Quantitative analysis method, treatment method, filter device preparation method, and filter device for petroleum emulsified waste liquid

Abstract

The application discloses a kind of quantitative analysis method, processing method, filter device preparation method and filter device of petroleum emulsion waste liquid, the quantitative analysis method includes: using filter device to 0.5~1.5mL / s with the filter rate of petroleum emulsion waste liquid is filtered and is handled, and the filtrate before petroleum emulsion waste liquid is filtered through each filter layer of filter device is obtained respectively;Filter device is washed back with 0.2~1.0mL / s with the filter rate, to obtain the filtrate of each filter layer;Determine the oil content in filtrate based on petroleum determination method, and determine the content of the combination of oil and particulate matter in petroleum emulsion waste liquid according to oil content and the weight of filtrate, the effect and quantification of emulsification caused by particulate matter are shown, which provides a basis for further demulsification.

Description

Technical Field

[0001] This invention relates to the field of petroleum and petrochemical oil-containing pollutant tracing and stability analysis technology, and in particular to a quantitative analysis method, treatment method, filtration device preparation method, and filtration device for petroleum-based emulsified wastewater. Background Technology

[0002] During crude oil processing, the increasing quality and density of crude oil leads to the formation of oily wastewater in an emulsified form. The interaction of oils, surfactants, and solid particles within this emulsified wastewater makes separation extremely difficult. Emulsified wastewater is challenging to treat using conventional processes; a clear understanding of its emulsification characteristics and the overcoming of interactions among the emulsions are essential for effective separation. Establishing quantitative analysis standards for petroleum-based emulsions, based on separation process performance, for highly stable emulsified systems can guide the design and optimization of separation and treatment processes for oily emulsified waste in the petroleum and petrochemical industry, ensuring the reduction, harmlessness, and resource recovery of oily waste in this sector.

[0003] Currently, oily substances in oily wastewater are classified into suspended oil, dispersed oil, emulsified oil, and dissolved oil based on particle size differences. However, for complex and stable systems involving interactions between the oil phase, solid phase, polymer, and aqueous phase, no clear quantitative analysis standard for petroleum emulsions based on separation performance has been established. Two standards for petroleum determination, "Determination of Petroleum and Animal / Vegetable Oils in Water - Infrared Spectrophotometry" (HJ637-2018) and "Determination of Petroleum in Water - Ultraviolet Spectrophotometry (Trial)" (HJ970-2018), clearly define the standard methods and procedures for determining petroleum in wastewater. However, these two methods determine total oil, total petroleum, and total animal / vegetable oils in wastewater, without explicitly proposing quantitative methods for suspended oil, dispersed oil, emulsified oil, and dissolved oil related to separation process performance. The petrochemical industry standard "Determination of Four Components of Petroleum Asphalt (NB SH T0509-2010)" proposes methods and processes for separating asphaltenes, saturated components, aromatic components, and gums from crude oil using heptane, toluene, and ethanol. However, it does not cover methods for separating and quantifying different oil-containing emulsions. Therefore, it is necessary to research and develop quantitative analysis methods for petroleum emulsion systems based on separation processes, providing a theoretical basis for the design and optimization of oil-containing emulsion waste treatment processes in the petroleum and petrochemical industry. Summary of the Invention

[0004] The inventors discovered that in existing technologies, after oily substances combine with particulate matter, the demulsification process for petroleum-based emulsion wastewater requires targeted additions or subtractions of equipment or processes. However, the content of each oily medium combined with particulate matter cannot be determined, resulting in poor processing precision for petroleum-based emulsion wastewater. The inventors have attempted quantitative analysis of petroleum-based emulsion wastewater using resin-based filtration media. However, due to the adsorption effect of resin-based filtration media on petroleum, the recovery rate error is within ±30%, making precise quantitative analysis impossible. In view of the above problems, this invention is proposed to provide a method for quantitative analysis, a treatment method, a filtration device preparation method, and a filtration device for petroleum-based emulsion wastewater that overcomes or at least partially solves the above problems.

[0005] In a first aspect, embodiments of the present invention provide a method for the quantitative analysis of petroleum-based emulsified wastewater, the method comprising:

[0006] The petroleum-based emulsified waste liquid was filtered using a filtration device at a filtration rate of 0.5 to 1.5 mL / s, and the filtrate of the petroleum-based emulsified waste liquid before passing through each filtration layer of the filtration device was obtained.

[0007] The filtration device is backwashed at a filtration rate of 0.2 to 1.0 mL / s to obtain the filtrate from each filter layer;

[0008] The content of oily substances in the filtrate before each filtration layer is determined, and the content of oily substances combined with particulate matter in the petroleum emulsified waste liquid is determined based on the content of oily substances and the weight of the filtered material.

[0009] The filtration device is prepared by soaking quartz sand of different particle sizes in hydrochloric acid solution for 6-24 hours, washing it with deionized water until the turbidity of the wash water does not exceed 1 NTU and the pH of the wash water is 6.5-7.0, so as to obtain a filtration separation medium; and is based on the filtration separation medium.

[0010] Optionally, the quartz sand is soaked in hydrochloric acid solution for 6–14 hours; the petroleum emulsion waste liquid is filtered using the aforementioned filtration device at a filtration rate of 0.5–1.0 mL / s; and the filtration device is backwashed at a filtration rate of 0.2–0.6 mL / s.

[0011] Optionally, the preparation of a filtration device based on the filtration separation medium includes:

[0012] After the filter separation medium is loaded into three sets of filter columns, the filter columns are connected in descending order of the particle size of the filter separation medium they contain. Then, a filter membrane is connected after the filter column with the smallest particle size of the filter separation medium to form a filter device.

[0013] Optionally, the bottom layer of the filter column is provided with a pad layer, which is glass beads and / or quartz sand with a particle size greater than 80 mesh.

[0014] Optionally, the filter column can be made of glass, stainless steel, carbon steel or polytetrafluoroethylene.

[0015] Optionally, the filtration device may further include a suction pump; the suction pump is located between the filter columns and is used to control the filtration rate of the filtration device.

[0016] Optionally, the pore size of the filter membrane is 0.45 μm.

[0017] Optionally, after obtaining the filter material of each filter layer, the method further includes: evaporating and concentrating the filter material and drying it to a constant weight to determine the total weight of the oily substances and the particulate matter bound to each filter layer.

[0018] Optionally, the quartz sand may be washed with deionized water until the residual particulate matter concentration in the wash water is 0.3–0.6 mg / L.

[0019] Optionally, the quartz sand may be washed with deionized water until the concentration of residual particulate matter in the wash water is 0.3–0.4 mg / L.

[0020] Optionally, the quartz sand with different particle sizes is quartz sand with three different particle sizes: 40-80 mesh, 20-40 mesh, and less than 20 mesh.

[0021] Secondly, embodiments of the present invention provide a method for treating petroleum-based emulsified wastewater, which may include:

[0022] Based on the process of increasing or decreasing the content of various oil substances and their combined particulate matter in oil emulsion waste liquid, the aggregates formed by the oil substances and their combined particulate matter are demulsified.

[0023] The content of each of the oily substances and the particulate matter bound to them is determined according to the quantitative analysis method for oily emulsion waste liquid described in the first aspect.

[0024] Thirdly, embodiments of the present invention provide a method for preparing a filtration device, which may include:

[0025] Quartz sand of different particle sizes is soaked in hydrochloric acid solution for 6–24 hours and then washed with deionized water until the turbidity of the wash water does not exceed 1 NTU and the pH of the wash water is 6.5–7.0 to obtain the filtration separation medium.

[0026] The filtration device is prepared based on the filtration separation medium.

[0027] Optionally, the quartz sand can be soaked in hydrochloric acid solution for 6–14 hours.

[0028] Optionally, the preparation of a filtration device based on the filtration separation medium includes:

[0029] After the filter separation medium is loaded into three sets of filter columns, the filter columns are connected in descending order of the particle size of the filter separation medium they contain. Then, a filter membrane is connected after the filter column with the smallest particle size of the filter separation medium to form a filter device.

[0030] Optionally, the bottom layer of the filter column is provided with a pad layer, which is glass beads and / or quartz sand with a particle size greater than 80 mesh.

[0031] Fourthly, embodiments of the present invention provide a filtration device, which is prepared according to the filtration device preparation method described in the third aspect.

[0032] The beneficial effects of the above-described technical solutions provided in the embodiments of the present invention include at least the following:

[0033] This invention provides a method for quantitative analysis of petroleum-based emulsified wastewater, a treatment method, a method for preparing a filtration device, and a filtration device. The quantitative analysis method includes: filtering the petroleum-based emulsified wastewater using a filtration device at a filtration rate of 0.5–1.5 mL / s, and obtaining filtrate before each filtration layer of the filtration device; determining the oil content in different filtrates; backwashing the filtration device at a filtration rate of 0.2–1.0 mL / s to obtain the filtrate from each filtration layer; further determining the content of oil and particulate aggregates in each filtration layer; and determining the content of oil and particulate aggregates in the petroleum-based emulsified wastewater based on the oil content and the weight of the filtrate. To determine the content of particles combined with different oily substances, in this embodiment of the invention, quartz sand of different particle sizes is soaked in hydrochloric acid solution for 6-24 hours, and then washed with deionized water until the turbidity of the wash water does not exceed 1 NTU and the pH of the wash water is 6.5-7.0, so as to obtain a filtration separation medium; and a filtration device is prepared based on the filtration separation medium; the filtration device can achieve the purpose of filtering and repelling oil, avoiding the adsorption of oily substances.

[0034] Based on the separation characteristics of oily substances and particulate matter, this invention separates them from oily emulsified wastewater, demonstrating the role and quantification of emulsification caused by particulate matter. The method provided in this embodiment fills a technical gap in the field and provides a theoretical basis for the design and optimization of oily emulsified waste treatment processes in the petroleum and petrochemical industry.

[0035] Other features and advantages of the invention will be set forth in the following description, and will be apparent in part from the description, or may be learned by practicing the invention. The objects and other advantages of the invention may be realized and obtained by means of the structures particularly pointed out in the written description and the accompanying drawings.

[0036] The technical solution of the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. Attached Figure Description

[0037] The accompanying drawings are provided to further illustrate the invention and form part of the specification. They are used in conjunction with embodiments of the invention to explain the invention and do not constitute a limitation thereof. In the drawings:

[0038] Figure 1 This is a schematic diagram of petroleum-based emulsified waste liquid separation provided in an embodiment of the present invention. Detailed Implementation

[0039] Exemplary embodiments of the present disclosure will now be described in more detail with reference to the accompanying drawings. While exemplary embodiments of the present disclosure are shown in the drawings, it should be understood that the present disclosure may be implemented in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.

[0040] Example 1

[0041] (1) Select three types of quartz sand with different particle sizes: <20 mesh, 20-40 mesh, and 40-80 mesh;

[0042] (2) Soak the quartz sand in hydrochloric acid solution for 6 hours, and rinse it with deionized water until the turbidity is 0.5 NTU and the pH is 7.0. The residual particulate matter concentration is 0.5 mg / L, which does not affect the separation effect on actual wastewater.

[0043] (3) Select glass filter columns and fill the filter columns with quartz sand of three different particle sizes, from large to small. Connect the three filter columns in series using a pump and pipeline.

[0044] (4) Petroleum emulsified waste liquid is sequentially passed through 3 sets of filter columns connected in series at a filtration rate of 0.5 mL / s. The filtrate of each set of filter columns is collected and retained according to a preset volume. The effluent from the third set of filter columns is filtered through a 0.45 μm membrane and the filtrate is collected.

[0045] (5) Deionized water was passed through the filter column from bottom to top using pumps and pipelines respectively. The pollutants trapped on the filter column were backwashed out at a flow rate of 0.2 mL / s. The oily pollutants trapped by the first filter column were suspended oil-particulate matter, the oily pollutants trapped by the second filter column were dispersed oil-particulate matter, and the oily pollutants trapped by the third filter column were emulsified oil-particulate matter. After filtration through a 0.45 μm membrane, the pollutants trapped on the membrane were colloidal emulsions.

[0046] (6) For petroleum emulsified waste liquid, filtrate from the first group of filter columns, filtrate from the second group of filter columns, filtrate from the third group of filter columns, and filtrate from the 0.45 μm membrane, the petroleum components were determined to be C0, C1, C2, C3, and C4 according to the HJ 637 method; the pollutants retained by the first, second, and third group of filter columns were evaporated, concentrated, and dried to constant weight, and the pollutants retained by the 0.45 μm filter membrane were dried to constant weight and weighed as M1, M2, M3, and M4, respectively.

[0047] (7) Based on C0, C1, C2, C3, C4, and M1, M2, M3, M4, calculate the oil content and particulate matter content in suspended oil-particulate matter, dispersed oil-particulate matter, emulsified oil-particulate matter, colloidal emulsions and soluble oils.

[0048] (8) Following the above steps, a typical oily waste liquid (petroleum emulsion waste liquid) was separated. The typical waste liquid had a pH of 7.18, a COD (chemical oxygen demand) of about 2818 mg / L, a total oil content of 617.2 mg / L, and an SS content of 450.2 mg / L.

[0049] The quartz sand in this embodiment of the invention contains impurities. Acid washing further improves its oleophobicity, preventing oil adsorption and focusing solely on retention. It should be noted that the filtration device in this embodiment can be prepared for each analysis of the petroleum-based emulsion waste liquid, or it can be prepared in advance for later use.

[0050] In this embodiment of the invention, the specific method for calculating the oil content and particulate matter content in suspended oil-particulate matter, dispersed oil-particulate matter, emulsified oil-particulate matter, colloidal emulsions, and soluble oils based on C0, C1, C2, C3, C4, and M1, M2, M3, M4 is as follows:

[0051] (1) Suspended oil-particulate matter

[0052] O1 = C0 - C1

[0053] In the formula

[0054] O1—Suspended oil content (mg / L);

[0055] CO—Petroleum hydrocarbons in raw water (mg / L);

[0056] C1—Petroleum content (mg / L) in the effluent from the first group of filter columns.

[0057]

[0058] In the formula

[0059] SS1—Content of suspended oil particles (mg / L);

[0060] O1—Suspended oil content (mg / L);

[0061] M1—Retention material of the first group of filter columns (mg);

[0062] V — Water sample volume (L).

[0063] (2) Dispersed oil-particulate matter

[0064] O2 = C1 - C2

[0065] In the formula

[0066] O2—Dispersed oil content (mg / L);

[0067] C1—Petroleum content (mg / L) in the effluent from the first group of filter columns;

[0068] C2—Petroleum content (mg / L) in the effluent from the second group of filter columns.

[0069]

[0070] In the formula

[0071] SS2—Dispersed oil encapsulated particle content (mg / L);

[0072] O2—Dispersed oil content (mg / L);

[0073] M2—Retention material (mg) from the second group of filter columns;

[0074] V—Water sample volume (L, it should be noted that the water sample volume here should be reduced by the preset volume retained by each filter column).

[0075] (3) Emulsified oil-particulate matter

[0076] O3 = C2 - C3

[0077] In the formula

[0078] O3—Emulsified oil content (mg / L);

[0079] C2—Petroleum content (mg / L) in the effluent from the second group of filter columns;

[0080] C3—Petroleum content (mg / L) in the effluent from the third group of filter columns.

[0081]

[0082] In the formula

[0083] SS3—Content of particles encapsulated in emulsified oil (mg / L);

[0084] O3—Emulsified oil content (mg / L);

[0085] M3—Retention material (mg) from the third group of filter columns;

[0086] V—Water sample volume (L, it should be noted that the water sample volume here should be reduced by the preset volume retained by each filter column).

[0087] (4) Colloidal emulsions

[0088] O4 = C3 - C4

[0089] In the formula

[0090] O4—Colloidal emulsion content (mg / L);

[0091] C3—Petroleum content (mg / L) in the effluent from the third group of filter columns;

[0092] C4-0.45µm membrane filtration of petroleum hydrocarbons (mg / L) in effluent.

[0093]

[0094] In the formula

[0095] SS4—Content of colloidal emulsions containing particles (mg / L);

[0096] O4—Colloidal emulsion content (mg / L);

[0097] M4—0.45µm filter membrane retention (mg);

[0098] V—Water sample volume (L, it should be noted that the water sample volume here should be reduced by the preset volume retained by each filter column).

[0099] (5) Soluble oils

[0100] C4-0.45µm filter membrane filters out petroleum hydrocarbons (mg / L) in the effluent.

[0101] After separation, the oil and particulate matter contents in suspended oil-particulate matter, dispersed oil-particulate matter, emulsified oil-particulate matter, colloidal emulsions, and soluble oil are shown in Table 1 below. The petroleum recovery rate was 98%, and the suspended solids (SS) recovery rate was 96%.

[0102] Table 1. Concentration analysis of various pollutants after separation in Example 1.

[0103]

[0104] Example 2

[0105] (1) Select three types of quartz sand with different particle sizes: <20 mesh, 20-40 mesh, and 40-80 mesh;

[0106] (2) Soak the quartz sand in hydrochloric acid solution for 7 hours, and rinse it with deionized water until the turbidity is 1 NTU and the pH is 7.0. The residual particulate matter concentration is 0.6 mg / L, which does not affect the separation effect on actual wastewater.

[0107] (3) Select glass filter columns and fill the filter columns with quartz sand of three different particle sizes, from large to small. Connect the three filter columns in series using pumps and pipelines.

[0108] (4) The oily wastewater is sequentially filtered through three sets of filter columns connected in series at a filtration rate of 0.6 mL / s. A certain amount of filtrate from each set of filter columns is collected and retained. The effluent from the third set of filter columns is filtered through a 0.45 μm membrane and the filtrate is collected.

[0109] (5) Deionized water was passed through the filter columns from bottom to top using pumps and pipelines respectively. The pollutants trapped on the filter columns were backwashed out at a flow rate of 0.3 mL / s. The oily pollutants trapped by the first group of filter columns were suspended oil-particulate matter, the oily pollutants trapped by the second group of filter columns were dispersed oil-particulate matter, and the oily pollutants trapped by the third group of filter columns were emulsified oil-particulate matter. After filtration through a 0.45 μm membrane, the pollutants trapped on the membrane were colloidal emulsions.

[0110] (6) For petroleum emulsified waste liquid, filtrate from the first group of filter columns, filtrate from the second group of filter columns, filtrate from the third group of filter columns, and filtrate from the 0.45 μm membrane, the petroleum components were determined to be C0, C1, C2, C3, and C4 according to the HJ 637 method; the pollutants retained by the first, second, and third group of filter columns were evaporated, concentrated, and dried to constant weight, and the pollutants retained by the 0.45 μm filter membrane were dried to constant weight and weighed as M1, M2, M3, and M4, respectively.

[0111] (7) Calculate the oil content and particulate matter content in suspended oil-particulate matter, dispersed oil-particulate matter, emulsified oil-particulate matter, colloidal emulsions and soluble oils based on C0, C1, C2, C3, C4 and M1, M2, M3, M4.

[0112] (8) Following the steps above, a typical oily waste liquid was separated. This typical waste liquid had a pH of 7.18, a COD of approximately 2818 mg / L, a total oil content of 617.2 mg / L, and a suspended solids (SS) content of 450.2 mg / L. The oil and particulate matter contents in the suspended oil-particulate matter, dispersed oil-particulate matter, emulsified oil-particulate matter, colloidal emulsions, and soluble oil after separation are shown in the table below. The petroleum recovery rate was 98%, and the SS recovery rate was 94%.

[0113] Table 2. Concentration analysis of various pollutants after separation in Example 1.

[0114]

[0115] The steps 1, 3, 6 and 7 of Examples 3 to 10 and Comparative Examples are the same as those of Examples 1 and 2. The specific filter column preparation conditions are shown in Table 1, and the separation conditions of oily waste liquid (petroleum emulsion waste liquid) are shown in Tables 3 and 4.

[0116] Table 3 shows the filtration and separation media conditions in Examples 3-10 and Comparative Examples 1-3.

[0117]

[0118] Table 4 shows the separation conditions and test results for Examples 3-10 and Comparative Examples 1-3.

[0119]

[0120]

[0121]

[0122] The quantitative analysis method for petroleum-based emulsified waste liquid described in this invention solves the problem that existing analytical methods fail to achieve quantitative analysis of suspended oil, dispersed oil, emulsified oil, and dissolved oil in complex emulsion systems. Since existing analytical methods do not consider the influence of particulate matter combined with oily substances, this invention has the following beneficial technical effects compared to the prior art:

[0123] Based on the separation characteristics of oily substances and particulate matter, this invention separates them from oily emulsified wastewater, demonstrating the role and quantification of emulsification caused by particulate matter. The method provided in this embodiment fills a technical gap in the field and provides a theoretical basis for the design and optimization of oily emulsified waste treatment processes in the petroleum and petrochemical industry.

[0124] Based on the same inventive concept, this embodiment of the invention also provides a method for treating petroleum-based emulsified wastewater. This method is based on the equipment that increases or decreases the content of the combination of oil substances and particulate matter in the oil-based emulsified wastewater, so as to achieve demulsification of the combination of oil substances and particulate matter.

[0125] The content of each of the oily substances and particulate matter combinations was determined by the quantitative analysis method for the oily emulsified waste liquid described above.

[0126] Obviously, those skilled in the art can make various modifications and variations to this invention without departing from its spirit and scope. Therefore, if these modifications and variations fall within the scope of the claims of this invention and their equivalents, this invention also intends to include these modifications and variations.

Claims

1. A quantitative analysis method for petroleum-based emulsified wastewater, characterized in that, include: The petroleum-based emulsion waste liquid was filtered using a filtration device at a filtration rate of 0.5 to 1.5 mL / s, and the filtrate before each filtration layer of the filtration device was obtained. The filtration device is backwashed at a filtration rate of 0.2~1.0 mL / s to obtain the filter material of each filter layer; The content of oily substances in the filtrate before each filtration layer is determined, and the content of oily substances combined with particulate matter in the petroleum emulsified waste liquid is determined based on the content of oily substances and the weight of the filtered material. The filtration device comprises soaking quartz sand of different particle sizes in hydrochloric acid solution for 6-24 hours, followed by washing with deionized water until the turbidity of the wash water does not exceed 1 NTU and the pH of the wash water is 6.5-7.0, to obtain the filtration separation medium. The filtration separation medium is loaded into three sets of filter columns, which are then connected in descending order of the particle size of the filtration separation medium they contain. A filter membrane is then connected after the filter column with the smallest particle size of the filtration separation medium to form the filtration device. The bottom layer of each filter column is provided with a pad, which is composed of glass beads and / or quartz sand with a particle size greater than 80 mesh. Specifically, the oil content in the petroleum-based emulsified waste liquid, the filtrate from the first filter column, the second filter column, the third filter column, and the filtrate from the filter membrane was determined to be C0, C1, C2, C3, and C4, respectively. The filtrates retained by the first filter column, the second filter column, the third filter column, and the filter membrane were evaporated, concentrated, dried to constant weight, and weighed as M1, M2, M3, and M4. Based on C0, C1, C2, C3, C4, and M1, M2, M3, and M4, the oil content and particulate matter content in the suspended oil-particulate matter, dispersed oil-particulate matter, emulsified oil-particulate matter, colloidal emulsions, and soluble oil in the petroleum-based emulsified waste liquid were determined.

2. The method according to claim 1, characterized in that, Quartz sand is soaked in hydrochloric acid solution for 6-14 hours; the petroleum emulsion waste liquid is filtered using the filter device at a filtration rate of 0.5-1.0 mL / s; the filter device is backwashed at a filtration rate of 0.2-0.6 mL / s.

3. The method according to claim 1, characterized in that, The filter column is made of glass, stainless steel, carbon steel, or polytetrafluoroethylene.

4. The method according to claim 1, characterized in that, The filtration device further includes a suction pump; the suction pump is located between the filter columns and is used to control the filtration rate of the filtration device.

5. The method according to claim 1, characterized in that, The pore size of the filter membrane is 0.45 μm.

6. The method according to claim 1, characterized in that, After obtaining the filter material for each filter layer, the method further includes: evaporating, concentrating, and drying the filter material to a constant weight to determine the total weight of the oily substances and their bound particulate matter in each filter layer.

7. The method according to claim 1, characterized in that, The quartz sand is washed with deionized water until the concentration of residual particulate matter in the wash water is 0.3~0.6 mg / L.

8. The method according to claim 1, characterized in that, The quartz sand is washed with deionized water until the concentration of residual particulate matter in the wash water is 0.3~0.4 mg / L.

9. The method according to any one of claims 1 to 8, characterized in that, The quartz sand with different particle sizes refers to quartz sand with particle sizes of 40-80 mesh, 20-40 mesh, and less than 20 mesh.

10. A method for treating petroleum-based emulsified wastewater, characterized in that, include: The content of oil substances and the content of oil-based particles combined with oil substances in the petroleum-based emulsified wastewater are determined by the quantitative analysis method of any one of claims 1 to 9. Based on the content of oil and particulate matter, demulsification treatment is performed on the aggregates formed by the oil and the bound particulate matter.

11. A method for preparing a filtration device, characterized in that, The filtration device prepared by this method is applied to the quantitative analysis method of petroleum emulsified waste liquid as described in any one of claims 1 to 9, comprising: Quartz sand of different particle sizes is soaked in hydrochloric acid solution for 6-24 hours and then washed with deionized water until the turbidity of the wash water does not exceed 1 NTU and the pH of the wash water is 6.5-7.0 to obtain the filtration separation medium. After loading the filter separation medium into three sets of filter columns, the filter columns are connected in descending order of the particle size of the filter separation medium they contain. A filter membrane is then connected after the filter column with the smallest particle size of the filter separation medium to form a filter device. The filter column has a bottom layer consisting of glass beads and / or quartz sand with a particle size greater than 80 mesh.

12. The method according to claim 11, characterized in that, Quartz sand is soaked in hydrochloric acid solution for 6-14 hours.

13. A filtration device, characterized in that, The filtration device is prepared by the method for preparing a filtration device according to any one of claims 11 to 12.

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