CN114736142B - Oil field sewage sterilization and degreasing agent, and synthetic method and application thereof - Google Patents
Oil field sewage sterilization and degreasing agent, and synthetic method and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C303/00—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
- C07C303/32—Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
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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
- C02F1/40—Devices for separating or removing fatty or oily substances or similar floating material
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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
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/04—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups
- C07C209/06—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups by substitution of halogen atoms
- C07C209/12—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups by substitution of halogen atoms with formation of quaternary ammonium compounds
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- C—CHEMISTRY; METALLURGY
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C309/00—Sulfonic acids; Halides, esters, or anhydrides thereof
- C07C309/01—Sulfonic acids
- C07C309/02—Sulfonic acids having sulfo groups bound to acyclic carbon atoms
- C07C309/03—Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton
- C07C309/13—Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton containing nitrogen atoms, not being part of nitro or nitroso groups, bound to the carbon skeleton
- C07C309/14—Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton containing nitrogen atoms, not being part of nitro or nitroso groups, bound to the carbon skeleton containing amino groups bound to the carbon skeleton
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention belongs to the technical field of sewage treatment, and particularly relates to an oil field sewage sterilization and oil removal agent, a synthesis method and application. The synthesis method comprises the following steps: adding tertiary amine, dihalo butene, isobutanol and copper chloride into a four-neck flask protected by nitrogen, stirring, heating, and carrying out reflux reaction to obtain an intermediate crude product; carrying out rotary evaporation on the crude intermediate product until the crude intermediate product is dry, adding water, heating, standing for layering, carrying out rotary evaporation on a lower-layer water phase until the lower-layer water phase is dry, and recrystallizing to obtain a pure intermediate product; adding the intermediate pure product into a four-neck flask, adding ethanol and sodium bisulfite, stirring, heating, and carrying out reflux reaction to obtain a product crude product; and (4) carrying out rotary evaporation on the crude product until the crude product is dried, and recrystallizing to obtain the sterilizing and degreasing agent. The sterilization degreasing agent has the characteristics of simple synthesis process, small using amount and low cost; the sterilization rate can reach 100% when the use concentration is 20 mg/L; the oil removal rate can reach more than 99 percent when the using concentration is 50 mg/L.
Description
Technical Field
The invention belongs to the technical field of sewage treatment, and particularly relates to an oil field sewage sterilization and oil removal agent, a synthesis method and application.
Background
At present, the pressure of an oil layer is gradually reduced in the process of oil field development, and the yield of crude oil is reduced along with the reduction, so that technological measures must be taken to supplement energy to the stratum in time so as to keep the oil layer at a certain pressure. The most effective technical measure is to inject a large amount of water into the stratum to supplement the stratum deficit energy, but the injected water is recycled, the components in the water are more and more complex, and various bacteria are easy to breed, mainly comprising sulfate reducing bacteria, saprophytic bacteria and iron bacteria. These bacteria growth, metabolism and propagation can cause corrosion and damage to drilling equipment and water injection pipelines and other metal materials, plugging of pipelines and water injection wells, resulting in reduced permeability of oil reservoir pores, hindering water injection and oil recovery, and directly affecting crude oil production. Therefore, the sewage is sterilized before reinjection, but the existing bactericide for oilfield produced water is single in variety, and can cause bacteria to generate certain drug resistance after long-term use, so that the using effect of the bactericide is remarkably reduced.
In addition, part of oil field reinjection water contains polymers, so that the viscosity of sewage is increased by times, and the oil carrying capacity of a water phase is increased; the oil droplets in the sewage have small particle size and oil droplets stably exist in the water; the sewage is easy to be sheared and further emulsified, the oil-water separation is difficult due to the reasons, and the treated sewage cannot meet the reinjection requirement of an oil well. Therefore, the sewage needs to be deoiled, and a common physical method such as air floatation is to introduce air into the sewage to generate micro bubbles as a carrier, so that pollutants such as emulsified oil, micro suspended matters and the like in the sewage are adhered to the bubbles to form a floatation body, and the floatation body is lifted to the water surface by utilizing the floatation action of the bubbles, so as to achieve the purposes of separating impurities and purifying the sewage by collecting foams or scum on the water surface. The air floatation oil removal cost is low, but two problems exist: firstly, oxygen is introduced in the air floatation process, so that corrosion to oil well equipment can be caused, secondly, the pure air floatation treatment effect is not ideal, and the better effect can be achieved by matching with chemical agents. At present, the oil removal by novel chemical agents draws more and more attention of people.
CN104488874A discloses a compound bactericide for an oil field water injection system. The composite bactericide for the oilfield water injection system is characterized by comprising, by weight, 0-80% of an aqueous solution of benzalkonium chloride with the mass fraction of 45-55%, 10-20% of an ethanol solution of cetylpyridinium bromide with the mass fraction of 25-35%, and 10-15% of a xylene solution of tetrachloroisophthalonitrile with the mass fraction of 18-22%. Has the advantages of simple components, convenient preparation, high sterilization rate and the like. However, the compound component contains a large amount of cetylpyridinium bromide, and the cetylpyridinium bromide has increased toxicity, and can cause secondary pollution and environmental damage after being used.
ZL201410254042.8 discloses a compound flocculation degreasing agent for oily sewage treatment, which is formed by compounding aluminum sulfate, magnesium chloride, magnesium hydroxide, bentonite and polyacrylamide, and has the characteristics of low consumption, high degreasing efficiency, simple preparation, low cost and the like, but the degreasing agent needs to use the magnesium hydroxide with corrosivity, and the compound has stronger corrosion effect on equipment.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides an oil field sewage sterilization and oil removal agent, a synthesis method and application thereof. The sterilization degreasing agent has the characteristics of simple synthesis process, small using amount, low cost and multiple functions of one agent; the sterilization rate can reach 100% when the using concentration is 20 mg/L; the oil removal rate can reach more than 99 percent when the using concentration is 50 mg/L.
Therefore, in order to achieve the above object, in one aspect, the invention discloses a sterilization and degreasing agent for oilfield sewage, wherein the molecular structural formula of the sterilization and degreasing agent is as follows:
wherein:
r is C 8 -C 18 Alkyl groups of (a);
x is one of chlorine, bromine and iodine.
On the other hand, the invention provides a synthesis method of the oil field sewage sterilization and oil removal agent, which comprises the following specific steps:
(1) adding tertiary amine, dihalo butene, isobutanol and copper chloride into a four-neck flask protected by nitrogen, stirring, heating, and carrying out reflux reaction to obtain a biquaternary ammonium salt intermediate crude product;
(2) carrying out rotary evaporation on the crude intermediate product until the crude intermediate product is dry, adding water, heating to 60-65 ℃, standing for layering, carrying out rotary evaporation on a lower water phase until the lower water phase is dry, and recrystallizing with ethyl acetate to obtain a pure biquaternary ammonium salt intermediate product;
(3) adding the pure biquaternary ammonium salt intermediate into a four-neck flask, adding 95wt% ethanol and sodium bisulfite, stirring, heating, and carrying out reflux reaction to obtain a crude product;
(4) and (4) carrying out rotary evaporation on the crude product until the crude product is dried, and recrystallizing with ethyl acetate to obtain the sterilizing and degreasing agent.
The third purpose of the invention discloses the application of the oil field sewage sterilization and oil removal agent in oil field sewage sterilization and oil removal.
The oil field sewage sterilizing and oil removing agent is a dication monoanionic surfactant, two cations are quaternary ammonium salts, and the anion is sulfonate. The surface of the bacteria is negatively charged and is easier to adsorb molecules with positive charges, thereby changing the permeability of cell walls and leading components in the bacterial cells to leak out and die. The quaternary ammonium cation can form hydrogen bonds with base groups of deoxyribonucleic acid (DNA) in proteins in bacteria, and the hydrogen bonds are adsorbed on cells of the bacteria to destroy the DNA structure of the bacteria, so that the bacteria lose the replication capacity and die. Quaternary ammonium salt and sulfonate in the molecule are hydrophilic groups and can be in close contact with water and interact with the water; the long-chain alkyl is a hydrophobic group, has lipophilicity, can be adsorbed with oil in sewage, can penetrate into the oil stain, and can generate similar intermiscibility with alkane, aromatic hydrocarbon, colloid and asphaltene in crude oil. The surfactant molecules extract emulsified oil and dissolved oil in the sewage through permeation, emulsification and stripping to form stable floccules which are dispersed and float on the surface of the solution, so that the aim of oil removal treatment of the sewage is fulfilled.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the sterilization and oil removal agent has the advantages of wide raw material source, simple synthesis process, strong adaptability and small dosage, and can meet the sterilization requirements of different sewage;
(2) the sterilization and oil removal agent has the advantages of low-concentration and high-efficiency sterilization, and the sterilization rate can reach 100% when the use concentration is 20 mg/L;
(3) the sterilization degreasing agent has the advantage of low-concentration efficient degreasing, and the degreasing rate can reach more than 99% when the use concentration is 50 mg/L.
Drawings
FIG. 1 shows a bactericidal degreaser Q 6 The infrared spectrum of the sample is shown.
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 numerical ranges, each range between its endpoints and individual point values, and each individual point value can be combined with each other to give one or more new numerical ranges, and such numerical ranges should be construed as specifically disclosed herein.
According to the first aspect of the invention, the invention discloses a sterilization and degreasing agent for oilfield sewage, which has the following molecular structural formula:
wherein:
r is C 8 -C 18 Alkyl of (2), preferably C 8 -C 18 More preferably C 12 -C 16 The linear alkyl group of (1);
x is one of chlorine, bromine and iodine, and bromine or iodine is more preferable.
In a second aspect, the invention provides a method for synthesizing the sterilization and degreasing agent, which comprises the following specific steps:
(1) adding tertiary amine, dihalo butene, isobutanol and copper chloride into a four-neck flask protected by nitrogen, stirring, heating, and carrying out reflux reaction to obtain a biquaternary ammonium salt intermediate crude product;
(2) carrying out rotary evaporation on the crude intermediate product until the crude intermediate product is dry, adding water, heating to 60-65 ℃, standing for layering, carrying out rotary evaporation on a lower water phase until the lower water phase is dry, and recrystallizing with ethyl acetate to obtain a pure biquaternary ammonium salt intermediate product;
(3) adding the pure biquaternary ammonium salt intermediate into a four-neck flask, adding 95wt% ethanol and sodium bisulfite, stirring, heating, and carrying out reflux reaction to obtain a crude product;
(4) and (3) carrying out rotary evaporation on the crude product until the crude product is dried, and recrystallizing with ethyl acetate to obtain the sterilizing and degreasing agent.
Preferably, in the step (1), the tertiary amine is one of N, N-dimethyloctylamine, N-dimethyldecylamine, N-dimethyldodecylamine, N-dimethyltetradecylamine, N-dimethylhexadecylamine, and N, N-dimethyleicosylamine.
Preferably, in the step (1), the dihalobutene is one of 1, 4-dichloro-2-butene, 1, 4-diiodo-2-butene and 1, 4-dibromo-2-butene.
In the present invention, preferably, the dihalobutene and the sodium bisulfite are used in amounts of 0.5 to 0.6 parts by mole and 0.5 to 0.7 parts by mole, respectively, based on 1 part by mole of the tertiary amine; preferably, the dihalobutene and the sodium bisulfite are used in amounts of 0.52 to 0.58 parts by mole and 0.52 to 0.65 parts by mole, respectively, based on 1 part by mole of the tertiary amine.
Preferably, in the step (1), the mass ratio of isobutanol, copper chloride and tertiary amine is 20-30: 0.05-0.1: 1; more preferably, the mass ratio of isobutanol, copper chloride to tertiary amine is 25-30: 0.05-0.07: 1.
preferably, in the step (1), the reflux reaction time is 24-48 h; more preferably, the reflux reaction time is 32-42 h.
In the present invention, it is preferable that in the step (2), the mass ratio of the water to the tertiary amine is 10-20: 1; more preferably, the mass ratio of water to tertiary amine is 12-15: 1.
In the present invention, preferably, in the step (3), the mass ratio of ethanol to tertiary amine is 20 to 30: 1; more preferably, the mass ratio of ethanol to tertiary amine is 20-25: 1.
preferably, in the step (3), the reflux reaction time is 24-48 h; more preferably, the reflux reaction time is 30-36 h.
The reaction equation for synthesizing the oil field sewage sterilization and oil removal agent is as follows:
the third purpose of the invention discloses the application of the sterilization and degreasing agent in sterilization and degreasing of oil field sewage. The specific application is not particularly required, and can be a conventional application mode in the field, and the detailed description is not repeated.
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 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.
Example 1:
(1) adding 0.1mol of N, N-dimethyl octylamine, 0.05mol of 1, 4-dichloro-2-butene, 471g of isobutanol and 1.57g of copper chloride into a four-neck flask protected by nitrogen, stirring, heating, and carrying out reflux reaction for 24 hours to obtain a crude biquaternary ammonium salt intermediate product;
(2) carrying out rotary evaporation on the crude intermediate product until the crude intermediate product is dried, adding 314g of water, heating to 60-65 ℃, standing for layering, carrying out rotary evaporation on a lower-layer water phase until the lower-layer water phase is dried, and recrystallizing by using ethyl acetate to obtain a pure biquaternary ammonium salt intermediate product;
(3) adding the pure biquaternary ammonium salt intermediate into a four-neck flask, adding 471g of 95wt% ethanol and 0.05mol of sodium bisulfite, stirring, heating, refluxing and reacting for 24 hours to obtain a crude product;
(4) the crude product is steamed to be dry in a rotating way and recrystallized by ethyl acetate to obtain the sterilizing and degreasing agent Q 1 。
Said Q 1 The molecular formula is:
example 2:
(1) adding 0.1mol of N, N-dimethyl decylamine, 0.06mol of 1, 4-diiodo-2-butene, 492g of isobutanol and 1.52g of copper chloride into a four-neck flask protected by nitrogen, stirring, heating, and carrying out reflux reaction for 30 hours to obtain a crude biquaternary ammonium salt intermediate product;
(2) carrying out rotary evaporation on the crude intermediate product until the crude intermediate product is dried, adding 300g of water, heating to 60-65 ℃, standing for layering, carrying out rotary evaporation on a lower-layer water phase until the lower-layer water phase is dried, and recrystallizing with ethyl acetate to obtain a pure biquaternary ammonium salt intermediate product;
(3) adding the pure biquaternary ammonium salt intermediate into a four-neck flask, adding 498g of 95wt% ethanol and 0.07mol of sodium bisulfite, stirring, heating, refluxing and reacting for 30 hours to obtain a crude product;
(4) the crude product is evaporated to be dry and recrystallized by ethyl acetate to obtain the sterilization degreaser Q 2 。
Said Q 2 The molecular formula is:
example 3:
(1) adding 0.1mol of N, N-dimethyldodecylamine, 0.052mol of 1, 4-diiodo-2-butene, 514g of isobutanol and 1.48g of copper chloride into a four-neck flask protected by nitrogen, stirring, heating, and carrying out reflux reaction for 36 hours to obtain a crude biquaternary ammonium salt intermediate product;
(2) carrying out rotary evaporation on the crude intermediate product until the crude intermediate product is dry, adding 289g of water, heating to 60-65 ℃, standing for layering, carrying out rotary evaporation on a lower-layer water phase until the lower-layer water phase is dry, and recrystallizing with ethyl acetate to obtain a pure biquaternary ammonium salt intermediate product;
(3) adding the pure biquaternary ammonium salt intermediate into a four-neck flask, adding 512g of 95wt% ethanol and 0.055mol of sodium bisulfite, stirring, heating, carrying out reflux reaction for 36h, and obtaining a crude product;
(4) the crude product is steamed to be dry in a rotating way and recrystallized by ethyl acetate to obtain the sterilizing and degreasing agent Q 3 。
Said Q 3 The molecular formula is:
example 4:
(1) adding 0.1mol of N, N-dimethyl tetradecylamine, 0.055mol of 1, 4-dibromo-2-butene, 516g of isobutanol and 1.48g of copper chloride into a four-neck flask protected by nitrogen, stirring, heating, and carrying out reflux reaction for 48 hours to obtain a biquaternary ammonium salt intermediate crude product;
(2) carrying out rotary evaporation on the crude intermediate product until the crude intermediate product is dry, adding 295g of water, heating to 60-65 ℃, standing for layering, carrying out rotary evaporation on a lower-layer water phase until the lower-layer water phase is dry, and recrystallizing with ethyl acetate to obtain a pure biquaternary ammonium salt intermediate product;
(3) adding the pure biquaternary ammonium salt intermediate into a four-neck flask, adding 516g of 95wt% ethanol and 0.06mol of sodium bisulfite, stirring, heating, and carrying out reflux reaction for 48 hours to obtain a crude product;
(4) the crude product is evaporated to dryness and recrystallized by ethyl acetate to obtain the pesticideBacteria degreasing agent Q 4 。
Said Q 4 The molecular formula is:
example 5:
(1) adding 0.1mol of N, N-dimethyl hexadecylamine, 0.053mol of 1, 4-dibromo-2-butene, 538g of isobutanol and 1.35g of copper chloride into a four-neck flask protected by nitrogen, stirring, heating, and carrying out reflux reaction for 48 hours to obtain a biquaternary ammonium salt intermediate crude product;
(2) carrying out rotary evaporation on the crude intermediate product until the crude intermediate product is dried, adding 269g of water, heating to 60-65 ℃, standing for layering, carrying out rotary evaporation on a lower-layer water phase until the lower-layer water phase is dried, and recrystallizing with ethyl acetate to obtain a pure biquaternary ammonium salt intermediate product;
(3) adding the pure biquaternary ammonium salt intermediate into a four-neck flask, adding 538g of 95wt% ethanol and 0.055mol of sodium bisulfite, stirring, heating, carrying out reflux reaction for 48 hours, and obtaining a crude product;
(4) the crude product is evaporated to be dry and recrystallized by ethyl acetate to obtain the sterilization degreaser Q 5 。
Said Q 5 The molecular formula is:
example 6:
(1) adding 0.1mol of N, N-dimethyldodecylamine, 0.054mol of 1, 4-dibromo-2-butene, 502g of isobutanol and 1.46g of copper chloride into a four-necked flask protected by nitrogen, stirring, heating, and carrying out reflux reaction for 48 hours to obtain a crude biquaternary ammonium salt intermediate product;
(2) carrying out rotary evaporation on the crude intermediate product until the crude intermediate product is dried, adding 288g of water, heating to 60-65 ℃, standing for layering, carrying out rotary evaporation on a lower-layer water phase until the lower-layer water phase is dried, and recrystallizing with ethyl acetate to obtain a pure biquaternary ammonium salt intermediate product;
(3) adding the pure biquaternary ammonium salt intermediate into a four-neck flask, adding 515g of 95wt% ethanol and 0.055mol of sodium bisulfite, stirring, heating, refluxing and reacting for 48 hours to obtain a crude product;
(4) the crude product is evaporated to be dry and recrystallized by ethyl acetate to obtain the sterilization degreaser Q 6 。
Said Q 6 The molecular formula is:
example 7: characterization of the Infrared Spectrum
Product sterilization and oil removal agent Q by adopting infrared spectrum 6 The characterization was performed and the results are shown in fig. 1.
As can be seen from FIG. 1, 2928cm -1 Is abundantly present in the molecule
A key expansion vibration absorption peak; 1192cm -1 Is a sulfonate salt
A key expansion vibration absorption peak; 1009cm -1 、678cm -1 Is in quaternary ammonium salt
Key stretching vibration and bending vibration absorption peaks.
Example 8: evaluation of Sterilization Rate
Respectively adding 500ml of water sample of a United station at the south of the Yangli oil field oil extraction plant, which contains SRB (sulfate reducing bacteria), TGB (saprophytic bacteria) and FB (iron bacteria), into a series of narrow-mouth bottles, and adding Q with different concentrations 1 -Q 6 And mixing with the bactericide, shaking uniformly, placing in a 60 ℃ oven, sampling after 1h, detecting the content of the residual bacteria by adopting a three-tube method MPN, and calculating the sterilization rate.
Table 1 SRB sterilization results (sterilization rate,%)
As can be seen from table 1: the invention relates to a sterilization degreaser Q 1 -Q 6 The sterilization rate of the SRB reaches more than 85 percent and the highest sterilization rate reaches 96.5 percent (Q) when the using concentration is 10mg/L 6 ) (ii) a The sterilization rate of SRB reaches 100% when the using concentration is 20mg/L or more; and the dichlorophenol and 1227 have respective sterilization rates of 0 and 0 for SRB at a use concentration of 10mg/L and 59.1% and 81.8% for SRB at a use concentration of 20 mg/L. Compared with the existing sterilization degreasing agent, the sterilization degreasing agent has good sterilization effect on SRB.
TABLE 2 TGB Sterilization results (Sterilization Rate,%)
As can be seen from table 2: the invention relates to a sterilization degreaser Q 1 -Q 6 The sterilization rate of TGB reaches more than 83 percent and reaches 96.2 percent at the highest when the use concentration is 10mg/L (Q) 6 ) (ii) a The sterilization rate of TGB reaches 100% when the use concentration is 20mg/L or more; and diclofenac and 1227 showed 0 and 0 sterilization rates of TGB at a concentration of 10mg/L and 55.6% and 64.4% sterilization rates of TGB at a concentration of 20mg/L, respectively. Compared with the existing sterilization degreasing agent, the sterilization degreasing agent has good sterilization effect on TGB.
TABLE 3 FB Sterilization results (Sterilization Rate,%)
As can be seen from table 3: the invention relates to a sterilization degreaser Q 1 -Q 6 The sterilization rate to FB reaches more than 91 percent and the highest sterilization rate to FB reaches 98.4 percent when the use concentration is 10mg/L (Q) 6 ) (ii) a The sterilization rate to FB reaches 100% when the use concentration is 20mg/L or more; and diclofenac and 1227 had respective sterilization rates for FB of 0 and 0 at a use concentration of 10mg/L and 55.6% and 64.4% at a use concentration of 20 mg/L. Compared with the existing sterilization degreasing agent, the sterilization degreasing agent has the sterilization effect on FBIs good.
Example 9 evaluation of degreasing effect
The indoor evaluation oil-containing sewage is produced water of a certain block of a Shengli oilfield estuary oil production plant, the oil content of the sewage is 517mg/L, 1000ml of the sewage is added into a series of beakers respectively, and Q with different concentrations is added into the beakers respectively 1 -Q 6 And an oil removal agent, stirring for 60S at a stirring speed of 100rpm, standing for 15min, taking lower-layer water to test oil content, and calculating the oil removal rate.
Table 4 oil removal effect (oil removal rate,%)
As can be seen from table 4: the invention relates to a sterilization degreaser Q 1 -Q 6 The oil removal rate reaches over 90 percent and reaches 92.6 percent (Q) at the maximum when the using concentration is 10mg/L 6 ) (ii) a The oil removal rate reaches more than 99 percent when the using concentration is 50 mg/L; and the oil removal agent SGR1711 has an oil removal rate of 36.6% at a use concentration of 10mg/L and an oil removal rate of 95.3% at a use concentration of 50 mg/L. Compared with the existing sterilization and degreasing agent, the sterilization and degreasing agent has better oil removing effect on oily sewage.
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 (8)
1. The oil field sewage sterilizing and oil removing agent is characterized in that the molecular structural formula of the oil field sewage sterilizing and oil removing agent is as follows:
wherein:
r is C 12 -C 16 The linear alkyl group of (1);
x is bromine or iodine.
2. The synthesis method of the oil field sewage sterilization and oil removal agent according to claim 1 is characterized by comprising the following steps:
(1) adding tertiary amine, dihalo butene, isobutanol and copper chloride into a four-neck flask protected by nitrogen, stirring, heating, and carrying out reflux reaction to obtain a biquaternary ammonium salt intermediate crude product;
(2) carrying out rotary evaporation on the crude intermediate product until the crude intermediate product is dry, adding water, heating to 60-65 ℃, standing for layering, carrying out rotary evaporation on a lower water phase until the lower water phase is dry, and recrystallizing with ethyl acetate to obtain a pure biquaternary ammonium salt intermediate product;
(3) adding the pure biquaternary ammonium salt intermediate into a four-neck flask, adding 95wt% ethanol and sodium bisulfite, stirring, heating, and carrying out reflux reaction to obtain a crude product;
(4) carrying out rotary evaporation on the crude product until the crude product is dried, and recrystallizing with ethyl acetate to obtain a sterilization degreasing agent;
the tertiary amine is one of N, N-dimethyldodecylamine, N-dimethyltetradecylamine and N, N-dimethylhexadecylamine;
the dihalo-butene is one of 1, 4-diiodo-2-butene and 1, 4-dibromo-2-butene.
3. The method of claim 2, wherein the dihalobutene and the sodium bisulfite are used in an amount of 0.5 to 0.6 parts by mole and 0.5 to 0.7 parts by mole, respectively, based on 1 part by mole of the tertiary amine.
4. The synthesis method according to claim 3, wherein the dihalobutene and the sodium bisulfite are used in amounts of 0.52 to 0.58 mol parts and 0.52 to 0.65 mol parts, respectively, based on 1mol part of the tertiary amine.
5. The synthesis method according to claim 2, wherein in the step (1), the mass ratio of isobutanol, copper chloride to tertiary amine is 20-30: 0.05-0.1: 1.
6. the synthesis method of claim 2, wherein in the step (1), the reflux reaction time is 24-48 h.
7. The synthesis method of claim 2, wherein in the step (3), the reflux reaction time is 24-48 h.
8. The application of the oil field sewage sterilization and oil removal agent according to claim 1, wherein the application is the application in oil field sewage sterilization and oil removal.
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