CN115672257A - Preparation method of adsorbent for oil-water separation - Google Patents
Preparation method of adsorbent for oil-water separation Download PDFInfo
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Abstract
The disclosure relates to the technical field of water body treatment, in particular to a preparation method of an adsorbent for oil-water separation, and aims to overcome the defects in the prior art, the disclosure provides a preparation method of an adsorbent for oil-water separation, which comprises the following steps: (1) preparing a solution A; (2) preparing a solution B; (3) carrying out hydrothermal reaction; (4) preparation of sample C; (5) preparation of sample D; and uniformly mixing the sample D and commercially available alumina according to a certain mass ratio, soaking the sample D and absolute ethyl alcohol in the same volume, then placing the mixture into a plasma reactor, and reacting in a plasma atmosphere to obtain the oil-water separation adsorbent.
Description
Technical Field
The disclosure relates to the technical field of water body treatment, in particular to a preparation method of an adsorbent for oil-water separation.
Background
Industrial oily wastewater mainly comes from petrochemical industry, in recent years, the problems of oil-water pollution are more serious due to continuous discharge of oily wastewater and frequent occurrence of oil spill accidents, and the oily wastewater is wasted if not recycled; when the water is discharged into rivers, lakes or gulfs, the water body is polluted, and the survival of aquatic organisms is influenced; when the water-oil separation agent is used for agricultural irrigation, soil gaps can be blocked, and the growth of crops is hindered, so that the water-oil separation agent not only causes catastrophic damage to the ecological environment, but also causes serious harm to human health, and therefore, the water-oil separation agent has important practical significance and application value in the development of oil-water separation technology.
The treatment of the oily wastewater should first consider the recovery of oil substances and make full use of the treated water resource. Therefore, the treatment of the oily wastewater can firstly utilize the oil separation tank to recover floating oil or heavy oil. The oil separation tank is suitable for separating oil products with larger particles in the wastewater, the treatment efficiency is 60-80%, the oil content in the effluent is about 100-200 mg/L, and however, fine oil droplets and emulsified oil in the wastewater are difficult to remove. Because the oily wastewater has harmfulness to industrial production and ecological environment, the deep purification of the oily wastewater in the petrochemical industry becomes a problem which needs to be solved in the petrochemical and chemical industries. At present, the commonly used methods for purifying oily wastewater include methods such as a float method, a gravity separation method, a filtration method, a biological method, an adsorption method and the like. The adsorption method has the characteristics of low operation cost, no by-product and the like, and is widely applied.
For example, chinese patent with an authorization publication number of CN107792912B discloses a preparation method of an oil-containing wastewater adsorbing material, which is prepared from polytrimethylene phthalate, bisphenol A epoxy resin, vinylbenzyltrimethylammonium chloride, coconut shells, phenol, polyvinyl alcohol and other raw materials.
And further discloses a wastewater adsorption treatment agent and a preparation method and application thereof as disclosed in a Chinese patent with an authorization publication number of CN110115990B, wherein the wastewater adsorption treatment agent comprises the following components in parts by weight: 30-60 parts of bio-based adsorption resin, 30-50 parts of pyrophyllite composite active particles, 10-20 parts of metal polysilicate and 10-25 parts of ceramsite. The wastewater adsorption treatment agent can strongly adsorb oil and polymers which are difficult to degrade in water, has remarkable wastewater treatment effect, stable property, no secondary pollution after treatment and low treatment cost, can ensure that the treated water can reach the discharge standard, and is suitable for sewage disposal in the fields of oily wastewater, printing and dyeing wastewater, papermaking wastewater, municipal wastewater and the like.
Disclosure of Invention
Aiming at the defects in the prior art, the method for preparing the adsorbent for oil-water separation is provided, the adsorbent prepared by the method can be used for separating oil substances from industrial wastewater, has wide water quality adaptability, and can effectively solve the problem of oil-water separation of oily wastewater.
The technical scheme adopted by the disclosure for solving the technical problems is as follows: a preparation method of an adsorbent for oil-water separation comprises the following steps:
(1) Preparation of solution A: stirring and mixing anhydrous ethanol and N, N-dimethylformamide uniformly at normal temperature according to a certain mass ratio to obtain a solution A;
(2) Preparation of solution B: adding an iron salt precursor into the solution A according to a certain mass ratio, and ultrasonically stirring for 1-2 h at a certain temperature to obtain a solution B;
(3) Hydrothermal reaction: transferring the solution B into a high-pressure reaction kettle, and placing the solution B into a forced air drying oven to perform hydrothermal reaction for 6-8 h at a certain temperature;
(4) Preparation of sample C: taking out the solid matter after the hydrothermal reaction, and drying the solid matter in a rotary evaporator to obtain a sample C;
(5) Preparation of sample D: placing the sample C in a tubular furnace for sectional roasting to obtain a sample D;
(6) And uniformly mixing the sample D and commercially available alumina according to a certain mass ratio, soaking the sample D and absolute ethyl alcohol in the same volume, then placing the mixture into a plasma reactor, and reacting in a plasma atmosphere to obtain the oil-water separation adsorbent.
Compared with the existing products, the beneficial effects of the present disclosure are: the preparation method has simple process and convenient and fast operation, and the used adsorbent can be regenerated by a simple heat treatment method through the sectional type roasting in the step (5) and the reaction of the plasma atmosphere in the step (6); the adsorbent prepared by the method does not contain harmful substances, and meanwhile, the adsorption of the adsorbent on oily substances is a physical adsorption process, and byproducts are not generated, so that no secondary pollution is generated in the oil-water separation process; because of sectional type roasting, the adsorbent can adapt to water quality with large oil content fluctuation.
Furthermore, the mass ratio of the absolute ethyl alcohol to the N, N-dimethylformamide in the step (1) is 5:1-1:1.
Further, the mass ratio of the iron salt precursor to the solution A in the step (2) is 1:5-1, and the stirring temperature is 40-70 ℃; the ferric salt precursor is ferrous nitrate or ferrous sulfate or ferrous chloride; the ultrasonic agitation enables the precursor of the ferric salt to be better dispersed in the solution A.
Further, the volume of the solution B added into the high-pressure reaction kettle in the step (3) is 1/6-1/3 of the maximum volume of the reaction kettle; the hydrothermal temperature in the air-blast drying box is kept between 80 and 100 ℃, the hydrothermal temperature determines the reaction pressure in the high-pressure reaction kettle, the reaction pressure influences the conversion and crystallization degree of the iron salt in the reaction kettle, and the conversion and crystallization degree of the iron salt is better in the temperature range.
Further, the temperature of the rotary evaporator in the step (4) is 80-90 ℃, the liquid phase is not easy to evaporate when the temperature is too low, the liquid phase is not easy to evaporate when the temperature is too high, and the obtained sample C is easy to agglomerate.
Further, the step (5) of the step-type roasting comprises a first stage and a second stage, wherein the first stage is an oxidation process, and the second stage is a reduction process.
Furthermore, the oxidizing atmosphere used in the first stage of roasting is 5-10% by volume of oxygen, nitrogen is used as balance gas, the roasting time is prolonged due to too low oxygen content, the roasting cost is increased, and the excessive oxygen content can cause excessive oxidation of iron salt and can not form a required oxide structure; the roasting temperature is 600-800 ℃, if the temperature exceeds the temperature range, the temperature is too low, the ferric salt precursor cannot be completely decomposed, the temperature is too high, the oxide can be sintered, the roasting time is 2-4 h, the ferric salt precursor cannot be completely decomposed if the roasting time is too short, and the roasting cost is increased if the roasting time is too long.
Furthermore, the reducing atmosphere used in the second stage of roasting is 1-3% by volume of hydrogen, nitrogen is used as balance gas, the content of hydrogen is too low to form sufficient unsaturated active sites, and the content of hydrogen is too high to cause excessive reduction of iron oxide, thereby reducing the adsorption performance of the adsorbent; the roasting temperature is 700-900 ℃, the temperature is too low, the hydrogen can not form unsaturated active sites on the surface through reduction reaction, and the excessive reduction of the iron oxide can be caused by too high temperature; the roasting time is 0.5-1 h, the roasting time is too short, the number of unsaturated active sites is small, and the excessive reduction of the iron oxide can be caused by too long time.
Further, the mass ratio of the sample D to the commercial alumina in the step (6) is 1:2-1:4; the reaction atmosphere in the plasma reactor is pure CO gas or pure CO 2 The reaction time of gas and plasma is 5-20 min.
The plasma reactor is used for raising the low voltage to positive high voltage and negative high voltage through the booster circuit, and utilizing the positive high voltage and negative high voltage to ionize air (mainly oxygen) to generate a large amount of positive ions and negative ions, wherein the number of the negative ions is larger than that of the positive ions (the number of the negative ions is about 1.5 times of that of the positive ions), and the positive ions and the negative ions simultaneously generated by the plasma generator instantaneously generate huge energy release during the neutralization of positive and negative charges in the air, so that the change of the surrounding bacterial structure or the energy conversion is caused, bacteria are killed, and the sterilization effect of the bacteria is realized. Because the quantity of the negative ions is greater than that of the positive ions, redundant negative ions still float in the air, the effects of smoke elimination, dust removal, peculiar smell elimination and air quality improvement can be achieved, and in addition, the plasma reactor has the characteristics of high efficiency, quickness, no pollution and the like.
Further, the used adsorbent is recycled by a thermal regeneration method.
Preferably, the used adsorbent is thermally purged at 350 to 500 ℃ for 10 to 30min under an atmosphere of nitrogen or carbon dioxide to separate the adsorbed oily substance from the adsorbent, the oily substance volatilizes at the current temperature and is carried away by the flowing gas, and the carried-away oily substance can be recovered by condensation.
Furthermore, a large amount of unsaturated active sites can be generated in the two-stage roasting process of the iron element, when the oil content of the water body is low, the oil substances are preferentially adsorbed and removed by the common adsorption sites on the surface of the adsorbent, and when the oil content of the water body is high, the unsaturated active sites on the surface of the adsorbent play a role in auxiliary adsorption through electronic defects, so that more oil substances can be adsorbed, and the water quality with high oil content fluctuation can be adapted.
Drawings
The present application will be described in further detail below with reference to the drawings and preferred embodiments, but those skilled in the art will appreciate that the drawings are only drawn for the purpose of illustrating the preferred embodiments and therefore should not be taken as limiting the scope of the present application. Furthermore, unless specifically stated otherwise, the drawings are merely schematic representations based on conceptual representations of elements or structures depicted and may contain exaggerated displays and are not necessarily drawn to scale.
Fig. 1 is a process flow diagram of the present disclosure.
Detailed Description
In order to make the technical solutions of the present disclosure better understood by those skilled in the art, the present disclosure will be described in detail, clearly and completely with reference to the accompanying drawings and examples. It should be understood that the specific embodiments described herein are merely illustrative of the disclosure and are not intended to limit the disclosure.
In the description of the present invention, if there are first and second described only for the purpose of distinguishing technical features, it is not understood that relative importance is indicated or implied or that the number of indicated technical features or the precedence of the indicated technical features is implicitly indicated or implied.
It will be understood by those skilled in the art that in the present disclosure, the terms "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in an orientation or positional relationship indicated in the drawings for ease of description and simplicity of description, and do not indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and thus, the above terms should not be construed as limiting the present invention.
Example 1
Anhydrous ethanol and N, N-dimethylformamide are stirred and mixed uniformly at normal temperature according to the mass ratio of 5:1 to obtain a solution A. Ferrous nitrate is added into the solution A according to the mass ratio of 1:8, and ultrasonic stirring is carried out for 1h at 70 ℃ to obtain a mixed solution B. And pouring the mixed solution B into a high-pressure reaction kettle, adding the mixed solution B into the high-pressure reaction kettle with the volume being 1/6 of the maximum volume in the kettle, and placing the high-pressure reaction kettle in an air-blast drying oven for hydrothermal reaction for 8 hours at the temperature of 90 ℃. The solid material after the hydrothermal reaction was taken out and dried to a powder form at 82 ℃ in a rotary evaporator to obtain sample C. Placing the sample C in a tube furnace for two-section roasting: the oxidizing atmosphere used in the first stage of roasting is oxygen (nitrogen is used as balance gas) with the volume percentage of 10 percent, the roasting temperature is 800 ℃, and the roasting time is 3 hours; the second stage of calcination uses a reducing atmosphere of 3 vol% hydrogen (nitrogen as the balance gas), the calcination temperature is 900 ℃, and the calcination time is 1h, as sample D. And uniformly mixing the sample D and commercial alumina according to a mass ratio of 1:3, soaking the mixture with absolute ethyl alcohol in the same volume, placing the mixture into a plasma reactor, and reacting for 5min in a pure CO plasma atmosphere to obtain the oil-water separation adsorbent.
The deoiling performance of the adsorbent is tested by adopting an oil-water mixture with the oil content of 18g/L, and the deoiling efficiency in a liquid phase reaches 100% after 30min, which shows that the adsorbent has an obvious effect on separating the oil-water mixture.
And (3) thermally blowing the used adsorbent at 350 ℃ for 20min under the atmosphere of nitrogen to realize the separation of the adsorbed oily substances from the adsorbent.
Example 2
Stirring and uniformly mixing absolute ethyl alcohol and N, N-dimethylformamide according to a mass ratio of 3.5. Ferrous nitrate is added into the solution A according to the mass ratio of 1:9, and ultrasonic stirring is carried out for 1.5h at 70 ℃ to obtain a mixed solution B. Pouring the mixed solution B into a high-pressure reaction kettle, adding the mixed solution B into the high-pressure reaction kettle with the volume being 1/5 of the maximum volume in the kettle, and placing the high-pressure reaction kettle in an air-blast drying oven for hydrothermal reaction for 6.5 hours at the temperature of 100 ℃. The solid material after the hydrothermal reaction was taken out and dried to a powder form at 80 ℃ in a rotary evaporator to obtain sample C. Placing the sample C in a tube furnace for two-section roasting: the oxidizing atmosphere used in the first stage of roasting is 5 volume percent of oxygen (nitrogen is used as balance gas), the roasting temperature is 750 ℃, and the roasting time is 2.5 hours; the second stage of calcination uses 1 vol% hydrogen (nitrogen as balance gas) as reducing atmosphere, the calcination temperature is 850 deg.C, and the calcination time is 0.6h, as sample D. And uniformly mixing the sample D and commercial alumina according to a mass ratio of 1:3, soaking the mixture with absolute ethyl alcohol in the same volume, placing the mixture into a plasma reactor, and reacting for 15min in a pure CO plasma atmosphere to obtain the oil-water separation adsorbent.
The deoiling performance of the adsorbent is tested by adopting an oil-water mixture with the oil content of 15g/L, and the deoiling efficiency in a liquid phase reaches 100% after 20min, which shows that the adsorbent has an obvious effect on the separation of the oil-water mixture.
And (3) thermally blowing the used adsorbent at 500 ℃ for 12min under the atmosphere of nitrogen to realize the separation of the adsorbed oily substances from the adsorbent.
Example 3
Anhydrous ethanol and N, N-dimethylformamide are stirred and mixed uniformly at room temperature according to the mass ratio of 4:1 to obtain a solution A. Adding ferrous sulfate into the solution A according to a mass ratio of 1. And pouring the mixed solution B into a high-pressure reaction kettle, adding the mixed solution B into the high-pressure reaction kettle, wherein the volume of the mixed solution B is 1/4 of the maximum volume in the kettle, and placing the high-pressure reaction kettle in an air-blowing drying oven for hydrothermal reaction for 7.5 hours at 95 ℃. The solid material after the hydrothermal reaction was taken out and dried to a powder form at 86 ℃ in a rotary evaporator to obtain sample C. Placing the sample C in a tube furnace for two-section roasting: the oxidizing atmosphere used in the first stage of roasting is oxygen (nitrogen is used as balance gas) with the volume percentage of 7 percent, the roasting temperature is 750 ℃, and the roasting time is 3 hours; the second stage of calcination uses a reducing atmosphere of 2 vol% hydrogen (nitrogen as the balance gas), the calcination temperature is 880 ℃, and the calcination time is 1h, as sample D. And uniformly mixing the sample D with commercial alumina according to a mass ratio of 1:2, soaking the mixture with absolute ethyl alcohol in the same volume, placing the mixture into a plasma reactor, and reacting for 18min in a pure CO plasma atmosphere to obtain the oil-water separation adsorbent.
The deoiling performance of the adsorbent is tested by adopting an oil-water mixture with the oil content of 22g/L, and the deoiling efficiency in a liquid phase reaches 100% after 45min, which shows that the adsorbent has an obvious effect on separating the oil-water mixture.
And (3) thermally blowing the used adsorbent at 400 ℃ for 25min under the atmosphere of carbon dioxide to realize the separation of the adsorbed oily substances from the adsorbent.
Example 4
Anhydrous ethanol and N, N-dimethylformamide were stirred and mixed uniformly at room temperature in a mass ratio of 4.5. Ferrous sulfate is added into the solution A according to the mass ratio of 1:7, and ultrasonic stirring is carried out for 1.5h at the temperature of 55 ℃ to obtain a mixed solution B. And pouring the mixed solution B into a high-pressure reaction kettle, adding the mixed solution B into the high-pressure reaction kettle with the volume being 1/3 of the maximum volume in the kettle, and placing the high-pressure reaction kettle in an air-blast drying oven for hydrothermal reaction for 8 hours at the temperature of 85 ℃. The solid material after the hydrothermal reaction was taken out and dried to a powder form at 90 ℃ in a rotary evaporator to obtain sample C. Placing the sample C in a tube furnace for two-section roasting: the oxidizing atmosphere used in the first stage of roasting is 6 volume percent of oxygen (nitrogen is used as balance gas), the roasting temperature is 600 ℃, and the roasting time is 4 hours; the second stage of calcination uses 1 vol% hydrogen (nitrogen as balance gas) as reducing atmosphere, the calcination temperature is 700 ℃, and the calcination time is 0.65h, which is taken as sample D. Sample D and commercial alumina were mixed well in a mass ratio of 1.5 and immersed in an equal volume of absolute ethanol, then placed in a plasma reactor, in pure CO 2 Reacting for 10min in the plasma atmosphere to obtain the oil-water separation adsorbent.
The deoiling performance of the adsorbent is tested by adopting an oil-water mixture with the oil content of 12g/L, and the deoiling efficiency in a liquid phase reaches 100% after 58min, which shows that the adsorbent has an obvious effect on separating the oil-water mixture.
And (3) thermally blowing the used adsorbent at 500 ℃ for 28min under the atmosphere of nitrogen or carbon dioxide to separate the adsorbed oily substances from the adsorbent.
Example 5
Anhydrous ethanol and N, N-dimethylformamide are stirred and mixed uniformly at room temperature according to the mass ratio of 3:1 to obtain a solution A. Adding ferrous chloride into the solution A according to a mass ratio of 1. Pouring the mixed solution B into a high-pressure reaction kettle, wherein the volume of the mixed solution B added into the high-pressure reaction kettle is 1/5 of the maximum volume in the kettleAnd placing the mixture in a forced air drying oven to perform hydrothermal reaction for 6 hours at the temperature of 80 ℃. The solid material after the hydrothermal reaction was taken out and dried to a powder at 88 ℃ in a rotary evaporator to be used as a sample C. Placing the sample C in a tube furnace for two-section roasting: the oxidizing atmosphere used in the first stage of roasting is oxygen (nitrogen is used as balance gas) with the volume percentage of 7 percent, the roasting temperature is 750 ℃, and the roasting time is 2 hours; the second stage of the calcination process used a reducing atmosphere of 3% by volume hydrogen (nitrogen as the balance gas), the calcination temperature was 800 ℃, the calcination time was 0.5h, as sample D. Uniformly mixing the sample D and commercial alumina according to the mass ratio of 1:4, soaking the mixture with absolute ethyl alcohol in the same volume, then placing the mixture into a plasma reactor, and carrying out pure CO reaction 2 Reacting for 13min in the plasma atmosphere to obtain the oil-water separation adsorbent.
The deoiling performance of the adsorbent is tested by adopting an oil-water mixture with the oil content of 25g/L, and the deoiling efficiency in a liquid phase reaches 100% after 42min, which shows that the adsorbent has an obvious effect on separating the oil-water mixture.
And (3) thermally blowing the used adsorbent at 450 ℃ for 10min under the atmosphere of nitrogen or carbon dioxide to realize the separation of the adsorbed oily substances from the adsorbent.
Example 6
Stirring and uniformly mixing absolute ethyl alcohol and N, N-dimethylformamide according to a mass ratio of 3.5. Ferrous chloride is added into the solution A according to the mass ratio of 1:8, and ultrasonic stirring is carried out for 2 hours at the temperature of 45 ℃ to obtain a mixed solution B. Pouring the mixed solution B into a high-pressure reaction kettle, adding the mixed solution B into the high-pressure reaction kettle with the volume being 1/5 of the maximum volume in the kettle, and placing the high-pressure reaction kettle in an air-blast drying oven for hydrothermal reaction for 6.5 hours at the temperature of 98 ℃. The solid material after the hydrothermal reaction was taken out and dried to a powder form at 85 ℃ in a rotary evaporator as sample C. Placing the sample C in a tube furnace for two-section roasting: the oxidizing atmosphere used in the first stage of roasting is oxygen (nitrogen is used as balance gas) with the volume percentage of 10 percent, the roasting temperature is 700 ℃, and the roasting time is 2.5 hours; the second stage of the calcination process used a reducing atmosphere of 3% by volume hydrogen (nitrogen as the balance gas), the calcination temperature was 720 ℃ and the calcination time was 0.7h, as sample D. Will be sampledUniformly mixing the product D with commercial alumina according to the mass ratio of 1 2 Reacting for 20min in the plasma atmosphere to obtain the oil-water separation adsorbent.
The deoiling performance of the adsorbent is tested by adopting an oil-water mixture with the oil content of 21g/L, and the deoiling efficiency in a liquid phase reaches 100% after 36min, which shows that the adsorbent has an obvious effect on separating the oil-water mixture.
And (3) thermally blowing the used adsorbent at 350 ℃ for 10min under the atmosphere of carbon dioxide to realize the separation of the adsorbed oily substances from the adsorbent.
Example 7
Stirring and uniformly mixing absolute ethyl alcohol and N, N-dimethylformamide according to a mass ratio of 2.5. Ferrous nitrate is added into the solution A according to the mass ratio of 1:6, and ultrasonic stirring is carried out for 1.5h at 50 ℃ to obtain a mixed solution B. And pouring the mixed solution B into a high-pressure reaction kettle, adding the mixed solution B into the high-pressure reaction kettle, wherein the volume of the mixed solution B is 1/4 of the maximum volume in the kettle, and placing the high-pressure reaction kettle in an air-blowing drying oven for hydrothermal reaction for 8 hours at 82 ℃. The solid material after the hydrothermal reaction was taken out and dried to a powder form at 83 ℃ in a rotary evaporator as sample C. Placing the sample C in a tube furnace for two-section roasting: the oxidizing atmosphere used in the first stage of roasting is 8 percent by volume of oxygen (nitrogen is used as balance gas), the roasting temperature is 760 ℃, and the roasting time is 2 hours; the second stage of calcination uses 2 vol% hydrogen (nitrogen as balance gas) as reducing atmosphere, the calcination temperature is 850 deg.C, and the calcination time is 0.8h, as sample D. And uniformly mixing the sample D with commercial alumina according to a mass ratio of 1.
The deoiling performance of the adsorbent is tested by adopting an oil-water mixture with the oil content of 9g/L, and the deoiling efficiency in a liquid phase reaches 100% after 16min, which shows that the adsorbent has an obvious effect on separating the oil-water mixture.
And (3) thermally blowing the used adsorbent at 400 ℃ for 30min under the atmosphere of nitrogen or carbon dioxide to realize the separation of the adsorbed oily substances from the adsorbent.
Example 8
Anhydrous ethanol and N, N-dimethylformamide are stirred and mixed uniformly at room temperature according to the mass ratio of 2:1 to obtain a solution A. Ferrous nitrate is added into the solution A according to the mass ratio of 1:5, and ultrasonic stirring is carried out for 2 hours at the temperature of 55 ℃ to obtain a mixed solution B. And pouring the mixed solution B into a high-pressure reaction kettle, adding the mixed solution B into the high-pressure reaction kettle with the volume being 1/6 of the maximum volume in the kettle, and placing the high-pressure reaction kettle in an air-blast drying oven for hydrothermal reaction for 7 hours at the temperature of 95 ℃. The solid material after the hydrothermal reaction was taken out and dried to a powder at 88 ℃ in a rotary evaporator to be used as a sample C. Placing the sample C in a tube furnace for two-section roasting: the oxidizing atmosphere used in the first stage of roasting is oxygen (nitrogen is used as balance gas) with the volume percentage of 9 percent, the roasting temperature is 600 ℃, and the roasting time is 3.5 hours; the second stage of calcination uses 1 vol.% hydrogen (nitrogen as the balance gas) as the reducing atmosphere, the calcination temperature is 880 ℃, and the calcination time is 0.5h, which is taken as sample D. Uniformly mixing the sample D and commercial alumina according to the mass ratio of 1:3, soaking the mixture with absolute ethyl alcohol in the same volume, then placing the mixture into a plasma reactor, and carrying out pure CO reaction 2 Reacting for 15min in the plasma atmosphere to obtain the oil-water separation adsorbent.
The deoiling performance of the adsorbent is tested by adopting an oil-water mixture with the oil content of 30g/L, and the deoiling efficiency in a liquid phase reaches 100% after 70min, which shows that the adsorbent has an obvious effect on separating the oil-water mixture.
And (3) thermally blowing the used adsorbent at 450 ℃ for 25min under the atmosphere of carbon dioxide to realize the separation of the adsorbed oily substances from the adsorbent.
Example 9
Anhydrous ethanol and N, N-dimethylformamide are stirred and mixed uniformly at room temperature according to the mass ratio of 1:1 to obtain a solution A. Ferrous sulfate is added into the solution A according to the mass ratio of 1:7, and ultrasonic stirring is carried out for 1h at 50 ℃ to obtain a mixed solution B. Pouring the mixed solution B into a high-pressure reaction kettle, adding the mixed solution B into the high-pressure reaction kettle with the volume being 1/3 of the maximum volume in the kettle, and placing the mixture in an air-blast drying ovenThe hydrothermal reaction was carried out at 100 ℃ for 7h. The solid material after the hydrothermal reaction was taken out and dried to a powder form at 89 ℃ in a rotary evaporator as sample C. Placing the sample C in a tube furnace for two-section roasting: the oxidizing atmosphere used in the first stage of roasting is 6 volume percent of oxygen (nitrogen is used as balance gas), the roasting temperature is 650 ℃, and the roasting time is 3.5 hours; the second stage of the calcination process used a reducing atmosphere of 1% by volume hydrogen (nitrogen as the balance gas), the calcination temperature was 900 ℃ and the calcination time was 0.75h, as sample D. Uniformly mixing the sample D and commercial alumina according to the mass ratio of 1:2, soaking the mixture with absolute ethyl alcohol in the same volume, then placing the mixture into a plasma reactor, and carrying out pure CO reaction 2 Reacting for 9min in the plasma atmosphere to obtain the oil-water separation adsorbent.
The deoiling performance of the adsorbent is tested by adopting an oil-water mixture with the oil content of 13g/L, and the deoiling efficiency in a liquid phase reaches 100% after 23min, which shows that the adsorbent has an obvious effect on separating the oil-water mixture.
And (3) thermally blowing the used adsorbent at 500 ℃ for 30min under the atmosphere of nitrogen to realize the separation of the adsorbed oily substances from the adsorbent.
Example 10
Stirring and uniformly mixing absolute ethyl alcohol and N, N-dimethylformamide according to a mass ratio of 1.5 at normal temperature to obtain a solution A. Ferrous chloride is added into the solution A according to the mass ratio of 1:8, and ultrasonic stirring is carried out for 1.5h at 65 ℃ to obtain a mixed solution B. Pouring the mixed solution B into a high-pressure reaction kettle, adding the mixed solution B into the high-pressure reaction kettle with the volume being 1/3 of the maximum volume in the kettle, and placing the high-pressure reaction kettle in an air-blast drying oven for hydrothermal reaction for 7.5 hours at the temperature of 80 ℃. The solid material after the hydrothermal reaction was taken out and dried to a powder form at 82 ℃ in a rotary evaporator to obtain sample C. Placing the sample C in a tube furnace for two-section roasting: the oxidizing atmosphere used in the first stage of roasting is 5 volume percent of oxygen (nitrogen is used as balance gas), the roasting temperature is 800 ℃, and the roasting time is 3 hours; the second stage of calcination uses 2 vol% hydrogen (nitrogen as balance gas) as reducing atmosphere, the calcination temperature is 850 deg.C, and the calcination time is 0.65h, as sample D. And uniformly mixing the sample D and commercial alumina according to the mass ratio of 1.
The deoiling performance of the adsorbent is tested by adopting an oil-water mixture with the oil content of 13g/L, and the deoiling efficiency in a liquid phase reaches 100% after 17min, which shows that the adsorbent has an obvious effect on separating the oil-water mixture.
And (3) thermally blowing the used adsorbent at 350 ℃ for 15min under the atmosphere of carbon dioxide to separate the adsorbed oily substances from the adsorbent.
Example 11
Stirring and uniformly mixing absolute ethyl alcohol and N, N-dimethylformamide according to a mass ratio of 2.5. Ferrous nitrate is added into the solution A according to the mass ratio of 1:9, and ultrasonic stirring is carried out for 1h at the temperature of 60 ℃ to obtain a mixed solution B. And pouring the mixed solution B into a high-pressure reaction kettle, adding the mixed solution B into the high-pressure reaction kettle, wherein the volume of the mixed solution B is 1/4 of the maximum volume in the kettle, and placing the high-pressure reaction kettle in an air-blast drying oven for hydrothermal reaction for 8 hours at 85 ℃. The solid material after the hydrothermal reaction was taken out and dried to a powder form at 90 ℃ in a rotary evaporator to obtain sample C. Placing the sample C in a tube furnace for two-section roasting: the oxidizing atmosphere used in the first stage of roasting is 8 percent by volume of oxygen (nitrogen is used as balance gas), the roasting temperature is 700 ℃, and the roasting time is 4 hours; the second stage of calcination uses a reducing atmosphere of 3 vol% hydrogen (nitrogen as the balance gas), the calcination temperature is 750 ℃, and the calcination time is 1h, which is taken as sample D. And uniformly mixing the sample D with commercial alumina according to a mass ratio of 1:4, soaking the mixture with absolute ethyl alcohol in the same volume, placing the mixture into a plasma reactor, and reacting for 20min in a pure CO plasma atmosphere to obtain the oil-water separation adsorbent.
The deoiling performance of the adsorbent is tested by adopting an oil-water mixture with the oil content of 16g/L, and the deoiling efficiency in a liquid phase reaches 100% after 23min, which shows that the adsorbent has an obvious effect on separating the oil-water mixture.
And (3) thermally blowing the used adsorbent at 400 ℃ for 10min under the atmosphere of nitrogen or carbon dioxide to realize the separation of the adsorbed oily substances from the adsorbent.
The present application has been described in detail above, and specific examples thereof are used herein to explain the principles and implementations of the present application, which are presented solely to aid in understanding the present application and its core concepts. It should be noted that, for those skilled in the art, without departing from the principle of the present application, the present application can also make several improvements and modifications, and those improvements and modifications also fall into the protection scope of the claims of the present application.
Claims (8)
1. A preparation method of an adsorbent for oil-water separation is characterized by comprising the following steps:
(1) Preparation of solution a: stirring and mixing anhydrous ethanol and N, N-dimethylformamide uniformly at normal temperature according to a certain mass ratio to obtain a solution A;
(2) Preparation of solution B: adding an iron salt precursor into the solution A according to a certain mass ratio, and ultrasonically stirring for 1-2 h at a certain temperature to obtain a solution B;
(3) Hydrothermal reaction: transferring the solution B into a high-pressure reaction kettle, and placing the solution B into a forced air drying oven to perform hydrothermal reaction for 6-8 h at a certain temperature;
(4) Preparation of sample C: taking out the solid matter after the hydrothermal reaction, and drying the solid matter in a rotary evaporator to obtain a sample C;
(5) Preparation of sample D: placing the sample C in a tubular furnace for sectional roasting to obtain a sample D;
(6) And uniformly mixing the sample D and commercially available alumina according to a certain mass ratio, soaking the sample D and absolute ethyl alcohol in the same volume, then placing the mixture into a plasma reactor, and reacting in a plasma atmosphere to obtain the oil-water separation adsorbent.
2. The method for preparing the adsorbent for oil-water separation according to claim 1, wherein the mass ratio of the absolute ethanol to the N, N-dimethylformamide in the step (1) is 5:1 to 1:1.
3. The preparation method of the adsorbent for oil-water separation according to claim 1, wherein the mass ratio of the iron salt precursor to the solution A in the step (2) is 1:5-1, and the stirring temperature is 40-70 ℃; the ferric salt precursor is ferrous nitrate, ferrous sulfate or ferrous chloride.
4. The method for preparing the adsorbent for oil-water separation according to claim 1, wherein the volume of the solution B added into the high-pressure reaction kettle in the step (3) is 1/6 to 1/3 of the maximum volume of the reaction kettle; the hydrothermal temperature in the air-blast drying oven is kept between 80 and 100 ℃.
5. The method for preparing the adsorbent for oil-water separation according to claim 1, wherein the temperature of the rotary evaporator in the step (4) is 80 to 90 ℃.
6. The method for preparing the adsorbent for oil-water separation according to claim 1, wherein the step (5) of the step of calcining in a staged manner comprises a first stage and a second stage, wherein the first stage is an oxidation process and the second stage is a reduction process.
7. The preparation method of the adsorbent for oil-water separation according to claim 6, wherein the oxidizing atmosphere used in the first stage of calcination is 5-10 vol% oxygen, nitrogen is used as balance gas, the calcination temperature is 600-800 ℃, and the calcination time is 2-4 h; the reducing atmosphere used in the second stage of roasting is 1-3% of hydrogen by volume percentage, nitrogen is used as balance gas, the roasting temperature is 700-900 ℃, and the roasting time is 0.5-1 h.
8. The method for preparing the adsorbent for oil-water separation according to claim 1, wherein the mass ratio of the sample D and the commercial alumina in the step (6) is 1:2-1:4; the reaction atmosphere in the plasma reactor is pure CO gas or pure CO 2 The reaction time of gas and plasma is 5-20 min.
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