CN116119796A - Ferroferric oxide nano-composite adsorption flocculant and preparation method thereof - Google Patents
Ferroferric oxide nano-composite adsorption flocculant and preparation method thereof Download PDFInfo
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Abstract
The invention provides a ferroferric oxide nano-composite adsorption flocculant and a preparation method thereof, belonging to the technical field of functional nano-materials. The invention is implemented by mixing Fe 3 O 4 The nano particles are directly copolymerized and grafted with N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxy silane (KH-602) and N- (beta-aminoethyl) -gamma-aminopropyl trimethoxy silane (KH-792). Fe according to the invention 3 O 4 The nano composite adsorption flocculant has the advantages of simple preparation condition, low cost, easy batch preparation and repeated use, can realize the efficient demulsification of the ternary composite flooding oil extraction sewage, can simultaneously remove polymers, anionic surfactants and the like in the sewage, and has wide application prospect.
Description
Technical Field
The invention belongs to the technical field of functional nano materials, and particularly relates to a ferroferric oxide nano composite adsorption flocculant and a preparation method thereof.
Background
Currently, to improve the recovery ratio of crude oil, the oil field mainly adopts a ternary compound flooding oil extraction technology. However, the technology can inevitably generate a large amount of ternary complex oil displacement sewage while improving the crude oil production amount. The sewage generally contains a large amount of emulsified crude oil, polymer, surfactant, strong alkali and inorganic salt metal ions, and the generated sewage can cause serious environmental damage if the sewage is directly discharged without treatment due to the extremely large oil-removing water quantity. However, the synergistic effect of the polymer, the surfactant and the strong alkali in the oil displacement sewage ensures that the sewage has the characteristics of high viscosity, high emulsification degree, stability and difficult flocculation and sedimentation of mechanical impurities. Therefore, it is difficult to effectively treat such sewage with the conventional adsorption flocculant.
With ferroferric oxide (Fe) 3 O 4 ) The magnetic nano particles mainly have been widely applied to the water treatment fields such as dye adsorption and the like due to the advantages of superparamagnetism, large specific surface area, easy modification and greenness and no toxicity. In particular to superparamagnetism unique to ferroferric oxide, so that the water treatment agent prepared by taking the ferroferric oxide as a raw material can be effectively separated only through the action of an external magnetic field after adsorption treatment. The method not only facilitates the recovery of the adsorbent after use, but also provides an important premise for the desorption and recycling of the adsorption flocculant.
But because of Fe 3 O 4 Nanoparticles themselves have weak adsorption capacity and often require additional surface modification means to improve their adsorption of target contaminants. At present, a silane coupling agent represented by 3-aminopropyl triethoxysilane (APTES) is often used for surface modification of various inorganic oxides, and the principle is that amino functional groups are connected to the surface of a material to improve the original surface positive charge property of the material, so that the electrostatic adsorption capacity of target pollutants is enhanced. For example, patent CN201510176768.9 discloses an amino-functionalized magnetic silica-Fe 3 O 4 Composite nano material and preparation method thereof, wherein Fe is synthesized by coprecipitation method 3 O 4 Nanoparticles, then coating the silicon dioxide on Fe 3 O 4 The surface of the nano particle is used for improving the grafting amount of APTES, thereby strengthening Fe 3 O 4 Nanoparticle surface positive charge properties. But the method hasThe following disadvantages: 1) The magnetic nano particles prepared by the coprecipitation method have the defect of uneven particle size (5-35 nm), are easy to agglomerate, and therefore reduce Fe 3 O 4 The specific surface area of the nano particles is not beneficial to the grafting effect of APTES; 2) The silicon dioxide can hardly realize single particle coating in the coating process, so secondary coating agglomeration can occur in the coating process, which directly causes Fe 3 O 4 The specific surface area of the nano particles is reduced, so that the subsequent APTES grafting effect is further influenced; 3) Nonmagnetic silica coating weakens Fe 3 O 4 The magnetic induction intensity of the nano particles is unfavorable for rapid magnetic separation. Patent CN201910951801.9 discloses an amino-functionalized magnetic Fe 3 O 4 Nanoparticle and preparation method thereof, and method for synthesizing Fe by polyol method 3 O 4 The nanoparticles were grafted directly with APTES. Although the preparation method effectively solves the problems of particle agglomeration and silica weakening magnetism existing in the coprecipitation method, the preparation method also has the following defects: 1) APTES has only one primary amino group in the molecular chain, thus APTES functionalized Fe 3 O 4 The positive charge attribute of the surface of the nano particle is relatively weak; 2) Fe (Fe) 3 O 4 The nano particles need to be heated to 65-70 ℃ in the APTES grafting process, which is unfavorable for large-scale low-cost preparation in practical water treatment application; 3) Because of the existence of strong alkali in the ternary complex oil displacement sewage, the pH value of the water body is usually in the range of 8.3-9.7, but the amino functional Fe prepared by the method 3 O 4 The nano particles have lower positive charge intensity under alkaline condition, and finally influence the adsorption treatment capacity.
Therefore, it is highly desirable to provide Fe with a higher adsorption capacity 3 O 4 And (3) nano composite adsorption flocculant.
Disclosure of Invention
In order to overcome the defects, the invention provides a new Fe modified by a silane coupling agent 3 O 4 A nano composite adsorption flocculant and a preparation method thereof. Fe prepared by the method 3 O 4 The nano composite adsorption flocculant has the advantages of simple preparation condition, low cost, easy batch preparation and repeated useThe method has the advantages that the method not only can realize the efficient demulsification of the ternary composite flooding oil extraction sewage, but also can remove polymers, anionic surfactants and the like in the sewage at the same time, and has wide application prospect.
In order to achieve the above object, the present invention has the following technical scheme:
in one aspect, the invention provides a preparation method of a ferroferric oxide nano-composite adsorption flocculant, which comprises the following steps: by mixing Fe with 3 O 4 The nano particles are directly copolymerized and grafted with N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxy silane (KH-602) and N- (beta-aminoethyl) -gamma-aminopropyl trimethoxy silane (KH-792).
Specifically, the preparation method comprises the following steps:
1) Adding ferric trichloride, sodium hydroxide and deionized water into ethylene glycol, stirring and mixing uniformly, heating to boiling, condensing and refluxing, cooling, separating and washing to obtain ferroferric oxide nano particles with the particle size distribution of 20-40 nm;
2) Dispersing the ferroferric oxide nano particles prepared in the step 1) into deionized water, adding N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxy silane (KH-602) and N- (beta-aminoethyl) -gamma-aminopropyl trimethoxy silane (KH-792), regulating the pH value of the mixed solution to 5-7, mechanically stirring, separating, washing and freeze-drying to obtain Fe 3 O 4 And (3) nano composite adsorption flocculant.
Further specifically, the ratio of the amounts of the substances of ferric trichloride, sodium hydroxide, deionized water and ethylene glycol in the step 1) is 1-5:1-10:10-50:30-150, preferably 1:3:20:100.
further specifically, the ferric trichloride may be anhydrous ferric trichloride or ferric trichloride hexahydrate.
Further specifically, the heating rate of the heating in the step 1) is 5-15 ℃/min.
Further specifically, the condensation reflux time described in step 1) is 4 to 6 hours.
Further specifically, the ratio of the amounts of the substances of the ferroferric oxide nanoparticles, KH-602, KH-792 described in step 2) is 1-10:1-20:1-15, preferably 2:1:1.
further specifically, the pH of the mixture in step 2) is 6.
Further specifically, the mechanical stirring speed in step 2) is 300-600rad/s and the mechanical stirring time is 6-12h.
On the other hand, the invention provides a ferroferric oxide nano-composite adsorption flocculant, which is obtained by the preparation method.
In still another aspect, the invention provides application of the ferroferric oxide nano-composite adsorption flocculant in ternary composite displacement oil wastewater removal.
In still another aspect, the invention provides a method for removing ternary composite displacement oil wastewater, the method comprising the following steps: fe prepared by the method 3 O 4 The nano composite adsorption flocculant is added into the oil displacement sewage, and after stirring or oscillating, the mixture is separated by a magnet, and the supernatant is taken out for detection after the magnet is separated.
Specifically, the stirring or oscillating time is 6-12h, and the magnetic separation time of the magnet is 0.5-2h.
Specifically, the method further comprises the following steps: magnetically separating Fe 3 O 4 Re-dispersing the nano composite adsorption flocculant into water, regulating the pH value of the dispersion liquid to 10-11, and separating Fe by using a magnet after ultrasonic treatment 3 O 4 The nano composite adsorption flocculant is repeatedly used for washing and separating for 2-5 times, and then Fe separated magnetically 3 O 4 Freeze drying the nano composite adsorption flocculant to obtain reusable Fe 3 O 4 And (3) nano composite adsorption flocculant.
Further specifically, the dispersion had a pH of 10.5 and the number of repeated washing separations was 3.
Compared with the prior art, the invention has the following positive and beneficial effects:
(1) Fe prepared by the method 3 O 4 Nano composite adsorption flocculationThe agent effectively enhances the positive charge quantity on the surface of the agent, and can simultaneously realize the functions of demulsification of ternary complex oil displacement sewage and removal of polymer and anionic surfactant.
2) Fe prepared by the method 3 O 4 The nano composite adsorption flocculant has good effect of removing the ternary composite oil displacement sewage under the alkaline condition, and meets the requirements of practical application.
3) Fe prepared by the method 3 O 4 The nano composite adsorption flocculant has the advantages of easily available raw materials, simple preparation method, low cost, environment friendliness and easiness in large-scale preparation and production, and the prepared Fe 3 O 4 The nano composite adsorption flocculant can be repeatedly used for a plurality of times, so that the nano composite adsorption flocculant has the advantage of low cost.
Drawings
Fig. 1 is a Transmission Electron Microscope (TEM) image of the ferroferric oxide nanoparticle in example 1.
FIG. 2 is Fe in example 1 3 O 4 Transmission Electron Microscopy (TEM) image of nanocomposite adsorbing flocculant.
Fig. 3 is a graph of the demulsification effect test results.
FIG. 4 is a graph showing HPAM adsorption results.
FIG. 5 is a graph showing HPAM adsorption results.
FIG. 6 is a graph showing the result of SDBS adsorption.
Fig. 7 is a graph of SDBS adsorption results.
FIG. 8 is a graph showing the effect of recycling and detecting the ternary complex flooding wastewater after repeated use for 5 times.
FIG. 9 is a schematic diagram of ternary complex flooding wastewater.
FIG. 10 is a diagram of Fe prepared in example 1 3 O 4 Schematic diagram of adsorption effect of nano composite adsorption flocculant.
FIG. 11 is Fe 3 O 4 Schematic of adsorption effectiveness of APTES (comparative example 1).
FIG. 12 is Fe 3 O 4 Schematic of adsorption effect of # APTES+KH602 (comparative example 2).
FIG. 13 is Fe 3 O 4 @APTES+KH792 (comparative example 3)Schematic of adsorption effect.
Detailed Description
The present invention will be described in further detail with reference to the following examples, which are not intended to limit the present invention, but are merely illustrative of the present invention. The experimental methods used in the following examples are not specifically described, but the experimental methods in which specific conditions are not specified in the examples are generally carried out under conventional conditions, and the materials, reagents, etc. used in the following examples are commercially available unless otherwise specified.
Example 1 Fe 3 O 4 Preparation method of nano composite adsorption flocculant
1) Adding ferric trichloride, sodium hydroxide and deionized water into ethylene glycol, and stirring and mixing uniformly. The mixture was heated to boiling at atmospheric pressure, then kept boiling and condensed at reflux. After cooling, separating and washing to obtain the ferroferric oxide nano particles with the particle size distribution of 20-40 nm. The mass ratio of the substances of the added ferric trichloride, sodium hydroxide, deionized water and ethylene glycol is controlled to be 1:3:20:100, the heating temperature rising rate is 10 ℃/min, and the condensing reflux time is 4h.
Fig. 1 is a Transmission Electron Microscope (TEM) photograph of the prepared ferroferric oxide nanoparticle, and it can be seen from the figure that the average size of the obtained nanoparticle is 20-40nm, the particle size is uniform, the size is moderate, the dispersibility is good, and the agglomeration is avoided.
2) Dispersing the obtained ferroferric oxide nano particles into deionized water, adding N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxy silane (KH-602) and N- (beta-aminoethyl) -gamma-aminopropyl trimethoxy silane (KH-792), regulating the pH value of the mixed solution to 6, mechanically stirring for 6h, separating, washing, and freeze-drying to obtain Fe 3 O 4 And (3) nano composite adsorption flocculant. The mass ratio of the substances of the ferroferric oxide nano particles, KH-602 and KH-792 is controlled to be 2:1:1, wherein the mechanical stirring rotating speed is 500rad/s.
FIG. 2 shows the Fe produced 3 O 4 Transmission Electron Microscope (TEM) photograph of nano composite adsorption flocculant, and the obtained Fe 3 O 4 Nanocomposite(s)The adsorption flocculant is uniformly coated, has a regular structure and has no secondary agglomeration phenomenon.
Comparative example 1. Fe 3 O 4 Preparation method of nano composite adsorption flocculant
1) Adding ferric trichloride, sodium hydroxide and deionized water into ethylene glycol, and stirring and mixing uniformly. The mixture was heated to boiling at atmospheric pressure, then kept boiling and condensed at reflux. After cooling, separating and washing to obtain the ferroferric oxide nano particles with the particle size distribution of 20-40 nm. The mass ratio of the substances of the added ferric trichloride, sodium hydroxide, deionized water and ethylene glycol is controlled to be 1:3:20:100, the heating temperature rising rate is 10 ℃/min, and the condensing reflux time is 4h.
2) Dispersing the obtained ferroferric oxide nano particles into deionized water, adding APTES, adjusting the pH value of the mixed solution to 6, mechanically stirring for 6h, separating, washing, and freeze-drying to obtain Fe 3 O 4 And (3) nano composite adsorption flocculant. The mass ratio of the ferroferric oxide nano particles to the APTES is controlled to be 1:1, wherein the mechanical stirring rotating speed is 500rad/s.
Comparative example 2. Fe 3 O 4 Preparation method of nano composite adsorption flocculant
1) Adding ferric trichloride, sodium hydroxide and deionized water into ethylene glycol, and stirring and mixing uniformly. The mixture was heated to boiling at atmospheric pressure, then kept boiling and condensed at reflux. After cooling, separating and washing to obtain the ferroferric oxide nano particles with the particle size distribution of 20-40 nm. The mass ratio of the substances of the added ferric trichloride, sodium hydroxide, deionized water and ethylene glycol is controlled to be 1:3:20:100, the heating temperature rising rate is 10 ℃/min, and the condensing reflux time is 4h.
2) Dispersing the obtained ferroferric oxide nano particles into deionized water, adding APTES and KH602, adjusting the pH value of the mixed solution to 6, mechanically stirring for 6h, separating, washing, and freeze-drying to obtain Fe 3 O 4 And (3) nano composite adsorption flocculant. The mass ratio of the ferroferric oxide nano particles, APTES and KH602 is controlled to be 2:1:1, the mechanical stirring is carried outThe speed was 500rad/s.
Comparative example 3A Fe 3 O 4 Preparation method of nano composite adsorption flocculant
1) Adding ferric trichloride, sodium hydroxide and deionized water into ethylene glycol, and stirring and mixing uniformly. The mixture was heated to boiling at atmospheric pressure, then kept boiling and condensed at reflux. After cooling, separating and washing to obtain the ferroferric oxide nano particles with the particle size distribution of 20-40 nm. The mass ratio of the substances of the added ferric trichloride, sodium hydroxide, deionized water and ethylene glycol is controlled to be 1:3:20:100, the heating temperature rising rate is 10 ℃/min, and the condensing reflux time is 4h.
2) Dispersing the obtained ferroferric oxide nano particles into deionized water, adding APTES and KH792, regulating the pH value of the mixed solution to 6, mechanically stirring for 6h, separating, washing, and freeze-drying to obtain Fe 3 O 4 And (3) nano composite adsorption flocculant. The mass ratio of the ferroferric oxide nano particles, APTES and KH792 is controlled to be 2:1:1, wherein the mechanical stirring rotating speed is 500rad/s.
Experimental example 1 demulsification test
And taking 12 parts of oil displacement sewage of an oil field, wherein each part is 5mL, and dividing the oil displacement sewage into 4 groups, and each group is respectively marked as A1-A3, B1-B3, C1-C3 and D1-D3. And respectively adjusting the pH value of the oil displacement sewage of each oil field to 7, 8 and 9 in each group. Then adding enough Fe into A, B, C, D group in turn 3 O 4 APTES (comparative example 1), fe 3 O 4 @APTES+KH602 (comparative example 2), fe 3 O 4 @APTES+KH792 (comparative example 3), fe 3 O 4 @AKH2+KH792 (example 1). After stirring or oscillating for 10min, separating by using a magnet for 1h, and taking out supernatant after the magnet separation for detection of demulsification rate.
The demulsification detection result is shown in FIG. 3, and as can be seen from FIG. 3, fe prepared by the method of the invention 3 O 4 The demulsification effect of the nano composite adsorption flocculant is obviously better than that of APTES amino functionalized ferroferric oxide nano particles.
Experimental example 2 HPAM removal detection
Taking 12 parts of oil displacement sewage of an oil field, 5mL each part,the groups are divided into 4 groups, and each group is respectively marked as A1-A3, B1-B3, C1-C3 and D1-D3. And respectively adjusting the pH value of the oil displacement sewage of each oil field to 7, 8 and 9 in each group. Then adding enough Fe into A, B, C, D group in turn 3 O 4 APTES (comparative example 1), fe 3 O 4 @APTES+KH602 (comparative example 2), fe 3 O 4 @APTES+KH792 (comparative example 3), fe 3 O 4 @AKH2+KH792 (example 1). After stirring or shaking for 10min, separating with magnet for 1h, and taking out supernatant after magnet separation to detect HPAM adsorption amount and adsorption rate.
As shown in FIGS. 4 and 5, the results of HPAM removal test are shown in FIGS. 4 and 5, and as can be seen from FIGS. 4 and 5, fe is prepared according to the present invention 3 O 4 The HPAM removal effect of the nano composite adsorption flocculant is obviously better than that of APTES amino functionalized ferroferric oxide nano particles.
Experimental example 3 SDBS removal detection
And taking 12 parts of oil displacement sewage of an oil field, wherein each part is 5mL, and dividing the oil displacement sewage into 4 groups, and each group is respectively marked as A1-A3, B1-B3, C1-C3 and D1-D3. And respectively adjusting the pH value of the oil displacement sewage of each oil field to 7, 8 and 9 in each group. Then adding enough Fe into A, B, C, D group in turn 3 O 4 APTES (comparative example 1), fe 3 O 4 @APTES+KH602 (comparative example 2), fe 3 O 4 @APTES+KH792 (comparative example 3), fe 3 O 4 @AKH2+KH792 (example 1). After stirring or oscillating for 10min, separating with magnet for 1h, taking out supernatant after magnet separation, and detecting the adsorption quantity and adsorption rate of SDBS.
As shown in FIG. 6 and FIG. 7, the result of SDBS removal detection shows that, as can be seen from FIG. 6 and FIG. 7, fe is prepared according to the present invention 3 O 4 The SDBS removal effect of the nano composite adsorption flocculant is obviously better than that of APTES amino functionalized ferroferric oxide nano particles.
Experimental example 4. Recovery and detection of the removal effect of the three-dimensional composite oil-displacing wastewater after 5 times of repeated use
Fe prepared in example 1 and comparative examples 1 to 3 3 O 4 Adding the nano composite adsorption flocculant into the oil displacement sewage, stirring or oscillating, separating by using a magnet, and taking after the magnet separationThe supernatant was removed and tested. The stirring or oscillating time is 10min, and the magnetic separation time of the magnet is 1h. Magnetically separating Fe 3 O 4 Re-dispersing the nano composite adsorption flocculant into water, regulating the pH value of the dispersion liquid to 10.5, and separating Fe by using a magnet after ultrasonic treatment 3 O 4 The nano composite adsorption flocculant is repeatedly washed and separated for 3 times by the steps, and then Fe separated magnetically 3 O 4 Freeze drying the nano composite adsorption flocculant to obtain reusable Fe 3 O 4 And (3) nano composite adsorption flocculant. The Fe is reused 3 O 4 And detecting the removal effect of the nano composite adsorption flocculant on the ternary composite displacement oil sewage after 5 times of nano composite adsorption flocculant.
As shown in FIG. 8, it can be seen from FIG. 8 that Fe prepared by the present invention 3 O 4 The nano composite adsorption flocculant has the effect of removing ternary composite oil displacement sewage obviously better than APTES amino functionalized ferroferric oxide nano particles after being repeatedly used for 5 times.
The foregoing examples illustrate only a few embodiments of the invention and are described in detail herein without thereby limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (10)
1. A preparation method of a ferroferric oxide nano-composite adsorption flocculant is characterized by comprising the following steps of: the preparation method comprises the following steps: by mixing Fe with 3 O 4 The nano particles are directly copolymerized and grafted with N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxy silane and N- (beta-aminoethyl) -gamma-aminopropyl trimethoxy silane.
2. The method of manufacturing according to claim 1, characterized in that: the preparation method comprises the following steps: 1) Adding ferric trichloride, sodium hydroxide and deionized water into ethylene glycol, stirring and mixing uniformly, heating to boiling, condensing and refluxing, cooling, separating and washing to obtain ferroferric oxide nano particles with the particle size distribution of 20-40 nm;
2) Dispersing the ferroferric oxide nano particles prepared in the step 1) into deionized water, adding N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxy silane and N- (beta-aminoethyl) -gamma-aminopropyl trimethoxy silane, regulating the pH value of the mixed solution to 5-7, mechanically stirring, separating, washing and freeze-drying to obtain Fe 3 O 4 And (3) nano composite adsorption flocculant.
3. The preparation method according to claim 2, characterized in that: the ratio of the amounts of the substances of ferric trichloride, sodium hydroxide, deionized water and ethylene glycol in the step 1) is 1-5:1-10:10-50:30-150; the heating temperature rise rate is 5-15 ℃/min; the condensing reflux time is 4-6h.
4. A method of preparation according to claim 3, characterized in that: the ratio of the amounts of the substances of ferric trichloride, sodium hydroxide, deionized water and ethylene glycol in the step 1) is 1:3:20:100.
5. the preparation method according to claim 2, characterized in that: the ratio of the amounts of the substances of the ferroferric oxide nano-particles, the N- (beta-aminoethyl) -gamma-aminopropyl methyl dimethoxy silane and the N- (beta-aminoethyl) -gamma-aminopropyl trimethoxy silane in the step 2) is 1 to 10:1-20:1-15; the pH value of the mixed solution is 6; the mechanical stirring speed is 300-600rad/s, and the mechanical stirring time is 6-12h.
6. The method of manufacturing according to claim 5, wherein: the ratio of the amounts of the substances of the ferroferric oxide nano-particles, the N- (beta-aminoethyl) -gamma-aminopropyl methyldimethoxy silane and the N- (beta-aminoethyl) -gamma-aminopropyl trimethoxy silane in the step 2) is 2:1:1.
7. a ferroferric oxide nano-composite adsorption flocculant is characterized in that: the ferroferric oxide nano-composite adsorption flocculant is obtained by the preparation method of any one of claims 1-6.
8. The use of the ferroferric oxide nano-composite adsorption flocculant according to claim 7 for removing ternary composite flooding wastewater.
9. A method for removing ternary composite oil displacement sewage is characterized by comprising the following steps: the removing method comprises the following steps: fe according to claim 7 3 O 4 The nano composite adsorption flocculant is added into the oil displacement sewage, and after stirring or oscillating, the mixture is separated by a magnet, and the supernatant is taken out for detection after the magnet is separated.
10. The removal method as claimed in claim 9, wherein: the stirring or oscillating time is 6-12h, and the magnetic separation time of the magnet is 0.5-2h.
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