CN110961073B - Application method of shale adsorption material in oil-water separation - Google Patents

Application method of shale adsorption material in oil-water separation Download PDF

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CN110961073B
CN110961073B CN201911232087.4A CN201911232087A CN110961073B CN 110961073 B CN110961073 B CN 110961073B CN 201911232087 A CN201911232087 A CN 201911232087A CN 110961073 B CN110961073 B CN 110961073B
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shale
sample
samples
adsorption
heating
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CN110961073A (en
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詹洪磊
张燕
陈儒
苗昕扬
赵昆
郝世杰
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China University of Petroleum Beijing
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12—Naturally occurring clays or bleaching earth
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
    • B01D17/02—Separation of non-miscible liquids
    • B01D17/0202—Separation of non-miscible liquids by ab- or adsorption

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  • Life Sciences & Earth Sciences (AREA)
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Abstract

The embodiment of the specification provides a shale adsorption material for oil-water separation and a preparation method thereof, and the method comprises the following steps: cutting shale into a plurality of shale samples; heating the plurality of shale samples to different temperatures; annealing the heated shale sample in different cooling modes to form a plurality of shale adsorption materials; and carrying out an adsorption experiment on the plurality of shale adsorption materials so as to select the shale adsorption material meeting preset conditions from the plurality of shale adsorption materials according to an experiment result. The embodiment of the present specification can reduce the manufacturing cost of the adsorbent.

Description

Application method of shale adsorption material in oil-water separation
Technical Field
The specification relates to the technical field of oil-water separation, in particular to an application method of a shale adsorbing material in oil-water separation.
Background
The oil and water are a pair of spears which are ubiquitous but incompatible in the nature, and the oil and water are mutually polluted and affect the normal use function, for example, when the waste mineral oil is discharged into a water body, an oil film can be formed on the water surface, the oxygen exchange between the water body and the atmosphere is blocked, the dissolved oxygen concentration of the water body is reduced, and the ecological system function is deteriorated (theoretically, 200L of oil can pollute 3.5km2Water surface), has a great influence on human production and life. Long-term practice proves that the separation of oil and water is the simplest and most effective method for solving the problem, so the development of the oil-water separation technology becomes the key for solving the contradiction.
Currently available process oilsWater separation techniques generally involve the chemical preparation of superhydrophobic, superoleophilic materials, e.g., the preparation of three-dimensional MoS2The method for preparing the oil-water separation material and the adsorption material comprises the following steps: MoS is treated by dip coating2MoS is prepared by combining flexible melamine formaldehyde sponge2Super-hydrophobic super-oleophilic sponge, and MoS is controlled by repeating dip-coating and drying process2When the loading amount of the nanosheets on the sponge is increased to 8.4%, the contact angle of the material reaches 150 +/-2 degrees, and the nanosheets have super-hydrophobic performance. The hydrophobic property of the material keeps high stability under different pH values and temperature conditions, and the material has higher oil absorption capacity to carry out oil-water separation.
However, the process for preparing the adsorbing material by a chemical method is complex and high in cost. Therefore, how to reduce the manufacturing cost of the adsorbent material has become a technical problem to be solved.
Disclosure of Invention
An object of the embodiments of the present disclosure is to provide a method for applying a shale adsorbing material in oil-water separation, so as to reduce the manufacturing cost of the adsorbing material.
In order to achieve the above object, in one aspect, an embodiment of the present specification provides an application method of a shale adsorption material in oil-water separation, including:
cutting shale into a plurality of shale samples;
heating the plurality of shale samples to different temperatures;
annealing the heated shale sample in different cooling modes to form a plurality of shale adsorption materials;
and carrying out an adsorption experiment on the plurality of shale adsorption materials so as to select the shale adsorption material meeting preset conditions from the plurality of shale adsorption materials according to an experiment result.
In one embodiment of the present disclosure, when the plurality of shale samples are cut from two or more shales, the two or more shales are taken from a formation at the same depth.
In an embodiment of the present description, the heating the plurality of shale samples to different temperatures includes:
heating the plurality of shale samples to different temperatures at different ramp rates.
In an embodiment of the present disclosure, the shale sample is a shale slice.
In an embodiment of the present specification, the cooling manner includes water cooling, air cooling, or furnace cooling.
On the other hand, the embodiment of the specification further provides a shale adsorption material for oil-water separation, and the shale adsorption material is obtained by the following preparation method:
cutting shale into a plurality of shale samples;
heating the plurality of shale samples to different temperatures;
annealing the heated shale sample in different cooling modes to form a plurality of shale adsorption materials;
and carrying out an adsorption experiment on the plurality of shale adsorption materials so as to select the shale adsorption material meeting preset conditions from the plurality of shale adsorption materials according to an experiment result.
In one embodiment of the present disclosure, when the plurality of shale samples are cut from two or more shales, the two or more shales are taken from a formation at the same depth.
In an embodiment of the present description, the heating the plurality of shale samples to different temperatures includes:
heating the plurality of shale samples to different temperatures at different ramp rates.
In an embodiment of the present disclosure, the shale sample is a shale slice.
In an embodiment of the present specification, the cooling manner includes water cooling, air cooling, or furnace cooling.
According to the technical scheme provided by the embodiment of the specification, the shale with extremely low cost is used as a raw material in the embodiment of the specification, and the shale is cut into a plurality of shale samples; heating a plurality of shale samples to different temperatures to change the phases and the structures of the shale samples in a high-temperature pyrolysis mode so as to form a structure rich in pore structures and oxide components; annealing the heated shale sample in different cooling modes to form a plurality of shale adsorption materials; finally, adsorption experiments are carried out on the various shale adsorption materials, so that the shale adsorption materials meeting preset conditions are selected from the various shale adsorption materials according to experiment results, and the natural shale is prepared into the novel material with high-efficiency adsorption performance through the simple process. Compared with the existing method for preparing the adsorption material by a chemical method, the method has the advantages of simple process and low cost. Moreover, the shale adsorption material in the embodiment of the specification takes natural shale as a material, and harmful chemical substances are not generated in the preparation process, so that the environment is protected.
Drawings
In order to more clearly illustrate the embodiments of the present specification or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, it is obvious that the drawings in the following description are only some embodiments described in the present specification, and for those skilled in the art, other drawings can be obtained according to the drawings without any creative effort. In the drawings:
FIG. 1 is a flow chart of a method for using a shale adsorbent material in oil-water separation in accordance with certain embodiments of the present disclosure;
FIG. 2a is a schematic diagram of a water absorption terahertz spectrum of a normal-temperature shale sample in an exemplary embodiment of the present specification;
FIG. 2b is a schematic representation of a terahertz spectrum of water absorption of a shale sample heated to 925 ℃ in an exemplary embodiment of the present description;
FIG. 2c is a schematic representation of a water absorption terahertz spectrum of a shale sample heated to 710 ℃ in an exemplary embodiment of the present description;
FIG. 2d is a schematic representation of the water absorption terahertz spectrum of a shale sample heated to 975 ℃ in an exemplary embodiment of the present description;
FIG. 2e is a schematic representation of a water absorption terahertz spectrum of a shale sample heated to 880 ℃ in an exemplary embodiment of the present description;
FIG. 2f is a schematic representation of a water absorption terahertz spectrum of a shale sample heated to 1000 ℃ in an exemplary embodiment of the present description;
FIG. 3 is a schematic representation of water absorption terahertz spectra of a shale sample heated to 925 ℃ under different cooling modes in an exemplary embodiment of the present description;
FIG. 4a is a schematic diagram of the terahertz time-domain amplitude of the oil-water mixture varying with time in an exemplary embodiment of the present disclosure;
FIG. 4b is a schematic diagram illustrating water content of the oil-water mixture over time in an exemplary embodiment of the disclosure.
Detailed Description
In order to make those skilled in the art better understand the technical solutions in the present specification, the technical solutions in the embodiments of the present specification will be clearly and completely described below with reference to the drawings in the embodiments of the present specification, and it is obvious that the described embodiments are only a part of the embodiments of the present specification, and not all of the embodiments. All other embodiments obtained by a person skilled in the art based on the embodiments in the present specification without any inventive step should fall within the scope of protection of the present specification.
Shale is the main form of unconventional oil and gas reservoirs, and shale has wide sources, extremely low cost and good thermal stability. Therefore, shale may be considered as the adsorbent material. However, studies have shown that natural shale has low adsorption properties and is difficult to use directly as an adsorbent material. Therefore, natural shale needs to be processed to greatly improve its adsorption performance, so that it can be applied to oil-water separation.
Therefore, the specification provides an application method of the shale adsorbing material in oil-water separation. Referring to fig. 1, a method for applying the shale adsorbing material in oil-water separation according to some embodiments of the present disclosure may include the following steps:
s101, cutting the shale into a plurality of shale samples.
In some embodiments of the present disclosure, the shale samples may be cut from the same block of shale samples such that the shale samples have the same or very similar shale structure, thereby facilitating subsequent comparisons. Of course, in some other embodiments of the present disclosure, when the plurality of shale samples are cut from two or more shales, the two or more shales may be taken from the same depth of the formation, so as to ensure that each shale sample has the same or very similar shale structure.
The present description is not limited to the shape of the shale sample, and the shale may be cut into any desired shape as desired. In some embodiments of the present disclosure, when the shale sample is a shale slice (i.e., the shale is sliced into slices), the adsorption area can be effectively increased, thereby facilitating the improvement of the adsorption capacity and the material utilization rate. For example, in an exemplary embodiment, the shale may be cut into slices having lengths, widths, and thicknesses of 20mm, and 2mm, respectively.
And S102, heating the plurality of shale samples to different temperatures.
In some embodiments of the present disclosure, the shale sample is heated (i.e., pyrolyzed) to change the phase and structure of the shale sample by pyrolysis to form a shale sample rich in the pore structure and oxide components, so as to greatly improve the adsorption performance of the shale sample. Because different heating temperatures have different degrees of influence on the phase and the structure of the shale sample, in order to be beneficial to finding out the shale sample with the optimal adsorption performance or better adsorption performance, a plurality of shale samples can be heated to different temperatures. For example, in an exemplary embodiment, three shale samples are cut: sample 1, sample 2 and sample 3, sample 1 may be heated to 700 ℃, sample 2 to 800 ℃, and sample 3 to 900 ℃.
In other embodiments of the present disclosure, considering that the temperature rising rate may also affect the phase and structure of the shale sample, for this purpose, several shale samples with the same heating temperature but different temperature rising rates may also be provided to facilitate the subsequent comparison and screening. For example, in one exemplary embodiment, nine shale samples are cut: sample 1 to sample 9. Samples 1-3 can be heated to 700 ℃, with the temperature rise rate of sample 1 being 10 ℃/min, the temperature rise rate of sample 2 being 20 ℃/min, and the temperature rise rate of sample 3 being 50 ℃/min. Samples 4-6 can be heated to 800 ℃, with the temperature rise rate of sample 4 being 10 ℃/min, the temperature rise rate of sample 5 being 20 ℃/min, and the temperature rise rate of sample 6 being 50 ℃/min. Samples 7-9 can be heated to 900 ℃, with sample 7 heating up at a rate of 10 ℃/min, sample 8 heating up at a rate of 20 ℃/min, and sample 9 heating up at a rate of 50 ℃/min.
In an exemplary embodiment of the present description, the shale sample may be placed into a tube furnace (or other suitable heating furnace) for heating.
And S103, annealing the heated shale sample in different cooling modes to form a plurality of shale adsorbing materials.
In some embodiments of the present disclosure, the shale sample is annealed to improve uniformity of adsorption properties of the shale sample. Different annealing modes have different degrees of influence on the uniformity of the adsorption performance of the shale samples, and in order to be beneficial to finding out the shale samples with the optimal adsorption performance or better adsorption performance, after a plurality of shale samples are heated to different temperatures, the shale samples after being heated can be annealed by adopting different cooling modes (the cooling modes comprise water cooling, air cooling or furnace cooling) so as to be beneficial to subsequent comparison and screening. In some embodiments, the cooling means may include, but is not limited to, water cooling, air cooling, furnace cooling, or the like. For example, in an exemplary embodiment, three shale samples are cut: sample a, sample B and sample C. After the three shale samples are heated to different temperatures, the sample A can be annealed in a water cooling mode, the sample B can be annealed in an air cooling mode, and the sample C can be annealed in a furnace cooling mode.
And S104, performing an adsorption experiment on the plurality of shale adsorption materials to select the shale adsorption materials meeting preset conditions from the plurality of shale adsorption materials according to an experiment result.
In some embodiments of the present disclosure, after obtaining a plurality of shale adsorption materials, in order to select a shale adsorption material with the optimal adsorption performance, the shale adsorption materials may be subjected to an adsorption experiment, and corresponding experimental results are obtained. Correspondingly, the selecting, according to the experimental result, a shale adsorption material meeting a preset condition from the plurality of shale adsorption materials may include: obtaining the adsorption performance of each shale adsorption material according to the experimental result; the shale adsorbing materials with better adsorption performance can be obtained by comparing the adsorption performance of various shale adsorbing materials.
For example, in an exemplary embodiment of the present specification, fig. 2a to 2f show water absorption terahertz spectra of shale samples at different heating temperatures, wherein the abscissa is the heating time and the ordinate is the terahertz spectrum value, and it can be seen from fig. 2a to 2f that the water absorption of the shale sample at a high temperature is better and the shale at a temperature range around 900 ℃ (925 ℃) has a better water absorption effect compared with the shale sample at a normal temperature. Referring to fig. 3, fig. 3 shows the result of uv spectrophotometer test of shale sample heated to 925 ℃ absorbing methyl orange under furnace cooling, air cooling and water cooling respectively, and it can be seen from fig. 3 that: the shale adsorption performance under the air cooling condition is better. Compared with the adsorption performance of the shale under different heat treatment modes and different cooling modes, the shale sample has better water adsorption performance under high-temperature and air-cooling conditions, so that a new shale material with high-efficiency adsorption can be obtained.
In an exemplary embodiment of the present disclosure, high temperature shale with superior water absorption may be selected for oil-water separation validation experiments, and the shale at 925 ℃ is crushed into particles and sieved to obtain uniform particles. Preparing an oil-water mixture in a water bath, putting the shale particles at 925 ℃ into the oil-water mixture for stirring, and testing the oil-water mixture every 10 minutes, so that a terahertz time-domain amplitude-versus-time variation curve of the oil-water mixture shown in fig. 4a can be obtained. It can be seen from fig. 4a that, as the oil-water mixture is adsorbed by the high-temperature shale, the terahertz time-domain amplitude of the oil-water mixture increases, and correspondingly, the terahertz wave absorption thereof decreases. The terahertz waves are greatly absorbed by water, and the terahertz waves are absorbed by the oil-water mixture to be reduced, so that the reduction of the water in the oil-water mixture is indicated. And taking the reciprocal of the terahertz time-domain amplitude of the oil-water mixture in fig. 4a, the water content change curve of the oil-water mixture with time as shown in fig. 4b can be obtained. As can be seen in fig. 4 b: along with the increase of the adsorption time of the high-temperature shale on the oil-water mixture, the water content in the oil-water mixture is continuously reduced, so that the high-temperature shale has better water absorbability. Therefore, in the embodiment of the specification, shale with extremely low cost is used as a raw material, and the shale is cut into a plurality of shale samples; heating a plurality of shale samples to different temperatures to change the phases and the structures of the shale samples in a high-temperature pyrolysis mode so as to form a structure rich in pore structures and oxide components; annealing the heated shale sample in different cooling modes to form a plurality of shale adsorption materials; finally, adsorption experiments are carried out on the various shale adsorption materials, so that the shale adsorption materials meeting preset conditions are selected from the various shale adsorption materials according to experiment results, and the natural shale is prepared into the novel material with high-efficiency adsorption performance through the simple process. Compared with the existing method for preparing the adsorption material by a chemical method, the method has the advantages of simple process and low cost. Moreover, the shale adsorption material in the embodiment of the specification takes natural shale as a material, and harmful chemical substances are not generated in the preparation process, so that the environment is protected.
While the process flows described above include operations that occur in a particular order, it should be clear that the processes may also include more or fewer operations.
It should also be noted that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other like elements in a process, method or apparatus that comprises the element.
The embodiments in the present specification are described in a progressive manner, and the same and similar parts among the embodiments are referred to each other, and each embodiment focuses on the differences from the other embodiments. In particular, for the system embodiment, since it is substantially similar to the method embodiment, the description is simple, and for the relevant points, reference may be made to the partial description of the method embodiment.
The above description is only an example of the present specification, and is not intended to limit the present specification. Various modifications and alterations to this description will become apparent to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present specification should be included in the scope of the claims of the present specification.

Claims (2)

1. An application method of a shale adsorbing material in oil-water separation is characterized by comprising the following steps:
cutting shale into a plurality of shale samples, wherein when the plurality of shale samples are cut from two or more pieces of shale, the two or more pieces of shale are taken from stratums with the same depth;
heating the plurality of shale samples to different temperatures at different heating rates, so that the phase and the structure of the shale samples are changed through high-temperature pyrolysis to form shale samples rich in pore structures and oxide components, specifically, obtaining samples 1-9, heating the samples 1-3 to 700 ℃, wherein the heating rate of the sample 1 is 10 ℃/min, the heating rate of the sample 2 is 20 ℃/min, and the heating rate of the sample 3 is 50 ℃/min; heating the samples 4-6 to 800 ℃, wherein the heating rate of the sample 4 is 10 ℃/min, the heating rate of the sample 5 is 20 ℃/min, and the heating rate of the sample 6 is 50 ℃/min; heating samples 7-9 to 900 ℃, wherein the heating rate of the sample 7 is 10 ℃/min, the heating rate of the sample 8 is 20 ℃/min, and the heating rate of the sample 9 is 50 ℃/min;
annealing the heated shale sample by adopting different cooling modes to improve the uniformity of the adsorption performance of the shale sample so as to form a plurality of shale adsorption materials, wherein the cooling modes comprise water cooling, air cooling or furnace cooling;
and carrying out an adsorption experiment on the plurality of shale adsorption materials so as to select the shale adsorption material meeting preset conditions from the plurality of shale adsorption materials according to an experiment result.
2. The method of using the shale adsorption material of claim 1 to separate oil and water, wherein the shale sample is a shale slice.
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JP2006232612A (en) * 2005-02-24 2006-09-07 Mizusawa Ind Chem Ltd Mesoporous silica
AU2007278836B2 (en) * 2006-07-26 2012-04-05 Nanotech Investment 2 (Pty) Ltd Activation, refining, and use of oil shale
CN105214604B (en) * 2015-09-21 2018-02-16 潍坊泥博士新型材料有限公司 A kind of preparation method of high adsorption diatomaceous shale material

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An optical mechanism for detecting the whole pyrolysis process of oil shale;Honglei Zhan et al;《Energy》;20191031;第190卷;第2节第1-2段 *
The mechanism of the terahertz spectroscopy for oil shale detection;Honglei Zhan et al;《Energy》;20180719;第161卷;第2节第1-2段 *

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