CN115818849A - Oilfield sewage purifying agent and preparation method thereof - Google Patents
Oilfield sewage purifying agent and preparation method thereof Download PDFInfo
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- CN115818849A CN115818849A CN202111101726.0A CN202111101726A CN115818849A CN 115818849 A CN115818849 A CN 115818849A CN 202111101726 A CN202111101726 A CN 202111101726A CN 115818849 A CN115818849 A CN 115818849A
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- 239000010865 sewage Substances 0.000 title claims abstract description 135
- 239000012629 purifying agent Substances 0.000 title claims abstract description 82
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 60
- 239000002245 particle Substances 0.000 claims abstract description 48
- -1 thiol compound Chemical class 0.000 claims abstract description 22
- 125000000217 alkyl group Chemical group 0.000 claims abstract description 12
- 150000001875 compounds Chemical class 0.000 claims abstract description 11
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- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 9
- 239000001257 hydrogen Substances 0.000 claims abstract description 9
- 125000002947 alkylene group Chemical group 0.000 claims abstract description 5
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 14
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 6
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 6
- 239000011236 particulate material Substances 0.000 claims description 4
- 238000002604 ultrasonography Methods 0.000 claims description 4
- 125000000816 ethylene group Chemical group [H]C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 2
- 125000001570 methylene group Chemical group [H]C([H])([*:1])[*:2] 0.000 claims description 2
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 2
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 17
- 238000005260 corrosion Methods 0.000 abstract description 16
- 230000007797 corrosion Effects 0.000 abstract description 16
- 239000003795 chemical substances by application Substances 0.000 abstract description 12
- 239000007789 gas Substances 0.000 abstract description 12
- 230000001954 sterilising effect Effects 0.000 abstract description 8
- 230000005764 inhibitory process Effects 0.000 abstract description 7
- 238000004659 sterilization and disinfection Methods 0.000 abstract description 7
- 238000005189 flocculation Methods 0.000 abstract description 6
- 230000016615 flocculation Effects 0.000 abstract description 6
- 238000006477 desulfuration reaction Methods 0.000 abstract description 4
- 230000023556 desulfurization Effects 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 2
- 238000006555 catalytic reaction Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 18
- 239000003921 oil Substances 0.000 description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 14
- IQDGSYLLQPDQDV-UHFFFAOYSA-N dimethylazanium;chloride Chemical compound Cl.CNC IQDGSYLLQPDQDV-UHFFFAOYSA-N 0.000 description 12
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 description 12
- 238000000746 purification Methods 0.000 description 11
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- 229910052717 sulfur Inorganic materials 0.000 description 9
- 239000011593 sulfur Substances 0.000 description 9
- 241000894006 Bacteria Species 0.000 description 8
- WQAQPCDUOCURKW-UHFFFAOYSA-N butanethiol Chemical compound CCCCS WQAQPCDUOCURKW-UHFFFAOYSA-N 0.000 description 8
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 8
- SUVIGLJNEAMWEG-UHFFFAOYSA-N propane-1-thiol Chemical compound CCCS SUVIGLJNEAMWEG-UHFFFAOYSA-N 0.000 description 8
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 7
- 239000008139 complexing agent Substances 0.000 description 7
- 229910052742 iron Inorganic materials 0.000 description 7
- 238000001035 drying Methods 0.000 description 5
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- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 2
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- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 2
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- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 2
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 2
- 229910052698 phosphorus Inorganic materials 0.000 description 2
- 239000011574 phosphorus Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000011435 rock Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- LSDPWZHWYPCBBB-UHFFFAOYSA-N Methanethiol Chemical compound SC LSDPWZHWYPCBBB-UHFFFAOYSA-N 0.000 description 1
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- YVPHBTUFPWLPEY-UHFFFAOYSA-M dimethyl-[2-(2-methylprop-2-enoyloxy)ethyl]-(oxiran-2-ylmethyl)azanium;chloride Chemical compound [Cl-].CC(=C)C(=O)OCC[N+](C)(C)CC1CO1 YVPHBTUFPWLPEY-UHFFFAOYSA-M 0.000 description 1
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- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to an oilfield sewage purifying agent and a preparation method thereof, belonging to the technical field of oilfield sewage treatment. The preparation method of the oilfield sewage purifying agent comprises the following steps: reacting the compound shown in the formula I, the thiol compound shown in the formula II and the particle material to obtain the compound; wherein R is 1 、R 2 And R 3 Is hydrogen or alkyl; r 4 And R 7 Is an alkylene group; r 5 、R 6 And R 8 Is an alkyl group. Oil field of the inventionThe preparation method of the sewage purifying agent is simple to operate, and the sewage purifying agent is prepared by taking the compound shown in the formula I and alkyl mercaptan as raw materials, taking a particle material as a catalyst and a catalytic reaction carrier and carrying out a mixing reaction. The prepared oil field sewage purifying agent has better desulfurization and corrosion inhibition effects on high-sulfur-content sewage, has flocculation and sterilization effects of a conventional sewage treating agent, and can be suitable for sewage treatment of high-sulfur-content and common oil and gas fields.
Description
Technical Field
The invention relates to an oilfield sewage purifying agent and a preparation method thereof, belonging to the technical field of oilfield sewage treatment.
Background
The sewage produced by the high-sulfur oil and gas field is generally reinjected into a stratum after being treated, the sewage components generally comprise divalent sulfide salts, dissolved hydrogen sulfide, stratum mineralized substances, oil phase, inorganic salt ions and the like, and experiments show that the conventional polyaluminium chloride coagulant has poor adsorption and net catching effects on the divalent sulfide and is difficult to achieve the aim of sewage flocculation. The prior auxiliary technologies such as alkali neutralization, negative pressure air stripping and the like can only reduce the content of divalent sulfide and can not fundamentally solve the problem of sewage purification.
In recent years, the oilfield sewage purifying agent is gradually applied to the field of oilfield chemical engineering, and is increasingly deeply applied to the field of oil and gas field sewage treatment, and the oilfield sewage purifying agent is combined with the traditional sewage treatment agent, so that the using effect of the sewage treatment agent can be obviously improved by utilizing the strong dispersibility and adsorbability of the oilfield sewage purifying agent. Chinese patent document CN106745367B discloses an iron-based nano sewage treatment agent, which is prepared by compounding surface-modified attapulgite clay, organic silicon rubber waste, an iron-based nano complexing agent, copperas, a dissolution promoter, a regeneration complexing agent and a nano mesoporous molecular sieve, and can be used for carrying out advanced treatment on low-phosphorus sewage after biochemical treatment. The attapulgite clay, the iron-based nano complexing agent and the copperas have strong phosphorus adsorption, but the attapulgite clay suspension is not easy to flocculate and precipitate, the iron-based nano complexing agent mainly removes heavy metals and halogenated organic matters and has poor adsorption effect on divalent sulfides, and the high activity of the iron-based nano complexing agent causes the iron-based nano complexing agent to be easily oxidized, so that the pollutant removal rate is reduced, and the iron-based nano complexing agent is not suitable for treating divalent sulfides and suspended matters in high-sulfur-containing sewage.
Chinese patent document CN106673265B discloses a method for treating high-sulfur-content sewage in oil and gas fields, which comprises the steps of firstly adjusting the pH value of the sewage to 7-8, then adding an oxidant to remove sulfur, and then adding a corrosion inhibitor and a bactericide to completely oxidize hydrogen sulfide, so that the corrosion of the sewage to equipment can be reduced while sulfate ions are not generated. However, the treatment method only has high sulfur removal rate and no flocculation, can not effectively remove suspended matters in the sulfur-containing sewage, and has the disadvantages of non-synchronous corrosion inhibition and sterilization and complex operation process.
Disclosure of Invention
The invention aims to provide a preparation method of an oil field sewage purifying agent, which is used for solving the problem of complex operation process caused by the fact that desulfurization, flocculation, corrosion inhibition and sterilization cannot be carried out simultaneously in the existing oil and gas field high-sulfur-content sewage treatment process.
The invention also aims to provide the oilfield sewage purifying agent.
In order to realize the purpose, the preparation method of the oilfield sewage purifying agent adopts the technical scheme that:
a preparation method of an oilfield sewage purifying agent comprises the following steps: reacting a compound shown in a formula I, a thiol compound shown in a formula II and a particle material; wherein R is 1 、R 2 And R 3 Is hydrogen or alkyl; r 4 And R 7 Is an alkylene group; r 5 、R 6 And R 8 Is an alkyl group; the particle material is beta-Al 2 O 3 And/or gamma-Al 2 O 3 。
The preparation method of the oilfield sewage purifying agent is simple to operate, and the oilfield sewage purifying agent is prepared by taking the compound shown in the formula I and alkyl mercaptan as raw materials, taking a particle material as a catalyst and a catalytic reaction carrier and carrying out mixed reaction. The prepared oil field sewage purifying agent has better desulfurization and corrosion inhibition effects on high-sulfur-content sewage, has flocculation and sterilization effects of a conventional sewage treating agent, and can be suitable for sewage treatment of high-sulfur-content and common oil and gas fields. The positive charges carried in the molecular chains of the organic materials formed after the compound shown in the formula I reacts with mercaptan have a strong adsorption charge neutralization effect, the contained hydroxyl groups have an adsorption bridging effect, the organic materials can be further adsorbed on the surfaces of the particle materials or in the holes of the particle materials or bonded with the particle materials through S in the molecular chains, the molecular chains of the organic materials combined on the particle materials can play a role in catching precipitates, and the long-chain organic amine has corrosion inhibition and sterilization effects.
Preferably, said R is 1 、R 2 And R 3 Each independently selected from hydrogen or C 1 -C 6 An alkyl group. Preferably, said R is 5 、R 6 And R 8 Each independently selected from C 1 -C 6 An alkyl group. Preferably, said R is 4 And R 7 Each independently selected from C 1 -C 5 An alkylene group.
Preferably, said R is 1 Is hydrogen. Preferably, said R is 2 Is hydrogen. Preferably, said R is 3 Is methyl. Preferably, said R is 4 Is an ethylene group. Preferably, said R is 7 Is methylene. Preferably, said R is 5 Is a methyl group. Preferably, said R is 6 Is methyl. Preferably, said R is 8 Is C 2 -C 6 An alkyl group. Preferably, said R is 8 Is C 2 -C 4 An alkyl group. Further preferably, said R 8 Is ethyl, n-propyl or n-butyl.
Preferably, the compound shown in the formula I is (2, 3-epoxypropyl) [2- (methacryloyloxy) ethyl ] dimethyl ammonium chloride, and the structural formula is as follows:
β-Al 2 O 3 and gamma-Al 2 O 3 Has higher surface activity, can adsorb or chemically bond more organic materials, thereby playing better purification effect.
Preferably, the particle size of the particulate material is from 30 to 100nm.
Preferably, the molar ratio of the compound shown in the formula I to the thiol compound shown in the formula II is 1.
Preferably, the mass ratio of the compound shown in the formula I to the thiol compound shown in the formula II is 100.
Preferably, the mass of the particulate material is 1% to 2% of the mass of the thiol compound represented by formula II.
Preferably, the solvent used for the reaction is water.
Preferably, the reaction is carried out under ultrasonic conditions. Further, the reaction system is heated to 50-70 ℃ under the action of ultrasound. The ultrasound functions to provide the energy required for the reaction, i.e., the thermal and kinetic energy required for the reaction.
Preferably, the reaction time is 60-90min.
Preferably, the conditions of the ultrasound include: the ultrasonic power is 50-150W cm -2 (ii) a The frequency is 20-30kHz.
Preferably, the preparation method of the oilfield sewage purifying agent further comprises the following steps: and drying after the reaction.
Preferably, the drying treatment is carried out at 50-70 ℃; the drying time is 3h. And after the drying is finished, naturally cooling to normal temperature, wherein the drying aims to remove water in the oilfield sewage purifying agent.
Preferably, the particle size of the oilfield sewage purifying agent is 50-150nm.
The technical scheme adopted by the oil field sewage purifying agent of the invention is as follows:
an oilfield sewage purifying agent prepared by the preparation method of the oilfield sewage purifying agent.
The oilfield sewage purifying agent has better desulfurization and corrosion inhibition effects on high-sulfur-content sewage, and simultaneously has flocculation and sterilization effects of a conventional sewage treating agent.
Preferably, the particle size of the oilfield sewage purifying agent is 50-150nm.
When the oilfield sewage purifying agent is used for purifying sewage, the addition amount of the oilfield sewage purifying agent in the sewage can be determined according to needs, and preferably, the addition amount of the oilfield sewage purifying agent in the sewage is 100ppm. The addition amount is the ratio of the mass of the oilfield sewage purifying agent to the mass of the sewage.
Drawings
FIG. 1 is a graph showing the relationship between the amount of the oilfield sewage purifying agent prepared in examples 1, 2 and 3 added to sewage and the content of suspended solids in the sewage after purification treatment;
FIG. 2 is a graph showing the relationship between the amount of the oilfield wastewater purifying agent prepared in example 1 added to wastewater and the sulfate-reducing bacteria (SRB), saprophytic bacteria (TGB) and iron bacteria (FB) contents in the wastewater after purification treatment.
Detailed Description
The technical solution of the present invention is further described below with reference to specific examples.
1. The specific embodiment of the preparation method of the oilfield sewage purifying agent of the invention is as follows:
example 1
The preparation method of the oilfield sewage purifying agent comprises the following steps:
100g of (2, 3-epoxypropyl) [2- (methacryloyloxy) ethyl ] ethyl]Dimethyl ammonium chloride, 30g ethanethiol and 1.5g beta-Al with particle size of 30-100nm 2 O 3 Then, water was added to the reaction system to a volume of 600mL, followed by a reaction under ultrasonic conditions for 60 minutes (ultrasonic power 50W. Cm) -2 And the frequency is 20 kHz), the temperature of the reaction system is 70 ℃, the product is dried at 50 ℃ for 3 hours after the reaction is finished, and then the product is cooled to room temperature to obtain particles, namely the oilfield sewage purifying agent prepared by the embodiment has the particle size of 50-150nm.
Example 2
The preparation method of the oilfield sewage purifying agent comprises the following steps:
100g of (2, 3-epoxypropyl) [2- (methacryloyloxy) ethyl ] ethyl]Dimethyl ammonium chloride, 50g of propyl mercaptan and 2.5g of gamma-Al with the particle size of 30-100nm 2 O 3 Then, water was added to the reaction system to a volume of 600mL, followed by a reaction under ultrasonic conditions for 80 minutes (ultrasonic power 100W. Cm) -2 Frequency of 20 kHz), the temperature of the reaction system is 65 ℃, the product is dried at 60 ℃ for 3 hours after the reaction is finished, and then is cooled to room temperature to obtain granules, namely the oilfield sewage purifying agent prepared by the embodiment has the particle size of 50-150nm.
Example 3
The preparation method of the oilfield sewage purifying agent comprises the following steps:
100g of (2, 3-epoxypropyl) [2- (methacryloyloxy) ethyl ] ethyl]Dimethyl ammonium chloride, 60g butyl mercaptan and 3g beta-Al with the grain diameter of 30-100nm 2 O 3 Then, water was added to the reaction system to a volume of 600mL, followed by reaction under ultrasonic conditions for 90 minutes (ultrasonic power 150W. Cm) -2 And the frequency is 30 kHz), the temperature of the reaction system is 60 ℃, the product is dried at 70 ℃ for 3 hours after the reaction is finished, and then the product is cooled to room temperature to obtain particles, namely the oilfield sewage purifying agent prepared by the embodiment has the particle size of 50-150nm.
Example 4
The preparation method of the oilfield sewage purifying agent comprises the following steps:
100g of (2, 3-epoxypropyl) [2- (methacryloyl) was charged in the reaction vesselOxy) ethyl]Dimethyl ammonium chloride, 35g ethanethiol and 2g beta-Al with particle size of 30-100nm 2 O 3 Then, water was added to the reaction system to a volume of 600mL, followed by reaction under ultrasonic conditions for 70 minutes (ultrasonic power 60W. Cm) -2 And the frequency is 20 kHz), the temperature of the reaction system is 70 ℃, the product is dried at 55 ℃ for 3 hours after the reaction is finished, and then the product is cooled to room temperature to obtain particles, namely the oilfield sewage purifying agent prepared by the embodiment has the particle size of 50-150nm.
Example 5
The preparation method of the oilfield sewage purifying agent comprises the following steps:
100g of (2, 3-epoxypropyl) [2- (methacryloyloxy) ethyl ] ethyl]Dimethyl ammonium chloride, 40g of propyl mercaptan and 2g of beta-Al with the particle size of 30-100nm 2 O 3 Then, water was added to the reaction system to a volume of 600mL, followed by a reaction under ultrasonic conditions for 80 minutes (ultrasonic power 70W. Cm) -2 Frequency 25 kHz), the temperature of the reaction system is 60 ℃, the product is dried for 3 hours at 65 ℃ after the reaction is finished, and then the product is cooled to room temperature to obtain particles, namely the oilfield sewage purifying agent prepared by the embodiment has the particle size of 50-150nm.
Example 6
The preparation method of the oilfield sewage purifying agent comprises the following steps:
100g of (2, 3-epoxypropyl) [2- (methacryloyloxy) ethyl ] ethyl]Dimethyl ammonium chloride, 50g butyl mercaptan and 2g beta-Al with particle size of 30-100nm 2 O 3 Then, water was added to the reaction system to a volume of 600mL, followed by reaction under ultrasonic conditions for 90 minutes (ultrasonic power 90W. Cm) -2 And the frequency is 30 kHz), the temperature of the reaction system is 55 ℃, the product is dried for 3 hours at 50 ℃ after the reaction is finished, and then the product is cooled to room temperature to obtain particles, namely the oilfield sewage purifying agent prepared by the embodiment has the particle size of 50-150nm.
Example 7
The preparation method of the oilfield sewage purifying agent comprises the following steps:
100g of (2, 3-epoxypropyl) [2- (methacryloyloxy) ethyl ] ethyl]Dimethyl ammonium chloride, 55g of ethanethiol and 3g of beta-Al with the particle size of 30-100nm 2 O 3 Then, water was added to the reaction system to a volume of 600mL, followed by reaction under ultrasonic conditions for 70 minutes (ultrasonic power 120W. Cm) -2 And the frequency is 25 kHz), the temperature of the reaction system is 70 ℃, after the reaction is finished, the product is dried for 3 hours at the temperature of 60 ℃, and then the product is cooled to the room temperature to obtain the granular material.
Example 8
The preparation method of the oilfield sewage purifying agent comprises the following steps:
100g of (2, 3-epoxypropyl) [2- (methacryloyloxy) ethyl ] ethyl]Dimethyl ammonium chloride, 45g of propyl mercaptan and 3g of beta-Al with the particle size of 30-100nm 2 O 3 Then, water was added to the reaction system to a volume of 600mL, followed by a reaction under ultrasonic conditions for 80 minutes (ultrasonic power 150W. Cm) -2 And the frequency is 30 kHz), the temperature of the reaction system is 65 ℃, the product is dried at 55 ℃ for 3 hours after the reaction is finished, and then the product is cooled to room temperature to obtain particles, namely the oilfield sewage purifying agent prepared by the embodiment has the particle size of 50-150nm.
Example 9
The preparation method of the oilfield sewage purifying agent comprises the following steps:
100g of (2, 3-epoxypropyl) [2- (methacryloyloxy) ethyl ] ethyl]Dimethyl ammonium chloride, 35g of butyl mercaptan and 2g of gamma-Al with the particle size of 30-100nm 2 O 3 Then, water was added to the reaction system to a volume of 600mL, followed by reaction under ultrasonic conditions for 90 minutes (ultrasonic power 80W. Cm) -2 And the frequency is 20 kHz), the temperature of the reaction system is 70 ℃, the product is dried at 65 ℃ for 3 hours after the reaction is finished, and then the product is cooled to room temperature to obtain particles, namely the oilfield sewage purifying agent prepared by the embodiment has the particle size of 50-150nm.
Example 10
The preparation method of the oilfield sewage purifying agent comprises the following steps:
100g of (2, 3-epoxypropyl) [2- (methacryloyloxy) ethyl ] ethyl]Dimethyl ammonium chloride, 40g ethanethiol and 2g gamma-Al with particle size of 30-100nm 2 O 3 Then, water was added to the reaction system to a volume of 600mL, followed by reaction under ultrasonic conditions for 70 minutes (ultrasonic power 100W. Cm) -2 And the frequency is 25 kHz), the temperature of the reaction system is 50 ℃, the product is dried at 70 ℃ for 3 hours after the reaction is finished, and then the product is cooled to room temperature to obtain particles, namely the oilfield sewage purifying agent prepared by the embodiment has the particle size of 50-150nm.
Example 11
The preparation method of the oilfield sewage purifying agent comprises the following steps:
100g of (2, 3-epoxypropyl) [2- (methacryloyloxy) ethyl ] ethyl]Dimethyl ammonium chloride, 50g of propyl mercaptan and 3g of gamma-Al with the particle size of 30-100nm 2 O 3 Then, water was added to the reaction system to a volume of 600mL, followed by a reaction under ultrasonic conditions for 80 minutes (ultrasonic power 120W. Cm) -2 And the frequency is 30 kHz), the temperature of the reaction system is 70 ℃, the product is dried at 50 ℃ for 3 hours after the reaction is finished, and then the product is cooled to room temperature to obtain particles, namely the oilfield sewage purifying agent prepared by the embodiment has the particle size of 50-150nm.
Example 12
The preparation method of the oilfield sewage purifying agent comprises the following steps:
100g of (2, 3-epoxypropyl) [2- (methacryloyloxy) ethyl ] ethyl]Dimethyl ammonium chloride, 45g of butyl mercaptan and 3g of gamma-Al with the particle size of 30-100nm 2 O 3 Then, water was added to the reaction system to a volume of 600mL, followed by reaction under ultrasonic conditions for 90 minutes (ultrasonic power 140W. Cm) -2 And the frequency is 30 kHz), the temperature of the reaction system is 60 ℃, the product is dried at 60 ℃ for 3 hours after the reaction is finished, and then the product is cooled to room temperature to obtain particles, namely the oilfield sewage purifying agent prepared by the embodiment has the particle size of 50-150nm.
2. The specific embodiment of the oilfield sewage purifying agent of the invention is as follows:
the oilfield sewage purifying agent of the embodiment is prepared by the preparation method of the oilfield sewage purifying agent of any one of embodiments 1 to 12. When the oilfield sewage purification agent of the embodiment is used for purifying sewage, the addition amount of the oilfield sewage purification agent in the sewage is 100ppm, and the addition amount is the ratio of the mass of the oilfield sewage purification agent to the mass of the sewage.
Examples of the experiments
The oilfield sewage purifying agents prepared in the examples 1, 2 and 3 are respectively applied to a purification treatment process (the oilfield sewage purifying agent is added into a water sample and stirred) of high-sulfur-content sewage (the sulfur content is about 3000 mg/L) of a certain gas field, the addition amounts of different oilfield sewage purifying agents in the high-sulfur-content sewage of the gas field are respectively 0ppm, 30ppm, 50ppm, 80ppm, 100ppm, 120ppm, 150ppm, 180ppm and 200ppm, the addition amounts are ratios of the quality of the oilfield sewage purifying agent to the quality of the sewage, and the sulfur content, the suspended solid content, the bacterial content and the corrosion rate in the purified sewage are respectively tested according to the specification of SY/T5329-2012 'clastic rock oil reservoir water injection quality index and analysis method'. Experimental results show that when the contents of different oil field sewage purifiers added into the high-sulfur-content gas field sewage are all 100ppm, the sulfur removal rate can reach more than 99%. As shown in FIG. 1, the suspended solid content in the purified sewage is less than 2mg/L, as can be seen from FIG. 1, when the addition amount of different oilfield sewage purifiers in the sewage is greater than 100ppm. The relationship between the Sulfate Reducing Bacteria (SRB) content, saprophytic bacteria (TGB) content and iron bacteria (FB) content of the purified wastewater and the amount of the oilfield wastewater purification agent prepared in example 1 is shown in fig. 2, and it can be seen from fig. 2 that when the amount of the oilfield wastewater purification agent prepared in example 1 added to wastewater is greater than 60ppm, the amounts of different bacteria in the purified wastewater are all less than 10/mL. The relationship between the corrosion rate and the addition amount of different oilfield sewage purifying agents in sewage is shown in Table 1, and it can be seen from Table 1 that when the contents of different oilfield sewage purifying agents added in sewage are all more than 100ppm, the corrosion rates are all less than 0.076mm/a. The above experiment was repeated with the oilfield wastewater purification agent prepared in other embodiments of the present invention, and the sulfur content, suspended solids content, bacteria content and corrosion rate in the purified wastewater were tested to obtain the same conclusions.
TABLE 1 relationship between the amount of different oilfield sewage purifiers added to sewage and the corrosion rate
According to experimental results, when the addition amounts of different oil field sewage purifying agents in high-sulfur-content sewage of a gas field are all 100ppm, the removal, sterilization and corrosion inhibition effects of suspended matters of the oil field sewage purifying agents meet the water quality index requirements of SY/T5329-2012 'water injection quality index and analysis method for clastic rock oil reservoirs', namely, the solid content of the suspended matters is less than 3mg/L, the content of Sulfate Reducing Bacteria (SRB) is less than or equal to 25/mL, the content of saprophytic bacteria (TGB) is less than or equal to 100/mL, the content of iron bacteria (FB) is less than or equal to 100/mL, and the corrosion rate is less than 0.076mm/a. When the addition amount of the oilfield sewage purifying agent in the high-sulfur-content sewage of the gas field is higher than 100ppm, the effects of removing suspended matters, sterilizing and inhibiting corrosion are not obviously improved, but the cost is obviously increased. Therefore, when the oil field sewage purifying agent is applied to the gas field high-sulfur-content sewage, the addition amount of the oil field sewage purifying agent in the sewage is 100ppm.
Claims (10)
1. The preparation method of the oilfield sewage purifying agent is characterized by comprising the following steps: reacting a compound shown in a formula I, a thiol compound shown in a formula II and a particle material; wherein R is 1 、R 2 And R 3 Is hydrogen or alkyl; r 4 And R 7 Is an alkylene group; r is 5 、R 6 And R 8 Is an alkyl group; the particle material is beta-Al 2 O 3 And/or gamma-Al 2 O 3 。
2. The method for preparing the oilfield sewage purifying agent according to claim 1, wherein R is R 1 、R 2 And R 3 Each independently selected from hydrogen or C 1 -C 6 An alkyl group; said R is 5 、R 6 And R 8 Each independently selected from C 1 -C 6 An alkyl group; the R is 4 And R 7 Each independently selected from C 1 -C 5 An alkylene group.
3. The method for preparing the oilfield sewage purifying agent according to claim 2, wherein R is R 1 Is hydrogen; the R is 2 Is hydrogen; said R is 3 Is methyl; said R is 5 Is methyl; the R is 6 Is methyl; the R is 8 Is ethyl, n-propyl or n-butyl; the R is 4 Is an ethylene group; the R is 7 Is methylene.
4. The method for preparing the oilfield sewage purifying agent according to claim 1, wherein the reaction is performed under ultrasonic conditions; the conditions of the ultrasound include: the ultrasonic power is 50-150W cm -2 (ii) a The frequency is 20-30kHz.
5. The method for preparing the oilfield sewage purifying agent according to claim 1, further comprising the steps of: after the reaction is finished, the reaction system is dried.
6. The method for preparing the oilfield sewage purifying agent according to claim 1, wherein the particle size of the particulate material is 30-100nm.
7. The method for preparing the oilfield sewage purifying agent according to claim 1, wherein the molar ratio of the compound represented by the formula I to the thiol compound represented by the formula II is 1.95-2.3.
8. The method for preparing the oilfield sewage purifying agent according to claim 1, wherein the mass of the particulate material is 1% to 2% of the mass of the thiol compound represented by formula II.
9. An oilfield sewage purifying agent prepared by the method for preparing an oilfield sewage purifying agent according to any one of claims 1 to 8.
10. The oilfield sewage purifying agent of claim 9, wherein the oilfield sewage purifying agent has a particle size of 50-150nm.
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| WO2011107764A1 (en) * | 2010-03-04 | 2011-09-09 | Johnson Matthey Plc | Sorbents |
| CN102718991A (en) * | 2012-04-05 | 2012-10-10 | 天津大学 | High strength injectable hydrogel and preparation method thereof |
| WO2018086100A1 (en) * | 2016-11-14 | 2018-05-17 | 江苏华安科研仪器有限公司 | Oil wastewater treatment agent for oil field |
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