CN114260160B - Pipeline steel-based decoupling wear-resistant super-hydrophobic oleophobic coating and preparation method and application thereof - Google Patents
Pipeline steel-based decoupling wear-resistant super-hydrophobic oleophobic coating and preparation method and application thereof Download PDFInfo
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Abstract
The application discloses a pipeline steel-based decoupling wear-resistant super-hydrophobic oleophobic coating which is decoupling nano SiO 2 Micron SiO 2 The EP coating belongs to the technical field of super-hydrophobic and oleophobic coatings, and has the advantages of excellent super-hydrophobic and oleophobic properties, excellent wear resistance, simple preparation method, easy operation, simple used equipment, extremely low cost, high success rate, no special requirement on the shape of an application matrix sample, and good industrial application prospect.
Description
Technical Field
The application relates to a pipeline steel-based decoupling wear-resistant super-hydrophobic oleophobic coating, and a preparation method and application thereof, and belongs to the technical field of super-hydrophobic oleophobic coatings.
Background
Since the 90 s of the last century, most of oil field exploitation in China enters the middle and later stages, the water content in the produced liquid is continuously increased, and the scaling problems of oil and gas well pipes, ground gathering and conveying system pipelines, equipment and the like are more serious. The existence of the scale can cause pipeline blockage, prevent fluid flow, reduce the transportation capacity of the pipeline, cause a plurality of problems such as energy waste, equipment damage, increase in maintenance cost and the like, is a very common destructive problem in the oil well operation process, and brings great harm and loss to production. Fouling is accompanied by complex physicochemical reactions, which can be divided into two steps: firstly, a solid surface is taken as a substrate to generate crystal nucleus of scale; and secondly, the crystal nucleus grows up to form a scaling layer. According to Young's theory, under the same condition, the smaller the solid surface energy is, the larger the contact angle is, the larger the nucleation work of the crystal on the solid surface is, and the lower the heteronuclear capacity is. Therefore, the contact angle between the oilfield produced liquid and the pipeline is increased, the super-hydrophobicity of the pipeline steel matrix is realized, the scale crystal is prevented from growing by taking the surface of the pipeline steel as a substrate, and the scaling problem of the surface of the scale crystal can be solved.
The research shows that the low wear resistance of the steel-based super-hydrophobic coating is always a problem to be solved in the wide application, and the prior art discloses some wear-resistant super-hydrophobic coatings, but most of used binders, micro-nano particles and the like need to be modified in advance, so that the practical use is not facilitated; in addition, the existing micro-nano coating is a 'coupling' coating, namely the micro-nano particle in the coating has a composite effect, and is only used for realizing super-hydrophobicity and has limited performance.
Disclosure of Invention
In order to solve the problems, the pipeline steel-based decoupling wear-resistant super-hydrophobic oleophobic coating and the preparation method and application thereof are provided, and the coating has excellent super-hydrophobic oleophobic performance and excellent wear-resistant performance, the preparation method is simple and easy to operate, the used equipment is simple, the cost is extremely low, the success rate is high, no special requirement is provided for the shape of an application matrix sample, and the coating has good industrial application prospect.
According to one aspect of the present application, there is provided a pipeline steel-based decoupling abrasion resistant superhydrophobic oleophobic coating that is a decoupling nano SiO 2 Micron SiO 2 -EP coating.
Alternatively, nano SiO 2 The particle diameter of the particles is 25-50nm, and the micron SiO 2 The particle size of the particles is 10-20 mu m, and the epoxy resin EP is epoxy resin E51.
Optionally, the contact angle of the surface of the water-repellent film with water is 158-159 DEG, and the rolling angle of the water drops is less than 4 DEG; and
the contact angle of the surface of the material with oil is 155-156 degrees, the rolling angle of the oil droplets is less than 5 °.
According to another aspect of the application, the preparation method of the pipeline steel-based decoupling wear-resistant super-hydrophobic oleophobic coating is further provided, and comprises the following steps:
(1) Pretreatment of a pipeline steel matrix: polishing the surface of the pipeline steel to be smooth, ultrasonically cleaning and drying for later use;
(2) Preparation of epoxy EP tie layer: mixing epoxy resin and a curing agent, adding a solvent, stirring uniformly, coating the mixture on the surface of pipeline steel, and preserving heat to reach a semi-cured state for later use;
(3) Spraying unmodified silicon dioxide SiO 2 Microparticles: to silica SiO 2 Adding the micron particles into a solvent, uniformly stirring, and spraying the mixture on an epoxy resin bonding layer in a semi-cured state after ultrasonic dispersion to obtain micron SiO 2 -an EP coating;
(4) Spraying low energy modified silicon dioxide SiO 2 Nanoparticles: to silica SiO 2 Adding the nano particles into the mixed solution, uniformly stirring, and spraying the nano particles on the micron SiO after ultrasonic dispersion 2 On the EP coating, cooling after heat preservation to obtain decoupling nano SiO 2 Micron SiO 2 -EP coating.
Preferably, the curing agent is a TAC-900 cycloaliphatic amine curing agent.
Optionally, in the step (1), 400# water abrasive paper, 800# water abrasive paper, 1500# water abrasive paper and 2500# water abrasive paper are sequentially adopted to polish the surface of the pipeline steel to be smooth, absolute ethyl alcohol is used for ultrasonic cleaning for 8-15min, and the pipeline steel is dried for 8-15min at 50-70 ℃ and then sealed for standby.
Optionally, the heat preservation temperature in the step (2) is 60-80 ℃ and the heat preservation time is 20-30min; the weight ratio of the epoxy resin to the curing agent in the step (2) is (1-1.5): 1.
optionally, magnetic stirring is adopted in the step (3), the stirring time is 0.5-1.5h, and the ultrasonic dispersion is carried out for 10-30min.
Alternatively, the solvent in step (2) and step (3) is absolute ethanol, and the mixed solution in step (4) is 1% wt stearic acid absolute ethanol solution.
Optionally, in the step (4), magnetic stirring is adopted, the stirring time is 1.5-3h, the ultrasonic dispersing is carried out for 10-30min, the heat preservation temperature is 60-80 ℃, and the heat preservation time is 4-6h.
Alternatively, the spraying methods in the step (3) and the step (4) are both spraying by adopting an air spray gun at a distance of 10-15cm and a pressure of 0.4 MPa.
Preferably, the preparation method of the pipeline steel-based decoupling wear-resistant super-hydrophobic oleophobic coating comprises the following steps of:
(1) Pretreatment of a pipeline steel matrix: sequentially polishing the pipeline steel sample by using 400# abrasive paper, 800# abrasive paper, 1500# abrasive paper and 2500# abrasive paper until the surface is smooth, then ultrasonically cleaning the steel sample by using absolute ethyl alcohol for 10min, drying the steel sample at the constant temperature of 60 ℃ for 10min, and then placing the steel sample in a sealed sample bag for standby;
(2) Preparation of epoxy EP tie layer: weighing epoxy resin and curing agent in a reaction container, adding absolute ethyl alcohol into the reaction container, stirring uniformly by using a glass rod, coating the mixture on the surface of a steel sample, preserving heat at 60-80 ℃ for 20-30min to reach a semi-cured state, and taking out for later use;
(3) Spraying unmodified silicon dioxide SiO 2 Microparticles: to micron SiO with the grain diameter of 10-20 mu m 2 Adding absolute ethyl alcohol, stirring with magnetic force for 1h, dispersing with ultrasonic for 20min, spraying with air spray gun at a distance of 10-15cm under a pressure of 0.4MPa on the semi-cured epoxy resin adhesive layer to obtain micrometer SiO 2 -an EP coating;
(4) Spraying low energy modified (stearic acid modified) silicon dioxide SiO 2 Nanoparticles: preparing 1% wt stearic acid absolute ethanol solution, adding nano SiO with particle size of 25-50nm 2 Magnetically stirring the mixed solution for 2h, ultrasonically dispersing for 20min, and finally spraying the mixed solution to the micron SiO by adopting an air spray gun under the pressure of 0.4MPa at the distance of 10-15cm 2 On the EP layer, then preserving heat for 4h at 60-80 ℃, cooling at room temperature to obtain decoupling nano SiO 2 Micron SiO 2 -EP coating.
According to still another aspect of the application, the application of the pipeline steel-based decoupling wear-resistant super-hydrophobic oleophobic coating or the pipeline steel-based decoupling wear-resistant super-hydrophobic oleophobic coating prepared by the preparation method in the petroleum pipeline steel scale prevention is also provided.
In this application, "room temperature" refers to 25℃and "coupled" is a conventional term known to those skilled in the art.
Benefits of the present application include, but are not limited to:
1. the steel-based decoupling wear-resistant super-hydrophobic oleophobic coating for the pipeline has a contact angle of 158-159 DEG between the surface and water, and the rolling angle of water drops is smaller than 4 DEG; the contact angle between the surface and oil is 155-156 degrees, and the rolling angle of oil drops is less than 5 degrees, so that the coating has excellent super-hydrophobic and oleophobic properties, and wear-resistant tests also show that the coating has excellent wear-resistant properties, has good anti-scaling capability and is suitable for wide application.
2. According to the preparation method of the pipeline steel-based decoupling wear-resistant super-hydrophobic oleophobic coating, epoxy resin is used as a bonding layer, the highly crosslinked three-dimensional network structure of the coating enables the coating to have excellent wear resistance, and then micron-sized SiO which is not subjected to any modification is subjected to a decoupling mechanism 2 Spraying on the bonding layer without low-energy modification, and then spraying low-energy modified (stearic acid modified) nano SiO 2 Particles, the decoupling wear-resistant super-hydrophobic coating is obtained, the hydrophobicity and the wear resistance are divided into different levels of microstructure dimensions, and the particles pass through an epoxy resin bonding layer and micron SiO 2 The particle has synergistic wear resistance, and the prepared decoupling super-hydrophobic coating has greatly raised wear resistance, so that micron SiO without any modification 2 The particles ensure the wear resistance of the coating, and the nano SiO modified by low energy (stearic acid) 2 The particles can ensure that the coating has excellent superhydrophobicity, can reduce the steps of low-energy modification, and obviously improves the superhydrophobic oleophobic performance and the wear resistance under the conditions of reducing the production cost and simplifying the production steps.
3. According to the preparation method of the pipeline steel-based decoupling wear-resistant super-hydrophobic oleophobic coating, decoupling refers to the step-by-step spraying of micro-nano particles, and the obtained micro-nano particles are not mutually dependent and interacted, but realize different functions of a micro-structure and a nano-structure: the microparticles provide abrasion resistance (no low energy modification is needed), the nanoparticles provide hydrophobicity (only the nanoparticles need to be modified), completely different from the traditional 'coupling' coating, which refers to micro-nano ion recombination and is only used for realizing superhydrophobicity, and in the coupling coating, the microparticles are wrapped by the nanoparticles, the hydrophobic nanoparticles and the firm microparticles wrapped by the hydrophobic nanoparticles are rubbed together during friction, and the hydrophobic durability and abrasion resistance are poor.
The decoupling nano SiO is finally formed by controlling the steps of raw material particle size, step-by-step spraying and the like 2 Micron SiO 2 EP coating, decoupling therefromIn the composite coating, the microparticles are embedded in the adhesive layer, the nanoparticles are coated on the microparticles (as can be seen in conjunction with SEM images of the coating), only a thin layer of nanoparticles on the microparticles is carried away during friction, and the hydrophobicity of the nanoparticles is still effectively maintained because the nanoparticles are not completely removed, and the coating has higher wear resistance (as can be seen in conjunction with friction coefficient images) than the coupling coating.
4. The preparation method of the pipeline steel-based decoupling wear-resistant super-hydrophobic oleophobic coating is simple and easy to operate, the used equipment is simple, the cost is extremely low, the success rate is high, no special requirement is imposed on the shape of the application matrix sample, and the preparation method has a good industrial application prospect.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiments of the application and together with the description serve to explain the application and do not constitute an undue limitation to the application. In the drawings:
FIG. 1 is an unmodified SiO in step (3) in example 1 of the present invention 2 SEM (scanning electron microscope) images of the EP coating surface;
FIG. 2 is an SEM image of the surface of the finally prepared coating 1# in example 1 of the present invention;
FIG. 3 shows the modified micrometer SiO of coating 1# and low energy prepared by the present invention 2 The contact angle and the rolling angle of the coating, namely the comparative coating 4# surface are compared;
FIG. 4 is a graph of the inventive coating 1# and EP coating, modified nano SiO 2 EP coating, homogeneously modified coupled micro-nano SiO 2 Abrasion resistance comparison of EP coating.
Detailed Description
The present application is described in detail below with reference to examples, but the present application is not limited to these examples.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. Reagents or starting materials for use in the invention, e.g. SiO 2 Particles, curing agent, epoxy resin and the like can pass throughThe reagents or starting materials used in the present invention are commercially available in conventional manner, unless otherwise specified, and are used in accordance with the art or according to the product specifications. In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention. The preferred methods and materials described in this patent are illustrative only.
The epoxy resins used in the examples and comparative examples herein were epoxy resin E51, and the curing agents were TAC-900 alicyclic amine curing agents.
Example 1 preparation of coating 1#
The preparation method of the coating No. 1 comprises the following steps:
(1) Pretreatment of a pipeline steel matrix: sequentially polishing the pipeline steel sample by using 400# abrasive paper, 800# abrasive paper, 1500# abrasive paper and 2500# abrasive paper until the surface is smooth, then ultrasonically cleaning the steel sample by using absolute ethyl alcohol for 10min, drying the steel sample at the constant temperature of 60 ℃ for 10min, and then placing the steel sample in a sealed sample bag for standby;
(2) Preparation of epoxy EP tie layer: weighing 6g of epoxy resin and 4g of curing agent in a reaction container, adding 25g of absolute ethyl alcohol into the reaction container, uniformly stirring the mixture by using a glass rod, coating the mixture on the surface of a steel sample, preserving heat at 70 ℃ for 25min to reach a semi-cured state, and taking out for later use;
(3) Spraying unmodified silicon dioxide SiO 2 Microparticles: to 8g of micron SiO with particle size of 15 μm 2 Adding 50mL of absolute ethyl alcohol, stirring for 1h by magnetic force, dispersing for 20min by ultrasonic, spraying on the epoxy resin bonding layer in a semi-cured state by using an air spray gun under the pressure of 0.4MPa at the distance of 12cm to obtain the micron SiO 2 -an EP coating;
(4) Spraying low energy modified (stearic acid modified) silicon dioxide SiO 2 Nanoparticles: 100mL of a 1% wt solution of stearic acid in absolute ethanol was prepared, and 8g of nano SiO having a particle size of 30nm was added thereto 2 Magnetically stirring the mixed solution for 2h, ultrasonically dispersing for 20min, and finally spraying the mixed solution to the micron SiO by adopting an air spray gun under the pressure of 0.4MPa at the distance of 13cm 2 On the EP layer, then preserving heat for 4h at 60-80 ℃, cooling at room temperature to obtain the decoupling nanoMi SiO 2 Micron SiO 2 EP coating # 1.
Example 2 preparation of coating 2#
The preparation method of the coating No. 2 comprises the following steps:
(1) Pretreatment of a pipeline steel matrix: sequentially polishing the pipeline steel sample by using 400# abrasive paper, 800# abrasive paper, 1500# abrasive paper and 2500# abrasive paper until the surface is smooth, then ultrasonically cleaning the steel sample by using absolute ethyl alcohol for 8min, drying the steel sample at the constant temperature of 50 ℃ for 10min, and then placing the steel sample in a sealed sample bag for later use;
(2) Preparation of epoxy EP tie layer: weighing 4g of epoxy resin and 2g of curing agent in a reaction container, adding 20g of absolute ethyl alcohol into the reaction container, uniformly stirring the mixture by using a glass rod, coating the mixture on the surface of a steel sample, preserving heat at 60 ℃ for 20min to reach a semi-cured state, and taking out for later use;
(3) Spraying unmodified silicon dioxide SiO 2 Microparticles: to 6g of micrometer SiO with particle size of 10 μm 2 Adding 50mL of absolute ethyl alcohol, stirring for 1h by magnetic force, dispersing for 20min by ultrasonic, spraying on the semi-cured epoxy resin bonding layer by using an air spray gun at a distance of 10cm under a pressure of 0.4MPa to obtain micron SiO 2 -an EP coating;
(4) Spraying low energy modified (stearic acid modified) silicon dioxide SiO 2 Nanoparticles: 100mL of a 1% wt solution of stearic acid in absolute ethanol was prepared, and 6g of nano SiO having a particle size of 25nm was added thereto 2 Magnetically stirring the mixed solution for 2h, ultrasonically dispersing for 20min, and finally spraying the mixed solution to the micron SiO by adopting an air spray gun at a distance of 10cm and a pressure of 0.4MPa 2 On the EP layer, then preserving heat for 4h at 60 ℃, cooling at room temperature to obtain decoupling nano SiO 2 Micron SiO 2 EP coating # 2.
Example 3 preparation of coating 3#
The preparation method of the coating 3# comprises the following steps:
(1) Pretreatment of a pipeline steel matrix: sequentially polishing the pipeline steel sample by using 400# abrasive paper, 800# abrasive paper, 1500# abrasive paper and 2500# abrasive paper until the surface is smooth, then ultrasonically cleaning the steel sample by using absolute ethyl alcohol for 15min, drying the steel sample at the constant temperature of 60 ℃ for 10min, and then placing the steel sample in a sealed sample bag for later use;
(2) Preparation of epoxy EP tie layer: weighing 8g of epoxy resin and 6g of curing agent in a reaction container, adding 30g of absolute ethyl alcohol into the reaction container, uniformly stirring the mixture by using a glass rod, coating the mixture on the surface of a steel sample, preserving heat at 80 ℃ for 30min to reach a semi-cured state, and taking out for later use;
(3) Spraying unmodified silicon dioxide SiO 2 Microparticles: to 10g of micron SiO with particle size of 20 μm 2 Adding 50mL of absolute ethyl alcohol, stirring for 1h by magnetic force, dispersing for 20min by ultrasonic, spraying on the semi-cured epoxy resin bonding layer by using an air spray gun at a distance of 15cm under a pressure of 0.4MPa to obtain micron SiO 2 -an EP coating;
(4) Spraying low energy modified (stearic acid modified) silicon dioxide SiO 2 Nanoparticles: 100mL of a 1% wt solution of stearic acid in absolute ethanol was prepared, and 10g of nano SiO having a particle size of 50nm was added thereto 2 Magnetically stirring the mixed solution for 2h, ultrasonically dispersing for 20min, and finally spraying the mixed solution to the micron SiO by adopting an air spray gun under the pressure of 0.4MPa at the distance of 15cm 2 On the EP layer, then preserving heat for 6h at 80 ℃, cooling at room temperature to obtain decoupling nano SiO 2 Micron SiO 2 EP coating # 3.
Comparative example 1 preparation of comparative coating 1#
Comparative example 2 preparation of comparative coating 2#
Comparative coating # 2 is modified nano SiO prepared by the prior art 2 -EP coating.
Comparative example 3 preparation of comparative coating 3#
Comparative coating 3# is SiO prepared using the prior art 2 Microparticles and SiO 2 Coupling micro-nano SiO with modified nano particles 2 -EP coating.
Comparative example 4 preparation of comparative coating # 4
The comparative coating 4# is low-energy modified micron SiO prepared by the prior art 2 Coating layer。
Example 4 characterization of Performance
1. Contact angle test experiment
(1) The unmodified micro SiO prepared in step (3) of example 1 was respectively 2 EP coating surface and finally prepared decoupling super-hydrophobic nano SiO 2 Micron SiO 2 SEM testing of the EP coating surface was performed and the results are shown in fig. 1 and 2.
(2) The contact angle and the rolling angle of the water drop, glycerin on the coating 1# surface and the comparative coating 4# surface were measured using a contact angle tester, respectively, and the results are shown in fig. 3.
The results show that, as can be seen from FIG. 1, unmodified micro SiO prepared in the present application 2 The EP coating surface has a plurality of spherical structures of the order of microns; as can be seen from fig. 2, the surface of the micron-sized spherical structure on the surface of the coating 1# prepared in the application is adhered with a nano structure, the nano particles are coated on the micron particles, and the aggregation phenomenon of some nano-sized spherical structures occurs, so that the micro-nano composite structure is presented.
As can be seen from fig. 3, the contact angles of the water drop and the glycerol on the surface of the coating 1# are 158.6 degrees and 155.3 degrees respectively, the rolling angles are 4 degrees and 5 degrees respectively, and the data of the comparative coating 4# are obviously improved.
2. Friction and wear test
After the coating 1# and the comparative coating 1# were respectively worn by a frictional wear tester at a pressure of 10kPa for 300 seconds, the change of the friction coefficient with time was recorded, and the results are shown in fig. 4.
The results show that compared with EP coating, modified nano SiO 2 EP coating, uniformly modified micro-nano SiO 2 The pipeline steel-based decoupling wear-resistant super-hydrophobic oleophobic coating prepared by the method has the advantages of good wear resistance, small fluctuation of friction coefficient along with time curve, small friction coefficient and stable wear resistance, and the decoupling wear-resistant super-hydrophobic oleophobic coating prepared by the method still has a water contact angle of more than 150 degrees and a glycerol contact angle after abrasion, and meanwhile, the rolling angle is less than 5 degrees.
The foregoing is merely exemplary of the present application, and the scope of the present application is not limited to the specific embodiments, but is defined by the claims of the present application. Various modifications and changes may be made to the present application by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the technical ideas and principles of the present application should be included in the protection scope of the present application.
Claims (7)
1. A pipeline steel-based decoupling wear-resistant super-hydrophobic oleophobic coating is characterized by being decoupling nano SiO 2 Micron SiO 2 -an EP coating; nano SiO 2 The particle diameter of the particles is 25-50nm, and the micron SiO 2 The particle diameter of the particles is 10-20 mu m, and the epoxy resin EP is epoxy resin E51;
the preparation method of the pipeline steel-based decoupling wear-resistant super-hydrophobic oleophobic coating comprises the following steps:
(1) Pretreatment of a pipeline steel matrix: polishing the surface of the pipeline steel to be smooth, ultrasonically cleaning and drying for later use;
(2) Preparation of epoxy EP tie layer: mixing epoxy resin and a curing agent, adding a solvent, stirring uniformly, coating the mixture on the surface of pipeline steel, and preserving heat to reach a semi-cured state for later use;
(3) Spraying unmodified silicon dioxide SiO 2 Microparticles: to silica SiO 2 Adding the micron particles into a solvent, uniformly stirring, and spraying the mixture on an epoxy resin bonding layer in a semi-cured state after ultrasonic dispersion to obtain micron SiO 2 -an EP coating;
(4) Spraying low energy modified silicon dioxide SiO 2 Nanoparticles: to silica SiO 2 Adding the nano particles into the mixed solution, uniformly stirring, and spraying the nano particles on the micron SiO after ultrasonic dispersion 2 On the EP coating, cooling after heat preservation to obtain decoupling nano SiO 2 Micron SiO 2 -an EP coating;
wherein the heat preservation temperature in the step (2) is 60-80 ℃ and the heat preservation time is 20-30min; the weight ratio of the epoxy resin to the curing agent in the step (2) is (1-1.5): 1.
2. the coating according to claim 1, wherein the pipeline steel surface is polished smooth by sequentially adopting 400# water abrasive paper, 800# water abrasive paper, 1500# water abrasive paper and 2500# water abrasive paper in the step (1), ultrasonically cleaned by using absolute ethyl alcohol for 8-15min, dried at 50-70 ℃ for 8-15min and sealed for standby.
3. The coating according to claim 1, wherein in step (3) magnetic stirring is used for a period of 0.5-1.5 hours and ultrasonic dispersion is performed for 10-30 minutes.
4. A coating according to claim 3, wherein the solvent in step (2) and step (3) is absolute ethanol and the mixed solution in step (4) is a 1% wt stearic acid absolute ethanol solution.
5. The coating according to claim 4, wherein in the step (4), magnetic stirring is adopted, the stirring time is 1.5-3h, the ultrasonic dispersion is carried out for 10-30min, the heat preservation temperature is 60-80 ℃, and the heat preservation time is 4-6h.
6. The coating according to claim 5, wherein the spraying method in step (3) and step (4) is spraying at a pressure of 0.4MPa at a distance of 10-15cm using an air spray gun.
7. Use of the pipeline steel-based decoupling wear-resistant super-hydrophobic oleophobic coating of claim 1 in petroleum pipeline steel scale control.
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