CN103937155A - Double-resistant high-strength solid buoyancy material - Google Patents
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- CN103937155A CN103937155A CN201410051148.8A CN201410051148A CN103937155A CN 103937155 A CN103937155 A CN 103937155A CN 201410051148 A CN201410051148 A CN 201410051148A CN 103937155 A CN103937155 A CN 103937155A
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Abstract
The invention discloses a double-resistant high-strength solid buoyancy material. The double-resistant high-strength solid buoyancy material is characterized in comprising following ingredients, by mass, 100 parts of epoxy resin, 1 to 15 parts of graphite powder, 5 to 20 parts of an epoxy diluent, 2 to 20 parts of a flexibilizer, 10 to 80 parts of hollow microbead, 0.5 to 10 parts of spherical nanometer silver powder, 50 to 80 parts of a curing agent, and 0.1 to 3 parts of a catalyst. The hollow microbead is modified hollow microbead obtained via surface modification with silane coupling agent KH560; the spherical nanometer silver powder is modified spherical nanometer silver powder or modified nanometer silver powder with a shape similar to that of a sphere, and is obtained via surface modification with a function compound containing sulfydryl and imidazolyl, and particle size of the spherical nanometer silver powder ranges from 5 to 100nm; the graphite powder is composed of natural flake graphite and synthesized graphite powder which are obtained via surface modification with cetyltrimethyl ammonium bromide (CTAB), and particle size of the graphite powder ranges from 5 to 324 meshes. A preparation method of the double-resistant high-strength solid buoyancy material is simple; the double-resistant high-strength solid buoyancy material is low in cost, high in strength, and long in service life, and possesses antibacterial properties and antistatic properties.
Description
Technical field
The present invention relates to a kind of antibacterial, antistatic and high-intensity solid buoyancy material, belong to functional nonmetallic composite technical field, specifically a kind of dual anti-high strength solid buoyancy material.
Background technology
Along with the propelling of development and the deep-sea exploration of Ocean Development Technology, deep-sea solid buoyancy material became domestic study hotspot in recent years.The application of solid buoyancy material has realized hardware and has been difficult to the function realizing, the application that the aspect such as bathyscaph, underwater robot, subbottom tunnel, submarine optical fiber cable, petroleum transportation pipeline has all obtained under water, and can be under water use safely under the deep-sea of thousands of meters.Solid buoyancy material mainly forms by polymkeric substance or resene matrix and hollow glass micropearl or hollow ceramic microspheres composite.Wherein, mainly taking epoxy group(ing) solid buoyancy material as representative, patent CN1018242206A is by the ultra-high-strength buoyancy material obtaining after hollow glass micropearl and epoxy resin composite curing, applicable to 6000～9000 meters of deepwater environments; Patent CN103013050A is compound by hollow glass micropearl and epoxy resin equally, and is spliced to form the solid buoyancy material of epoxy group(ing) by module.
But in the time that solid buoyancy material is used to deep ocean work, subbottom tunnel, submarine optical fiber cable, petroleum transportation pipeline, outer field solid buoyancy material is not only subject to the impact of deep-sea pressure, and the surface attachment of microorganism in the seawater can not be ignored, simultaneously in deep ocean work process, the function influence of static is very important, especially in deep-sea oil pipeline uses, the processing of outer solid buoyancy material anti-electrostatic seems more important.Solid buoyancy material has launched a lot of work in enhancing resistance to compression etc. at present, selects glass microballon surface treatment, linking agent use etc. but mainly concentrate on solidifying agent.Therefore be necessary very much solid buoyancy material to carry out processing and improvement antibacterial, antistatic aspect.Have good anti-microbial property based on nanometer silver itself, therefore we have introduced the nano-silver powder of modification in solid buoyancy material; Graphite itself has excellent conductivity, usually used as composite material conductive filler, make matrix material there is good conductivity, Graphite Powder 99 is incorporated in solid buoyancy material, make solid buoyancy material possess certain conductivity, thereby possess antistatic property.Based on this, we are incorporated into nano-silver powder and Graphite Powder 99 modification in the solid composite material of epoxy group(ing), can prepare high strength antibacterial antistatic solid buoyancy material, there is not yet report and the application of antibacterial antistatic epoxy group(ing) solid buoyancy material.
Summary of the invention
The object of the invention is to: a kind of dual anti-high strength solid buoyancy material is provided, merge the conductivity of nano-silver powder good antimicrobial property and graphite excellence, prepare spherical nano-silver powder by adopting liquid phase reduction, and utilize to contain modifying surface to spherical nano-silver powder of sulfydryl and imidazoles functional compounds and be applied in epoxy base material and prepare solid buoyancy material, reach and make prepared solid buoyancy material possess antistatic, antibacterial and high-intensity object.
To achieve these goals, the present invention adopts following technical scheme:
A kind of dual anti-high strength solid buoyancy material, it is characterized in that: in mass parts, the recipe ingredient of this material comprises following raw material: 100 parts of epoxy resin, 1～15 part of Graphite Powder 99,5～20 parts of epoxide diluents, 2～20 parts of toughner, 10～80 parts of cenospheres, 0.5～10 part of spherical nano-silver powder, 50～80 parts, solidifying agent, 0.1～3 part of catalyzer.
Described epoxy resin is the one in dihydroxyphenyl propane based epoxy resin, novolac epoxy, aliphatic epoxy resin or hydridization type epoxy resin.
Described toughner is the common toughner of epoxy, can be one or more in rubber-like toughner, thermoplastic elastomer class toughner, Versamid and low molecular nonactive toughner.
Described solidifying agent is the matching used solidifying agent of epoxy, comprises one or more in alkaline amine curing agent, acid acid anhydride type curing agent, fatty amines, low molecular polyamides class add-on type solidifying agent or imidazole curing agent.
Described catalyzer is one or more in methyl tetrahydro phthalic anhydride, methyl hexahydrophthalic anhydride, diethylenetriamine, triethylene tetramine etc.
Described cenosphere is that ultimate compression strength is 30～125MPa, and real density is 0.125～0.6g/cm
3, particle diameter is 10～120 μ m, inner chamber is filled with gas or hollow glass micropearl and hollow ceramic microspheres for vacuum, it is characterized in that: described cenosphere is to adopt silane coupling agent KH560 to carry out the modification cenosphere after surface treatment.
Further, the concrete implementation step of the surface modification treatment of described cenosphere is: by 30～50% aqueous sodium hydroxide solution or 30% superoxol processing for cenosphere, make cenosphere surface hydroxylation; Then after washing after filtration,, being dried, join in ethanolic soln, add again the silane coupling agent KH560 that is equivalent to cenosphere quality 1～5%, by silane hydrolysis reaction, silane coupling agent KH560 is grafted on cenosphere surface, then after filtration, washing, the dry silane coupling agent KH560 surface-treated cenosphere that obtains.
The object that adopts silane coupling agent KH560 to carry out surface modification treatment to cenosphere is: treated cenosphere can well be scattered in epoxy base material, and then for the filler of solid buoyancy material, can obviously improve the bonding force between cenosphere and epoxy resin.
Described spherical nano-silver powder is spherical or class spherical nano-silver powder, it is characterized in that: this spherical nano-silver powder adopts liquid phase reduction to prepare, its particle diameter is 5～l00nm, concrete preparation method is: taking Silver Nitrate as raw material, after adding reductive agent, stablizer and dispersion agent, adopt liquid phase reduction to react preparation, reaction finishes rear solid-liquid separation, and purifying washing obtains spherical nano-silver powder after being dried.Wherein, described reductive agent is hydrazine hydrate (N
2h
4h
2o), sodium borohydride (NaBH
4), sodium hypophosphite (NaPO
2h
2) or L-AA (C
6h
8o
6) in one or more; Described stablizer and dispersion agent are sodium lauryl sulphate (SDS), Sodium dodecylbenzene sulfonate (SDBS), polyvinylpyrrolidone (one or more in PVP, polyvinyl alcohol (PVA) or polyoxyethylene glycol (PEG).
Further, described spherical nano-silver powder is to contain sulfydryl and imidazoles functional compounds carries out surface-treated modified spherical nano-silver powder by employing, and described functional compound is 2-mercaptoimidazole (C
3h
4n
2s), 2-sulfydryl-1-Methylimidazole (C
4h
6n
2or 2-mercaptobenzimidazole (C S)
7h
6n
2etc. S) one in.
The object that utilization contains sulfydryl and the modifying surface processing of imidazoles functional compounds to spherical nano-silver powder is: utilize complexing action very strong between spherical nano-silver powder and sulfydryl, by the functional nano-silver powder surface that is grafted to of this compounds, strengthen on the one hand the dispersiveness of nano-silver powder in epoxy base material, in addition on the one hand because the existence of imidazoles group has improved spherical nano-silver powder and epoxy base material bonding force greatly.
Described Graphite Powder 99 is natural flake graphite and synthetic graphite powder, order number is 5～324 orders, it is characterized in that: described Graphite Powder 99 adopts hexadecyl brometo de amonio (CTAB) to carry out surface modification treatment, concrete modifying process is: take 5～10g Graphite Powder 99, join 20～50mL deionized water for stirring, with salt acid for adjusting pH value 7～8, ultrasonic 1～10 minute, add the cetyl trimethylammonium bromide of 1～5g, after ultrasonic 10～30 minutes, decompress filter, obtain filter cake with distilled water wash and be that 60～70 DEG C of vacuum-dryings obtain surface-treated Graphite Powder 99 for 24～48 hours.
The preparation method of described dual anti-high strength solid buoyancy material is: by the epoxy resin of described mass fraction, Graphite Powder 99, epoxide diluent, toughner and cenosphere join in vacuum mixer, in the vacuum mixer of 60～80 DEG C, stir 20～30 minutes, then add spherical nano-silver powder, solidifying agent and catalyzer continue to stir 20 minutes, gained mixture is injected to mould, adopt vulcanizing press hot-press solidifying moulding under the pressure of 20MPa, program curing is followed successively by 110 DEG C 2 hours, at 140 DEG C 4 hours, at 160 DEG C 4 hours, the cooling rear demoulding, obtain thering is high strength, antibacterial, anlistatig solid buoyancy material.
Compared with prior art, beneficial effect of the present invention is:
In conjunction with the anti-microbial property of spherical nano-silver powder and the conductivity of Graphite Powder 99, contain sulfydryl and imidazoles functional compounds processes to adopt CTAB to the processing of Graphite Powder 99 modifying surface to spherical nano-silver powder modifying surface by employing, then add in epoxy matrix as filler, make the epoxy group(ing) buoyancy material of preparation possess excellent antibacterial, antistatic effect, required step is few, cost is low, and technique is simpler, easily realizes large-scale commercial production; In addition, first silver powder and Graphite Powder 99 are carried out adding in epoxy matrix after modification, can strengthen dispersed and raising spherical nano-silver powder and the epoxy base material bonding force of nano-silver powder in epoxy base material, make solid buoyancy material not only there is very high intensity, and reduce use in the effect of biological adsorption and generation of static electricity, thereby the work-ing life and the security that improve solid buoyancy material.
Embodiment
Below in conjunction with specific examples, technical scheme of the present invention is described further.
Embodiment 1
A kind of dual anti-high strength solid buoyancy material, it is characterized in that: in mass parts, the recipe ingredient of this material comprises following raw material: 100 parts of epoxy resin, 5 parts of Graphite Powder 99s, 15 parts of epoxide diluents, 10 parts of toughner, 50 parts of cenospheres, 2 parts of spherical nano-silver powders, 60 parts, solidifying agent, 0.5 part of catalyzer.
Described epoxy resin is bisphenol A type epoxy resin E51.
Described epoxide diluent is ethylene glycol diglycidylether type.
Described toughner is acrylonitrile-butadiene-styrene copolymer (ABS).
Described solidifying agent is 1-cyanoethyl-2-ethyl-4-methylimidazole.
Described catalyzer is methyl hexahydrophthalic anhydride.
Described cenosphere is that ultimate compression strength is 30～125MPa, and real density is 0.125～0.6g/cm
3, particle diameter is 10～120 μ m, the hollow glass micropearl K37 that inner chamber is vacuum.
Described cenosphere is to adopt silane coupling agent KH560 to carry out the modification cenosphere after surface treatment, the concrete implementation step of its surface modification treatment is: under the aqueous sodium hydroxide solution room temperature that is 50% by 20g cenosphere 500mL weight fraction, stir 2 hours, make cenosphere surface hydroxylation; Wash 5～10 times with a large amount of deionized waters, then by the hollow glass micropearl obtaining vacuum-drying 6 hours at 80 DEG C, join in a large amount of ethanolic solns, add again the silane coupling agent KH560 of 10g, as a child took out at 60 DEG C of stirring reactions 5, with after a large amount of deionized water wash, the dry silane coupling agent KH560 surface-treated hollow glass micropearl K37 that obtains for 6 hours in 60 DEG C of vacuum drying ovens.
Described spherical nano-silver powder is that particle diameter is the spherical of 30nm or class spherical nano-silver powder, by adopting liquid phase reduction to prepare, concrete preparation method is: it is for subsequent use that the deionized water that the PVP-K30 that takes 20g is dissolved in 200mL obtains the aqueous solution of PVP, takes in addition the silver nitrate solution that obtains 100mg/mL in the deionized water that solid nitric acid silver 50g is dissolved in 500mL; Measure after the PVP aqueous solution of 100mL and 100mL silver nitrate solution be mixed evenly, under magnetic agitation, under room temperature, drip 80% hydrazine hydrate solution 10mL, then the mixing solutions obtaining is contained in to sealing in sample bottle and preserves, after ultrasonic 10～20 minutes, be placed in 80 DEG C of baking ovens, react 6 hours, centrifugation, will precipitate and use a large amount of deionized water wash, and in 60 DEG C of vacuum drying ovens, dry 12 as a child obtained spherical nano-silver powder.
Further, described spherical nano-silver powder is to contain sulfydryl and imidazoles functional compounds carries out surface-treated modified spherical nano-silver powder by employing, concrete method of modifying is: the spherical nano-silver powder that takes 5g, joining 100mL deionized water for ultrasonic disperses 30 minutes, obtain the aqueous dispersions of spherical nano-silver powder, add the 2-mercaptoimidazole of 5g until all dissolve, at 80 DEG C, react 2 hours, centrifugation will precipitate uses a large amount of deionized water wash, dry 12 spherical nano-silver powders that as a child obtained 2-mercaptoimidazole functionalization in 60 DEG C of vacuum drying ovens.
Described Graphite Powder 99 is natural flake graphite and synthetic graphite powder, order number is 5～324 orders, adopt hexadecyl brometo de amonio (CTAB) to carry out surface modification treatment, concrete modifying process is: the Graphite Powder 99 that takes 5g joins in 250mL deionized water water, add the acetum of 5mL1%, after ultrasonic 10～20 minutes, add 20g hexadecyl brometo de amonio (CTAB) to continue after ultrasonic 10～20 minutes, filter and use a large amount of deionized water wash to be dried the Graphite Powder 99 that obtains ctab surface processing for 12 hours by the filter obtaining and in 60 DEG C of vacuum drying ovens.
The preparation method of described dual anti-high strength solid buoyancy material is: by the epoxy resin of described mass fraction, Graphite Powder 99, epoxide diluent, toughner and cenosphere join in vacuum mixer, in the vacuum mixer of 60～80 DEG C, stir 20～30 minutes, then add spherical nano-silver powder, solidifying agent and catalyzer continue to stir 20 minutes, gained mixture is injected to mould, adopt vulcanizing press hot-press solidifying moulding under the pressure of 20MPa, program curing is followed successively by 110 DEG C 2 hours, at 140 DEG C 4 hours, at 160 DEG C 4 hours, the cooling rear demoulding, obtain thering is high strength, antibacterial, anlistatig solid buoyancy material.
Embodiment 2
A kind of dual anti-high strength solid buoyancy material, it is characterized in that: in mass parts, the recipe ingredient of this material comprises following raw material: 100 parts of epoxy resin, 2 parts of Graphite Powder 99s, 10 parts of epoxide diluents, 8 parts of toughner, 60 parts of cenospheres, 2 parts of spherical nano-silver powders, 60 parts, solidifying agent, 0.2 part of catalyzer.
Described epoxy resin is bisphenol A type epoxy resin E44.
Described epoxide diluent is polypropylene glycol diglycidyl ether.
Described toughner is liquid polybutadiene rubber.
Described solidifying agent is MALEIC ANHYDRIDE.
Described catalyzer is mphenylenediamine.
Described cenosphere is that ultimate compression strength is 30～125MPa, and real density is 0.125～0.6g/cm
3, particle diameter is 10～120 μ m, the hollow glass micropearl K46 that inner chamber is vacuum.
Described cenosphere is to adopt silane coupling agent KH560 to carry out the modification cenosphere after surface treatment, the concrete implementation step of its surface modification treatment is: under the aqueous sodium hydroxide solution room temperature that is 50% by 20g cenosphere 200mL weight fraction, stir 2 hours, make cenosphere surface hydroxylation; Wash 5～10 times with a large amount of deionized waters, then by the hollow glass micropearl obtaining vacuum-drying 6 hours at 80 DEG C, join in a large amount of ethanolic solns, add again the silane coupling agent KH560 of 10g, as a child took out at 60 DEG C of stirring reactions 5, with after a large amount of deionized water wash, the dry silane coupling agent KH560 surface-treated hollow glass micropearl K46 that obtains for 6 hours in 60 DEG C of vacuum drying ovens.
Described spherical nano-silver powder is that particle diameter is the spherical of 30nm or class spherical nano-silver powder, by adopting liquid phase reduction to prepare, concrete preparation method is: it is for subsequent use that the deionized water that the PVP-K30 that takes 20g is dissolved in 200mL obtains the aqueous solution of PVP, takes in addition the silver nitrate solution that obtains 100mg/mL in the deionized water that solid nitric acid silver 50g is dissolved in 500mL; Measure after the PVP aqueous solution of 100mL and 100mL silver nitrate solution be mixed evenly, under magnetic agitation, under room temperature, add sodium borohydride solids 0.5g to dissolving completely, then the mixing solutions obtaining is contained in to sealing in sample bottle and preserves, after ultrasonic 10～20 minutes, be placed in 80 DEG C of baking ovens, react 6 hours, centrifugation, will precipitate and use a large amount of deionized water wash, and in 60 DEG C of vacuum drying ovens, dry 12 as a child obtained spherical nano-silver powder.
Further, described spherical nano-silver powder is to contain sulfydryl and imidazoles functional compounds carries out surface-treated modified spherical nano-silver powder by employing, concrete method of modifying is: the spherical nano-silver powder that takes 5g, join in 100mL acetone soln ultrasonic dispersion 30 minutes, obtain the acetone dispersion liquor of spherical nano-silver powder, add the 2-mercaptoimidazole of 5g until all dissolve, at 80 DEG C, react 2 hours, centrifugation will precipitate uses a large amount of washing with acetones, dry 12 spherical nano-silver powders that as a child obtained 2-mercaptoimidazole functionalization in 60 DEG C of vacuum drying ovens.
Described Graphite Powder 99 is natural flake graphite and synthetic graphite powder, order number is 5～324 orders, adopt hexadecyl brometo de amonio (CTAB) to carry out surface modification treatment, concrete modifying process is: the Graphite Powder 99 that takes 5g joins in 250mL deionized water water, add the acetum of 5mL1%, after ultrasonic 10～20 minutes, add 20g hexadecyl brometo de amonio (CTAB) to continue after ultrasonic 10～20 minutes, filter and use a large amount of deionized water wash to be dried the Graphite Powder 99 that obtains ctab surface processing for 12 hours by the filter obtaining and in 60 DEG C of vacuum drying ovens.
The preparation method of described dual anti-high strength solid buoyancy material is: by the epoxy resin of described mass fraction, Graphite Powder 99, epoxide diluent, toughner and cenosphere join in vacuum mixer, in the vacuum mixer of 60～80 DEG C, stir 20～30 minutes, then add spherical nano-silver powder, solidifying agent and catalyzer continue to stir 20 minutes, gained mixture is injected to mould, adopt vulcanizing press hot-press solidifying moulding under the pressure of 20MPa, program curing is followed successively by 110 DEG C 2 hours, at 140 DEG C 4 hours, at 160 DEG C 4 hours, the cooling rear demoulding, obtain thering is high strength, antibacterial, anlistatig solid buoyancy material.
Claims (9)
1. a dual anti-high strength solid buoyancy material, it is characterized in that: in mass parts, the recipe ingredient of this material comprises following raw material: 100 parts of epoxy resin, 1～15 part of Graphite Powder 99,5～20 parts of epoxide diluents, 2～20 parts of toughner, 10～80 parts of cenospheres, 0.5～10 part of spherical nano-silver powder, 50～80 parts, solidifying agent, 0.1～3 part of catalyzer.
2. the dual anti-high strength solid buoyancy material of one as claimed in claim 1, is characterized in that: described cenosphere is that ultimate compression strength is 30～125MPa, and real density is 0.125～0.6g/cm
3, particle diameter is 10～120 μ m, inner chamber is filled with gas or hollow glass micropearl and hollow ceramic microspheres for vacuum.
3. the dual anti-high strength solid buoyancy material of one as claimed in claim 1, is characterized in that: described spherical nano-silver powder is to adopt the spherical or class spherical nano-silver powder that the particle diameter for preparing of liquid phase reduction is 5～l00nm.
4. the dual anti-high strength solid buoyancy material of one as claimed in claim 1, is characterized in that: described Graphite Powder 99 is that particle diameter is 5～324 object natural flake graphites and synthetic graphite powder.
5. a kind of dual anti-high strength solid buoyancy material as claimed in claim 2 cenosphere used, is characterized in that: described cenosphere is to adopt silane coupling agent KH560 to carry out the modification cenosphere after surface treatment.
6. the method for modifying of a kind of dual anti-high strength solid buoyancy material as claimed in claim 5 cenosphere used, it is characterized in that: the concrete implementation step of the method is: by cenosphere 30～50% aqueous sodium hydroxide solution or 30% superoxol processing, make cenosphere surface hydroxylation; Then after washing after filtration,, being dried, join in ethanolic soln, add again the silane coupling agent KH560 that is equivalent to cenosphere quality 1～5%, by silane hydrolysis reaction, silane coupling agent KH560 is grafted on cenosphere surface, then after filtration, washing, the dry silane coupling agent KH560 surface-treated cenosphere that obtains.
7. a kind of dual anti-high strength solid buoyancy material as claimed in claim 3 spherical nano-silver powder used, it is characterized in that: described spherical nano-silver powder is to contain sulfydryl and imidazoles functional compounds carries out surface-treated modified spherical nano-silver powder by employing, wherein, described functional compound is 2-mercaptoimidazole (C
3h
4n
2s), 2-sulfydryl-1-Methylimidazole (C
4h
6n
2or 2-mercaptobenzimidazole (C S)
7h
6n
2etc. S) one in.
8. a kind of dual anti-high strength solid buoyancy material as claimed in claim 4 Graphite Powder 99 used, is characterized in that: described Graphite Powder 99 is to adopt hexadecyl brometo de amonio (CTAB) to carry out the modified graphite powder that surface modification treatment is crossed.
9. a kind of dual anti-high strength solid buoyancy material as claimed in claim 4 Graphite Powder 99 used, it is characterized in that: the concrete modifying process of described Graphite Powder 99 is: take 5～10g Graphite Powder 99, join 20～50mL deionized water for stirring, with salt acid for adjusting pH value 7～8, ultrasonic 1～10 minute, add the cetyl trimethylammonium bromide of 1～5g, after ultrasonic 10～30 minutes, decompress filter, obtains filter cake with distilled water wash and is that 60～70 DEG C of vacuum-dryings obtain surface-treated Graphite Powder 99 for 24～48 hours.
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| CN112341206A (en) * | 2020-11-05 | 2021-02-09 | 衡阳凯新特种材料科技有限公司 | Forming method of rare earth praseodymium-holmium-stabilized silicon nitride ceramic |
| CN113603501A (en) * | 2021-08-12 | 2021-11-05 | 南京工业大学 | Selective adsorption cooling material and preparation method and application thereof |
| CN115093194A (en) * | 2022-08-24 | 2022-09-23 | 江苏夸迪安防集团有限公司 | Antibacterial floating bead fireproof heat-insulation plate and preparation method and application thereof |
| CN115093194B (en) * | 2022-08-24 | 2022-11-08 | 江苏夸迪安防集团有限公司 | Antibacterial floating bead fireproof heat-insulation plate and preparation method and application thereof |
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