Dispersing type demulsification and water cleaning integrated agent for thickened oil and preparation method of dispersing type demulsification and water cleaning integrated agent

Abstract

The invention discloses a dispersing type demulsification and water cleaning integrated agent for thickened oil and a preparation method thereof. Aromatic amine, polychlorohydrin, alkylamine, a sulfonating reagent and carbon disulfide serve as raw materials, firstly, polyether and aromatic amine serve as raw materials to synthesize aromatic polyether amine, then the aromatic polyether amine reacts with alkylamine to complete chain extension, then the aromatic polyether amine reacts with the sulfonating reagent, and finally the aromatic polyether amine reacts with carbon disulfide and sodium hydroxide to generate the dispersing type demulsification and water cleaning integrated agent suitable for the heavy oil field. The prepared dispersing type demulsification and water cleaning integrated agent is good in water cleaning effect, compact in floc and clear in water quality, and especially can achieve a better effect when being applied to treatment of heavy oil oily sewage.

Description

Technical Field

[0001] The invention relates to the technical field of heavy oil wastewater treatment, and in particular to a dispersed demulsifier and water-clearing agent for heavy oil and a preparation method thereof. Background Art

[0002] In the current heavy oil field exploitation, the treatment of oily wastewater mainly relies on water purifiers such as polydimethyldienyl ammonium chloride-acrylamide (PDADMA-AM) copolymer and methacryloyloxyethyl trimethyl ammonium chloride-acrylamide (DMC-AM) copolymer. However, with the rapid development of the heavy oil exploitation industry and the widespread application of enhanced oil recovery technologies such as chemical flooding and steam flooding, the heavy oil wastewater treated by the primary separator shows a trend of increasing difficulty in treatment.

[0003] The primary difficulty is that heavy oil has a high density and its specific gravity is close to that of water. In addition, due to the high natural emulsifier and higher interfacial activity, the separation speed of crude oil in the separator and crude oil storage tank is reduced, and the difficulty of oil-water separation is much higher than that of conventional oilfield emulsions, which puts higher requirements on the performance of the agent. Secondly, the viscosity of heavy oil is high, and the colloids and asphaltene in the heavy oil are the main reasons for the high viscosity of heavy oil. The association interaction between these macromolecules forms a stable colloid. The oil-water produced fluid emulsion formed by this colloid coating is relatively stable, while conventional agents have weak dispersibility and poor wettability in this system, and it is difficult for all agents to reach the interface of the oil-water emulsion to complete the demulsification process. Therefore, the performance requirements for demulsification and water-clearing agents required for the treatment of heavy oil-containing oily wastewater are becoming more and more stringent. Existing water-clearing agent products generally have problems such as insufficient performance, attenuated water-clearing efficiency, and large dosage. In addition, the dirty oil treated with existing chemicals tends to stick together and adhere to the tube wall of the inclined plate separator and the inner wall of the fluid delivery pipeline, which not only reduces the separation efficiency of the equipment, but also increases the frequency and difficulty of tank cleaning and pollution removal operations. Summary of the invention

[0004] In order to solve the above technical problems, the present invention provides a dispersed demulsifying and water-clearing agent for thick oil and a preparation method thereof.

[0005] In a first aspect, the present invention provides a method for preparing a dispersed demulsifier and water-liquid integrated agent for heavy oil, which is achieved by adopting the following technical scheme.

[0006] A method for preparing a dispersed demulsifier and water-liquid integrated agent for thick oil comprises 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 the polychlorohydrin, and the temperature is controlled at 80°C to 100°C. After the addition of the mixture of aromatic amine and organic solvent is completed, the temperature is raised to 100°C to 110°C, and the mixture is kept at this temperature for 1 to 3 hours. Then, the dynamic viscosity is measured. When the viscosity reaches 100 to 150 CP, an alkylamine is added to continue the reaction, and the reaction temperature is controlled at 50°C to 105°C for 2 to 5 hours to obtain an aromatic polyetheramine.

[0009] S2. Preparation of dispersed demulsifier and water-based agent

[0010] The aromatic polyetheramine prepared in step S1 and deionized water are mixed in a mass ratio of 1:0.5 to 1:3.0, and then a sulfonating reagent is added dropwise, while the reaction temperature is controlled at 50°C to 80°C and kept warm for 1 to 2.5 hours; then an alkali solution is added and stirred for 20 to 40 minutes, and then carbon disulfide is added dropwise, and the reaction temperature is controlled at 0°C to 30°C; after the addition is completed, the temperature is raised to 30°C to 40°C, the reaction is continued for 5 to 7 hours, and the temperature is lowered to obtain a dispersed demulsifier water-clearing 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 reaction molar ratio of aromatic amine to polychlorohydrin 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 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, nonaethylenedecaamine or polyethylenepolyamine.

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

[0017] Furthermore, in step S2, the sulfonating reagent 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 reaction molar ratio of the aromatic polyetheramine and carbon disulfide is 1:1.0 to 1:5.0.

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

[0020] Furthermore, in step S2, sodium hydroxide is used as the alkali solution, and the amount of the alkali solution added is determined by controlling the system to be in the range of pH = 9.5-12.5 after the carbon disulfide is added dropwise.

[0021] Furthermore, in step S2, the dropping time of carbon disulfide is controlled within 40-60 minutes.

[0022] In a second aspect, the present invention provides a dispersed demulsifier and water-liquid integrated agent for thick oil, which is realized by adopting the following technical scheme.

[0023] A dispersed demulsifying and water-clearing agent for thick oil prepared by the above preparation method.

[0024] This application has the following beneficial effects.

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

[0026] (2) In heavy oil, colloids and asphaltenes are the main factors that lead to the increase of its viscosity. The introduction of aromatic groups into the dispersible demulsifier for heavy oil of the present invention can change the polarity and hydrogen bond structure of colloid and asphaltenes molecules, thereby dispersing the molecules in the heavy oil and effectively reducing its viscosity.

[0027] (3) The introduction of the sulfonic acid group of the dispersed demulsifier for heavy oil of the present invention significantly improves the dispersibility and wettability of the agent in the heavy oil system. This enables the agent to penetrate the oil-water produced fluid emulsion formed by the colloid coating in the heavy oil, making it easy to reach the interface of the oil-water emulsion, thereby efficiently completing the demulsification process. DETAILED DESCRIPTION

[0028] The present patent application is further described below in conjunction with embodiments.

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

[0030] The molecular weight of the polychlorohydrin selected in the following examples of this application is

[0031] Example 1

[0032] A method for preparing a dispersed demulsifier and water-liquid integrated agent for thick oil comprises the following steps:

[0033] Step 1: Preparation of aromatic polyetheramine

[0034] In a reactor equipped with a thermometer and stirring, add polychlorohydrin (22.2g, 0.24mol), start stirring, slowly drop a uniform mixture of 2,3-diaminophenolazine (2.1g, 0.01mol), ethylene glycol monobutyl ether (21.1g) and ethylene glycol (21.0g), and control the temperature at 90°C. After the aromatic amine mixed solution is added, raise the temperature to 105°C and keep it at this temperature for 2.5h. Then, measure the dynamic viscosity. When the viscosity reaches 120CP, add triethylenetetramine (33.6g, 0.23mol) to continue the reaction. The reaction temperature is 65°C and the reaction time is 2h. Finally, a brown-yellow transparent product is obtained.

[0035] Step 2: Preparation of dispersed demulsifier and water-integrated agent

[0036] In a reactor equipped with a thermometer and a stirrer, add aromatic polyetheramine (100g, 0.24mol) and deionized water (100g); slowly drop 2-chloroethylsulfonate sodium (3.7g, 0.02mol), control the reaction temperature to 70℃, and keep warm for 2h. Then add sodium hydroxide (34.6g), stir for 30 minutes, and then drop carbon disulfide (54.7g, 0.72mol), control the reaction temperature to 25℃; after the addition is completed, heat to 30℃, continue the reaction for 6h, cool down and discharge, and obtain a brown-red transparent liquid.

[0037] Example 2

[0038] A method for preparing a dispersed demulsifier and water-liquid integrated agent for thick oil comprises the following steps:

[0039] Step 1: Preparation of aromatic polyetheramine

[0040] In a reactor equipped with a thermometer and stirring, add polychlorohydrin (22.2g, 0.24mol), start stirring, slowly drop a uniform mixture of p-phenylenediamine (1.1g, 0.01mol), ethylene glycol monobutyl ether (21.1g) and ethylene glycol (21.0g), and control the temperature at 90°C. After the aromatic amine mixed solution is added, raise the temperature to 105°C and keep it at this temperature for 2.5h. Then, measure the dynamic viscosity. When the viscosity reaches 120CP, add triethylenetetramine (33.6g, 0.23mol) to continue the reaction. The reaction temperature is 65°C and the reaction time is 2h. Finally, a brown-yellow transparent product is obtained.

[0041] Step 2: Preparation of dispersed demulsifier and water-integrated agent

[0042] In a reactor equipped with a thermometer and a stirrer, add aromatic polyetheramine (100g, 0.24mol) and deionized water (100g); slowly drop 2-chloroethylsulfonate sodium (3.7g, 0.02mol), control the reaction temperature to 70℃, and keep warm for 2h. Then add sodium hydroxide (34.6g), stir for 30 minutes, and then drop carbon disulfide (54.7g, 0.72mol), control the reaction temperature to 25℃; after the addition is completed, heat to 30℃, continue the reaction for 6h, cool down and discharge, and obtain a brown-red transparent liquid.

[0043] Example 3

[0044] A method for preparing a dispersed demulsifier and water-liquid integrated agent for thick oil comprises the following steps:

[0045] Step 1: Preparation of aromatic polyetheramine

[0046] In a reactor equipped with a thermometer and stirring, add polychlorohydrin (22.2g, 0.24mol), start stirring, slowly drop a uniform mixture of diethyltoluenediamine (1.8g, 0.01mol), ethylene glycol monobutyl ether (21.1g) and ethylene glycol (21.0g), and control the temperature at 90°C. After the aromatic amine mixed solution is added, raise the temperature to 105°C and keep it at this temperature for 2.5h. Then, measure the dynamic viscosity. When the viscosity reaches 120CP, add triethylenetetramine (33.6g, 0.23mol) to continue the reaction. The reaction temperature is 65°C and the reaction time is 2h. Finally, a brown-yellow transparent product is obtained.

[0047] Step 2: Preparation of dispersed demulsifier and water-integrated agent

[0048] In a reactor equipped with a thermometer and a stirrer, add aromatic polyetheramine (100g, 0.24mol) and deionized water (100g); slowly drop 2-chloroethylsulfonate sodium (3.7g, 0.02mol), control the reaction temperature to 70℃, and keep warm for 2h. Then add sodium hydroxide (34.6g), stir for 30 minutes, and then drop carbon disulfide (54.7g, 0.72mol), control the reaction temperature to 25℃; after the addition is completed, heat to 30℃, continue the reaction for 6h, cool down and discharge, and obtain a brown-red transparent liquid.

[0049] Example 4

[0050] A method for preparing a dispersed demulsifier and water-liquid integrated agent for thick oil comprises the following steps:

[0051] Step 1: Preparation of aromatic polyetheramine

[0052] In a reactor equipped with a thermometer and stirring, add polychlorohydrin (22.2g, 0.24mol), start stirring, slowly drop a uniform mixture of 2,3-diaminophenolazine (2.1g, 0.01mol), ethylene glycol monobutyl ether (21.1g) and ethylene glycol (21.0g), and control the temperature at 90°C. After the aromatic amine mixed solution is added, raise the temperature to 105°C and keep it at this temperature for 2.5h. Then, measure the dynamic viscosity. When the viscosity reaches 120CP, add triethylenetetramine (33.6g, 0.23mol) to continue the reaction. The reaction temperature is 65°C and the reaction time is 2h. Finally, a brown-yellow transparent product is obtained.

[0053] Step 2: Preparation of dispersed demulsifier and water-integrated agent

[0054] In a reactor equipped with a thermometer and a stirrer, add aromatic polyetheramine (100g, 0.24mol) and deionized water (100g); slowly drop 3-chloro-2-hydroxypropanesulfonic acid sodium (3.9g, 0.02mol), control the reaction temperature to 70℃, and keep warm for 2h. Then add sodium hydroxide (34.6g), stir for 30 minutes, and then drop carbon disulfide (54.7g, 0.72mol), control the reaction temperature to 25℃; after the dropwise addition, heat to 30℃, continue the reaction for 6h, cool down and discharge to obtain a brown-red transparent liquid.

[0055] Example 5

[0056] A method for preparing a dispersed demulsifier and water-liquid integrated agent for thick oil comprises the following steps:

[0057] Step 1: Preparation of aromatic polyetheramine

[0058] In a reactor equipped with a thermometer and stirring, add polychlorohydrin (22.2g, 0.24mol), start stirring, slowly drop a uniform mixture of 2,3-diaminophenolazine (2.1g, 0.01mol), ethylene glycol ethyl ether (21.1g) and ethanol (21.0g), and control the temperature at 90°C. After the aromatic amine mixed solution is added, raise the temperature to 105°C and keep it at this temperature for 2.5h. Then, measure the dynamic viscosity. When the viscosity reaches 120CP, add triethylenetetramine (33.6g, 0.23mol) to continue the reaction. The reaction temperature is 65°C and the reaction time is 2h. Finally, a brown-yellow transparent product is obtained.

[0059] Step 2: Preparation of dispersed demulsifier and water-integrated agent

[0060] In a reactor equipped with a thermometer and a stirrer, add aromatic polyetheramine (100g, 0.24mol) and deionized water (100g); slowly drop 3-chloro-2-hydroxypropanesulfonic acid sodium (3.9g, 0.02mol), control the reaction temperature to 70℃, and keep warm for 2h. Then add sodium hydroxide (34.6g), stir for 30 minutes, and then drop carbon disulfide (54.7g, 0.72mol), control the reaction temperature to 25℃; after the dropwise addition, heat to 30℃, continue the reaction for 6h, cool down and discharge to obtain a brown-red transparent liquid.

[0061] Example 6

[0062] A method for preparing a dispersed demulsifier and water-liquid integrated agent for thick oil comprises the following steps:

[0063] Step 1: Preparation of aromatic polyetheramine

[0064] In a reactor equipped with a thermometer and stirring, add polychlorohydrin (22.2g, 0.24mol), start stirring, slowly drop a uniform mixture of 2,3-diaminophenolazine (2.5g, 0.012mol), ethylene glycol ethyl ether (21.1g) and ethanol (21.0g), and control the temperature at 90°C. After the aromatic amine mixed solution is added, raise the temperature to 105°C and keep it at this temperature for 2.5h. Then, measure the dynamic viscosity. When the viscosity reaches 120CP, add triethylenetetramine (33.6g, 0.23mol) to continue the reaction. The reaction temperature is 65°C and the reaction time is 2h. Finally, a brown-yellow transparent product is obtained.

[0065] Step 2: Preparation of dispersed demulsifier and water-integrated agent

[0066] In a reactor equipped with a thermometer and a stirrer, add aromatic polyetheramine (100g, 0.24mol) and deionized water (100g); slowly drop 3-chloro-2-hydroxypropanesulfonic acid sodium (3.9g, 0.02mol), control the reaction temperature to 70℃, and keep warm for 2h. Then add sodium hydroxide (34.6g), stir for 30 minutes, and then drop carbon disulfide (54.7g, 0.72mol), control the reaction temperature to 25℃; after the dropwise addition, heat to 30℃, continue the reaction for 6h, cool down and discharge to obtain a brown-red transparent liquid.

[0067] Example 7

[0068] A method for preparing a dispersed demulsifier and water-liquid integrated agent for thick oil comprises the following steps:

[0069] Step 1: Preparation of aromatic polyetheramine

[0070] In a reactor equipped with a thermometer and stirring, add polychlorohydrin (22.2g, 0.24mol), start stirring, slowly drop a uniform mixture of 2,3-diaminophenolazine (1.7g, 0.008mol), ethylene glycol ethyl ether (21.1g) and ethanol (21.0g), and control the temperature at 90°C. After the aromatic amine mixed solution is added, raise the temperature to 105°C and keep it at this temperature for 2.5h. Then, measure the dynamic viscosity. When the viscosity reaches 120CP, add triethylenetetramine (33.6g, 0.23mol) to continue the reaction. The reaction temperature is 65°C and the reaction time is 2h. Finally, a brown-yellow transparent product is obtained.

[0071] Step 2: Preparation of dispersed demulsifier and water-integrated agent

[0072] In a reactor equipped with a thermometer and a stirrer, add aromatic polyetheramine (100g, 0.24mol) and deionized water (100g); slowly drop 3-chloro-2-hydroxypropanesulfonic acid sodium (3.9g, 0.02mol), control the reaction temperature to 70℃, and keep warm for 2h. Then add sodium hydroxide (34.6g), stir for 30 minutes, and then drop carbon disulfide (54.7g, 0.72mol), control the reaction temperature to 25℃; after the dropwise addition, heat to 30℃, continue the reaction for 6h, cool down and discharge to obtain a brown-red transparent liquid.

[0073] Example 8

[0074] A method for preparing a dispersed demulsifier and water-liquid integrated agent for thick oil comprises the following steps:

[0075] Step 1: Preparation of aromatic polyetheramine

[0076] In a reactor equipped with a thermometer and stirring, add polychlorohydrin (22.2g, 0.24mol), start stirring, slowly drop a uniform mixture of 2,3-diaminophenolazine (2.1g, 0.01mol), ethylene glycol ethyl ether (21.1g) and ethanol (21.0g), and control the temperature at 90°C. After the aromatic amine mixed solution is added, raise the temperature to 105°C and keep it at this temperature for 2.5h. Then, measure the dynamic viscosity. When the viscosity reaches 120CP, add triethylenetetramine (21.1g, 0.144mol) to continue the reaction. The reaction temperature is 65°C and the reaction time is 2h. Finally, a brown-yellow transparent product is obtained.

[0077] Step 2: Preparation of dispersed demulsifier and water-integrated agent

[0078] In a reactor equipped with a thermometer and a stirrer, add aromatic polyetheramine (100g, 0.24mol) and deionized water (100g); slowly drop 3-chloro-2-hydroxypropanesulfonic acid sodium (3.9g, 0.02mol), control the reaction temperature to 70℃, and keep warm for 2h. Then add sodium hydroxide (34.6g), stir for 30 minutes, and then drop carbon disulfide (54.7g, 0.72mol), control the reaction temperature to 25℃; after the dropwise addition, heat to 30℃, continue the reaction for 6h, cool down and discharge to obtain a brown-red transparent liquid.

[0079] Example 9

[0080] A method for preparing a dispersed demulsifier and water-liquid integrated agent for thick oil comprises the following steps:

[0081] Step 1: Preparation of aromatic polyetheramine

[0082] In a reactor equipped with a thermometer and stirring, add polychlorohydrin (22.2g, 0.24mol), start stirring, slowly drop a uniform mixture of 2,3-diaminophenolazine (2.1g, 0.01mol), ethylene glycol ethyl ether (21.1g) and ethanol (21.0g), and control the temperature at 90°C. After the aromatic amine mixed solution is added, raise the temperature to 105°C and keep it at this temperature for 2.5h. Then, measure the dynamic viscosity. When the viscosity reaches 120CP, add triethylenetetramine (42.1g, 0.288mol) to continue the reaction. The reaction temperature is 65°C and the reaction time is 2h. Finally, a brown-yellow transparent product is obtained.

[0083] Step 2: Preparation of dispersed demulsifier and water-integrated agent

[0084] In a reactor equipped with a thermometer and a stirrer, add aromatic polyetheramine (100g, 0.24mol) and deionized water (100g); slowly drop 3-chloro-2-hydroxypropanesulfonic acid sodium (3.9g, 0.02mol), control the reaction temperature to 70℃, and keep warm for 2h. Then add sodium hydroxide (34.6g), stir for 30 minutes, and then drop carbon disulfide (54.7g, 0.72mol), control the reaction temperature to 25℃; after the dropwise addition, heat to 30℃, continue the reaction for 6h, cool down and discharge to obtain a brown-red transparent liquid.

[0085] Example 10

[0086] A method for preparing a dispersed demulsifier and water-liquid integrated agent for thick oil comprises the following steps:

[0087] Step 1: Preparation of aromatic polyetheramine

[0088] In a reactor equipped with a thermometer and stirring, add polychlorohydrin (22.2g, 0.24mol), start stirring, slowly drop a uniform mixture of 2,3-diaminophenolazine (2.1g, 0.01mol), ethylene glycol monobutyl ether (21.1g) and ethylene glycol (21.0g), and control the temperature at 90°C. After the aromatic amine mixed solution is added, raise the temperature to 105°C and keep it at this temperature for 2.5h. Then, measure the dynamic viscosity. When the viscosity reaches 120CP, add triethylenetetramine (33.6g, 0.23mol) to continue the reaction. The reaction temperature is 65°C and the reaction time is 2h. Finally, a brown-yellow transparent product is obtained.

[0089] Step 2: Preparation of dispersed demulsifier and water-integrated agent

[0090] In a reactor equipped with a thermometer and a stirrer, add aromatic polyetheramine (100g, 0.24mol) and deionized water (100g); slowly drop 3-chloro-2-hydroxypropanesulfonic acid sodium (3.9g, 0.02mol), control the reaction temperature to 70℃, and keep warm for 2h. Then add sodium hydroxide (11.52g), stir for 30 minutes, and then drop carbon disulfide (18.2g, 0.24mol), control the reaction temperature to 25℃; after the addition is completed, heat to 30℃, continue the reaction for 6h, cool down and discharge, and obtain a brown-red transparent liquid.

[0091] Embodiment 11

[0092] A method for preparing a dispersed demulsifier and water-liquid integrated agent for thick oil comprises the following steps:

[0093] Step 1: Preparation of aromatic polyetheramine

[0094] In a reactor equipped with a thermometer and stirring, add polychlorohydrin (22.2g, 0.24mol), start stirring, slowly drop a uniform mixture of 2,3-diaminophenolazine (2.1g, 0.01mol), ethylene glycol monobutyl ether (21.1g) and ethylene glycol (21.0g), and control the temperature at 90°C. After the aromatic amine mixed solution is added, raise the temperature to 105°C and keep it at this temperature for 2.5h. Then, measure the dynamic viscosity. When the viscosity reaches 120CP, add triethylenetetramine (33.6g, 0.23mol) to continue the reaction. The reaction temperature is 65°C and the reaction time is 2h. Finally, a brown-yellow transparent product is obtained.

[0095] Step 2: Preparation of dispersed demulsifier and water-integrated agent

[0096] In a reactor equipped with a thermometer and stirring, add aromatic polyetheramine (100g, 0.24mol) and deionized water (100g); slowly drop 3-chloro-2-hydroxypropanesulfonic acid sodium (3.9g, 0.02mol), control the reaction temperature to 70℃, and keep warm for 2h. Then add sodium hydroxide (46.08g), stir for 30 minutes, and then drop carbon disulfide (73.0g, 0.96mol), control the reaction temperature to 25℃; after the addition is completed, heat to 30℃, continue the reaction for 6h, cool down and discharge, and obtain a brown-red transparent liquid.

[0097] Performance evaluation of dispersed demulsifier and water-clearing agent in treating heavy oil-containing wastewater

[0098] First, take 100ml of oily wastewater (oil content 2000mg / L) from a heavy oil field and pour it into a 100ml colorimetric tube, place it at 80℃ for 10min; finally add 35mg / L of oil-water separator, shake it back and forth 100 times, let it stand for 10min, take the lower layer of water sample to determine the oil content and calculate the oil removal rate. The oil removal rate results of different demulsifiers are shown in Table 1.

[0099] Table 1 Oil removal rate of different agents for oily wastewater

[0100]

[0101]

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

[0103] The present application develops a demulsifying and water-clearing agent suitable for heavy oil by introducing an aromatic group, and at the same time introduces a sulfonic acid group to increase the dispersibility of oil-viscous flocs, thereby obtaining a dispersed demulsifying and water-clearing agent for heavy oil. The dispersed demulsifying and water-clearing agent suitable for heavy oil fields, which is prepared with aromatic amines, polychlorohydrins, alkylamines, sulfonated reagents and carbon disulfide as raw materials, has good water purification effect, dense flocs and clear water quality, and can achieve good results in treating heavy oil-containing wastewater.

[0104] The embodiments of this specific implementation method are all preferred embodiments of the present invention, and are not intended to limit the protection scope of the present invention. Therefore, any equivalent changes made based on the structure, shape, and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A method for preparing a dispersed demulsifier and water-in-one agent for thick oil, characterized in that: The following steps are involved: S1. Preparation of aromatic polyetheramines Under stirring conditions, a mixture of aromatic amine and organic solvent is added dropwise to the polychlorohydrin, and the temperature is controlled at 80°C to 100°C. After the addition of the mixture of aromatic amine and organic solvent is completed, the temperature is raised to 100°C to 110°C, and the mixture is kept at this temperature for 1 to 3 hours. Then, the dynamic viscosity is measured. When the viscosity reaches 100 to 150 CP, an alkylamine is added to continue the reaction, and the reaction temperature is controlled at 50°C to 105°C for 2 to 5 hours to obtain an aromatic polyetheramine. S2. Preparation of dispersed demulsifier and water-in-one agent The aromatic polyetheramine prepared in step S1 and deionized water are mixed in a mass ratio of 1:0.5 to 1:3.0, and then a sulfonating reagent is added dropwise, while the reaction temperature is controlled at 50°C to 80°C and kept warm for 1 to 2.5 hours; then an alkali solution is added and stirred for 20 to 40 minutes, and then carbon disulfide is added dropwise, and the reaction temperature is controlled at 0°C to 30°C; after the addition is completed, the temperature is raised to 30°C to 40°C, the reaction is continued for 5 to 7 hours, and the temperature is lowered to obtain a dispersed demulsifier water-clearing agent.

2. The method for preparing a dispersed demulsifier and water-in-one agent for thick oil according to claim 1, characterized in that: In step S1, the aromatic amine is selected from one of 2,3-diaminophenolazine, 4-methoxyaniline, 4-methylaniline, benzidine, p-phenylenediamine or diethyltoluenediamine.

3. The method for preparing a dispersed demulsifier and water-in-one agent for thick oil according to claim 1, characterized in that: In step S1, the reaction molar ratio of aromatic amine to polychlorohydrin is 1:20 to 1:

30.

4. The method for preparing a dispersed demulsifier and water-in-one agent for thick oil according to claim 1, characterized in that: In step S1, the organic solvent accounts for 20 wt% to 45 wt% of the total reaction system.

5. The method for preparing a dispersed demulsifier and water-in-one agent for thick oil according to claim 1, characterized in that: In step S1, the alkylamine is selected from one of diethylenetriamine, triethylenetetramine, tetraethylenepentamine, pentaethylenehexamine, hexaethyleneheptamine, heptaethyleneoctamine, octaethylenenonamine, nonaethylenedecaamine or polyethylenepolyamine.

6. The method for preparing a dispersed demulsifier and water-in-one agent for thick oil according to claim 1, characterized in that: In step S1, the reaction molar ratio of alkylamine to polychlorohydrin is 1:0.6 to 1:1.

2.

7. The method for preparing a dispersed demulsifier and water-in-one agent for thick oil according to claim 1, characterized in that: In step S2, the sulfonating reagent is selected from one of sodium 2-chloroethylsulfonate, chlorosulfonic acid, sodium sulfite, sodium bisulfite, aminosulfonic acid or sodium 3-chloro-2-hydroxypropanesulfonate.

8. The method for preparing a dispersed demulsifier and water-in-one agent for thick oil according to claim 1, characterized in that: In step S2, the molar ratio of the sulfonating agent to the aromatic polyetheramine is 1:11-1:

13.

9. The method for preparing a dispersed demulsifier and water-in-one agent for thick oil according to claim 1, characterized in that: In step S2, the reaction molar ratio of aromatic polyetheramine to carbon disulfide is 1:1.0 to 1:5.

0.

10. A dispersed demulsifying and water-liquid integrated agent for heavy oil prepared by the preparation method according to any one of claims 1 to 9.

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