CN113402000A - Flotation agent for treating oily sewage in oil field and preparation method thereof - Google Patents
Flotation agent for treating oily sewage in oil field and preparation method thereof Download PDFInfo
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/24—Treatment of water, waste water, or sewage by flotation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2618—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen
- C08G65/2621—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen containing amine groups
- C08G65/2624—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing nitrogen containing amine groups containing aliphatic amine groups
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/32—Hydrocarbons, e.g. oil
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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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Abstract
The invention provides a flotation agent for treating oily sewage in an oil field and a preparation method thereof, wherein polyamine, long-chain alkyl dimethyl tertiary amine, 1, 6-hexamethylene diamine and distilled water are mixed and then placed at 30-40 ℃, stirred and reacted for 0.1-0.3h, epoxy chloropropane is dripped into a reaction container, and after the dripping is finished, the reaction is continued for 2-4h at 30-40 ℃; and continuously heating to 45-55 ℃, continuously reacting for 1-3h at 45-55 ℃, continuously heating to 65-75 ℃, and continuously reacting for 2-4h at 65-75 ℃ to obtain the flotation agent for treating the oily sewage in the oil field. The flotation agent has higher cationic degree and surface activity, can quickly reduce the surface tension of the oily sewage in the oil field, thereby reducing the surface tension of water, facilitating the acquisition of micro bubbles after air entraining, enhancing the adhesion degree of the bubbles and suspended matters, achieving better water purification effect, being very suitable for the treatment of the oily sewage in the offshore oil field, and having the characteristics of small dosage, strong foamability, excellent water purification effect, high oil removal rate and the like.
Description
Technical Field
The invention relates to the technical field of oil-gas-water treatment, in particular to a flotation agent for treating oily sewage in an oil field and a preparation method thereof.
Background
The comprehensive water content of the produced liquid gradually rises along with the oil field exploitation in the middle and later stages, the water yield gradually rises under the condition of ensuring the oil yield and the stable yield, and the treatment capacity of the current treatment facility is close to saturation. The yield of crude oil in offshore oil fields is increased, and the discharge amount of water production and oil-containing pollutants is increased rapidly. The problems of short sewage treatment time, different characteristics, large treatment capacity and the like of the offshore oil field are solved, and the problem puzzling the offshore oil field production to be solved urgently is solved. In recent years, the social requirements on environmental protection, energy conservation and emission reduction are continuously increased, and the offshore oilfield oily sewage treatment faces more serious challenges. In order to alleviate the contradiction between the treatment capacity of the equipment and the increase of the treatment capacity of the oily sewage, the treatment capacity of the existing facility must be improved by adding a flotation agent.
The development of flotation machines drives the development of the variety and the performance of flotation agents, and early flotation agents are inorganic small-molecular compounds, such as alum, aluminum trichloride, ferric trichloride, ferrous sulfate and the like, but the flotation agents have the defects of large exposure dosage, more residues and the like in application. In 60-70 years of the 20 th century, polyaluminium chloride and polyaluminium sulfate were developed successively in Japan, and at present, the two agents are still used for air floatation treatment of sewage of oil refineries in China. The organic cation polymer flotation agent is developed in 80 years and is widely applied due to the advantages of small using amount, high demulsification efficiency, low residue and the like. In 90 years, the research pace of organic macromolecular flotation agents is accelerated and some agents are developed successively in oil fields in China aiming at the water quality characteristics of oily sewage, and at present, deep research is still carried out. At present, foreign flotation agents are developed more mature, but the difference between the domestic flotation agents and foreign developed countries is larger. Compared with foreign countries, the organic water treatment medicament in China has fewer varieties and is more extensive in use. The research, production and application of the organic polymer flotation agent in China still belong to weak links. There is also a great gap compared to developed countries abroad. The main points are as follows:
(1) the research on the action mechanism of the flotation agent is not enough
In the middle of the 70's of the 20 th century abroad, the air flotation principle is researched. Because the flotation agent in China mainly adopts the coagulant, the research on the flotation mechanism of the coagulant is deeper, and the research on the flotation action mechanism of the organic macromolecular flotation agent is less. The current domestic research work is mainly focused on practical application, and the system research aiming at the basic aspects of the action mechanism of the flotation agent and the like is less. Only when the development and application of a novel flotation agent are conducted under theoretical guidance can the gap between the flotation agent and foreign countries be shortened as soon as possible.
(2) Low seriation level and few special varieties
Compared with foreign countries, the natural and modified cationic organic polymer flotation agents have fewer varieties. The polymer polymers commonly adopted in China are mainly cationic and nonionic, various types of flotation agents are more applied in water supply and wastewater treatment in developed countries, and meanwhile, corresponding flotation agents are developed for oily sewage, so that the flotation agents have the advantages of low viscosity, good water purification effect and the like, while the flotation agents for oil field sewage treatment in China are rarely reported, and particularly the flotation agents for offshore oil field oily sewage treatment are not reported.
Disclosure of Invention
The invention overcomes the defects in the prior art, and the problems that the water yield and the discharge amount of oily pollutants are rapidly increased, the capacity of a sewage treatment facility is close to saturation and the oil content of the treated production water exceeds the standard after the offshore oil field is lifted can not be well met by the conventional flotation agent.
The purpose of the invention is realized by the following technical scheme.
A flotation agent for treating oily sewage in an oil field and a preparation method thereof are carried out according to the following steps:
step 1, mixing polyamine, long-chain alkyl dimethyl tertiary amine, 1, 6-hexamethylene diamine and distilled water, and then placing the mixture at the temperature of 30-40 ℃ to stir for reaction for 0.1-0.3h, wherein the molar ratio of the polyamine, the long-chain alkyl dimethyl tertiary amine and the 1, 6-hexamethylene diamine is (38-45): 8-12: 15-20, and the mass of the added distilled water is 35-40 times of that of the 1, 6-hexamethylene diamine;
step 2, dripping epichlorohydrin into the reaction container at the temperature of 30-40 ℃, and continuing to react for 2-4 hours at the temperature of 30-40 ℃ after finishing dripping, wherein the molar ratio of the epichlorohydrin to the 1, 6-hexanediamine is (6-9) to 1;
and 3, continuously heating to 45-55 ℃, continuously reacting for 1-3h at 45-55 ℃, continuously heating to 65-75 ℃, and continuously reacting for 2-4h at 65-75 ℃ to obtain the flotation agent for treating the oily sewage in the oil field.
In the step 1, the molar ratio of the polyamine, the long-chain alkyl dimethyl tertiary amine and the 1, 6-hexamethylene diamine is (40-42) to (9-11) to (17-19), the polyamine adopts one of diethylenetriamine, triethylene tetramine and tetraethylene pentamine, the long-chain alkyl dimethyl tertiary amine adopts dodecyl dimethyl tertiary amine or tetradecyl dimethyl tertiary amine, and the mass of the added distilled water is 37-39 times of that of the 1, 6-hexamethylene diamine.
In the step 2, the mol ratio of the epichlorohydrin to the 1, 6-hexanediamine is (7-8) to 1, and the dripping speed of the epichlorohydrin is 1-2 drops/s.
When the flotation agent for treating the oily sewage in the oil field is used for treating the oily sewage in the oil field with the oil content of 346-1500mg/L, the oil removal rate is 57.2-89.8 percent, and the turbidity of the oily sewage in the oil field is reduced to 23.5-182 NTU.
The invention has the beneficial effects that: the method has simple process, easy operation, convenient control of reaction temperature and stable polymerization reaction, and is suitable for treating sewage with high oil content in the oil field output liquid; the flotation agent for treating the oily sewage in the oil field prepared by the invention has higher cationic degree and surface activity, can quickly reduce the surface tension of the oily sewage, is convenient to obtain micro bubbles after air entraining, enhances the adhesion degree of the bubbles and suspended matters, achieves better water purification effect, and has universal applicability.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples.
Example 1
A preparation method of a flotation agent for treating oily sewage in an oil field comprises the following steps:
(1) mixing 5.0g of diethylenetriamine, 2.6g of dodecyl dimethyl tertiary amine, 2.4g of 1, 6-hexamethylene diamine and 91.2g of distilled water, and stirring and reacting at 30-40 ℃ for 0.1-0.3 h;
(2) continuously dripping 13.4g of epoxy chloropropane into the reaction container at the temperature of 30-40 ℃, and continuously reacting for 2-4h after dripping is finished;
(3) continuously heating to 45-55 ℃, and continuously reacting for 1-3h at the temperature;
(4) and continuously heating to 65-75 ℃, and continuously reacting for 2-4h at the temperature to obtain the flotation agent for treating the oily sewage in the oil field.
Example 2
A preparation method of a flotation agent for treating oily sewage in an oil field comprises the following steps:
(1) mixing 5.0g of diethylenetriamine, 2.8g of dodecyl dimethyl tertiary amine, 2.6g of 1, 6-hexamethylene diamine and 101.4g of distilled water, and stirring and reacting at 30-40 ℃ for 0.1-0.3 h;
(2) continuously dripping 16.6g of epoxy chloropropane into the reaction container at the temperature of 30-40 ℃, and continuously reacting for 2-4h after dripping is finished;
(3) continuously heating to 45-55 ℃, and continuously reacting for 1-3h at the temperature;
(4) and continuously heating to 65-75 ℃, and continuously reacting for 2-4h at the temperature to obtain the flotation agent for treating the oily sewage in the oil field.
Example 3
A preparation method of a flotation agent for treating oily sewage in an oil field comprises the following steps:
(1) mixing 5.0g of diethylenetriamine, 2.2g of dodecyl dimethyl tertiary amine, 2.4g of 1, 6-hexamethylene diamine and 88.8g of distilled water, and stirring and reacting at 30-40 ℃ for 0.1-0.3 h;
(2) continuously dripping 14.3g of epoxy chloropropane into the reaction container at the temperature of 30-40 ℃, and continuously reacting for 2-4h after dripping is finished;
(3) continuously heating to 45-55 ℃, and continuously reacting for 1-3h at the temperature;
(4) and continuously heating to 65-75 ℃, and continuously reacting for 2-4h at the temperature to obtain the flotation agent for treating the oily sewage in the oil field.
Example 4
A preparation method of a flotation agent for treating oily sewage in an oil field comprises the following steps:
(1) mixing 5.0g of diethylenetriamine, 2.9g of tetradecyldimethylamine, 2.4g of 1, 6-hexanediamine and 91.2g of distilled water, and stirring at 30-40 ℃ for reaction for 0.1-0.3 h;
(2) continuously dripping 13.4g of epoxy chloropropane into the reaction container at the temperature of 30-40 ℃, and continuously reacting for 2-4h after dripping is finished;
(3) continuously heating to 45-55 ℃, and continuously reacting for 1-3h at the temperature;
(4) and continuously heating to 65-75 ℃, and continuously reacting for 2-4h at the temperature to obtain the flotation agent for treating the oily sewage in the oil field.
Example 5
A preparation method of a flotation agent for treating oily sewage in an oil field comprises the following steps:
(1) mixing 5.0g of diethylenetriamine, 3.1g of tetradecyldimethylamine, 2.6g of 1, 6-hexanediamine and 101.4g of distilled water, and stirring at 30-40 ℃ for reaction for 0.1-0.3 h;
(2) continuously dripping 16.6g of epoxy chloropropane into the reaction container at the temperature of 30-40 ℃, and continuously reacting for 2-4h after dripping is finished;
(3) continuously heating to 45-55 ℃, and continuously reacting for 1-3h at the temperature;
(4) and continuously heating to 65-75 ℃, and continuously reacting for 2-4h at the temperature to obtain the flotation agent for treating the oily sewage in the oil field.
Example 6
A preparation method of a flotation agent for treating oily sewage in an oil field comprises the following steps:
(1) mixing 5.0g of diethylenetriamine, 2.5g of tetradecyldimethylamine, 2.4g of 1, 6-hexanediamine and 88.8g of distilled water, and stirring at 30-40 ℃ for reaction for 0.1-0.3 h;
(2) continuously dripping 14.3g of epoxy chloropropane into the reaction container at the temperature of 30-40 ℃, and continuously reacting for 2-4h after dripping is finished;
(3) continuously heating to 45-55 ℃, and continuously reacting for 1-3h at the temperature;
(4) and continuously heating to 65-75 ℃, and continuously reacting for 2-4h at the temperature to obtain the flotation agent for treating the oily sewage in the oil field.
Example 7
A preparation method of a flotation agent for treating oily sewage in an oil field comprises the following steps:
(1) mixing 7.0g of triethylene tetramine, 2.6g of dodecyl dimethyl tertiary amine, 2.4g of 1, 6-hexamethylene diamine and 91.2g of distilled water, and stirring and reacting at 30-40 ℃ for 0.1-0.3 h;
(2) continuously dripping 13.4g of epoxy chloropropane into the reaction container at the temperature of 30-40 ℃, and continuously reacting for 2-4h after dripping is finished;
(3) continuously heating to 45-55 ℃, and continuously reacting for 1-3h at the temperature;
(4) and continuously heating to 65-75 ℃, and continuously reacting for 2-4h at the temperature to obtain the flotation agent for treating the oily sewage in the oil field.
Example 8
A preparation method of a flotation agent for treating oily sewage in an oil field comprises the following steps:
(1) mixing 7.0g of triethylene tetramine, 2.7g of dodecyl dimethyl tertiary amine, 2.6g of 1, 6-hexamethylene diamine and 101.4g of distilled water, and stirring and reacting at 30-40 ℃ for 0.1-0.3 h;
(2) continuously dripping 16.6g of epoxy chloropropane into the reaction container at the temperature of 30-40 ℃, and continuously reacting for 2-4h after dripping is finished;
(3) continuously heating to 45-55 ℃, and continuously reacting for 1-3h at the temperature;
(4) and continuously heating to 65-75 ℃, and continuously reacting for 2-4h at the temperature to obtain the flotation agent for treating the oily sewage in the oil field.
Example 9
A preparation method of a flotation agent for treating oily sewage in an oil field comprises the following steps:
(1) mixing 7.0g of triethylene tetramine, 2.2g of dodecyl dimethyl tertiary amine, 2.4g of 1, 6-hexamethylene diamine and 88.8g of distilled water, and stirring and reacting at 30-40 ℃ for 0.1-0.3 h;
(2) continuously dripping 14.3g of epoxy chloropropane into the reaction container at the temperature of 30-40 ℃, and continuously reacting for 2-4h after dripping is finished;
(3) continuously heating to 45-55 ℃, and continuously reacting for 1-3h at the temperature;
(4) and continuously heating to 65-75 ℃, and continuously reacting for 2-4h at the temperature to obtain the flotation agent for treating the oily sewage in the oil field.
Example 10
A preparation method of a flotation agent for treating oily sewage in an oil field comprises the following steps:
(1) mixing 7.0g of triethylene tetramine, 2.9g of tetradecyl dimethyl tertiary amine, 2.4g of 1, 6-hexamethylene diamine and 91.2g of distilled water, and stirring and reacting at 30-40 ℃ for 0.1-0.3 h;
(2) continuously dripping 13.4g of epoxy chloropropane into the reaction container at the temperature of 30-40 ℃, and continuously reacting for 2-4h after dripping is finished;
(3) continuously heating to 45-55 ℃, and continuously reacting for 1-3h at the temperature;
(4) and continuously heating to 65-75 ℃, and continuously reacting for 2-4h at the temperature to obtain the flotation agent for treating the oily sewage in the oil field.
Example 11
A preparation method of a flotation agent for treating oily sewage in an oil field comprises the following steps:
1) mixing 7.0g of triethylene tetramine, 3.1g of tetradecyl dimethyl tertiary amine, 2.6g of 1, 6-hexamethylene diamine and 101.4g of distilled water, and stirring and reacting at 30-40 ℃ for 0.1-0.3 h;
(2) continuously dripping 16.6g of epoxy chloropropane into the reaction container at the temperature of 30-40 ℃, and continuously reacting for 2-4h after dripping is finished;
(3) continuously heating to 45-55 ℃, and continuously reacting for 1-3h at the temperature;
(4) and continuously heating to 65-75 ℃, and continuously reacting for 2-4h at the temperature to obtain the flotation agent for treating the oily sewage in the oil field.
Example 12
A preparation method of a flotation agent for treating oily sewage in an oil field comprises the following steps:
1) mixing 7.0g of triethylene tetramine, 2.5g of tetradecyl dimethyl tertiary amine, 2.4g of 1, 6-hexamethylene diamine and 88.8g of distilled water, and stirring and reacting at 30-40 ℃ for 0.1-0.3 h;
(2) continuously dripping 14.3g of epoxy chloropropane into the reaction container at the temperature of 30-40 ℃, and continuously reacting for 2-4h after dripping is finished;
(3) continuously heating to 45-55 ℃, and continuously reacting for 1-3h at the temperature;
(4) and continuously heating to 65-75 ℃, and continuously reacting for 2-4h at the temperature to obtain the flotation agent for treating the oily sewage in the oil field.
Example 13
A preparation method of a flotation agent for treating oily sewage in an oil field comprises the following steps:
1) mixing 9.0g of tetraethylenepentamine, 2.5g of dodecyl dimethyl tertiary amine, 2.4g of 1, 6-hexamethylene diamine and 91.2g of distilled water, and stirring and reacting at 30-40 ℃ for 0.1-0.3 h;
(2) continuously dripping 13.4g of epoxy chloropropane into the reaction container at the temperature of 30-40 ℃, and continuously reacting for 2-4h after dripping is finished;
(3) continuously heating to 45-55 ℃, and continuously reacting for 1-3h at the temperature;
(4) and continuously heating to 65-75 ℃, and continuously reacting for 2-4h at the temperature to obtain the flotation agent for treating the oily sewage in the oil field.
Example 14
A preparation method of a flotation agent for treating oily sewage in an oil field comprises the following steps:
1) mixing 9.0g of tetraethylenepentamine, 2.7g of dodecyl dimethyl tertiary amine, 2.6g of 1, 6-hexamethylene diamine and 101.4g of distilled water, and stirring and reacting at 30-40 ℃ for 0.1-0.3 h;
(2) continuously dripping 16.6g of epoxy chloropropane into the reaction container at the temperature of 30-40 ℃, and continuously reacting for 2-4h after dripping is finished;
(3) continuously heating to 45-55 ℃, and continuously reacting for 1-3h at the temperature;
(4) and continuously heating to 65-75 ℃, and continuously reacting for 2-4h at the temperature to obtain the flotation agent for treating the oily sewage in the oil field.
Example 15
A preparation method of a flotation agent for treating oily sewage in an oil field comprises the following steps:
1) mixing 9.0g of tetraethylenepentamine, 2.2g of dodecyl dimethyl tertiary amine, 2.4g of 1, 6-hexamethylene diamine and 88.8g of distilled water, and stirring and reacting at 30-40 ℃ for 0.1-0.3 h;
(2) continuously dripping 14.3g of epoxy chloropropane into the reaction container at the temperature of 30-40 ℃, and continuously reacting for 2-4h after dripping is finished;
(3) continuously heating to 45-55 ℃, and continuously reacting for 1-3h at the temperature;
(4) and continuously heating to 65-75 ℃, and continuously reacting for 2-4h at the temperature to obtain the flotation agent for treating the oily sewage in the oil field.
Example 16
A preparation method of a flotation agent for treating oily sewage in an oil field comprises the following steps:
1) mixing 9.0g of tetraethylenepentamine, 2.9g of tetradecyldimethylamine, 2.4g of 1, 6-hexanediamine and 91.2g of distilled water, and stirring at 30-40 ℃ for reaction for 0.1-0.3 h;
(2) continuously dripping 13.4g of epoxy chloropropane into the reaction container at the temperature of 30-40 ℃, and continuously reacting for 2-4h after dripping is finished;
(3) continuously heating to 45-55 ℃, and continuously reacting for 1-3h at the temperature;
(4) and continuously heating to 65-75 ℃, and continuously reacting for 2-4h at the temperature to obtain the flotation agent for treating the oily sewage in the oil field.
Example 17
A preparation method of a flotation agent for treating oily sewage in an oil field comprises the following steps:
1) mixing 9.0g of tetraethylenepentamine, 3.1g of tetradecyldimethylamine, 2.6g of 1, 6-hexanediamine and 101.4g of distilled water, and stirring at 30-40 ℃ for reaction for 0.1-0.3 h;
(2) continuously dripping 16.6g of epoxy chloropropane into the reaction container at the temperature of 30-40 ℃, and continuously reacting for 2-4h after dripping is finished;
(3) continuously heating to 45-55 ℃, and continuously reacting for 1-3h at the temperature;
(4) and continuously heating to 65-75 ℃, and continuously reacting for 2-4h at the temperature to obtain the flotation agent for treating the oily sewage in the oil field.
Example 18
A preparation method of a flotation agent for treating oily sewage in an oil field comprises the following steps:
1) mixing 9.0g of tetraethylenepentamine, 2.5g of tetradecyldimethylamine, 2.4g of 1, 6-hexanediamine and 88.8g of distilled water, and stirring at 30-40 ℃ for reaction for 0.1-0.3 h;
(2) continuously dripping 14.3g of epoxy chloropropane into the reaction container at the temperature of 30-40 ℃, and continuously reacting for 2-4h after dripping is finished;
(3) continuously heating to 45-55 ℃, and continuously reacting for 1-3h at the temperature;
(4) and continuously heating to 65-75 ℃, and continuously reacting for 2-4h at the temperature to obtain the flotation agent for treating the oily sewage in the oil field.
The first test example:
experiment raw materials: certain offshore oilfield wastewater (high oil content wastewater, oil content of wastewater 1500mg/L)
Experiment temperature: 65 deg.C
The concentration of the medicament: 100mg/L
Evaluation criteria: GB 13200-91 determination of water turbidity
SY/T5797-93 & lt & ltmethod for evaluating demulsification usability of oil-in-water emulsion & gt
The evaluation method comprises the following steps: at the temperature of 65 ℃ of high oily sewage, 60mL of sewage is added with 100mg/L of flotation agent, the mixture is uniformly oscillated, the height of bubbles is observed, and the turbidity of the lower layer sewage is measured after 30 minutes.
TABLE 1 high oil-contaminated water test data
Remarking: water color: a. the-、A、A+-Qing B-、B、B+General C-、C、C+-difference
Interface: a. the-、A、A+-is not substituted by B-、B、B+General C-、C、C+-irregularity
Test example two:
experiment raw materials: certain offshore oilfield wastewater (middle oil-containing wastewater, wastewater oil-containing 700mg/L)
Experiment temperature: 65 deg.C
The concentration of the medicament: 100mg/L
Evaluation criteria: GB 13200-91 determination of water turbidity
SY/T5797-93 & lt & ltmethod for evaluating demulsification usability of oil-in-water emulsion & gt
The evaluation method comprises the following steps: at the temperature of 65 ℃ of high oily sewage, 60mL of sewage is added with 100mg/L of flotation agent, the mixture is uniformly oscillated, the height of bubbles is observed, and the turbidity of the lower layer sewage is measured after 30 minutes.
Oily wastewater test data in Table 1
Remarking: water color: a. the-、A、A+-Qing B-、B、B+-oneGeneral formula C-、C、C+-difference
Interface: a. the-、A、A+-is not substituted by B-、B、B+General C-、C、C+-irregularity
Test example three:
experiment raw materials: certain offshore oilfield wastewater (Low oil content wastewater, sewage oil content 346mg/L)
Experiment temperature: 65 deg.C
The concentration of the medicament: 100mg/L
Evaluation criteria: GB 13200-91 determination of water turbidity
SY/T5797-93 & lt & ltmethod for evaluating demulsification usability of oil-in-water emulsion & gt
The evaluation method comprises the following steps: at the temperature of 65 ℃ of high oily sewage, 60mL of sewage is added with 100mg/L of flotation agent, the mixture is uniformly oscillated, the height of bubbles is observed, and the turbidity of the lower layer sewage is measured after 30 minutes.
TABLE 1 Low oily wastewater test data
Remarking: water color: a. the-、A、A+-Qing B-、B、B+General C-、C、C+-difference
Interface: a. the-、A、A+-is not substituted by B-、B、B+General C-、C、C+-irregularity
The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (10)
1. The flotation agent for treating the oily sewage in the oil field is characterized by comprising the following components in parts by weight: the method comprises the following steps:
step 1, mixing polyamine, long-chain alkyl dimethyl tertiary amine, 1, 6-hexamethylene diamine and distilled water, and then placing the mixture at the temperature of 30-40 ℃ to stir for reaction for 0.1-0.3h, wherein the molar ratio of the polyamine, the long-chain alkyl dimethyl tertiary amine and the 1, 6-hexamethylene diamine is (38-45): 8-12: 15-20, and the mass of the added distilled water is 35-40 times of that of the 1, 6-hexamethylene diamine;
step 2, dripping epichlorohydrin into the reaction container at the temperature of 30-40 ℃, and continuing to react for 2-4 hours at the temperature of 30-40 ℃ after finishing dripping, wherein the molar ratio of the epichlorohydrin to the 1, 6-hexanediamine is (6-9) to 1;
and 3, continuously heating to 45-55 ℃, continuously reacting for 1-3h at 45-55 ℃, continuously heating to 65-75 ℃, and continuously reacting for 2-4h at 65-75 ℃ to obtain the flotation agent for treating the oily sewage in the oil field.
2. The flotation agent for treating oily sewage in an oil field according to claim 1, which is characterized in that: in the step 1, the molar ratio of the polyamine, the long-chain alkyl dimethyl tertiary amine and the 1, 6-hexamethylene diamine is (40-42) to (9-11) to (17-19), and the adding mass of the distilled water is 37-39 times of the mass of the 1, 6-hexamethylene diamine.
3. The flotation agent for treating oily sewage in an oil field according to claim 1, which is characterized in that: in the step 1, the polyamine is one of diethylenetriamine, triethylenetetramine and tetraethylenepentamine, and the long-chain alkyl dimethyl tertiary amine is dodecyl dimethyl tertiary amine or tetradecyl dimethyl tertiary amine.
4. The flotation agent for treating oily sewage in an oil field according to claim 1, which is characterized in that: in the step 2, the mol ratio of the epichlorohydrin to the 1, 6-hexanediamine is (7-8) to 1, and the dripping speed of the epichlorohydrin is 1-2 drops/s.
5. A preparation method of a flotation agent for treating oily sewage in an oil field is characterized by comprising the following steps: the method comprises the following steps:
step 1, mixing polyamine, long-chain alkyl dimethyl tertiary amine, 1, 6-hexamethylene diamine and distilled water, and then placing the mixture at the temperature of 30-40 ℃ to stir for reaction for 0.1-0.3h, wherein the molar ratio of the polyamine, the long-chain alkyl dimethyl tertiary amine and the 1, 6-hexamethylene diamine is (38-45): 8-12: 15-20, and the mass of the added distilled water is 35-40 times of that of the 1, 6-hexamethylene diamine;
step 2, dripping epichlorohydrin into the reaction container at the temperature of 30-40 ℃, and continuing to react for 2-4 hours at the temperature of 30-40 ℃ after finishing dripping, wherein the molar ratio of the epichlorohydrin to the 1, 6-hexanediamine is (6-9) to 1;
and 3, continuously heating to 45-55 ℃, continuously reacting for 1-3h at 45-55 ℃, continuously heating to 65-75 ℃, and continuously reacting for 2-4h at 65-75 ℃ to obtain the flotation agent for treating the oily sewage in the oil field.
6. The preparation method of the flotation agent for treating the oily sewage in the oil field according to claim 5, which is characterized by comprising the following steps: in the step 1, the molar ratio of the polyamine, the long-chain alkyl dimethyl tertiary amine and the 1, 6-hexamethylene diamine is (40-42) to (9-11) to (17-19), and the adding mass of the distilled water is 37-39 times of the mass of the 1, 6-hexamethylene diamine.
7. The preparation method of the flotation agent for treating the oily sewage in the oil field according to claim 5, which is characterized by comprising the following steps: in the step 1, the polyamine is one of diethylenetriamine, triethylenetetramine and tetraethylenepentamine, and the long-chain alkyl dimethyl tertiary amine is dodecyl dimethyl tertiary amine or tetradecyl dimethyl tertiary amine.
8. The preparation method of the flotation agent for treating the oily sewage in the oil field according to claim 5, which is characterized by comprising the following steps: in the step 2, the mol ratio of the epichlorohydrin to the 1, 6-hexanediamine is (7-8) to 1, and the dripping speed of the epichlorohydrin is 1-2 drops/s.
9. The use of the flotation agent for treating oily sewage in an oil field according to any one of claims 1 to 4 for treating oily sewage in an oil field.
10. Use according to claim 9, characterized in that: when the flotation agent for treating the oily sewage in the oil field is used for treating the oily sewage in the oil field with the oil content of 346-1500mg/L, the oil removal rate is 57.2-89.8 percent, and the turbidity of the oily sewage in the oil field is reduced to 23.5-182 NTU.
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