CN110759451A - Rare earth cationic-composite aluminum organic heteropolymeric flocculant - Google Patents
Rare earth cationic-composite aluminum organic heteropolymeric flocculant Download PDFInfo
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/54—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using organic material
- C02F1/56—Macromolecular compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
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Abstract
The invention discloses a rare earth cation type-composite aluminum organic heteropolymerization flocculant, which is obtained by grafting acrylamide and dimethyl diallyl ammonium chloride on a polymerization product of aluminum chloride and rare earth chloride; solves the problems of floating of the existing flocculating agent flocs and large using amount of the flocculating agent.
Description
Technical Field
The invention relates to the field of petrochemical industry, in particular to a flocculating agent for flocculating substances harmful to the environment, such as oil, suspended matters, heavy metal ions and the like in sewage in the process of treating the sewage in an oil field and a preparation method thereof.
Background
Oilfield wastewater typically contains a variety of environmentally harmful substances that, if left untreated or disposed of improperly into the surrounding environment, would inevitably cause significant damage to the surrounding environment. In many oil fields, because the components of sewage are complex, the traditional sewage treatment agent cannot meet the national environmental protection requirements, and at the moment, a high-efficiency and environment-friendly flocculating agent is needed to solve the problem of complex sewage and ensure that the sewage reaches the discharge or reinjection standard.
At the present stage, the polyaluminium chloride flocculating agent with the most use and the widest use range is used, and aluminum salt is rapidly hydrolyzed and polymerized after being added into sewage, so that a plurality of positive charges of the aluminum salt are generated and diffused to the surface of particles, and the particles are electrically neutralized. The flocculation mechanism of polyaluminium chloride is actually surface complexation and surface precipitation. The polyaluminium chloride used as a flocculating agent for treating sewage is required to cover a certain degree of aluminium ions on the surface of particles in the sewage, so that the particles are electrically neutralized to a certain degree, and the adsorption bridging and net capturing and rolling sweeping mechanisms of the polyaluminium chloride can play a role, which means that when the particles in the sewage are too much and the components are more complex, a large amount of polyaluminium is required for treatment, the water amount of the sewage in an oil field is huge, and the excessive treatment cost is unrealistic; and the single use of polyaluminium chloride has a single action mechanism, cannot adapt to complex water quality conditions, and has the problems of complex sewage components, more impurities and high oil content along with the increasing complexity of oil field exploitation modes at the present stage, so that flocs float upwards under the conditions, and the field operation is seriously influenced.
Disclosure of Invention
In view of the above, the invention provides a rare earth cationic-composite aluminum organic heteropolymeric flocculant, which solves the problems of floating of the existing flocculant and large flocculant consumption.
In order to realize the aim, the rare earth cation type-composite aluminum organic heteropolymerization flocculant is obtained by grafting acrylamide and dimethyl diallyl ammonium chloride on a polymerization product of aluminum chloride and rare earth chloride.
Preferably, the rare earth chloride is lanthanum chloride or cerium chloride or a mixture of lanthanum chloride and cerium chloride as main components.
Preferably, the aluminum chloride is aluminum chloride hexahydrate.
Preferably, the polymerization product of aluminum chloride and rare earth chloride is obtained by hydrolytic polymerization.
Preferably, the hydrolytic polymerization reaction is a reaction in which sodium hydroxide is added to an aqueous solution obtained by dissolving the aluminum chloride and the rare earth chloride in water.
Preferably, the adding time of the sodium hydroxide is 20-30 min; and continuing stirring for 2-4 h after the sodium hydroxide is added.
Preferably, the grafting is a reaction of completely dissolving the acrylamide and the dimethyldiallylammonium chloride in a dissolved substance in the polymerization product and adding an initiator.
Preferably, the initiator is ammonium persulfate and sodium bisulfite.
Preferably, the ammonium persulfate and the sodium bisulfite are added in sequence; the adding time of the sodium bisulfite is 10-20 min.
Preferably, the grafting reaction temperature is 40-45 ℃, the reaction time is 4-6 h, and the reaction process is carried out under the stirring condition.
Preferably, before the initiator is added, nitrogen is introduced into the dissolved matter for 30min to 1 h;
the nitrogen is used for removing oxygen in the dissolved matter.
Preferably, by mass, 36.2-54.3 parts of aluminum chloride hexahydrate, 3.7-5.5 parts of rare earth chloride, 2-2.5 parts of sodium hydroxide, 8 parts of acrylamide, 1.6-4.8 parts of dimethyldiallylammonium chloride, 0.02 part of ammonium persulfate, 0.012 part of sodium bisulfite and 76 parts of water.
The invention has the following beneficial effects:
the rare earth cation type-composite aluminum organic heteropolymerization flocculant is an inorganic polymer obtained by heteropolymerization of aluminum element and lanthanum and cerium elements in rare earth, and then the inorganic polymer is subjected to graft copolymerization with acrylamide and dimethyl diallyl ammonium chloride monomers to form an inorganic-organic heteropolymerization cation high polymer. Compared with polyaluminium chloride, rare earth ions in the flocculant of the invention are easy to generate hydrolysis reaction to form mixed sol of polymeric lanthanum hydroxide and cerium hydroxide, on the basis, a longer and more stable polymer network with a stable core is formed by graft polymerization of acrylamide and dimethyl diallyl ammonium chloride and inorganic-organic cross copolymerization, and the flocculant takes net-captured precipitation as a main mechanism after sewage is added;
the rare earth cation type-composite aluminum organic heteropolymeric flocculant is still an aluminum-based composite flocculant, so that the addition of rare earth elements and organic high polymer strengthens the function of adsorption bridging while the aluminum-salt flocculant has the flocculation characteristic, thereby greatly improving the flocculation effect and enabling the sewage to meet the index requirement under the condition of low dosage.
Drawings
FIG. 1 is a graph showing the results of laboratory experiments on flocculants according to examples 1 to 3 of the present invention;
FIG. 2 is an infrared spectrum of a flocculant of example 1 of the present invention;
FIG. 3 shows the experimental results of the flocculant of example 4 in an oilfield water station, wherein the stirring and standing time is 30min, and the addition amount of the flocculant is 300 mg/L;
FIG. 4 shows the experimental results of the flocculant of example 4 in an oilfield water station, wherein the stirring and standing time is 1h, and the addition amount of the flocculant is 300 mg/L;
FIG. 5 is a comparison of untreated wastewater (left) versus treated (right) for the flocculant of example 4 tested at an oilfield water station showing a flocculant addition of 180 mg/L.
Detailed Description
The present invention will be described below based on embodiments and drawings, but it should be noted that the present invention is not limited to these embodiments. In the following detailed description of the present invention, certain specific details are set forth. However, the present invention may be fully understood by those skilled in the art for those parts not described in detail.
The rare earth chlorides used in the following examples have the composition shown in table 1:
TABLE 1 ingredient table of rare earth chlorides
Example 1
Firstly, raw material composition
According to the mass components, 54.3 parts of aluminum chloride hexahydrate, 5.5 parts of rare earth chloride, 2.5 parts of sodium hydroxide, 8 parts of acrylamide, 4.8 parts of dimethyl diallyl ammonium chloride, 0.02 part of ammonium persulfate, 0.012 part of sodium bisulfite and 76 parts of water.
Secondly, the preparation step
(1) Adding 54.3 parts of aluminum chloride hexahydrate into 76 parts of water by using a beaker, stirring for 10min by using a magnetic stirring paddle, and then completely hydrolyzing the aluminum chloride hexahydrate, wherein the mark of the completion of dissolution is transparent and clear solution;
(2) after the aluminum chloride hexahydrate is dissolved, adding 5.5 parts of rare earth chloride into the solution, continuously stirring for 10min, and then completing the hydrolysis of the rare earth chloride, wherein the mark of the completion of the dissolution indicates that no solid exists in the solution;
(3) slowly adding 2.5 parts of sodium hydroxide into the solution obtained in the step (2), stirring simultaneously, adding for 30min, continuously stirring for 3h after adding, completely dispersing crystals in the solution, finishing the hydrolytic polymerization reaction, recovering the solution to a clear and transparent state, and dispersing the crystals to form a heteropolymerization mixed sol of polymeric aluminum hydroxide, lanthanum hydroxide and cerium hydroxide;
(4) adding 8 parts of acrylamide and 4.8 parts of dimethyl diallyl ammonium chloride into the mixed sol obtained in the step (3), stirring for 10min, dissolving the two monomers, introducing high-purity nitrogen for 30min after the monomers are completely dissolved, and removing oxygen;
(5) adding 0.02 part of ammonium persulfate into the solution obtained in the step (4), stirring for 5min, and slowly adding 0.012 part of sodium bisulfite for 10 min;
(6) and (4) stirring and controlling the temperature of the solution obtained in the step (5) at 45 ℃ for 4 hours to obtain the rare earth cation type-composite aluminum organic heteropolymeric flocculant No. 1.
Infrared spectroscopic analysis is carried out on the rare earth cation type-composite aluminum organic heteropolymeric flocculant No. 1.
Tabletting the KBr, uniformly coating the product in a liquid state on the KBr tablet, and placing the tablet in a Fourier infrared spectrometer for detection. The detection wavelength range is 4000-300 cm-1Measurement resolution of 4cm-1。
As shown in figure 2, the rare earth cation type-composite aluminum organic heteropolymeric flocculant is at 3427cm-1Is treated as an N-H symmetric telescopic peak in polyacrylamide, and is 3200-3000 cm-1The wider absorption peak is the absorption peak generated by the stretching vibration of-OH groups in the poly-aluminum, lanthanum and cerium molecules connected with Al (III), La (III) and Ce (III) ions and the absorption of the-OH groups in water molecules, and the absorption peak is also the most main absorption peak in the polymeric metal salt; 2854cm-1The absorption peak belongs to the stretching vibration of C-H bond; 1673cm-1The absorption peak at (A) belongs to the stretching vibration of an amide group C ═ O bond; 851cm-1An absorption peak generated by bending vibration of Al (La, Ce) -O-Al (La, Ce); reflecting the bonding of atoms of aluminum chloride and rare earth chloride through oxygen bridges during the conversion into polymeric metal salt, and the strength of the bonding reflects the number of the bonding. The bond has higher capability of forming a polynuclear aluminum hydroxide complex during hydrolysis, and can be used as one of the signs of quality of the polymetallic salt compound; 619cm-1The wave number is the telescopic absorption wave number of C-Cl, and the hybrid structure of the rare earth cation type-composite aluminum organic heteropolymerization flocculant is verified in an infrared spectrum.
Example 2
Firstly, raw material composition
According to the mass components, 45.25 parts of aluminum chloride hexahydrate, 4.58 parts of rare earth chloride, 2.25 parts of sodium hydroxide, 8 parts of acrylamide, 3.2 parts of dimethyl diallyl ammonium chloride, 0.02 part of ammonium persulfate, 0.012 part of sodium bisulfite and 76 parts of water.
Secondly, the preparation step
(1) Adding 45.25 parts of aluminum chloride hexahydrate into 76 parts of water by using a beaker, and stirring for 10min by using a magnetic stirring paddle to completely hydrolyze the aluminum chloride hexahydrate;
(2) after the aluminum chloride hexahydrate is dissolved, 4.58 parts of rare earth chloride is added into the solution, and the solution is continuously stirred for 10min, so that the rare earth chloride is hydrolyzed;
(3) slowly adding 2.25 parts of sodium hydroxide into the solution obtained in the step (2), stirring simultaneously, adding for 25min, after the addition is finished and stirring is continued for 2.5h, completely dispersing crystals in the solution, finishing the first-step hydrolytic polymerization reaction, recovering the solution to be in a clear and transparent state, and dispersing the crystals to form heteropolymeric mixed sol of polymeric aluminum hydroxide, lanthanum hydroxide and cerium hydroxide;
(4) adding 8 parts of acrylamide and 3.2 parts of dimethyl diallyl ammonium chloride into the sol obtained in the step (3), stirring for 10min, dissolving the two monomers, introducing high-purity nitrogen for 30min after the monomers are completely dissolved, and removing oxygen;
(5) adding 0.02 part of ammonium persulfate into the solution obtained in the step (4), stirring for 5min, and slowly adding 0.012 part of sodium bisulfite for 10 min;
(6) and (4) stirring and controlling the temperature of the solution obtained in the step (5) at 45 ℃ for 4 hours to obtain the rare earth cation type-composite aluminum organic heteropolymeric flocculant No. 2.
Example 3
Firstly, raw material composition
According to the mass components, 36.2 parts of aluminum chloride hexahydrate, 3.7 parts of rare earth chloride, 2 parts of sodium hydroxide, 8 parts of acrylamide, 1.6 parts of dimethyl diallyl ammonium chloride, 0.02 part of ammonium persulfate, 0.012 part of sodium bisulfite and 76 parts of water.
Secondly, the preparation step
(1) Adding 36.2 parts of aluminum chloride hexahydrate into 76 parts of water by using a beaker, and stirring for 10min by using a magnetic stirring paddle to completely hydrolyze the aluminum chloride hexahydrate;
(2) after the aluminum chloride hexahydrate is dissolved, 3.7 parts of rare earth chloride is added into the solution, and the solution is continuously stirred for 10min, so that the rare earth chloride is hydrolyzed;
(3) slowly adding 2 parts of sodium hydroxide into the solution obtained in the step (2), stirring simultaneously, wherein the adding time is 20min, continuously stirring for 2h after the adding is finished, completely dispersing crystals in the solution, finishing the first-step hydrolytic polymerization reaction, recovering the solution to be in a clear and transparent state, and dispersing the crystals to form a heteropolymerization mixed sol of polymeric aluminum hydroxide, lanthanum hydroxide and cerium hydroxide;
(4) adding 8 parts of acrylamide and 1.6 parts of dimethyl diallyl ammonium chloride into the sol obtained in the step (3), stirring for 10min, dissolving the two monomers, introducing high-purity nitrogen for 30min after the monomers are completely dissolved, and removing oxygen;
(5) adding 0.02 part of ammonium persulfate into the solution obtained in the step (4), stirring for 5min, and slowly adding 0.012 part of sodium bisulfite for 10 min;
(6) and (3) stirring and controlling the temperature of the solution obtained in the step (5) at 45 ℃ for 4 hours to obtain the rare earth cation type-composite aluminum organic heteropolymeric flocculant No. 3.
Examples 1 to 3 Effect test
The same oilfield wastewater was treated with 3 kinds of flocculants synthesized in examples 1, 2 and 3 and the flocculant PAC currently used on site, respectively, and the effects were compared.
The test steps are as follows:
(1) taking five test tubes, and respectively taking 100ml of sewage of a certain oil field;
(2) no. 1 test tube is not added with any flocculant, No. 2 to No. 5 test tubes are respectively added with 200mg/L on-site PAC and No. 1 to No. 3 rare earth cation type-composite aluminum organic heteropolymeric flocculant and then are shaken for 30 times;
(3) after standing for 1h, the flocculation of each flocculant was observed, and the test results are shown in FIG. 1.
(4) The oil content and the suspended matter content of the water samples of the test tubes are respectively tested, and the test results are shown in table 2.
Table 2 comparative effect test
Through comparison between fig. 1 and table 2, it can be found that, at the same addition, the rare earth cation type-composite aluminum organic heteropolymeric flocculant has better flocculation effect and more compact and complete floc sinking compared with the flocculant PAC used on site.
Example 4
Firstly, raw material composition
1400kg of aluminum chloride hexahydrate, 142kg of rare earth chloride, 64kg of sodium hydroxide, 206kg of acrylamide,82.5kg of dimethyl diallyl ammonium chloride, 0.52kg of ammonium persulfate, 0.31kg of sodium bisulfite, 1957kg of water and 1m of nitrogen3(3atm, 25 ℃ C.). (by mass, 54.3 parts of aluminum chloride hexahydrate, 5.5 parts of rare earth chloride, 2.5 parts of sodium hydroxide, 8 parts of acrylamide, 3.2 parts of dimethyl diallyl ammonium chloride, 0.02 part of ammonium persulfate, 0.012 part of sodium bisulfite and 76 parts of water.)
Secondly, the preparation step
(1) 1957kg of water is injected into the chemical reaction kettle, and 1400kg of AlCl is added3·6H2O, stirring with a stirring paddle, AlCl3·6H2Adding O under stirring for 2h, continuously adding 142kg of rare earth chloride after the aluminum chloride hexahydrate is added for 30min, and completely dissolving the aluminum chloride hexahydrate and the rare earth chloride after the aluminum chloride hexahydrate is added and continuously stirred for 1 h;
the maximum capacity of the chemical reaction kettle in the step (1) is 4.5 square; 1400kgAlCl3·6H2626.5kg of water and AlCl can be decomposed after the O is dissolved in the water3·6H2The volume of the solution after the O and the rare earth chloride are completely dissolved is about 2.6 square.
(2) Slowly adding 64kg of sodium hydroxide into the reaction kettle while stirring for 30min, after the addition is finished and the stirring is continued for 2h, completely dispersing crystals in the solution, and after the first-step hydrolytic polymerization reaction is finished, recovering the solution to a clear state;
(3) adding 206kg of acrylamide and 82.5kg of dimethyl diallyl ammonium chloride into the reaction kettle, stirring while adding for 1h, and stirring for 30min after adding to completely dissolve the two reaction monomers. Introducing high-purity nitrogen for 30min after the reaction monomers are dissolved, and removing dissolved oxygen;
(4) adding an initiator to initiate the second-step graft polymerization reaction after deoxygenation is finished, firstly adding 0.52kg of ammonium persulfate for 10min, and continuing stirring for 20min after the addition is finished; then adding 0.31kg of sodium bisulfite for 20min, and continuing stirring after the addition is finished;
(5) heating the reaction kettle to 45 ℃, then sealing the reaction kettle and continuously stirring for 6 hours to obtain the rare earth cation type-composite aluminum organic heteropolymeric flocculant, and finally obtaining the finished flocculant with the mass of about 3.4 tons and the formula of about 2.6.
The flocculant is applied to the field, and the field test report is as follows:
the indexes of the sewage of the on-site treatment station are respectively that the oil content is less than or equal to 3mg/L and the suspended matter is less than or equal to 8 mg/L.
The water quality monitoring using the original flocculant polyaluminium chloride (PAC) is reported in table 3.
TABLE 3 data of the original flocculant water quality on site
The detection shows that the original PAC flocculant can not make the oil content and the suspended matter content reach the standard under higher addition, and the effect of the on-site flocculant is unstable along with the change of sewage components because the sewage components are not invariable.
The addition mode of the rare earth cationic-composite aluminum organic heteropolymeric flocculant of this example 4 is consistent with that of the original flocculant PAC used on site, and the report of water quality monitoring after adding the rare earth cationic-composite aluminum organic heteropolymeric flocculant is shown in Table 4.
TABLE 4 rare earth cation type-composite aluminum organic heteropolymeric flocculant field test data
Note: the main reason for taking the high-level water for detection is to evaluate the sinking of flocs.
And (4) field test conclusion:
(1) as can be seen from Table 4, the agent has good performance, and when the addition of the agent is 300mg/L, the oil removal rate of the station 1 can reach 98.3 percent, and the oil removal rate of the station 2 can reach 99.2 percent; the suspension 1 station can be reduced to 4.5mg/L, and the suspension 2 station can be reduced to 3.7 mg/L.
(2) As can be seen from Table 4, it was found that the oil content and solid content of both sites reached the standard when the amount of addition was only 180 mg/L; under the adding amount, the oil content of the station No. 1 is 2.8mg/L at most, and the suspended matter content is 7.9mg/L at most; the oil content of the station 2 is up to 2.8mg/L, and the suspended matter content is up to 7.2 mg/L.
(3) FIG. 3 shows the effect of flocculant addition of 300mg/L after stirring and standing for 30min, the floc completely sinks, and the water quality is clear after treatment;
(4) FIG. 4 shows the effect of a flocculant added at 300mg/L after stirring and standing for 1 hour, wherein the flocculant is tightly agglomerated and has large flocs, and the flocculant is suitable for field filtration;
(5) FIG. 5 is the effect chart of the flocculant of the present invention at the lowest addition level verified by field tests, wherein the minimum addition level for reaching the water quality standard of the flocculant of the present invention is verified to be 180mg/L, and the flocculant of the present invention not only can reach the water quality standard after sewage treatment, but also can completely sink flocs.
From example 4, it can be seen that the flocculant of the present application has the advantages of clarified water quality, reduced oil content and suspended matter content obviously higher than PAC (polyaluminium chloride) in the same amount, and good field test effect.
The above-mentioned embodiments are merely embodiments for expressing the invention, and the description is specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for those skilled in the art, various changes, substitutions of equivalents, improvements and the like can be made without departing from the spirit of the invention, and these are all within the scope of the invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A rare-earth cationic-composite aluminium organic heteropolymeric flocculant is prepared through grafting acrylamide and dimethyl diallyl ammonium chloride on the polymerized product of aluminium chloride and rare-earth chloride.
2. The rare earth cationic-composite aluminum organic heteropolymeric flocculant of claim 1, wherein:
the rare earth chloride is lanthanum chloride or cerium chloride or a mixture of the lanthanum chloride and the cerium chloride as main components.
3. The rare earth cationic-composite aluminum organic heteropolymeric flocculant of claim 1, wherein:
the polymerization product of the aluminum chloride and the rare earth chloride is obtained by hydrolytic polymerization reaction.
4. The rare earth cationic-composite aluminum organic heteropolymeric flocculant according to claim 3, characterized in that:
the hydrolytic polymerization reaction is a reaction in which sodium hydroxide is added into an aqueous solution obtained by dissolving the aluminum chloride and the rare earth chloride with water.
5. The rare earth cationic-composite aluminum organic heteropolymeric flocculant of claim 4, wherein:
the adding time of the sodium hydroxide is 20-30 min; and continuing stirring for 2-4 h after the sodium hydroxide is added.
6. The rare earth cationic-composite aluminum organic heteropolymeric flocculant of claim 1, wherein:
the grafting is a reaction of completely dissolving the acrylamide and the dimethyl diallyl ammonium chloride in a dissolved substance in the polymerization product and adding an initiator.
7. The rare earth cationic-composite aluminum organic heteropolymeric flocculant of claim 6, wherein:
the initiator is ammonium persulfate and sodium bisulfite.
8. The rare earth cationic-composite aluminum organic heteropolymeric flocculant of claim 7, wherein:
the ammonium persulfate and the sodium bisulfite are added in sequence; the adding time of the sodium bisulfite is 10-20 min.
9. The rare earth cationic-composite aluminum organic heteropolymeric flocculant of claim 8, wherein:
and grafting, wherein the reaction temperature is 40-45 ℃, the reaction time is 4-6 h, and the reaction process is carried out under the stirring condition.
10. The rare earth cationic-composite aluminum organic heteropolymeric flocculant according to any one of claims 6 to 9, characterized in that:
before the initiator is added, introducing nitrogen into the dissolved matter for 30 min-1 h;
the nitrogen is used for removing oxygen in the dissolved matter.
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| US5738795A (en) * | 1996-06-14 | 1998-04-14 | Betzdearborn Inc. | Compositions and methods for water clarification |
| CN1554592A (en) * | 2003-12-21 | 2004-12-15 | 浙江大学 | Organic-inorganic ionic hetero high efficiency flocculant |
| CN101575130A (en) * | 2009-06-15 | 2009-11-11 | 山东大学 | Method for preparing rare earth ceria modified inorganic polymeric flocculant by using industrial waste |
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