CN114426326A - Oily sewage treatment flocculant and preparation method and application thereof - Google Patents
Oily sewage treatment flocculant and preparation method and application thereof Download PDFInfo
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- CN114426326A CN114426326A CN202010998550.2A CN202010998550A CN114426326A CN 114426326 A CN114426326 A CN 114426326A CN 202010998550 A CN202010998550 A CN 202010998550A CN 114426326 A CN114426326 A CN 114426326A
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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
- 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
- C02F2103/10—Nature of the water, waste water, sewage or sludge to be treated from quarries or from mining activities
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/10—Solids, e.g. total solids [TS], total suspended solids [TSS] or volatile solids [VS]
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Abstract
The invention belongs to the technical field of sewage treatment, and particularly relates to a flocculant for treating oily sewage, and a preparation method and application thereof. The preparation method comprises the following steps: adding micromolecular olefine acid, diallylamine, methacrylamide, a cosolvent and a buffer solution into water, and uniformly mixing to obtain an emulsion; respectively preparing aqueous solutions of an initiator and a reducing agent; dividing the emulsion into two parts according to the mass ratio, dripping the second part of emulsion and the aqueous solution of the initiator into the first part of emulsion under the stirring condition for polymerization reaction to obtain a primary product after the reaction; and dropwise adding the aqueous solution of the reducing agent into the primary product to remove residual initiator to obtain the flocculant. The flocculant has the characteristics of simple synthesis process, low cost, strong adaptability, good removal of suspended matters and no secondary pollution, the removal rate of the suspended matters in the oily sewage reaches more than 95 percent, and the flocculation effect is improved by more than 20 percent compared with the prior medicament.
Description
Technical Field
The invention belongs to the technical field of sewage treatment, and particularly relates to a flocculant for treating oily sewage, and a preparation method and application thereof.
Background
With the increasing environmental pollution, the control and treatment of water environmental pollution gradually draws attention and makes various progress. The produced water of the oil field contains higher suspended matters, the components are more complex, and the treatment difficulty is more and more large. Too high suspended solids can lead to the increase of oil field water injection pressure, and the energy consumption increases, can harm the stratum moreover, and serious influence recovery ratio, therefore the oil field has strict standard to the suspended solids in the water injection quality of water.
The addition of the flocculating agent in the oily sewage is a conventional, simple and effective method for removing suspended matters, and has short settling time and good treatment effect, so the method is widely adopted at home and abroad. The flocculant is the core of a technology for treating oily sewage by a flocculation method, the commonly used flocculant for treating the oily sewage of the oil field mainly comprises an inorganic flocculant and an organic polymeric flocculant, the inorganic flocculant mainly comprises two systems of ferric salt and aluminum salt, and the organic polymeric flocculant mainly comprises polyacrylamide and derivatives thereof.
In patent literature, CN 107879447 a, "a preparation method for treating flocculant for oily sewage", discloses a preparation method for treating flocculant for oily sewage, which mainly uses chitosan as main raw material, and adds polymeric ferric sulfate, polymeric aluminum sulfate, poly dimethyl diallyl ammonium chloride and copper complex of diphenyl thiourea in the preparation process for modification treatment. The flocculant comprises an inorganic flocculant. The inorganic flocculant has the defects of large usage amount, large sludge production amount, easy corrosion of equipment, secondary pollution (such as increase of water quality chromaticity caused by iron salt and overproof aluminum ions in water caused by aluminum salt), adverse influence on human and other organisms caused by entering into an ecological environment and the like, and is complex in use process and difficult to popularize.
CN 03124417.3 discloses an organic polymer flocculant which is compounded by a polymer A, B composed of dimethyl diallyl ammonium chloride and acrylamide and poly dimethyl diallyl ammonium chloride. But the polyacrylamide is a chemical which is difficult to degrade, residual acrylamide monomer in the polymerization process has toxicity, and the manufacturing cost of the polyacrylamide is higher; the commercially available poly (dimethyldiallylammonium chloride) is a liquid, requires a relatively complicated process to process into solid particles, and is very water-absorbent in a solid state, so that it is difficult to form a stable mixture when preparing a solid blend.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide the flocculant for treating the oily sewage and the preparation method and the application thereof, the flocculant has the characteristics of simple synthesis process, low cost, strong adaptability, good removal of suspended matters and no secondary pollution, the removal rate of the suspended matters in the oily sewage reaches more than 95 percent, and the flocculation effect is improved by more than 70 percent compared with the prior medicament.
Therefore, in order to achieve the above objects, in one aspect, the present invention provides a method for preparing a flocculant for treating oily sewage, comprising the steps of:
(1) adding micromolecular olefine acid, diallylamine, methacrylamide, a cosolvent and a buffer solution into water, and uniformly mixing to obtain an emulsion;
(2) dividing the emulsion into two parts, wherein the second part of emulsion and the aqueous solution of an initiator are simultaneously added into the first part of emulsion in a dropwise manner under the stirring condition for polymerization reaction, and a primary product is obtained after the reaction;
(3) and dropwise adding an aqueous solution of a reducing agent into the primary product to remove residual initiator to obtain the flocculant.
In another aspect, the invention provides a flocculant prepared by the above method, wherein the flocculant has the following formula:
wherein m is 150-4000;
n＝8000-180000；
p＝500-40000；
r is H or C1-C4Alkyl group of (1).
The molecular weight of the flocculant is 2000000-20000000.
In a third aspect, the invention provides the use of a flocculant as described above in the treatment of oily sewage in an oil field.
The suspended matter in the oily sewage is usually colloid particles which usually have negative charges, and because the surface charges of the particles have the same sign, electrostatic repulsion is generated among the particles, so that the colloid particles can not form aggregation and are suspended in water, and the turbidity of the water body is increased. The invention provides a flocculant for treating oily sewage in an oil field, which is a high molecular polymer, wherein the polymer molecule contains polar groups such as amino, amide and the like, and the surface of the polymer has positive charges. When the flocculant is added into the oily sewage, the signs of charges carried by the colloidal particles in the sewage and the flocculant are opposite, electrostatic attraction effect is generated between the colloidal particles and the flocculant until the dosing amount of the flocculant reaches a certain degree, the charges on the surfaces of the colloidal particles are completely neutralized, electrostatic repulsion force disappears, and the particles can approach each other through Brownian motion, so that the colloidal particles are destabilized, larger flocs are formed, and the solid-liquid separation purpose is achieved. The flocculant for treating oily sewage in the oil field provided by the invention is a high molecular polymer, has large molecular weight and long molecular chain, can adsorb a plurality of colloidal particles onto active groups of a molecular chain to play a bridging role, and the macromolecules adsorbing a plurality of particles can be intertwined with each other to generate flocs with larger size, so that residual fine particles in some solutions are curled and collected in flocs in the slow sinking process to play a net catching role and sink together with the fine particles, and the effect of the flocculant is a comprehensive effect with multiple functions.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the synthesis process of the invention is a one-pot method, all products are effective components, the yield is 100%, and no by-product is generated;
(2) the flocculant has the advantages of wide raw material source, simple synthesis process, strong adaptability and small using amount, and the monomer does not contain benzene rings, thereby meeting the requirement of environmental protection;
(3) the flocculant of the invention does not contain inorganic components, does not produce pollution and is environment-friendly;
(4) the flocculant of the invention has a removal rate of suspended matters in oily sewage of more than 95 percent, improves the flocculation effect by more than 70 percent compared with the prior medicament, and meets the flocculation requirement of the oily sewage.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
According to a first aspect of the present invention, there is provided a method for preparing a flocculant for treating oily sewage, comprising the steps of:
(1) adding micromolecular olefine acid, diallylamine, methacrylamide, a cosolvent and a buffer solution into water, and uniformly mixing to obtain an emulsion;
(2) dividing the emulsion into two parts, wherein the second part of emulsion and the aqueous solution of an initiator are simultaneously added into the first part of emulsion in a dropwise manner under the stirring condition for polymerization reaction, and a primary product is obtained after the reaction;
(3) and dropwise adding an aqueous solution of a reducing agent into the primary product to remove residual initiator to obtain the flocculant.
In the present invention, the diallylamine, the methacrylamide, the cosolvent, the buffer and the water are used in amounts of 4 to 20 parts by weight, 20 to 100 parts by weight, 20 to 50 parts by weight and 50 to 200 parts by weight, respectively, based on 1 part by weight of the small molecule olefinic acid. Preferably, the diallyl amine, the methacrylamide, the cosolvent, the buffer solution and the water are respectively used in the amount of 10-15 parts by weight, 50-60 parts by weight, 30-50 parts by weight, 30-45 parts by weight and 100-120 parts by weight based on 1 part by weight of the small molecular weight olefine acid.
More preferably, the diallyl amine, the methacrylamide, the cosolvent, the buffer solution and the water are respectively used in an amount of 10-12 parts by weight, 50-55 parts by weight, 35-40 parts by weight and 110-115 parts by weight based on 1 part by weight of the small molecular weight olefine acid.
In the present invention, preferably, the small molecule olefinic acid is one of acrylic acid, butenoic acid, pentenoic acid, hexenoic acid, heptenoic acid, more preferably butenoic acid or pentenoic acid, and most preferably pentenoic acid.
Preferably, the cosolvent is one or more of OP-10, sodium dodecyl sulfate and MS-1, and more preferably is a mixture of OP-10, sodium dodecyl sulfate and MS-1.
Preferably, the buffer solution is one of 20% ammonia water, sodium phosphate and potassium phosphate, and more preferably 20% ammonia water.
Further, in the step (1), the mixing conditions are that the temperature is room temperature, the stirring speed is 40-120rpm, and the stirring time is 0.5-2 h.
In the present invention, the initiator is preferably one of potassium persulfate, sodium persulfate, and ammonium persulfate, and more preferably ammonium persulfate.
Preferably, the mass concentration of the aqueous initiator solution is 5 to 20%, and more preferably, the mass ratio concentration of the aqueous initiator solution is 6 to 10%.
In the present invention, the aqueous initiator solution is preferably used in an amount of 5 to 20 parts by weight, more preferably 6 to 10 parts by weight, based on 1 part by weight of the small molecular weight olefinic acid.
Preferably, the mass ratio of the first part of emulsion to the second part of emulsion is 1: 3-9, more preferably, the mass ratio of the first part of emulsion to the second part of emulsion is 1: 5-6.
Preferably, in the step (2), the polymerization reaction comprises the temperature of 40-80 ℃, the time of 5-15h and the stirring speed of 100-300 rpm.
Preferably, in step (2), the polymerization reaction comprises two stages which are sequentially carried out, and the reaction conditions of the first stage comprise: the temperature is 40-50 ℃, the time is 3-10h, and the stirring speed is 200-300 rpm; the reaction conditions of the second stage include: the temperature is 70-80 ℃, the time is 2-5h, and the stirring speed is 100-150 rpm. The dropping time of the second part of emulsion and the initiator aqueous solution is consistent with the first-stage reaction time.
Preferably, in the step (3), the reducing agent is one of sodium bisulfite and sodium hydrosulfite, and more preferably sodium bisulfite.
Preferably, the mass concentration of the reducing agent aqueous solution is 5 to 15%, and more preferably, the mass ratio concentration of the reducing agent aqueous solution is 8 to 10%.
In the present invention, preferably, in step (3), the specific steps are: dropwise adding the aqueous solution of the reducing agent and sampling until the starch potassium iodide test paper shows no blue color; then the temperature is reduced to 30-50 ℃ by using circulating water, and the pH value is adjusted to 5-6 by using 20% ammonia water to obtain the flocculant.
In a second aspect, the present invention provides a flocculant prepared by the above process, said flocculant having the formula:
wherein m is 150-4000;
n＝8000-180000；
p＝500-40000；
r is H or C1-C4Alkyl group of (1).
The molecular weight of the flocculant is 2000000-20000000.
In the present invention, preferably, m is 500 to 4000, more preferably 1000 to 4000.
Preferably, n is 20000 to 180000, more preferably 50000 to 180000.
Preferably, p is 2000 to 40000, more preferably 5000 to 40000.
Preferably, R is a methyl or hexyl group, more preferably a hexyl group.
Preferably, the molecular weight of the flocculant is 5000000-20000000.
In a third aspect, the invention provides the use of a flocculant as described above in the treatment of oily sewage in an oil field. The specific application is not particularly required, and can be a conventional application mode in the field, and the detailed description is not repeated.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
The present invention will be further described with reference to specific examples.
In the present invention, the apparatus or equipment used is a conventional apparatus or equipment known in the art, and is commercially available.
In the following examples and comparative examples, the reagents used are all chemically pure reagents from commercial sources, unless otherwise specified.
The performance test of the product is carried out by adopting the following method:
the molecular weight test method refers to GB/T31816-2015 gel chromatography for determining molecular weight and distribution of water treatment agent polymer
The method for testing the removal rate of suspended matters refers to QSH 10201356-2016 technical conditions for general flocculant for treating water conventionally produced in oil field
Example 1 preparation of flocculant A
(1) 1kg of acrylic acid, 4kg of diallylamine, 100kg of methacrylamide, 100kg of OP-10, 50kg of sodium phosphate and 200kg of water are mixed uniformly to obtain an emulsion.
The mixing conditions are that the temperature is room temperature, the stirring speed is 40rpm, and the stirring time is 0.5 h.
(2) Respectively preparing a sodium persulfate aqueous solution with the mass concentration of 5% and a sodium hydrosulfite aqueous solution with the mass concentration of 15%.
(3) And (3) dividing the emulsion into two parts according to the mass ratio of 1: 3, simultaneously dripping the second part of emulsion and the sodium persulfate aqueous solution into the first part of emulsion for polymerization reaction, and obtaining a primary product after the reaction.
The polymerization reaction comprises two stages which are sequentially carried out, and the reaction conditions of the first stage comprise: stirring at 200rpm while heating to 40 deg.C for 10 hr; the reaction conditions of the second stage include: the stirring speed was 100rpm, while the temperature was raised to 70 ℃ and maintained for 2 hours.
The dripping time of the second part of emulsion and the sodium persulfate aqueous solution is consistent with the reaction time of the first stage, and the mass of the sodium persulfate aqueous solution is 20 kg.
(4) And dropwise adding the sodium hydrosulfite aqueous solution into the primary product to remove residual initiator to obtain the flocculant A. The test results are shown in Table 1.
The method comprises the following specific steps: dropwise adding sodium hydrosulfite aqueous solution while sampling until the starch potassium iodide test paper shows no blue color; then the temperature is reduced to 30 ℃ by using circulating water, and the pH value is adjusted to 5 by using 20% ammonia water.
Example 2 preparation of flocculant B
(1) 1kg of crotonic acid, 13kg of diallylamine, 60kg of methacrylamide, 50kg of MS _1, 45kg of ammonia water and 120kg of water are mixed uniformly to obtain an emulsion.
The mixing conditions are that the temperature is room temperature, the stirring speed is 60rpm, and the stirring time is 1 h.
(2) Respectively preparing 6% ammonium persulfate aqueous solution and 10% sodium bisulfite aqueous solution.
(3) And (2) dividing the emulsion into two parts according to the mass ratio of 1: 4, simultaneously dripping the second part of emulsion and the ammonium persulfate aqueous solution into the first part of emulsion for polymerization reaction, and obtaining a primary product after the reaction.
The polymerization reaction comprises two stages which are sequentially carried out, and the reaction conditions of the first stage comprise: stirring at 220rpm while heating to 42 deg.C for 8 hr; the reaction conditions of the second stage include: the stirring speed is 110rpm, the temperature is raised to 72 ℃ simultaneously, and the temperature is kept for 3 h.
The dropping time of the second part of emulsion and the aqueous solution of ammonium persulfate is consistent with the reaction time of the first stage, and the mass of the aqueous solution of ammonium persulfate is 12 kg.
(4) And dropwise adding the sodium bisulfite aqueous solution into the primary product to remove residual initiator to obtain the flocculant B. The test results are shown in Table 1.
The method comprises the following specific steps: dropwise adding the sodium bisulfite aqueous solution while sampling until the test paper shows no blue color; then the temperature is reduced to 50 ℃ by using circulating water, and the pH value is adjusted to 6 by using 20% ammonia water.
Example 3 preparation of flocculant C
(1) 1kg of pentenoic acid, 11kg of diallylamine, 52kg of methacrylamide, 38kg of OP-10, MS-1, a sodium dodecyl sulfate mixture, 35kg of ammonia water and 110kg of water are uniformly mixed to obtain an emulsion.
The mixing conditions are that the temperature is room temperature, the stirring speed is 80rpm, and the stirring time is 1 h.
(2) Respectively preparing an ammonium persulfate aqueous solution with the mass concentration of 8% and a sodium bisulfite aqueous solution with the mass concentration of 8%.
(3) And (2) dividing the emulsion into two parts according to the mass ratio of 1: 5, simultaneously dripping the second part of emulsion and the ammonium persulfate aqueous solution into the first part of emulsion for polymerization reaction, and obtaining a primary product after the reaction.
The polymerization reaction comprises two stages which are sequentially carried out, and the reaction conditions of the first stage comprise: stirring at 240rpm while heating to 44 deg.C for 6 h; the reaction conditions of the second stage include: the stirring speed was 120rpm while the temperature was raised to 74 ℃ and the temperature was maintained for 4 hours.
The dropping time of the second part of emulsion and the aqueous solution of ammonium persulfate is consistent with the reaction time of the first stage, and the mass of the aqueous solution of ammonium persulfate is 8 kg.
(4) And dropwise adding the sodium bisulfite aqueous solution into the primary product to remove residual initiator to obtain the flocculant C. The test results are shown in Table 1.
The method comprises the following specific steps: dropwise adding the sodium bisulfite aqueous solution while sampling until the test paper shows no blue color; then the temperature is reduced to 30 ℃ by using circulating water, and the pH value is adjusted to 5 by using 20% ammonia water.
Example 4 preparation of flocculant D
(1) 1kg of hexenoic acid, 15kg of diallylamine, 50kg of methacrylamide, 48kg of OP-10, MS-1, a sodium dodecyl sulfate mixture and 115kg of water are uniformly mixed to obtain an emulsion.
The mixing conditions are that the temperature is room temperature, the stirring speed is 100rpm, and the stirring time is 1 h.
(2) Respectively preparing 10% ammonium persulfate aqueous solution and 8% sodium bisulfite aqueous solution.
(3) And (2) dividing the emulsion into two parts according to the mass ratio of 1: 7, simultaneously dripping the second part of emulsion and the ammonium persulfate aqueous solution into the first part of emulsion for polymerization reaction, and obtaining a primary product after the reaction.
The polymerization reaction comprises two stages which are sequentially carried out, and the reaction conditions of the first stage comprise: stirring at 280rpm while heating to 47 deg.C for 4 hr; the reaction conditions of the second stage include: the stirring speed was 130rpm while the temperature was raised to 76 ℃ and the temperature was maintained for 5 hours.
The dropping time of the second part of emulsion and the aqueous solution of ammonium persulfate is consistent with the reaction time of the first stage, and the mass of the aqueous solution of ammonium persulfate is 6 kg.
(4) And dropwise adding the sodium bisulfite aqueous solution into the primary product to remove residual initiator to obtain the flocculant D. The test results are shown in Table 1.
The method comprises the following specific steps: dropwise adding the sodium bisulfite aqueous solution while sampling until the test paper shows no blue color; then the temperature is reduced to 40 ℃ by using circulating water, and the pH value is adjusted to 6 by using 20% ammonia water.
Example 5 preparation of flocculant E
(1) 1kg of heptenoic acid, 20kg of diallylamine, 20kg of methacrylamide, 20kg of sodium dodecyl sulfate, 20kg of potassium phosphate and 100kg of water were mixed uniformly to obtain an emulsion.
The mixing conditions are that the temperature is room temperature, the stirring speed is 120rpm, and the stirring time is 2 h.
(2) Respectively preparing a potassium persulfate aqueous solution with the mass concentration of 20% and a sodium hydrosulfite aqueous solution with the mass concentration of 6%.
(3) And (2) dividing the emulsion into two parts according to the mass ratio of 1: 9, dripping the second part of emulsion and the potassium persulfate aqueous solution into the first part of emulsion simultaneously for polymerization reaction, and obtaining a primary product after the reaction.
The polymerization reaction comprises two stages which are sequentially carried out, and the reaction conditions of the first stage comprise: stirring at 300rpm while heating to 50 deg.C for 3 hr; the reaction conditions of the second stage include: the stirring speed is 150rpm, the temperature is raised to 80 ℃ simultaneously, and the temperature is kept for 5 h.
The dripping time of the second part of emulsion and the potassium persulfate aqueous solution is consistent with the first-stage reaction time, and the mass of the potassium persulfate aqueous solution is 5 kg.
(4) And dropwise adding the sodium hydrosulfite aqueous solution into the primary product to remove residual initiator to obtain a flocculant E. The test results are shown in Table 1.
The method comprises the following specific steps: dropwise adding sodium hydrosulfite aqueous solution while sampling until the starch potassium iodide test paper shows no blue color; then the temperature is reduced to 30 ℃ by using circulating water, and the pH value is adjusted to 5 by using 20% ammonia water.
Example 6 in situ application of flocculant A
United station B2The incoming water is produced water of an oil well of an oil production plant of a victory oil field, and the treatment scale is 5000m3D, the content of suspended matters in the sewage is 120mg/L, and the flocculant A is utilized to the combination station B2The produced water is flocculated, the adding amount of the flocculating agent A is 50kg/d, the content of the treated suspended matters is reduced to 5mg/L, the removal rate of the suspended matters is 95.8 percent, the flocculation effect is good, and the process requirement is met.
Example 7 in situ application of flocculant B
United station L2The incoming water is the produced water of an oil well of a certain oil production plant of the victory oil field, and the treatment scale is 2000m3D, the content of suspended matters in the sewage is 120mg/L, and the flocculant B is utilized to the combination station L2The produced water is flocculated, the adding amount of the flocculating agent B is 20kg/d, the content of the treated suspended matters is reduced to 4.5mg/L, the removal rate of the suspended matters is 96.3 percent, the flocculation effect is good, and the process requirement is met.
Example 8 in situ application of flocculant C
United station G11The incoming water is produced water of an oil well of a certain oil production plant of the victory oil field, and the treatment scale is 4000m3D, the content of suspended matters in the sewage is 98mg/L, and the flocculant C of the invention is utilized to the combination station B2The produced water is flocculated, the adding amount of the flocculating agent A is 40kg/d, the content of the treated suspended matters is reduced to 2.7mg/L, the removal rate of the suspended matters is 97.3 percent, the flocculation effect is good, and the process requirement is met.
Example 9 in situ application of flocculant D
United station C3The incoming water is produced water of an oil well of an oil production plant of a victory oil field, and the treatment scale is 3000m3D, the content of suspended matters in the sewage is 96mg/L, and the flocculant D is utilized to the combination station C3The produced water is flocculated, the adding amount of the flocculating agent A is 30kg/d, the content of the treated suspended matters is reduced to 4.2mg/L, the removal rate of the suspended matters is 95.6 percent, the flocculation effect is good, and the process requirement is met.
Example 10 in situ application of flocculant E
United station L4The incoming water is produced water of an oil well of an oil production plant of a victory oil field, and the treatment scale is 1500m3D, the content of suspended matters in the sewage is 150mg/L, and the flocculant E of the invention is utilized to the combination station L4The produced water is flocculated, the adding amount of the flocculating agent E is 15kg/d, the content of the treated suspended matters is reduced to 7.3mg/L, the removal rate of the suspended matters is 95.1 percent, the flocculation effect is good, and the following technical requirements are met.
Comparative example 1
United station B2The incoming water is produced water of an oil well of an oil production plant of a victory oil field, and the treatment scale is 5000m3D, the content of suspended matters in the sewage is 120mg/L, and conventional flocculating agents PAC and PAM are utilized to combine the station B2The produced water is flocculated, the adding amount of PAC is 100kg/d, the adding amount of PAM is 50kg/d, the content of suspended substances after treatment is reduced to 35mg/L, the removal rate of the suspended substances is 70.8 percent, and the flocculation effect is general.
Comparative example 2
United station L2The incoming water is the produced water of an oil well of a certain oil production plant of the victory oil field, and the treatment scale is 2000m3D, the content of suspended matters in the sewage is 120mg/L, and conventional flocculating agents PAC and PAM are utilized to combine the station B2The produced water is flocculated, the adding amount of PAC is 100kg/d, the adding amount of PAM is 50kg/d, the content of suspended matters after treatment is reduced to 38rng/L, the removal rate of the suspended matters is 68.3 percent, and the flocculation effect is general.
TABLE 1 flocculant A, B, C, D, E Performance index test results
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (21)
1. A preparation method of a flocculant for treating oily sewage is characterized by comprising the following steps:
(1) adding micromolecular olefine acid, diallylamine, methacrylamide, a cosolvent and a buffer solution into water, and uniformly mixing to obtain an emulsion;
(2) dividing the emulsion into two parts, wherein the second part of emulsion and the aqueous solution of an initiator are simultaneously added into the first part of emulsion in a dropwise manner under the stirring condition for polymerization reaction, and a primary product is obtained after the reaction;
(3) and dropwise adding an aqueous solution of a reducing agent into the primary product to remove residual initiator to obtain the flocculant.
2. The method according to claim 1, wherein the diallylamine, the methacrylamide, the cosolvent, the buffer and the water are used in an amount of 4 to 20 parts by weight, 20 to 100 parts by weight, 20 to 50 parts by weight and 50 to 200 parts by weight, respectively, based on 1 part by weight of the small molecular weight olefinic acid.
3. The method according to claim 2, wherein the diallylamine, the methacrylamide, the cosolvent, the buffer and the water are used in an amount of 10 to 15 parts by weight, 50 to 60 parts by weight, 30 to 50 parts by weight, 30 to 45 parts by weight and 100 to 120 parts by weight, respectively, based on 1 part by weight of the small molecular weight olefinic acid.
4. The method of claim 1, wherein the small-molecule olefinic acid is one of acrylic acid, butenoic acid, pentenoic acid, hexenoic acid, and heptenoic acid.
5. The preparation method of claim 1, wherein the cosolvent is one or more of OP-10, sodium dodecyl sulfate, and MS-1.
6. The preparation method of claim 5, wherein the cosolvent is a mixture of OP-10, sodium dodecyl sulfate and MS-1.
7. The method of claim 1, wherein the buffer is one of 20% ammonia, sodium phosphate and potassium phosphate.
8. The preparation method according to claim 1, wherein in the step (1), the mixing conditions are room temperature, stirring speed of 40-120rpm, and stirring time of 0.5-2 h.
9. The method according to claim 1, wherein in the step (2), the initiator is one of potassium persulfate, sodium persulfate and ammonium persulfate.
10. The method according to claim 1, wherein the aqueous initiator solution has a mass concentration of 5 to 20% and is used in an amount of 5 to 20 parts by weight based on 1 part by weight of the small molecular weight olefinic acid.
11. The method according to claim 1, wherein the mass ratio of the first part emulsion to the second part emulsion is 1: 3-9.
12. The process according to claim 1, wherein the polymerization reaction comprises a temperature of 40 to 80 ℃ for 5 to 15 hours and a stirring speed of 100 to 300 rpm.
13. The process according to claim 1 or 12, wherein the polymerization reaction comprises two stages carried out in sequence, and the reaction conditions of the first stage comprise: the temperature is 40-50 ℃, the time is 3-10h, and the stirring speed is 200-300 rpm; the reaction conditions of the second stage include: the temperature is 70-80 ℃, the time is 2-5h, and the stirring speed is 100-150 rpm.
14. The method according to claim 1, wherein the reducing agent is one of sodium bisulfite and sodium hydrosulfite.
15. The production method according to claim 1, wherein the mass concentration of the aqueous reducing agent solution is 5 to 15%.
16. The preparation method according to claim 1, wherein in the step (4), the specific steps are as follows: dropwise adding the aqueous solution of the reducing agent and sampling until the starch potassium iodide test paper shows no blue color; then the temperature is reduced to 30-50 ℃ by using circulating water, and the pH value is adjusted to 5-6 by using 20% ammonia water to obtain the flocculant.
17. The flocculant produced by the production method according to any one of claims 1 to 16.
18. A flocculant according to claim 17, wherein the flocculant has the formula:
wherein m is 150-4000;
n＝8000-180000；
p＝500-40000；
r is H or C1-C4Alkyl groups of (a);
the molecular weight of the flocculant is 2000000-20000000.
19. The flocculant of claim 18, wherein R is a methyl or hexyl group.
20. The flocculant of claim 18, wherein m is 500-4000, n is 20000-180000, p is 2000-40000, and the molecular weight is 5000000-20000000.
21. Use of a flocculant according to any one of claims 17 to 20 in the treatment of oily sewage in an oil field.
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