A dispersible demulsifier and water-based additive for heavy oil and its preparation method

Abstract

This invention discloses a dispersible demulsifier and water-clearing agent for heavy oil and its preparation method. Using aromatic amines, polyvinyl alcohols, alkylamines, sulfonating agents, and carbon disulfide as raw materials, the invention first synthesizes aromatic polyetheramines from polyethers and aromatic amines. Then, chain extension is achieved through reaction with alkylamines, followed by reaction with sulfonating agents, and finally, reaction with carbon disulfide and sodium hydroxide to generate a dispersible demulsifier and water-clearing agent suitable for heavy oil fields. The prepared dispersible demulsifier and water-clearing agent exhibits good water-clearing effect, producing dense flocs and clear water, especially showing good results in treating oily wastewater from heavy oil.

Description

Technical Field

[0001] This invention relates to the field of heavy oil wastewater treatment technology, and in particular to a dispersible demulsifier and dewatering agent for heavy oil and its preparation method. Background Technology

[0002] In the current heavy oilfield development sector, the treatment of oily wastewater mainly relies on water purification agents such as polydimethyldiene ammonium chloride-acrylamide (PDADMA-AM) copolymer and methacryloyloxyethyltrimethylammonium chloride-acrylamide (DMC-AM) copolymer. However, with the rapid development of the heavy oil extraction industry and the widespread application of enhanced oil recovery technologies such as chemical flooding and steam flooding, the treatment of oily wastewater from heavy oil after primary separator treatment is becoming increasingly difficult.

[0003] The primary challenge lies in the high density of heavy oil, with a specific gravity close to that of water. Combined with natural emulsifiers and higher interfacial activity, this slows the separation rate of crude oil in separators and storage tanks, making oil-water separation far more difficult than with conventional oilfield emulsions, thus placing higher demands on the performance of reagents. Secondly, heavy oil has high viscosity, primarily due to the presence of gums and asphaltenes. The association and interaction between these macromolecules form a stable colloid. This colloidal coating results in a relatively stable oil-water emulsion, while conventional reagents exhibit poor dispersibility and wettability in such systems, making it difficult for the reagents to fully reach the oil-water emulsion interface and complete the demulsification process. Therefore, the performance requirements for demulsifying agents needed for treating oily wastewater from heavy oil are becoming increasingly stringent. Existing demulsifying agents generally suffer from insufficient performance, reduced demulsification efficiency, and excessive dosage. In addition, the sludge treated with existing agents tends to clump together and adhere to the walls of the inclined plate separator and the inner walls of the fluid transport pipeline, which not only reduces the separation efficiency of the equipment, but also increases the frequency and difficulty of tank cleaning and sludge removal operations. Summary of the Invention

[0004] In order to solve the above-mentioned technical problems, the present invention provides a dispersible demulsifier and water-integrated agent for heavy oil and its preparation method.

[0005] In a first aspect, the present invention provides a method for preparing a dispersible demulsifier and water-soluble agent for heavy oil, which is achieved by the following technical solution.

[0006] A method for preparing a dispersible demulsifier and water-soluble additive for heavy oil includes the following steps:

[0007] S1. Preparation of aromatic polyetheramines

[0008] Under stirring conditions, a mixture of aromatic amine and organic solvent is added dropwise to polyvinyl chloride. The temperature is controlled at 80℃~100℃. After the mixture of aromatic amine and organic solvent is added, the temperature is raised to 100℃~110℃ and kept at this temperature for 1~3 hours. Then the dynamic viscosity is measured. When the viscosity reaches 100~150CP, alkylamine is added to continue the reaction. The reaction temperature is controlled at 50℃~105℃ and the reaction time is 2~5 hours to obtain aromatic polyether amine.

[0009] S2. Preparation of a dispersible demulsifier / water-based integrated agent

[0010] The aromatic polyetheramine prepared in step S1 was mixed with deionized water at a mass ratio of 1:0.5 to 1:3.0. Then, a sulfonating agent was added dropwise while the reaction temperature was controlled at 50℃ to 80℃ and kept at that temperature for 1 to 2.5 hours. After that, an alkaline solution was added and stirred for 20 to 40 minutes. Then, carbon disulfide was added dropwise while the reaction temperature was controlled at 0℃ to 30℃. After the addition was completed, the temperature was raised to 30℃ to 40℃ and the reaction was continued for 5 to 7 hours. The mixture was then cooled to obtain a dispersible demulsifier and water-soluble agent.

[0011] Furthermore, in step S1, the aromatic amine is selected from one of 2,3-diaminophenolazine, 4-methoxyaniline, 4-methylaniline, benzidine, p-phenylenediamine, or diethyltoluenediamine.

[0012] Furthermore, in step S1, the molar ratio of the aromatic amine to the polyvinyl chloride is 1:20 to 1:30.

[0013] Furthermore, in step S1, the organic solvent accounts for 20 wt% to 45 wt% of the total reaction system.

[0014] Furthermore, in step S1, the organic solvent is selected from two of the following: methanol, ethanol, isopropanol, ethylene glycol, ethylene glycol methyl ether, ethylene glycol dimethyl ether, ethylene glycol ethyl ether, ethylene glycol diethyl ether, ethylene glycol monobutyl ether, diethylene glycol butyl ether, dipropylene glycol methyl ether, and propylene glycol methyl ether.

[0015] Furthermore, in step S1, the alkylamine is selected from one of diethylenetriamine, triethylenetetramine, tetraethylenepentamine, pentaethylenehexamine, hexaethyleneheptamine, heptaethyleneoctamine, octaethylenenonamine, nonaethylenedecamine, or polyethylenepolyamine.

[0016] Furthermore, in step S1, the molar ratio of alkylamine to polyvinyl chloride is 1:0.6 to 1:1.2.

[0017] Furthermore, in step S2, the sulfonating agent is selected from one of sodium 2-chloroethylsulfonate, chlorosulfonic acid, sodium sulfite, sodium bisulfite, aminosulfonic acid, or sodium 3-chloro-2-hydroxypropanesulfonate.

[0018] Furthermore, in step S2, the molar ratio of aromatic polyetheramine to carbon disulfide is 1:1.0 to 1:5.0.

[0019] Furthermore, in step S2, the amount of sulfonating agent is determined according to the amount of aromatic polyetheramine, and the molar ratio of sulfonating agent to aromatic polyetheramine is controlled to be 1:11 to 1:13.

[0020] Furthermore, in step S2, sodium hydroxide is selected as the alkali solution, and the amount of alkali solution added is determined based on controlling the system within the pH range of 9.5-12.5 after the carbon disulfide is added.

[0021] Furthermore, in step S2, the carbon disulfide is added over a time of 40-60 minutes.

[0022] Secondly, the present invention provides a dispersible demulsifier and water-integrated agent for heavy oil, which is achieved by the following technical solution.

[0023] A dispersible demulsifier and water-integrated agent for heavy oil prepared by the above preparation method.

[0024] This application has the following beneficial effects.

[0025] (1) The heavy oil dispersible demulsifier and water clarifying agent of the present invention has a dithiocarbamate anion structure, wherein the polar group –CSS- is a bidentate ligand with the ability to coordinate with most transition metal ions (except alkali and alkaline earth metals) to form supramolecular coordination structures. These structures further promote the formation of dense flocs, effectively purifying oily wastewater and making it clear.

[0026] (2) In heavy oil, gums and asphaltenes are the main factors leading to increased viscosity. The heavy oil dispersing demulsifier and water-soluble agent of the present invention introduces aromatic groups, which can change the polarity and hydrogen bond structure of gum and asphaltenes molecules, thereby dispersing the molecules in the heavy oil and effectively reducing its viscosity.

[0027] (3) The introduction of sulfonic acid groups into the heavy oil dispersible demulsifier and water-clearing agent of the present invention significantly improves the dispersibility and wettability of the agent in the heavy oil system. This allows the agent to penetrate the oil-water emulsion formed by colloidal coating in the heavy oil, making it easy to reach the interface of the oil-water emulsion, thereby efficiently completing the demulsification process. Detailed Implementation

[0028] The present patent application will be further described below with reference to the embodiments.

[0029] Unless otherwise specified, the experimental methods used in the following preparation examples and embodiments are conventional methods; the materials and reagents used in the following preparation examples and embodiments are commercially available unless otherwise specified.

[0030] The molecular weight of the polyvinyl chloride used in the following embodiments of this application is [missing information].

[0031] Example 1

[0032] A method for preparing a dispersible demulsifier and water-soluble additive for heavy oil includes the following steps:

[0033] Step 1: Preparation of Aromatic Polyetheramine

[0034] In a reactor equipped with a thermometer and a stirrer, polyvinyl chloride (22.2 g, 0.24 mol) was added, and stirring was started. A homogeneous mixture of 2,3-diaminophenolazine (2.1 g, 0.01 mol), ethylene glycol monobutyl ether (21.1 g), and ethylene glycol (21.0 g) was slowly added dropwise, with the temperature controlled at 90°C. After the aromatic amine mixture was completely added, the temperature was raised to 105°C and maintained at this temperature for 2.5 h. Subsequently, the dynamic viscosity was measured. When the viscosity reached 120 CP, triethylenetetramine (33.6 g, 0.23 mol) was added to continue the reaction at 65°C for 2 h. The final product was a clear, brownish-yellow color.

[0035] Step 2: Preparation of Dispersible Demulsifier and Water-Based Integrated Agent

[0036] In a reactor equipped with a thermometer and a stirrer, 100 g of aromatic polyetheramine (0.24 mol) and 100 g of deionized water were added. Sodium 2-chloroethylsulfonate (3.7 g, 0.02 mol) was slowly added dropwise, and the reaction temperature was controlled at 70 °C for 2 h. Then, sodium hydroxide (34.6 g) was added and stirred for 30 minutes. Carbon disulfide (54.7 g, 0.72 mol) was then added dropwise, and the reaction temperature was controlled at 25 °C. After the addition was complete, the temperature was raised to 30 °C and the reaction was continued for 6 h. The mixture was then cooled and discharged to obtain a clear, brownish-red liquid.

[0037] Example 2

[0038] A method for preparing a dispersible demulsifier and water-soluble additive for heavy oil includes the following steps:

[0039] Step 1: Preparation of Aromatic Polyetheramine

[0040] In a reactor equipped with a thermometer and a stirrer, polyvinyl chloride (22.2 g, 0.24 mol) was added, and stirring was started. A homogeneous mixture of p-phenylenediamine (1.1 g, 0.01 mol), ethylene glycol monobutyl ether (21.1 g), and ethylene glycol (21.0 g) was slowly added dropwise, with the temperature controlled at 90°C. After the aromatic amine mixture was completely added, the temperature was raised to 105°C and maintained at this temperature for 2.5 h. Subsequently, the dynamic viscosity was measured. When the viscosity reached 120 CP, triethylenetetramine (33.6 g, 0.23 mol) was added to continue the reaction at 65°C for 2 h. The final product was a clear, brownish-yellow color.

[0041] Step 2: Preparation of Dispersible Demulsifier and Water-Based Integrated Agent

[0042] In a reactor equipped with a thermometer and a stirrer, 100 g of aromatic polyetheramine (0.24 mol) and 100 g of deionized water were added. Sodium 2-chloroethylsulfonate (3.7 g, 0.02 mol) was slowly added dropwise, and the reaction temperature was controlled at 70 °C for 2 h. Then, sodium hydroxide (34.6 g) was added and stirred for 30 minutes. Carbon disulfide (54.7 g, 0.72 mol) was then added dropwise, and the reaction temperature was controlled at 25 °C. After the addition was complete, the temperature was raised to 30 °C and the reaction was continued for 6 h. The mixture was then cooled and discharged to obtain a clear, brownish-red liquid.

[0043] Example 3

[0044] A method for preparing a dispersible demulsifier and water-soluble additive for heavy oil includes the following steps:

[0045] Step 1: Preparation of Aromatic Polyetheramine

[0046] In a reactor equipped with a thermometer and a stirrer, polyvinyl chloride (22.2 g, 0.24 mol) was added, and stirring was started. A homogeneous mixture of diethyltoluene diamine (1.8 g, 0.01 mol), ethylene glycol monobutyl ether (21.1 g), and ethylene glycol (21.0 g) was slowly added dropwise, with the temperature controlled at 90°C. After the aromatic amine mixture was completely added, the temperature was raised to 105°C and maintained at this temperature for 2.5 h. Subsequently, the dynamic viscosity was measured. When the viscosity reached 120 CP, triethylenetetramine (33.6 g, 0.23 mol) was added to continue the reaction at 65°C for 2 h. The final product was a clear, brownish-yellow color.

[0047] Step 2: Preparation of Dispersible Demulsifier and Water-Based Integrated Agent

[0048] In a reactor equipped with a thermometer and a stirrer, 100 g of aromatic polyetheramine (0.24 mol) and 100 g of deionized water were added. Sodium 2-chloroethylsulfonate (3.7 g, 0.02 mol) was slowly added dropwise, and the reaction temperature was controlled at 70 °C for 2 h. Then, sodium hydroxide (34.6 g) was added and stirred for 30 minutes. Carbon disulfide (54.7 g, 0.72 mol) was then added dropwise, and the reaction temperature was controlled at 25 °C. After the addition was complete, the temperature was raised to 30 °C and the reaction was continued for 6 h. The mixture was then cooled and discharged to obtain a clear, brownish-red liquid.

[0049] Example 4

[0050] A method for preparing a dispersible demulsifier and water-soluble additive for heavy oil includes the following steps:

[0051] Step 1: Preparation of Aromatic Polyetheramine

[0052] In a reactor equipped with a thermometer and a stirrer, polyvinyl chloride (22.2 g, 0.24 mol) was added, and stirring was started. A homogeneous mixture of 2,3-diaminophenolazine (2.1 g, 0.01 mol), ethylene glycol monobutyl ether (21.1 g), and ethylene glycol (21.0 g) was slowly added dropwise, with the temperature controlled at 90°C. After the aromatic amine mixture was completely added, the temperature was raised to 105°C and maintained at this temperature for 2.5 h. Subsequently, the dynamic viscosity was measured. When the viscosity reached 120 CP, triethylenetetramine (33.6 g, 0.23 mol) was added to continue the reaction at 65°C for 2 h. The final product was a clear, brownish-yellow color.

[0053] Step 2: Preparation of Dispersible Demulsifier and Water-Based Integrated Agent

[0054] In a reactor equipped with a thermometer and a stirrer, 100 g of aromatic polyetheramine (0.24 mol) and 100 g of deionized water were added. Sodium 3-chloro-2-hydroxypropanesulfonate (3.9 g, 0.02 mol) was slowly added dropwise, and the reaction temperature was controlled at 70 °C for 2 h. Then, sodium hydroxide (34.6 g) was added and stirred for 30 minutes. Carbon disulfide (54.7 g, 0.72 mol) was then added dropwise, and the reaction temperature was controlled at 25 °C. After the addition was complete, the temperature was raised to 30 °C and the reaction was continued for 6 h. The mixture was then cooled and discharged to obtain a clear, brownish-red liquid.

[0055] Example 5

[0056] A method for preparing a dispersible demulsifier and water-soluble additive for heavy oil includes the following steps:

[0057] Step 1: Preparation of Aromatic Polyetheramine

[0058] In a reactor equipped with a thermometer and a stirrer, polyvinyl chloride (22.2 g, 0.24 mol) was added, and stirring was started. A homogeneous mixture of 2,3-diaminophenolazine (2.1 g, 0.01 mol), ethylene glycol ethyl ether (21.1 g), and ethanol (21.0 g) was slowly added dropwise, and the temperature was controlled at 90°C. After the aromatic amine mixture was completely added, the temperature was raised to 105°C and maintained at this temperature for 2.5 h. Subsequently, the dynamic viscosity was measured. When the viscosity reached 120 CP, triethylenetetramine (33.6 g, 0.23 mol) was added to continue the reaction at 65°C for 2 h. The final product was a clear, brownish-yellow color.

[0059] Step 2: Preparation of Dispersible Demulsifier and Water-Based Integrated Agent

[0060] In a reactor equipped with a thermometer and a stirrer, 100 g of aromatic polyetheramine (0.24 mol) and 100 g of deionized water were added. Sodium 3-chloro-2-hydroxypropanesulfonate (3.9 g, 0.02 mol) was slowly added dropwise, and the reaction temperature was controlled at 70 °C for 2 h. Then, sodium hydroxide (34.6 g) was added and stirred for 30 minutes. Carbon disulfide (54.7 g, 0.72 mol) was then added dropwise, and the reaction temperature was controlled at 25 °C. After the addition was complete, the temperature was raised to 30 °C and the reaction was continued for 6 h. The mixture was then cooled and discharged to obtain a clear, brownish-red liquid.

[0061] Example 6

[0062] A method for preparing a dispersible demulsifier and water-soluble additive for heavy oil includes the following steps:

[0063] Step 1: Preparation of Aromatic Polyetheramine

[0064] In a reactor equipped with a thermometer and a stirrer, polyvinyl chloride (22.2 g, 0.24 mol) was added, and stirring was started. A homogeneous mixture of 2,3-diaminophenolazine (2.5 g, 0.012 mol), ethylene glycol ethyl ether (21.1 g), and ethanol (21.0 g) was slowly added dropwise, and the temperature was controlled at 90°C. After the aromatic amine mixture was completely added, the temperature was raised to 105°C and maintained at this temperature for 2.5 h. Subsequently, the dynamic viscosity was measured. When the viscosity reached 120 CP, triethylenetetramine (33.6 g, 0.23 mol) was added to continue the reaction at 65°C for 2 h. The final product was a clear, brownish-yellow color.

[0065] Step 2: Preparation of Dispersible Demulsifier and Water-Based Integrated Agent

[0066] In a reactor equipped with a thermometer and a stirrer, 100 g of aromatic polyetheramine (0.24 mol) and 100 g of deionized water were added. Sodium 3-chloro-2-hydroxypropanesulfonate (3.9 g, 0.02 mol) was slowly added dropwise, and the reaction temperature was controlled at 70 °C for 2 h. Then, sodium hydroxide (34.6 g) was added and stirred for 30 minutes. Carbon disulfide (54.7 g, 0.72 mol) was then added dropwise, and the reaction temperature was controlled at 25 °C. After the addition was complete, the temperature was raised to 30 °C and the reaction was continued for 6 h. The mixture was then cooled and discharged to obtain a clear, brownish-red liquid.

[0067] Example 7

[0068] A method for preparing a dispersible demulsifier and water-soluble additive for heavy oil includes the following steps:

[0069] Step 1: Preparation of Aromatic Polyetheramine

[0070] In a reactor equipped with a thermometer and a stirrer, polyvinyl chloride (22.2 g, 0.24 mol) was added, and stirring was started. A homogeneous mixture of 2,3-diaminophenolazine (1.7 g, 0.008 mol), ethylene glycol ethyl ether (21.1 g), and ethanol (21.0 g) was slowly added dropwise, with the temperature controlled at 90°C. After the aromatic amine mixture was completely added, the temperature was raised to 105°C and maintained at this temperature for 2.5 h. Subsequently, the dynamic viscosity was measured. When the viscosity reached 120 CP, triethylenetetramine (33.6 g, 0.23 mol) was added to continue the reaction at 65°C for 2 h. The final product was a clear, brownish-yellow color.

[0071] Step 2: Preparation of Dispersible Demulsifier and Water-Based Integrated Agent

[0072] In a reactor equipped with a thermometer and a stirrer, 100 g of aromatic polyetheramine (0.24 mol) and 100 g of deionized water were added. Sodium 3-chloro-2-hydroxypropanesulfonate (3.9 g, 0.02 mol) was slowly added dropwise, and the reaction temperature was controlled at 70 °C for 2 h. Then, sodium hydroxide (34.6 g) was added and stirred for 30 minutes. Carbon disulfide (54.7 g, 0.72 mol) was then added dropwise, and the reaction temperature was controlled at 25 °C. After the addition was complete, the temperature was raised to 30 °C and the reaction was continued for 6 h. The mixture was then cooled and discharged to obtain a brownish-red transparent liquid.

[0073] Example 8

[0074] A method for preparing a dispersible demulsifier and water-soluble additive for heavy oil includes the following steps:

[0075] Step 1: Preparation of Aromatic Polyetheramine

[0076] In a reactor equipped with a thermometer and a stirrer, polyvinyl chloride (22.2 g, 0.24 mol) was added, and stirring was started. A homogeneous mixture of 2,3-diaminophenolazine (2.1 g, 0.01 mol), ethylene glycol ethyl ether (21.1 g), and ethanol (21.0 g) was slowly added dropwise, and the temperature was controlled at 90°C. After the aromatic amine mixture was completely added, the temperature was raised to 105°C and maintained at this temperature for 2.5 h. Subsequently, the dynamic viscosity was measured. When the viscosity reached 120 CP, triethylenetetramine (21.1 g, 0.144 mol) was added to continue the reaction at 65°C for 2 h. The final product was a clear, brownish-yellow color.

[0077] Step 2: Preparation of Dispersible Demulsifier and Water-Based Integrated Agent

[0078] In a reactor equipped with a thermometer and a stirrer, 100 g of aromatic polyetheramine (0.24 mol) and 100 g of deionized water were added. Sodium 3-chloro-2-hydroxypropanesulfonate (3.9 g, 0.02 mol) was slowly added dropwise, and the reaction temperature was controlled at 70 °C for 2 h. Then, sodium hydroxide (34.6 g) was added and stirred for 30 minutes. Carbon disulfide (54.7 g, 0.72 mol) was then added dropwise, and the reaction temperature was controlled at 25 °C. After the addition was complete, the temperature was raised to 30 °C and the reaction was continued for 6 h. The mixture was then cooled and discharged to obtain a clear, brownish-red liquid.

[0079] Example 9

[0080] A method for preparing a dispersible demulsifier and water-soluble additive for heavy oil includes the following steps:

[0081] Step 1: Preparation of Aromatic Polyetheramine

[0082] In a reactor equipped with a thermometer and a stirrer, polyvinyl chloride (22.2 g, 0.24 mol) was added, and stirring was started. A homogeneous mixture of 2,3-diaminophenolazine (2.1 g, 0.01 mol), ethylene glycol ethyl ether (21.1 g), and ethanol (21.0 g) was slowly added dropwise, and the temperature was controlled at 90°C. After the aromatic amine mixture was completely added, the temperature was raised to 105°C and maintained at this temperature for 2.5 h. Subsequently, the dynamic viscosity was measured. When the viscosity reached 120 CP, triethylenetetramine (42.1 g, 0.288 mol) was added to continue the reaction at 65°C for 2 h. The final product was a clear, brownish-yellow color.

[0083] Step 2: Preparation of Dispersible Demulsifier and Water-Based Integrated Agent

[0084] In a reactor equipped with a thermometer and a stirrer, 100 g of aromatic polyetheramine (0.24 mol) and 100 g of deionized water were added. Sodium 3-chloro-2-hydroxypropanesulfonate (3.9 g, 0.02 mol) was slowly added dropwise, and the reaction temperature was controlled at 70 °C for 2 h. Then, sodium hydroxide (34.6 g) was added and stirred for 30 minutes. Carbon disulfide (54.7 g, 0.72 mol) was then added dropwise, and the reaction temperature was controlled at 25 °C. After the addition was complete, the temperature was raised to 30 °C and the reaction was continued for 6 h. The mixture was then cooled and discharged to obtain a clear, brownish-red liquid.

[0085] Example 10

[0086] A method for preparing a dispersible demulsifier and water-soluble additive for heavy oil includes the following steps:

[0087] Step 1: Preparation of Aromatic Polyetheramine

[0088] In a reactor equipped with a thermometer and a stirrer, polyvinyl chloride (22.2 g, 0.24 mol) was added, and stirring was started. A homogeneous mixture of 2,3-diaminophenolazine (2.1 g, 0.01 mol), ethylene glycol monobutyl ether (21.1 g), and ethylene glycol (21.0 g) was slowly added dropwise, with the temperature controlled at 90°C. After the aromatic amine mixture was completely added, the temperature was raised to 105°C and maintained at this temperature for 2.5 h. Subsequently, the dynamic viscosity was measured. When the viscosity reached 120 CP, triethylenetetramine (33.6 g, 0.23 mol) was added to continue the reaction at 65°C for 2 h. The final product was a clear, brownish-yellow color.

[0089] Step 2: Preparation of Dispersible Demulsifier and Water-Based Integrated Agent

[0090] In a reactor equipped with a thermometer and a stirrer, 100 g of aromatic polyetheramine (0.24 mol) and 100 g of deionized water were added. Sodium 3-chloro-2-hydroxypropanesulfonate (3.9 g, 0.02 mol) was slowly added dropwise, and the reaction temperature was controlled at 70 °C for 2 h. Then, sodium hydroxide (11.52 g) was added and stirred for 30 minutes. Carbon disulfide (18.2 g, 0.24 mol) was then added dropwise, and the reaction temperature was controlled at 25 °C. After the addition was complete, the temperature was raised to 30 °C and the reaction was continued for 6 h. The mixture was then cooled and discharged to obtain a clear, brownish-red liquid.

[0091] Example 11

[0092] A method for preparing a dispersible demulsifier and water-soluble additive for heavy oil includes the following steps:

[0093] Step 1: Preparation of Aromatic Polyetheramine

[0094] In a reactor equipped with a thermometer and a stirrer, polyvinyl chloride (22.2 g, 0.24 mol) was added, and stirring was started. A homogeneous mixture of 2,3-diaminophenolazine (2.1 g, 0.01 mol), ethylene glycol monobutyl ether (21.1 g), and ethylene glycol (21.0 g) was slowly added dropwise, with the temperature controlled at 90°C. After the aromatic amine mixture was completely added, the temperature was raised to 105°C and maintained at this temperature for 2.5 h. Subsequently, the dynamic viscosity was measured. When the viscosity reached 120 CP, triethylenetetramine (33.6 g, 0.23 mol) was added to continue the reaction at 65°C for 2 h. The final product was a clear, brownish-yellow color.

[0095] Step 2: Preparation of Dispersible Demulsifier and Water-Based Integrated Agent

[0096] In a reactor equipped with a thermometer and a stirrer, 100 g of aromatic polyetheramine (0.24 mol) and 100 g of deionized water were added. Sodium 3-chloro-2-hydroxypropanesulfonate (3.9 g, 0.02 mol) was slowly added dropwise, and the reaction temperature was controlled at 70 °C for 2 h. Then, sodium hydroxide (46.08 g) was added and stirred for 30 minutes. Carbon disulfide (73.0 g, 0.96 mol) was then added dropwise, and the reaction temperature was controlled at 25 °C. After the addition was complete, the temperature was raised to 30 °C and the reaction was continued for 6 h. The mixture was then cooled and discharged to obtain a clear, brownish-red liquid.

[0097] Performance evaluation of dispersible demulsifier and water-clearing agent for treating heavy oily wastewater

[0098] First, 100 ml of oily wastewater (oil content 2000 mg / L) from a heavy oil field was poured into a 100 ml colorimetric tube and kept at 80℃ for 10 min. Finally, 35 mg / L of oil-water separator was added, the mixture was shaken 100 times, and allowed to stand for 10 min. A sample of the lower layer was taken to determine the oil content and calculate the oil removal rate. The oil removal rate results for different demulsifier-water separators are shown in Table 1.

[0099] Table 1. Oil removal rates of different reagents for oily wastewater

[0100]

[0101]

[0102] The results in the table above show that Example 4 of this application has a high oil removal rate, good light transmittance, and stable oil droplet state.

[0103] This application develops a demulsifier and dewatering agent suitable for heavy oil by introducing aromatic groups, and simultaneously introduces sulfonic acid groups to increase the dispersibility of oil-viscous flocs, resulting in a dispersible demulsifier and dewatering agent for heavy oil. This dispersible demulsifier and dewatering agent, prepared from aromatic amines, polyvinyl alcohols, alkylamines, sulfonating agents, and carbon disulfide, is suitable for heavy oil fields and exhibits good water purification effects, producing dense flocs and clear water. It is particularly effective in treating oily wastewater containing heavy oil.

[0104] The embodiments described herein are preferred embodiments of the present invention and are not intended to limit the scope of protection of the present invention. Therefore, all equivalent changes made in accordance with the structure, shape, and principle of the present invention should be covered within the scope of protection of the present invention.

Claims

1. A method for preparing a dispersed demulsifying water integrator for heavy oil, characterized by: The preparation method comprises the following steps: S1. Preparation of aromatic hydrocarbon polyether amine Under stirring, a mixture of aromatic amine and organic solvent is added dropwise to the polychlorohydrin, the temperature is controlled at 80-100℃, after the dropwise addition of the mixture of aromatic amine and organic solvent is completed, the temperature is increased to 100-110℃, and the temperature is kept at this temperature for 1-3h; then the dynamic viscosity is measured, when the viscosity reaches 100-150CP, alkylamine is added for continuous reaction, the reaction temperature is controlled at 50-105℃, and the reaction time is 2-5h, to obtain the aromatic hydrocarbon polyether amine; The aromatic amine is selected from one of 2,3-diaminophenoxazine, 4-methoxyaniline, 4-methylaniline, benzidine, p-phenylenediamine or diethyltoluene diamine; The alkylamine is selected from one of diethylene triamine, triethylene tetramine, tetraethylene pentamine, pentaethylene hexamine, hexaethylene heptamine, heptaethylene octamine, octaethylene nonamine, nonaethylene decamine or polyethylene polyamine; S2. Preparation of the dispersion type demulsification and water integration agent The aromatic hydrocarbon polyether amine prepared in step S1 and deionized water are mixed in a mass ratio of 1:0.5-1:3.0, then a sulfonating agent is added dropwise, and the reaction temperature is controlled at 50-80℃, and the temperature is kept for 1-2.5h; then lye is added and stirred for 20-40min, then carbon disulfide is added dropwise, and the reaction temperature is controlled at 0-30℃; after the dropwise addition is completed, the temperature is increased to 30-40℃, and the reaction is continued for 5-7h, and the temperature is decreased to obtain the dispersion type demulsification and water integration agent.

2. The preparation method of the dispersed demulsifying water integrator for heavy oil according to claim 1, characterized in that: In step S1, the reaction molar ratio of the aromatic amine to the polychlorohydrin is 1:20-1:

30.

3. The preparation method of the dispersed demulsifying water integrator for heavy oil according to claim 1, characterized in that: In step S1, the organic solvent accounts for 20wt%-45wt% of the total reaction system.

4. The preparation method of the dispersed demulsifying water integrator for heavy oil according to claim 1, characterized in that: In step S1, the reaction molar ratio of the alkylamine to the polychlorohydrin is 1:0.6-1:1.

2.

5. The preparation method of the dispersed demulsifying water integrator for heavy oil according to claim 1, characterized in that: In step S2, the sulfonating agent is selected from one of 2-chloroethylsulfonic acid sodium, chlorosulfonic acid, sodium sulfite, sodium bisulfite, sulfamic acid or 3-chloro-2-hydroxypropanesulfonic acid sodium.

6. The preparation method of the dispersed demulsifying water integrator for heavy oil according to claim 1, characterized in that: In step S2, the molar ratio of the sulfonating agent to the aromatic hydrocarbon polyether amine is 1:11-1:

13.

7. The preparation method of the dispersed demulsifying water integrator for heavy oil according to claim 1, characterized in that: In step S2, the reaction molar ratio of the aromatic hydrocarbon polyether amine to carbon disulfide is 1:1.0-1:5.

0.

8. A dispersion type demulsification and water integration agent for thick oil, which is prepared by the preparation method of any one of claims 1-7.

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