CN108992972B - On-demand oil-water separation column biomass filler and preparation method thereof - Google Patents
On-demand oil-water separation column biomass filler and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of chemical separation, relates to a biomass separation column filler, and particularly relates to an oil-water separation column biomass filler on demand and a preparation method thereof. The filler is porous biomass with controllable wettability; the filler is in an ellipse-like cage structure with a major axis of 19-25 μm and a minor axis of 15-22 μm, and the pores among the fillers are 2-30 μm. And filling the filler into a glass tube or a plastic tube with the diameter of 2-15 cm, wherein the filling height is 1-10 cm, and two ends of the separation column are fixed by a metal net or a gauze with the mesh size of more than 200. The invention also discloses a preparation method of the filler. The biomass resource used by the invention is pollen, has wide and renewable sources, has a stable special cage-shaped structure, and has the advantages of low price, safety, environmental protection and the like. The filler has the advantages of wetting adjustability, realization of separation of water-in-oil emulsion and oil-in-water emulsion as required, simple and convenient operation of the preparation method, simple preparation process equipment and wide application range.
Description
Technical Field
The invention belongs to the technical field of chemical separation, relates to a biomass separation column filler, and particularly relates to an oil-water separation column biomass filler on demand and a preparation method thereof.
Technical Field
In recent years, oil pollution leakage is frequent due to the increasing production activities related to the petroleum industry worldwide, and oil-water separation has become a global problem and challenge. The emulsion, especially the emulsion with stable surface activity, has stable structure and is difficult to separate, thus becoming the difficulty of oil-water separation at present. At present, two-dimensional separation membrane materials with fixed wettability are the main route for emulsion separation. A two-dimensional membrane with a fixed wettability can absorb or penetrate the aqueous phase (or oil phase) and repel the oil phase (or aqueous phase) in an emulsion, but can only separate a specific one of them when facing both water-in-oil and oil-in-water emulsions. Meanwhile, the two-dimensional membrane needs a specific small pore structure in order to be able to separate the emulsion, and the small pore structure is easy to cause pollution and blockage of the two-dimensional membrane. Therefore, there is a need for a separation material that is capable of separating multiple types of emulsions and has a large pore size.
The separation column with the three-dimensional structure has the unique advantage of avoiding the limitation of small pore diameter, and simultaneously can realize the separation of water-in-oil and oil-in-water emulsions according to the requirement by filling the filler with controllable wetting property, thereby achieving the aim of completely separating the emulsions.
The pollen is a biomass material with low cost, environmental protection, regeneration and rich sources. Meanwhile, the carbonized pollen has an ellipse-like cage-shaped porous structure, and through random accumulation, a high-tortuosity pore channel can be formed, so that the contact area of emulsion liquid drops and the filler is increased, and the separation efficiency is improved. More importantly, reversible conversion of the pollen between super-hydrophobic/underwater super-oleophilic property and underwater super-oleophobic/oily super-hydrophilic property can be realized by regulating and controlling the content of oxygen-containing groups on the surface of the pollen. Therefore, the pollen-filled separation column is a very ideal emulsion separation material.
The invention takes pollen as the filling material of the packed column, and constructs the emulsion separation packed column with the reversible adjustment of the wetting property. When the water-in-oil emulsion is separated, the water drop in the emulsion can be selectively absorbed by the filling column filled with the underwater super-oleophobic/oily super-hydrophilic pollen, so that the water-in-oil emulsion separation is realized; when the oil-in-water emulsion is separated, the filling column filled with the super-hydrophobic/underwater super-oleophylic pollen can selectively absorb oil drops in the oil-in-water emulsion, so that the aim of separating the oil-in-water emulsion is fulfilled. The method has the advantages of simple equipment, convenience and quickness in operation and high separation efficiency, and has a good application prospect in treatment of various emulsions.
Disclosure of Invention
The invention aims to provide an on-demand oil-water separation column filler and a preparation method thereof. The material has wide source, stable structure and reversible regulation and control of wettability, and the filled packed column can realize the separation of various emulsions according to requirements and realize the efficient separation of various emulsions.
The technical scheme is as follows:
an on-demand oil-water separation column filler, which is porous biomass with controllable wettability; the filler is in an ellipse-like cage structure with a major axis of 19-25 μm and a minor axis of 15-22 μm, and the pores among the fillers are 2-30 μm.
Further, the filler is filled in a glass tube or a plastic tube with the diameter of 2-15 cm, the filling height is 1-10 cm, and two ends of the separation column are fixed by a metal net or a gauze with the mesh size of more than 200.
After the biomass filler is subjected to oxygen-isolated calcination, the contact angle of a water drop is 152-157 degrees, and the contact angle of an underwater oil drop is 0 degree; after high-temperature steam modification, the contact angle of the underwater oil drops is 154-162 degrees, and the contact angle of the underwater oil drops is 0 degree; the reversible regulation and control of the wettability of the biomass filler are realized by alternately carrying out oxygen-insulating calcination and high-temperature steam modification, so that the aim of separating an oil-water mixture as required is fulfilled.
The preparation method of the oil-water separation column filler on demand comprises the following steps:
a) removing impurities of the biomass filler: crushing the biomass filler, adding 20-50 mL of organic solvent into each gram of biomass filler, soaking the biomass filler in the organic solvent for 2-24 hours at 30-80 ℃, filtering, washing with ethanol and water for 2-4 times respectively, drying at 40-80 ℃ for 5-10 hours, and repeating the soaking, washing and drying processes for 2-4 times to obtain the biomass filler without organic impurities;
b) adding 10-30 mL of 0.05-0.2M acid solution into each gram of biomass filler without organic impurities, soaking for 2-12 h at 25-50 ℃, filtering, washing for 2-4 times, and drying for 6-12 h at 50-80 ℃ to obtain the biomass filler without impurities;
c) oxygen-isolated calcination: according to the method, the biomass filler with impurities removed is placed in a tubular furnace according to the nitrogen gas introduction flow of 2-50 sccm per gram of biomass filler, and the biomass filler is reacted for 1-3 hours at the temperature of 600-900 ℃ to obtain the super-hydrophobic/underwater super-oleophilic biomass filler;
d) high-temperature steam modification: and (3) reacting for 2-5 h at 100-125 ℃ according to the weight of 0.2-2 mL of deionized water added into each gram of biomass filler to obtain the biomass filler with underwater super oleophobic/oily super hydrophilic property.
In a preferred embodiment of the invention, the biomass filler in the step a) is pollen, specifically one or a mixture of more of rape pollen, sunflower pollen, watermelon pollen, pine pollen, plum blossom pollen, acacia pollen, senna pollen and the like in any proportion; the organic solvent is one or more of ethanol, benzene, toluene, acetone, tetrahydrofuran, dichloromethane, trichloromethane, gasoline, carbon tetrachloride, n-hexane and the like which are mixed in any proportion.
In the preferred embodiment of the present invention, the acid in step b) is any one of hydrochloric acid, acetic acid, nitric acid, sulfuric acid, hypochlorous acid, and the like.
In a better disclosed example of the invention, the biomass filler in the step c) is the biomass filler obtained in the step b) and subjected to impurity removal or the underwater super-oleophobic/oily super-hydrophilic biomass filler obtained in the step d).
In a better disclosure example of the invention, the biomass filler in the step d) is the biomass filler obtained in the step b) and impurities are removed or the super-hydrophobic/underwater super-oleophilic biomass filler obtained in the step c).
Advantageous effects
The invention discloses an on-demand oil-water separation column filler which has the advantages of wide source, stable structure and reversible regulation and control of wettability, and the filled filler column can realize on-demand separation of various emulsions and realize high-efficiency separation of the various emulsions. The pollen used in the invention is a biomass resource, has wide sources and can be regenerated, and the special cage-shaped structure is stable, thus having the advantages of low price, safety, environmental protection and the like; the packing of the packed column has wetting adjustability, realizes the separation of water-in-oil and oil-in-water emulsions according to the requirements, and has the advantages of simple and convenient operation, simple equipment and wide application range; the packing of the packed column is randomly stacked to form a pore channel structure with high tortuosity, so that the contact area of the packing and the wetting packing is increased, and the emulsion separation efficiency of the packed column is improved.
Drawings
FIG. 1 is an SEM image of the packing for the on-demand oil-water separation column prepared by the invention.
Detailed Description
The present invention will be described in detail below with reference to examples to enable those skilled in the art to better understand the present invention, but the present invention is not limited to the following examples.
Example 1
A preparation method of an on-demand oil-water separation column filler comprises the following steps:
a) pulverizing rape pollen, adding 20mL ethanol per gram of pollen, soaking rape pollen in ethanol at 50 deg.C for 8 hr, repeating the soaking process for 4 times, filtering, washing with ethanol and water for 4 times, and drying at 50 deg.C for 10 hr to obtain rape pollen without organic impurities. Adding 20mL of 0.1M hydrochloric acid solution into per gram of organic impurity-removed rape pollen, soaking at 25 deg.C for 12h, filtering, washing with water for 3 times, and drying at 50 deg.C for 12h to obtain impurity-removed rape pollen;
b) introducing 10sccm nitrogen gas into per gram of rape pollen, placing the rape pollen without impurities in a tubular furnace, and reacting for 1h at 600 ℃ to obtain super-hydrophobic/underwater super-lipophilic rape pollen;
c) adding 1mL of deionized water into per gram of rape pollen, and reacting at 100 ℃ for 5h to obtain the rape pollen with underwater super-oleophobic/oily super-hydrophilic property.
And c, filling the super-hydrophobic/underwater super-lipophilic rape pollen obtained in the step b into a glass tube with the diameter of 2cm, wherein the filling height is 5cm, two ends of the rape pollen are fixed by using a 200-mesh metal net, and the filling column can realize the separation of water-in-oil emulsion.
And c, filling the underwater super-oleophobic/oily super-hydrophilic rape pollen obtained in the step c into a glass tube with the diameter of 2cm, wherein the filling height is 5cm, two ends of the glass tube are fixed by using a 200-mesh metal net, and the filling column can realize the separation of the oil-in-water emulsion.
Example 2
A preparation method of an on-demand oil-water separation column filler comprises the following steps:
a) pulverizing the robinia pseudoacacia flower powder, adding 30mL of toluene into each gram of pollen, soaking the robinia pseudoacacia flower powder in the toluene for 8h at 50 ℃, repeating the soaking process for 2 times, filtering, washing with ethanol and water for 4 times respectively, and drying at 60 ℃ for 8h to obtain the robinia pseudoacacia flower powder without organic impurities. Adding 20mL of 0.1M acetic acid solution into per gram of the black locust flower powder without organic impurities, soaking at 30 ℃ for 10h, filtering, washing with water for 3 times, and drying at 50 ℃ for 12h to obtain the black locust flower powder without impurities;
b) according to the flow of introducing 15sccm nitrogen gas into per gram of the robinia pseudoacacia powder, placing the robinia pseudoacacia powder without impurities in a tubular furnace, and reacting for 1h at 900 ℃ to obtain the robinia pseudoacacia powder with super-hydrophobicity/super-lipophilicity under water;
c) adding 1mL of deionized water into per gram of the robinia pseudoacacia flower powder, and reacting for 5h at 100 ℃ to obtain the robinia pseudoacacia flower powder with underwater super-oleophobic/oily super-hydrophilic property.
And c, filling the super-hydrophobic/underwater super-lipophilic robinia pseudoacacia flower powder obtained in the step b into a glass tube with the diameter of 5cm, wherein the filling height is 3cm, two ends of the glass tube are fixed by using a 300-mesh metal net, and the filling column can realize the separation of water-in-oil emulsion.
And c, filling the underwater super-oleophobic/oily super-hydrophilic robinia pseudoacacia flower powder obtained in the step c into a glass tube with the diameter of 5cm, wherein the filling height is 3cm, two ends of the glass tube are fixed by using a 300-mesh metal net, and the filling column can realize the separation of oil-in-water emulsions.
Example 3
A preparation method of an on-demand oil-water separation column filler comprises the following steps:
a) pulverizing flos Dendrobii pollen, adding 30mL chloroform per gram pollen, soaking in chloroform at 60 deg.C for 24h, repeating the soaking process for 3 times, filtering, washing with ethanol and water for 3 times, and drying at 40 deg.C for 7h to obtain flos Dendrobii pollen without organic impurities. Adding 10mL of 0.05M nitric acid solution into per gram of the foreign substance-removed powder, soaking at 50 deg.C for 5h, filtering, washing with water for 3 times, and drying at 80 deg.C for 12h to obtain foreign substance-removed powder;
b) introducing 50sccm nitrogen gas per gram of the powder, placing the powder in a tubular furnace, and reacting at 800 deg.C for 1h to obtain super-hydrophobic/underwater super-lipophilic powder;
c) adding 1mL of deionized water into per gram of the ocean tree pollen, and reacting at 125 ℃ for 2h to obtain the ocean tree pollen with underwater super oleophobic/oily super hydrophilic property.
And c, filling the super-hydrophobic/underwater super-lipophilic sea tree pollen obtained in the step b into a plastic pipe with the diameter of 8cm, wherein the filling height is 6cm, two ends of the sea tree pollen are fixed by using 300-mesh gauze, and the filling column can realize the separation of water-in-oil emulsion.
And c, filling the underwater super-oleophobic/oily super-hydrophilic foreign tree pollen obtained in the step c into a plastic pipe with the diameter of 8cm, wherein the filling height is 6cm, two ends of the foreign tree pollen are fixed by using a 300-mesh gauze, and the packed column can realize the separation of oil-in-water emulsions.
Example 4
A preparation method of an on-demand oil-water separation column filler comprises the following steps:
a) crushing the plum blossom pollen, adding 40mL of acetone into each gram of pollen, soaking the plum blossom pollen in chloroform at 80 ℃ for 12h, repeating the soaking process for 2 times, filtering, washing with ethanol and water for 2 times respectively, and drying at 80 ℃ for 10h to obtain the plum blossom pollen without organic impurities. Adding 30mL of 0.1M sulfuric acid solution into each gram of plum blossom pollen without organic impurities, soaking at 25 ℃ for 2h, filtering, washing with water for 3 times, and drying at 60 ℃ for 6h to obtain the plum blossom pollen without the impurities;
b) according to the method, per gram of plum blossom pollen, introducing nitrogen gas with the flow of 2sccm, placing the plum blossom pollen without impurities in a tubular furnace, and reacting for 2 hours at 700 ℃ to obtain super-hydrophobic/underwater super-lipophilic plum blossom pollen;
c) according to the method, 0.2mL of deionized water is added into each gram of plum blossom pollen, and the reaction is carried out for 3h at 110 ℃ to obtain the plum blossom pollen with underwater super-oleophobic/oily super-hydrophilic property.
And c, filling the super-hydrophobic/underwater super-lipophilic plum blossom pollen obtained in the step b into a plastic pipe with the diameter of 10cm, wherein the filling height is 8cm, two ends of the plum blossom pollen are fixed by using a 300-mesh metal net, and the filling column can realize the separation of water-in-oil emulsion.
And c, filling the underwater super-oleophobic/oily super-hydrophilic plum blossom pollen obtained in the step c into a plastic pipe with the diameter of 10cm, wherein the filling height is 8cm, two ends of the plastic pipe are fixed by using a 300-mesh metal net, and the packed column can realize the separation of the oil-in-water emulsion.
Example 5
A preparation method of an on-demand oil-water separation column filler comprises the following steps:
a) pulverizing watermelon pollen, adding 50mL of dichloromethane into per gram of pollen, soaking in chloroform at 30 deg.C for 8h, repeating the soaking process for 2 times, filtering, washing with ethanol and water for 4 times, and drying at 60 deg.C for 8h to obtain watermelon pollen without organic impurities. Adding 20mL of 0.2M sulfuric acid solution into per gram of watermelon pollen without organic impurities, soaking at 35 deg.C for 12h, filtering, washing with water for 3 times, and drying at 50 deg.C for 12h to obtain watermelon pollen without impurities;
b) introducing nitrogen gas with the flow of 30sccm into per gram of watermelon pollen, placing the watermelon pollen without impurities in a tubular furnace, and reacting for 3h at 600 ℃ to obtain the watermelon pollen with super hydrophobicity/underwater super lipophilicity;
c) adding 2mL of deionized water into per gram of watermelon pollen, and reacting at 115 deg.C for 3h to obtain watermelon pollen with super oleophobic/super hydrophilic property under water and oil.
And c, filling the super-hydrophobic/underwater super-lipophilic watermelon pollen obtained in the step b into a glass tube with the diameter of 15cm, wherein the filling height is 10cm, two ends of the watermelon pollen are fixed by using a 400-mesh metal net, and the filling column can realize the separation of water-in-oil emulsion.
And c, filling the underwater super-oleophobic/oily super-hydrophilic watermelon pollen obtained in the step c into a glass tube with the diameter of 15cm, wherein the filling height is 10cm, two ends of the watermelon pollen are fixed by using a 400-mesh metal net, and the packed column can realize the separation of oil-in-water emulsions.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present invention or directly or indirectly applied to other related technical fields are included in the scope of the present invention.
Claims (9)
1. The preparation method of the on-demand oil-water separation column filler is characterized by comprising the following steps of:
a) crushing the biomass filler, adding 20-50 mL of organic solvent into each gram of biomass filler, soaking the biomass filler in the organic solvent for 2-24 hours at 30-80 ℃, filtering, washing with ethanol and water for 2-4 times respectively, drying at 40-80 ℃ for 5-10 hours, and repeating the soaking, washing and drying processes for 2-4 times to obtain the biomass filler without organic impurities;
b) adding 10-30 mL of 0.05-0.2M acid solution into each gram of biomass filler without organic impurities, soaking for 2-12 h at 25-50 ℃, filtering, washing for 2-4 times, and drying for 6-12 h at 50-80 ℃ to obtain the biomass filler without impurities;
c) according to the method, the biomass filler with impurities removed is placed in a tubular furnace according to the nitrogen gas introduction flow of 2-50 sccm per gram of biomass filler, and the biomass filler is reacted for 1-3 hours at the temperature of 600-900 ℃ to obtain the super-hydrophobic/underwater super-oleophilic biomass filler;
d) and (3) reacting for 2-5 h at 100-125 ℃ according to the weight of 0.2-2 mL of deionized water added into each gram of biomass filler to obtain the biomass filler with underwater super oleophobic/oily super hydrophilic property.
2. The method for preparing the packing for an on-demand oil-water separation column according to claim 1, wherein: the biomass filler in the step a) is pollen.
3. The method for preparing the packing for an on-demand oil-water separation column according to claim 1, wherein: the organic solvent in the step a) is one or more of ethanol, benzene, toluene, acetone, tetrahydrofuran, dichloromethane, trichloromethane, gasoline, carbon tetrachloride and n-hexane which are mixed in any proportion.
4. The method for preparing the packing for an on-demand oil-water separation column according to claim 1, wherein: the acid in the step b) is any one of hydrochloric acid, acetic acid, nitric acid, sulfuric acid and hypochlorous acid.
5. The method for preparing the packing for an on-demand oil-water separation column according to claim 1, wherein: the biomass filler obtained in the step c) is the biomass filler obtained in the step b) and subjected to impurity removal or the underwater super-oleophobic/oily super-hydrophilic biomass filler obtained in the step d).
6. The method for preparing the packing for an on-demand oil-water separation column according to claim 1, wherein: the biomass filler obtained in the step d) is the biomass filler obtained in the step b) and subjected to impurity removal or the super-hydrophobic/underwater super-oleophilic biomass filler obtained in the step c).
7. An on-demand oil-water separation column packing prepared by the method of any one of claims 1-6, which is porous biomass with controllable wettability, and is characterized in that: the filler has a long axis of 19-25 mu m, a short axis of 15-22 mu m, an elliptical cage-like structure, and pores between the fillers of 2-30 mu m.
8. The on-demand oil-water separation column packing of claim 7, wherein: and filling the filler into a glass tube or a plastic tube with the diameter of 2-15 cm, wherein the filling height is 1-10 cm, and two ends of the separation column are fixed by a metal net or a gauze with the mesh size of more than 200.
9. The on-demand oil-water separation column packing of claim 7, wherein: after the filler is subjected to oxygen-insulating calcination, the contact angle of a water drop is 152-157 degrees, and the contact angle of an underwater oil drop is 0 degree; after high-temperature steam modification, the contact angle of the underwater oil drops is 154-162 degrees, and the contact angle of the underwater oil drops is 0 degree.
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| CN110237567B (en) * | 2019-05-19 | 2021-08-31 | 天津大学 | Super-hydrophobic filler based on 3D printing, preparation method thereof and application thereof in oil-water emulsion separation |
| CN110548312A (en) * | 2019-08-26 | 2019-12-10 | 江苏大学 | method for separating water-in-oil or oil-in-water emulsion by using fly ash |
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| CN103945924A (en) * | 2011-09-28 | 2014-07-23 | 阿卜杜拉国王科技大学 | Grafted membranes and substrates having surfaces with switchable superoleophilicity and superoleophobicity and applications thereof |
| CN107540866A (en) * | 2017-09-07 | 2018-01-05 | 哈尔滨工业大学 | A kind of method that surface wettability regulation and control are carried out using PDPAEMA embellishment shapes memory polymer |
| CN107998687A (en) * | 2017-12-08 | 2018-05-08 | 刘丁菡 | A kind of preparation method of intelligent water-oil separating material |
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2018
- 2018-07-23 CN CN201810809122.3A patent/CN108992972B/en active Active
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| CA995171A (en) * | 1971-02-16 | 1976-08-17 | Kewanee Oil Company | Removal of hydrocoumaric acid from acid nickel plating baths containing coumarin |
| CN103945924A (en) * | 2011-09-28 | 2014-07-23 | 阿卜杜拉国王科技大学 | Grafted membranes and substrates having surfaces with switchable superoleophilicity and superoleophobicity and applications thereof |
| CN107540866A (en) * | 2017-09-07 | 2018-01-05 | 哈尔滨工业大学 | A kind of method that surface wettability regulation and control are carried out using PDPAEMA embellishment shapes memory polymer |
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