Active water washing dehydration process for thickened oil aging oil

Abstract

The application discloses a kind of active water washing dehydration processes of thick oil aging oil, the present application will be prepared by mixing thick oil aging oil and active water premix, then the premix is added to buffer tank and is separated from mud, then enters oil mud separator and is washed again by active water, and then thick oil aging oil is separated from mud and water;The present application has the characteristics of simple process, fast dehydration speed, good dehydration effect and strong applicability.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of petroleum purification treatment, and particularly relates to a thickened oil aging oil active water washing dehydration process. BACKGROUND

[0002] In the exploitation of thickened oil, various chemical composite drives such as polymer drive, ternary composite drive and composite drive with surface activity are used to improve the recovery rate of oil fields, resulting in the increase of the exploitation amount of thickened oil and the difficulty of processing year by year. The refining treatment of thickened oil has always been a difficult problem, mainly due to the complex composition of thickened oil, high content of gum and asphaltene, high degree of oil-water emulsification and strong stability of oil-water emulsion, which leads to difficult dehydration and poor oil-water separation effect.

[0003] Fast demulsification and dehydration is an important research topic for realizing the green and sustainable development of oil fields. At present, the methods for dehydrating thickened oil at home and abroad mainly include electric field treatment method, chemical demulsification and sedimentation method, ultrasonic treatment method, centrifugal separation technology and the like. The chemical demulsification and sedimentation method is considered to be the most promising treatment method at present. Chinese patent CN113481026A discloses a low-temperature demulsifier, which is obtained by reacting hydrogen-containing silicone oil and allyl polyether derivative to obtain a silicone oil modified polyether demulsifier, and has the ability of low-temperature demulsification and dehydration. Chinese patent CN104774645B discloses a polyether type thickened oil demulsifier, which is prepared from alkyl phenol polyoxyethylene propylene ether polymer, aliphatic polyether phosphate and methanol, and solves the problem of large amount of demulsifier used.

[0004] Although the above related technologies have certain effects on the treatment of thickened oil, the process conditions are strict, the diffusion speed of the demulsifier is slow, the water droplets are difficult to aggregate, the oil-water separation is not complete, and the comprehensive effect is not ideal. SUMMARY

[0005] The purpose of the present application is to overcome the shortcomings in the prior art, and to provide a thickened oil aging oil active water washing dehydration process.

[0006] In order to achieve the above purpose, the technical scheme adopted by the present application is as follows:

[0007] A thickened oil aging oil active water washing dehydration process, comprising the following steps:

[0008] Step 1: The thickened oil aging oil in the sewage and the active water are introduced into a mixer through a slurry pump and a proportional pump for strong shearing to obtain a premix;

[0009] Step 2: Steam is introduced into the premix to make the temperature of the mixed material reach 70-90 DEG C, and then the material A is obtained by entering a buffer tank for sedimentation separation;

[0010] Step 3: The material A is delivered to the oil sludge sand separator by a booster pump, and the material A is separated again by active water washing in the oil sludge sand separator to obtain finished oil, and the pressure in the booster pump is 0.2-0.5 MPa.

[0011] Further, the volume ratio of the thickened oil aging oil to the active water in step 1 is 1:0.8-1.2.

[0012] Further, the preparation method of the active water is as follows: the active water washing agent is mixed with water to prepare 0.5 g / L active water, and then 0.2%-0.5% of the quaternary ammonium salt and 1%-3% of the small molecule alcohol are added and uniformly mixed to obtain the active water.

[0013] Further, the preparation method of the active water washing agent is as follows: 1-3 parts of the hydrophilic penetrating material, 1-3 parts of the oleophilic penetrating material and dodecyl benzene sulfonic acid are mixed and stirred for 0.5-1 h, 5-7 parts of the reverse demulsifier are added and heated to 50-65℃, and then mixed and stirred for 1-2 h to obtain the active water washing agent, and the weight of the dodecyl benzene sulfonic acid accounts for 0.5%-2% of the total weight of the hydrophilic penetrating material and the oleophilic material.

[0014] Further, the quaternary ammonium salt is one or both of trimethylammonium bromide and cetyltrimethylammonium bromide, and the small molecule alcohol is one or more of methanol, ethanol, n-propanol and isopropanol.

[0015] Further, the preparation method of the hydrophilic penetrating material is as follows: 3-5 parts of lauryl alcohol and 0.2-0.5 parts of potassium hydroxide are added to a reactor, heated and warmed to 110-155℃, then 50 parts of propylene oxide are added, stirred under vacuum for 0.5-1 h, 20-30 parts of ethylene oxide are introduced, the temperature is maintained at 110-155℃, and the reaction is carried out under vacuum for 0.5-1 h to obtain the oleophilic penetrating material.

[0016] Further, the preparation method of the oleophilic penetrating material is as follows: 10 parts of p-tert-butyl phenol, 2-3 parts of formaldehyde and 0.1-0.3 parts of sodium hydroxide are added to a reaction kettle, the pressure is adjusted to 0.3-0.5 MPa under nitrogen atmosphere, the temperature is warmed to 75-90℃, the reaction is carried out for 0.5-1 h, then 12-15 parts of propylene oxide are added under the condition of warming to 110-150℃, the temperature is maintained for 0.5-1 h, then 7-8 parts of ethylene oxide are added, the temperature is maintained for 0.5-1 h, the temperature is lowered to 90℃, 1.5-2.5 parts of triethylene glycol are added, and stirred for 0.5-1 h to obtain the oleophilic penetrating material.

[0017] Further, the preparation method of the reverse demulsifier is as follows:

[0018] A: 0.2-0.4 parts of emulsifier and 2-3 parts of deionized water are taken by weight, heated to 50-65 DEG C under nitrogen atmosphere, 3-5 parts of composite monomer is added, emulsified for 10-20 minutes, to obtain a pre-polymer liquid;

[0019] B: 0.3-0.6 parts of 2%-3% ammonium persulfate aqueous solution is added to the pre-polymer liquid, stirred uniformly at room temperature, then heated to 60-80 DEG C, 30 parts of composite monomer is added, the PH is adjusted to 7-8, and incubated for 0.5-1h, to obtain the reverse demulsifier.

[0020] Further, the emulsifier is a mixture of sodium stearate and sodium stearate with a mass ratio of 2:1.

[0021] Further, the composite monomer is a mixture of butyl acrylate, acrylic acid and beta-hydroxyethyl acrylate, with a mass ratio of 5:2-3:2-3.

[0022] After adopting the above technical solution, the present application has the following beneficial effects compared with the prior art:

[0023] 1. The active water washing agent provided by the present application has adjustable hydrophilic and lipophilic properties, and the components are matched by using lipophilic penetrating substances, hydrophilic penetrating substances and reverse demulsifiers, so that the three components play a synergistic role in demulsification, and in the process of treating thickened aging oil, the dehydration speed is fast, the dehydration rate is high, the oil content in the water phase is low, and excellent demulsification and dehydration effects are exhibited.

[0024] 2. The present application provides an active water washing dehydration process for thickened aging oil, which is safe in raw material and mild in process conditions, and is suitable for industrial automation application. BRIEF DESCRIPTION OF DRAWINGS

[0025] Figure 1 The process flow chart of the active water washing dehydration process for thickened aging oil of the present application.

[0026] Wherein 1 is a medicament tank, 2 is a water inlet pipe, 3 is an aging oil inlet pipe, 4 is a mixer, 5 is a buffer tank, 6 is a three-phase separator, 7 is an oil outlet pipe, and 8 is a sewage outlet pipe. DETAILED DESCRIPTION

[0027] The technical solutions in the present application will be described clearly and completely below by combining with the embodiments in the present application. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. The following description of at least one exemplary embodiment is actually only illustrative, but not as any limitation on the present application and its application or use. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative labor fall within the scope of protection of the present application.

[0028] Embodiment 1: A thickened oil aging oil active water washing dehydration process, comprising the following steps:

[0029] Step 1: The thickened oil aging oil in the sewage and the active water are pumped into a mixer by a slurry pump and a proportional pump for strong shearing to obtain a premix, wherein the volume ratio of the thickened oil aging oil and the active water is 1:1;

[0030] Step 2: Steam is introduced into the premix to make the temperature of the mixed material reach 80℃, and then the material is introduced into a buffer tank for settlement to remove part of the silt to obtain material A;

[0031] Step 3: The material A is transported to an oil-silt separator by a lifting pump, and the active water washing is performed again in the oil-silt separator to separate the material A again to obtain finished oil, the pressure in the lifting pump is 0.4 MPa, the treated finished oil is stored in a finished oil tank, the sewage is introduced into a sewage treatment system, and the silt at the bottom of the oil-silt separator is discharged periodically.

[0032] Further, the preparation method of the active water is as follows: the active water washing agent is mixed with water to prepare 0.5 g / L active agent water, then 0.35% of quaternary ammonium salt and 2% of small molecule alcohol are added and uniformly mixed to obtain the active water.

[0033] The quaternary ammonium salt is cetyltrimethylammonium bromide.

[0034] The small molecule alcohol is methanol.

[0035] The preparation method of the active water washing agent is as follows: 2 parts of hydrophilic penetrating material, 2 parts of oleophilic penetrating material and dodecylbenzenesulfonic acid are mixed and stirred for 0.5 h, 6 parts of reverse demulsifier is added and heated to 60℃, and then mixed and stirred for 0.5 h to obtain the active water washing agent, and the weight of the dodecylbenzenesulfonic acid accounts for 1% of the total weight of the hydrophilic penetrating material and the oleophilic material.

[0036] The preparation method of the hydrophilic penetrating material is as follows: 4 parts of lauryl alcohol and 0.3 parts of potassium hydroxide are added into a reactor and heated to 130℃, then 50 parts of propylene oxide is added, stirred under vacuum for 1 h, 25 parts of ethylene oxide is introduced, and the temperature is kept at 130℃, and the reaction is carried out under vacuum for 0.5 h to obtain the oleophilic penetrating material.

[0037] The preparation method of the oleophilic penetrating material is as follows: 10 parts of p-tert-butyl phenol, 2.5 parts of formaldehyde and 0.2 parts of sodium hydroxide are added into a reaction kettle, the pressure is adjusted to 0.4 MPa under nitrogen atmosphere, the temperature is raised to 80℃, and the reaction is carried out for 0.5 h, then 12 parts of propylene oxide is added under the condition of heating to 130℃, and the temperature is kept for 0.5 h, then 8 parts of ethylene oxide is added, the temperature is kept for 1 h, the temperature is lowered to 90℃, 2 parts of triethylene glycol is added, and stirred for 1 h to obtain the oleophilic penetrating material.

[0038] The preparation method of the reverse demulsifier is:

[0039] A: 0.3 parts of emulsifier and 2.5 parts of deionized water are taken by weight, heated to 55℃ under nitrogen atmosphere, 4 parts of composite monomer is added, emulsified for 15 minutes, and a prepolymer solution is obtained;

[0040] B: 0.4 parts of 2.5% ammonium persulfate aqueous solution is added to the prepolymer solution, stirred uniformly at room temperature, then heated to 55℃, 30 parts of composite monomer is added, the PH is adjusted to 7-8, and the reverse demulsifier is obtained after 0.5h of incubation.

[0041] The emulsifier is a mixture of sodium stearate and stearic acid with a mass ratio of 2:1.

[0042] The composite monomer is a mixture of butyl acrylate, acrylic acid and acrylic acid-β-hydroxyethyl ester with a mass ratio of 5:2:3.

[0043] Example 2: A thick oil aging oil active water washing dehydration process, comprising the following steps:

[0044] Step 1: The thick oil aging oil and active water in the sewage are fed into a mixer through a slurry pump and a proportional pump for strong shearing to obtain a premix, wherein the volume ratio of the thick oil aging oil to the active water is 1:0.8;

[0045] Step 2: Steam is introduced into the premix to heat the mixed material to 70℃, and then the material is fed into a buffer tank for sedimentation to remove part of the silt to obtain material A;

[0046] Step 3: The material A is fed into an oil-silt separator by a booster pump, and the active water washing is carried out again in the oil-silt separator to separate the material A again to obtain finished oil, the pressure in the booster pump is 0.2Mpa, the treated finished oil is stored in a finished oil tank, the sewage is fed into a sewage treatment system, and the silt at the bottom of the oil-silt separator is discharged periodically.

[0047] The preparation method of the active water is: mixing the active water washing agent with water to prepare 0.5g / L active agent water, then adding 0.2% quaternary ammonium salt and 1% small molecule alcohol, and mixing uniformly to obtain the active water.

[0048] The quaternary ammonium salt is cetyltrimethylammonium bromide.

[0049] The small molecule alcohol is ethanol.

[0050] The preparation method of the active water washing agent is as follows: 1 part of hydrophilic penetrating material, 1 part of oleophilic penetrating material and dodecyl benzene sulfonic acid are mixed and stirred for 0.5 h, 5 parts of reverse demulsifier is added and heated to 50℃, and mixed and stirred for 1 h to obtain the active water washing agent, and the weight of dodecyl benzene sulfonic acid accounts for 1% of the total weight of the hydrophilic penetrating material and the oleophilic material.

[0051] The preparation method of the hydrophilic penetrating material is as follows: 3 parts of lauryl alcohol and 0.4 parts of potassium hydroxide are added into a reactor and heated to 120℃, then 50 parts of propylene oxide is added, stirred for 1 h under vacuum, 20 parts of ethylene oxide is introduced, and the temperature is kept at 140℃, and reacted for 0.8 h under vacuum to obtain the oleophilic penetrating material.

[0052] The preparation method of the oleophilic penetrating material is as follows: 10 parts of p-tert-butyl phenol, 2 parts of formaldehyde and 0.1 parts of sodium hydroxide are added into a reaction kettle, the pressure is adjusted to 0.4 MPa under nitrogen atmosphere, heated to 80℃, reacted for 0.7 h, then 14 parts of propylene oxide is added under the condition of heating to 140℃, kept for 0.5 h, then 8 parts of ethylene oxide is added, kept for 1 h, cooled to 90℃, 1.5 parts of triethylene glycol is added, stirred for 0.5 h to obtain the oleophilic penetrating material.

[0053] The preparation method of the reverse demulsifier is as follows:

[0054] A: 0.2 parts of emulsifier and deionized water are taken by weight, heated to 50℃ under nitrogen atmosphere, 3 parts of composite monomer is added, and emulsified for 10 minutes to obtain a prepolymer solution;

[0055] B: 0.3 parts of 3% ammonium persulfate aqueous solution is added into the prepolymer solution, stirred uniformly at room temperature, then heated to 60℃, 30 parts of composite monomer is added, the PH is adjusted to 7-8, and kept for 1 h to obtain the reverse demulsifier.

[0056] The emulsifier is a mixture of lauric acid soap and sodium stearate with a mass ratio of 2:1.

[0057] The composite monomer is a mixture of butyl acrylate, acrylic acid and acrylic acid-β-hydroxyethyl ester with a mass ratio of 5:2:2.

[0058] Example 3: An active water washing dehydration process for thickened aging oil, which comprises the following steps:

[0059] Step 1: The thickened aging oil and active water in the sewage are mixed by a slurry pump and a proportional pump into a mixer for strong shearing to obtain a premix, wherein the volume ratio of the thickened aging oil to the active water is 1:1;

[0060] Step 2: Steam is introduced into the premix to raise the temperature of the mixed material to 90℃, and then the material is transferred to a buffer tank for sedimentation to remove part of the sludge, obtaining material A;

[0061] Step 3: The material A is transported to the oil sludge separator by a booster pump, and active water washing is performed again in the oil sludge separator to separate the material A again to obtain the finished oil, the pressure in the booster pump is 0.4 MPa, the treated finished oil is stored in the finished oil tank, the sewage is discharged into the sewage treatment system, and the sludge at the bottom of the oil sludge separator is periodically discharged.

[0062] The preparation method of the active water is as follows: mixing the active water washing agent with water to prepare 0.5 g / L active agent water, then adding 0.5% quaternary ammonium salt and 3% small molecule alcohol and mixing uniformly to obtain the active water.

[0063] The quaternary ammonium salt is a mixture of trimethylammonium bromide and trimethylammonium bromide.

[0064] The small molecule alcohol is isopropyl alcohol.

[0065] The preparation method of the active water washing agent is as follows: taking 3 parts of hydrophilic penetrating material, 3 parts of oleophilic penetrating material and dodecylbenzenesulfonic acid, mixing and stirring for 1.5 h, adding 7 parts of reverse demulsifier, heating to 65℃, mixing and stirring for 2 h to obtain the active water washing agent, and the weight of dodecylbenzenesulfonic acid accounts for 1% of the total weight of the hydrophilic penetrating material and the oleophilic material.

[0066] The preparation method of the hydrophilic penetrating material is as follows: adding 5 parts of lauryl alcohol and 0.5 parts of potassium hydroxide into a reactor, heating to 130℃, then adding 50 parts of propylene oxide, stirring under vacuum for 1 h, introducing 30 parts of ethylene oxide, maintaining the temperature at 155℃, and reacting for 1 h under vacuum to obtain the oleophilic penetrating material.

[0067] The preparation method of the oleophilic penetrating material is as follows: taking 10 parts of p-tert-butyl phenol, 3 parts of formaldehyde and 0.3 parts of sodium hydroxide into a reaction kettle, adjusting the pressure to 0.5 MPa under nitrogen atmosphere, heating to 90℃, reacting for 1 h, then heating to 150℃, adding 15 parts of propylene oxide, maintaining the temperature for 1 h, then adding 8 parts of ethylene oxide, maintaining the temperature for 1 h, cooling to 90℃, adding 2.5 parts of triethylene glycol, and stirring for 1 h to obtain the oleophilic penetrating material.

[0068] The preparation method of the reverse demulsifier is as follows:

[0069] A: Taking 0.3 parts of emulsifier and deionized water by weight, heating to 65℃ under nitrogen atmosphere, adding 5 parts of composite monomer, and maintaining emulsification for 20 minutes to obtain a prepolymer liquid;

[0070] B: 0.6 parts of 3% ammonium persulfate aqueous solution is added to the prepolymer solution, stirred uniformly at room temperature, then heated to 80°C, 30 parts of composite monomer is added, PH is adjusted to 7-8, and incubated for 1 h to obtain the reverse demulsifier.

[0071] The emulsifier is a mixture of sodium stearate and sodium stearate with a mass ratio of 2:1.

[0072] The composite monomer is a mixture of butyl acrylate, acrylic acid and acrylic acid-β-hydroxyethyl ester with a mass ratio of 5:3:3.

[0073] Example 4: A thick oil aging oil active water washing dehydration process, comprising the following steps:

[0074] Step 1: The thick oil aging oil and active water in the sewage are pumped into the mixer by the slurry pump and the proportional pump for strong shearing to obtain a premix, wherein the volume ratio of the thick oil aging oil and the active water is 1:1;

[0075] Step 2: Steam is introduced into the premix to make the temperature of the mixed material reach 80°C, and then the material A is obtained by entering the buffer tank for sedimentation to remove part of the silt;

[0076] Step 3: The material A is transported to the oil-sand separator by the lifting pump, and the active water washing is carried out again in the oil-sand separator to separate the material A again to obtain the finished oil, the pressure in the lifting pump is 0.4 Mpa, the treated finished oil is stored in the finished oil tank, the sewage enters the sewage treatment system, and the silt at the bottom of the oil-sand separator is discharged regularly.

[0077] The preparation method of the active water is as follows: the active water washing agent is mixed with water to prepare 0.5 g / L active agent water, based on the total weight of the active agent water, then 0.4% of quaternary ammonium salt and 2% of small molecule alcohol are added and mixed uniformly to obtain the active water.

[0078] The quaternary ammonium salt is trimethylammonium bromide.

[0079] The small molecule alcohol is isopropyl alcohol.

[0080] The preparation method of the active water washing agent is as follows: 1 part of hydrophilic penetrant, 1 part of oleophilic penetrant and dodecylbenzenesulfonic acid are mixed and stirred for 0.5 h, 6 parts of reverse demulsifier is added and heated to 60°C, and mixed and stirred for 0.5 h to obtain the active water washing agent, and the weight of dodecylbenzenesulfonic acid accounts for 1% of the total weight of the hydrophilic penetrant and the oleophilic substance.

[0081] The preparation method of the hydrophilic penetrating material is: 4 parts of lauryl alcohol and 0.4 parts of potassium hydroxide are added into a reactor and heated to 130°C, then 50 parts of propylene oxide is added, stirring under vacuum for 1h, 30 parts of ethylene oxide is introduced, keeping the temperature at 120°C, and reacting for 0.5h under vacuum to obtain the oleophilic penetrating material.

[0082] The preparation method of the oleophilic penetrating material is: 10 parts of p-tert-butyl phenol, 2 parts of formaldehyde and 0.1 parts of sodium hydroxide are added into a reactor, the pressure is adjusted to 0.4MPa under nitrogen atmosphere, and the temperature is raised to 80°C, and reacted for 0.5h, then 14 parts of propylene oxide is added under the condition of heating to 130°C, and kept for 0.5h, then 7.3 parts of ethylene oxide is added, and kept for 1h, the temperature is lowered to 90°C, 2 parts of triethylene glycol is added, and stirred for 1h to obtain the oleophilic penetrating material.

[0083] The preparation method of the reverse demulsifier is:

[0084] A: 0.2 parts of emulsifier and deionized water are heated to 60°C under nitrogen atmosphere, 4 parts of composite monomer is added, and emulsified for 15 minutes to obtain a prepolymer solution;

[0085] B: 0.4 parts of 2.5% ammonium persulfate aqueous solution is added into the prepolymer solution, stirred uniformly at room temperature, then heated to 70°C, 30 parts of composite monomer is added, the pH is adjusted to 7-8, and kept for 0.5h to obtain the reverse demulsifier.

[0086] The emulsifier is a mixture of lauric acid soap and sodium stearate with a mass ratio of 2:1.

[0087] The composite monomer is a mixture of butyl acrylate, acrylic acid and β-hydroxyethyl acrylate with a mass ratio of 5:3:2.

[0088] Example 5: A kind of active water dewatering process for thickened oil aging oil, comprising the following steps:

[0089] Step 1: The thickened oil aging oil and active water in the sewage are mixed by a slurry pump and a proportional pump into a mixer for strong shearing to obtain a premix, wherein the volume ratio of the thickened oil aging oil and the active water is 1:1;

[0090] Step 2: Steam is introduced into the premix to make the temperature of the mixed material reach 85°C, and then the material A is obtained by entering a buffer tank for sedimentation to remove part of the silt.

[0091] Step 3: The material A is delivered to the oil sludge sand separator by a booster pump, and the material A is separated again by active water washing in the oil sludge sand separator to obtain finished oil, the pressure in the booster pump is 0.4 MPa, the treated finished oil is stored in a finished oil tank, the sewage enters a sewage treatment system, and the sludge at the bottom of the oil sludge sand separator is discharged periodically.

[0092] The preparation method of the active water is as follows: the active water washing agent is mixed with water to prepare 0.5 g / L active agent water, then 0.45% of the quaternary ammonium salt and 3% of the small molecule alcohol are added and uniformly mixed to obtain the active water.

[0093] The quaternary ammonium salt is trimethylammonium bromide.

[0094] The small molecule alcohol is methanol.

[0095] The preparation method of the active water washing agent is as follows: 3 parts of hydrophilic penetrating material, 3 parts of oleophilic penetrating material and dodecylbenzenesulfonic acid are mixed and stirred for 0.5 h, 6 parts of reverse demulsifier are added and heated to 60℃, and then mixed and stirred for 0.5 h to obtain the active water washing agent, and the weight of the dodecylbenzenesulfonic acid accounts for 1% of the total weight of the hydrophilic penetrating material and the oleophilic material.

[0096] The preparation method of the hydrophilic penetrating material is as follows: 4 parts of lauryl alcohol and 0.3 parts of potassium hydroxide are added into a reactor and heated to 145℃, then 50 parts of propylene oxide are added, and stirred under vacuum for 1 h, then 30 parts of ethylene oxide are introduced, and the temperature is kept at 130℃, and the reaction is carried out under vacuum for 0.5 h to obtain the oleophilic penetrating material.

[0097] The preparation method of the oleophilic penetrating material is as follows: 10 parts of p-tert-butyl phenol, 2.5 parts of formaldehyde and 0.2 parts of sodium hydroxide are added into a reaction kettle, the pressure is adjusted to 0.4 MPa under nitrogen atmosphere, the temperature is raised to 80℃, and the reaction is carried out for 0.5 h, then 14 parts of propylene oxide are added under the condition of raising the temperature to 130℃, and the temperature is kept for 0.5 h, then 8 parts of ethylene oxide are added, and the temperature is kept for 1 h, then the temperature is lowered to 90℃, 3 parts of triethylene glycol are added, and stirred for 1 h to obtain the oleophilic penetrating material.

[0098] The preparation method of the reverse demulsifier is as follows:

[0099] A: 0.3 parts of emulsifier and deionized water are heated to 60℃ under nitrogen atmosphere, 4 parts of composite monomer are added, and the pre-polymer liquid is obtained by emulsifying for 20 minutes;

[0100] B: 0.4 parts of 2.5% ammonium persulfate aqueous solution is added into the pre-polymer liquid, and stirred uniformly at room temperature, then the temperature is raised to 55℃, 30 parts of composite monomer are added, the PH value is adjusted to 7-8, and the temperature is kept for 0.5 h to obtain the reverse demulsifier.

[0101] The emulsifier is a mixture of sodium stearate and lauric acid soap with a mass ratio of 2:1.

[0102] The complex monomer is a mixture of butyl acrylate, acrylic acid and β-hydroxyethyl acrylate with mass ratios of 5:3:2 respectively.

[0103] Comparative Example 1: The difference between Comparative Example 1 and Example 1 is that no hydrophilic penetrating material is added in the preparation of the active water washing agent of Comparative Example 1, and 4 parts of oleophilic penetrating material and 6 parts of reverse demulsifier are added.

[0104] Comparative Example 2: The difference between Comparative Example 2 and Example 1 is that no oleophilic penetrating material is added in the preparation of the active water washing agent of Comparative Example 1, and 4 parts of hydrophilic penetrating material and 6 parts of reverse demulsifier are added.

[0105] Comparative Example 3: The difference between Comparative Example 3 and Example 1 is that only reverse demulsifier is added in the preparation of the active water washing agent of Comparative Example 1, and 10 parts of reverse demulsifier are added.

[0106] Demulsification experiment

[0107] The oil sample is taken from the waste oil pool, and the water content is 51.5%. Accurately weigh 50 ml of oil sample, add the same volume of active water prepared in the examples and comparative examples, shake up and down for 50 times, mix the active water and oil sample, put into 80°C water bath for constant temperature observation, detect the water separation amount, and calculate the water separation rate, the calculation formula is as follows: water separation rate=(water separation mass / oil sample water content mass)*100%, the test results are shown in Table 1.

[0108]

[0109] Running test:

[0110] The active water washing dehydration process for thickened oil aging oil is carried out, first connect all the equipment, supplement nitrogen for ensuring the gas-liquid interface, pass in waste water for equipment preheating, the parameters of all aspects are normal, inject aging oil for testing, as shown in Figure 1 .

[0111] 1. Test site: Jinglou thickened oil joint station of Nanyang oil field in Henan

[0112] 2. Occupied area: 7.5m x 3m x 3.5m

[0113] 3. Technical parameters: water content of aging oil is 56.2%, the volume mixing ratio of aging oil and active water is 1:1, the treatment speed is 3-5m3 / h; the treatment temperature is 75-80°C; the pressure is 0.4Mpa, the active water washing agent dosage is 0.5g / L;

[0114] 4. Test results: the water content of the treated oil phase is less than 2%, and the oil content of the water phase is less than 1500 mg / L.

[0115] According to Table 1, it is shown from Example 1, Example 2, Example 3, Example 4 and Example 5 that the aged heavy oil prepared by the active water washing dehydration process of the technical solution has low water content, and the technical solution has good dehydration effect;

[0116] Comparative Example 1: The difference between Comparative Example 1 and Example 1 is that no hydrophilic penetrating material is added in the preparation of the active water washing agent in Comparative Example 1. The settling dehydration rate of the aged heavy oil in Comparative Example 1 is 50.5% at 45 min and 66.7% at 90 min, and the settling dehydration rate of the aged heavy oil in Example 1 is 80.1% at 45 min and 95.5% at 90 min. The experimental results show that the addition of the hydrophilic penetrating material improves the dehydration rate of the aged heavy oil.

[0117] Comparative Example 2: The difference between Comparative Example 2 and Example 1 is that no oleophilic penetrating material is added in the preparation of the active water washing agent in Comparative Example 1. The settling dehydration rate of the aged heavy oil in Comparative Example 2 is 51.2% at 45 min and 62.1% at 90 min, and the settling dehydration rate of the aged heavy oil in Example 1 is 80.1% at 45 min and 95.5% at 90 min. The experimental results show that the addition of the oleophilic penetrating material improves the dehydration rate of the aged heavy oil.

[0118] Comparative Example 3: The difference between Comparative Example 3 and Example 1 is that only a reverse demulsifier is used in the preparation of the active water washing agent in Comparative Example 1. The settling dehydration rate of the aged heavy oil in Comparative Example 3 is 34.5% at 45 min and 41.4% at 90 min, and the settling dehydration rate of the aged heavy oil in Example 1 is 80.1% at 45 min and 95.5% at 90 min. In combination with the settling dehydration rates of the aged heavy oil in Comparative Example 1 and Comparative Example 2, the settling dehydration rate of the aged heavy oil in Comparative Example 3 is lower than that in Comparative Example 1 and Comparative Example 2. In combination with the settling dehydration rate of the aged heavy oil in Example 1, it can be seen that the hydrophilic penetrating material and the oleophilic penetrating material have a positive synergistic effect on the dehydration of the aged heavy oil.

[0119] The above is only a preferred specific embodiment of the present application, but the protection scope of the present application is not limited thereto, and any person skilled in the art can make equivalent replacement or change within the technical scope disclosed in the present application according to the technical solution and inventive concept of the present application, which should be covered within the protection scope of the present application.

Claims

1. A process for the removal of water from a heavy oil aged oil active water wash, characterized by: The method comprises the following steps: Step 1: the thick oil aging oil in sewage and active water are mixed by a slurry pump and a proportional pump into a mixer for strong shearing to obtain a premix; Step 2: steam is introduced into the premix to make the temperature of the mixed material reach 70-90 DEG C, and then the material is introduced into a buffer tank for settlement separation to obtain material A; Step 3: the material A is transported to an oil sludge sand separator by a lifting pump, and the material A is separated again by active water washing in the oil sludge sand separator to obtain finished oil, and the pressure in the lifting pump is 0.2-0.5 MPa; The preparation method of the active water is as follows: active water washing agent is mixed with water to prepare 0.5 g / L active agent water, and then 0.2%-0.5% quaternary ammonium salt and 1%-3% small molecule alcohol are added and uniformly mixed to obtain the active water. The preparation method of the active water washing agent is as follows: 1-3 parts of hydrophilic penetrating material, 1-3 parts of oleophilic penetrating material and dodecylbenzenesulfonic acid are weighed, mixed and stirred for 0.5-1 h, 5-7 parts of reverse demulsifier is added and heated to 50-65 DEG C, and mixed and stirred for 1-2 h to obtain the active water washing agent, and the weight of dodecylbenzenesulfonic acid accounts for 0.5%-2% of the total weight of the hydrophilic penetrating material and the oleophilic penetrating material. The preparation method of the hydrophilic penetrating material is as follows: 3-5 parts of lauryl alcohol and 0.2-0.5 parts of potassium hydroxide are added into a reactor, heated and warmed to 110-155 DEG C, then 50 parts of propylene oxide is added, stirred under vacuum for 0.5-1 h, 20-30 parts of ethylene oxide is introduced, the temperature is kept at 110-155 DEG C, and the reaction is carried out under vacuum for 0.5-1 h to obtain the hydrophilic penetrating material. The preparation method of the oleophilic penetrating material is as follows: 10 parts of p-tert-butyl phenol, 2-3 parts of formaldehyde and 0.1-0.3 parts of sodium hydroxide are added into a reaction kettle under nitrogen atmosphere, the pressure is adjusted to 0.3-0.5 MPa, the temperature is raised to 75-90 DEG C, and the reaction is carried out for 0.5-1 h, then 12-15 parts of propylene oxide is added under the condition of warming to 110-150 DEG C, the temperature is kept for 0.5-1 h, then 7-8 parts of ethylene oxide is added, the temperature is kept for 0.5-1 h, the temperature is lowered to 90 DEG C, 1.5-2.5 parts of triethylene glycol is added, and stirred for 0.5-1 h to obtain the oleophilic penetrating material.

2. The active water washing dehydration process for thick oil aging oil according to claim 1, characterized in that: The volume ratio of the thick oil aging oil to the active water in step 1 is 1:0.8-1.

2.

3. The active water washing dehydration process for thick oil aging oil according to claim 1, characterized in that: The small molecule alcohol is one or more of methanol, ethanol, n-propanol and isopropanol, and the quaternary ammonium salt is one or both of trimethylammonium bromide and hexadecyl trimethylammonium bromide.

4. The active water washing dehydration process for thick oil aging oil according to claim 1, characterized in that: The preparation method of the reverse demulsifier is as follows: A: 0.2-0.4 parts of emulsifier and 2-3 parts of deionized water are taken in weight parts, heated to 50-65 DEG C under nitrogen atmosphere, 3-5 parts of composite monomer is added, and kept for 10-20 minutes to obtain a prepolymer liquid; B: 0.3-0.6 parts of 2%-3% ammonium persulfate aqueous solution is added into the prepolymer solution, stirred uniformly at room temperature, then heated to 60-80 DEG C, 30 parts of the composite monomer is added, pH is adjusted to 7-8, and incubated for 0.5-1 h, and then the reverse demulsifier is obtained.

5. The active water washing dehydration process of thick oil aged oil according to claim 4, characterized in that: The emulsifier is a mixture of lauric acid soap and sodium stearate, and the mass ratio of lauric acid soap to sodium stearate is 2:

1.

6. The active water washing dehydration process of thick oil aged oil according to claim 4, characterized in that: The composite monomer is a mixture of butyl acrylate, acrylic acid and beta-hydroxyethyl acrylate, and the mass ratio of butyl acrylate, acrylic acid and beta-hydroxyethyl acrylate is 5:2-3:2-3.

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