CN111777757A - Preparation method of super heavy oil demulsifier - Google Patents
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- CN111777757A CN111777757A CN202010733306.3A CN202010733306A CN111777757A CN 111777757 A CN111777757 A CN 111777757A CN 202010733306 A CN202010733306 A CN 202010733306A CN 111777757 A CN111777757 A CN 111777757A
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Abstract
The invention provides a preparation method of a super heavy oil demulsifier, (1) heating 4, 4' -dihydroxy diphenyl sulfone and triethylene tetramine to be completely dissolved, dripping formaldehyde, and generating an initiator A after full reaction; (2) putting the initiator A and the catalyst into a reaction kettle, sealing, vacuumizing, introducing propylene oxide, heating and controlling the pressure to obtain an intermediate product Z; (3) putting the intermediate product Z and a catalyst into a reaction kettle for reaction and sealing, vacuumizing and introducing propylene oxide, heating and controlling the pressure to obtain polyether B; (4) mixing polyether B with an alkaline solution, heating, slowly dropwise adding benzyl chloride with the concentration of 5%, continuously dipping the reaction solution to observe the drawable length of the reaction solution, and stopping the reaction when the drawable length is 3-4 cm to obtain an ultra-thick oil demulsifier; the invention has high wettability, permeability and surface activity, and proper molecular structure and branching degree, effectively reduces the surface tension of the oil-water interface of the ultra-thick oil, and improves the oil-water separation efficiency.
Description
Technical Field
The invention belongs to the technical field of oil field chemicals, and particularly relates to a preparation method of a super-heavy oil demulsifier.
Background
The super-thick oil in China has huge yield every year, has the characteristics of high viscosity, high density and high colloid content, and colloid and asphaltene exist in crude oil in a colloid particle state, so that the crude oil is more difficult to treat than a common crude oil emulsion, and the demulsification and dehydration difficulty of the crude oil is increased. Because the crude oil emulsion contains water, impurities dissolved in the water can cause scaling and corrosion on the metal surface, and the service life of a pump, a pipeline and a storage tank is greatly reduced; in addition, the oil content in the discharged water can cause resource waste and cause great damage to the environment.
In recent years, each main oil field in China has entered the later stage of high water content exploitation. In order to maintain stable crude oil yield, each large oil field adopts a mode of increasing water injection and steam injection to improve the liquid yield of an oil well, so that the water content of the produced liquid of the oil well is rapidly increased; meanwhile, the large amount of oil extraction additives applied in the oil field exploitation process also makes the composition of the produced liquid of crude oil (especially thick oil and super thick oil) more complex, so that the high-efficiency rapid demulsification technology of the thick oil and the super thick oil becomes a key technology which influences the oil extraction cost, the quality and the yield of the crude oil and controls the environmental pollution of the oil field.
With the deepening of the heavy degree of crude oil, new demulsifier products are required to be developed continuously. At present, the new varieties of the demulsifiers in China are not developed much, and the requirements of heavy oil and poor oil of crude oil cannot be met.
The invention is provided in view of the above.
Disclosure of Invention
The invention provides a preparation method of a super heavy oil demulsifier aiming at the technical problems.
In order to achieve the purpose, the invention adopts the technical scheme that:
the preparation method of the super heavy oil demulsifier comprises the following steps:
(1) preparation of the initiator A: heating 4, 4' -dihydroxy diphenyl sulfone and triethylene tetramine to 50-55 ℃ for complete dissolution, slowly dropwise adding a formaldehyde solution with the concentration of 37-40% at the temperature of 45-55 ℃, and fully reacting for 1-2 hours to generate an initiator A; wherein the mass parts of the 4, 4' -dihydroxy diphenyl sulfone, the triethylene tetramine and the formaldehyde solution are 1: (2.3-2.4): (0.4-0.5);
(2) preparation of intermediate product Z: putting an initiator A and a catalyst into a reaction kettle, and sealing, wherein the mass ratio of the catalyst to the initiator A is 0.26-1.08; replacing air in the kettle, vacuumizing the kettle to negative pressure, slowly introducing propylene oxide, heating, controlling the pressure to be 0.19-0.21 MPa, closing a feed valve after all the propylene oxide is added, and reducing the pressure in the reaction kettle until the negative pressure reaction is finished to obtain an intermediate product Z;
(3) polyether reaction: putting the intermediate product Z and a catalyst into a reaction kettle, and sealing, wherein the mass ratio of the catalyst to the initiator A is 0.19-0.81; replacing air in the kettle, vacuumizing the kettle to negative pressure, slowly introducing ethylene oxide, heating, controlling the pressure to be 0.19-0.21 MPa, closing a feed valve after the ethylene oxide is completely added, and reducing the pressure in the reaction kettle until the negative pressure reaction is finished to obtain polyether B;
(4) preparing a demulsifier: and mixing the polyether B with an alkaline solution, heating to 100-120 ℃, slowly dropwise adding benzyl chloride with the concentration of 5%, keeping the reaction, continuously dipping the reaction solution to observe the drawable length of the reaction solution, and stopping the reaction when the drawable length is 3-4 cm to obtain the super-heavy oil demulsifier.
Preferably, in the step (1), the mass parts of the 4, 4' -dihydroxy diphenyl sulfone, the triethylene tetramine and the formaldehyde solution are 1: 2.31: 0.48.
preferably, the reaction temperature in steps (2) and (3) is 140 ℃.
Preferably, the catalyst for the polyether reaction in the steps (2) and (3) is potassium hydroxide; wherein the dosage of the catalyst in the step (2) is 0.2 percent of the total mass of the ethylene oxide and the propylene oxide. The dosage of the catalyst added in the step (3) is 0.15 percent of the total mass of the ethylene oxide and the propylene oxide.
Preferably, in the steps (2) and (3), the gas used for replacing the high-pressure reaction kettle is nitrogen, and the vacuumizing time is 4-6 min.
Preferably, in the steps (2) and (3), the vacuumizing time is 5min, and the vacuumizing is carried out until the pressure in the reaction kettle is-0.09 MPa.
Preferably, the mass ratio of the propylene oxide to the initiator A in the steps (2) and (3) is (99-359): 1.
preferably, the mass ratio of the ethylene oxide introduced to the intermediate product Z is 1: (2-3.7).
Preferably, the reaction temperature in step (4) is 110 ℃.
Preferably, the mass ratio of the benzyl chloride solution to the polyether is (0.025-0.05): 1.
compared with the prior art, the invention has the advantages and positive effects that:
the novel efficient aging oil demulsifier disclosed by the invention has the advantages of high demulsification efficiency, improved wettability and permeability, high surface activity, appropriate molecular structure and branching degree, capability of effectively reducing the surface tension of an oil-water interface of ultra-thick oil, improvement on oil-water separation efficiency and better demulsification effect than the traditional demulsifier. The method has the characteristics of simple preparation, low cost and high demulsification efficiency, and has better prospect in the field of crude oil demulsification research.
Drawings
FIG. 1 is a graph showing the demulsification effect of the samples 1-4 of the present invention on super-heavy crude oil at 2h, from left to right;
FIG. 2 is a graph showing the demulsification effect of the samples 5 to 8 of the present invention on super-heavy crude oil at 2 hours from left to right;
FIG. 3 is a graph showing the demulsification effect of the samples 9-12 of the present invention on super heavy crude oil at 2h, from left to right;
FIG. 4 is a graph showing the demulsification effect of the samples 1-4 of the present invention on the super heavy crude oil at 18h, from left to right;
FIG. 5 is a graph showing the demulsification effect of the samples 5-8 of the present invention on super heavy crude oil at 18h, from left to right;
fig. 6 is a graph showing the demulsification effect of the samples 9-12 of the present invention on the ultra-thick oil at 18h from left to right.
Detailed Description
The present invention is further described below in conjunction with specific examples so that those skilled in the art may better understand the present invention and can practice it.
Example one
A preparation method of a super heavy oil demulsifier comprises the following steps:
(1) preparation of the initiator A: 20g of 4, 4' -dihydroxy diphenyl sulfone and 46.2g of triethylene tetramine are put into a four-mouth bottle and heated to 50 ℃ for complete dissolution, 9.6g of formaldehyde solution with the concentration of 37% is slowly dripped at the temperature of 50 ℃, and the initiator A is generated after full reaction for 1 hour. The specific reaction formula is as follows:
(2) preparation of intermediate product Z: adding 5g of initiator A and 1.37g of potassium hydroxide into a high-temperature high-pressure reaction kettle, sealing, replacing air in the kettle in a nitrogen purging mode, vacuumizing for 4-6 min by using a vacuum pump, starting heating after the pressure in the reaction kettle is reduced to negative pressure (in the embodiment, the pressure is-0.09 MPa), and opening a feed valve to slowly introduce 995g of propylene oxide; in the process, the temperature is raised to 140 ℃, the reading of a pressure gauge is controlled to be between 0.19MPa, after the propylene oxide is added, a feeding valve is closed, the heating is stopped, and the reaction is finished when the pressure in the reaction kettle is reduced to negative pressure, so that an intermediate product Z is obtained.
(3) Polyether reaction: putting the intermediate product Z and 1.03g of potassium hydroxide into a high-temperature high-pressure reaction kettle, sealing, replacing air in the kettle in a nitrogen purging mode, vacuumizing for 4-6 min by using a vacuum pump, starting heating after the pressure in the reaction kettle is reduced to negative pressure (in the embodiment, the pressure is-0.09 MPa), and opening a feed valve to slowly feed 333.3g of ethylene oxide; in the process, the temperature is raised to 140 ℃, the reading of the pressure gauge is controlled to be between 0.19MPa, after the ethylene oxide is added, the feeding valve is closed, the reaction is continued for 20min after the pressure is returned, and the reaction is finished when the pressure is reduced to negative pressure (in the embodiment, the pressure is-0.09 MPa), so that polyether B is obtained.
It can be seen that the amount of the catalyst used in step (2) in this example is 0.2% of the total mass of ethylene oxide and propylene oxide. The catalyst is added in the step (3) and the dosage of the catalyst is 0.15 percent of the total mass of the ethylene oxide and the propylene oxide, and the integral reaction formula of the steps (2) and (3) is as follows:
wherein the content of the first and second substances,
(4) preparing a demulsifier: and (3) putting 50g of polyether B into a three-mouth bottle, heating to 110 ℃ (heating in an oil bath), slowly dropwise adding 2.5g of benzyl chloride with the concentration of 5%, keeping the reaction, continuously dipping the reaction liquid with a glass rod to observe the drawable length of the reaction liquid, and stopping the reaction when the drawable length is 3-4 cm to obtain the novel thick oil demulsifier. Wherein, benzyl chloride can be dripped through a separating funnel; the specific reaction formula is as follows:
wherein the content of the first and second substances,
the preparation method in the above embodiment is simple and convenient to prepare, low in cost and efficient in demulsification. By grafting a certain amount of propylene oxide and ethylene oxide on an initiator, the wettability and the permeability of the obtained demulsifier are improved, the surface activity is high, the molecular structure and the branching degree are suitable, the surface tension of an oil-water interface of the ultra-thick oil is effectively reduced, the oil-water separation efficiency is improved, the water-in-oil or oil-in-water structure is effectively destroyed, and water or oil is separated.
Example two
A preparation method of a super heavy oil demulsifier comprises the following steps:
(1) preparation of the initiator A: and (2) putting 20g of 4, 4' -dihydroxy diphenyl sulfone and 46g of triethylene tetramine into a four-mouth bottle, heating to 55 ℃ to completely dissolve, slowly dropwise adding 8g of 39% formaldehyde solution at the temperature of 45 ℃, and fully reacting for 2 hours to generate an initiator A. The specific reaction formula is as shown in step (1) of the example.
(2) Preparation of intermediate product Z: adding 5g of initiator A and 1.3g of potassium hydroxide into a high-temperature high-pressure reaction kettle, sealing, replacing air in the kettle in a nitrogen purging mode, vacuumizing for 4-6 min by using a vacuum pump, starting heating after the pressure in the reaction kettle is reduced to negative pressure (in the embodiment, the pressure is-0.09 MPa), and opening a feed valve to slowly introduce 495g of propylene oxide; in the process, the temperature is raised to 140 ℃, the reading of a pressure gauge is controlled to be between 0.21MPa, after the propylene oxide is added, a feeding valve is closed, the heating is stopped, and the reaction is finished when the pressure in the reaction kettle is reduced to negative pressure, so that an intermediate product Z is obtained.
(3) Polyether reaction: putting the intermediate product Z and 0.95g of potassium hydroxide into a high-temperature high-pressure reaction kettle, sealing, replacing air in the kettle in a nitrogen purging mode, vacuumizing for 4-6 min by using a vacuum pump, starting heating after the pressure in the reaction kettle is reduced to negative pressure (in the embodiment, the pressure is-0.09 MPa), and simultaneously opening a feed valve to slowly introduce 185.2g of ethylene oxide; in the process, the temperature is raised to 140 ℃, the reading of the pressure gauge is controlled to be between 0.21MPa, after the ethylene oxide is added, the feeding valve is closed, the reaction is continued for 20min after the pressure is returned, and the reaction is finished when the pressure is reduced to negative pressure (in the embodiment, the pressure is-0.09 MPa), so that polyether B is obtained. The following were used: the specific reaction formula is the same as the whole reaction formula of steps (2) and (3) in one step of the example.
(4) Preparing a demulsifier: and (3) putting 50g of polyether B into a three-mouth bottle, heating to 120 ℃ (heating in an oil bath), slowly dropwise adding 1.25g of benzyl chloride with the concentration of 5%, keeping the reaction, continuously dipping the reaction liquid with a glass rod to observe the drawable length of the reaction liquid, and stopping the reaction when the drawable length is 3-4 cm to obtain the novel thick oil demulsifier. Wherein, benzyl chloride can be dripped through a separating funnel; the specific reaction formula is as shown in step (4) of the example.
EXAMPLE III
A preparation method of a super heavy oil demulsifier comprises the following steps:
(1) preparation of the initiator A: and (2) putting 20g of 4, 4' -dihydroxy diphenyl sulfone and 48g of triethylene tetramine into a four-mouth bottle, heating to 52 ℃ to completely dissolve, slowly dropwise adding 10g of 40% formaldehyde solution at the temperature of 55 ℃, and fully reacting for 1.5h to generate an initiator A. The specific reaction formula is as shown in step (1) of the example.
(2) Preparation of intermediate product Z: 5g of initiator A and 5.4g of potassium hydroxide are put into a high-temperature high-pressure reaction kettle for sealing, air in the kettle is replaced in a nitrogen purging mode, the vacuum pump is used for vacuumizing for 4-6 min, the heating is started after the pressure in the reaction kettle is reduced to negative pressure (minus 0.09MPa in the embodiment), and meanwhile, a feeding valve is opened to slowly introduce 1795g of propylene oxide; in the process, the temperature is raised to 140 ℃, the reading of a pressure gauge is controlled to be between 0.2MPa, after the propylene oxide is added, a feeding valve is closed, the heating is stopped, and the reaction is finished when the pressure in the reaction kettle is reduced to negative pressure, so that an intermediate product Z is obtained.
(3) Polyether reaction: putting the intermediate product Z and 4.05g of potassium hydroxide into a high-temperature high-pressure reaction kettle, sealing, replacing air in the kettle in a nitrogen purging mode, vacuumizing for 4-6 min by using a vacuum pump, starting heating after the pressure in the reaction kettle is reduced to negative pressure (in the embodiment, the pressure is-0.09 MPa), and opening a feed valve to slowly feed 900g of ethylene oxide; in the process, the temperature is raised to 140 ℃, the reading of the pressure gauge is controlled to be between 0.2MPa, after the ethylene oxide is added, the feeding valve is closed, the reaction is continued for 20min after the pressure is returned, and the reaction is finished when the pressure is reduced to negative pressure (in the embodiment, the pressure is-0.09 MPa), so that polyether B is obtained. The following were used: the specific reaction formula is the same as the whole reaction formula of steps (2) and (3) in one step of the example.
(4) Preparing a demulsifier: and (3) putting 50g of polyether B into a three-necked bottle, heating to 100 ℃ (heating in an oil bath), slowly dropwise adding 2g of benzyl chloride with the concentration of 5%, keeping the reaction, continuously dipping the reaction liquid with a glass rod to observe the drawable length of the reaction liquid, and stopping the reaction when the drawable length is 3-4 cm to obtain the novel thick oil demulsifier. Wherein, benzyl chloride can be dripped through a separating funnel; the specific reaction formula is as shown in step (4) of the example.
Example four
In the invention, the mass ratio of propylene oxide to initiator is recorded as M, the mass ratio of intermediate product Z (the amount of initiator to propylene oxide) to ethylene oxide is recorded as N, and the obtained novel heavy oil demulsifier is named according to the mass ratio of propylene oxide to initiator M and the mass ratio of intermediate product Z (the amount of initiator to propylene oxide) to ethylene oxide N: is marked as 2-M-N. For example, the mass ratio M of propylene oxide to the initiator, and the mass ratio N of the initiator to ethylene oxide in the above examples one to three are equal; the novel thick oil demulsifiers obtained in examples one to three were recorded as 2 to 99(2.7: 1).
According to the same steps of the first embodiment, different novel super heavy oil demulsifiers can be obtained by changing the mass parts of the introduced propylene oxide and ethylene oxide; the same steps are not described again, and the differences between the embodiments are described in a table form; wherein the first embodiment corresponds to the number 3 of the experimental groups, the second embodiment corresponds to the number 1 of the experimental groups, and the third embodiment corresponds to the number 5 of the experimental groups; the other experimental group numbers correspond to the examples with different parts by mass of propylene oxide and ethylene oxide. The specific parameter settings are shown in table 1 below.
For each example in table 1 above, the dewatering effect of the novel super heavy oil demulsifier obtained from each example was evaluated. When the evaluation is carried out, the crude oil produced liquid of a certain oil field is taken as a processing object, the dehydration amounts of the evaluation object at different time periods of 60min, 120min and 18h are recorded and compared, and the characteristic of whether the wall is hung or not is evaluated as shown in fig. 1-6. The specific experimental results are shown in the following table 2:
in conclusion, the novel super heavy oil demulsifier obtained in each embodiment is compared with the evaluation results to obtain the novel super heavy oil demulsifier, and the novel super heavy oil demulsifier provided by the invention has the advantages of good demulsification effect, high dehydration rate and high demulsification speed, and can effectively reduce the viscosity of super heavy oil and improve the crude oil extraction efficiency. The demulsifier has good hydrophilic capacity, permeability and wetting performance, can effectively reduce the surface tension of an oil-water interfacial film, and can be used for demulsification and dehydration, and the demulsifier has the advantages of simple preparation method, low cost and high demulsification efficiency.
The above description is only a preferred embodiment of the present invention, and not intended to limit the present invention in other forms, and any person skilled in the art may apply the above modifications or changes to the equivalent embodiments with equivalent changes, without departing from the technical spirit of the present invention, and any simple modification, equivalent change and change made to the above embodiments according to the technical spirit of the present invention still belong to the protection scope of the technical spirit of the present invention.
Claims (10)
1. The preparation method of the super heavy oil demulsifier is characterized by comprising the following steps:
(1) preparation of the initiator A: heating 4, 4' -dihydroxy diphenyl sulfone and triethylene tetramine to 50-55 ℃ for complete dissolution, slowly dropwise adding a formaldehyde solution with the concentration of 37-40% at the temperature of 45-55 ℃, and fully reacting for 1-2 hours to generate an initiator A; wherein the mass parts of the 4, 4' -dihydroxy diphenyl sulfone, the triethylene tetramine and the formaldehyde solution are 1: (2.3-2.4): (0.4-0.5);
(2) preparation of intermediate product Z: putting an initiator A and a catalyst into a reaction kettle, and sealing, wherein the mass ratio of the catalyst to the initiator A is 0.26-1.08; replacing air in the kettle, vacuumizing the kettle to negative pressure, slowly introducing propylene oxide, heating, controlling the pressure to be 0.19-0.21 MPa, closing a feed valve after all the propylene oxide is added, and reducing the pressure in the reaction kettle until the negative pressure reaction is finished to obtain an intermediate product Z;
(3) polyether reaction: putting the intermediate product Z and a catalyst into a reaction kettle, and sealing, wherein the mass ratio of the catalyst to the initiator A is 0.19-0.81; replacing air in the kettle, vacuumizing the kettle to negative pressure, slowly introducing ethylene oxide, heating, controlling the pressure to be 0.19-0.21 MPa, closing a feed valve after the ethylene oxide is completely added, and reducing the pressure in the reaction kettle until the negative pressure reaction is finished to obtain polyether B;
(4) preparing a demulsifier: and mixing the polyether B with an alkaline solution, heating to 100-120 ℃, slowly dropwise adding benzyl chloride with the concentration of 5%, keeping the reaction, continuously dipping the reaction solution, observing the drawable length of the reaction solution, and stopping the reaction when the drawable length is 3-4 cm to obtain the super-heavy oil demulsifier.
2. The method for preparing the demulsifier for ultra-thick oil according to claim 1, wherein the demulsifier comprises: in the step (1), the mass parts of the 4, 4' -dihydroxy diphenyl sulfone, the triethylene tetramine and the formaldehyde solution are 1: 2.31: 0.48.
3. the method for preparing the demulsifier for ultra-thick oil according to claim 1 or 2, wherein the method comprises the following steps: the reaction temperature in the steps (2) and (3) is 140 ℃.
4. The method for preparing the demulsifier for ultra-thick oil according to claim 3, wherein the demulsifier comprises: in the step (2) and the step (3), the catalyst for the polyether reaction is potassium hydroxide; wherein the dosage of the catalyst in the step (2) is 0.2 percent of the total mass of the ethylene oxide and the propylene oxide. The dosage of the catalyst added in the step (3) is 0.15 percent of the total mass of the ethylene oxide and the propylene oxide.
5. The method for preparing the demulsifier for ultra-thick oil according to claim 4, wherein the demulsifier comprises: in the steps (2) and (3), the gas used for replacing the high-pressure reaction kettle is nitrogen, and the vacuumizing time is 4-6 min.
6. The method for preparing the demulsifier for ultra-thick oil according to claim 5, wherein the demulsifier comprises: in the steps (2) and (3), vacuumizing for 5min until the pressure in the reaction kettle is-0.09 Mpa.
7. The method for preparing the super heavy oil demulsifier according to any one of claims 1 to 6, wherein the method comprises the following steps: the mass ratio of the propylene oxide to the initiator A in the steps (2) and (3) is (99-359): 1.
8. the method for preparing the super heavy oil demulsifier according to any one of claims 1 to 6, wherein the method comprises the following steps: the mass ratio of the introduced ethylene oxide to the intermediate product Z is 1: (2-3.7).
9. The method for preparing the demulsifier for ultra-thick oil according to claim 1, wherein the demulsifier comprises: the reaction temperature in step (4) was 110 ℃.
10. The method for preparing the demulsifier for ultra-thick oil according to claim 9, wherein the demulsifier comprises: the mass ratio of the benzyl chloride solution to the polyether is (0.025-0.05): 1.
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| US20160257892A1 (en) * | 2015-03-04 | 2016-09-08 | Ecolab Usa Inc. | Reverse emulsion breaker polymers |
| CN111019117A (en) * | 2019-12-25 | 2020-04-17 | 东北石油大学 | Preparation method of modified multi-branched polyether demulsifier |
| CN111303399A (en) * | 2020-03-23 | 2020-06-19 | 东北石油大学 | Preparation method of demulsifier suitable for ternary combination flooding crude oil |
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2020
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| US5117058A (en) * | 1990-11-09 | 1992-05-26 | Baker Hughes Incorporated | Cationic amide/ester compositions as demulsifiers |
| CN103642518A (en) * | 2013-12-10 | 2014-03-19 | 天津亿利科能源科技发展股份有限公司 | High-water-cut heavy oil demulsifier used for oil fields and preparation method thereof |
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| CN111019117A (en) * | 2019-12-25 | 2020-04-17 | 东北石油大学 | Preparation method of modified multi-branched polyether demulsifier |
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