CN106752598A - A kind of anti-scratch expansible graphite water super-thin steel structure fire-proof paint and preparation method thereof - Google Patents
A kind of anti-scratch expansible graphite water super-thin steel structure fire-proof paint and preparation method thereof Download PDFInfo
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- 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
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- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
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Abstract
The invention discloses a kind of anti-scratch expansible graphite water super-thin steel structure fire-proof paint, it is made from the following raw materials in parts by weight：APP 20 22, pentaerythrite 78, melamine 78, expansible graphite 45, chlorinated paraffin 3 3.5,0.1Mol/L zinc nitrate aqueous solutions 23 25, the 0.1Mol/L hexamethylene tetramines aqueous solution 23 25, tetraethyl orthosilicate 0.8 1, lithium metasilicate 1.6 1.8, appropriate amount of water, methyl methacrylate 42 43, Graphene 3 3.5, molybdenum disulfide nano sheet 1.2 1.5, gelatin 34, barium fluoride 0.6 0.8.The present invention is modified using gelatin to Graphene, molybdenum disulfide nano sheet, barium fluoride, so that Graphene, molybdenum disulfide nano sheet, barium fluoride are dispersed in coating, compactness, water proofing property, the anti-corrosive properties of coating are improve, especially Scratch Resistance can be greatly improved.
Description
Technical field
The present invention relates to fireproof coating technical field, more particularly to a kind of anti-scratch expansible graphite aqueous ultra-thin shaped steel knot
Structure fireproof coating and preparation method thereof.
Background technology
Solvent-borne type super-thin steel structure fireproof coating contains substantial amounts of volatile organic matter（VOC）, it is applied and is increasingly subject to
Limitation, or even disabled by developed country.Water super-thin steel structure fire-proof paint is reduced using waterborne polymeric as film forming matter
The discharge capacity of VOC, reduce coating production, construction, using etc. the harm to human body and the pollution to environment, symbol in link
Energy-saving and emission-reduction, the development trend of environmental protection are closed, is the emphasis of fireproof coating research.This paper is directed to water super-thin steel structure
The fire protecting performance of fireproof coating is poor, expansion multiplying power is low, low expanding layer structural strength, poor water resistance the problems such as deeply ground
Study carefully, and to film forming matter（The tertiary polymer of vinegar）Thermal decomposition process and charcoal forming machine reason, APP to the thermal decomposition of vinegar tertiary polymer
The influence of process is discussed；Nano zirconium dioxide and aqueous phosphorous polymer are have studied exploratoryly in fireproof coating
Using.Main research work is as follows：（1）Film forming is have studied from the angle of thermal decomposition characteristic, Dynamic Rheological Properties and compound viscosity
Influence of the material to fireproof coating expansible fireproof performance.Result of study shows：Pure third and the storage modulu of cinepazid polymer melt
（G ＇）More than loss modulus（G ＂）, based on elasticity flowing, it is combined viscosity high（>1000Pa·s）；The G ＂ of the tertiary polymer melt of vinegar
More than G ＇, based on VISCOUS FLOW, viscosity is combined low（33Pa·s）.With heat endurance is good, char forming ability strong, compound viscosity
Low, viscous fluid characteristics polymer are suitable as the film forming matter of fireproof coating, are conducive to expansion and the fire protecting performance of coating
Raising.（2）With the tertiary polymer of vinegar（VAc-VeoVa）As film forming matter, APP/pentaerythrite/melamine/can be swollen
Swollen graphite（APP/PER/MEL/EG）As Intumescent Retardant System（IFR）, have studied IFR and its with VAc-VeoVa with comparing
The influence of Properties of Fire-Proofing Coatings.Orthogonal experiment analysis result directly perceived shows that influence of each component to Properties of Fire-Proofing Coatings is suitable in IFR
Sequence is followed successively by：APP ＞ EG ＞ PER ＞ MEL, optimum proportioning is APP:PER:MEL:EG=22:8:8:4.5.When VAc-VeoVa is used
Measure be 30%, IFR consumptions be 40% when, the fire protecting performance of fire resistant coating is optimal（Steel plate back of the body temperature is 262 DEG C after burning 30min）.（3）
Have studied influence of the factors such as composition, granular size and the form of inorganic filler to fireproof coating.TG, capillary rheology test,
The results of study such as fire protecting performance test show：With TiO2/SAp/HNTs（8/1/1）During as inorganic filler, fireproof coating it is anti-
Fiery excellent performance（3327s）, expansion multiplying power is higher（28.14）, expansion Rotating fields are good, intensity is high.Inorganic filler is by being constrained to
The lax and rotation of membrane polymer strand, and reduction APP influences to prevent on the catalytic dehydration efficiency of PER and VAc-VeoVa
The expansion multiplying power and fire protecting performance of fiery coating.Simultaneously when viscosity is higher, inorganic filler is difficult to move to expanding layer surface aggregation
Inorganic thermal insulation layer is formed, causes the fire protecting performance of fireproof coating to decline.By formulation optimization, the performance of aqueous fire-proof coating is made by oneself
Famous foreign brand is exceeded.（4）Have studied nano zirconium dioxide（nano-ZrO2）Effect in fireproof coating.Research knot
Fruit shows：Silane coupler γ-methacryloxypropyl trimethoxy silane（Z-6030）Modified nano-ZrO2
There is good dispersiveness in VAc-VeoVa emulsions.In the halogen-free flameproof coating without EG, nano-ZrO is added2After expand
Layer no longer has continuous fine and close structure, and structural strength reduction, and fire protecting performance is with nano-ZrO2Under consumption ground increases on the contrary
Drop.There is halogen fireproof coating containing EG, EG is interspersed in expanding layer, play a part of structural support；ZrO2In expanding layer
In play a part of heat-insulated and prevent thermal oxide from decomposing, the fire prevention time reaches 3837s.XRD results show to be generated in expanding layer
Titanium pyrophosphate（TiP2O7）, zirconium pyrophosphate（ZrP2O7）With zirconium pyrophosphate magnesium-titanium solid solution（Ti0.8Zr0.2P2O7）.（5）Have studied
Influence of the thermal decomposition process and APP of Vac-VeoVa to VAc-VeoVa thermal decomposition processes.Result of study shows：In air atmosphere
The thermal oxide decomposable process of middle VAc-VeoVa is divided into three phases：（1）Removing acetic acid and tertiary carbon acid groups, generate unsaturated carbon
Chain；（2）The oxidative dehydrogenation of unsaturated carbon chains, cyclisation, aromatisation, generate hexagonal crystal system carbon；（3）The thermal oxide of hexagonal crystal system carbon.
VAc-VeoVa thermal decomposition processes are divided into two stages in nitrogen atmosphere：（1）Removing acetic acid and tertiary carbon acid groups, generate insatiable hunger
And carbochain；（2）The chain rupture or cyclisation of unsaturated carbon chains, aromatisation, generate hexagonal crystal system carbon.Density functional theory（DFT）Meter
Calculate result and show versatic acid and the relation that the removing of acetic acid group is competition fracture in VAc-VeoVa molecules.TG and FTIR results
Show, APP reduces the heat decomposition temperature of VAc-VeoVa, accelerate the removing speed of VAc-VeoVa side-chain radicals.Additionally,
The polyphosphoric acid that APP is thermally decomposed to generate removes the pendant hydroxyl group reaction generation P-O-C generated after ketenes with VAc-VeoVa molecules
Key.The product generated after ethylenic unsaturation hydrocarbon aromatizing is connected to become cross-linked network shape structure by P-O-C keys, has charcoal residue
More preferable heat endurance.（6）Aqueous phosphorous cinepazid polymer P is synthesized（MMA/St/BA/MAA/PAM100）, and in this, as
Film forming matter, have studied its application in fireproof coating.Result of study shows, vinyl alkoxy phosphate（PAM100）Carry
The heat endurance of polymer high, belongs to the condensed phase mechanism of action.Fire protecting performance test result shows, using StA-P1.5 as into
The fire protecting performance of fireproof coating prepared by membrane substance is optimal.Flymn-Wall-Ozawa（FWO）Method and Kissinger-
Akahira-Sunose（KAS）Method result of calculation shows that PAM100 considerably increases the thermal degradation activation energy of polymer, but
Activation energy increasing with PAM100 consumptions and reducing.The mechanism function of polymer thermal decomposition is respectively g（α）=-ln（1-α）, f（α）
=1- α, order of reaction n=1, rhermal decomposition rate expression formula are ddtAexpE/RT1.
《The preparation of water super-thin steel structure fire-proof paint and fireproofing function study mechanism》The fireproof coating that one text is obtained
Containing substantial amounts of phosphate group, water absorption rate is big, easily causes coating and metal erosion, expansible graphite and organic macromolecule phase
Capacitive is poor, and the insufficient strength of coating is, it is necessary to improve, in addition it is also necessary to improve the Scratch Resistance of coating.
The content of the invention
The object of the invention is exactly to make up the defect of prior art, there is provided a kind of anti-scratch expansible graphite aqueous ultra-thin
Formed steel construction fireproof coating and preparation method thereof.
The present invention is achieved by the following technical solutions：
A kind of anti-scratch expansible graphite water super-thin steel structure fire-proof paint, is made from the following raw materials in parts by weight：Poly- phosphorus
Sour ammonium 20-22, pentaerythrite 7-8, melamine 7-8, expansible graphite 4-5, chlorinated paraffin 3-3.5,0.1Mol/L zinc nitrate
Aqueous solution 23-25,0.1Mol/L hexamethylene tetramine aqueous solution 23-25, tetraethyl orthosilicate 0.8-1, lithium metasilicate 1.6-1.8,
Appropriate amount of water, methyl methacrylate 42-43, styrene 42-43, butyl acrylate 58-60, methacrylic acid 4-5, vinyl alkane
Base epoxide phosphate 1.5-1.8, nonyl phenyl polyethoxy ether 0.3-0.4, neopelex 1.1-1.5, bicarbonate
Sodium 1.3-1.5, potassium peroxydisulfate 1.2-1.5, appropriate ammoniacal liquor, Graphene 3-3.5, molybdenum disulfide nano sheet 1.2-1.5, gelatin 3-4,
Barium fluoride 0.6-0.8.
The preparation method of the anti-scratch expansible graphite water super-thin steel structure fire-proof paint, comprises the following steps：
（1）Expansible graphite, absolute ethyl alcohol and 12-14 weight portions water are mixed, 45-48 DEG C is heated with stirring in a water bath, plus
It is 8-9 to enter ammoniacal liquor regulation pH, continues to stir 10-15min, then is slowly added dropwise tetraethyl orthosilicate, in 45-48 DEG C of perseverance after completion of dropping
Warm stirring reaction 4-4.5h, is cooled to room temperature, washed, suction filtration, drying, obtain modified expansible graphite；
（2）0.1Mol/L zinc nitrate aqueous solutions, the 0.1Mol/L hexamethylene tetramines aqueous solution are mixed, ultrasonic disperse 6-
8min, reacts two hours in 94-97 DEG C of water-bath, obtains slurry；
（3）Methyl methacrylate, styrene, butyl acrylate, methacrylic acid are well mixed, mix monomer is obtained, will
Neopelex, sodium acid carbonate are added in the water of 50-52 weight portions, are stirred, and 80-83 is heated in a water bath
DEG C, 1/3 potassium peroxydisulfate is added under 240-260rmin stirrings, stir 20-23 minutes, then the mixing list for being added dropwise 1/3
Body, is incubated 20-23 minutes, then remaining mix monomer, potassium peroxydisulfate are mixed with the water and the slurry of stating of 50-52 weight portions
Uniformly, it is added dropwise in reactant, then vinyl alkyl epoxide phosphate, nonyl phenyl polyethoxy ether is well mixed, is added dropwise
Enter in reactant, dropwise operation was completed in 3-3.2 hours, be cooled to less than 50 DEG C, filtering obtains glue；
（4）By Graphene, molybdenum disulfide nano sheet, gelatin, barium fluoride mixed grinding 20-25 minutes, mixed material is obtained；
（5）The water of 7-8 weight portions is mixed with modified expansible graphite, mixed material, melamine, is uniformly dispersed, added
The glue of 30-32 weight portions and other residual components, are uniformly dispersed, and obtain final product.
It is an advantage of the invention that：The present invention reacts generation dandelion shape and aoxidizes using zinc nitrate and hexamethylene tetramine
Zinc, polymerisation is carried out with monomer, improves heat resistance, inoxidizability and the antifouling water resistance of glue, improves the strong of coating
Degree, fire line, prevent cracking, it is aging, extend service life；Expansible graphite is changed by using tetraethyl orthosilicate
Property so that expansible graphite improves with the interface interaction of glue, is dispersed in coating, improves intensity and the densification of coating
Property, the hole even compact of expanding layer after being heated, fire protecting performance is improved；By using gelatin to Graphene, molybdenum disulfide nano
Piece, barium fluoride are modified so that Graphene, molybdenum disulfide nano sheet, barium fluoride are dispersed in coating, improve coating
Compactness, water proofing property, anti-corrosive properties, especially Scratch Resistance can greatly improve.
Specific embodiment
A kind of anti-scratch expansible graphite water super-thin steel structure fire-proof paint, by following weight portion（Kilogram）Raw material
It is made：APP 20, pentaerythrite 7, melamine 7, expansible graphite 4, chlorinated paraffin 3,0.1Mol/L zinc nitrates are water-soluble
Liquid 23, the 0.1Mol/L hexamethylene tetramines aqueous solution 23, tetraethyl orthosilicate 0.8, lithium metasilicate 1.6, appropriate amount of water, methacrylic acid
Methyl esters 42, styrene 42, butyl acrylate 58, methacrylic acid 4, vinyl alkyl epoxide phosphate 1.5, the poly- second of nonyl phenyl
Oxygen ether 0.3, neopelex 1.1, sodium acid carbonate 1.3, potassium peroxydisulfate 1.2, appropriate ammoniacal liquor, Graphene 3, curing
Molybdenum nanometer sheet 1.2, gelatin 3, barium fluoride 0.6.
The preparation method of the anti-scratch expansible graphite water super-thin steel structure fire-proof paint, comprises the following steps：
（1）Expansible graphite, absolute ethyl alcohol and 12 weight portion water are mixed, 45 DEG C are heated with stirring in a water bath, add ammoniacal liquor
Regulation pH is 8, continues to stir 10min, then is slowly added dropwise tetraethyl orthosilicate, in 45 DEG C of constant temperature stirring reaction 4h after completion of dropping,
Be cooled to room temperature, washed, suction filtration, drying, obtain modified expansible graphite；
（2）0.1Mol/L zinc nitrate aqueous solutions, the 0.1Mol/L hexamethylene tetramines aqueous solution are mixed, ultrasonic disperse 6min,
Two hours are reacted in 94 DEG C of water-baths, slurry is obtained；
（3）Methyl methacrylate, styrene, butyl acrylate, methacrylic acid are well mixed, mix monomer is obtained, will
Neopelex, sodium acid carbonate are added in the water of 50 weight portions, are stirred, and 80 DEG C are heated in a water bath,
The potassium peroxydisulfate of the lower addition 1/3 of 240rmin stirrings, stirs 20 minutes, then 1/3 mix monomer is added dropwise, and is incubated 20 minutes,
Remaining mix monomer, potassium peroxydisulfate are well mixed with the water and the slurry of stating of 50 weight portions again, are added dropwise in reactant,
Vinyl alkyl epoxide phosphate, nonyl phenyl polyethoxy ether are well mixed again, are added dropwise in reactant, dropwise operation exists
Completed in 3 hours, be cooled to less than 50 DEG C, filtering obtains glue；
（4）By Graphene, molybdenum disulfide nano sheet, gelatin, barium fluoride mixed grinding 20 minutes, mixed material is obtained；
（5）The water of 7 weight portions is mixed with modified expansible graphite, mixed material, melamine, is uniformly dispersed, add 30
The glue of weight portion and other residual components, are uniformly dispersed, and obtain final product.
Experimental data：
The fireproof coating of embodiment is placed into 24h, is brushed on clean steel plate, brushed once every 8 hours, coating thickness is
1mm, dries 20d under aeration-drying environment, and film water absorption rate is 9.5%, and the decomposition temperature in nitrogen atmosphere is 469 DEG C, aobvious
Micro- Microscopic observation contains 4-5 microns of uniform cell through the coating of high-temperature expansion.
Claims (2)
1. a kind of anti-scratch expansible graphite water super-thin steel structure fire-proof paint, it is characterised in that：By following weight portion
Raw material is made：APP 20-22, pentaerythrite 7-8, melamine 7-8, expansible graphite 4-5, chlorinated paraffin 3-3.5,
0.1Mol/L zinc nitrate aqueous solution 23-25,0.1Mol/L hexamethylene tetramine aqueous solution 23-25, tetraethyl orthosilicate 0.8-1,
Lithium metasilicate 1.6-1.8, appropriate amount of water, methyl methacrylate 42-43, styrene 42-43, butyl acrylate 58-60, metering system
Sour 4-5, vinyl alkyl epoxide phosphate 1.5-1.8, nonyl phenyl polyethoxy ether 0.3-0.4, neopelex
1.1-1.5, sodium acid carbonate 1.3-1.5, potassium peroxydisulfate 1.2-1.5, appropriate ammoniacal liquor, Graphene 3-3.5, molybdenum disulfide nano sheet
1.2-1.5, gelatin 3-4, barium fluoride 0.6-0.8.
2. the preparation method of anti-scratch expansible graphite water super-thin steel structure fire-proof paint according to claim 1, its
It is characterised by comprising the following steps：
（1）Expansible graphite, absolute ethyl alcohol and 12-14 weight portions water are mixed, 45-48 DEG C is heated with stirring in a water bath, plus
It is 8-9 to enter ammoniacal liquor regulation pH, continues to stir 10-15min, then is slowly added dropwise tetraethyl orthosilicate, in 45-48 DEG C of perseverance after completion of dropping
Warm stirring reaction 4-4.5h, is cooled to room temperature, washed, suction filtration, drying, obtain modified expansible graphite；
（2）0.1Mol/L zinc nitrate aqueous solutions, the 0.1Mol/L hexamethylene tetramines aqueous solution are mixed, ultrasonic disperse 6-
8min, reacts two hours in 94-97 DEG C of water-bath, obtains slurry；
（3）Methyl methacrylate, styrene, butyl acrylate, methacrylic acid are well mixed, mix monomer is obtained, will
Neopelex, sodium acid carbonate are added in the water of 50-52 weight portions, are stirred, and 80-83 is heated in a water bath
DEG C, 1/3 potassium peroxydisulfate is added under 240-260rmin stirrings, stir 20-23 minutes, then the mixing list for being added dropwise 1/3
Body, is incubated 20-23 minutes, then remaining mix monomer, potassium peroxydisulfate are mixed with the water and the slurry of stating of 50-52 weight portions
Uniformly, it is added dropwise in reactant, then vinyl alkyl epoxide phosphate, nonyl phenyl polyethoxy ether is well mixed, is added dropwise
Enter in reactant, dropwise operation was completed in 3-3.2 hours, be cooled to less than 50 DEG C, filtering obtains glue；
（4）By Graphene, molybdenum disulfide nano sheet, gelatin, barium fluoride mixed grinding 20-25 minutes, mixed material is obtained；
（5）The water of 7-8 weight portions is mixed with modified expansible graphite, mixed material, melamine, is uniformly dispersed, added
The glue of 30-32 weight portions and other residual components, are uniformly dispersed, and obtain final product.
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| CN201611143555.7A CN106752598A (en) | 2016-12-13 | 2016-12-13 | A kind of anti-scratch expansible graphite water super-thin steel structure fire-proof paint and preparation method thereof |
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| CN201611143555.7A Pending CN106752598A (en) | 2016-12-13 | 2016-12-13 | A kind of anti-scratch expansible graphite water super-thin steel structure fire-proof paint and preparation method thereof |
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| CN108641551A (en) * | 2018-05-28 | 2018-10-12 | 广东金刚玻璃科技股份有限公司 | A kind of fire resistant coating and preparation method thereof |
| CN112473065A (en) * | 2020-12-07 | 2021-03-12 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of fluorinated graphene oxide fire extinguishing agent and product thereof |
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