High-efficiency oil sludge separation agent, preparation method and application thereof in oil sludge cleaning

Abstract

The present application relates to a kind of high-efficiency oil sludge separating agent, preparation method and its application in oil sludge cleaning.The high-efficiency oil sludge separating agent includes the following weight parts of component, coconut oil diethanolamide 25-45 parts, sulfonated succinic acid dioctyl ester sodium salt 15-25 parts, sodium dodecyl sulfate 3-10 parts, propylene glycol 1-5 parts, alpha-pinene or limonene 3-10 parts, alpha-terpineol or menthol 3-10 parts, acetyl linaloe 3-8 parts, citral 1-5 parts, water 15-25 parts.The application of the high-efficiency oil sludge separating agent in oil sludge cleaning includes the following steps, S1, oil sludge and agent are loaded into first container;S2, add cleaning water, keep the temperature of mixed solution at 50-70 DEG C, use stirrer to carry out high-speed shearing stirring, stirring speed is above 3000r / min;S3, after stirring, mixed solution is transferred to second container, continue to add cleaning water;S4, continue to stir, stirring speed is above 100r / min.The present application has good oil sludge separation efficiency.

Description

Technical Field

[0001] This invention belongs to the field of CO2F sludge treatment technology, and specifically relates to a highly efficient oil sludge separation agent, its preparation method, and its application in oil sludge cleaning. Background Technology

[0002] Oil sludge is one of the main pollutants generated during oilfield production and is classified as HW08 hazardous waste in the National Hazardous Waste List. In recent years, pyrolysis has gradually become the preferred method for oil sludge treatment. For oil sludge with oil recovery value, a hot washing process is often used to pre-wash the sludge. This involves adding oil-sludge separating agents, supplemented by heating and stirring, to promote the separation of oil and mud-water. After the separated oil is recovered, the remaining portion enters the next processing stage. The selection of the oil-sludge separating agent is a decisive factor in the effectiveness of the hot washing process.

[0003] Existing technologies have continuously explored formulations for oil sludge separation agents. For example, Chinese patent document CN109231355A discloses a method for purifying and treating polymer-containing oil sludge and the cleaning agent used. The cleaning agent comprises the following components by weight: 2-6 parts by weight of anionic surfactant, 0.5-3 parts by weight of nonionic surfactant, and 3-15 parts by weight of detergent builder. The anionic surfactant includes branched alkylbenzene sulfonates, the nonionic surfactant includes any one or at least two combinations of cocamidopropyl hydroxysulfonate, alkylphenol polyoxyethylene ether, and cocamidopropyl hydroxysulfonate, and the detergent builder includes any one or at least two combinations of sodium silicate, sodium hydroxide, and sodium citrate. This method first adds hydrogen peroxide to the polymer-containing oil sludge to break it up, then adds the cleaning agent composed of the above formulation, claiming that after a reaction of 15-20 minutes, oil sludge with an oil content of less than 1% can be obtained. Chinese patent document CN 111575122A discloses an oil sludge cleaning agent, its preparation method, and its application. The sludge cleaning agent, by weight percentage, comprises the following components: 5-20% phosphate, 5-20% inorganic salt, 10-20% silicate, 2-5% alkali, 2-4% coconut oil fatty acid diethanolamide, 2-4% nonylphenol polyoxyethylene ether, 2-4% fatty alcohol polyoxyethylene ether phosphate, 2-4% oil stain remover, with the balance being water. When the sludge cleaning agent is added at 5-8% of the sludge mass, the mixture is stirred in a water bath at 70-80℃ for 40-60 minutes. After the reaction, the solution is transferred to centrifuge tubes and centrifuged while hot at 3000-3500 r / min for 3-5 minutes. The resulting sludge (dry basis) contains less than 1% oil.

[0004] While existing technologies disclose various formulations of sludge separation agents, claiming highly satisfactory experimental results, the sludge separation agents available to the applicant have not yielded ideal results in actual application. Therefore, the applicant organized manpower to develop sludge separation agents, resulting in the solution described in this application. Summary of the Invention

[0005] The first objective of this invention is to provide a highly efficient oil sludge separation agent to improve the separation effect of oil and sludge in oil sludge.

[0006] The high-efficiency oil sludge separation agent comprises the following components in parts by weight: 25-45 parts of cocoyl diethanolamide, 15-25 parts of sodium dioctyl sulfosuccinate, 3-10 parts of sodium dodecyl sulfate, 1-5 parts of propylene glycol, 3-10 parts of α-pinene or limonene, 3-10 parts of α-terpineol or menthol, 3-8 parts of linalool acetate, 1-5 parts of citral, and 15-25 parts of water.

[0007] In one embodiment, the high-efficiency sludge separation agent comprises the following components in parts by weight: 30 parts of cocoyl diethanolamide, 20 parts of sodium dioctyl sulfosuccinate, 6 parts of sodium dodecyl sulfate, 3 parts of propylene glycol, 5 parts of α-pinene, 5 parts of α-terpineol, 3 parts of linalool acetate, 3 parts of citral, and 20 parts of water.

[0008] In another embodiment, the high-efficiency sludge separation agent comprises the following components in parts by weight: 30 parts of cocoyl diethanolamide, 15 parts of sodium dioctyl sulfosuccinate, 5 parts of sodium dodecyl sulfate, 3 parts of propylene glycol, 8 parts of limonene, 4 parts of menthol, 5 parts of linaloyl acetate, 2 parts of citral, and 15 parts of water.

[0009] Another aspect of the present invention is to provide a method for preparing the above-mentioned high-efficiency sludge separation agent, comprising the following steps:

[0010] S1. Dissolve sodium dodecyl sulfate and propylene glycol in water to obtain solution A;

[0011] S2. Mix α-pinene or limonene, α-terpineol or menthol, linalool acetate, citral, sodium dioctyl sulfosuccinate, and diethanolamide of cocoate, and stir until homogeneous to obtain solution B.

[0012] S3. Add reagent A to solution B, stir well, and obtain the target reagent.

[0013] A third aspect of the present invention is to provide the application of the above-mentioned high-efficiency sludge separation agent in sludge cleaning, comprising the following steps:

[0014] S1. Add the sludge to the cleaning water and keep the temperature of the mixture at 50-70℃;

[0015] S2. Adjust the pH range of the mixture to 7-11;

[0016] S3. Add the reagent, with the ratio of reagent to sludge being 1:10-20.

[0017] S4. Use a stirrer for high-speed shearing and stirring, with a stirring speed of 3000 r / min or higher, for 15-25 minutes;

[0018] S5. After settling and separating, the oil layer, water layer, and sand layer are separated.

[0019] As an alternative application method, the application of the above-mentioned high-efficiency sludge separation agent in sludge cleaning includes the following steps:

[0020] S1. Put the sludge and the agent into the first container, with the ratio of the amount of agent added to the amount of sludge added being 1:10-20.

[0021] S2. Add cleaning water to keep the temperature of the mixture at 50-70℃. Use a stirrer to perform high-speed shearing and stirring at a speed of 3000r / min or more for 10-15min.

[0022] S3. Transfer the stirred mixture to the second container, continue to add washing water, and adjust the pH range of the mixture to 7-11;

[0023] S4. Continue stirring at a speed of 100 r / min or higher for 10-20 minutes.

[0024] S5. After settling and separating, the oil layer, water layer, and sand layer are separated.

[0025] The beneficial effects of the present invention are as follows: the agent described in the present invention has a good oil-sludge separation effect, which can reduce the oil content of the treated bottom mud to about 2%; secondly, the application method of the high-efficiency oil-sludge separation agent in oil-sludge cleaning proposed in this application provides a new model for its practical application in engineering. Attached Figure Description

[0026] Figure 1 This is a graph showing the relationship between different dosages of reagents and the oil content of the sediment in Example 1 of the present invention.

[0027] Figure 2 This is a graph showing the relationship between different stirring speeds and the oil content of the bottom mud in Example 1 of the present invention. Detailed Implementation

[0028] Example 1

[0029] 1. Preparation of high-efficiency oil sludge separation agents

[0030] Dissolve 6g of sodium dodecyl sulfate and 3g of propylene glycol in 20g of water to obtain solution A. Mix 5g of α-pinene, 5g of α-terpineol, 3g of linalool acetate, 3g of citral, 20g of sodium dioctyl sulfosuccinate, and 30g of cocoyl diethanolamide, and stir until homogeneous to obtain solution B. Then slowly add solution A to solution B and stir until homogeneous to obtain the target reagent.

[0031] 2. Application of high-efficiency oil sludge separation agents

[0032] The experimental sludge came from Liaohe Oilfield, with a viscosity of 16 Cp, an oil content of 26%, a water content of 44%, and a solid content of 30%.

[0033] (1) Effect of different dosages of reagents on the oil content of sediment

[0034] Take 20g of oil sludge, add 100ml of water and an appropriate amount of reagent to adjust the pH to 10. Use a stirrer for high-speed shear stirring at 3000 rpm and 60°C. Stir for 15 minutes, then let stand for 1 hour. The oil sludge mixture is separated into three layers: an upper oil layer, a middle water layer, and a lower mud and sand layer.

[0035] Take samples of bottom sediment and use an infrared oil analyzer to measure the oil content of the sediment.

[0036] Figure 1 The image shows the oil content distribution of the sediment after adding 0.2g (1% of the oily sludge mass), 0.4g (1%), 0.6g (3%), 1g (5%), 2g (10%), and 4g (20%) of the reagent, respectively. Figure 1 It can be seen that as the dosage of the chemical increases, the oil content in the sediment gradually decreases, reaching 1.29 mg / g when the dosage reaches 1g. Furthermore, when the dosage is further increased, the decreasing trend in sediment oil content slows down, thus reducing the economic benefits of adding the chemical.

[0037] (2) Effect of different stirring speeds on the oil content of bottom sediment

[0038] Take 20g of sludge, add 100ml of water and 1g of reagent, adjust the pH to 10, and maintain the temperature at 60°C. Use a stirrer for shearing and mixing at speeds of 50r / min, 100r / min, 200r / min, 500r / min, 1000r / min, 3000r / min, 5000r / min, and 8000r / min. Speeds above 1000r / min represent high-speed shearing using a spiral reamer. Mix for 15 minutes, then allow to stand for 1 hour.

[0039] The results are as follows Figure 2As shown, the oil content in the sediment gradually decreases with increasing stirring speed. When the stirring speed increases from 50 r / min to 500 r / min, the oil content in the sediment decreases from 24.3 mg / g to 16.59 mg / g, a relatively limited decrease. When the stirring speed is further increased and high-speed shearing is applied, the oil content decreases significantly. When the shearing speed increases from 1000 r / min to 8000 r / min, the oil content in the sediment decreases from 6.54 mg / g to 1.17 mg / g. When the stirring speed is above 3000 r / min, the oil content is below 2%.

[0040] (3) Effect of pre-high-speed shearing on oil content in bottom sediment

[0041] The aforementioned experiments demonstrate that the crushing effect generated by high-speed shearing effectively promotes oil-sludge separation and reduces the oil content of bottom sludge. Considering the size of the oil-sludge separation tank, the viscosity of the oil-sludge, and economic benefits in engineering applications, a process of pre-treatment crushing followed by agitation and separation is considered in engineering practice.

[0042] Take 20g of sludge, add 1g of reagent, add 100ml of water, adjust the pH to 10, and perform high-speed shearing (3000r / min) at 60°C for 15min. This is experimental group 1#.

[0043] Take 20g of sludge and add 30ml of water. Then, mix the sludge and water together and stir at high speed for 15 minutes at 3000 rpm. Then, transfer the mixture to a beaker, add 70ml of water and 1g of reagent, adjust the pH to 10, heat and stir for 15 minutes at 60°C and 100 rpm. This is experimental group #2.

[0044] In sample #1, the oil-sludge mixture produced almost no foam. In sample #2, however, a certain amount of foam was generated during the pre-shearing process, which disappeared after the addition of the reagent and completion of the stirring process. This indicates that the product can also reduce the surface tension of the oil-sludge mixture, reduce bubble generation, and facilitate subsequent processing.

[0045] After standing for 1 hour, bottom sediment was collected, and its oil content was tested using an infrared oil analyzer. The measurements showed that the oil content of group 1# was 1.81 mg / g, while the oil content of group 2# was approximately 2.04 mg / g, indicating similar results.

[0046] (4) Effects of pre-shearing rate and post-stirring rate on the content of oily sludge bottom mud

[0047] We established a more detailed orthogonal experiment to explore the effects of pre-shearing rate and stirring speed on separation efficiency and oil content in the sediment during the pre-shearing process. Specific experimental parameters are shown in the table below. The high-speed pre-shearing time and low-speed stirring time were both 15 min.

[0048] Table 1. Effects of pre-shear rate and post-stirring rate on the content of oily sludge in the bottom mud.

[0049]

[0050] As shown in the table above, the oil content of the sludge decreases with increasing pre-shear speed. While increasing the stirring speed also slightly reduces the oil content, the effect is not as significant as increasing the pre-shear speed. This indicates that the degree of fragmentation caused by shearing has a greater impact on the separation effect. Considering economic factors, the minimum requirements are a pre-high-speed shear speed of 3000 r / min and a stirring speed of 100 r / min.

[0051] 3. Comparison of the effects of sludge cleaning conditioner and commercial chemicals

[0052] This reagent was compared with a commercially available reagent. The commercially available reagent, model JRC-31884, mainly consists of 8 parts sodium silicate, 20 parts n-butanol, 18 parts sodium dodecyl sulfonate, 24 parts coconut diethanolamide, 8 parts fatty alcohol polyoxyethylene ether, 8 parts alkylphenol polyoxyethylene ether, 10 parts water, and 4 parts other trace components. The reagent underwent shear separation and pre-shear stirring separation processes, and the results were compared with the experimental reagent prepared according to this specification.

[0053] Take 20g of sludge, add 1g of commercial reagent, add 100ml of water, adjust the pH to 10, and perform high-speed shearing (3000r / min) at 60°C for 15min. This is experimental group 3#.

[0054] Take 20g of sludge and add 30ml of water. Then, mix the sludge and water together and stir at high speed for 15 minutes at 3000 rpm. Then, transfer the mixture to a beaker, add 70ml of water and 1g of commercial reagent to adjust the pH to 10. Heat and stir for 15 minutes at 60°C and 100 rpm. This is experimental group #4.

[0055] After standing for 1 hour, bottom sediment was collected, and its oil content was tested using an infrared oil analyzer. The measurements showed that group #3 had an oil content of 5.93 mg / g, while group #4 had an oil content of approximately 7.48 mg / g. The separation effect was not as good as that of the reagent prepared in this application.

[0056] Example 2

[0057] 1. Preparation of high-efficiency oil sludge separation agents

[0058] Dissolve 5g sodium dodecyl sulfate and 3g propylene glycol in 15g water to obtain solution A. Mix 8g limonene, 4g menthol, and 5g linalool acetate. Combine 2g citral, 15g sodium dioctyl sulfosuccinate, and 30g cocoyl diethanolamide, and stir until homogeneous to obtain solution B. Slowly add solution A to solution B and stir until homogeneous to obtain the target reagent.

[0059] 2. Application of high-efficiency oil sludge separation agents

[0060] The experimental sludge came from an oil field in Xinjiang. It had a viscosity of 14 Cp, an oil content of 18%, a water content of 38%, and a solid content of 44%.

[0061] Take 20g of oil sludge, add 100ml of water and an appropriate amount of reagent to adjust the pH to 10. Mechanically stir using a stirrer at 3000 rpm and 60°C for 20 minutes, then allow it to stand and separate into three layers. The oil sludge mixture was separated into three layers: an upper oil layer, a middle water layer, and a lower mud and sand layer. This was designated as experimental group 5.

[0062] A commercially available reagent was used in the experiment, designated as experimental group 6#. The main components of the commercial reagent were sodium silicate, n-butanol, and sodium dodecyl sulfate, which were compared with other reagents. 20g of oil sludge was taken, 100ml of water was added, and 1g of the reagent was added to adjust the pH to 10. Mechanical stirring was performed using a stirrer at 3000 rpm and a temperature of 60°C. Stirring was carried out for 20 minutes, followed by settling. The mixture of oil sludge and water separated into three layers: an upper oil layer, a middle water layer, and a lower mud and sand layer.

[0063] Testing revealed that the oil content of the sediment in experimental group #5 was 1.3 mg / g, while the oil content of the sediment in commercial reagent #6 was 2.0 mg / g. Both materials can reduce the oil content of the sediment to below or reach 2.0 mg / g. However, the treatment effect of the reagent described in this experiment is still superior to that of the commercial material.

Claims

1. A high-efficiency oil sludge separation agent, characterized in that: It includes the following components in parts by weight: 25-45 parts of cocoyl diethanolamide, 15-25 parts of sodium dioctyl sulfosuccinate, 3-10 parts of sodium dodecyl sulfate, 1-5 parts of propylene glycol, 3-10 parts of α-pinene or limonene, 3-10 parts of α-terpineol or menthol, 3-8 parts of linalool acetate, 1-5 parts of citral, and 15-25 parts of water.

2. The high-efficiency oil sludge separation agent as described in claim 1, characterized in that: The product comprises the following components in parts by weight: 30 parts of cocoyl diethanolamide, 20 parts of sodium dioctyl sulfosuccinate, 6 parts of sodium dodecyl sulfate, 3 parts of propylene glycol, 5 parts of α-pinene, 5 parts of α-terpineol, 3 parts of linalool acetate, 3 parts of citral, and 20 parts of water.

3. The high-efficiency oil sludge separation agent as described in claim 1, characterized in that: The product comprises the following components in parts by weight: 30 parts cocoyl diethanolamide, 15 parts sodium dioctyl sulfosuccinate, 5 parts sodium dodecyl sulfate, 3 parts propylene glycol, 8 parts limonene, 4 parts menthol, 5 parts linalyl acetate, 2 parts citral, and 15 parts water.

4. The application of the high-efficiency oil sludge separation agent according to claim 1 in oil sludge cleaning, characterized in that, Includes the following steps, S1. Add the sludge to the cleaning water and keep the temperature of the mixture at 50-70℃; S2. Adjust the pH range of the mixture to 7-11; S3. Add the reagent, with the ratio of reagent to sludge being 1:10-20. S4. Use a stirrer for high-speed shearing and stirring, with a stirring speed of 3000 r / min or higher, for 15-25 minutes; S5. After settling and separating, the oil layer, water layer, and sand layer are separated.

5. The application of the high-efficiency oil sludge separation agent according to claim 1 in oil sludge cleaning, characterized in that, Includes the following steps, S1. Put the sludge and the agent into the first container, with the ratio of the amount of agent added to the amount of sludge added being 1:10-20. S2. Add cleaning water to keep the temperature of the mixture at 50-70℃. Use a stirrer to perform high-speed shearing and stirring at a speed of 3000r / min or more for 10-15min. S3. Transfer the stirred mixture to the second container, continue to add washing water, and adjust the pH range of the mixture to 7-11; S4. Continue stirring at a speed of 100 r / min or higher for 10-20 minutes. S5. After settling and separating, the oil layer, water layer, and sand layer are separated.

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