CN105694658A - High-temperature-resistant graphene/vinyl-based resin anticorrosive coating and preparation method thereof - Google Patents
High-temperature-resistant graphene/vinyl-based resin anticorrosive coating and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of high-temperature acidic flue gas corrosion protection of metal and inorganic building materials, and in particular, relates to a high-temperature-resistant graphene/vinyl-based resin anticorrosive coating and a preparation method thereof. A graphene/vinyl-based resin masterbatch with the graphene content of 10 wt% is added to vinyl-based resin, then a diluent and an auxiliary agent are added and stirred to be uniformly dispersed, and a component A is formed; a component B is a curing agent, and a component C is a curing accelerator. According to the weight percentage, the component A accounts for 52.8-92.7% of, the component B accounts for 3.3-33.0%, and the component C accounts for 3.1-24.7%. In the component A, the content of graphene is in a range of 0.064-4.7 wt%. The graphene/vinyl-based resin anticorrosive coating is prepared by mixing and stirring evenly the three components; after the coating is coated and dried by a conventional method, a corrosion protection coating layer resistant to high-temperature acidic flue gas corrosion can be prepared. Compared with the prior art, the prepared graphene composite coating layer can take high-temperature resistance, acid resistance and HF corrosion resistance into account, and the comprehensive performance of the coating is superior to that of a conventional glass flake composite coating.
Description
Technical field
The present invention relates to metal and inorganic building material high-temperature acidic flue gas corrosion protection field, be specially a kind of anticorrosion of flue duct high temperature resistant Graphene/vinylite anticorrosive paint and preparation method thereof with high temperature resistant flue gas corrosion。
Background technology
In China's energy resource structure, the proportion of coal-fired thermal power generation occupies the ratio of about 70%。Thermal power plant mainly uses high heating value coal-fired, and coal-fired 50% is above bituminous coal, and meager coal takes second place, and anthracite only accounts for less than 1/10th。Coal combustion process produces a large amount of silico-calcium dust, and discharge simultaneously is a large amount of based on sulfur dioxide, contains the sour gas of the compound of fluorine, chlorine, nitrogen element simultaneously。Each equipment of power plant, under high temperature and water vapour environment, is produced huge chemical attack and physical abrasion by these dust and gas。When discharging for a long time, flue and chimney are produced huge corrosion pressure。Power plant to some waste incineration and generating electricities, producing will HCl, HF, SO in the process of electric power2、NOx, CO etc. be blended in high-temperature flue gas, meet with water in air vapour phase, produce the erosions such as hydrochloric acid, sulphuric acid, nitric acid, Fluohydric acid., bring serious etching problem also can to metal flue and chimney。So, stop above-mentioned high-temperature acidic flue gas that the corrosion of metal flue and chimney has been become critical technical problem。
At present, the corrosion-inhibiting coating of flue and chimney is divided into alloy lining, composite foam glass brick lining, steel bushing inwall to paste the modes such as acid-resistant paint and clay, polyethylene anticorrosion coating, polyurethane anticorrosion coating such as foam glass, polyureas, heatproof vinyl glass flake。First three class all involves great expense, and market acceptance is very low。The current domestic rare running example of polyureas, and polyethylene and polyurethane anticorrosion coating all to there is use temperature all low, when maintenance or during stoppage in transit desulfurizer (FGD), the discharge of bypass high-temperature flue gas can burn coating。So, it is that market is most widely used that current vinyl glass-flake coating and clay are coated with。
Flue gas, after FGD purifies, usually contain a small amount of Fluohydric acid., although amount seldom, but great strong exfoliation corrosion, also very strong to coating under for a long time。At present, it mostly is vinyl glass-flake coating or vinyl glass flake plasticine is in the majority at the corrosion-inhibiting coating of the power plant's flue built with built operation and chimney。The defect that this series products exists is mainly reflected in coating hardness height, and the performance of hydrofluoric acid corrosion resistance is not good。Fluohydric acid. can react with the glass flake in coating faster, generates SiF4Loosening layer。Meanwhile, Silicon fluoride. can continue with Fluohydric acid. to react into the acid hexafluosilicic acid worked as with sulfuric acid phase, thus steel body is produced corrosion。
Concrete chemical reaction is: SiO2+ 4HF=SiF4+2H2O
SiF4+ 2HF=H2SiF6
Meanwhile, the pliability of vinyl glass flake coatings is slightly worse, and hardness is high。In fume emission process, steel structure high structure chimney can produce certain vibrations。When equipment swings and trembles, the directivity changed due to power and pressure is inconsistent, it is possible to causes that coating produces gap and crackle, peeling-off separation with equipment body, loses protective effect。
Summary of the invention
In order to overcome, the vinyl resistance to HF of glass flake corrosion-inhibiting coating is not good, pliability is poor, the problem such as wear no resistance, it is an object of the invention to provide a kind of high temperature resistant Graphene/vinylite anticorrosive paint and preparation method thereof, the vinyl composite coating that glass flake is filler is substituted with graphene nanometer sheet, anticorrosion for flue and chimney, can taking into account the corrosion of HF high temperature resistant, acidproof, resistance to, the combination property of coating is substantially better than Conventional glass scale composite coating simultaneously。
The technical scheme is that
A kind of high temperature resistant Graphene/vinylite anticorrosive paint, this coating is A, B, C tri-component-type, wherein: component A comprises vinylite, Graphene/vinylite masterbatch, diluent, additive, and B component is firming agent, and component C is curing accelerator；With vinylite amount for 100 parts of weighing scales, the weight of each component consists of:
Component A:
B component:
1～60 part of firming agent；
Component C:
Curing accelerator 1～40 part。
Described high temperature resistant Graphene/vinylite anticorrosive paint, by weight percentage, component A accounts for 52.8～99.2%, and B component accounts for 0.33～34.7%, and component C accounts for 0.32～26.1%；In component A, the content range of Graphene is 0.064～4.7wt%。
Described high temperature resistant Graphene/vinylite anticorrosive paint, in component A, Graphene/vinylite masterbatch is Graphene content at the Graphene of 10wt% and vinylite masterbatch composite resin slurry。
Described high temperature resistant Graphene/vinylite anticorrosive paint, in component A, vinylite is phenol aldehyde type vinylite；Additive is the auxiliary agent that paint field is conventional: one or more mixing of dispersant, defoamer, levelling agent and anti-settling agent, the respective parts by weight of dispersant, defoamer, levelling agent and anti-settling agent are 0.1～2 part；Diluent adopts organic solvent: one or more mixing in toluene, dimethylbenzene, ethanol, propanol, butanol, butanone, Ketohexamethylene。
Described high temperature resistant Graphene/vinylite anticorrosive paint, B component is firming agent, including one or more the mixture in methyl ethyl ketone peroxide, isopropyl benzene hydroperoxide, benzoyl peroxide, dibenzoyl peroxide。
Described high temperature resistant Graphene/vinylite anticorrosive paint, component C is curing accelerator, including cobalt naphthenate, naphthoic acid cobalt, cobalt iso-octoate, one or more the mixture in DMA, diethylaniline。
The preparation method of described high temperature resistant Graphene/vinylite anticorrosive paint, in agitator, add vinylite, Graphene/vinylite masterbatch, diluent and additive according to formula proportion at the uniform velocity to stir, rotating speed is 500～800 revs/min, stirs 1～10 hour, makes the uniform subpackage of various mixing of materials can obtain component A；A, B, C tri-after component mixes in proportion, can be used。
The preparation method of described high temperature resistant Graphene/vinylite anticorrosive paint, Graphene/vinylite masterbatch refers to the Graphene content composite resin slurry at 10wt%。
The preparation method of described high temperature resistant Graphene/vinylite anticorrosive paint, the preparation method of Graphene/vinylite masterbatch is:
Dry nano-sized carbon powder body is joined stirring in alcoholic solvent and makes its complete wetting, utilize ultrasonic, high-speed stirred or shearing dispersion to process and form it into nano-sized carbon/alcohol suspension；Nano-sized carbon/alcohol suspension is added and stir in liquid liquid vinylite to alcoholic solution and resin layering, its be at the middle and upper levels milky to canescence low viscosity alcoholic solution, lower floor is black high-viscosity material；After upper strata alcoholic solution and lower floor's feed separation, collect lower floor's material；The material collected being heated evacuation dried, namely obtain the dispersed composite resin slurry having nano-sized carbon, the upper strata alcoholic solution of collection is reused after utilizing the Methods For Purification distilled。
The preparation method of described high temperature resistant Graphene/vinylite anticorrosive paint, joins in 30kg hexanol by graphene powder prepared by 1000g intercalation stripping method, ultrasonic disperse 30 minutes, can obtain the scattered Graphene of transient state/alcohol suspension；Mechanical agitation 5 hours after being mixed with 10kg vinylite by above-mentioned suspension, mixing speed is 200 revs/min；Stirring stands 10 minutes after terminating, and makes above-mentioned mixing liquid layered；Being poured out by linen for upper strata solution, leave the viscous paste of lower black, insert evacuation in vacuum drying oven and heat to 120 DEG C, in maintenance baking oven, vacuum is lower than 100Pa；Take out after drying 24 hours and namely obtain Graphene content and be about the Graphene/vinylite composite master batch of 10wt%。
The design principle of the present invention is:
Graphene has high chemical stability and heat stability, it is possible to long-time stable work in 600 DEG C of air；Graphene nanometer sheet has the lamellar structure thinner than Conventional glass scale and bigger sheet footpath/thickness ratio simultaneously。Under unit thickness, Graphene can form the protection of the antiseepage isolation of more number of plies in the coating than glass flake。Infiltration in corrosive medium graphene-containing composite coating after hardening, the path of process extends ratio much larger than glass flake, is equivalent to effectively increase the thickness of corrosion-resistant coating。Select the graphene nanometer sheet of flexibility as filler simultaneously, the glass flake of relative brittleness, toughness and the self lubricity of coating can be effectively improved, dither and fretting wear that swiftly flowing flue gas brings can be resisted, thus giving the high-temperature corrosion resistance protective benefits that Graphene/vinylite composite coating is long-acting。
Beneficial effects of the present invention is as follows:
1, dope preparing process of the present invention only needs simple stirring, Graphene high-quality dispersion in coating can be realized so that the preparation process of Graphene composite coating and technique simplify。
2, Graphene prepared by the present invention/vinylite coating has the high temperature resistant flue gas corrosion performance of excellence, and the Graphene addition needed can be down to 1wt%, far below conventional ethylene base glass-flake coating。
3, Graphene prepared by the present invention/vinylite coating, has good pliability and shock resistance。
Accompanying drawing explanation
Fig. 1. embodiment 1 Graphene/vinylite composite coating and certain commercially available vinyl glass flake composite coating are heat-resisting soak with sulphuric acid (80 DEG C, 30wt%, 60 days) test after surface topography contrast: (a) commercially available vinyl glass flake composite coating, (b) Graphene/vinylite composite coating。
Fig. 2. embodiment 1 Graphene/vinylite composite coating and certain commercially available vinyl glass flake composite coating are heat-resisting nitric acid dousing (80 DEG C, 15wt%, 60 days) test after surface topography contrast: (a) commercially available vinyl glass flake composite coating, (b) Graphene/vinylite composite coating。
Fig. 3. embodiment 1 Graphene/vinylite composite coating and certain commercially available vinyl glass flake composite coating are heat-resisting hydrofluoric acid dips (60 DEG C, 10wt%, 60 days) surface topography contrast after test: (a) commercially available vinyl glass flake composite coating (soaks 8 days later pattern), (b) Graphene/vinylite composite coating。
Detailed description of the invention
In a specific embodiment, it is A, B, C tri-component-type that the present invention has the Graphene/vinylite composite anticorrosion coating of high temperature resistant flue gas corrosion, wherein: component A comprises vinylite, Graphene/vinylite masterbatch, diluent, additive, B component is firming agent, and component C is curing accelerator。Weight composition (with vinylite amount for 100 parts of weighing scales) of each component is:
Component A:
B component:
1～60 part of firming agent；
Component C:
Curing accelerator 1～40 part。
In component A, vinylite is mainly phenol aldehyde type vinylite, its trade mark such as FUCHEM898HT, SWANCOR900,907,977 series etc.。Additive is the auxiliary agent that paint field is conventional, adopts one or more mixing of commercial dispersants, defoamer, levelling agent and anti-settling agent。Preferably, the respective parts by weight of dispersant, defoamer, levelling agent and anti-settling agent are 0.1～2 part。Diluent adopts organic solvent: one or more mixing in toluene, dimethylbenzene, ethanol, propanol, butanol, butanone, Ketohexamethylene。
In component A, 10wt% Graphene/vinylite masterbatch refers to Chinese invention patent application: " preparation method (application number 201410617460.9) of a kind of nano-sized carbon/liquid resin masterbatch "。Graphene/liquid resin masterbatch refers to the Graphene content composite resin slurry at more than 5wt%, Graphene is dispersed wherein, and the composite resin of low concentration can be diluted into, and after dilution, the dispersity of Graphene is constant, this masterbatch dispersive property when application is good。Grapheme material can realize the dispersion of transient state in lower alcohol solvent, and lower alcohol solvent is also liquid resinous poor solvent simultaneously, and resin dissolubility wherein is very low。But resin dissolving of trace in alcohol makes it can form good combination with Graphene, makes the interaction force between Graphene and resin strengthen gradually。Macroscopically show as Graphene to transfer in resin from alcoholic solution gradually, and formed dispersed。After transferring in resin in Graphene is completely by alcohol, under static conditions, alcoholic solution will be layered with resin。Owing to the adhesion between alcoholic solution and resin is very weak, it is possible to by the processing method of thermal evaporation so that it is be kept completely separate with resin。
B component is firming agent, one or more the mixture in including methyl ethyl ketone peroxide, isopropyl benzene hydroperoxide, benzoyl peroxide, dibenzoyl peroxide etc.。
Component C is curing accelerator, one or more the mixture in including cobalt naphthenate, naphthoic acid cobalt, cobalt iso-octoate, DMA, diethylaniline etc.。
The preparation process of anticorrosive paint of the present invention is as follows:
Adding vinylite, Graphene/vinylite masterbatch, diluent and additive in agitator according to formula proportion at the uniform velocity to stir, rotating speed is 500～800 revs/min, stirs 1～10 hour, makes the uniform subpackage of various mixing of materials can obtain component A；A, B, C tri-after component mixes in proportion, can be used。By weight percentage, component A accounts for 52.8～99.2%, and B component accounts for 0.33～34.7%, and component C accounts for 0.32～26.1%；In component A, the content range of Graphene is 0.064～4.7wt% (being preferably 1～3wt%)。Apply dried according to a conventional method, the corrosion protective coating with high temperature resistant acidic flue gas corrosion can be prepared。
Below, by embodiment, the present invention is described in more detail。
Embodiment 1
Graphene powder prepared by 1000g intercalation stripping method is joined in 30kg hexanol, ultrasonic disperse 30 minutes, the scattered Graphene of transient state/alcohol suspension can be obtained；Mechanical agitation 5 hours after being mixed with 10kg vinylite by above-mentioned suspension, mixing speed is 200 revs/min；Stirring stands 10 minutes after terminating, and makes above-mentioned mixing liquid layered；Being poured out by linen for upper strata solution, leave the viscous paste of lower black, insert evacuation in vacuum drying oven and heat to 120 DEG C, in maintenance baking oven, vacuum is lower than 100Pa；Take out after drying 24 hours and namely obtain Graphene content and be about the Graphene/vinylite composite master batch of 10wt%。
Counting by weight, the raw material of composite anticorrosion coating is composed as follows:
The composition of component A is:
Vinylite 100 parts；
10wt% Graphene/vinylite masterbatch 40 parts；
Solvent includes following component and ratio:
Toluene 10 parts；
Ethanol 15 parts；
N-butyl alcohol 5 parts；
Additive includes following component and ratio:
Defoamer 0.2 part；
Levelling agent 0.5 part；
Anti-settling agent 1 part；
The composition of component B is:
Methyl ethyl ketone peroxide 2.5 parts；
Benzoyl peroxide 0.5 part；
The composition of component C is:
Cobalt naphthenate 2 parts。
In the present embodiment, the preparation process of anticorrosive paint is as follows:
(1) the component A raw material of the above-mentioned weight ratio of Homogeneous phase mixing, speed of agitator is 600 revs/min, and mixing time is 2 hours；
(2) the component B raw material of the above-mentioned weight ratio of Homogeneous phase mixing；
(3) step can be used after tri-component proportionally mixing and stirring of A, B, C。
(4) in above-mentioned coating, the content of Graphene is about 1.9wt%, utilizes spread coating to be coated in carbon steel test piece by mixed paint brush and makes coating test corrosion protection。The performance comparison of gained performance indications and certain commercially available vinyl glass-flake coating is reported as follows table:
Embodiment 2
Difference from Example 1 is in that:
Counting by weight, the composition of component A is:
Vinylite 100 parts；
10wt% Graphene/vinylite masterbatch 20 parts；
Solvent includes following component and ratio:
Dimethylbenzene 10 parts；
Ethanol 25 parts；
Additive includes following component and ratio:
Defoamer 0.5 part；
Levelling agent 0.5 part；
Anti-settling agent 0.5 part；
The composition of component B is:
Isopropyl benzene hydroperoxide 3 parts；
The composition of component C is:
Ring cobalt octoate 1 part；
Diethylaniline 1 part。
In the present embodiment, the preparation process of anticorrosive paint is as follows:
(1) the component A raw material of the above-mentioned weight ratio of Homogeneous phase mixing, speed of agitator is 800 revs/min, and mixing time is 5 hours；
(2) the component C raw material of the above-mentioned weight ratio of Homogeneous phase mixing；
(3) step can be used after tri-component proportionally mixing and stirring of A, B, C。
(4) in above-mentioned coating, the content of Graphene is about 1.0wt%, utilizes spread coating to be coated in carbon steel test piece by mixed paint brush and makes coating test corrosion protection。The performance comparison of gained performance indications and certain commercially available vinyl glass-flake coating is reported as follows table:
Embodiment is it is shown that the obtained Graphene composite coating of the present invention is obtained with the conventional heat refractory antiseptic property suitable with 25wt% glass flake addition when Graphene addition is only 1.6wt%。As Figure 1-3, coating to be especially much better than conventional ethylene base glass flake coatings at hydrofluoric acid corrosion resistance aspect of performance in acid resistance, and the adhesive force of coating and resistance to impact all relatively vinyl glass flake coatings increases。Illustrating, the present invention obtained vinyl Graphene composite coating combination property in high-temperature flue anticorrosion is better than existing vinyl glass flake composite coating。
Claims (10)
1. high temperature resistant Graphene/vinylite anticorrosive paint, it is characterized in that, this coating is A, B, C tri-component-type, wherein: component A comprises vinylite, Graphene/vinylite masterbatch, diluent, additive, B component is firming agent, and component C is curing accelerator；With vinylite amount for 100 parts of weighing scales, the weight of each component consists of:
Component A:
B component:
1～60 part of firming agent；
Component C:
Curing accelerator 1～40 part。
2. the high temperature resistant Graphene/vinylite anticorrosive paint described in claim 1, it is characterised in that by weight percentage, component A accounts for 52.8～99.2%, and B component accounts for 0.33～34.7%, and component C accounts for 0.32～26.1%；In component A, the content range of Graphene is 0.064～4.7wt%。
3. the high temperature resistant Graphene/vinylite anticorrosive paint described in claim 1, it is characterised in that in component A, Graphene/vinylite masterbatch is Graphene content at the Graphene of 10wt% and vinylite masterbatch composite resin slurry。
4. the high temperature resistant Graphene/vinylite anticorrosive paint described in claim 1, it is characterised in that in component A, vinylite is phenol aldehyde type vinylite；Additive is the auxiliary agent that paint field is conventional: one or more mixing of dispersant, defoamer, levelling agent and anti-settling agent, the respective parts by weight of dispersant, defoamer, levelling agent and anti-settling agent are 0.1～2 part；Diluent adopts organic solvent: one or more mixing in toluene, dimethylbenzene, ethanol, propanol, butanol, butanone, Ketohexamethylene。
5. the high temperature resistant Graphene/vinylite anticorrosive paint described in claim 1, it is characterized in that, B component is firming agent, including one or more the mixture in methyl ethyl ketone peroxide, isopropyl benzene hydroperoxide, benzoyl peroxide, dibenzoyl peroxide。
6. the high temperature resistant Graphene/vinylite anticorrosive paint described in claim 1, it is characterized in that, component C is curing accelerator, including cobalt naphthenate, naphthoic acid cobalt, cobalt iso-octoate, one or more mixture in DMA, diethylaniline。
7. the preparation method of the high temperature resistant Graphene/vinylite anticorrosive paint described in a claim 1, it is characterized in that, in agitator, add vinylite, Graphene/vinylite masterbatch, diluent and additive according to formula proportion at the uniform velocity to stir, rotating speed is 500～800 revs/min, stirs 1～10 hour, makes the uniform subpackage of various mixing of materials can obtain component A；A, B, C tri-after component mixes in proportion, can be used。
8. the preparation method of the high temperature resistant Graphene/vinylite anticorrosive paint described in claim 7, it is characterised in that Graphene/vinylite masterbatch refers to the Graphene content composite resin slurry at 10wt%。
9. the preparation method of the high temperature resistant Graphene/vinylite anticorrosive paint described in claim 7 or 8, it is characterised in that the preparation method of Graphene/vinylite masterbatch is:
Dry nano-sized carbon powder body is joined stirring in alcoholic solvent and makes its complete wetting, utilize ultrasonic, high-speed stirred or shearing dispersion to process and form it into nano-sized carbon/alcohol suspension；Nano-sized carbon/alcohol suspension is added and stir in liquid liquid vinylite to alcoholic solution and resin layering, its be at the middle and upper levels milky to canescence low viscosity alcoholic solution, lower floor is black high-viscosity material；After upper strata alcoholic solution and lower floor's feed separation, collect lower floor's material；The material collected being heated evacuation dried, namely obtain the dispersed composite resin slurry having nano-sized carbon, the upper strata alcoholic solution of collection is reused after utilizing the Methods For Purification distilled。
10. the preparation method of the high temperature resistant Graphene/vinylite anticorrosive paint described in claim 7 or 8, it is characterized in that, graphene powder prepared by 1000g intercalation stripping method is joined in 30kg hexanol, ultrasonic disperse 30 minutes, the scattered Graphene of transient state/alcohol suspension can be obtained；Mechanical agitation 5 hours after being mixed with 10kg vinylite by above-mentioned suspension, mixing speed is 200 revs/min；Stirring stands 10 minutes after terminating, and makes above-mentioned mixing liquid layered；Being poured out by linen for upper strata solution, leave the viscous paste of lower black, insert evacuation in vacuum drying oven and heat to 120 DEG C, in maintenance baking oven, vacuum is lower than 100Pa；Take out after drying 24 hours and namely obtain Graphene content and be about the Graphene/vinylite composite master batch of 10wt%。
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| CN106178618A (en) * | 2016-09-09 | 2016-12-07 | 成都九十度工业产品设计有限公司 | A kind of precipitation still for processing Metallurgical Waste Water |
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| CN107057532A (en) * | 2017-02-17 | 2017-08-18 | 德阳烯碳科技有限公司 | A kind of graphene compound ethylene base ester anticorrosive paint and preparation method thereof |
| CN110358413A (en) * | 2019-06-27 | 2019-10-22 | 新疆同业盛远工程技术有限公司 | Graphene fire resistant anticorrosive conductive ethylene base ester cold coating and preparation method |
| CN110305567A (en) * | 2019-06-29 | 2019-10-08 | 新疆同业盛远工程技术有限公司 | A kind of graphene oxide flake anticorrosive paint and preparation method |
| WO2023279763A1 (en) * | 2022-01-05 | 2023-01-12 | 方亨 | Method for improving corrosion resistance of vinyl resin |
| US11692103B1 (en) * | 2022-01-05 | 2023-07-04 | Guangdong Meiheng New Material Technology Co., Ltd | Method for improving corrosion resistance of vinyl ester resin |
| GB2614963A (en) * | 2022-01-05 | 2023-07-26 | Guangdong Meiheng New Material Tech Co Ltd | Method for improving corrosion resistance of vinyl resin |
| GB2614963B (en) * | 2022-01-05 | 2024-02-14 | Guangdong Meiheng New Material Tech Co Ltd | Method for improving corrosion resistance of vinyl ester resin |
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