Anti-scale desulfurizer and preparation method thereof

By using anti-scaling and desulfurization agent composed of triazine-based quaternized graphene, modified phenolic resin and activated carbon, the problems of pipeline blockage and poor anti-scaling effect caused by existing desulfurization agents are solved, and efficient desulfurization and prevention are achieved The scale effect improves the smoothness and corrosion resistance of the equipment.

CN119144354AInactive Publication Date: 2024-12-17BINZHOU QIANKUN CHEM MASCH CO LTD

Patent Information

Application Number
CN202411653932.6
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-19
Publication Date
2024-12-17
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

Although existing desulfurization agents can effectively remove hydrogen sulfide gas in oil field development, long-term use will lead to pipeline blockage and lack of anti-scaling effect.

Method used

The anti-scaling and desulfurization agent composed of triazine-based quaternized graphene, modified phenolic resin and activated carbon is prepared by a specific synthetic method, and the adsorption of graphene and hydrogen bonding of modified phenolic resin are used to form a phase. Capacitance, improve desulfurization and anti-scaling properties.

Benefits of technology

It achieves good desulfurization efficiency and anti-scaling effect, significantly improving the smoothness of the pipeline and the anti-corrosion performance of the equipment.

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Abstract

The invention relates to the technical field of chemical desulfurization, and discloses an anti-scale desulfurizer and a preparation method thereof.Triazinyl quaternized graphene, modified phenolic resin, activated carbon and 5-hydroxytryptamine are added into a stirrer and stirred, and the anti-scale desulfurizer is obtained. Hydroxyl groups in the triazinyl quaternized graphene and carboxyl groups and hydroxyl groups in the modified phenolic resin form hydrogen bonds, the compatibility between the triazinyl quaternized graphene and the carboxyl groups and the hydroxyl groups in the modified phenolic resin is improved, the triazinyl, the phenolic resin and the graphene have a good adsorption effect on hydrogen sulfide gas, and meanwhile the agglomeration effect of the graphene is reduced. The triazinyl quaternized graphene contains biquaternary ammonium salt and a large amount of hydroxyl, and also has a good adsorption effect on hydrogen sulfide gas. Quaternary ammonium salt groups in the triazinyl quaternized graphene and carboxyl groups in the modified phenolic resin have a good anti-scaling effect, and synergistic anti-scaling is achieved.
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Description

Technical Field

[0001] The invention relates to the technical field of chemical desulfurization, in particular to an anti-scaling desulfurization agent and a preparation method thereof. Background Art

[0002] In the process of oil field development, hydrogen sulfide gas is produced due to the oxidation decomposition of microorganisms and the high-temperature cracking process. Hydrogen sulfide is a toxic and harmful acidic gas that is harmful to the human body and the environment, and has a certain corrosive effect on equipment. Therefore, desulfurization agents are needed for desulfurization, but long-term use of desulfurizers will cause blockage of pipelines. For example, the document "Evaluation of Modified Triazine Liquid Desulfurizers and Applications in Offshore Gas Fields" shows that the liquid triazine desulfurizer composed of modified triazine compounds, stabilizers, enhancers and organic solvents is significantly better than other liquid desulfurizer products in the desulfurization process of Bohai gas fields; however, its anti-scaling effect has not been improved. Summary of the invention

[0003] 1. Technical issues to be resolved In view of the deficiencies of the prior art, the present invention provides an anti-scaling desulfurization agent and a preparation method thereof, which has good desulfurization efficiency and anti-scaling effect.

[0004] (II) Technical solution To achieve the above objectives, the present invention provides the following technical solution: an anti-scaling and desulfurizing agent, comprising the following components by weight: 6-9 parts by weight of triazine-quaternized graphene, 5-10 parts by weight of modified phenolic resin, 10-16 parts by weight of activated carbon, and 11-14 parts by weight of 5-hydroxytryptamine.

[0005] Preferably, the preparation method of the triazine-quaternized graphene is: (1) 4-7 parts by weight of graphene oxide are ultrasonically dispersed in 60-85 parts by weight of thionyl chloride, and after being evenly dispersed, the mixture is reacted at 75-80° C. for 6-15 hours. After the reaction, the mixture is filtered, washed, and dried to obtain graphene chloride; 8-15 parts by weight of 2,4,6-trihydroxy-1,3,5-triazine and 2-4 parts by weight of graphene chloride are added to tetrahydrofuran solvent, and ultrasonically dispersed evenly. 0.01-0.02 parts by weight of a catalyst are continuously added, and the mixture is reacted at 15-35° C. for 7-9 hours. After the reaction, the mixture is cooled, centrifuged, and washed with deionized water to obtain an intermediate 1; the structure of graphene chloride is as follows:

[0006] (2) Add intermediate 1 and p-toluenesulfonyl chloride to N,N-dimethylformamide solvent, then add sodium hydroxide dropwise to control the pH of the reaction to 10-13, and stir the reaction at room temperature for 4-8 hours. After the reaction, remove low-boiling substances by distillation under reduced pressure, and wash the product with distilled water and acetone in turn to obtain intermediate 2; (3) adding 3-6 parts by weight of intermediate 2 and 8-15 parts by weight of diethanolamine to dichloromethane, and then adding 0.01-0.03 parts by weight of potassium carbonate catalyst, reacting at 65-90° C., and after the reaction, removing the solvent by distillation under reduced pressure, and washing with distilled water and dichloromethane by centrifugation in turn to obtain hydroxylated triazine-based quaternary graphene; (4) Add 4-7 parts by weight of hydroxylated triazine-based quaternary graphene and 14-20 parts by weight of 2-bromoethanol to N,N-dimethylformamide solvent, stir and disperse, and carry out quaternization reaction for 5-8 hours. After the reaction, perform rotary distillation, wash and dry to obtain triazine-based quaternized graphene.

[0007] Preferably, the catalyst in (1) is triethylamine.

[0008] Preferably, in said (2), the weight parts of intermediate 1 are 4-7, and the weight parts of p-toluenesulfonyl chloride are 12-18.

[0009] Preferably, the reaction time in (3) is 12-20 hours.

[0010] Preferably, the reaction temperature in (4) is 65-80°C.

[0011] Preferably, the preparation method of the modified phenolic resin is: S1. The phenolic resin and epichlorohydrin are mixed evenly, reacted at 65-80 ° C for 8-12 hours, and then concentrated under reduced pressure and washed to obtain an epoxidized phenolic resin; S2. Dissolve 4-10 parts by weight of epoxy phenolic resin in toluene solvent, then add 14-20 parts by weight of aminoacetic acid, stir evenly, and react at 100-110° C. for 3-5 hours. After completion, a modified phenolic resin is obtained.

[0012] Preferably, the mass ratio of the phenolic resin to epichlorohydrin is 1:5.1-6.8.

[0013] Preferably, the preparation method of the anti-scaling and desulfurizing agent is: adding triazine-based quaternized graphene, modified phenolic resin, activated carbon and 5-hydroxytryptamine into a stirrer, stirring for 6-10 minutes, and obtaining the anti-scaling and desulfurizing agent.

[0014] 3. Beneficial technical effects The invention prepares the anti-scaling and desulfurizing agent by adding triazine-based quaternized graphene, modified phenolic resin, activated carbon and 5-hydroxytryptamine into a stirrer and stirring the mixture.

[0015] The hydroxyl group in 2,4,6-trihydroxy-1,3,5-triazine reacts with the acyl chloride group in acyl chloride graphene to introduce graphene and hydroxyl groups, thereby obtaining intermediate 1; the hydroxyl group in intermediate 1 reacts with p-toluenesulfonyl chloride to obtain intermediate 2; intermediate 2 reacts with diethanolamine to introduce hydroxyl groups to obtain hydroxylated triazine-based quaternary graphene; the tertiary amine group in hydroxylated triazine-based quaternary graphene reacts with the bromine in 2-bromoethanol to quaternize, generate quaternary ammonium salt, and introduce hydroxyl groups to obtain triazine-based quaternized graphene. The phenolic hydroxyl group in phenolic resin and the chlorine in epichlorohydrin undergo substitution reaction to introduce epoxy groups to obtain epoxidized phenolic resin; the epoxy group in epoxy phenolic resin reacts with the amino group in aminoacetic acid to generate hydroxyl groups, and then introduces carboxyl groups to obtain modified phenolic resin.

[0016] The hydroxyl groups in triazine-quaternized graphene will form hydrogen bonds with the carboxyl and hydroxyl groups in the modified phenolic resin, increasing the compatibility between each other. The triazine group, phenolic resin, and graphene itself have a good adsorption effect on hydrogen sulfide gas, while also reducing the agglomeration effect of graphene; triazine-quaternized graphene contains diquaternary ammonium salts and a large amount of hydroxyl groups, which also have a good adsorption effect on hydrogen sulfide gas. The quaternary ammonium salt groups in triazine-quaternized graphene and the carboxyl groups in the modified phenolic resin have a good anti-scaling effect, and synergistic anti-scaling. DETAILED DESCRIPTION Example 1

[0017] (1) 4 parts by weight of graphene oxide are ultrasonically dispersed in 60 parts by weight of thionyl chloride, and after being evenly dispersed, the mixture is reacted at 75° C. for 6 hours. After the reaction, the mixture is filtered, washed, and dried to obtain graphene chloride; 8 parts by weight of 2,4,6-trihydroxy-1,3,5-triazine and 2 parts by weight of graphene chloride are added to tetrahydrofuran solvent, and ultrasonically dispersed evenly. 0.01 parts by weight of triethylamine catalyst are continuously added, and the mixture is reacted at 15° C. for 7 hours. After the reaction is completed, the mixture is cooled, centrifuged, and washed with deionized water to obtain intermediate 1; (2) 4 parts by weight of intermediate 1 and 12 parts by weight of p-toluenesulfonyl chloride were added to N,N-dimethylformamide solvent, and then sodium hydroxide was added dropwise to control the pH of the reaction to 10. The reaction was stirred at room temperature for 4 hours. After the reaction, low boiling points were removed by distillation under reduced pressure, and the product was washed with distilled water and acetone in turn to obtain intermediate 2; (3) adding 3 parts by weight of intermediate 2 and 8 parts by weight of diethanolamine to dichloromethane, and then adding 0.01 parts by weight of potassium carbonate catalyst, reacting at 65° C. for 12 hours, and then distilling off the solvent under reduced pressure after the reaction, centrifuging and washing with distilled water and dichloromethane in turn to obtain hydroxylated triazine-based quaternary graphene; (4) adding 4 parts by weight of hydroxylated triazine-based quaternary graphene and 14 parts by weight of 2-bromoethanol to N,N-dimethylformamide solvent, stirring and dispersing, and carrying out quaternization reaction at 65° C. for 5 h. After the reaction, rotary distillation is performed, and the quaternized triazine-based graphene is washed and dried to obtain the quaternized graphene; (5) 1 part by weight of phenolic resin and 5.1 parts by weight of epichlorohydrin were mixed uniformly, reacted at 65° C. for 8 h, and then concentrated under reduced pressure and washed to obtain an epoxidized phenolic resin; (6) dissolving 4 parts by weight of epoxy phenolic resin in toluene solvent, then adding 14 parts by weight of aminoacetic acid, stirring evenly, and reacting at 100° C. for 3 hours to obtain a modified phenolic resin; (7) 6 parts by weight of triazine quaternized graphene, 5 parts by weight of modified phenolic resin, 10 parts by weight of activated carbon, and 11 parts by weight of 5-hydroxytryptamine were added into a stirrer and stirred for 6 minutes to obtain an anti-scaling and desulfurization agent. Example 2

[0018] (1) Ultrasonic dispersion of 7 parts by weight of graphene oxide in 85 parts by weight of thionyl chloride, after uniform dispersion, react at 80° C. for 15 h, filter after reaction, wash, and dry to obtain graphene chloride; 15 parts by weight of 2,4,6-trihydroxy-1,3,5-triazine and 4 parts by weight of graphene chloride are added to tetrahydrofuran solvent, ultrasonic dispersion is uniform, and 0.02 parts by weight of triethylamine catalyst is added, react at 35° C. for 9 h, and after completion, the mixture is cooled, centrifuged, and washed with deionized water to obtain intermediate 1; (2) 7 parts by weight of intermediate 1 and 18 parts by weight of p-toluenesulfonyl chloride were added to N,N-dimethylformamide solvent, and then sodium hydroxide was added dropwise to control the pH of the reaction to 13. The reaction was stirred at room temperature for 8 hours. After the reaction, low boiling points were removed by distillation under reduced pressure, and the product was washed with distilled water and acetone in turn to obtain intermediate 2; (3) adding 6 parts by weight of intermediate 2 and 15 parts by weight of diethanolamine to dichloromethane, and then adding 0.03 parts by weight of potassium carbonate catalyst, reacting at 90° C. for 20 hours, and after the reaction, removing the solvent by distillation under reduced pressure, and washing with distilled water and dichloromethane by centrifugation in turn to obtain hydroxylated triazine-based quaternary graphene; (4) adding 7 parts by weight of hydroxylated triazine-based quaternary graphene and 20 parts by weight of 2-bromoethanol to N,N-dimethylformamide solvent, stirring and dispersing, and carrying out quaternization reaction at 80° C. for 8 h. After the reaction, rotary distillation is performed, and the quaternized triazine-based graphene is washed and dried to obtain the quaternized graphene; (5) 3 parts by weight of phenolic resin and 20.4 parts by weight of epichlorohydrin were uniformly mixed, reacted at 80° C. for 12 h, and then concentrated under reduced pressure and washed to obtain an epoxidized phenolic resin; (6) dissolving 10 parts by weight of epoxy phenolic resin in toluene solvent, then adding 20 parts by weight of aminoacetic acid, stirring evenly, and reacting at 110° C. for 5 hours to obtain a modified phenolic resin; (7) 9 parts by weight of triazine quaternized graphene, 10 parts by weight of modified phenolic resin, 16 parts by weight of activated carbon, and 14 parts by weight of 5-hydroxytryptamine were added into a stirrer and stirred for 10 minutes to obtain an anti-scaling and desulfurization agent. Example 3

[0019] (1) Ultrasonic dispersion of 5 parts by weight of graphene oxide in 70 parts by weight of thionyl chloride, after uniform dispersion, react at 78° C. for 12 hours, filter after reaction, wash, and dry to obtain graphene chloride; add 10 parts by weight of 2,4,6-trihydroxy-1,3,5-triazine and 3 parts by weight of graphene chloride to tetrahydrofuran solvent, ultrasonic dispersion, continue to add 0.015 parts by weight of triethylamine catalyst, react at 30° C. for 8 hours, cool after reaction, centrifuge, and wash with deionized water to obtain intermediate 1; (2) 6 parts by weight of intermediate 1 and 16 parts by weight of p-toluenesulfonyl chloride were added to N,N-dimethylformamide solvent, and then sodium hydroxide was added dropwise to control the pH of the reaction to 12. The reaction was stirred at room temperature for 6 hours. After the reaction, low boiling points were removed by distillation under reduced pressure, and the product was washed with distilled water and acetone in turn to obtain intermediate 2; (3) adding 5 parts by weight of intermediate 2 and 12 parts by weight of diethanolamine to dichloromethane, and then adding 0.02 parts by weight of potassium carbonate catalyst, reacting at 75° C. for 16 hours, and then distilling under reduced pressure to remove the solvent, and washing with distilled water and dichloromethane by centrifugation in turn to obtain hydroxylated triazine-based quaternary graphene; (4) adding 5 parts by weight of hydroxylated triazine-based quaternary graphene and 18 parts by weight of 2-bromoethanol to N,N-dimethylformamide solvent, stirring and dispersing, and carrying out quaternization reaction at 72° C. for 7 h. After the reaction, rotary distillation is performed, and the quaternized triazine-based graphene is washed and dried to obtain the quaternized graphene; (5) 2 parts by weight of phenolic resin and 16 parts by weight of epichlorohydrin were mixed evenly, reacted at 72° C. for 10 hours, and then concentrated under reduced pressure and washed to obtain an epoxidized phenolic resin; (6) dissolving 7 parts by weight of epoxy phenolic resin in toluene solvent, then adding 16 parts by weight of aminoacetic acid, stirring evenly, and reacting at 105° C. for 4 hours to obtain a modified phenolic resin; (7) 7 parts by weight of triazine quaternized graphene, 8 parts by weight of modified phenolic resin, 13 parts by weight of activated carbon, and 13 parts by weight of 5-hydroxytryptamine were added into a stirrer and stirred for 8 minutes to obtain an anti-scaling and desulfurization agent. Example 4

[0020] (1) 4 parts by weight of graphene oxide are ultrasonically dispersed in 60 parts by weight of thionyl chloride, and after being evenly dispersed, the mixture is reacted at 75° C. for 6 hours. After the reaction, the mixture is filtered, washed, and dried to obtain graphene chloride; 8 parts by weight of 2,4,6-trihydroxy-1,3,5-triazine and 2 parts by weight of graphene chloride are added to tetrahydrofuran solvent, and ultrasonically dispersed evenly. 0.01 parts by weight of triethylamine catalyst are continuously added, and the mixture is reacted at 15° C. for 7 hours. After the reaction is completed, the mixture is cooled, centrifuged, and washed with deionized water to obtain intermediate 1; (2) 4 parts by weight of intermediate 1 and 12 parts by weight of p-toluenesulfonyl chloride were added to N,N-dimethylformamide solvent, and then sodium hydroxide was added dropwise to control the pH of the reaction to 10. The reaction was stirred at room temperature for 4 hours. After the reaction, low boiling points were removed by distillation under reduced pressure, and the product was washed with distilled water and acetone in turn to obtain intermediate 2; (3) adding 6 parts by weight of intermediate 2 and 15 parts by weight of diethanolamine to dichloromethane, and then adding 0.03 parts by weight of potassium carbonate catalyst, reacting at 90° C. for 20 hours, and after the reaction, removing the solvent by distillation under reduced pressure, and washing with distilled water and dichloromethane by centrifugation in turn to obtain hydroxylated triazine-based quaternary graphene; (4) adding 7 parts by weight of hydroxylated triazine-based quaternary graphene and 20 parts by weight of 2-bromoethanol to N,N-dimethylformamide solvent, stirring and dispersing, and carrying out quaternization reaction at 80° C. for 8 h. After the reaction, rotary distillation is performed, and the quaternized triazine-based graphene is washed and dried to obtain the quaternized graphene; (5) 2 parts by weight of phenolic resin and 16 parts by weight of epichlorohydrin were mixed evenly, reacted at 72° C. for 10 hours, and then concentrated under reduced pressure and washed to obtain an epoxidized phenolic resin; (6) dissolving 7 parts by weight of epoxy phenolic resin in toluene solvent, then adding 16 parts by weight of aminoacetic acid, stirring evenly, and reacting at 105° C. for 4 hours to obtain a modified phenolic resin; (7) 7 parts by weight of triazine quaternized graphene, 8 parts by weight of modified phenolic resin, 13 parts by weight of activated carbon, and 13 parts by weight of 5-hydroxytryptamine were added into a stirrer and stirred for 8 minutes to obtain an anti-scaling and desulfurization agent. Example 5

[0021] (1) Ultrasonic dispersion of 7 parts by weight of graphene oxide in 85 parts by weight of thionyl chloride, after uniform dispersion, react at 80° C. for 15 h, filter after reaction, wash, and dry to obtain graphene chloride; 15 parts by weight of 2,4,6-trihydroxy-1,3,5-triazine and 4 parts by weight of graphene chloride are added to tetrahydrofuran solvent, ultrasonic dispersion is uniform, and 0.02 parts by weight of triethylamine catalyst is added, react at 35° C. for 9 h, and after completion, the mixture is cooled, centrifuged, and washed with deionized water to obtain intermediate 1; (2) 7 parts by weight of intermediate 1 and 18 parts by weight of p-toluenesulfonyl chloride were added to N,N-dimethylformamide solvent, and then sodium hydroxide was added dropwise to control the pH of the reaction to 13. The reaction was stirred at room temperature for 8 hours. After the reaction, low boiling points were removed by distillation under reduced pressure, and the product was washed with distilled water and acetone in turn to obtain intermediate 2; (3) adding 5 parts by weight of intermediate 2 and 12 parts by weight of diethanolamine to dichloromethane, and then adding 0.02 parts by weight of potassium carbonate catalyst, reacting at 75° C. for 16 hours, and then distilling under reduced pressure to remove the solvent, and washing with distilled water and dichloromethane by centrifugation in turn to obtain hydroxylated triazine-based quaternary graphene; (4) adding 5 parts by weight of hydroxylated triazine-based quaternary graphene and 18 parts by weight of 2-bromoethanol to N,N-dimethylformamide solvent, stirring and dispersing, and carrying out quaternization reaction at 72° C. for 7 h. After the reaction, rotary distillation is performed, and the quaternized triazine-based graphene is washed and dried to obtain the quaternized graphene; (5) 1 part by weight of phenolic resin and 5.1 parts by weight of epichlorohydrin were mixed uniformly, reacted at 65° C. for 8 h, and then concentrated under reduced pressure and washed to obtain an epoxidized phenolic resin; (6) dissolving 4 parts by weight of epoxy phenolic resin in toluene solvent, then adding 14 parts by weight of aminoacetic acid, stirring evenly, and reacting at 100° C. for 3 hours to obtain a modified phenolic resin; (7) 6 parts by weight of triazine quaternized graphene, 5 parts by weight of modified phenolic resin, 10 parts by weight of activated carbon, and 11 parts by weight of 5-hydroxytryptamine were added into a stirrer and stirred for 6 minutes to obtain an anti-scaling and desulfurization agent.

[0022] Comparative Example 1 This comparative example is compared with Example 5, except that no triazine-based quaternized graphene is added.

[0023] Comparative Example 2 The difference between this comparative example and Example 5 is that no modified phenolic resin is added.

[0024] The desulfurization rate test was carried out with reference to ASTM D4810-88 (1999) "Standard Method for Determination of Hydrogen Sulfide Content in Natural Gas by Colorimetric Detector Tube Method". The test results are shown in Table 1.

[0025] Table 1: Desulfurization rate test.

[0026] project Desulfurization rate (%) Example 1 98.8 Example 2 99.7 Example 3 98.6 Example 4 99.2 Example 5 98.7 Comparative Example 1 94.3 Comparative Example 2 94.1 It can be seen from Table 1 that Examples 1-5 of the present invention have better desulfurization efficiency than Comparative Examples 1-2.

[0027] Refer to SY / T5673-1993 Performance evaluation method of antiscalant for oil field to carry out antiscaling test.

[0028] Table 2: Antifouling test.

[0029] project Anti-scaling rate (%) Example 1 87.2 Example 2 89.6 Example 3 88.5 Example 4 87.7 Example 5 88.1 Comparative Example 1 80.3 Comparative Example 2 81.4 It can be seen from Table 2 that Examples 1-5 of the present invention have a better anti-scaling rate than Comparative Examples 1-2.

[0030] The preferred embodiments of the present invention disclosed above are only used to help illustrate the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to the specific implementation methods described. Obviously, many modifications and changes can be made according to the content of this specification. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and use the present invention well. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. An anti-scaling and desulfurizing agent, characterized in that: The invention comprises the following components by weight: 6-9 parts by weight of triazine-based quaternized graphene, 5-10 parts by weight of modified phenolic resin, 10-16 parts by weight of activated carbon, and 11-14 parts by weight of 5-hydroxytryptamine.

2. The anti-scaling and desulfurizing agent according to claim 1, characterized in that: The preparation method of the triazine-based quaternized graphene is as follows: (1) Ultrasonic dispersion of 4-7 parts by weight of graphene oxide in 60-85 parts by weight of thionyl chloride, after uniform dispersion, react at 75-80° C. for 6-15 hours, filter after reaction, wash, and dry to obtain graphene chloride; add 8-15 parts by weight of 2,4,6-trihydroxy-1,3,5-triazine and 2-4 parts by weight of graphene chloride to tetrahydrofuran solvent, ultrasonic dispersion, continue to add 0.01-0.02 parts by weight of catalyst, react at 15-35° C. for 7-9 hours, cool after reaction, centrifuge, and wash with deionized water to obtain intermediate 1; (2) Add intermediate 1 and p-toluenesulfonyl chloride to N,N-dimethylformamide solvent, then add sodium hydroxide dropwise to control the pH of the reaction to 10-13, and stir the reaction at room temperature for 4-8 hours. After the reaction, remove low-boiling substances by distillation under reduced pressure, and wash the product with distilled water and acetone in turn to obtain intermediate 2; (3) adding 3-6 parts by weight of intermediate 2 and 8-15 parts by weight of diethanolamine to dichloromethane, and then adding 0.01-0.03 parts by weight of potassium carbonate catalyst, reacting at 65-90° C., and after the reaction, removing the solvent by distillation under reduced pressure, and washing with distilled water and dichloromethane by centrifugation in turn to obtain hydroxylated triazine-based quaternary graphene; (4) Add 4-7 parts by weight of hydroxylated triazine-based quaternary graphene and 14-20 parts by weight of 2-bromoethanol to N,N-dimethylformamide solvent, stir and disperse, and carry out quaternization reaction for 5-8 hours. After the reaction, perform rotary distillation, wash and dry to obtain triazine-based quaternized graphene.

3. The anti-scaling and desulfurizing agent according to claim 2, characterized in that: The catalyst in (1) is triethylamine.

4. The anti-scaling and desulfurizing agent according to claim 2, characterized in that: In the above (2), the weight parts of the intermediate 1 are 4-7, and the weight parts of p-toluenesulfonyl chloride are 12-18.

5. The anti-scaling and desulfurizing agent according to claim 2, characterized in that: The reaction time in (3) is 12-20 hours.

6. The anti-scaling and desulfurizing agent according to claim 2, characterized in that: The reaction temperature in (4) is 65-80°C.

7. The anti-scaling and desulfurizing agent according to claim 1, characterized in that: The preparation method of the modified phenolic resin is: S1. The phenolic resin and epichlorohydrin are mixed evenly, reacted at 65-80 ° C for 8-12 hours, and then concentrated under reduced pressure and washed to obtain an epoxidized phenolic resin; S2. Dissolve 4-10 parts by weight of epoxy phenolic resin in toluene solvent, then add 14-20 parts by weight of aminoacetic acid, stir evenly, and react at 100-110° C. for 3-5 hours. After completion, a modified phenolic resin is obtained.

8. The anti-scaling and desulfurizing agent according to claim 7, characterized in that: The mass ratio of the phenolic resin to epichlorohydrin is 1:5.1-6.

8.

9. A method for preparing an anti-scaling and desulfurizing agent according to any one of claims 1 to 8, characterized in that: The preparation method of the anti-scaling and desulfurizing agent comprises the following steps: adding triazine-based quaternized graphene, modified phenolic resin, activated carbon and 5-hydroxytryptamine into a stirrer, stirring for 6-10 minutes, and obtaining the anti-scaling and desulfurizing agent.

Citation Information

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