CN111608606A - Oil removing method for shale gas-oil-based drilling cuttings - Google Patents
Oil removing method for shale gas-oil-based drilling cuttings Download PDFInfo
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- 239000002518 antifoaming agent Substances 0.000 claims description 16
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- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 15
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 15
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 15
- 239000000203 mixture Substances 0.000 claims description 13
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- 239000003093 cationic surfactant Substances 0.000 claims description 12
- 150000007529 inorganic bases Chemical class 0.000 claims description 12
- 239000002736 nonionic surfactant Substances 0.000 claims description 12
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical group CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 9
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- 239000002994 raw material Substances 0.000 claims description 6
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical compound CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims description 4
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- VBIIFPGSPJYLRR-UHFFFAOYSA-M Stearyltrimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCCCCCCCCCC[N+](C)(C)C VBIIFPGSPJYLRR-UHFFFAOYSA-M 0.000 description 5
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Images
Classifications
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B21/00—Methods or apparatus for flushing boreholes, e.g. by use of exhaust air from motor
- E21B21/06—Arrangements for treating drilling fluids outside the borehole
- E21B21/068—Arrangements for treating drilling fluids outside the borehole using chemical treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09B—DISPOSAL OF SOLID WASTE NOT OTHERWISE PROVIDED FOR
- B09B3/00—Destroying solid waste or transforming solid waste into something useful or harmless
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B21/00—Methods or apparatus for flushing boreholes, e.g. by use of exhaust air from motor
- E21B21/06—Arrangements for treating drilling fluids outside the borehole
-
- E—FIXED CONSTRUCTIONS
- E21—EARTH OR ROCK DRILLING; MINING
- E21B—EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- E21B21/00—Methods or apparatus for flushing boreholes, e.g. by use of exhaust air from motor
- E21B21/06—Arrangements for treating drilling fluids outside the borehole
- E21B21/063—Arrangements for treating drilling fluids outside the borehole by separating components
- E21B21/065—Separating solids from drilling fluids
- E21B21/066—Separating solids from drilling fluids with further treatment of the solids, e.g. for disposal
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- Engineering & Computer Science (AREA)
- Geology (AREA)
- Mining & Mineral Resources (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Mechanical Engineering (AREA)
- Fluid Mechanics (AREA)
- Physics & Mathematics (AREA)
- Geochemistry & Mineralogy (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Processing Of Solid Wastes (AREA)
- Treatment Of Sludge (AREA)
Abstract
The invention relates to a method for removing oil from shale gas oil-based drilling cuttings, which comprises the steps of adding a dispersing agent into the oil-based drilling cuttings, stirring at room temperature, wherein the stirring speed is 150-450 rpm, the stirring time is 40-90min, and standing for layering; separating the oil-water phase from the solid phase; adding a sulfuric acid solution into the oil-water phase, adjusting the pH to 3-4, stirring, performing centrifugal separation at a centrifugal speed of 5000-12000 rpm for 8-20 min, and recovering the upper oil phase. The method has the advantages of simple process, simple equipment, mild treatment conditions, small dosage of medicament, low energy consumption, low cost and no potential safety hazard. The oil removal is thorough, the residual oil rate of the oil removal residues is lower than 0.5 percent, the oil removal residues reach the national specified standard, and the oil removal residues can be used for preparing baking-free bricks, sintered bricks, road materials and the like, so that the land occupation is reduced; the oil component has high recovery rate, and the oil-based drilling fluid is returned, so that the resource recycling is realized, and the environmental pollution is reduced.
Description
Technical Field
The invention belongs to the technical field of oil-based drilling cutting treatment in shale gas drilling, relates to the technical field of environmental protection, and particularly relates to an oil removing method for shale gas-based drilling cutting.
Background
The oil-based drilling cuttings are black sticky oil-based drilling cuttings which are harmful to the environment and are formed by adopting the oil-based drilling fluid in the drilling process of the oil-gas field, wherein the drilling fluid is taken out of an oil well while drilling and is uniformly mixed with the oil-based drilling fluid, and the drilling fluid is attached to the surface of rock debris. The oil-based drilling fluid is a complex multiphase system containing mineral oil, alkane, derivatives thereof and a plurality of heavy metals, if the oil-based drilling fluid is piled up for a long time, harmful substances in the oil-based drilling cuttings are gradually brought into soil or infiltrated into underground water along with infiltration of rainfall or snowfall, surrounding soil and water resources are polluted, growth and survival of animals and plants are inhibited, and even the health and the environment which is resistant to survival of human beings are threatened. Along with the increasing of the development of unconventional energy of the global shale gas, the quantity of drill cuttings generated by well drilling is increased day by day, and the volume of the drill cuttings generated in China every year is up to 230000m according to statistics3Left and right. By the beginning of the 80's of the 20 th century, global environmental awareness has increased, and the oil and gas industry and its regulators have begun to understand and rely on the potential impact of drill cuttings on the ecological environment and human health. Because the oil-based drill cuttings contain pollutants such as petroleum hydrocarbons, heavy metals and organic matters, the oil-based drill cuttings are listed in national hazardous wastes (national hazardous waste catalogue, HW08), and how to treat the waste oil-based drill cuttings and research and develop a harmless treatment method of the oil-based drill cuttings is the research objective of each professional.
Currently, the main methods of treating oil-based drill cuttings include: extraction, incineration, landfill, pyrolysis, solidification, reinjection, biological treatment and the like.
The extraction method is characterized in that petroleum substances are transferred into an organic solvent from the surface of drill cuttings by utilizing different solubilities of the petroleum substances in different solvents, the purpose of separating the petroleum hydrocarbons from the solvent is achieved by means of distillation according to different boiling points of the petroleum hydrocarbons and the organic solvent, the separated petroleum hydrocarbons can be recycled to reconfigure oil-based mud, and an extracting agent can also be used for secondary extraction; however, the extractant is expensive, has certain loss in the treatment process, has higher cost, and has the problems of potential safety hazard and secondary pollution.
The incineration method is a direct and simple solid waste treatment method which treats the oil-based drilling cuttings by utilizing the characteristics of higher organic components and certain calorific value of the oil-based drilling cuttings; however, oil-based drilling cuttings generally contain a large amount of water, dehydration pretreatment needs to be carried out firstly to enable the oil-based drilling cuttings to meet the combustion requirements, the investment and operation cost of incineration equipment are high, complex toxic gas is generated in the incineration process, and the standard treatment of generated fly ash, slag and smoke has certain difficulty.
The landfill method is a method for covering the oil-based drilling cuttings by using a soil layer by selecting a proper natural place or a proper place for manual reconstruction on land; however, the site construction and drill cuttings transportation cost is high, the occupied area is large, petroleum hydrocarbons and chemical agents in the drill cuttings cannot be decomposed in a short time, and the pollution to underground water is caused.
The pyrolysis method is that the oil-based drilling cuttings are heated to a certain temperature under the anaerobic condition to desorb hydrocarbons and organic matters, the hydrocarbons and the organic matters are separated from the drilling cuttings, the hydrocarbon components are recycled, the thermally decomposed hydrocarbons can be condensed into recycled oil for recycling, and non-condensable gas can be used as fuel gas; however, the process is generally carried out at high temperature, the requirements on energy consumption and reaction conditions are high, and the operation is complex.
The solidification method is a harmless treatment process for solidifying or containing the oil-based drilling cuttings in an inert solidification substrate by a physical and chemical method; however, the method has high requirements on the oil content, the salt content and the like of the oil-based drilling cuttings, and the curing strength can be greatly reduced due to the fact that the oil content and the salt content are too high.
The reinjection method is to process the oil-based drill cuttings through shearing, crushing and sorting processes and reinject the remainder into the formation. However, the method is greatly influenced by pipelines and equipment, the injection pipeline bears high pressure and corrosion for a long time and is easily damaged, and once the injection pipeline is damaged, pollution is caused; in addition, the method has a limited processing speed.
Biological treatment of oil-based drill cuttings with the aid of microorganismsThe petroleum hydrocarbon and organic matter in the oil are degraded and converted into harmless CO2、H2O and simultaneously increases the soil humus content. However, the method takes a long time, the conditions such as pH, humidity, temperature and the like need to be strictly controlled during treatment, and the method also has higher technical requirements on operators.
Disclosure of Invention
In view of the above, the present invention aims to provide an efficient oil removing method for shale gas-oil-based drill cuttings under convenient use conditions.
In order to achieve the purpose, the invention provides the following technical scheme:
1. the oil removing method of the shale gas-oil-based drilling cuttings comprises the following specific steps:
1) adding the oil-based drilling cuttings into a dispersing agent in a container 1, stirring at room temperature, wherein the stirring speed is 150-450 rpm, the stirring time is 40-90min, and standing for layering; pouring the oil-water phase into the container 2; the dispersing agent comprises, by mass, 10-40 parts of inorganic base, 0.01-2 parts of organic base, 0.01-2 parts of surfactant, 0.01-0.5 part of defoaming agent and 5-30 parts of sodium hexametaphosphate;
2) adding a sulfuric acid solution into the container 2, adjusting the pH to 3-4, stirring, performing centrifugal separation at a centrifugal speed of 5000-12000 rpm for 8-20 min, and recovering an upper oil phase.
Further, the method is characterized in that the volume ratio of the oil-based drilling cuttings to the dispersing agent in the step 1) is 1:1-3, and the mass fraction of the dispersing agent is 5-35%.
Further, the volume ratio of the oil-based drilling cuttings to the dispersing agent in the step 1) is 1:2, and the mass fraction of the dispersing agent is 10-20%.
Further, step 1) of the oil removal method further comprises: and (3) putting the rest solid phase into hot water of 50-90 ℃, continuously stirring for 40-90min, pouring the oil-water phase into the container 2 again, filtering and drying the rest solid phase.
Further, the volume ratio of the hot water consumption to the solid phase is 1.5-3.0: 1.
further, the raw materials of the dispersing agent comprise the following components in parts by weight: 15-35 parts of inorganic base, 0.05-2 parts of organic base, 0.5-2 parts of surfactant, 0.1-0.5 part of defoaming agent and 10-25 parts of sodium hexametaphosphate.
Further, the raw materials of the dispersing agent comprise the following components in parts by weight: 30 parts of inorganic base, 2 parts of organic base, 2 parts of surfactant, 0.4 part of defoaming agent and 25 parts of sodium hexametaphosphate.
Further, the inorganic base is any one of sodium carbonate and sodium hydroxide; the organic base is any one of triethylamine, triethylene diamine and tetramethyl ethylene diamine; the surfactant is a mixture of cationic surfactant and nonionic surfactant; the defoaming agent is tributyl phosphate.
Furthermore, the mass ratio of the cationic surfactant to the nonionic surfactant in the surfactant is 1: 1-3.
Further, the mass ratio of the cationic surfactant to the nonionic surfactant in the surfactant is 1: 1.
The invention has the beneficial effects that: the oil removal method for the shale gas-oil-based drilling cuttings is provided, oil can be effectively separated from a rock debris solid phase through the research on the composition and the proportion of a dispersing agent suitable for the oil-based drilling cuttings, and the method has universality and is not influenced by the composition and the property of the oil-based drilling cuttings; the method has the advantages of simple process, simple equipment, mild treatment conditions, small medicament dosage, low energy consumption, low cost and no potential safety hazard; the oil removal is thorough, the residual oil rate of the oil removal residues is lower than 0.5 percent, the oil removal residues reach the national specified standard, and the oil removal residues can be used for preparing baking-free bricks, sintered bricks, road materials and the like, so that the land occupation is reduced; the oil component has high recovery rate, and the oil-based drilling fluid is returned, so that the resource recycling is realized, and the environmental pollution is reduced.
Drawings
In order to make the object, technical scheme and beneficial effect of the invention more clear, the invention provides the following drawings for explanation:
FIG. 1 is a flow chart of the oil removal method for shale gas-oil based drill cuttings of the present invention;
figure 2 shows the effect of the final oil and water phases obtained by three different treatments of the comparative example and the example.
Detailed Description
Preferred embodiments of the present invention will be described in detail below with reference to the accompanying drawings. The experimental procedures, in which specific conditions are not specified in the examples, are generally carried out under conventional conditions or under conditions recommended by the manufacturers.
Dispersing agent for removing oil of shale gas-oil-based drilling cuttings
The raw materials are as follows by mass: 10-40 parts of inorganic base, 0.01-2 parts of organic base, 0.01-2 parts of surfactant, 0.01-0.5 part of defoaming agent and 5-30 parts of sodium hexametaphosphate.
The preferable raw materials are as follows by weight: 15-35 parts of inorganic base, 0.05-2 parts of organic base, 0.5-2 parts of surfactant, 0.1-0.5 part of defoaming agent and 10-25 parts of sodium hexametaphosphate.
Wherein the inorganic base is any one of sodium carbonate and sodium hydroxide; the organic base is any one of triethylamine, triethylene diamine and tetramethyl ethylene diamine; the surfactant is a mixture of cationic (octadecyl trimethyl ammonium chloride and hexadecyl trimethyl ammonium bromide) and nonionic (Tween, span and monolauryl phosphate) in a mass ratio of 1:1-3, preferably 1: 1; the defoaming agent is tributyl phosphate. When in use, the weight percentage of the compound is 1 to 35 percent, preferably 10 to 20 percent.
Inorganic base and surfactant are added into the dispersant for synergistic effect, so that the oil-water interfacial tension is reduced, and the oil removal effect is enhanced; the cationic surfactant and the nonionic surfactant have synergistic effect to strengthen the demulsification function and the solubilization function; the organic base is not easy to emulsify again, and the sodium hexametaphosphate is dispersed and wetted; a large amount of foam can be generated in the dispersing process, the dispersing effect is influenced, and tributyl phosphate is used for reducing the surface tension to break the foam.
A method for removing oil from shale gas-oil-based drill cuttings, and fig. 1 is a flow chart of the method for removing oil from shale gas-oil-based drill cuttings, which comprises the following specific steps:
1) adding the oil-based drilling cuttings into the dispersing agent according to the volume ratio of 1:1-3 in a container 1, stirring at room temperature, wherein the stirring speed is 150-450 rpm, the stirring time is 40-90min, and standing for layering; pouring the oil-water phase into a container 2, placing the rest solid phase into hot water at 50-90 ℃, wherein the volume ratio of the hot water usage to the solid phase is 1.5-3.0: 1, continuously stirring for 40-90min, pouring the oil-water phase into the container 2 again, and filtering and drying the rest solid phase.
The volume ratio of the oil-based drill cuttings to the dispersing agent is preferably 1:2, and the mass fraction of the dispersing agent is 10-20%.
2) Adding a sulfuric acid solution with the mass fraction of 0.1-10% into the container 2, adjusting the pH to 3-4, and stirring for 5-30 min; and after stirring, carrying out centrifugal separation at the centrifugal rotation speed of 5000-12000 rpm for 8-20 min, and recovering the upper oil phase.
The oil removing method 1 of the oil-based drill cuttings has universality and is not influenced by the composition and the properties of the oil-based drill cuttings, such as two typical oil-based drill cuttings: both horizontal wells (white oil as drilling fluid base) and vertical wells (diesel oil as drilling fluid base) can be used.
2. Simple process and equipment, mild treatment condition, small dosage of medicament, low energy consumption, low cost and no potential safety hazard.
3. The oil removal is thorough, the residual oil rate of the oil removal residues is lower than 0.5 percent, the oil removal residues reach the national specified standard, and the oil removal residues can be used for preparing baking-free bricks, sintered bricks, road materials and the like, so that the land occupation is reduced.
4. The oil component has high recovery rate, and the oil-based drilling fluid is returned, so that the resource recycling is realized, and the environmental pollution is reduced.
Example 1
A dispersing agent for removing oil from shale gas-oil-based drilling cuttings and an oil removing method thereof are disclosed, which specifically comprise the following steps:
a. oil removal dispersing agent for shale gas oil-based drilling cuttings: 20 parts of inorganic base sodium hydroxide, 1 part of organic base triethylene diamine, 2 parts of surfactant, 0.3 part of defoaming agent tributyl phosphate and 10 parts of sodium hexametaphosphate; the surfactant is a mixture of a cationic surfactant and a nonionic surfactant, and comprises 1 part of octadecyl trimethyl ammonium chloride and 1 part of tween; adding water to prepare a dispersing agent into a solvent with the mass fraction of 10%;
b. weighing 400g of oil-based drilling cuttings in a beaker 1, adding 600g of oil-removing dispersing agent, stirring at room temperature, wherein the stirring speed is 150-450 rpm, the stirring time is 50min, and standing for layering; pouring the oil-water phase into a beaker 2, putting the rest solid phase into hot water at 50-90 ℃, wherein the volume ratio of the hot water to the solid phase is 1.5: 1, continuously stirring for 40-90min, pouring the oil-water phase into the beaker 2 again, and filtering, drying and detecting the rest solid phase;
c. adding a sulfuric acid solution with the mass fraction of 5% into the beaker 2, adjusting the pH to 3-4, and stirring for 5-30 min; and after stirring, carrying out centrifugal separation at the centrifugal rotation speed of 5000-12000 rpm for 8-20 min, and recovering the upper oil phase.
Example 2
A dispersing agent for removing oil from shale gas-oil-based drilling cuttings and an oil removing method thereof are disclosed, which specifically comprise the following steps:
a. oil removal dispersing agent for shale gas oil-based drilling cuttings: 40 parts of inorganic base sodium carbonate, 0.5 part of organic base triethylamine, 2 parts of surfactant, 0.5 part of defoamer tributyl phosphate and 20 parts of sodium hexametaphosphate; the surfactant is a mixture of a cationic surfactant and a nonionic surfactant, and 1 part of octadecyl trimethyl ammonium chloride and 1 part of span are used as the surfactant; adding water to prepare a dispersant into a solvent with the mass fraction of 5%;
b. weighing 500g of oil-based drilling cuttings in a beaker 1, adding 1000g of deoiling dispersant, stirring at room temperature, wherein the stirring speed is 150-450 rpm, the stirring time is 50min, and standing for layering; pouring the oil-water phase into a beaker 2, putting the rest solid phase into hot water at 50-90 ℃, wherein the volume ratio of the hot water to the solid phase is 2: 1, continuously stirring for 40-90min, pouring the oil-water phase into the beaker 2 again, and filtering, drying and detecting the rest solid phase.
c. Adding a sulfuric acid solution with the mass fraction of 10% into the beaker 2, adjusting the pH to 3-4, and stirring for 5-30 min; and after stirring, carrying out centrifugal separation at the centrifugal rotation speed of 5000-12000 rpm for 8-20 min, and recovering the upper oil phase.
Example 3
A dispersing agent for removing oil from shale gas-oil-based drilling cuttings and an oil removing method thereof are disclosed, which specifically comprise the following steps:
a. oil removal dispersing agent for shale gas oil-based drilling cuttings: 30 parts of inorganic base sodium hydroxide, 1.5 parts of organic base triethylene diamine, 1.5 parts of surfactant, 0.3 part of defoaming agent tributyl phosphate and 20 parts of sodium hexametaphosphate; the surfactant is a mixture of a cationic surfactant and a nonionic surfactant, 0.75 part of cetyl trimethyl ammonium bromide and 0.75 part of span; adding water to prepare a dispersing agent into a solvent with the mass fraction of 15%;
b. weighing 400g of oil-based drilling cuttings in a beaker 1, adding 600g of oil-removing dispersant, stirring at the temperature of 50 ℃, wherein the stirring speed is 150-450 rpm, the stirring time is 50min, and standing for layering; pouring the oil-water phase into a beaker 2, putting the rest solid phase into hot water at 50-90 ℃, wherein the volume ratio of the hot water to the solid phase is 2: 1, continuously stirring for 40-90min, pouring the oil-water phase into the beaker 2 again, and filtering, drying and detecting the rest solid phase.
c. Adding a sulfuric acid solution with the mass fraction of 5% into the beaker 2, adjusting the pH to 3-4, and stirring for 5-30 min; and after stirring, carrying out centrifugal separation at the centrifugal rotation speed of 5000-12000 rpm for 8-20 min, and recovering the upper oil phase.
Example 4
A dispersing agent for removing oil from shale gas-oil-based drilling cuttings and an oil removing method thereof are disclosed, which specifically comprise the following steps:
a. oil removal dispersing agent for shale gas oil-based drilling cuttings: 25 parts of inorganic alkali sodium hydroxide, 1.5 parts of organic alkali tetramethyl ethylenediamine, 1 part of surfactant, 0.3 part of defoaming agent tributyl phosphate and 25 parts of sodium hexametaphosphate; the surfactant is a mixture of a cationic surfactant and a nonionic surfactant, 0.4 part of octadecyl trimethyl ammonium chloride and 0.6 part of tween; adding water to prepare a dispersing agent into a solvent with the mass fraction of 10%;
b. weighing 500g of oil-based drilling cuttings in a beaker 1, adding 1000g of deoiling dispersant, stirring at the temperature of 50 ℃, wherein the stirring speed is 150-450 rpm, the stirring time is 50min, and standing for layering; pouring the oil-water phase into a beaker 2, putting the rest solid phase into hot water at 50-90 ℃, wherein the volume ratio of the hot water to the solid phase is 3: 1, continuously stirring for 40-90min, pouring the oil-water phase into the beaker 2 again, and filtering, drying and detecting the rest solid phase.
c. Adding a sulfuric acid solution with the mass fraction of 3% into the beaker 2, adjusting the pH to 3-4, and stirring for 5-30 min; and after stirring, carrying out centrifugal separation at the centrifugal rotation speed of 5000-12000 rpm for 8-20 min, and recovering the upper oil phase.
Example 5
A dispersing agent for removing oil from shale gas-oil-based drilling cuttings and an oil removing method thereof are disclosed, which specifically comprise the following steps:
a. oil removal dispersing agent for shale gas oil-based drilling cuttings: 30 parts of inorganic base sodium hydroxide, 2 parts of organic base triethylene diamine, 0.5 part of surfactant, 0.5 part of defoaming agent tributyl phosphate and 15 parts of sodium hexametaphosphate; the surfactant is a mixture of a cationic surfactant and a nonionic surfactant, 0.2 part of cetyl trimethyl ammonium bromide and 0.3 part of monolauryl phosphate; adding water to prepare a dispersant into a solvent with the mass fraction of 5%;
b. weighing 500g of oil-based drilling cuttings in a beaker 1, adding 1000g of deoiling dispersant, stirring at the temperature of 50 ℃, wherein the stirring speed is 150-450 rpm, the stirring time is 50min, and standing for layering; pouring the oil-water phase into a beaker 2, putting the rest solid phase into hot water at 50-90 ℃, wherein the volume ratio of the hot water to the solid phase is 3: 1, continuously stirring for 40-90min, pouring the oil-water phase into the beaker 2 again, filtering the rest solid phase, drying and measuring.
c. Adding a sulfuric acid solution with the mass fraction of 10% into the beaker 2, adjusting the pH to 3-4, and stirring for 5-30 min; and after stirring, carrying out centrifugal separation at the centrifugal rotation speed of 5000-12000 rpm for 8-20 min, and recovering the upper oil phase.
Example 6
A dispersing agent for removing oil from shale gas-oil-based drilling cuttings and an oil removing method thereof are disclosed, which specifically comprise the following steps:
a. oil removal dispersing agent for shale gas oil-based drilling cuttings: 30 parts of inorganic base sodium carbonate, 2 parts of organic base triethylamine, 2 parts of surfactant, 0.4 part of defoaming agent tributyl phosphate and 25 parts of sodium hexametaphosphate; the surfactant is a mixture of a cationic surfactant and a nonionic surfactant, and 1 part of octadecyl trimethyl ammonium chloride and 1 part of span are used as the surfactant; adding water to prepare a dispersing agent into a solvent with the mass fraction of 10%;
b. weighing 500g of oil-based drilling cuttings in a beaker 1, adding 1000g of deoiling dispersant, stirring at the temperature of 50 ℃, wherein the stirring speed is 150-450 rpm, the stirring time is 50min, and standing for layering; pouring the oil-water phase into a beaker 2, placing the rest solid phase into hot water at 50-90 ℃, wherein the volume ratio of the hot water consumption to the oil-based drilling cuttings is 2.5: 1, continuously stirring for 40-90min, pouring the oil-water phase into the beaker 2 again, filtering the rest solid phase, drying and measuring.
c. Adding a sulfuric acid solution with the mass fraction of 10% into the beaker 2, adjusting the pH to 3-4, and stirring for 5-30 min; and after stirring, carrying out centrifugal separation at the centrifugal rotation speed of 5000-12000 rpm for 8-20 min, and recovering the upper oil phase.
Comparative example 1
Dispersing agent: 40 parts of sodium carbonate and 2 parts of span are prepared into a 10% aqueous solution.
The rest of the treatment was the same as in example 6.
Comparative example 2
Dispersing agent: 40 parts of sodium carbonate are formulated into a 10% aqueous solution.
The rest of the treatment was the same as in example 6.
Comparative example 3
Dispersing agent: 2 parts of span are prepared into a 10% aqueous solution.
The rest of the treatment was the same as in example 6.
And (3) oil content determination: measuring the OIL content of the OIL-based drilling cuttings by using an OIL460 type infrared spectroscopy OIL analyzer, wherein carbon tetrachloride is used as an extracting agent:
1. weighing a mass (m) of oil-based drill cuttings (dry basis), (to the nearest 0.0001 g);
2. weighing 25mL of carbon tetrachloride and the oil-based drilling cuttings, mixing and stirring for 30min, and standing for 20 min;
3. taking 5mL of the extract liquid after standing in the previous step, adding the extract liquid into a 25mL colorimetric tube, diluting the extract liquid to a scale mark by using carbon tetrachloride, uniformly mixing the extract liquid and the scale mark by shaking, and measuring the oil content (C, unit: mg/L);
4. and converting the measured data into the oil content in the oil-based drilling cuttings (dry bases) according to the dilution factor, wherein the residual oil rate is calculated according to the formula:
determination of ignition loss:
1. drying and pulverizing the solid phase obtained by dispersion, weighing 1g (M) of solid powder, and uniformly spreading in a cupel (to the accuracy of 0.0001 g);
2. and (3) feeding the cupel into a muffle furnace with the temperature not exceeding 100 ℃, closing the furnace door and leaving a gap of about 15mm on the furnace door.
3. The temperature of the furnace was slowly raised to 500 ℃ over a period of not less than 30min and maintained at this temperature for 30 min. The temperature is increased to 815-10 ℃ and the mixture is burned for 1 h.
4. The cupel is removed from the oven, placed on a heat resistant or asbestos plate, cooled in air for about 5min, transferred to a desiccator, cooled to room temperature (about 20min), and weighed (m).
5. And carrying out checking ignition for 20min each time until the mass of the coal sample dried twice continuously does not exceed 0.001g, and taking the mass of the last ignition as a calculation basis. Below 15% ash, no check-burning is required.
The formula for calculating the loss on ignition is as follows: (M-M)/M.
The results of examination of each of the processing data in examples 1 to 6 and the oil-based drill cutting processing methods according to each comparative example are shown in table 1.
TABLE 1 data of the examples
FIG. 2 shows the effect of the final oil and water phases obtained by three different treatments according to the comparative example and the invention. The effect of the final oil-water phase after treatment of comparative example 1 is shown on the left, the effect of the final oil-water phase after treatment of comparative example 3 is shown in the middle, and the effect of the final oil-water phase after treatment of example 6 according to the invention is shown on the right. As can be seen from fig. 2, the oil phase after the stratified phase separation and the centrifugal treatment after the treatment with different dispersants can find that the oil removing effect is poor and the dispersive stratified effect is not obvious in the comparative example, which seriously affects the oil removing efficiency, but the third group of effects obtained by a series of treatments after the treatment with the dispersant of the present invention is obviously improved, the oil removing efficiency is high and the dispersive effect is obvious, which indicates that the dispersant and the oil removing method of the present invention have a good effect on the oil removing of shale gas-oil based drill cuttings.
Finally, it is noted that the above-mentioned preferred embodiments illustrate rather than limit the invention, and that, although the invention has been described in detail with reference to the above-mentioned preferred embodiments, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the scope of the invention as defined by the appended claims.
Claims (9)
1. The oil removing method of the shale gas-oil-based drilling cuttings is characterized by comprising the following specific steps:
1) adding the oil-based drilling cuttings into a dispersing agent in a container 1, stirring at room temperature, wherein the stirring speed is 150-450 rpm, the stirring time is 40-90min, and standing for layering; pouring the oil-water phase into the container 2; the dispersing agent comprises, by mass, 10-40 parts of inorganic base, 0.01-2 parts of organic base, 0.01-2 parts of surfactant, 0.01-0.5 part of defoaming agent and 5-30 parts of sodium hexametaphosphate;
2) adding a sulfuric acid solution into the container 2, adjusting the pH to 3-4, stirring, performing centrifugal separation at a centrifugal speed of 5000-12000 rpm for 8-20 min, and recovering an upper oil phase.
2. The shale gas-oil-based drill cuttings deoiling method of claim 1, wherein the volume ratio of the oil-based drill cuttings to the dispersing agent in the step 1) is 1:1-3, and the mass fraction of the dispersing agent is 5-35%.
3. The method for removing oil from shale gas-oil-based drill cuttings according to claim 1, wherein the volume ratio of the oil-based drill cuttings to the dispersing agent in the step 1) is 1:2, and the mass fraction of the dispersing agent is 10-20%.
4. The method of deoiling shale gas-oil based drill cuttings as claimed in claim 1, wherein step 1) of the deoiling method further comprises: and (3) putting the rest solid phase into hot water of 50-90 ℃, continuously stirring for 40-90min, pouring the oil-water phase into the container 2 again, filtering and drying the rest solid phase.
5. The oil removing method for the shale gas-oil-based drill cuttings according to claim 4, wherein the volume ratio of the consumption of hot water to the solid phase is 1.5-3.0: 1.
6. the method for removing oil from shale gas-oil-based drill cuttings according to any one of claims 1-5, wherein the raw material of the dispersing agent comprises the following components in parts by mass: 15-35 parts of inorganic base, 0.05-2 parts of organic base, 0.5-2 parts of surfactant, 0.1-0.5 part of defoaming agent and 10-25 parts of sodium hexametaphosphate.
7. The dispersing agent according to claim 1, wherein the dispersing agent raw material comprises the following components in parts by weight: 30 parts of inorganic base, 2 parts of organic base, 2 parts of surfactant, 0.4 part of defoaming agent and 25 parts of sodium hexametaphosphate.
8. The dispersant according to any one of claims 1 to 3, wherein the inorganic base is any one of sodium carbonate and sodium hydroxide; the organic base is any one of triethylamine, triethylene diamine and tetramethyl ethylene diamine; the surfactant is a mixture of cationic surfactant and nonionic surfactant; the defoaming agent is tributyl phosphate.
9. The dispersant according to claim 4, wherein the mass ratio of the cationic surfactant to the nonionic surfactant in the surfactant is 1:1 to 3.
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