CN102585697B - Nuclear radiation-resistant coating and preparation method thereof - Google Patents
Nuclear radiation-resistant coating and preparation method thereof Download PDFInfo
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- CN102585697B CN102585697B CN201210038184.1A CN201210038184A CN102585697B CN 102585697 B CN102585697 B CN 102585697B CN 201210038184 A CN201210038184 A CN 201210038184A CN 102585697 B CN102585697 B CN 102585697B
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Abstract
The invention discloses a nuclear radiation-resistant coating, which is characterized by consisting of a component A and a component B, wherein the component A comprises epoxy resin, inorganic mineral filler, a diluting agent and a processing agent; the component B comprises an amine hardener and a coupling agent; the molar ratio of the component A to the component B is 6-8:1; and the coating comprises the components in parts by mass respectively: 30-90 parts of epoxy resin, 35-90 parts of inorganic mineral filler, 0-50 parts of diluting agent, 5-40 parts of processing agent, 10-30 parts of amine hardener and 0-15 parts of coupling agent. The nuclear radiation-resistant coating has the advantages of superior radiation resistance and superior thermal stability.
Description
Technical field
The present invention relates to a kind of coating of resistance to nuclear radiation and preparation method thereof, is a kind of coating of resistance to nuclear radiation applicable to the nuclear installation of resistance to high-level radiation and preparation method thereof specifically.
Background technology
Nuclear energy is a kind of novel energy, and under the prerequisite of our times various countries growing interest energy problem, nuclear energy, with advantages such as it are clean, pollution-free, quantity discharged is little, is paid attention to by countries in the world gradually.Yet the application of nuclear energy but exists self unvanquishable significant deficiency.First, nuclear energy application be take nuclear power conventionally as main, and in order to prevent nuclear leakage situation infringement public health, nuclear power plant is generally located at seashore, and nuclear power plant structure be take concrete and steel as main.Marine atmosphere has extremely strong corrodibility, causes the nuclear installation of concrete and steel construction easily to occur catabiosis.In addition; nuclear reactor all exists hiding nuclear radiation around; nuclear radiation meeting accelerated material aging; radioactive dust also can stick to the surface of building or equipment; even infiltrate in the fine gap of concrete and steel construction and form permanent radioactive source, so all need to carry out coating protection on current nuclear reaction facility.Secondly, the coating that application is used need to be considered the possibility that nuclear reactor has an accident, such as rare circuit cools agent escapes accident, now reactor heats up rapidly, boosts, and is accompanied by cold water spray, and the dope layer of application will be subject to the violent effect of expanding with heat and contract with cold, if there is peeling phenomenon in coating, coating can stop up circulated sprinkling passage, and water coolant can not be supplied, and it forms greatly and threaten Nuclear Safety.Therefore, how to develop a kind of radiation hardness, paint application that stability is strong, become a great technical barrier in nuclear energy application.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide that a kind of radioresistance is good, the good coating of resistance to nuclear radiation of thermal stability.
Another goal of the invention of the present invention is to provide a kind of preparation method of the above-mentioned coating of resistance to nuclear radiation.
Goal of the invention of the present invention is achieved in that a kind of coating of resistance to nuclear radiation, it is characterized in that: the described coating of resistance to nuclear radiation comprises A component and B component, A component comprises epoxy resin, inorganic mineral filler, thinner and processing aid, B component comprises amine hardener and coupling agent, the mol ratio of A component and B component is 6-8:1, and each component is respectively by massfraction: epoxy resin 30-90 part; Inorganic mineral filler 35-90 part; Thinner 0-50 part; Processing aid 5-40 part; Amine hardener 10-30 part; Coupling agent 0-15 part.
Described epoxy resin is comprised of main resin and secondary resin, main resin is epoxy modified silicone resin, secondary resin is that a kind of or above-mentioned three kinds of compositions in epoxy resin E51, epoxy resin E20 and novolac epoxy mix in any proportion, and the mol ratio of main resin and secondary resin is 2-3.5:1.
The oxirane value of described epoxy modified silicone resin is 0.01-0.1.
Described novolac epoxy is that a kind of or mentioned component in line style phenol formaldehyde (PF) epoxy resin and ortho-cresol formaldehyde epoxy resin mixes in any proportion.
The particle diameter of described inorganic mineral filler is 2 μ m-10 μ m.
Described inorganic mineral filler is that a kind of or mentioned component in titanium dioxide, barium sulfate, feldspar in powder, mica powder, kaolin, wilkinite, composite iron-titanium powder and talcum powder mixes in any proportion.
Described thinner is that a kind of or mentioned component in acetone, propylene glycol monomethyl ether, propyl carbinol, Virahol and methyl iso-butyl ketone (MIBK) mixes in any proportion.
Described processing aid is that a kind of or mentioned component in defoamer, flow agent, wetting agent and dispersion agent mixes in any proportion.
Described defoamer is that a kind of or mentioned component in German Bi Ke BYK-067A, BYK-085, BYK-A530 and BYK-A535 mixes in any proportion.
Described flow agent is that a kind of or mentioned component in German Bi Ke BYK-350, BYK-358N and BYK-388 mixes in any proportion.
Described wetting agent is that a kind of or mentioned component in German Bi Ke BYK-302, BYK-322, BYK-377 and BYK-333 mixes in any proportion.
Described dispersion agent is that a kind of or mentioned component in German Bi Ke BYK-108, BYK-111, BYK-140 and BYK-P105 mixes in any proportion.
Described amine hardener is that a kind of or mentioned component in modified fatty amine, aliphatic cyclic amine, aromatic amine, polymeric amide and amido amine mixes in any proportion.
Described coupling agent is that a kind of or mentioned component in KH550, KH900, KH560, A-1100, sec.-propyl dioleate and oxygen base azido-silane mixes in any proportion.
The preparation method of the above-mentioned coating of resistance to nuclear radiation comprises the following steps:
A: take according to the above ratio raw material;
B: under normal temperature and pressure state, epoxy resin, thinner and processing aid are placed in and are disperseed in cylinder, and stir 8-14 minute with 500-1000 rev/min;
C: add inorganic mineral filler in the mixture drawing in b step, stir 15-25 minute with 1000-2000 rev/min under normal temperature and pressure state;
D: check that the compound particles fineness obtaining in c step is to 35-40 μ m, stir and obtain A component for 4-8 minute with 200-500 rev/min;
E: under normal temperature and pressure state, amine curing agent and coupling agent are placed in dispersion cylinder, and with 200-450 rev/min of stirring 5-25 minute, then filter and obtain B component with 100-150 mesh filter screen;
F: A component and B component are obtained to the coating of resistance to nuclear radiation by the even mixing of the mol ratio of 6-8:1.
The present invention has the following advantages:
1, the coating of resistance to nuclear radiation of the present invention utilizes epoxy resin, thinner and inorganic mineral filler to coordinate amine curing agent and coupling agent reaction, formation can anti-high-level radiation compactness coating, greatly improved radiation resistance and the radiation absorption performance after paint spraying.Even if the equipment after application and concrete-steel structure are at 1.0X10
7under heavy dose of build-up radiation of GY/h, still there will not be crackle, bubble, peel off or the phenomenon of efflorescence.And in coating, add organosilicon epoxy resin, and make coating there is good chemical stability and thermostability, coating can keep adhesive capacity and the chemical property of paint film under the environment that expands with heat and contract with cold sharply.
2, the asbestos that do not contain traditional coating process in the coating of resistance to nuclear radiation of the present invention, safety in utilization is good.In addition, the coating that epoxy resin, inorganic mineral filler and amine curing agent form has good scrubbing, guarantees to there will not be in circulating cooling water channel the phenomenon of sticky dirt, to guarantee the smoothness of water coolant circulation, has also improved the security that nuclear installation uses.
Embodiment
The coating of resistance to nuclear radiation of the present invention comprises A component and B component, A component comprises epoxy resin, inorganic mineral filler, thinner and processing aid, B component comprises amine hardener and coupling agent, the mol ratio of A component and B component is 6-8:1, and each component is respectively by massfraction: epoxy resin 30-90 part; Inorganic mineral filler 35-90 part; Thinner 0-50 part; Processing aid 5-40 part; Amine hardener 10-30 part; Coupling agent 0-15 part.
Epoxy resin in A component of the present invention is mainly comprised of main resin and secondary resin, wherein main resin adopts epoxy modified silicone resin, secondary resin adopts a kind of or above-mentioned three kinds of compositions in epoxy resin E51, epoxy resin E20 and novolac epoxy to mix in any proportion, and the mol ratio of main resin and secondary resin is 2-3.5:1.Wherein, the oxirane value of epoxy modified silicone resin is 0.01-0.1, in the time of can guaranteeing resin reaction, can provide enough epoxide groups; And novolac epoxy can adopt a kind of or mentioned component in line style phenol formaldehyde (PF) epoxy resin and ortho-cresol formaldehyde epoxy resin to mix in any proportion.Epoxy modified silicone resin has excellent radiation resistance, thermostability, erosion resistance and chemical stability; And epoxy resin E51, epoxy resin E20 and novolac epoxy and epoxy modified silicone resin have synergistic effect, and epoxy resin E51 and epoxy resin E20 have, and viscosity is low, mechanical stability advantages of higher, the viscosity in the time of can improving paint spraying and compactness; Line style phenol formaldehyde (PF) epoxy resin and ortho-cresol formaldehyde epoxy resin all have good electrical insulating property, water tolerance and erosion resistance.Inorganic mineral filler in A component adopts a kind of or mentioned component in titanium dioxide, barium sulfate, feldspar in powder, mica powder, kaolin, wilkinite, composite iron-titanium powder and talcum powder to mix in any proportion, and particle diameter is 2 μ m-10 μ m.Ligation by fine grain size weighting material in epoxy-resin systems, makes coating have good physical and mechanical property.Thinner in A component adopts a kind of or mentioned component in acetone, propylene glycol monomethyl ether, propyl carbinol, Virahol and methyl iso-butyl ketone (MIBK) to mix in any proportion, thinner can reduce the viscosity of coating, and improve macromole chain flexibility in coating, improve the adhesive capacity of coating.In order to make the processing of coating and synthetic more convenient, in A component, also added processing aid.A kind of or the mentioned component of processing aid in defoamer, flow agent, wetting agent and dispersion agent mixes and forms in any proportion, and defoamer adopts a kind of or mentioned component in German Bi Ke BYK-067A, BYK-085, BYK-A530 and BYK-A535 to mix in any proportion; Flow agent adopts a kind of or mentioned component in German Bi Ke BYK-350, BYK-358N and BYK-388 to mix in any proportion; Wetting agent adopts a kind of or mentioned component in German Bi Ke BYK-302, BYK-322, BYK-377 and BYK-333 to mix in any proportion; Dispersion agent adopts a kind of or mentioned component in German Bi Ke BYK-108, BYK-111, BYK-140 and BYK-P105 to mix in any proportion.Above-mentioned processing aid can be to coating processing characteristics, can improve soil removability, mobility and the adhesive capacity of coating simultaneously.B component of the present invention comprises amine hardener and coupling agent.Amine hardener adopts a kind of or mentioned component in modified fatty amine, aliphatic cyclic amine, aromatic amine, polymeric amide and amido amine to mix in any proportion, and amine hardener can strengthen the cementability of coating when application, makes coating can form fine and close paint film when application.Coupling agent adopts a kind of or mentioned component in KH550, KH900, KH560, A-1100, sec.-propyl dioleate and oxygen base azido-silane to mix in any proportion, coupling agent can improve the bonding strength between epoxy resin and inorganic mineral filler, make coating bonding coat between formation and equipment or concrete-steel structure after application, strengthen the bounding force between coating and equipment or concrete-steel structure.
And the preparation method for coating of resistance to nuclear radiation of the present invention comprises the steps:
A: take according to the above ratio raw material;
B: under normal temperature and pressure state, epoxy resin, thinner and processing aid are placed in and are disperseed in cylinder, and stir 8-14 minute with 500-1000 rev/min;
C: add inorganic mineral filler in the mixture drawing in b step, stir 15-25 minute with 1000-2000 rev/min under normal temperature and pressure state;
D: check that the compound particles fineness obtaining in c step is to 35-40 μ m, stir and obtain A component for 4-8 minute with 200-500 rev/min;
E: under normal temperature and pressure state, amine curing agent and coupling agent are placed in dispersion cylinder, and with 200-450 rev/min of stirring 5-25 minute, then filter and obtain B component with 100-150 mesh filter screen;
F: A component and B component are obtained to the coating of resistance to nuclear radiation by the even mixing of the mol ratio of 6-8:1.
The coating of resistance to nuclear radiation of the present invention has good radiation resistance and radiation absorption performance.After tested, when film thickness reaches 70-80 μ m, at dosage, be more than or equal to 2.5 * 10
5under the radiation irradiation environment of Gy/h, coating paint film is intact, without peeling off, without cracking with without metachromatism; In integral dose, be more than or equal to 1.0X10
7under the radiation irradiation environment of GY/h, coating paint film is intact, without peeling off, without cracking with without metachromatism.In addition, coating paint film continues 200 hours under the temperature environment of 120 ℃, and paint film is intact, nothing cracking, and paint film adhesion reaches 3.2-3.8MPa.
According to table 1, each embodiment is elaborated below, but does not therefore limit the invention in described scope of embodiments:
Embodiment 1
The coating of resistance to nuclear radiation of the present invention comprises A component and B component, and A component comprises epoxy resin, inorganic mineral filler, thinner and processing aid, and B component comprises amine hardener and coupling agent, and the mol ratio of A component and B component is 8:1.In A component, epoxy resin is comprised of main resin and secondary resin, and it is 0.01 epoxy modified silicone resin that main resin is selected oxirane value, and secondary resin adopts epoxy resin E51 and line style phenol formaldehyde (PF) epoxy resin composition, and main resin and secondary resin mol ratio are 2:1.Inorganic mineral filler is comprised of titanium dioxide, barium sulfate, feldspar in powder, mica powder, kaolin, wilkinite and composite iron-titanium powder, and inorganic mineral filler particle diameter is 2 μ m; Thinner is comprised of acetone, propylene glycol monomethyl ether, propyl carbinol, Virahol and methyl iso-butyl ketone (MIBK); Processing aid is comprised of BYK-067A, BYK-085, BYK-350, BYK-302 and BYK-108.In B component, amine hardener is comprised of modified fatty amine and aliphatic cyclic amine.Said components content is respectively by massfraction: epoxy modified silicone resin: 20 parts; Epoxy resin E51:5 part; Line style phenol formaldehyde (PF) epoxy resin: 5 parts; Titanium dioxide: 5 parts; Barium sulfate: 5 parts; Feldspar in powder: 5 parts; Mica powder: 5 parts; Kaolin: 5 parts; Wilkinite: 5 parts; Composite iron-titanium powder: 5 parts; Acetone: 2 parts; Propylene glycol monomethyl ether: 2 parts; Propyl carbinol: 2 parts; Virahol: 2 parts; Methyl iso-butyl ketone (MIBK): 2 parts; BYK-067A:1 part; BYK-085:1 part; BYK-350:1 part; BYK-302:1 part; BYK-108:1 part; Modified fatty amine: 5 parts; Aliphatic cyclic amine: 5 parts.
The preparation method of the above-mentioned coating of resistance to nuclear radiation comprises the steps:
A: take according to the above ratio raw material;
B: under normal temperature and pressure state, epoxy resin, thinner and processing aid are placed in and are disperseed in cylinder, and stir 8 minutes with 500 revs/min;
C: add inorganic mineral filler in the mixture drawing in b step, stir 15 minutes with 1000 revs/min under normal temperature and pressure state;
D: check compound particles fineness to the 35 μ m obtaining in c step, stir and obtain A component for 4 minutes with 200 revs/min;
E: under normal temperature and pressure state, amine curing agent and coupling agent are placed in dispersion cylinder, and with 200 revs/min of stirrings 5 minutes, then filter and obtain B component with 100 mesh filter screens;
F: A component and B component are obtained to the coating of resistance to nuclear radiation by the even mixing of the mol ratio of 8:1.
After tested, when film thickness reaches 70 μ m, at dosage, be more than or equal to 2.5 * 10
5under the radiation irradiation environment of Gy/h, coating paint film is intact, without peeling off, without cracking with without metachromatism; In integral dose, be more than or equal to 1.0X10
7under the radiation irradiation environment of GY/h, coating paint film is intact, without peeling off, without cracking with without metachromatism.In addition, coating paint film continues 200 hours under the temperature environment of 120 ℃, and paint film is intact, nothing cracking, and paint film adhesion reaches 3.2MPa.
Embodiment 2
The coating of resistance to nuclear radiation of the present invention comprises A component and B component, and A component comprises epoxy resin, inorganic mineral filler, thinner and processing aid, and B component comprises amine hardener and coupling agent, and the mol ratio of A component and B component is 6:1.In A component, epoxy resin is comprised of main resin and secondary resin, it is 0.1 epoxy modified silicone resin that main resin is selected oxirane value, secondary resin adopts epoxy resin E51, epoxy resin E20, line style phenol formaldehyde (PF) epoxy resin and ortho-cresol formaldehyde epoxy resin composition, and main resin and secondary resin mol ratio are 3.5:1.Inorganic mineral filler is comprised of titanium dioxide, barium sulfate, feldspar in powder, mica powder, kaolin, wilkinite, composite iron-titanium powder and talcum powder, and inorganic mineral filler particle diameter is 10 μ m; Thinner is comprised of acetone, propylene glycol monomethyl ether, propyl carbinol, Virahol and methyl iso-butyl ketone (MIBK); Processing aid is comprised of BYK-067A, BYK-085, BYK-A530, BYK-A535, BYK-350, BYK-358N, BYK-388, BYK-302, BYK-322, BYK-377, BYK-333, BYK-108, BYK-111, BYK-140 and BYK-P105.In B component, amine hardener is comprised of modified fatty amine, aliphatic cyclic amine, aromatic amine, polymeric amide and amido amine, and coupling agent is comprised of KH550, KH900, KH560, A-1100, sec.-propyl dioleate oxygen base and azido-silane.Said components content is respectively by massfraction: epoxy modified silicone resin: 70 parts; Epoxy resin E51:5 part; Epoxy resin E20:5 part; Line style phenol formaldehyde (PF) epoxy resin: 5 parts; Ortho-cresol formaldehyde epoxy resin: 5 parts; Titanium dioxide: 12 parts; Barium sulfate: 11 parts; Feldspar in powder: 11 parts; Mica powder: 13 parts; Kaolin: 10 parts; Wilkinite: 11 parts; Composite iron-titanium powder: 12 parts; Talcum powder: 10 parts; Acetone: 10 parts; Propylene glycol monomethyl ether: 10 parts; Propyl carbinol: 10 parts; Virahol: 10 parts; Methyl iso-butyl ketone (MIBK): 10 parts; BYK-067A:2 part; BYK-085:2 part; BYK-A530:4 part; BYK-A535:2 part; BYK-350:2 part; BYK-358N:4 part; BYK-388:4 part; BYK-302:2 part; BYK-322:4 part; BYK-377:2 part; BYK-333:2 part; BYK-108:2 part; BYK-111:4 part; BYK-140:2 part; BYK-P105:2 part; Modified fatty amine: 6 parts; Aliphatic cyclic amine: 6 parts; Aromatic amine: 6 parts; Polymeric amide: 6 parts; Amido amine: 6 parts; KH550:3 part; KH900:3 part; KH560:2 part; A-1100:1 part; Sec.-propyl dioleate: 3 parts; Oxygen base azido-silane: 3 parts.
The preparation method of the above-mentioned coating of resistance to nuclear radiation comprises the steps:
A: take according to the above ratio raw material;
B: under normal temperature and pressure state, epoxy resin, thinner and processing aid are placed in and are disperseed in cylinder, and stir 14 minutes with 1000 revs/min;
C: add inorganic mineral filler in the mixture drawing in b step, stir 25 minutes with 2000 revs/min under normal temperature and pressure state;
D: check compound particles fineness to the 40 μ m obtaining in c step, stir and obtain A component for 8 minutes with 500 revs/min;
E: under normal temperature and pressure state, amine curing agent and coupling agent are placed in dispersion cylinder, and with 450 revs/min of stirrings 25 minutes, then filter and obtain B component with 150 mesh filter screens;
F: A component and B component are obtained to the coating of resistance to nuclear radiation by the even mixing of the mol ratio of 6:1.
After tested, when film thickness reaches 80 μ m, at dosage, be more than or equal to 2.5 * 10
5under the radiation irradiation environment of Gy/h, coating paint film is intact, without peeling off, without cracking with without metachromatism; In integral dose, be more than or equal to 1.0X10
7under the radiation irradiation environment of GY/h, coating paint film is intact, without peeling off, without cracking with without metachromatism.In addition, coating paint film continues 200 hours under the temperature environment of 120 ℃, and paint film is intact, nothing cracking, and paint film adhesion reaches 3.8MPa.
Embodiment 3
The coating of resistance to nuclear radiation of the present invention comprises A component and B component, and A component comprises epoxy resin, inorganic mineral filler, thinner and processing aid, and B component comprises amine hardener and coupling agent, and the mol ratio of A component and B component is 6.3:1.In A component, epoxy resin is comprised of main resin and secondary resin, it is 0.03 epoxy modified silicone resin that main resin is selected oxirane value, secondary resin adopts epoxy resin E51, epoxy resin E20, line style phenol formaldehyde (PF) epoxy resin and ortho-cresol formaldehyde epoxy resin composition, and main resin and secondary resin mol ratio are 2.1:1.Inorganic mineral filler is comprised of titanium dioxide, feldspar in powder, mica powder, kaolin, wilkinite, composite iron-titanium powder and talcum powder, and inorganic mineral filler particle diameter is 4 μ m; Thinner is comprised of acetone, propyl carbinol, Virahol and methyl iso-butyl ketone (MIBK); Processing aid is comprised of BYK-085, BYK-A535, BYK-358N, BYK-388, BYK-322, BYK-377, BYK-333, BYK-111, BYK-140 and BYK-P105.In B component, amine hardener is comprised of aliphatic cyclic amine, aromatic amine, polymeric amide and amido amine, and coupling agent is comprised of KH900, KH560, A-1100, sec.-propyl dioleate oxygen base and azido-silane.Said components content is respectively by massfraction: epoxy modified silicone resin: 30 parts; Epoxy resin E51:4 part; Epoxy resin E20:3 part; Line style phenol formaldehyde (PF) epoxy resin: 3 parts; Ortho-cresol formaldehyde epoxy resin: 4 parts; Titanium dioxide: 8 parts; Feldspar in powder: 9 parts; Mica powder: 4 parts; Kaolin: 7 parts; Wilkinite: 4 parts; Composite iron-titanium powder: 8 parts; Talcum powder: 3 parts; Acetone: 4 parts; Propyl carbinol: 3 parts; Virahol: 4 parts; Methyl iso-butyl ketone (MIBK): 2 parts; BYK-085:1 part; BYK-A535:3 part; BYK-358N:3 part; BYK-388:1 part; BYK-322:1 part; BYK-377:1 part; BYK-333:1 part; BYK-111:1 part; BYK-140:1 part; BYK-P105:1 part; Aliphatic cyclic amine: 2 parts; Aromatic amine: 2 parts; Polymeric amide: 4 parts; Amido amine: 5 parts; KH900:1 part; KH560:1 part; A-1100:1 part; Sec.-propyl dioleate: 1 part; Oxygen base azido-silane: 1 part.
The preparation method of the above-mentioned coating of resistance to nuclear radiation comprises the steps:
A: take according to the above ratio raw material;
B: under normal temperature and pressure state, epoxy resin, thinner and processing aid are placed in and are disperseed in cylinder, and stir 9 minutes with 600 revs/min;
C: add inorganic mineral filler in the mixture drawing in b step, stir 16 minutes with 1200 revs/min under normal temperature and pressure state;
D: check compound particles fineness to the 36 μ m obtaining in c step, stir and obtain A component for 5 minutes with 220 revs/min;
E: under normal temperature and pressure state, amine curing agent and coupling agent are placed in dispersion cylinder, and with 220 revs/min of stirrings 8 minutes, then filter and obtain B component with 110 mesh filter screens;
F: A component and B component are obtained to the coating of resistance to nuclear radiation by the even mixing of the mol ratio of 6.3:1.
After tested, when film thickness reaches 72 μ m, at dosage, be more than or equal to 2.5 * 10
5under the radiation irradiation environment of Gy/h, coating paint film is intact, without peeling off, without cracking with without metachromatism; In integral dose, be more than or equal to 1.0X10
7under the radiation irradiation environment of GY/h, coating paint film is intact, without peeling off, without cracking with without metachromatism.In addition, coating paint film continues 200 hours under the temperature environment of 120 ℃, and paint film is intact, nothing cracking, and paint film adhesion reaches 3.4MPa.
Embodiment 4
The coating of resistance to nuclear radiation of the present invention comprises A component and B component, and A component comprises epoxy resin, inorganic mineral filler, thinner and processing aid, and B component comprises amine hardener and coupling agent, and the mol ratio of A component and B component is 7:1.In A component, epoxy resin is comprised of main resin and secondary resin, it is 0.07 epoxy modified silicone resin that main resin is selected oxirane value, secondary resin adopts epoxy resin E51, epoxy resin E20, line style phenol formaldehyde (PF) epoxy resin and ortho-cresol formaldehyde epoxy resin composition, and main resin and secondary resin mol ratio are 2.8:1.Inorganic mineral filler is comprised of titanium dioxide, barium sulfate, feldspar in powder, mica powder, kaolin, wilkinite, composite iron-titanium powder and talcum powder, and inorganic mineral filler particle diameter is 10 μ m; Thinner is comprised of acetone, propylene glycol monomethyl ether, propyl carbinol and Virahol; Processing aid is comprised of BYK-067A, BYK-A530, BYK-A535, BYK-350, BYK-358N, BYK-388, BYK-302, BYK-322, BYK-377, BYK-333, BYK-108, BYK-111, BYK-140 and BYK-P105.In B component, amine hardener is comprised of modified fatty amine, aliphatic cyclic amine, aromatic amine and polymeric amide, and coupling agent is comprised of KH550, KH900, KH560, A-1100, sec.-propyl dioleate oxygen base and azido-silane.Said components content is respectively by massfraction: epoxy modified silicone resin: 50 parts; Epoxy resin E51:5 part; Epoxy resin E20:4 part; Line style phenol formaldehyde (PF) epoxy resin: 5 parts; Ortho-cresol formaldehyde epoxy resin: 4 parts; Titanium dioxide: 10 parts; Barium sulfate: 9 parts; Feldspar in powder: 8 parts; Mica powder: 8 parts; Kaolin: 8 parts; Wilkinite: 6 parts; Composite iron-titanium powder: 7 parts; Talcum powder: 8 parts; Acetone: 8 parts; Propylene glycol monomethyl ether: 9 parts; Propyl carbinol: 4 parts; Virahol: 5 parts; BYK-067A:1 part; BYK-A530:2 part; BYK-A535:1 part; BYK-350:2 part; BYK-358N:2 part; BYK-388:2 part; BYK-302:1 part; BYK-322:1 part; BYK-377:1 part; BYK-333:1 part; BYK-108:1 part; BYK-111:1 part; BYK-140:1 part; BYK-P105:1 part; Modified fatty amine: 3 parts; Aliphatic cyclic amine: 3 parts; Aromatic amine: 3 parts; Polymeric amide: 5 parts; KH550:2 part; KH900:2 part; KH560:1 part; A-1100:2 part; Sec.-propyl dioleate: 2 parts; Oxygen base azido-silane: 2 parts.
The preparation method of the above-mentioned coating of resistance to nuclear radiation comprises the steps:
A: take according to the above ratio raw material;
B: under normal temperature and pressure state, epoxy resin, thinner and processing aid are placed in and are disperseed in cylinder, and stir 11 minutes with 800 revs/min;
C: add inorganic mineral filler in the mixture drawing in b step, stir 20 minutes with 1600 revs/min under normal temperature and pressure state;
D: check compound particles fineness to the 38 μ m obtaining in c step, stir and obtain A component for 6 minutes with 380 revs/min;
E: under normal temperature and pressure state, amine curing agent and coupling agent are placed in dispersion cylinder, and with 400 revs/min of stirrings 21 minutes, then filter and obtain B component with 120 mesh filter screens;
F: A component and B component are obtained to the coating of resistance to nuclear radiation by the even mixing of the mol ratio of 7:1.
After tested, when film thickness reaches 78 μ m, at dosage, be more than or equal to 2.5 * 10
5under the radiation irradiation environment of Gy/h, coating paint film is intact, without peeling off, without cracking with without metachromatism; In integral dose, be more than or equal to 1.0X10
7under the radiation irradiation environment of GY/h, coating paint film is intact, without peeling off, without cracking with without metachromatism.In addition, coating paint film continues 200 hours under the temperature environment of 120 ℃, and paint film is intact, nothing cracking, and paint film adhesion reaches 3.6MPa.
Embodiment 5
The coating of resistance to nuclear radiation of the present invention comprises A component and B component, and A component comprises epoxy resin, inorganic mineral filler, thinner and processing aid, and B component comprises amine hardener and coupling agent, and the mol ratio of A component and B component is 6.8:1.In A component, epoxy resin is comprised of main resin and secondary resin, it is 0.09 epoxy modified silicone resin that main resin is selected oxirane value, secondary resin adopts epoxy resin E51, epoxy resin E20, line style phenol formaldehyde (PF) epoxy resin and ortho-cresol formaldehyde epoxy resin composition, and main resin and secondary resin mol ratio are 3.3:1.Inorganic mineral filler is comprised of titanium dioxide, barium sulfate, feldspar in powder, mica powder, kaolin, wilkinite, composite iron-titanium powder and talcum powder, and inorganic mineral filler particle diameter is 10 μ m; Thinner is comprised of acetone, propylene glycol monomethyl ether, propyl carbinol and methyl iso-butyl ketone (MIBK); Processing aid is comprised of BYK-067A, BYK-085, BYK-A530, BYK-A535, BYK-350, BYK-358N, BYK-388, BYK-302, BYK-322, BYK-377, BYK-333, BYK-108, BYK-111, BYK-140 and BYK-P105.In B component, amine hardener is comprised of modified fatty amine, aliphatic cyclic amine, aromatic amine, polymeric amide and amido amine, and coupling agent is comprised of KH550, KH900, KH560, A-1100, sec.-propyl dioleate oxygen base and azido-silane.Said components content is respectively by massfraction: epoxy modified silicone resin: 63 parts; Epoxy resin E51:5 part; Epoxy resin E20:5 part; Line style phenol formaldehyde (PF) epoxy resin: 4 parts; Ortho-cresol formaldehyde epoxy resin: 5 parts; Titanium dioxide: 11 parts; Barium sulfate: 9 parts; Feldspar in powder: 8 parts; Mica powder: 8 parts; Kaolin: 12 parts; Wilkinite: 10 parts; Composite iron-titanium powder: 11 parts; Talcum powder: 9 parts; Acetone: 7 parts; Propylene glycol monomethyl ether: 7 parts; Propyl carbinol: 8 parts; Methyl iso-butyl ketone (MIBK): 9 parts; BYK-067A:3 part; BYK-085:2 part; BYK-A530:1 part; BYK-A535:3 part; BYK-350:3 part; BYK-358N:1 part; BYK-388:3 part; BYK-302:3 part; BYK-322:2 part; BYK-377:3 part; BYK-333:2 part; BYK-108:2 part; BYK-111:3 part; BYK-140:2 part; BYK-P105:2 part; Modified fatty amine: 4 parts; Aliphatic cyclic amine: 5 parts; Aromatic amine: 5 parts; Polymeric amide: 4 parts; Amido amine: 4 parts; KH550:2 part; KH900:2 part; KH560:2 part; A-1100:1 part; Sec.-propyl dioleate: 2 parts; Oxygen base azido-silane: 2 parts.
The preparation method of the above-mentioned coating of resistance to nuclear radiation comprises the steps:
A: take according to the above ratio raw material;
B: under normal temperature and pressure state, epoxy resin, thinner and processing aid are placed in and are disperseed in cylinder, and stir 13 minutes with 900 revs/min;
C: add inorganic mineral filler in the mixture drawing in b step, stir 23 minutes with 1800 revs/min under normal temperature and pressure state;
D: check compound particles fineness to the 38 μ m obtaining in c step, stir and obtain A component for 7 minutes with 470 revs/min;
E: under normal temperature and pressure state, amine curing agent and coupling agent are placed in dispersion cylinder, and with 420 revs/min of stirrings 23 minutes, then filter and obtain B component with 130 mesh filter screens;
F: A component and B component are obtained to the coating of resistance to nuclear radiation by the even mixing of the mol ratio of 6.8:1.
After tested, when film thickness reaches 75 μ m, at dosage, be more than or equal to 2.5 * 10
5under the radiation irradiation environment of Gy/h, coating paint film is intact, without peeling off, without cracking with without metachromatism; In integral dose, be more than or equal to 1.0X10
7under the radiation irradiation environment of GY/h, coating paint film is intact, without peeling off, without cracking with without metachromatism.In addition, coating paint film continues 200 hours under the temperature environment of 120 ℃, and paint film is intact, nothing cracking, and paint film adhesion reaches 3.7MPa.
Table one (each component concentration is pressed massfraction and calculated)
Claims (14)
1. the coating of resistance to nuclear radiation, it is characterized in that: the described coating of resistance to nuclear radiation comprises A component and B component, A component comprises epoxy resin, inorganic mineral filler, thinner and processing aid, B component comprises amine hardener and coupling agent, the mol ratio of A component and B component is 6-8:1, and each components in mass portion is figured and is respectively: epoxy resin 30-90 part; Inorganic mineral filler 35-90 part; Thinner 0-50 part; Processing aid 5-40 part; Amine hardener 10-30 part; Coupling agent is greater than 0 and is less than or equal to 15 parts, described epoxy resin is comprised of main resin and secondary resin, main resin is epoxy modified silicone resin, secondary resin is that a kind of or above-mentioned three kinds of compositions in epoxy resin E51, epoxy resin E20 and novolac epoxy mix in any proportion, and the mol ratio of main resin and secondary resin is 2-3.5:1.
2. the coating of resistance to nuclear radiation according to claim 1, is characterized in that: the oxirane value of described epoxy modified silicone resin is 0.01-0.1.
3. the coating of resistance to nuclear radiation according to claim 1, is characterized in that: described novolac epoxy is that a kind of or mentioned component in line style phenol formaldehyde (PF) epoxy resin and ortho-cresol formaldehyde epoxy resin mixes in any proportion.
4. the coating of resistance to nuclear radiation according to claim 1, is characterized in that: the particle diameter of described inorganic mineral filler is 2 μ m-10 μ m.
5. the coating of resistance to nuclear radiation according to claim 1, is characterized in that: described inorganic mineral filler is that a kind of or mentioned component in titanium dioxide, barium sulfate, feldspar in powder, mica powder, kaolin, wilkinite, composite iron-titanium powder and talcum powder mixes in any proportion.
6. the coating of resistance to nuclear radiation according to claim 1, is characterized in that: described thinner is that a kind of or mentioned component in acetone, propylene glycol monomethyl ether, propyl carbinol, Virahol and methyl iso-butyl ketone (MIBK) mixes in any proportion.
7. the coating of resistance to nuclear radiation according to claim 1, is characterized in that: described processing aid is that a kind of or mentioned component in defoamer, flow agent, wetting agent and dispersion agent mixes in any proportion.
8. the coating of resistance to nuclear radiation according to claim 7, is characterized in that: described defoamer is that a kind of or mentioned component in German Bi Ke BYK-067A, BYK-085, BYK-A530 and BYK-A535 mixes in any proportion.
9. the coating of resistance to nuclear radiation according to claim 7, is characterized in that: described flow agent is that a kind of or mentioned component in German Bi Ke BYK-350, BYK-358N and BYK-388 mixes in any proportion.
10. the coating of resistance to nuclear radiation according to claim 7, is characterized in that: described wetting agent is that a kind of or mentioned component in German Bi Ke BYK-302, BYK-322, BYK-377 and BYK-333 mixes in any proportion.
11. coating of resistance to nuclear radiation according to claim 7, is characterized in that: described dispersion agent is that a kind of or mentioned component in German Bi Ke BYK-108, BYK-111, BYK-140 and BYK-P105 mixes in any proportion.
12. coating of resistance to nuclear radiation according to claim 1, is characterized in that: described amine hardener is that a kind of or mentioned component in modified fatty amine, aliphatic cyclic amine, aromatic amine, polymeric amide and amido amine mixes in any proportion.
13. coating of resistance to nuclear radiation according to claim 1, is characterized in that: described coupling agent is that a kind of or mentioned component in KH550, KH900, KH560, A-1100, sec.-propyl dioleate oxygen base and azido-silane mixes in any proportion.
14. 1 kinds of preparation methods of the coating of resistance to nuclear radiation as claimed in claim 1, comprise the following steps:
A: take according to the above ratio raw material;
B: under normal temperature and pressure state, epoxy resin, thinner and processing aid are placed in and are disperseed in cylinder, and stir 8-14 minute with 500-1000 rev/min;
C: add inorganic mineral filler in the mixture drawing in b step, stir 15-25 minute with 1000-2000 rev/min under normal temperature and pressure state;
D: check that the compound particles fineness obtaining in c step is to 35-40 μ m, stir and obtain A component for 4-8 minute with 200-500 rev/min;
E: under normal temperature and pressure state, amine curing agent and coupling agent are placed in dispersion cylinder, and with 200-450 rev/min of stirring 5-25 minute, then filter and obtain B component with 100-150 mesh filter screen;
F: A component and B component are obtained to the coating of resistance to nuclear radiation by the even mixing of the mol ratio of 6-8:1.
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| CN103131326B (en) * | 2013-02-22 | 2015-11-25 | 广西标牌化学科技有限公司 | A kind of collocation method of radiation shielding coating |
| CN103483970A (en) * | 2013-09-10 | 2014-01-01 | 常熟市方塔涂料化工有限公司 | Multifunctional epoxy primer and preparation method for same |
| CN104263204A (en) * | 2014-09-12 | 2015-01-07 | 江苏宏盛化学有限公司 | Preparation method for carbon nanotube-epoxy resin radiation-resistant coating for steel-based surface of nuclear power station |
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| CN105400413B (en) * | 2015-12-21 | 2018-07-03 | 中昊北方涂料工业研究设计院有限公司 | Core radiation hardness, anticorrosive coating with rippability and preparation method thereof |
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| CN115873474B (en) * | 2022-12-09 | 2023-11-28 | 中国核动力研究设计院 | Light cover coating material for preventing pollution of wall and ceiling surface Po-210 in nuclear facilities and application |
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