CN111607097A - Titanium-based fluorine-silicon polymer alloy and synthesis and application methods thereof - Google Patents
Titanium-based fluorine-silicon polymer alloy and synthesis and application methods thereof Download PDFInfo
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Abstract
The invention discloses a titanium-based fluorine-silicon polymer alloy and a synthesis and application method thereof, wherein the titanium-based fluorine-silicon polymer alloy is composed of the following raw materials by mass ratio: organic titanium polymer (TPP) and organic fluorine silicone prepolymer (F-Si/F)4) TPP, F-Si 70EBlending at a mass ratio of 90: 10-30 (wt), stirring and heating in a reaction kettle for 60-80 ℃/30-60 min → heating to 100-120 ℃/1-4 h, and discharging to obtain the titanium-based fluorosilicone polymer alloy (TFSMA). The low-surface energy anti-drag anticorrosive coating prepared from the high-performance coating matrix film-forming material can remarkably improve the internal anti-drag scaling anticorrosive effect of the oil and gas pipeline coating, increase the gas transmission amount by 5-20%, and is far longer than the service life of a pipeline.
Description
Technical Field
The invention relates to a novel coating film-forming material, which belongs to the technical field of fine chemical engineering and application thereof, and the product is mainly applied to manufacturing low-surface-energy non-adhesive coatings, and the typical industrial application is to prepare impedance-reducing scaling anticorrosive coatings in oil and gas pipelines.
Background
Foreign data show that the economic and technical benefits of the inner anti-drag coating are very obvious, the gas transmission amount of the pipeline with the inner anti-drag coating can be improved by 5-20% compared with the pipeline without the inner anti-drag coating under the same condition, the investment recovery period of the inner anti-drag coating is only 3 years and is far longer than the service life of the pipeline.
The oil and gas transmission pipeline coating developed in China is also a coating with corrosion prevention as a main purpose, and belongs to epoxy resin powder coatings from published paper information and CN101698773B, CN103013284A, CN101974282A and CN102417780B patents. The coating has the defects that the heat resistance of the coating is poor, high-temperature sintering is required during use, the energy consumption is high, the smoothness of the coating is not enough, dirt is easy to retain, and the oil-gas conveying resistance is increased. These are related to the properties of the matrix material and are difficult to overcome.
On the basis of summarizing the research experience of predecessors, a nano organic titanium polymer (ZL 200810029936.1; ZL 201210437940.9) and an organic fluorine-silicon material are copolymerized by utilizing a core technology and key materials of independent intellectual property rights to prepare a titanium-based fluorine-silicon polymer alloy, so that the invention provides a coating material for preparing a high-performance film-forming substrate for coating protection in an oil and gas pipeline, and solves the bottleneck technology of drag reduction, scaling prevention and corrosion prevention in the oil and gas pipeline.
Disclosure of Invention
The invention provides a preparation method and an application method of a titanium-based fluorine-silicon polymer alloy, and aims to at least solve the bottleneck technology of drag reduction, no scaling and corrosion prevention in an oil and gas pipeline.
The titanium-based fluorosilicone polymer alloy of the invention is prepared from organic fluorosilicone prepolymer (F-Si/F)4) The organic silicon-fluorine copolymer is obtained by blending and pre-polymerizing with an organic titanium polymer (TPP) according to the mass ratio of 10-30: 70-90, and the organic silicon-fluorine copolymer is obtained by polymerizing fluoroalkyl acrylate and hydroxyl-terminated silane.
Further, the organic fluorine-silicon copolymer is prepared from the following raw materials in parts by weight: 5-30 parts of fluoroalkyl acrylate, 1-5 parts of hydroxyl-terminated silane, 0.2-1 part of initiator and 30-110 parts of solvent. Wherein the solvent is selected from one or more of toluene, xylene and butyl acetate; the initiator is selected from one or more of acyl peroxides, hydroperoxides, dialkyl peroxides, ester peroxides and ketone peroxides.
Further, the fluoroalkyl acrylate has the following structural formula:
x is (C)1～C8) Alkyl, (C)1～C8) Alkenyl or (C)4-C8) A cycloalkyl group;
R1is- (CF)2)nCF3Wherein n is less than or equal to 6.
Further, the vinyl resin is a tetrafluoroethylene/vinyl copolymer resin.
Further, the hydroxyl-terminated silane is hydroxyl-terminated polysiloxane.
Further, the solvent is selected from one or more of toluene, xylene and butyl acetate.
Further, the initiator is selected from one or more of acyl peroxides, hydroperoxides, dialkyl peroxides, ester peroxides and ketone peroxides.
The invention also discloses a preparation method of the organic fluorine-silicon prepolymer, which comprises the following steps: blending the organic fluorine-silicon copolymer and tetrafluoroethylene resin, heating for 30-60 min at 60-80 ℃, heating to 100-120 ℃, reacting for 1-4 h, and discharging.
Further, the preparation method of the organic fluorine-silicon copolymer comprises the following steps:
step 1: taking solvent in N2Heating to 80-100 ℃ under protection, adding 1/2 fluoroalkyl acrylate and 1/2 initiator, and stirring to react for 1-4 h at 100-120 ℃;
step 2: and (3) dropwise adding hydroxyl-terminated silane, the residual fluoroalkyl acrylate and an initiator into the solution obtained in the step (1) at a constant temperature, and reacting for 3-5 h at 120-150 ℃.
Further, the step 2 specifically includes: and (2) dropwise adding hydroxyl-terminated silane and residual fluoroalkyl acrylate into the solution obtained in the step (1) at a constant temperature, reacting for 3-5 h at 120-130 ℃, adding an initiator, and reacting for 3-5 h at 120-130 ℃.
The preparation method of the organic fluorine-silicon prepolymer comprises the following steps:
blending the F-Si copolymer and the tetrafluoroethylene/vinyl copolymer resin according to the mass ratio of 20-50: 50-80 (wt), stirring and heating in a reaction kettle for 60-80 ℃/30-60 min → heating to 100-120 ℃/1-4 h, and discharging to obtain the organic fluorine-silicon prepolymer (hereinafter referred to as F-Si/F for short)4)。
Furthermore, the titanium-based fluorosilicone polymer alloy (TFSMA) adopts an organic fluorosilicone copolymer (F-Si/F)4) Premixing with organic titanium polymer (TPP) according to the mass ratio of 10-30: 70-90, stirring and heating in a reaction kettle for 60-80 ℃/30-60 min → heating to 100-120 ℃/1-4 h, and discharging to obtain TFSMA. The characteristic IR picture of the sample after infrared spectrum detection is shown in figure 1.
The invention also discloses a formulation technology of the anti-drag non-scaling anticorrosive coating specially used in an oil and gas pipeline, which is mainly applied to thermosetting finish paint and comprises the following raw materials in parts by mass: 10-30 parts of titanium-based fluorine-silicon polymer alloy, 1-15 parts of epoxy resin solution, 1-15 parts of phenolic resin solution, 1-8 parts of elastic saturated polyester resin, 5-10 parts of diamino diphenyl sulfone (latent curing agent), 2-5 parts of coating auxiliary agent, 5-10 parts of superfine mica powder, 5-10 parts of graphene dispersion slurry, 1-5 parts of pigment carbon black and 10-15 parts of mixed solvent.
The invention also discloses a formula technology of the anti-drag non-scaling anticorrosive coating special for the oil and gas pipeline, which is mainly applied to self-crosslinking finish paint and comprises a component A and a component B. The component A is prepared from the following raw materials in parts by mass: 10-30 parts of titanium-based fluorosilicone polymer alloy, 1-15 parts of epoxy resin solution, 1-15 parts of phenolic resin solution, 1-8 parts of liquid nitrile rubber, 2-5 parts of paint auxiliary agent, 5-10 parts of superfine mica powder, 5-10 parts of graphene dispersion slurry, 1-5 parts of pigment carbon black and 10-15 parts of mixed solvent. The component B is 10-20 parts of polyamide epoxy curing agent.
Furthermore, the titanium-based fluorosilicone polymer alloy material cannot be used for manufacturing a primer, and the interlayer adhesion with a finish paint is influenced because the titanium-based fluorosilicone polymer alloy material has non-adhesion characteristics after film formation, but other anticorrosion primers such as a titanium-based polymer alloy primer, an epoxy primer or a polyurethane primer can be matched with the titanium-based fluorosilicone polymer alloy material, and the interlayer adhesion is not influenced.
Compared with the prior art, the TFSMA can endow the coating with ultra-low surface energy (theta is more than or equal to 150 degrees), form a super-hydrophobic interface, reduce the friction force of the surface of the coating and realize the drag reduction effect, which cannot be realized by the epoxy resin coating, as shown in figure 2.
Drawings
FIG. 1 is a characteristic IR spectrum of a TFSMA of the present invention;
FIG. 2 shows the super-hydrophobic effect of the TFSMA coating of the invention.
Detailed Description
In order to make the technical solutions of the present invention better understood, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
In example 1 of the present invention, the fluoroalkyl acrylate was perfluoroalkylethyl methacrylate (i.e., X is ethyl and R is R)1is-CF3) (ii) a The hydroxyl-terminated silane is WS62M organosilicon; the initiator is acyl peroxide, in particular benzoyl peroxide; the solvent is mixed solution of xylene and butyl acetate, and is shown in Table-1. Different processes are adopted to optimize the scheme of the embodiment 1 of the invention.
TABLE-1 synthetic F-Si interpolymer formulation
Weighing a solvent according to the formula amount shown in the table-1, placing the solvent in a flask with a stirring paddle, stirring, heating to 60-80 ℃, adding 50-100 g of fluoroalkyl acrylate, 1-3 g of benzoyl peroxide → heating to 100-120 ℃, reacting for 1-5 h → dripping 50-100 g of the rest fluoroalkyl acrylate, 50-100 g of WS62M organic silicon → reacting for 2-5 h → dripping 1-3 g of the rest benzoyl peroxide → heating to 120-150 ℃, reacting for 2-5 h, and discharging to obtain the F-Si copolymer solution.
Example 2
And (3) process optimization test: taking 750g of solvent, heating to 80 ℃ under stirring, adding 100g of perfluoroalkyl ethyl methacrylate, 3g of benzoyl peroxide, heating to 100 ℃ for reaction for 2h → dripping 100g of residual perfluoroalkyl ethyl methacrylate and 45g of WS62M organic silicon → reaction for 4h → dripping 2g of residual benzoyl peroxide, heating to 120 ℃ for reaction for 2.5h, and discharging to obtain the F-Si copolymer solution.
Example 3
Further process optimization test: taking 750g of solvent, heating to 100 ℃ under stirring, adding 100g of perfluoroalkyl ethyl methacrylate, 3g of benzoyl peroxide, heating to 110 ℃ for reaction for 2h → dripping 100g of residual perfluoroalkyl ethyl methacrylate and 45g of WS62M organic silicon → reaction for 4h → dripping 2g of residual benzoyl peroxide, heating to 120 ℃ for reaction for 2.5h, and discharging to obtain the F-Si copolymer solution.
Example 4
Further process optimization test: taking 750g of solvent, heating to 110 ℃ under stirring, adding 100g of perfluoroalkyl ethyl methacrylate, 3g of benzoyl peroxide, heating to 120 ℃ for reaction for 2h → dripping 100g of residual perfluoroalkyl ethyl methacrylate and 45g of WS62M organic silicon → reaction for 4h → dripping 2g of residual benzoyl peroxide, heating to 130 ℃ for reaction for 2.5h, and discharging to obtain the F-Si copolymer solution.
Example 5
Further process optimization test: taking 750g of solvent, heating to 120 ℃ under stirring, adding 100g of perfluoroalkyl ethyl methacrylate, 3g of benzoyl peroxide, heating to 130 ℃ for reaction for 2h → dripping 100g of residual perfluoroalkyl ethyl methacrylate and 45g of WS62M organic silicon, reacting for 4h → dripping 2g of residual benzoyl peroxide, heating to 140 ℃ for reaction for 2.5h, and gelling.
Through comparison of the optimization tests of the synthesis examples 1-5, the increase of the synthesis temperature can not only increase the decomposition rate of the initiator and accelerate the polymerization reaction rate, but also correspondingly increase the chain transfer rate of the solvent along with the increase of the temperature. Thus, increasing the temperature reduces the molecular weight of the polymer, while decreasing the temperature and increasing the reaction time increases the molecular weight, but the resin synthesis temperature should be matched to the half-life of the initiator, and benzoyl peroxide dissociates rapidly at a higher temperature of 130 ℃ into the highly reactive benzene radical and CO2The highly reactive benzene radical is an effective hydrogen abstracting agent at temperatures above 130 ℃, resulting in considerable branching, increasing the C-F-Si branching of the polymer, giving it a lower surface free energy. The experimental results show that as the temperature of the synthesis process is increased, the branching of the polymer is increased and the contact angle is increased. However, when the temperature is 140 ℃ or higher, the synthesis experiment fails. This is because the initiator benzoyl peroxide loses its effectiveness at too high a temperature.
Example 6
The F-Si copolymer can be blended with an organic Titanium polymer (TPP) for modification and prepolymerization to prepare a Titanium-based fluorosilicone polymer alloy (TFSMA), wherein the premixing mass ratio is TPP to F-Si is 70-90: 10-30 (wt); stirring and heating in a reaction kettle for 60-80 ℃/30-60 min → heating to 100-120 ℃/1-4 h, and discharging. The preparation of the organic titanium polymer (TPP) can be carried out according to the method with the patent number ZL200810029936.1, and the details are not repeated.
In the embodiment 6 of the invention, the mass ratio of the F-Si copolymer to the TPP is 25: 75(wt) mixing, stirring and heating in a reaction kettle at 80 ℃/1h → heating to 120 ℃/2h, discharging to obtain the TFSMA prepolymer.
Example 7
The invention also provides a single-component drying type finish paint which comprises the following components in percentage by weight: weighing titanium-based fluorine-silicon polymer alloy premix (TFSMA) or titanium-based fluorine-silicon polymer alloy (F-Si/F)4) 10-30 parts of epoxy resin solution, 1-15 parts of phenolic resin solution, 1-15 parts of elastic saturated polyester resin, 2-8 parts of liquid nitrile rubber, 5-10 parts of Diamino Diphenyl Sulfone (DDS), 2-5 parts of paint auxiliaries (including wetting dispersion, defoaming, rheological, thickening, anti-settling and the like), 5-10 parts of superfine mica powder, 5-10 parts of graphene dispersion slurry, 10-15 parts of carbon black color paste and 5-10 parts of mixed solvent. Curing conditions are as follows: 180 ℃/30min or 200 ℃/20 min.
Example 8
Group A) taking 20 parts of titanium-based fluorine-silicon polymer alloy (TFSMA), 15 parts of 609 epoxy resin solution, 10 parts of 2402 phenolic resin solution, 6 parts of LG607 elastic saturated polyester resin, 6 parts of SH-810 liquid nitrile rubber, 0.5 part of FR-0516 wetting dispersant, 0.3 part of BYK-052 defoamer, 0.2 part of BYK-306 rheological agent, 1 part of SD-1 organic bentonite, 1 part of F118 anti-settling agent, 10 parts of 1250-mesh mica powder, 10 parts of graphene dispersion slurry with solid content of 5 percent, 10 parts of MA-100 color paste carbon black and 10 parts of mixed solvent. All the components participate in dispersion and grinding, and the fineness of the components reaches 20-30 mu m, so that the finished finish is obtained. B group) R-4030 solvent-free low-viscosity epoxy curing agent 20 parts, and can be directly subpackaged.
The embodiment is a bi-component cross-linking type self-drying finish paint, and the application mass ratio of A to B is 4-5 to 1 (wt); the drying conditions are surface drying at 25 ℃/2-4 h, solid drying at 25 ℃/24h, and complete curing at 25 ℃/7 d.
The finished coating prepared by the optimized formula in the embodiment 7-8 is verified and detected according to SY/T6530 industrial standard, and the detection result is shown in Table-2.
TABLE-2 coating Performance test results
Finally, it should be noted that the above-mentioned embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the above-mentioned embodiments, it should be understood by those skilled in the art that the modifications and equivalents of the specific embodiments of the present invention can be made by those skilled in the art after reading the present specification, but these modifications and variations do not depart from the scope of the claims of the present application.
Claims (14)
1. The titanium-based fluorine-silicon polymer alloy is characterized in that the titanium-based fluorine-silicon polymer alloy is prepared from organic fluorine-silicon prepolymer F-Si/F4Copolymerizing with organic titanium polymer TPP according to the mass ratio of 10-30: 70-90 to obtain the copolymer; wherein the organic fluorine-silicon prepolymer F-Si/F4Is prepared from the F-Si and F copolymer of organic fluorosilicone4The resin is obtained by pre-polymerization according to the mass ratio of 3: 7.
2. The titanium-based fluorosilicone polymer alloy of claim 1, wherein the organic fluorosilicone copolymer comprises the following raw materials in parts by weight: 5-30 parts of fluoroalkyl acrylate, 1-5 parts of hydroxyl-terminated silane, 0.2-1 part of initiator and 30-110 parts of solvent.
3. The titanium-based fluorosilicone polymer alloy of claim 2, wherein the solvent is one or more selected from the group consisting of toluene, xylene, and butyl acetate.
4. The titanium-based fluorosilicone polymer alloy of claim 2, wherein the fluoroalkyl acrylate has the following structural formula:
x is (C)1～C8) Alkyl, (C)1～C8) Alkenyl or (C)4-C8) A cycloalkyl group;
R1is- (CF)2)nCF3Wherein n is less than or equal to 6.
5. The titanium-based fluorosilicone polymer alloy of claim 2, wherein the hydroxyl terminated silane is hydroxyl terminated polysiloxane having a structural formula:
6. the titanium-based fluorosilicone polymer alloy of claim 2, wherein the initiator is selected from one or more of acyl peroxides, hydroperoxides, dialkyl peroxides, ester peroxides, and ketone peroxides.
7. The method for preparing the titanium-based fluorosilicone polymer alloy of any one of claims 1 to 6, wherein the organofluorosilicone copolymer F-Si is prepared by the following synthetic route:
8. the method of claim 7, comprising the steps of:
step 1: taking solvent in N2Heating to 80-100 ℃ under protection, adding 1/2 fluoroalkyl acrylate and 1/2 initiator, and stirring at 100-120 DEG CStirring and reacting for 1-4 h;
step 2: and (3) dropwise adding hydroxyl-terminated silane, the residual fluoroalkyl acrylate and an initiator into the solution obtained in the step (1) at a constant temperature, and reacting for 3-5 h at 120-150 ℃.
9. The preparation method according to claim 8, wherein the step 2 is specifically: and (2) dropwise adding hydroxyl-terminated silane and residual fluoroalkyl acrylate into the solution obtained in the step (1) at a constant temperature, reacting for 3-5 h at 120-130 ℃, adding an initiator, and reacting for 3-5 h at 120-130 ℃.
10. The titanium-based fluorosilicone polymer alloy of claim 1, wherein F is4The resin is tetrafluoroethylene/vinyl copolymer resin.
11. The titanium-based fluorosilicone polymer alloy according to claim 1, wherein said organofluorosilicone prepolymer is F-Si/F4The synthesis method comprises the following steps: the organic fluorine-silicon copolymer F-Si and F4Blending the resins, heating the mixture for 30-60 min at the temperature of 60-80 ℃, heating the mixture to 100-120 ℃, reacting the mixture for 1-4 h and discharging the product to obtain the organic fluorine-silicon prepolymer F-Si/F4。
12. The titanium-based fluorosilicone polymer alloy according to claim 1, wherein the titanium-based fluorosilicone polymer alloy is prepared by the following steps: organic fluorine silicon prepolymer F-Si/F4Premixing with organic titanium polymer TPP according to the mass ratio of 10-30: 70-90, stirring and heating in a reaction kettle for 60-80 ℃/30-60 min, heating to 100-120 ℃/1-4 h, and discharging to obtain the titanium-based fluorosilicone polymer alloy.
13. A coating, characterized in that the coating contains the titanium-based fluorosilicone polymer alloy as defined in claim 1, the coating is a high-performance coating substrate film-forming material for manufacturing a low-surface-energy non-stick coating, and the typical industrial application of the coating is to prepare an impedance-reducing scale-forming anticorrosive coating in an oil and gas pipeline.
14. The coating of claim 13, wherein the coating is a one-component thermosetting topcoat comprising, in parts by weight: 10-30 parts of titanium-based fluorine-silicon polymer alloy, 1-15 parts of epoxy resin solution, 1-15 parts of phenolic resin solution, 1-8 parts of solvent-free elastic saturated polyester resin, 2-8 parts of liquid nitrile rubber, 5-10 parts of diamino diphenyl sulfone, 2-5 parts of paint auxiliary agent, 5-10 parts of superfine mica powder, 5-10 parts of graphene dispersion slurry, 10-15 parts of carbon black color paste and 5-10 parts of epoxy active diluent.
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| CN115678434A (en) * | 2022-10-24 | 2023-02-03 | 扬州工业职业技术学院 | High-molecular chemical material and preparation method thereof |
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| CN114702904A (en) * | 2022-05-19 | 2022-07-05 | 玉环加鑫汽车配件有限公司 | Guide ring surface coating, coating manufacturing method and guide ring coating manufacturing method |
| CN114702904B (en) * | 2022-05-19 | 2023-01-03 | 玉环加鑫汽车配件有限公司 | Guide ring surface coating, coating manufacturing method and guide ring coating manufacturing method |
| CN115678434A (en) * | 2022-10-24 | 2023-02-03 | 扬州工业职业技术学院 | High-molecular chemical material and preparation method thereof |
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Application publication date: 20200901 |