CN104263204A - Preparation method for carbon nanotube-epoxy resin radiation-resistant coating for steel-based surface of nuclear power station - Google Patents
Preparation method for carbon nanotube-epoxy resin radiation-resistant coating for steel-based surface of nuclear power station Download PDFInfo
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- CN104263204A CN104263204A CN201410465153.3A CN201410465153A CN104263204A CN 104263204 A CN104263204 A CN 104263204A CN 201410465153 A CN201410465153 A CN 201410465153A CN 104263204 A CN104263204 A CN 104263204A
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- carbon nanotube
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
- C09D163/04—Epoxynovolacs
-
- 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
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
-
- 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
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
Abstract
The invention discloses a preparation method for a carbon nanotube-epoxy resin radiation-resistant coating for a steel-based surface of a nuclear power station. The preparation method comprises the following step: functionally filling the epoxy resin by virtue of a nano modification technique by using linear phenol formaldehyde epoxy resin and a modified arylamine curing agent as a film forming matter by using a carbon nanotube as filler. By adopting a technique of nano-modifying a composite material, the preparation method is low in instrument and equipment requirements, high in production efficiency and easy to operate under a high-temperature high-pressure condition.
Description
Technical field
The invention belongs to chemical material field, be specifically related to a kind of preparation method of Nuclear power plants steel substrate surface carbon nanotube-epoxy resin radiation resistant coating.
Background technology
At present, the protective coating mainly epoxy resin coating that China's Nuclear power plants radiation control zone steel substrate surface is used, mainly because such coating has good corrosion resistance nature, chemical resistance and good radiation resistance and be widely used, but in order to improve the radiation resistance of coating, usual meeting adds functional radiation hardness filler by the technique of solution blending or melt blending in epoxy-resin systems, used in nuclear power station radioprotective coating is related to as " radioresistant paint for nuclear power plant and preparation method thereof " (CN101245215) disclosed in Chinese invention patent, it utilizes potassium titanate crystal whisker to add in epoxy resin to have prepared used in nuclear power station epoxy radiation shielding coating, this coating have passed radiation resistance, detergency ability is tested, but be only radiation shielding coating, do not relate to protection against corrosion, therefore be applied on steel construction and be not suitable for, and the more general filler of potassium titanate crystal whisker price adopted is expensive, be not suitable for commercial applications, in addition " used in nuclear power station epoxy is coated with system " (CN101235246), this coat system is the nuclear power plant concrete factory building coating of resistance to radiation protection, can not be applied in steel structures coating, limits the Application Areas of this coating.
Along with country is to the attention of radio-protective safety, the sfgd. of the base steel of Nuclear power plants radiation control zone is also optimized further, except requiring that this protective coating has excellent radiation resistance, outside erosion resistance and chemical resistance, also need to possess higher mechanical property, this is just except requiring the polymer-based external of better performances, also need the filler reinforcement of excellent performance, because nanoparticle has special surface effects, volume effect and quantum size effect, it is made to be used widely in nano modification field of compound material, carbon nanotube is due to the constructional feature of its uniqueness, it is made to play a role as radical scavenger under gamma Rays, and matrix mechanical property can be improved preferably.This preparation method adopts carbon nanotube to be filler, take epoxy resin as matrix, prepares radiation resistant coating by nano modification method.
Summary of the invention
Goal of the invention: the object of the invention is to for the deficiencies in the prior art, provides a kind of preparation method of Nuclear power plants steel substrate surface carbon nanotube-epoxy resin radiation resistant coating.
Technical scheme: in order to achieve the above object, the present invention is specifically achieved like this: a kind of preparation method of Nuclear power plants steel substrate surface carbon nanotube-epoxy resin radiation resistant coating, comprises the following steps:
(1) chloride of carbon nanotube: 0.5 ~ 1 part of carbon nanotube is joined in 40 ~ 60 parts of thionyl chloride solution, under 65 DEG C ~ 85 DEG C conditions, condensing reflux 24h ~ 30h, with tetrahydrofuran solution by the centrifugation of reaction product repetitive scrubbing to upper liquid clear, take off layer black precipitate for subsequent use after dry 12h under 50 DEG C ~ 60 DEG C vacuum conditions, wherein unit number is mass fraction, lower same;
(2) amination of carbon nanotube: step (1) gains are joined in 70 ~ 80 parts of modified amine, and add the ethanolic soln of 10 ~ 15 parts, under 120 DEG C ~ 140 DEG C conditions, condensing reflux 45h ~ 50h, with the centrifugation of ethanolic soln repetitive scrubbing to upper liquid clear, dry 24h under 50 DEG C ~ 60 DEG C vacuum conditions, obtains the carbon nanotube after modification again;
(3) carbon nanotube EtOH Sonicate process: join in 10 ~ 15 parts of ethanolic solns by products therefrom in step (2), obtains carbon nanotube EtOH Sonicate dispersion liquid after supersound process 5 ~ 10min;
(4) products therefrom in step (3) being joined in 30 ~ 40 parts of linear phenolic epoxy resins, adding 4-6 part reactive thinner, the defoamer of 0.5 ~ 1.12 part and the flow agent of 0.55 ~ 1.4 part, with high speed dispersor to being uniformly dispersed; Wherein, reactive thinner preferred HUNTSMAN company Araldite DY-K type thinner, defoamer preferred BYK company BYK-530 type, flow agent preferred BYK company BYK-054 type.
(5) 60 ~ 80 parts of curing agents are joined in step (4) products therefrom, curing agent preferred HUNTSMAN Aradur 830 type solidifying agent;
(6) be sprayed on steel plate after products therefrom in step (5) being stirred, and dry 24h, finally thermofixation 20 ~ 30min under 80 DEG C of conditions at normal temperatures, obtain Nuclear power plants steel substrate surface carbon nano tube epoxy resin radiation resistant coating.
Wherein, step (1) described carbon nanotube is the carbon nanotube after acidifying, and its caliber (OD) is less than 8nm ,-COOH group content 3wt% ~ 4wt%.
Wherein, in step (2), modified amine is poly-aminosiloxane modified amine, polymeric amide, diethylenetriamine or wherein two or more mixing.
Wherein, in step (3), ultrasonic frequency is 40 ~ 50K.
Wherein, step (4) neutral line resol is epoxy equivalent (weight) 170 ~ 180g/Eq, second-order transition temperature 180 ~ 210 DEG C, one or more mixed with resin of functionality 2.1 ~ 2.5.
Beneficial effect: the present invention, compared with conventional art, does not need high-temperature and high-pressure conditions, require low to plant and instrument, production cost is low, and production efficiency is high, easy handling.Gained radiation resistant coating not only has excellent radiation resistance, also has higher erosion resistance.
Embodiment
Embodiment 1:
1. first getting 0.5 part of carbon nanotube joins in 50 parts of thionyl chloride solution, condensing reflux 24h under 70 DEG C of conditions, on settling centrifuge, repeatedly with tetrahydrofuran solution by product washing precipitation to upper liquid clear, obtain lower black throw out dry 24h under 50 DEG C ~ 60 DEG C vacuum conditions.
2. (active hydrogen equivalent weight is step 1 products therefrom to be joined 80 parts of modified polyorganosiloxane modified amine
240g/Eq), add 10 parts of ethanolic solns, under 120 DEG C of conditions, condensing reflux 48h, with the centrifugation of ethanolic soln repetitive scrubbing to upper liquid clear, then by lower black throw out dry 24h under 60 DEG C of vacuum conditions, obtain the carbon nanotube after modification.
3. products therefrom in step 2 is joined in 12 parts of ethanolic solns, after supersound process (40k) 10min, obtain carbon nanotube EtOH Sonicate dispersion liquid.
4. (epoxy equivalent (weight) is 170 ~ 180g/Eq products therefrom in step 3 to be joined 40 parts of linear phenolic epoxy resins, second-order transition temperature is 172 DEG C ~ 179 DEG C, functionality is about 2.5) in, add 4 portions of reactive thinners, the defoamer of 0.5 part and the flow agent of 0.55 part, stir 10min with high speed dispersor.
5. 60 parts of curing agents are joined in step 4 products therefrom, stir.
6. be sprayed on steel plate after step 5 products therefrom being stirred, and dry 24h, finally thermofixation 20min under 80 DEG C of conditions at normal temperatures, obtain Nuclear power plants steel substrate surface carbon nano tube/epoxy resin radiation resistant coating.
Embodiment 2:
1. 0.8 part of carbon nanotube is joined in 60 parts of thionyl chloride solution, under 70 DEG C of conditions, condensing reflux 24h, with tetrahydrofuran solution by the centrifugation of reaction product repetitive scrubbing to upper liquid clear, take off layer black precipitate dry 24h under 50 DEG C ~ 60 DEG C vacuum conditions.
2. step 1 gains are joined in 70 parts of diethylenetriamines, and add 15 parts of ethanolic solns, and under 140 DEG C of conditions, condensing reflux 48h, with the centrifugation of ethanolic soln repetitive scrubbing to upper liquid clear, then the carbon nanotube after dry 24h obtains modification under 50 DEG C of vacuum conditions.
3. products therefrom in step 2 is joined in 15 parts of ethanolic solns, after supersound process (45k) 10min, obtain carbon nanotube EtOH Sonicate dispersion liquid.
4. products therefrom in step 3 is joined in 40 parts of linear phenolic epoxy resins, add 6 portions of reactive thinners, the defoamer of 1.12 parts and the flow agent of 1.4 parts, stir 10min with high speed dispersor.
5. 60 parts of curing agents are joined in step 4 products therefrom, stir.
6. be sprayed on steel plate after step 5 products therefrom being stirred, and dry 24h, finally thermofixation 20min under 80 DEG C of conditions at normal temperatures, obtain Nuclear power plants steel substrate surface carbon nano tube/epoxy resin radiation resistant coating.
Embodiment 3:
1. 0.5 part of carbon nanotube is joined in 40 parts of thionyl chloride solution, under 75 DEG C of conditions, condensing reflux 24h ~ 30h, with tetrahydrofuran solution by the centrifugation of reaction product repetitive scrubbing to upper liquid clear, it is for subsequent use after dry 12h under 50 DEG C ~ 60 DEG C vacuum conditions to take off layer black precipitate.
2. step 1 gains are joined in 80 parts of polysiloxane-modified amine, and add 12 parts of ethanolic solns, and under 120 DEG C of conditions, condensing reflux 48h, with the centrifugation of ethanolic soln repetitive scrubbing to upper liquid clear, then the carbon nanotube after dry 24h obtains modification under 60 DEG C of vacuum conditions.
3. products therefrom in step 2 is joined in 15 parts of ethanolic solns, after supersound process (50k) 10min, obtain carbon nanotube EtOH Sonicate dispersion liquid.
4. products therefrom in step 3 being joined in 50 parts of linear phenolic epoxy resins, adding 5 portions of reactive thinners, the defoamer of 0.6 part and the flow agent of 0.8 part, with high speed dispersor to being uniformly dispersed.
5. 70 parts of curing agents are joined in step 4 products therefrom, stir
6., by step 5 products therefrom, be sprayed on steel plate after stirring, and dry 24h, finally thermofixation 25min under 80 DEG C of conditions at normal temperatures, obtain Nuclear power plants steel substrate surface carbon nano tube/epoxy resin radiation resistant coating.
Embodiment 4:
Table 1 Nuclear power plants steel substrate surface carbon nano tube/epoxy resin radiation resistant coating detection perform:
Claims (5)
1. a Nuclear power plants steel substrate surface preparation method for carbon nanotube-epoxy resin radiation resistant coating, is characterized in that, comprise the following steps:
(1) chloride of carbon nanotube: 0.5 ~ 1 part of carbon nanotube is joined in 40 ~ 60 parts of thionyl chloride solution, under 65 DEG C ~ 85 DEG C conditions, condensing reflux 24h ~ 30h, with tetrahydrofuran solution by the centrifugation of reaction product repetitive scrubbing to upper liquid clear, take off layer black precipitate for subsequent use after dry 12h under 50 DEG C ~ 60 DEG C vacuum conditions, wherein unit number is mass fraction, lower same;
(2) amination of carbon nanotube: step (1) gains are joined in 70 ~ 80 parts of modified amine, and add 10 ~ 15 parts of ethanolic solns, under 120 DEG C ~ 140 DEG C conditions, condensing reflux 45h ~ 50h, with the centrifugation of ethanolic soln repetitive scrubbing to upper liquid clear, dry 24h under 50 DEG C ~ 60 DEG C vacuum conditions, obtains the carbon nanotube after modification again;
(3) carbon nanotube EtOH Sonicate process: join in 10 ~ 15 parts of ethanolic solns by products therefrom in step (2), obtains carbon nanotube EtOH Sonicate dispersion liquid after supersound process 5 ~ 10min;
(4) products therefrom in step (3) being joined in 30 ~ 40 parts of linear phenolic epoxy resins, adding 4-6 part reactive thinner, the defoamer of 0.5 ~ 1.12 part and the flow agent of 0.55 ~ 1.4 part, with high speed dispersor to being uniformly dispersed;
(5) 60 ~ 80 parts of curing agents are joined in step (4) products therefrom;
(6) be sprayed on steel plate after products therefrom in step (5) being stirred, and dry 24h, finally thermofixation 20 ~ 30min under 80 DEG C of conditions at normal temperatures, obtain Nuclear power plants steel substrate surface carbon nano tube epoxy resin radiation resistant coating.
2. Nuclear power plants steel substrate surface carbon nanotube-epoxy resin radiation resistant coating preparation method according to claim 1, it is characterized in that, step (1) described carbon nanotube is the carbon nanotube after acidifying, and its caliber is less than 8nm ,-COOH group content 3 ~ 4wt%.
3. Nuclear power plants steel substrate surface carbon nanotube-epoxy resin radiation resistant coating preparation method according to claim 1, it is characterized in that, in step (2), modified amine is poly-aminosiloxane modified amine, polymeric amide, diethylenetriamine or wherein two or more mixing.
4. Nuclear power plants steel substrate surface carbon nanotube-epoxy resin radiation resistant coating preparation method according to claim 1, is characterized in that, in step (3), ultrasonic frequency is 40 ~ 50K.
5. Nuclear power plants steel substrate surface carbon nanotube-epoxy resin radiation resistant coating preparation method according to claim 1, it is characterized in that, step (4) neutral line resol is epoxy equivalent (weight) 170 ~ 180g/Eq, second-order transition temperature 180 ~ 210 DEG C, one or more mixed with resin of functionality 2.1 ~ 2.5.
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Cited By (12)
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CN105694677A (en) * | 2016-04-27 | 2016-06-22 | 黄河科技学院 | Novolac epoxy resin radiation protective paint and preparation method thereof |
CN105802453A (en) * | 2016-04-27 | 2016-07-27 | 黄河科技学院 | Novolac epoxy resin multifunctional anti-radiation and anti-flaming coating and preparation method thereof |
CN105802299A (en) * | 2016-04-27 | 2016-07-27 | 黄河科技学院 | Anti-corrosion and anti-radiation coating and preparation method thereof |
CN105820630A (en) * | 2016-04-27 | 2016-08-03 | 黄河科技学院 | Radiation-resistant paint and preparation method thereof |
CN105820718A (en) * | 2016-04-27 | 2016-08-03 | 黄河科技学院 | Anti-corrosion anti-radiation ceramic coating and preparation method thereof |
CN105820629A (en) * | 2016-04-27 | 2016-08-03 | 黄河科技学院 | Novolac epoxy resin multifunctional radiation-resistant paint and preparation method thereof |
CN105820711A (en) * | 2016-04-27 | 2016-08-03 | 黄河科技学院 | Phenolic epoxy resin anti-corrosion anti-radiation coating and preparation method thereof |
CN105838197A (en) * | 2016-04-27 | 2016-08-10 | 黄河科技学院 | Environment-friendly anti-radiation coating and preparation method thereof |
CN105860621A (en) * | 2016-04-27 | 2016-08-17 | 黄河科技学院 | Corrosion-resistant radiation-resistant novolac epoxy resin paint and preparation method thereof |
CN105860622A (en) * | 2016-04-27 | 2016-08-17 | 黄河科技学院 | Radiation-resistant novolac epoxy resin paint and preparation method thereof |
CN108977807A (en) * | 2018-08-07 | 2018-12-11 | 杨瑞冰 | A kind of surface of steel plate environment friendly corrosion protection etching method |
CN109971309A (en) * | 2019-03-09 | 2019-07-05 | 金华市易途新材料有限公司 | A kind of preparation method of fire resistant water-based anticorrosive paint |
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Cited By (12)
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CN105694677A (en) * | 2016-04-27 | 2016-06-22 | 黄河科技学院 | Novolac epoxy resin radiation protective paint and preparation method thereof |
CN105802453A (en) * | 2016-04-27 | 2016-07-27 | 黄河科技学院 | Novolac epoxy resin multifunctional anti-radiation and anti-flaming coating and preparation method thereof |
CN105802299A (en) * | 2016-04-27 | 2016-07-27 | 黄河科技学院 | Anti-corrosion and anti-radiation coating and preparation method thereof |
CN105820630A (en) * | 2016-04-27 | 2016-08-03 | 黄河科技学院 | Radiation-resistant paint and preparation method thereof |
CN105820718A (en) * | 2016-04-27 | 2016-08-03 | 黄河科技学院 | Anti-corrosion anti-radiation ceramic coating and preparation method thereof |
CN105820629A (en) * | 2016-04-27 | 2016-08-03 | 黄河科技学院 | Novolac epoxy resin multifunctional radiation-resistant paint and preparation method thereof |
CN105820711A (en) * | 2016-04-27 | 2016-08-03 | 黄河科技学院 | Phenolic epoxy resin anti-corrosion anti-radiation coating and preparation method thereof |
CN105838197A (en) * | 2016-04-27 | 2016-08-10 | 黄河科技学院 | Environment-friendly anti-radiation coating and preparation method thereof |
CN105860621A (en) * | 2016-04-27 | 2016-08-17 | 黄河科技学院 | Corrosion-resistant radiation-resistant novolac epoxy resin paint and preparation method thereof |
CN105860622A (en) * | 2016-04-27 | 2016-08-17 | 黄河科技学院 | Radiation-resistant novolac epoxy resin paint and preparation method thereof |
CN108977807A (en) * | 2018-08-07 | 2018-12-11 | 杨瑞冰 | A kind of surface of steel plate environment friendly corrosion protection etching method |
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