CN114933712A - Preparation and application of reduced graphene oxide grafted aminated polyphenylene sulfide composite material - Google Patents
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Abstract
The invention provides a preparation method of a reduced graphene oxide grafted aminated polyphenylene sulfide composite material, which comprises the steps of ultrasonically dispersing graphene oxide in a tetrahydrofuran solution, uniformly ultrasonically dispersing, adding aminated polyphenylene sulfide, stirring and reacting at 45-55 ℃ for 10-12 hours to obtain PPS-GO, adding hydrazine hydrate, reacting at 75-85 ℃ for 1.5-2.5 hours, washing and drying to obtain PPS-rG. The aminated polyphenylene sulfide has excellent corrosion resistance, the reduced graphene oxide has a large lamellar structure, more functional groups are easy to act on organic matters and graft, the corrosion resistance can be effectively improved by grafting the reduced graphene oxide onto the aminated polyphenylene sulfide, and the reduced graphene oxide has better effect than the graphene oxide in stability, so that the composite material has lower corrosion current density and more excellent corrosion resistance. The composite material is sprayed on the surface of metal, can play a role in protecting the surface of metal, and has good application prospect.
Description
Technical Field
The invention relates to a preparation method of a reduced graphene oxide grafted aminated polyphenylene sulfide composite material, and also relates to an application of the composite material in preparation of an anticorrosive coating, belonging to the technical field of composite materials and the field of anticorrosive coatings.
Background
Polyphenylene sulfide is a high performance engineering polymer with high thermal stability, good mechanical properties, chemical resistance, flammability and high dimensional stability. Therefore, the outstanding characteristics of PPS make it widely used in various fields of filters for chemical and industrial facilities, heat sensors, automobiles, aerospace industry, and oceans. PPS is called "plastic gold", and is called six special engineering plastics together with Polysulfone (PSF), Polyarylate (PAR), polyether ether ketone (PEEK), Polyimide (PI) and Liquid Crystal Polymer (LCP), and is also one of eight aerospace materials. The high-quality composite material is characterized in that a main chain formed by connecting a rigid benzene ring and a flexible thioether bond has the characteristics of rigidity and flexibility, the microscopic form of the polyphenylene sulfide has structures such as lamellar, hollow spherical, rod-shaped and flower-shaped structures, and the polyphenylene sulfide has good compatibility, so that the polyphenylene sulfide can be modified by means of blending, chemical mixing and the like, and the high-quality composite material is obtained and used in the field of coatings with anticorrosion performance.
Currently, nanofillers are considered important materials for the preparation of nanocomposites with excellent properties. The graphene oxide has special application in the fields of films, anticorrosive coatings, polymer composite materials, sensors and the like due to unique mechanical properties, thermal properties and electrical properties of the graphene oxide. Graphene oxide consists of two-dimensional nanoplates of carbon atoms bonded together by covalent bonds. Graphene oxide has a structure similar to graphite, but functional groups, including hydroxyl and carbonyl groups, are present on the surface of graphene oxide. The presence of these groups on the surface of graphene oxide makes it possible to produce the desired chemical changes on the surface by using modifiers, which in many cases will result in a greater advantage of graphene oxide over graphene. The appearance of graphene oxide, which is a derivative of graphene, is just solving the above-mentioned problem, and has substantially the same structure as graphene. Except that a large number of oxygen-containing groups are attached to a base plane formed by a layer of carbon atoms and extending infinitely in two dimensions, the plane contains-OH and C-O-C, and the edge of the sheet contains C = O and COOH. Compared with graphene, graphene oxide has more excellent performance, not only has good wetting performance and surface activity, but also can be peeled off by small molecules or polymers after intercalation, and plays a very important role in improving comprehensive properties of materials such as heat, electricity, mechanics and the like. Many experts and scholars have conducted intensive research on the preparation and application of graphene oxide, wherein the development of graphene oxide composite materials is rapid, and the application field of graphene oxide is further expanded.
At present, some composite materials are mostly prepared from graphene quantum dots, the graphene quantum dots have smaller sizes and can increase certain mechanical properties and catalytic properties, but the performances of the graphene quantum dots on electrochemical corrosion resistance and chemical stability are poor, and the performances of the graphene quantum dots on reduction and oxidation are more excellent. Therefore, the composite coating is prepared by adopting the reduced graphene oxide grafted aminated polyphenylene sulfide, so that the material with excellent electrochemical corrosion resistance and chemical stability can be obtained.
Disclosure of Invention
The invention aims to provide a preparation method of a reduced graphene oxide grafted aminated polyphenylene sulfide composite material,
another object of the invention is to provide the use of the composite material in the preparation of corrosion resistant coatings
Preparation of reduced graphene oxide grafted aminated polyphenylene sulfide composite material
The preparation method of the reduced graphene oxide grafted aminated polyphenylene sulfide composite material comprises the following process steps:
（1）preparation of aminated polyphenylene sulfide: anhydrous sodium sulfide, p-dichlorobenzene and 2, 5-dichloroaniline are used as raw materials, N-methyl pyrrolidone is used as a solvent, isopropyl titanate is used as a catalyst, nitrogen is used as protective gas, the reaction is carried out for 1.5 to 2.5 hours at 260 to 280 ℃ in an alkaline environment, and the aminated polyphenylene sulfide is obtained by washing, filtering and drying and is marked as PPS-NH 2 . Wherein the mass ratio of the 2, 5-dichloroaniline to the anhydrous sodium sulfide is 1: 10-1: 15; the mass ratio of the 2, 5-dichloroaniline to the p-dichlorobenzene is 1: 10-1: 12; the mass ratio of the 2, 5-dichloroaniline to the isopropyl titanate is 1: 0.8-1: 1.
(2) Preparing a reduced graphene oxide grafted aminated polyphenylene sulfide composite material: firstly, graphene oxide is ultrasonically dispersed and dissolved in a tetrahydrofuran solution, after the graphene oxide is ultrasonically dispersed uniformly, aminated polyphenylene sulfide is added, the mixture is stirred and reacts for 10-12 hours at the temperature of 45-55 ℃, PPS-GO is obtained, hydrazine hydrate is added, the mixture reacts for 1.5-2.5 hours at the temperature of 75-85 ℃, and the mixture is washed and dried, so that PPS-rG is obtained. Wherein the mass ratio of the aminated polyphenylene sulfide to the oxidized graphene is 1: 1-1.5: 1. The mass ratio of hydrazine hydrate to graphene oxide is 20: 1-50: 1.
Structural analysis and performance characterization of reduced graphene oxide grafted aminated polyphenylene sulfide composite material
1. Infrared spectroscopic analysis
FIG. 1 is an infrared spectrum of a graphene oxide, aminated polyphenylene sulfide and PPS-rG composite material, and it can be found that in the composite material, the original graphene oxide shows a spectrum ranging from 3680 to 1860 cm -1 Corresponding to the hydroxyl functional groups on the surface of the graphene oxide. At 1720, 1617, 1048 and 970 cm -1 FT-IR peaks at (a) are associated with C = O, C = C, C-OH and C = C bonds, respectively, at PPS-NH 2 In the spectrum, several new peaks, two at 3460 cm, were found -1 And 3366 cm -1 Belongs to asymmetric and symmetric N-H stretching vibration. The composite material PPS-rG discovers that characteristic peaks of graphene oxide and aminated polyphenylene sulfide in an infrared spectrogram exist, and the successful preparation of the composite material is confirmed.
2、PPS-NH 2 SEM image of, GO and composite material PPS-rG
FIG. 2 shows aminated polyphenylene sulfide, graphite oxideThe SEM image of the alkene and PPS-rG composite material is shown in the figure 2a, the SEM image of aminated polyphenylene sulfide can be found, the aminated polyphenylene sulfide is flat in appearance and has smaller micropores, GO is found to exist in a layered structure form in the figure 2b, and a PPS-rG structure coating is found to be accompanied with the appearance of lamellar sheets on an original PPS compact coating in the figure 2c, because the GO sheet layer is grafted to PPS-NH 2 In addition, the corrosion path is greatly prolonged, and the corrosion rate is delayed. This is also fully demonstrated by the partial enlargement of PPS-rG in 2 d.
3、 PPS-NH 2 PPS-rG electrochemical stability
FIG. 3 is a Bode diagram of aminated polyphenylene sulfide, acid-base composite coating. It can be seen that PPS-NH 2 After the coating is soaked in acid and alkali for a certain time, the coating is in certain shedding and bulging, the PPS-rG composite coating is still observed to be tightly combined on the substrate after being soaked in acid and alkali, the electrochemical performance of the composite coating is measured, the phase margin of the PPS-rG composite coating is found to be larger than 0 in a Bode diagram, the reduction frequency of the impedance of the composite coating is basically unchanged after the composite coating is soaked, and a larger impedance value is still kept. Therefore, it was revealed that PPS-rG had excellent electrochemical stability.
4. Impedance performance of reduced graphene oxide grafted aminated polyphenylene sulfide composite material
FIG. 4 shows PPS-NH 2 Potentiodynamic polarization curves of GO and PPS-rG composite materials and composite materials with different contents thereof. The test solution was a 3.5% NaCl solution, and the test items were: polarization curve, corrosion potential, corrosion current. The data obtained as shown in FIG. 4 were analyzed as follows, pure PPS-NH when not doped 2 The corrosion potential Ec of (1) Ec = -601mV, and the corrosion current ic = 2.502 × 10 -4 A/cm 2 High corrosion current values indicate PPS-NH 2 The corrosion resistance of (2) is not good. GO has the corrosion potential of 583mV and the corrosion current ic =1.134 x 10 -3 。PPS-NH 2 When the mass ratio of the composite material to GO is 1:1, the corrosion potential of the composite material is Ec = -603mV, and the corrosion current is ic = 1.832 multiplied by 10 -4 A/cm 2 The corrosion current becomes lower, the corrosion resistance of the composite coating is improved, and the corrosion rate is slightly slowed down. PPS-NH 2 And GOThe corrosion potential is-576 mV and the corrosion current value is ic =6.171 × 10 when the mass ratio is 1.1: 1 -5 A/cm 2 The corrosion current is lower, when the mass ratio is 1.2:1, the corrosion potential is-462 mV, and the corrosion current is 2.042 multiplied by 10 -7 A/cm 2 The electrochemical corrosion resistance is optimal when the electrochemical corrosion resistance is the highest corrosion potential and the lowest corrosion current. When PPS-NH 2 When the mass ratio of the metal oxide to GO is 1.3:1, the corrosion potential is-558 mV, and the corrosion current is 3.25 multiplied by 10 -6 A/cm 2 When the mass ratio is further increased to 1.5:1, the corrosion potential is-580 mV, and the corrosion current becomes ic =8.82 × 10 -6 A/cm 2 But relative to pure PPS-NH 2 The corrosion resistance is higher than pure PPS-NH 2 Much higher. In conclusion, the PPS-rG content ratio is 1.2:1, and the composite coating has the best corrosion resistance.
The invention has the beneficial effects that:
(1) according to the preparation method, graphene oxide and aminated polyphenylene sulfide are used as raw materials to prepare the redox graphene oxide grafted aminated polyphenylene sulfide composite material PPS-GO, and then the redox graphene oxide grafted aminated polyphenylene sulfide composite material PPS-rG is obtained through reduction by hydrazine hydrate. The graphene oxide has a large lamellar structure, has more functional groups which are easy to be subjected to organic matter action and grafting, and the large lamellar structure is grafted on the aminated polyphenylene sulfide, so that the effect of blocking corrosive substances can be achieved in a coating, and the corrosion path of the coating is prolonged, thereby improving the anticorrosion effect. The graphene oxide is of a large lamellar structure, physical barrier is stronger, conductivity is poorer than that of graphene quantum dots, and electrochemical corrosion resistance of the graphene oxide is more excellent.
(2) The reduced graphene oxide further reduced by hydrazine hydrate has better stability, fewer groups on the reduced graphene oxide, better structural stability, high-temperature heat resistance and the like than the reduced graphene oxide, and the finally obtained material has better comprehensive performance and electrochemical stability. And the reduction mode of hydrazine hydrate is green and environment-friendly.
(3) Different from physical doping, the graphene oxide is linked with aminated polyphenylene sulfide through chemical amide bondAre branched together and a part of the PPS-NH can be doped in the molten mixture 2 The flat surface is attached with a layered structure, so that the surface is more compact, and meanwhile, the large lamellar graphene oxide doped in the layered structure can prolong the corrosion path of the ionic medium, so that the corrosion resistance is improved. Because the coating is simple to prepare, has lower corrosion current density and more excellent corrosion resistance, the coating can be ultrasonically dispersed into ethanol to be used as a coating to be sprayed on the surface of metal, can play a role in protecting the surface of the metal, and has wide application prospect in the environment of corrosion resistance and pollution resistance.
Drawings
FIG. 1 is an infrared spectrum of aminated PPS, graphene oxide, and composites thereof.
Fig. 2 is an SEM image of aminated PPS, graphene oxide, and composite coatings thereof.
FIG. 3 is a Bode diagram of aminated polyphenylene sulfide, acid-base composite coating.
FIG. 4 is a potentiodynamic polarization curve diagram of graphene oxide grafted aminated polyphenylene sulfide composite coatings with different content ratios.
Detailed Description
The preparation and properties of the reduced graphene oxide grafted aminated polyphenylene sulfide composite material of the present invention are further illustrated by the following specific examples
Example 1
(1) Preparation of aminated polyphenylene sulfide: weighing 86.7 g of sodium sulfide nonahydrate, adding into 250mL of N-dimethyl pyrrolidone, reacting for 1.5 h at 160 ℃ in a nitrogen atmosphere to obtain a green anhydrous sodium sulfide solution, and pouring into a reaction kettle while the solution is hot; then weighing 0.2 g of catalyst isopropyl titanate, 60.13 g of p-dichlorobenzene and 5.5 g of 2, 5-dichloroaniline, adding the catalyst isopropyl titanate, introducing nitrogen, removing air in the kettle, reacting at 270 ℃ for 2 hours, repeatedly washing with deionized water and ethanol after the reaction is finished, carrying out hot filtration at 50 ℃, and freeze-drying to obtain aminated polyphenylene sulfide, which is marked as PPS-NH 2 。
(2) Preparing graphene oxide: taking 0.1g of the prepared expanded graphite, uniformly mixing and dispersing in 100ml of MAF solution, and then, addingUltrasonically stripping for 24h under the condition of high-power ultrasound, filtering, washing and drying the obtained product to obtain a liquid-phase ultrasonically stripped graphite sheet, then adding 1g of the prepared graphite sheet into mixed acid at 0 ℃ (90 mL of concentrated sulfuric acid and 30mL of concentrated phosphoric acid are mixed in an ice-water bath), continuously stirring the mixture, maintaining the temperature of the ice-water bath, and slowly adding 9g of KMnO 4， After the addition was complete, the reaction was allowed to continue stirring at 50 ℃ for 12 h. After the completion of the above reaction, 200mL of ice water and 5mL of 30% H were added to the mixed solution at room temperature 2 O 2 And (3) observing the solution, wherein the color of the solution gradually changes from purple red to golden yellow, separating, filtering, washing and drying the solution to obtain the graphene oxide.
(3) Preparing a reduced graphene oxide grafted aminated polyphenylene sulfide composite material: firstly, 0.083 g of graphene oxide is ultrasonically dispersed and dissolved in 50mL of tetrahydrofuran solution, the mixture is ultrasonically treated for 1 h to obtain a good dispersion state, then 0.1g of aminated polyphenylene sulfide is slowly added into the solution, magnetic stirring is carried out for 12h at the temperature of 50 ℃ to obtain PPS-GO, then 2-3 mL of hydrazine hydrate is dropwise added into the prepared PPS-GO to react for 2h at the temperature of 80 ℃ to obtain PPS-rG (1.2: 1).
(4) Testing of Corrosion resistance
Coating the composite coating according to GB/T1727 and 1992 general preparation method of coating, wherein the specific method comprises the steps of dispersing the composite material into ethanol at normal temperature, and then carrying out ultrasonic treatment to obtain the anticorrosive coating; the anticorrosive paint with the optimal proportion is sprayed on clean and dry tinplate with the size of 20 multiplied by 50 multiplied by 1 mm, and is cured for 3 hours in a tube furnace at 320 ℃, and then an anticorrosive test is carried out. The corrosion resistance is tested as shown in FIG. 3, the corrosion potential is-462 mV, and the corrosion current is ic = 2.042 × 10 -7 A/cm 2 。
Example 2
(1) Preparation of aminated polyphenylene sulfide: the same as in example 1.
(2) Preparing graphene oxide: the same as in example 1.
(3) Preparing a reduced graphene oxide grafted aminated polyphenylene sulfide composite material: firstly, 0.1g of graphene oxide is ultrasonically dispersed and dissolved in 50mL of tetrahydrofuran solution, the mixture is ultrasonically treated for 1 h to obtain a good dispersion state, then 0.1g of aminated polyphenylene sulfide is slowly added into the solution, magnetic stirring is carried out for 12h at the temperature of 50 ℃ to obtain PPS-GO, and then 2-3 mL of hydrazine hydrate is dropwise added into the prepared PPS-GO to react for 2h at the temperature of 80 ℃ to obtain PPS-rG (1: 1).
(4) And (3) testing the corrosion resistance: the specific operation is the same as in example 1; the corrosion resistance test is shown in FIG. 3, the corrosion potential Ec = -603mV, and the corrosion current is ic = 1.832 × 10 -4 A/cm 2 。
Example 3
(1) Preparation of aminated polyphenylene sulfide: the same as in example 1.
(2) Preparing graphene oxide: the same as in example 1.
(3) Preparing a reduced graphene oxide grafted aminated polyphenylene sulfide composite material: preparing a redox graphene oxide grafted aminated polyphenylene sulfide composite material: firstly, 0.091 g of graphene oxide is ultrasonically dispersed and dissolved in 50mL of tetrahydrofuran solution, the mixture is ultrasonically treated for 1 h to obtain a good dispersion state, then 0.1g of aminated polyphenylene sulfide is slowly added into the solution, magnetic stirring is carried out for 12h at the temperature of 50 ℃ to obtain PPS-GO, then 2-3 mL of hydrazine hydrate is dropwise added into the prepared PPS-GO to react for 2h at the temperature of 80 ℃ to obtain PPS-rG (1.1: 1).
(4) And (3) testing the corrosion resistance: the specific operation is the same as in example 1; the corrosion resistance test is shown in FIG. 3, the corrosion potential Ec = -576mV, and the corrosion current ic =6.171 × 10 -5 A/cm 2 。
Example 4
(1) Preparation of aminated polyphenylene sulfide: the same as in example 1.
(2) Preparing graphene oxide: example 1.
(3) Preparing a reduced graphene oxide grafted aminated polyphenylene sulfide composite material: preparing a redox graphene oxide grafted aminated polyphenylene sulfide composite material: firstly, 0.077 g of graphene oxide is ultrasonically dispersed and dissolved in 50mL of tetrahydrofuran solution, the mixture is ultrasonically treated for 1 h to obtain a good dispersion state, then 0.1g of aminated polyphenylene sulfide is slowly added into the solution, the mixture is magnetically stirred for 12h at the temperature of 50 ℃ to obtain PPS-GO, and then 2-3 mL of hydrazine hydrate is dropwise added into the prepared PPS-GO to react for 2h at the temperature of 80 ℃ to obtain PPS-rG (1.3: 1).
(4) And (3) testing the corrosion resistance: the specific operation was the same as in example 1; the corrosion resistance is tested as shown in FIG. 3, the corrosion potential Ec = -558mV, and the corrosion current ic = 3.25 × 10 -6 A/cm 2 。
Example 5
(1) Preparation of aminated polyphenylene sulfide: the same as in example 1.
(2) Preparing graphene oxide: example 1.
(3) Preparing a reduced graphene oxide grafted aminated polyphenylene sulfide composite material: preparing a redox graphene oxide grafted aminated polyphenylene sulfide composite material: firstly, 0.067g of graphene oxide is ultrasonically dispersed and dissolved in 50mL of tetrahydrofuran solution, the ultrasonic treatment is carried out for 1 h to obtain a good dispersion state, then 0.1g of aminated polyphenylene sulfide is slowly added into the solution, magnetic stirring is carried out for 12h at the temperature of 50 ℃ to obtain PPS-GO, then 2-3 mL of hydrazine hydrate is dripped into the prepared PPS-GO to react for 2h at the temperature of 80 ℃ to obtain PPS-rG (1.5: 1).
(4) And (3) testing the corrosion resistance: the specific operation was the same as in example 1; as shown in FIG. 3, the corrosion resistance test shows that the corrosion potential Ec = -580mV, and the corrosion current ic =8.82 × 10 -6 A/cm 2 。
Claims (7)
1. A preparation method of a reduced graphene oxide grafted aminated polyphenylene sulfide composite material comprises the following process steps:
(1) preparation of aminated polyphenylene sulfide: anhydrous sodium sulfide, p-dichlorobenzene and 2, 5-dichloroaniline are used as raw materials, N-methyl pyrrolidone is used as a solvent, isopropyl titanate is used as a catalyst, nitrogen is used as a protective gas, the reaction is carried out for 1.5 to 2.5 hours at 260 to 280 ℃ in an alkaline environment, and the sample is washed, filtered and dried to obtain aminated polyphenylene sulfide;
(2) preparing a reduced graphene oxide grafted aminated polyphenylene sulfide composite material: firstly, graphene oxide is ultrasonically dispersed and dissolved in a tetrahydrofuran solution, aminated polyphenylene sulfide is added after uniform ultrasonic dispersion, stirring and reaction are carried out for 10-12 hours at the temperature of 45-55 ℃, PPS-GO is obtained, hydrazine hydrate is added, reaction is carried out for 1.5-2.5 hours at the temperature of 75-85 ℃, and PPS-rG is obtained after washing and drying.
2. The method for preparing a reduced graphene oxide grafted aminated polyphenylene sulfide composite material according to claim 1, wherein: in the step (1), the mass ratio of the 2, 5-dichloroaniline to the anhydrous sodium sulfide is 1: 10-1: 15.
3. The method of claim 1, wherein the reduced graphene oxide grafted aminated polyphenylene sulfide composite material comprises: in the step (1), the mass ratio of the 2, 5-dichloroaniline to the p-dichlorobenzene is 1: 10-1: 12.
4. The method for preparing a reduced graphene oxide grafted aminated polyphenylene sulfide composite material according to claim 1, wherein: in the step (1), the mass ratio of the 2, 5-dichloroaniline to the isopropyl titanate is 1: 0.8-1: 1.
5. The method of claim 1, wherein the reduced graphene oxide grafted aminated polyphenylene sulfide composite material comprises: in the step (2), the mass ratio of the aminated polyphenylene sulfide to the oxidized graphene is 1: 1-1.5: 1.
6. The method for preparing a reduced graphene oxide grafted aminated polyphenylene sulfide composite material according to claim 1, wherein: in the step (2), the mass ratio of hydrazine hydrate to graphene oxide is 20: 1-50: 1.
7. Use of a reduced graphene oxide grafted aminated polyphenylene sulfide composite material prepared according to the method of claim 1 for the preparation of an anticorrosive coating.
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| CN105153614A (en) * | 2015-08-26 | 2015-12-16 | 苏州卓伟企业管理咨询有限公司 | Method for manufacturing modified graphene oxide/PMMA (polymethyl methacrylate) composite materials |
| CN110194839A (en) * | 2019-06-25 | 2019-09-03 | 西北师范大学 | A kind of preparation and application of graphene quantum dot/polyphenyl thioether composite material |
| CN114410218A (en) * | 2022-02-23 | 2022-04-29 | 西北师范大学 | Preparation method of polyvinylidene fluoride/aminated polyphenylene sulfide/stearic acid-titanium dioxide composite coating |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115678279A (en) * | 2022-11-15 | 2023-02-03 | 扬州万盛实业有限公司 | Graphene network reinforced polyphenylene sulfide conductive composite material and preparation method thereof |
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