, and smoke density test, and the results are shown in Table 1.
Example 4
The flame-retardant smoke-suppressing polymer composite material and the preparation method thereof provided by the embodiment of the invention are basically the same as the embodiment 1, and the difference is that:
the composite material is prepared from three-dimensional carbon felt, zinc hydroxystannate and PVC, and the mass percentages of the three are as follows in sequence: 12.5%, 7.5% and 80%.
The three-dimensional carbon felt is petroleum asphalt-based carbon fiber with carboxyl or hydroxyl active groups on the surface, all the fibers are mutually overlapped in a three-dimensional space to form the carbon felt, and the diameter of the fibers is 5-10 mu m.
The zinc hydroxystannate is prepared by a hydrothermal synthesis method;
in the step S3, the preparation process of the three-dimensional loaded zinc hydroxystannate carbon felt PVC composite material comprises the following steps: adding a proper amount of deionized water, a proper amount of dispersing agent, initiator and other auxiliary agents, vinyl chloride monomer and three-dimensional loaded zinc stannate carbon felt into a polymerization reaction kettle, controlling the reaction temperature to be 60 ℃, adding a terminator when the reaction pressure is reduced to a specified pressure, and discharging; and cleaning and drying to obtain the composite material.
In the step S3, the PVC composite material of the three-dimensional loaded zinc hydroxystannate carbon felt is prepared by in-situ polymerization of PVC, and the interfacial interaction between the three-dimensional carbon felt and the matrix resin is generated in the in-situ polymerization process, so that the wettability of the three-dimensional carbon felt is improved, the compatibility of the three-dimensional structure and the matrix resin polymer material interface is enhanced, and the prepared composite material has excellent mechanical and flame retardant properties and smoke suppression properties.
The composite material sample prepared in this example was subjected to mechanical property test, limiting oxygen index test, UL-94 vertical burning test, and smoke density test, and the results are shown in table 1.
Table 1: the composite combustion and mechanical test results obtained for the material samples of each example were:
as can be seen from table 1, the flame-retardant smoke-suppressing polymer composite material containing a three-dimensional network skeleton structure prepared in the embodiments of the present invention can significantly improve the flame-retardant property, smoke-suppressing property and mechanical property of the composite material. The flame retardant property of the composite material prepared by each embodiment can reach V-0, the limiting oxygen index is more than 36%, and the mechanical property (tensile strength) is obviously improved, so that the composite material has balanced and excellent material properties.
The invention is characterized in that a three-dimensional carbon felt is introduced, the structural characteristics of the carbon felt are formed by mutually lapping fibers in a three-dimensional carbon felt preform, the components, the proportion and the preparation process are synchronously improved, zinc stannate is introduced by dipping, coating, evaporating and self-assembling to construct a three-dimensional flame-retardant and smoke-suppressing network framework, and the composite material is prepared by in-situ vacuum infusion or in-situ polymerization of matrix resin. The composite material prepared by the invention has excellent flame retardance, smoke suppression and mechanical properties, and can be widely applied to the field of flame retardance.
It should be noted that, with reference to the specific formula, the value range of the chemical formula parameters, and the specific conditions of the preparation process in the above embodiments, other embodiments may also specifically select different components, ratios, and process conditions within the ranges described in the present invention, for example: the three-dimensional carbon felt can also be one or more than one of viscose-based carbon fiber, vapor grown carbon fiber and various carbon fibers with carboxyl or hydroxyl active groups on the surface, and the technical effects of the invention can be realized.
While the embodiments of the present invention have been described in detail, it should be understood that the present invention is not limited to the embodiments, but is applicable to various other embodiments.
Claims (10)
1. The preparation method of the flame-retardant smoke-inhibiting polymer composite material is characterized by comprising the following steps of:
s1: the raw materials are prepared according to the following mass percentages: 10-15% of three-dimensional carbon felt, 5-10% of zinc stannate and 75-85% of matrix resin;
s2: loading zinc stannate on the three-dimensional carbon felt by a coprecipitation method, a hydrothermal synthesis method or a homogeneous precipitation method to prepare a three-dimensional zinc stannate-loaded carbon felt preform, wherein the three-dimensional zinc stannate-loaded carbon felt preform accounts for 15-25% of the total weight of the final composite material;
s3: and (3) pouring or in-situ polymerizing matrix resin into the three-dimensional zinc stannate-loaded carbon felt preform in vacuum to prepare the flame-retardant smoke-suppressing polymer composite material with the three-dimensional zinc stannate-loaded carbon felt.
2. The preparation method of the flame-retardant smoke-suppressing polymer composite material as claimed in claim 1, characterized by further comprising the following steps:
s4: and further cutting or hot-pressing the prepared flame-retardant smoke-inhibiting polymer composite material to finally prepare the flame-retardant smoke-inhibiting polymer composite material.
3. The method for preparing the flame-retardant smoke-suppressing polymer composite material according to claim 1, wherein the S2 specifically comprises the following steps:
s21: ultrasonically soaking the three-dimensional carbon felt in a solution of ethanol and acetone for 40min, taking out and drying to obtain a three-dimensional carbon felt A with a clean surface and active groups;
s22: and adding the three-dimensional carbon felt A into a solution system of zinc stannate prepared in advance, preparing a three-dimensional zinc stannate loaded carbon felt preform by adopting a coprecipitation method, a hydrothermal synthesis method or a homogeneous precipitation method, taking out and drying for later use.
4. The method for preparing the flame-retardant smoke-suppressing polymer composite material as claimed in claim 1, wherein the matrix resin is one of PP, PVC, PS resin or monomers thereof.
5. The method for preparing the flame-retardant smoke-suppressing polymer composite material according to claim 4,
the S3, the matrix resin is PP resin, which comprises the following steps:
s31: adding xylene with the volume three times that of PP resin into a beaker, gradually adding the PP resin, heating and stirring, controlling the heating temperature to be 120-140 ℃, and adding a three-dimensional zinc stannate loaded carbon felt into the dissolved PP resin after the PP resin is dissolved; and then drying the xylene solvent to obtain the three-dimensional zinc stannate-loaded carbon felt PP system composite material, namely the flame-retardant smoke-suppressing polymer composite material.
6. The method for preparing the flame-retardant smoke-suppressing polymer composite material according to claim 4,
the S3, the matrix resin is PVC, which comprises the following steps:
s32: adding a proper amount of deionized water, a proper amount of dispersing agent, initiator and other auxiliary agents, PVC monomers and the three-dimensional loaded zinc stannate carbon felt into a polymerization reaction kettle, controlling the reaction temperature to be 60 ℃, adding a terminator when the reaction pressure is reduced to a specified pressure, discharging, cleaning and drying to obtain the three-dimensional loaded zinc stannate carbon felt PVC system composite material, namely the flame-retardant smoke-suppression high polymer composite material.
7. The method for preparing the flame-retardant smoke-suppressing polymer composite material according to claim 4,
the S3, the matrix resin being PS, specifically includes the following steps:
s33: mixing a three-dimensional zinc stannate-loaded carbon felt with a styrene PS monomer, magnetically stirring for a period of time at room temperature, adding a certain amount of dibenzoyl peroxide as an initiator into the mixed solution, pouring the mixture into a three-neck flask after the initiator is stirred and dissolved, stirring at 90 ℃, and carrying out condensation reflux to initiate polymerization; when the polymerization is viscous, taking down the condenser pipe and stirring for a period of time at a low speed to discharge non-polymerized styrene monomers; and then taking off the three-mouth bottle, quickly pouring out the primary polymerization product, putting the primary polymerization product into a container, putting the container into a drying oven at 90 ℃, and continuously polymerizing until the reaction is complete to obtain the three-dimensional zinc stannate-loaded carbon felt PS composite material, namely the flame-retardant smoke-suppressing polymer composite material.
8. The method for preparing the flame-retardant smoke-suppressing polymer composite material according to claim 1,
the three-dimensional carbon felt is one or two or more of polyacrylonitrile carbon fiber, petroleum pitch-based carbon fiber, viscose-based carbon fiber, vapor-grown carbon fiber and polyimide-based carbon fiber with carboxyl or hydroxyl active groups on the surface; the fibers are mutually overlapped in a three-dimensional space to form a carbon felt, and the diameter of the fibers is 5-20 mu m.
9. The method for preparing the flame-retardant smoke-suppressing polymer composite material according to claim 1,
the zinc stannate is one of zinc stannate or zinc hydroxystannate or a compound of the two, and is prepared by adopting a coprecipitation method, a hydrothermal synthesis method or a homogeneous precipitation method.
10. The flame-retardant smoke-suppressing polymer composite material prepared by the method of any one of claims 1 to 9 is characterized in that a three-dimensional carbon felt is used as a dispersion template, impregnation, coating, evaporation and self-assembly are utilized, zinc stannate is uniformly dispersed and loaded in a three-dimensional structure of the three-dimensional carbon felt, a three-dimensional carbon felt preform with a flame-retardant smoke-suppressing network framework which is overlapped with each other to form the carbon felt is constructed, and then matrix resin is poured into the three-dimensional network framework in situ in a vacuum manner or polymerized in situ, so that a composite material system with the three-dimensional carbon felt preform as a framework and the matrix resin as a reinforcing filler is obtained.
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