CN115491097B - Anticorrosive paint and preparation method thereof - Google Patents
Anticorrosive paint and preparation method thereof Download PDFInfo
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- CN115491097B CN115491097B CN202110680680.6A CN202110680680A CN115491097B CN 115491097 B CN115491097 B CN 115491097B CN 202110680680 A CN202110680680 A CN 202110680680A CN 115491097 B CN115491097 B CN 115491097B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5046—Amines heterocyclic
- C08G59/5053—Amines heterocyclic containing only nitrogen as a heteroatom
- C08G59/5073—Amines heterocyclic containing only nitrogen as a heteroatom having two nitrogen atoms in the ring
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
- C09D5/10—Anti-corrosive paints containing metal dust
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0856—Iron
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
- C08K2003/0881—Titanium
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Abstract
The application discloses an anticorrosive paint and a preparation method thereof, wherein the anticorrosive paint comprises the following components in parts by weight: 1 part of phenolic aldehyde modified epoxy resin and 0.15 to 0.25 part of modified curing agent. Wherein, the structural formula of the modified curing agent is as follows:
Description
Technical Field
The application relates to the technical field of corrosion prevention, in particular to an anticorrosive paint and a preparation method thereof.
Background
The oil and gas field part oil pipe, single well pipeline, gathering pipeline caliber is little, and delivery pressure is big, and operating temperature is high, and the medium corrosivity is strong, and the anticorrosion degree is big, and conventional coating protection effect is not ideal. The cost of adopting the corrosion-resistant alloy and the nonmetallic pipeline is high, the operation and maintenance of adding the corrosion inhibitor are difficult, and the corrosion inhibitor needs to be frequently adjusted and replaced along with the component change of the produced liquid. Statistics of the related data show that 90% of the total corrosion perforation amount of the oil field site pipeline is from the corrosion of the inner wall. Part of pipelines run for 1-3 years, namely corrosion perforation, running, overflowing, dripping and the like, perforation, puncture and leakage occur for more than 600 times a year on a certain oilfield gathering pipeline, the safe operation of oilfield production is seriously influenced, large economic loss is caused, and hidden danger in the aspect of safety and environmental protection is brought.
Content of the application
The application provides an anticorrosive paint and a preparation method thereof, which can avoid internal corrosion caused by poor temperature resistance and permeability resistance of a conventional coating in high-temperature high-pressure and corrosion-serious environments such as a single well pipeline and a gathering pipeline of an oil-gas field at present.
The application adopts the following technical scheme:
in a first aspect, the present application provides an anticorrosive coating comprising the following components in parts by weight: 1 part of phenolic aldehyde modified epoxy resin and 0.15 to 0.25 part of modified curing agent. Wherein, the structural formula of the modified curing agent is as follows:
wherein, phenolic aldehyde modified epoxy resin (such as NPES-303L) is used as a coating base resin, and too little is added to form infiltration on filler in the curing process, thereby affecting the coating performance, and too much is added to have adverse effects of high coating cost, poor coating mechanical property and the like.
The modified curing agent is used as the curing agent of the coating, so that the coating can be cured at a lower temperature, and the temperature resistance and ageing resistance of the coating are obviously improved due to the introduction of titanium in the curing agent. Too little epoxy resin is added to react completely and too much is added to affect the basic properties of the coating.
Further, the anticorrosive paint also comprises the following components in parts by weight: 0.01 to 0.02 portion of graphene, 0.1 to 0.2 portion of composite ferrotitanium powder, 0.1 to 0.2 portion of mica powder, 0.1 to 0.2 portion of barium sulfate, 0.01 to 0.03 portion of flatting agent and 0.01 to 0.03 portion of benzoin.
Wherein, graphene can improve the permeation resistance, salt fog resistance and wear resistance of the coating. Too little addition does not play a role in improving the coating, and too much addition has the adverse effects of high cost, influence on the coating performance and the like.
The composite ferrotitanium powder as inorganic filler plays a role of reinforcing agent in the coating. Too little addition has the effect of not improving the coating performance, and too much addition affects the coating performance.
The mica powder can improve the water resistance and compactness of the coating. Too little addition has the effect of not improving the water resistance and compactness of the coating, and too much addition affects the basic performance of the coating.
Barium sulfate can improve the hardness and impact resistance of the coating. Too little addition does not improve the hardness and impact resistance of the coating, and too much addition is poor in the performance of the coating.
Further, the preparation method of the 2-methylimidazole titanium complex modified curing agent comprises the following steps: adding 2-methyl-imidazole and an organic solvent into a reaction kettle, so that the 2-methyl-imidazole is dissolved in the organic solvent. Adding Ti (SO) into a reaction kettle 4 ) 2 And (3) chelating 2-methylimidazole and titanium sulfate with NaOH, cooling, filtering, washing with water, and drying to obtain the modified curing agent. The modified curing agent is light yellow.
Further, the organic solvent includes n-butanol corresponding to 400ml of n-butanol per 0.1 mole of 2-methyl-imidazole.
Further, 2-methyl-imidazole and Ti (SO 4 ) 2 The molar ratio of (1) is (0.8-1.0) to (0.2-0.4). Preferably, 2-methyl-imidazole and Ti (SO 4 ) 2 The molar ratio of (2) is 0.9:0.3. The 2-methyl-imidazole is not fully chelated, and the too little chelation is not fully chelated.
Further, the molar ratio of the 2-methyl-imidazole to the NaOH is (0.8-1.0): 0.1-0.2. Preferably, the molar ratio of 2-methyl-imidazole to NaOH is 0.9:0.15. Too much NaOH has low chelation yield, and too little chelation reaction has low yield.
Further, the dissolution temperature is 40-60 ℃, the stirring speed of dissolution is 40-70 rpm, and the dissolution time is 3-5 min.
Further, the temperature of the chelation reaction is 100-120 ℃, and the time of the chelation reaction is 4-6 h. Preferably, the temperature of the chelation reaction is 110 ℃.
Further, the drying temperature is 50-70 ℃, and the drying time is 2-3 h.
Further, the drying mode is drying by heating through an oven.
In a second aspect, the present application provides a method for preparing the anticorrosive paint described above, comprising the steps of: premixing phenolic aldehyde modified epoxy resin and a modified curing agent to obtain a premix. And adding the premix into a screw extruder for melting, rolling into slices, cooling and crushing to obtain the anticorrosive coating.
Further, the graphene, the composite ferrotitanium powder, the mica powder, the barium sulfate, the leveling agent and the benzoin are premixed with the phenolic aldehyde modified epoxy resin and the modified curing agent.
Further, the premixing mode is to use a high-speed mixer for premixing.
Further, the stirring speed of the premixing is 400-600 rpm, and the time is 5-10 min.
Further, the temperature of the feeding section of the screw extruder is 60-80 ℃, and the temperature of the extrusion section is 100-110 ℃.
Further, the thickness of the sheet was 1mm.
Further, the crushing mode is crushing by a crusher.
In a third aspect, the present application provides the use of the anticorrosive coating described above to form an anticorrosive coating on a carbon steel substrate.
In a fourth aspect, the present application provides an anticorrosive coating sprayed from the anticorrosive coating described above, cured by heating.
Compared with the prior art, the application has the following beneficial effects:
crude oil (100deg.C, 90 d), 10% HCl (100deg.C, 90 d), 10% NaCl (100deg.C, 90 d), 10% H were used to make the anticorrosive coatings and conventional coatings of the present application 2 SO 4 (100 ℃ C., 90 d) performance test, the results are shown in the following table.
From the data in the above table, the chemical medium resistance and the crude oil resistance of the anticorrosive paint are far higher than those of the conventional paint.
Detailed description of the preferred embodiments
The technical methods in the embodiments of the present application will be clearly and completely described below. It will be apparent that the described embodiments are only some, but not all, of the embodiments of the present application. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments herein without making any inventive effort, are intended to be within the scope of the present application.
Phenolic-modified epoxy resin, 2-methylimidazole, graphene, composite ferrotitanium powder, mica powder, barium sulfate, leveling agent, benzoin, n-butanol, naOH, ti (SO) 4 ) 2 All purchased from Tianjin, jiang Tian chemical technology Co., ltd.
Example 1
S1, preparing a modified curing agent.
S101, adding 0.1mol of 2-methyl-imidazole and 400ml of n-butanol into a reaction kettle, heating to 60 ℃, and stirring for 3min at the rotating speed of 70 r/min to obtain a 2-methyl-imidazole solution.
S102, ti (SO) 4 ) 2 NaOH is added into 2-methyl-imidazole solution in a reaction kettle, and the 2-methyl-imidazole and Ti (SO 4 ) 2 Is heated to 120 ℃ for 6 hours to react the 2-methyl-imidazole and the Ti (SO 4 ) 2 And (3) carrying out chelation reaction to obtain a chelation reaction product.
And S103, cooling the chelate reaction product, filtering, washing with water, heating to 70 ℃ in an oven, and drying for 3 hours to obtain the modified curing agent.
S2, adding 1 part of phenolic aldehyde modified epoxy resin, 0.25 part of modified curing agent, 0.02 part of graphene, 0.2 part of composite ferrotitanium powder, 0.2 part of mica powder, 0.2 part of barium sulfate, 0.03 part of flatting agent and 0.03 part of benzoin into a high-speed mixer for premixing for 10min according to each 1000g, and stirring at 600rpm to obtain a premix.
S3, taking out the premix from the high-speed mixer, putting the premix into a screw extruder for heating and melting, controlling the temperature of a feeding section to be 80 ℃, controlling the temperature of an extrusion section to be 110 ℃, rolling the premix into a sheet with the thickness of 1mm, cooling, and putting the sheet into a pulverizer for pulverizing to obtain the anticorrosive coating.
Example 2
S1, preparing a modified curing agent.
S101, adding 0.1mol of 2-methyl-imidazole and 400ml of n-butanol into a reaction kettle, heating to 50 ℃, and stirring for 4min at the rotating speed of 60 revolutions per minute to obtain a 2-methyl-imidazole solution.
S102, ti (SO) 4 ) 2 NaOH is added into 2-methyl-imidazole solution in a reaction kettle, and the 2-methyl-imidazole and Ti (SO 4 ) 2 Is heated to 100 ℃ for 4 hours to react the 2-methyl-imidazole and the Ti (SO 4 ) 2 And (3) carrying out chelation reaction to obtain a chelation reaction product.
And S103, cooling the chelate reaction product, filtering, washing with water, heating to 50 ℃ in an oven, and drying for 2 hours to obtain the modified curing agent.
S2, adding 1 part of phenolic aldehyde modified epoxy resin, 0.15 part of modified curing agent, 0.01 part of graphene, 0.1 part of composite ferrotitanium powder, 0.1 part of mica powder, 0.1 part of barium sulfate, 0.01 part of flatting agent and 0.01 part of benzoin into a high-speed mixer for premixing for 5min according to each 1000g, and stirring at a rotation speed of 400rpm to obtain a premix.
S3, taking out the premix from the high-speed mixer, putting the premix into a screw extruder for heating and melting, controlling the temperature of a feeding section to be 60 ℃, controlling the temperature of an extrusion section to be 100 ℃, rolling the premix into a sheet with the thickness of 1mm, cooling, and putting the sheet into a pulverizer for pulverizing to obtain the anticorrosive coating.
Example 3
S1, preparing a modified curing agent.
S101, adding 0.1mol of 2-methyl-imidazole and 400ml of n-butanol into a reaction kettle, heating to 50 ℃, and stirring for 4min at the rotating speed of 60 revolutions per minute to obtain a 2-methyl-imidazole solution.
S102, ti (SO) 4 ) 2 NaOH is added into 2-methyl-imidazole solution in a reaction kettle, and the 2-methyl-imidazole and Ti (SO 4 ) 2 Is heated to 100 ℃ for 4 hours to react the 2-methyl-imidazole and the Ti (SO 4 ) 2 And (3) carrying out chelation reaction to obtain a chelation reaction product.
And S103, cooling the chelate reaction product, filtering, washing with water, heating to 50 ℃ in an oven, and drying for 2 hours to obtain the modified curing agent.
S2, adding 1 part of phenolic aldehyde modified epoxy resin, 0.2 part of modified curing agent, 0.015 part of graphene, 0.15 part of composite ferrotitanium powder, 0.15 part of mica powder, 0.15 part of barium sulfate, 0.02 part of flatting agent and 0.02 part of benzoin into a high-speed mixer for premixing for 8min according to each 1000g, and stirring at a rotation speed of 500rpm to obtain a premix.
S3, taking out the premix from the high-speed mixer, putting the premix into a screw extruder for heating and melting, controlling the temperature of a feeding section to be 70 ℃, controlling the temperature of an extrusion section to be 105 ℃, rolling the premix into a sheet with the thickness of 1mm, cooling, and putting the sheet into a pulverizer for pulverizing to obtain the anticorrosive coating.
Example 4
S1, preparing a modified curing agent.
S101, adding 0.1mol of 2-methyl-imidazole and 400ml of n-butanol into a reaction kettle, heating to 40 ℃, and stirring for 5min at the rotating speed of 40 rpm to obtain a 2-methyl-imidazole solution.
S102, ti (SO) 4 ) 2 NaOH is added into 2-methyl-imidazole solution in a reaction kettle, and the 2-methyl-imidazole and Ti (SO 4 ) 2 Is heated to 100 ℃ for 4 hours to react 2-methyl-imidazole and Ti (SO 4 ) 2 And (3) carrying out chelation reaction to obtain a chelation reaction product.
And S103, cooling the chelate reaction product, filtering, washing with water, heating to 50 ℃ in an oven, and drying for 2 hours to obtain the modified curing agent.
S2, adding 1 part of phenolic aldehyde modified epoxy resin, 0.25 part of modified curing agent, 0.02 part of graphene, 0.2 part of composite ferrotitanium powder, 0.2 part of mica powder, 0.2 part of barium sulfate, 0.03 part of flatting agent and 0.03 part of benzoin into a high-speed mixer for premixing for 10min according to each 1000g, and stirring at 600rpm to obtain a premix.
S3, taking out the premix from the high-speed mixer, putting the premix into a screw extruder for heating and melting, controlling the temperature of a feeding section to be 80 ℃, controlling the temperature of an extrusion section to be 110 ℃, rolling the premix into a sheet with the thickness of 1mm, cooling, and putting the sheet into a pulverizer for pulverizing to obtain the anticorrosive coating.
Example 5
S1, preparing a modified curing agent.
S101, adding 0.1mol of 2-methyl-imidazole and 400ml of n-butanol into a reaction kettle, heating to 60 ℃, and stirring for 3min at the rotating speed of 70 r/min to obtain a 2-methyl-imidazole solution.
S102, ti (SO) 4 ) 2 NaOH is added into 2-methyl-imidazole solution in a reaction kettle, and the 2-methyl-imidazole and Ti (SO 4 ) 2 Is heated to 120 ℃ for 6 hours to react the 2-methyl-imidazole and the Ti (SO 4 ) 2 And (3) carrying out chelation reaction to obtain a chelation reaction product.
And S103, cooling the chelate reaction product, filtering, washing with water, heating to 70 ℃ in an oven, and drying for 3 hours to obtain the modified curing agent.
S2, adding 1 part of phenolic aldehyde modified epoxy resin, 0.15 part of modified curing agent, 0.01 part of graphene, 0.1 part of composite ferrotitanium powder, 0.1 part of mica powder, 0.1 part of barium sulfate, 0.01 part of flatting agent and 0.01 part of benzoin into a high-speed mixer for premixing for 5min according to each 1000g, and stirring at a rotation speed of 400rpm to obtain a premix.
S3, taking out the premix from the high-speed mixer, putting the premix into a screw extruder for heating and melting, controlling the temperature of a feeding section to be 60 ℃, controlling the temperature of an extrusion section to be 100 ℃, rolling the premix into a sheet with the thickness of 1mm, cooling, and putting the sheet into a pulverizer for pulverizing to obtain the anticorrosive coating.
Example 6
S1, preparing a modified curing agent.
S101, adding 0.1mol of 2-methyl-imidazole and 400ml of n-butanol into a reaction kettle, heating to 50 ℃, and stirring for 4min at the rotating speed of 60 revolutions per minute to obtain a 2-methyl-imidazole solution.
S102, ti (SO) 4 ) 2 NaOH is added into 2-methyl-imidazole solution in a reaction kettle, and the 2-methyl-imidazole and Ti (SO 4 ) 2 Is heated to 100 ℃ for 4 hours to react 2-methyl-imidazole and Ti (SO 4 ) 2 And (3) carrying out chelation reaction to obtain a chelation reaction product.
And S103, cooling the chelate reaction product, filtering, washing with water, heating to 50 ℃ in an oven, and drying for 2 hours to obtain the modified curing agent.
S2, adding 1 part of phenolic aldehyde modified epoxy resin, 0.15 part of modified curing agent, 0.01 part of graphene, 0.1 part of composite ferrotitanium powder, 0.1 part of mica powder, 0.1 part of barium sulfate, 0.01 part of flatting agent and 0.01 part of benzoin into a high-speed mixer for premixing for 5min according to each 1000g, and stirring at a rotation speed of 400rpm to obtain a premix.
S3, taking out the premix from the high-speed mixer, putting the premix into a screw extruder for heating and melting, controlling the temperature of a feeding section to be 60 ℃, controlling the temperature of an extrusion section to be 100 ℃, rolling the premix into a sheet with the thickness of 1mm, cooling, and putting the sheet into a pulverizer for pulverizing to obtain the anticorrosive coating.
Example 7
S1, preparing a modified curing agent.
S101, adding 0.1mol of 2-methyl-imidazole and 400ml of n-butanol into a reaction kettle, heating to 50 ℃, and stirring for 4min at the rotating speed of 60 revolutions per minute to obtain a 2-methyl-imidazole solution.
S102, ti (SO) 4 ) 2 NaOH is added into 2-methyl-imidazole solution in a reaction kettle, and the 2-methyl-imidazole and Ti (SO 4 ) 2 Is heated to 110 ℃ for 5 hours to react 2-methyl-imidazole and Ti (SO 4 ) 2 And (3) carrying out chelation reaction to obtain a chelation reaction product.
And S103, cooling the chelate reaction product, filtering, washing with water, heating to 60 ℃ in an oven, and drying for 2.5 hours to obtain the modified curing agent.
S2, adding 1 part of phenolic aldehyde modified epoxy resin, 0.15 part of modified curing agent, 0.01 part of graphene, 0.1 part of composite ferrotitanium powder, 0.1 part of mica powder, 0.1 part of barium sulfate, 0.01 part of flatting agent and 0.01 part of benzoin into a high-speed mixer for premixing for 5min according to each 1000g, and stirring at a rotation speed of 400rpm to obtain a premix.
S3, taking out the premix from the high-speed mixer, putting the premix into a screw extruder for heating and melting, controlling the temperature of a feeding section to be 60 ℃, controlling the temperature of an extrusion section to be 100 ℃, rolling the premix into a sheet with the thickness of 1mm, cooling, and putting the sheet into a pulverizer for pulverizing to obtain the anticorrosive coating.
Example 8
S1, preparing a modified curing agent.
S101, adding 0.1mol of 2-methyl-imidazole and 400ml of n-butanol into a reaction kettle, heating to 60 ℃, and stirring for 3min at the rotating speed of 70 r/min to obtain a 2-methyl-imidazole solution.
S102, ti (SO) 4 ) 2 NaOH is added into 2-methyl-imidazole solution in a reaction kettle, and the 2-methyl-imidazole and Ti (SO 4 ) 2 Is heated to 120 ℃ for 6 hours to react the 2-methyl-imidazole and the Ti (SO 4 ) 2 And (3) carrying out chelation reaction to obtain a chelation reaction product.
And S103, cooling the chelate reaction product, filtering, washing with water, heating to 70 ℃ in an oven, and drying for 3 hours to obtain the modified curing agent.
S2, adding 1 part of phenolic aldehyde modified epoxy resin and 0.25 part of modified curing agent into a high-speed mixer for premixing for 10min according to 1000g each part, and obtaining a premix with the stirring speed of 600 rpm.
S3, taking out the premix from the high-speed mixer, putting the premix into a screw extruder for heating and melting, controlling the temperature of a feeding section to be 80 ℃, controlling the temperature of an extrusion section to be 110 ℃, rolling the premix into a sheet with the thickness of 1mm, cooling, and putting the sheet into a pulverizer for pulverizing to obtain the anticorrosive coating.
In short, example 8 differs from example 1 only in that in S2, graphene, composite ferrotitanium powder, mica powder, barium sulfate, leveling agent, benzoin are not present.
Example 9
S1, preparing a modified curing agent.
S101, adding 0.1mol of 2-methyl-imidazole and 400ml of n-butanol into a reaction kettle, heating to 50 ℃, and stirring for 4min at the rotating speed of 60 revolutions per minute to obtain a 2-methyl-imidazole solution.
S102, ti (SO) 4 ) 2 NaOH is added into 2-methyl-imidazole solution in a reaction kettle, and the 2-methyl-imidazole and Ti (SO 4 ) 2 Is heated to 100 ℃ for 4 hours to react the 2-methyl-imidazole and the Ti (SO 4 ) 2 And (3) carrying out chelation reaction to obtain a chelation reaction product.
And S103, cooling the chelate reaction product, filtering, washing with water, heating to 50 ℃ in an oven, and drying for 2 hours to obtain the modified curing agent.
S2, adding 1 part of phenolic aldehyde modified epoxy resin and 0.15 part of modified curing agent into a high-speed mixer for premixing for 5min according to 1000g each part, and obtaining a premix with the stirring speed of 400 rpm.
S3, taking out the premix from the high-speed mixer, putting the premix into a screw extruder for heating and melting, controlling the temperature of a feeding section to be 60 ℃, controlling the temperature of an extrusion section to be 100 ℃, rolling the premix into a sheet with the thickness of 1mm, cooling, and putting the sheet into a pulverizer for pulverizing to obtain the anticorrosive coating.
In short, example 9 differs from example 2 only in that in S2, graphene, composite ferrotitanium powder, mica powder, barium sulfate, leveling agent, benzoin are not present.
Example 10
S1, preparing a modified curing agent.
S101, adding 0.1mol of 2-methyl-imidazole and 400ml of n-butanol into a reaction kettle, heating to 50 ℃, and stirring for 4min at the rotating speed of 60 revolutions per minute to obtain a 2-methyl-imidazole solution.
S102, ti (SO) 4 ) 2 NaOH is added into 2-methyl-imidazole solution in a reaction kettle, and the 2-methyl-imidazole and Ti (SO 4 ) 2 Is heated to 100 ℃ for 4 hours to react the 2-methyl-imidazole and the Ti (SO 4 ) 2 And (3) carrying out chelation reaction to obtain a chelation reaction product.
And S103, cooling the chelate reaction product, filtering, washing with water, heating to 50 ℃ in an oven, and drying for 2 hours to obtain the modified curing agent.
S2, adding 1 part of phenolic aldehyde modified epoxy resin and 0.2 part of modified curing agent into a high-speed mixer for premixing for 8min according to 1000g each part, and obtaining a premix with the stirring speed of 500 rpm.
S3, taking out the premix from the high-speed mixer, putting the premix into a screw extruder for heating and melting, controlling the temperature of a feeding section to be 70 ℃, controlling the temperature of an extrusion section to be 105 ℃, rolling the premix into a sheet with the thickness of 1mm, cooling, and putting the sheet into a pulverizer for pulverizing to obtain the anticorrosive coating.
In short, example 10 differs from example 3 only in that in S2, graphene, composite ferrotitanium powder, mica powder, barium sulfate, leveling agent, benzoin are not present.
Comparative example 1
In this comparative example, no modified curing agent was added, and the other steps and components were the same as in example 1.
Comparative example 2
In this comparative example, 0.5 part of the modified curing agent was used, and the other steps and components were the same as in example 1.
Comparative example 3
In the preparation of the modified curing agent in this comparative example, 2-methyl-imidazole and Ti (SO 4 ) 2 The molar ratio of (2) was 1.0:0.1, and the other steps and components were the same as in example 1.
Comparative example 4
In the preparation of the modified curing agent in this comparative example, 2-methyl-imidazole and Ti (SO 4 ) 2 The molar ratio of (2) was 1.0:0.6, and the other steps and components were the same as in example 1.
Comparative example 5
In the preparation process of the modified curing agent in the comparative example, the chelating reaction temperature was 80 ℃, and other steps and components were the same as in example 1.
Comparative example 6
In the preparation process of the modified curing agent in the comparative example, the time of the chelation reaction was 2 hours, and other steps and components were the same as in example 1.
The components of each example and each comparative example were listed as shown in the following table.
Test example 1
The anticorrosive coatings prepared in examples 1 to 7 and comparative examples 1 to 6 were subjected to crude oil resistance (100 ℃,90 d), 10% HCl (100 ℃,90 d), 10% NaCl (100 ℃,90 d), 10% H 2 SO 4 (100 ℃ C., 90 d) performance test, the test method is referred to GB/T9274 standard, and the results are shown in the following table.
From the data in the table above, it can be seen that:
in comparative example 1, the modified curing agent was not added, and the other components were the same as in example 1, so that the coating layer was foamed and peeled off.
In comparative example 2,2 parts of a modified curing agent was added, and the rest was the same as in example 1, so that the coating layer foamed and peeled off.
In comparative example 3, 2-methyl-imidazole and Ti (SO 4 ) 2 The molar ratio of the reaction of (2) to (0.2) was 1.0:0.1, which was greater than the range of (0.8-1.0) of the present application, and the remainder was the same as in example 1, resulting in bubbling and peeling of the coating.
Comparative example 4, preparation of modified curing agent 2-methyl-imidazole and Ti (SO 4 ) 2 The molar ratio of the reaction of (2) to (0.2) was 1.0:0.6, which is less than the range of (0.8-1.0) of the present application, and the remainder was the same as in example 1, resulting in bubbling and peeling of the coating.
In comparative example 5, the temperature of the chelating reaction during the preparation of the modified curing agent was 80℃and less than the range of 100 to 120℃in the present application, and the remainder was the same as in example 1, with the result that the coating foamed and peeled off.
In comparative example 6, the time of the chelation reaction in the preparation process of the modified curing agent was 2 hours, which is less than the range of 4 to 6 hours in the present application, and the rest was the same as in example 1, with the result that the coating foamed and peeled off.
The coating formed by the anticorrosive paint prepared by the embodiments 1-7 has the advantages of excellent temperature resistance, medium corrosion resistance, low curing reaction temperature and the like, and can effectively prevent the corrosion of pipelines and equipment in an oilfield station, thereby ensuring the safe operation of the oilfield station.
Test example 2
The anticorrosive coatings obtained in examples 1 to 3 and examples 8 to 10 were subjected to crude oil resistance (100 ℃), 10% HCl (100 ℃), 10% NaCl (100 ℃), 10% H 2 SO 4 (100 ℃ C.) performance test results are shown in the following table.
From the data in the table above, it can be seen that:
according to the method, the graphene, the composite ferrotitanium powder, the mica powder, the barium sulfate, the leveling agent and the benzoin are added, so that the coating formed by the prepared anticorrosive coating has more excellent temperature resistance and medium corrosion resistance.
The foregoing has outlined and described the basic principles, main features and advantages of the present application. It will be appreciated by persons skilled in the art that the present application is not limited to the embodiments described above, and that the embodiments and descriptions described herein are merely illustrative of the principles of the application, and various changes and modifications may be made therein without departing from the spirit and scope of the application, which is defined in the appended claims, specification and their equivalents.
Finally, it should be noted that the above embodiments are only for illustrating the technical solutions of the present application and not for limiting the scope of protection of the present application, and although the present application has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solutions of the present application without departing from the spirit and scope of the technical solutions of the present application.
Claims (7)
1. An anticorrosive paint is characterized by comprising the following components in parts by weight:
1 part of phenolic aldehyde modified epoxy resin and 0.15 to 0.25 part of 2-methylimidazole titanium complex modified curing agent;
wherein the structural formula of the 2-methylimidazole titanium complex modified curing agent is as follows:
the preparation method of the 2-methylimidazole titanium complex modified curing agent comprises the following steps:
adding 2-methyl-imidazole and an organic solvent into a reaction kettle, so that the 2-methyl-imidazole is dissolved in the organic solvent;
adding Ti (SO) into a reaction kettle 4 ) 2 Chelating the 2-methylimidazole and the titanium sulfate by NaOH, cooling, filtering, washing with water and drying to obtain the 2-methylimidazole titanium complex modified curing agent;
said 2-methyl-imidazole and said Ti (SO 4 ) 2 The molar ratio of (0.8-1.0) to (0.2-0.4);
the mol ratio of the 2-methyl-imidazole to the NaOH is (0.8-1.0): 0.1-0.2;
the dissolution temperature is 40-60 ℃, the stirring speed of the dissolution is 40-70 rpm, and the dissolution time is 3-5 min;
the temperature of the chelation reaction is 100-120 ℃, and the time of the chelation reaction is 4-6 h;
the drying temperature is 50-70 ℃, and the drying time is 2-3 h.
2. An anticorrosive coating according to claim 1, further comprising the following components in parts by weight:
0.01 to 0.02 portion of graphene, 0.1 to 0.2 portion of composite ferrotitanium powder, 0.1 to 0.2 portion of mica powder, 0.1 to 0.2 portion of barium sulfate, 0.01 to 0.03 portion of flatting agent and 0.01 to 0.03 portion of benzoin.
3. An anticorrosive coating according to claim 1, wherein,
the organic solvent comprises n-butanol, 400ml of which corresponds to 0.1mol of 2-methyl-imidazole.
4. A method of preparing an anticorrosive coating according to any one of claims 1 to 3, comprising the steps of:
premixing phenolic aldehyde modified epoxy resin and a 2-methylimidazole titanium complex modified curing agent to obtain a premix;
and adding the premix into a screw extruder for melting, rolling into slices, cooling and crushing to obtain the anticorrosive coating.
5. The method according to claim 4, wherein,
and premixing graphene, composite ferrotitanium powder, mica powder, barium sulfate, a leveling agent and benzoin with the phenolic aldehyde modified epoxy resin and the 2-methylimidazole titanium complex modified curing agent.
6. The method according to claim 5, wherein,
the stirring speed of the premixing is 400-600 rpm, and the time is 5-10 min.
7. The method according to claim 4, wherein,
the temperature of the feeding section of the screw extruder is 60-80 ℃, and the temperature of the extrusion section is 100-110 ℃.
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| JP2004156081A (en) * | 2002-11-05 | 2004-06-03 | Jfe Steel Kk | Surface treated steel sheet superior in electromagnetic wave shielding property and corrosion resistance, and manufacturing method therefor |
| CN110713774A (en) * | 2019-09-27 | 2020-01-21 | 洛阳双瑞防腐工程技术有限公司 | High-toughness low-temperature fast-curing heavy-duty anticorrosive epoxy powder coating and preparation method thereof |
| CN112280422A (en) * | 2020-09-30 | 2021-01-29 | 中国石油天然气集团公司 | Zirconium-titanium binary modified epoxy anticorrosive paint and preparation method and application thereof |
| WO2021088222A1 (en) * | 2019-11-06 | 2021-05-14 | 石家庄圣泰化工有限公司 | Method for synthesizing imidazole additive |
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| JP2004156081A (en) * | 2002-11-05 | 2004-06-03 | Jfe Steel Kk | Surface treated steel sheet superior in electromagnetic wave shielding property and corrosion resistance, and manufacturing method therefor |
| CN110713774A (en) * | 2019-09-27 | 2020-01-21 | 洛阳双瑞防腐工程技术有限公司 | High-toughness low-temperature fast-curing heavy-duty anticorrosive epoxy powder coating and preparation method thereof |
| WO2021088222A1 (en) * | 2019-11-06 | 2021-05-14 | 石家庄圣泰化工有限公司 | Method for synthesizing imidazole additive |
| CN112280422A (en) * | 2020-09-30 | 2021-01-29 | 中国石油天然气集团公司 | Zirconium-titanium binary modified epoxy anticorrosive paint and preparation method and application thereof |
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