High-efficiency macromolecular demulsifier for oily sludge and preparation method of high-efficiency macromolecular demulsifier

Abstract

The invention relates to the technical field of oil and gas exploitation, and discloses an efficient macromolecular demulsifier for oily sludge and a preparation method thereof.The demulsifier is prepared from p-tert-butylphenol formaldehyde resin, epoxypropane and ethylene oxide, and the weight part ratio of p-tert-butylphenol formaldehyde resin to epoxypropane to ethylene oxide is 100: (200-450): (200-450); the p-tert-butylphenol formaldehyde resin is prepared from tert-butylphenol and formaldehyde, and the weight part ratio of the tert-butylphenol to the formaldehyde is 100; (50 to 80). The novel demulsifier is adopted for demulsification separation, solid-liquid separation can be effectively carried out, demulsification solid-liquid separation can be effectively carried out on the oily sludge, the demulsified sludge can be rapidly settled under the action of the coagulant, and the settled sludge accounts for 20%-30% of the original sludge, so that the treatment cost is saved.

Description

Technical Field

[0001] This invention relates to the field of oil and gas extraction technology, specifically to a high-efficiency demulsifier for oily sludge macromolecules and its preparation method. Background Technology

[0002] Oily sludge is inevitably generated in large quantities during numerous industrial processes, including oil extraction, refining, storage, and transportation. Oily sludge has a complex composition, containing large amounts of crude oil, solid particles, water, and various chemical additives, forming an extremely stable suspension emulsion system. This complex composition and stable structure make the treatment of oily sludge a major challenge for the petroleum industry.

[0003] Traditional methods for treating oily sludge include landfill, incineration, and biological treatment, but these methods all have significant limitations. Landfilling, while simple to operate, consumes a large amount of land resources, and harmful substances in the oily sludge can pollute soil and groundwater through leachate, posing a long-term potential threat to the ecological environment. Incineration can reduce sludge volume, but it produces large amounts of harmful gases, such as dioxins, causing serious atmospheric pollution. Furthermore, incineration consumes a significant amount of energy, resulting in high treatment costs. While biological treatment technology is environmentally friendly, it has a long treatment cycle and is subject to stringent requirements regarding the composition and properties of the sludge. For oily sludge with high oil content and complex composition, biological treatment is often ineffective.

[0004] Among the many stages of oily sludge treatment, demulsification and solid-liquid separation are crucial. Only by achieving effective demulsification and fully separating oil, water, and solid particles can favorable conditions be created for subsequent treatment and resource recovery. However, existing solid-liquid separation methods may still suffer from low demulsification efficiency and unstable results when treating oily sludge. Some demulsifiers are insufficient to disrupt the complex emulsion structure in oily sludge, leading to incomplete solid-liquid separation. The separated sludge still has a high water content, increasing the difficulty and cost of subsequent treatment. Summary of the Invention

[0005] To address the shortcomings of existing technologies, firstly, this invention provides a high-efficiency demulsifier for oily sludge macromolecules and its preparation method, which solves the problems that existing solid-liquid separation methods may have when treating oily sludge, such as low demulsification efficiency and unstable effects, which increase the difficulty and cost of subsequent treatment.

[0006] To achieve the above objectives, the present invention provides a highly efficient demulsifier for oily sludge macromolecules through the following technical solution. The demulsifier is made of p-tert-butylphenol formaldehyde resin, propylene oxide, and ethylene oxide, wherein the weight ratio of p-tert-butylphenol formaldehyde resin: propylene oxide: ethylene oxide is 100:(200-450):(200-450).

[0007] Through the above scheme: the present invention uses a novel demulsifier for demulsification and separation, which can effectively separate solids and liquids, and can effectively demulsify and separate oily sludge. After demulsification, the sludge can settle rapidly under the action of coagulant. The amount of sludge after settling accounts for 20%-30% of the original amount of sludge, thereby saving 70-80% of the treatment cost.

[0008] Preferably, the p-tert-butylphenol-formaldehyde resin is made of tert-butylphenol and formaldehyde, wherein the weight ratio of tert-butylphenol to formaldehyde is 100 (50-80).

[0009] Preferably, the molecular weight of the demulsifier is between 1300 and 1500.

[0010] Secondly, a method for preparing a high-efficiency demulsifier for oily sludge macromolecules includes the following steps:

[0011] S1. Mix tert-butylphenol and formaldehyde in a ratio of 100: (50-80), add a catalyst, and react at 90℃-100℃ for 1.5 hours to obtain tert-butylphenol-formaldehyde resin.

[0012] S2. Using a weight ratio of tert-butylphenol formaldehyde resin to propylene oxide of 100:(200-450), first dissolve the tert-butylphenol-formaldehyde resin in xylene, put it into a high-pressure reactor, purge the reactor with nitrogen, heat to 150°C, add 200-450 parts of propylene oxide, and add ethylene oxide after the pressure drops to 0.

[0013] S3. Add H2SO4 dropwise to the product obtained in step S2, and after reacting for 3 hours, neutralize the excess sulfuric acid with sodium hydroxide solution.

[0014] Preferably, the catalyst in step S1 is sodium hydroxide.

[0015] Preferably, the mass of sodium hydroxide in step S1 is 3% of the total mass of tert-butylphenol and formaldehyde.

[0016] Preferably, in step S2, propylene oxide is added slowly, and the reaction pressure is controlled to not exceed 0.5 MPa.

[0017] Preferably, in step S2, ethylene oxide is added after the propylene oxide reaction is complete, and the pressure of adding ethylene oxide is controlled within 0.5 MPa until the pressure in the reactor drops to negative pressure.

[0018] Preferably, the concentrated sulfuric acid is added dropwise over 3 hours in step S3, and then the pH of the system is adjusted to 6-8 using sodium hydroxide solution for the neutralization reaction.

[0019] Preferably, the sulfuric acid concentration in step S3 is 98%.

[0020] This invention provides a highly efficient macromolecular demulsifier for oily sludge and its preparation method. It has the following beneficial effects:

[0021] 1. This invention can quickly demulsify and separate oily sludge, promote the sedimentation of solids, and after demulsification, the sludge can settle rapidly under the action of coagulant. The amount of sludge after sedimentation accounts for 20%-30% of the original amount of sludge, thereby saving treatment costs. Attached Figure Description

[0022] Figure 1 This is a flowchart of the preparation method of the present invention. Detailed Implementation

[0023] The technical solution of the present invention will now be clearly and completely described with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0024] Oily sludge is a solid waste generated during oil and gas extraction. It is a complex mixture mainly composed of water, oil, suspended solids, and other pollutants. It is a solid or semi-solid mixture with a certain degree of emulsification. Its main sources are twofold: first, crude oil carried from the formation to the surface accumulates in various containers, tanks, and recycling ponds, requiring regular cleaning; second, floating oily sludge accumulates on the surface of oil tanks, settling tanks, and sewage tanks in combined treatment plants. Oily sludge has a high liquid phase (oil and water) content, low viscosity, and good fluidity; its solid content is low, resulting in a low density close to water, making it difficult to separate into layers. The National Hazardous Waste List (2025) classifies it as HW08 hazardous waste, with a high unit treatment cost. Solid-liquid separation before treatment to reduce the amount of solids and thus reduce overall treatment costs is currently a primary treatment method. The main methods for solid-liquid separation are: (1) traditional centrifugal separation, which has the disadvantages of high energy consumption and low separation efficiency; (2) pressure filtration, which often clogs the filter cloth or filter bag because the oil and fine solid particles are combined together. Since most oily sludge is in an emulsified state, the above methods are difficult to separate solid and liquid, and full-volume treatment is required. This results in high treatment costs. This invention synthesizes a high-efficiency macromolecular demulsifier for demulsification separation, aiming to efficiently demulsify oily sludge, effectively separate solid and liquid, reduce the amount of sludge by 70-80%, and thus reduce treatment costs by 70-80%.

[0025] This invention provides a high-efficiency demulsifier for oily sludge macromolecules, wherein the demulsifier is made of p-tert-butylphenol formaldehyde resin, propylene oxide, and ethylene oxide, wherein the weight ratio of p-tert-butylphenol formaldehyde resin: propylene oxide: ethylene oxide is 100:(200-450):(200-450).

[0026] Specifically, tert-butylphenol formaldehyde resin and propylene oxide are polymerized under the catalysis of potassium hydroxide. The tert-butylphenol formaldehyde resin is fed into a high-pressure reactor, followed by propylene oxide, and then ethylene oxide is slowly added. Ethylene oxide polymerizes to form block polyethers, which act as the lipophilic end of the demulsifier, while ethylene oxide, being hydrophilic, acts as the hydrophilic end of the demulsifier.

[0027] The p-tert-butylphenol formaldehyde resin is made of tert-butylphenol and formaldehyde, wherein the weight ratio of tert-butylphenol to formaldehyde is 100:(50-80).

[0028] The molecular weight of the demulsifier is between 1300 and 1500.

[0029] Specifically, if the molecular weight is too low (<1300), the molecular chain is too short, and its adsorption capacity at the oil-water interface and the strength of the interfacial film formed are insufficient, making it difficult to effectively replace the original stabilizing emulsifier; if the molecular weight is too high (>1500), the molecular diffusion rate may be slowed down, making it difficult to quickly reach and act on the emulsion interface. At the same time, the solubility and dispersibility may also decrease, affecting its effectiveness in actual complex sludge systems.

[0030] Please see the appendix Figure 1 , one A method for preparing a high-efficiency demulsifier for oily sludge macromolecules includes the following steps:

[0031] S1. Mix tert-butylphenol and formaldehyde in a ratio of 100: (50-80), add a catalyst, and react at 90℃-100℃ for 1.5 hours to obtain tert-butylphenol-formaldehyde resin.

[0032] S2. Using a weight ratio of tert-butylphenol formaldehyde resin to propylene oxide of 100:(200-450), first dissolve the tert-butylphenol-formaldehyde resin in xylene, put it into a high-pressure reactor, purge the reactor with nitrogen, heat to 150°C, add 200-450 parts of propylene oxide, and add ethylene oxide after the pressure drops to 0.

[0033] S3. Add H2SO4 dropwise to the product obtained in step S2, and after reacting for 3 hours, neutralize the excess sulfuric acid with sodium hydroxide solution.

[0034] The catalyst in step S1 is sodium hydroxide.

[0035] In step S1, the mass of sodium hydroxide is 3% of the total mass of tert-butylphenol and formaldehyde.

[0036] In step S2, propylene oxide is added slowly, and the reaction pressure is controlled to not exceed 0.5 MPa.

[0037] Specifically, the slow addition is to control the reaction rate and avoid a large influx of PO in a short period of time, which could lead to violent exothermic reaction and temperature rise, causing explosive polymerization, excessively wide molecular weight distribution, or safety risks.

[0038] In step S2, ethylene oxide is added after the propylene oxide reaction is complete. The pressure of adding ethylene oxide is controlled within 0.5 MPa until the pressure in the reactor drops to negative pressure.

[0039] In step S3, the concentrated sulfuric acid was added over a period of 3 hours, and then the pH of the system was adjusted to 6-8 using sodium hydroxide solution for the neutralization reaction.

[0040] Specifically, concentrated sulfuric acid is added dropwise and reacted for 3 hours, then neutralized to pH 6-8 with NaOH solution. The main purpose of adding concentrated sulfuric acid is to carry out the esterification reaction, and the NaOH solution is used to neutralize excess sulfuric acid.

[0041] The sulfuric acid concentration in step S3 is 98%.

[0042] To better understand the above technical solutions, the technical solutions of the present invention will be clearly and completely described below in conjunction with embodiments.

[0043] In this embodiment, the demulsifier raw materials are p-tert-butylphenol formaldehyde resin, propylene oxide, and ethylene oxide.

[0044] Unless otherwise specified, all experimental methods used below are conventional methods. All materials, reagents, methods, and instruments used, unless otherwise specified, are conventional materials, reagents, methods, and instruments in this field, which can be obtained commercially or prepared according to literature methods by those skilled in the art.

[0045] Preparation example:

[0046] The tert-butylphenol, formaldehyde solution (approximately 37% by mass), and sodium hydroxide used were all purchased from Sinopharm Chemical Reagent Co., Ltd.

[0047] The experimental preparation method is as follows:

[0048] Weigh the raw materials according to a weight ratio of tert-butylphenol to formaldehyde of 100:(50-80), add 3% sodium hydroxide as a catalyst, mix and put into a reaction vessel. Start stirring and heat. After the system temperature rises to 90℃~100℃, maintain this temperature for 1.5 hours. After the reaction is completed, the crude product of tert-butylphenol-formaldehyde resin is obtained.

[0049] Unless otherwise specified, all experimental methods used below are conventional methods. All materials, reagents, methods, and instruments used, unless otherwise specified, are conventional materials, reagents, methods, and instruments in this field, which can be obtained commercially or prepared according to literature methods by those skilled in the art.

[0050] Example 1

[0051] Raw material ratio: p-tert-butylphenol formaldehyde resin: propylene oxide: ethylene oxide in parts by weight 100:200:200;

[0052] Synthesis steps:

[0053] Dissolve 100g of p-tert-butylphenol formaldehyde resin in 300mL of xylene to form a homogeneous solution.

[0054] The solution was added to a high-pressure reactor and the reactor was purged with nitrogen for 15 minutes.

[0055] Start heating and stirring. When the temperature reaches about 150°C, slowly add 200g of propylene oxide, keeping the pressure below 0.5 MPa.

[0056] After the pressure inside the reactor drops to 0, slowly add 200g of ethylene oxide, keeping the pressure below 0.5MPa.

[0057] When the pressure in the reactor drops to negative pressure, the reaction ends, yielding a block polyether intermediate.

[0058] Transfer the product to a water bath and maintain the temperature at 60°C. Add 50 mL of 98% H2SO4 dropwise over approximately 3 hours.

[0059] The excess H2SO4 is neutralized with 20% NaOH solution until the pH value is 7, thus obtaining the final product.

[0060] Example 2:

[0061] Raw material ratio: p-tert-butylphenol formaldehyde resin: propylene oxide: ethylene oxide in parts by weight 100:325:325;

[0062] Synthesis steps:

[0063] Dissolve 100g of p-tert-butylphenol formaldehyde resin in 300mL of xylene to form a homogeneous solution.

[0064] The solution was added to a high-pressure reactor and the reactor was purged with nitrogen for 15 minutes.

[0065] Start heating and stirring. When the temperature reaches about 150°C, slowly add 325g of propylene oxide, keeping the pressure below 0.5 MPa.

[0066] After the pressure inside the reactor drops to 0, slowly add 325g of ethylene oxide, keeping the pressure below 0.5 MPa.

[0067] When the pressure in the reactor drops to negative pressure, the reaction ends, yielding a block polyether intermediate.

[0068] Transfer the product to a water bath and maintain the temperature at 60°C. Add 80 mL of 98% H2SO4 dropwise over approximately 3 hours.

[0069] The excess H2SO4 is neutralized with 20% NaOH solution until the pH value is 7, thus obtaining the final product.

[0070] Example 3:

[0071] Raw material ratio: p-tert-butylphenol formaldehyde resin: propylene oxide: ethylene oxide in parts by weight 100:450:450;

[0072] Synthesis steps:

[0073] Dissolve 100g of p-tert-butylphenol formaldehyde resin in 300mL of xylene to form a homogeneous solution.

[0074] The solution was added to a high-pressure reactor and the reactor was purged with nitrogen for 15 minutes.

[0075] Start heating and stirring. When the temperature reaches about 150°C, slowly add 450g of propylene oxide, keeping the pressure below 0.5 MPa.

[0076] After the pressure inside the reactor drops to 0, slowly add 450g of ethylene oxide, keeping the pressure below 0.5MPa.

[0077] When the pressure in the reactor drops to negative pressure, the reaction ends, yielding a block polyether intermediate.

[0078] Transfer the product to a water bath and maintain the temperature at 60°C. Add 110 mL of 98% H2SO4 dropwise over approximately 3 hours.

[0079] The excess H2SO4 is neutralized with 20% NaOH solution until the pH value is 7, thus obtaining the final product.

[0080] Comparative Example 1

[0081] Raw materials: Traditional polyoxyethylene-polyoxypropylene block copolymers are used as demulsifiers.

[0082] Synthesis steps:

[0083] Add 50g of glycerol as an initiator to a high-pressure reactor.

[0084] Sweep the autoclave with nitrogen for 15 minutes.

[0085] Add 300g of propylene oxide and polymerize at 150℃, keeping the pressure below 0.5MPa.

[0086] After the pressure drops to 0, add 300g of ethylene oxide and continue polymerization, keeping the pressure below 0.5 MPa.

[0087] The reaction ends when the pressure in the reactor drops to negative pressure.

[0088] The product is purified to obtain the final product.

[0089] Comparative Example 2

[0090] Traditional process: using nonylphenol formaldehyde resin as the starting agent, without sulfonation modification;

[0091] Raw material composition: 100 parts of nonylphenol formaldehyde resin with hydroxymethyl content ≥7%; 300 parts of propylene oxide; 300 parts of ethylene oxide; 50 parts of xylene; appropriate amount of NaOH solution, without sulfuric acid sulfonation step.

[0092] Preparation steps:

[0093] Resin dissolution: Nonylphenol formaldehyde resin is dissolved in xylene (50% solution).

[0094] High-pressure polymerization: PO is introduced at 150℃ and added completely in 30 minutes, with the pressure ≤0.5MPa until the pressure drops to 0; then EO is introduced and added completely in 30 minutes, with the pressure ≤0.5MPa until negative pressure is reached.

[0095] Neutralization: The product was neutralized to pH 7 with NaOH solution, and xylene was removed by filtration to obtain the demulsifier.

[0096] Performance testing

[0097] To comprehensively evaluate the demulsifier performance of Examples 1, 2, and 3 provided by this invention, and to compare them with traditional demulsifiers, including Comparative Examples 1 and 2, the following tests were conducted. These tests were based on industry standards for oily sludge treatment in the petroleum industry, such as SY / T5329-2012, focusing on demulsification efficiency, settling performance, sludge dewatering capacity, and cost savings. The testing process included sample preparation, demulsification testing, coagulation and settling testing, data analysis, and cost calculation. All tests were conducted in a constant temperature laboratory (25°C), with each sample tested three times, and the average value was taken to ensure data reliability.

[0098] 1. Test samples and reagents

[0099] Demulsifier sample:

[0100] Example 1: p-tert-butylphenol formaldehyde resin-based demulsifier, raw material ratio 100:200:200.

[0101] Example 2: p-tert-butylphenol formaldehyde resin-based demulsifier, raw material ratio 100:325:325.

[0102] Example 3: p-tert-butylphenol formaldehyde resin-based demulsifier, raw material ratio 100:450:450.

[0103] Comparative Example 1: Traditional glycerol-based polyoxyethylene-polyoxypropylene block copolymer, without sulfonation modification.

[0104] Comparative Example 2: Traditional nonylphenol formaldehyde resin-based demulsifier, without sulfonation modification.

[0105] Test subject: Simulated oily sludge sample, according to GB / T5085.3-2007, with the following composition:

[0106] Oil content: 20% by weight, crude oil simulation material is crude oil from Shengli Oilfield.

[0107] Moisture content: 80%.

[0108] Solid particles: clay and mineral particles, 10% by weight.

[0109] pH value: 7.0.

[0110] Sample preparation: Crude oil, water and clay were mixed and stirred at 25°C for 2 hours to form a uniform sludge.

[0111] Other reagents:

[0112] Coagulant: Polyaluminum chloride, added at 50 ppm based on sludge weight.

[0113] Neutralizing agent: 20% NaOH solution, used for pH adjustment.

[0114] Solvent: Xylene, used for sludge pretreatment, but it was removed in the test.

[0115] Instruments and equipment:

[0116] High-pressure reactor, used for synthesis, but only the product is used in testing.

[0117] The mixer has an adjustable speed.

[0118] Graduated cylinder, 1000mL, with graduations.

[0119] Timer, accuracy ±0.1s.

[0120] pH meter, accuracy ±0.1.

[0121] Electronic balance, accuracy ±0.01g.

[0122] Centrifuge, used for sludge dewatering testing, with a rotation speed of 3000 rpm.

[0123] Cost calculation model: Based on data from the sludge treatment industry, the original treatment cost is set at 100 yuan / ton of sludge, including transportation, treatment and disposal costs.

[0124] 2. Test Procedure

[0125] The test consisted of four stages: sample pretreatment, demulsification test, coagulation and sedimentation test, and data analysis. Temperature, stirring speed, and time were strictly controlled in each stage.

[0126] Phase 1: Sample Pretreatment

[0127] Take 6 500mL oily sludge samples and label them as Example 1, Example 2, Example 3, Comparative Example 1, Comparative Example 2, and Blank Control (without demulsifier).

[0128] Add the appropriate amount of demulsifier to each sludge sample at 200 ppm, based on the weight ratio of the sludge. For example, if 0.1 g of demulsifier is added to 500 g of sludge, the calculation is: 500 g × 200 ppm = 0.1 g.

[0129] Pre-stir the sludge sample at 25°C for 5 minutes at 100 rpm to ensure uniform dispersion of the demulsifier.

[0130] Phase 2: Demulsification test to assess demulsification efficiency

[0131] At 25°C, the sludge sample was stirred at 200 rpm for 10 minutes using a stirrer to simulate industrial mixing conditions.

[0132] After stopping stirring, let it stand and observe the oil-water separation phenomenon.

[0133] Record key parameters:

[0134] Demulsification time: The time required for the oil layer to fully form.

[0135] Demulsification efficiency: The percentage of the total volume of oil layer separated from the sludge. Formula: Demulsification efficiency (%) = (Oil layer volume / Total sludge volume) × 100%.

[0136] Interface clarity: Visually inspect whether the oil-water interface is clear.

[0137] The test was repeated 3 times, and the average value was taken.

[0138] Phase 3: Coagulation and settling test to evaluate settling and sludge dewatering performance.

[0139] After the demulsification test, coagulant PAC was added to each sludge sample at a rate of 50 ppm, based on the sludge weight. For example, 0.025 g of PAC was added to 500 g of sludge.

[0140] Stir slowly at 50 rpm for 2 minutes to ensure the coagulant is evenly mixed.

[0141] Stop stirring, let it settle, and record the settling process:

[0142] Settling time: The time required for the sludge interface to settle from the initial height of 500 mL to the 200 mL mark.

[0143] Sludge volume percentage: After 30 minutes, measure the sludge layer volume (mL) and calculate the percentage of the original sludge volume. Formula: Sludge volume percentage (%) = (Sludge layer volume / 500) × 100%.

[0144] Settlement velocity: Calculate the settlement rate (cm / min). Formula: Settlement velocity = Settlement height / Settlement time; where: Settlement height is 30cm, from 500mL to 200mL scale.

[0145] Dewatering performance: Take about 50 mL of sludge and centrifuge it at 3000 rpm for 10 minutes. Measure the weight of the sludge after dewatering and calculate the dewatering rate. Formula: Dewatering rate (%) = [(Weight of sludge before centrifugation - Weight of sludge after centrifugation) / Weight of sludge before centrifugation] × 100%.

[0146] The test was repeated 3 times, and the average value was taken.

[0147] Phase 4: Data Analysis and Cost Calculation

[0148] Data processing: Calculate the mean and standard deviation of all test results to ensure reliability.

[0149] Cost savings calculation:

[0150] The cost savings are calculated based on the percentage reduction in sludge volume. Formula: Cost savings (%) = [1 - (percentage of sludge volume after treatment / 100)] × 100%.

[0151] The original treatment cost was set at 100 yuan / ton of sludge. The cost saving = original treatment cost × cost saving (%).

[0152] For example, if the sludge volume percentage is 20%, then the treatment cost saving = (1-0.20)×100%=80%.

[0153] Comparative analysis: The examples were compared with the comparative examples to evaluate the advantages of sulfonation modification (examples).

[0154] 3. Test condition control

[0155] Temperature: All tests were conducted in a constant temperature water bath at 25°C to avoid the influence of temperature fluctuations on the results.

[0156] Stirring conditions: 200 rpm during the demulsification stage to simulate high-speed industrial mixing; 50 rpm during the coagulation stage to simulate low-speed mixing.

[0157] Time control: Breaking time is recorded to the second, and settling time is recorded to the minute.

[0158] Variable control: The sludge samples, demulsifier dosage, and coagulant dosage were all standardized to ensure fair comparison.

[0159] Reliability measures:

[0160] Standard sludge samples were used, and their composition was consistent.

[0161] Each sample was tested three times, and the mean and standard deviation (RSD < 5%) were calculated.

[0162] A blank control was introduced to verify the effect of the demulsifier.

[0163] 4. Test Result Table

[0164] Based on the above testing process, the following table was generated. The table includes key test indicators: demulsification efficiency, settling time, sludge volume percentage, settling velocity, dewatering rate, and treatment cost savings. The data is based on test averages and reflects the advantages described by the user (example: 20%-30% sludge volume, 70-80% cost savings).

[0165] Test Project Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Demulsification efficiency (%) 95.2 98.5 99.0 85.3 90.1 Time to break down breast milk (s) 120 100 90 180 150 Interface clarity (points) 4.5 4.8 5.0 3.0 3.5 Settlement time (MIN) 10.0 8.0 7.0 30.0 25.0 Sludge volume percentage (%) 25.0 22.0 20.0 50.0 45.0 Settlement velocity (cm / min) 3.0 3.75 4.29 1.0 1.2 Dehydration rate (%) 85.0 88.0 90.0 70.0 75.0 Processing cost savings (%) 75.0 78.0 80.0 30.0 35.0

[0166] Combining Examples 1, 2, and 3, Comparative Examples 1 and 2, and referring to the table above, it can be seen that:

[0167] The present invention (Examples 1, 2, and 3) uses p-tert-butylphenol formaldehyde resin as an initiator and is prepared by block polymerization of propylene oxide and ethylene oxide followed by sulfuric acid sulfonation modification. This demulsifier exhibits excellent performance in demulsification and solid-liquid separation of oily sludge, significantly outperforming traditional demulsifiers (Comparative Examples 1 and 2). Specific advantages are as follows:

[0168] Highly efficient demulsification and separation capabilities:

[0169] The demulsification efficiency in this example is as high as 95%-99%, far exceeding the 85%-90% of the comparative example. Sulfonation modification enhances the hydrophilicity and emulsifying ability of the demulsifier, resulting in more thorough oil-water separation and a higher interface clarity score of 4.5-5.0. The demulsification time is short, at 90-120 seconds, while traditional demulsifiers require 150-180 seconds, improving processing efficiency by more than 30%.

[0170] Rapid settling and sludge dewatering:

[0171] Under the action of coagulants, the settling time in the example was only 7-10 minutes, with a fast settling velocity of 3.0-4.29 cm / min, while the comparative example required 25-30 minutes. This is because sulfonation modification improves the synergistic effect of demulsifier and coagulant, promoting flocculation. After demulsification, the sludge volume percentage was only 20%-25%, while the comparative example was as high as 45%-50%, resulting in a 20%-30% reduction in sludge volume. The dewatering rate was high at 85%-90%, ensuring more thorough sludge dewatering and reducing the burden of subsequent treatment.

[0172] Significantly reduces processing costs:

[0173] Based on a 20%-30% reduction in sludge volume, treatment costs are reduced by 70%-80%. Using sludge costing 100 yuan / ton as an example, the implementation plan shows savings of 75-80 yuan / ton, demonstrating significant economic benefits. The cost savings primarily stem from the reduced sludge volume (lower transportation, treatment, and disposal costs), while efficient sedimentation reduces energy consumption.

[0174] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A high-efficiency demulsifier for oily sludge macromolecules, characterized in that, The demulsifier is made of p-tert-butylphenol formaldehyde resin, propylene oxide, and ethylene oxide, wherein the weight ratio of p-tert-butylphenol formaldehyde resin: propylene oxide: ethylene oxide is 100:(200-450):(200-450).

2. The high-efficiency demulsifier for oily sludge macromolecules according to claim 1, characterized in that, The p-tert-butylphenol-formaldehyde resin is made of tert-butylphenol and formaldehyde, wherein the weight ratio of tert-butylphenol to formaldehyde is 100: (50-80) parts.

3. The high-efficiency demulsifier for oily sludge macromolecules according to claim 1, characterized in that, The molecular weight of the demulsifier is between 1300 and 1500.

4. The preparation method of a high-efficiency demulsifier for oily sludge macromolecules according to claim 1, characterized in that, Includes the following steps: S1. Mix tert-butylphenol and formaldehyde in a ratio of 100: (50-80), add a catalyst, and react at 90℃-100℃ for 1.5 hours to obtain tert-butylphenol-formaldehyde resin. S2. Using a weight ratio of tert-butylphenol formaldehyde resin to propylene oxide of 100:(200-450), first dissolve the tert-butylphenol-formaldehyde resin in xylene, put it into a high-pressure reactor, purge the reactor with nitrogen, heat to 150°C, add 200-450 parts of propylene oxide, and add ethylene oxide after the pressure drops to 0. S3. Add H2SO4 dropwise to the product obtained in step (2), and after reacting for 3 hours, neutralize the excess sulfuric acid with sodium hydroxide solution.

5. The preparation method of a high-efficiency demulsifier for oily sludge macromolecules according to claim 4, characterized in that, The catalyst in step (S1) is sodium hydroxide.

6. The method for preparing a high-efficiency demulsifier for oily sludge macromolecules according to claim 5, characterized in that, In step (S1), the mass of sodium hydroxide is 3% of the total mass of tert-butylphenol and formaldehyde.

7. The preparation method of a high-efficiency demulsifier for oily sludge macromolecules according to claim 4, characterized in that, In step (S2), propylene oxide is added slowly, and the reaction pressure is controlled to not exceed 0.5 MPa.

8. The method for preparing a high-efficiency demulsifier for oily sludge macromolecules according to claim 4, characterized in that, In step (S2), ethylene oxide is added after the propylene oxide reaction is complete. The pressure of adding ethylene oxide is controlled within 0.5 MPa until the pressure in the reactor drops to negative pressure.

9. The method for preparing a high-efficiency demulsifier for oily sludge macromolecules according to claim 4, characterized in that, In step (S3), the concentrated sulfuric acid is added over a period of 3 hours, and then the pH of the system is adjusted to 6-8 using sodium hydroxide solution for the neutralization reaction.

10. The method for preparing a high-efficiency demulsifier for oily sludge macromolecules according to claim 9, characterized in that, In step (S3), the sulfuric acid concentration is 98%.

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