CN113583645A - Hydrate inhibitor and application thereof - Google Patents
Hydrate inhibitor and application thereof Download PDFInfo
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- CN113583645A CN113583645A CN202110733327.XA CN202110733327A CN113583645A CN 113583645 A CN113583645 A CN 113583645A CN 202110733327 A CN202110733327 A CN 202110733327A CN 113583645 A CN113583645 A CN 113583645A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/52—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning
- C09K8/524—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning organic depositions, e.g. paraffins or asphaltenes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
- C09K8/52—Compositions for preventing, limiting or eliminating depositions, e.g. for cleaning
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
- C09K2208/22—Hydrates inhibition by using well treatment fluids containing inhibitors of hydrate formers
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17D—PIPE-LINE SYSTEMS; PIPE-LINES
- F17D1/00—Pipe-line systems
- F17D1/08—Pipe-line systems for liquids or viscous products
- F17D1/16—Facilitating the conveyance of liquids or effecting the conveyance of viscous products by modification of their viscosity
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Abstract
The invention discloses a hydrate inhibitor, which comprises at least 50 wt% of dimethylamino alkyl acrylamide, and can effectively inhibit a large amount of generation and aggregation of hydrates at a low dosage, prevent and treat wellbore blockage, greatly reduce the dosage of a thermodynamic inhibitor, reduce the cost of the inhibitor, reduce the logistics support burden and safety risk of storage and transportation of a large amount of hydrate thermodynamic inhibitor on a deep sea operation platform, reduce environmental hazards and simplify the preparation and maintenance treatment of working fluid.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a hydrate inhibitor and application thereof.
Background
Natural gas hydrates are ice-like crystalline substances formed by water and natural gas under low-temperature and high-pressure conditions. In the drilling development of ocean deepwater oil gas and natural gas hydrates, the temperature of ocean bottom seawater and stratum is low, and the hydrostatic pressure is high, so that favorable conditions are created for the generation of hydrates. Under the conditions of low temperature and high pressure, hydrate is generated, grows, aggregates and deposits, finally flow obstacles are caused, and normal operation of well drilling, well completion, testing and hydrate exploitation is influenced.
At present, in deepwater oil and gas drilling development, a thermodynamic hydrate inhibition method is mainly adopted. Thermodynamic inhibitors include methanol, ethylene glycol, and sodium chloride. The inhibitor reduces the generation temperature of the hydrate or increases the generation pressure of the hydrate by changing the phase equilibrium condition of the hydrate, thereby preventing the generation of the hydrate. However, the dosage of the thermodynamic inhibitor is large, usually more than 20% of the water phase, and some even up to 60%, so that the thermodynamic inhibitor has high cost, pollutes the environment, and can cause the problems of corrosion of equipment and the like. The space of the offshore operation platform is limited, and the logistics support burden is increased by transporting and storing a large amount of hydrate inhibitors, so that the space is more tense, and potential safety hazards exist.
Aiming at the problems of hydrate thermodynamic inhibitors, low-dose hydrate kinetic inhibitors are researched at home and abroad, and hopefully, the hydrate kinetic inhibitors can replace the thermodynamic inhibitors, and mainly comprise hydrate kinetic inhibitors and anti-polymerization agents, including polyvinylpyrrolidone, polyvinyl caprolactam, copolymers of pyrrolidone and caprolactam, copolymers of vinylpyrrolidone and butyl acrylate and the like. However, studies and practice have shown that kinetic inhibitors fail severely at high supercooling. In the process of drilling and developing the marine deepwater oil gas and natural gas hydrate, the low-temperature and high-pressure environment of the sea bottom provides a high supercooling degree condition, and the hydrate is easy to generate and cause blockage. The single use of the kinetic inhibitor cannot meet the control requirement of the hydrate in deepwater operation, and still depends on the thermodynamic inhibitor with higher concentration.
Thus, current deepwater oil and gas hydrate drilling developments still rely on the addition of large amounts of thermodynamic inhibitors to control hydrate flow impediments. The method develops the low-dosage hydrate inhibitor suitable for deepwater operation under low-temperature and high-pressure conditions, effectively reduces the dosage of the hydrate thermodynamic inhibitor, is vital to safe and efficient hydrate blockage prevention, and is a main idea for solving a plurality of defects of the traditional thermodynamic hydrate prevention and treatment method.
Disclosure of Invention
The invention aims to solve the problems of large dosage, high cost and environmental pollution of hydrate inhibitors in the prior art, and provides a hydrate inhibitor with low dosage, low cost, safety, environmental protection and good inhibition effect.
In order to achieve the above object, the present invention provides a hydrate inhibitor comprising at least 50% by mass of a dimethylaminoalkylacrylamide.
Preferably, the inhibitor comprises 60-90 wt% of a dimethylaminoalkylacrylamide.
Preferably, the alkyl group of the dimethylaminoalkylacrylamide is a chain alkyl group; the alkyl group is preferably a chain alkyl group having C1 to C5.
Preferably, the dimethylaminoalkyl acrylamide is at least two of dimethylaminopropyl methacrylamide, N- (2-dimethylaminoethyl) acrylamide, and dimethylaminopropyl acrylamide.
Preferably, the dimethylamino alkyl acrylamide is a mixture of dimethylamino propyl methacrylamide and N- (2-dimethylaminoethyl) acrylamide, and the mass ratio of the two is preferably 1-4: 1.
preferably, the inhibitor further comprises epoxypropyldimethylalkylammonium chloride.
Preferably, the mass content of the epoxypropyldimethyl alkyl ammonium chloride is 10-40 wt%.
Preferably, the mass ratio of the dimethylamino alkyl acrylamide to the epoxypropyl dimethyl alkyl ammonium chloride is 4-7: 1.
Preferably, the structural formula of the epoxypropyldimethyl alkyl ammonium chloride is shown as formula I:
wherein n is 4-12.
The invention provides application of the inhibitor in oil and gas exploitation and gathering processes.
The hydrate inhibitor can effectively inhibit the generation and aggregation of a large amount of hydrate under a low dosage (0.5-2.0%), and prevent and treat the blockage of a shaft. Compared with the traditional thermodynamic method for completely preventing the generation of the hydrate by using a high-concentration (15-60%) hydrate inhibitor (methanol, ethylene glycol or sodium chloride), the thermodynamic method for completely preventing the generation of the hydrate inhibitor changes from the thermodynamic prevention and control angle of completely inhibiting the formation of the hydrate into the thermodynamic prevention and control method for inhibiting the growth of the hydrate and preventing the aggregation and the blockage of hydrate particles, greatly reduces the dosage of the thermodynamic inhibitor, reduces the cost of the inhibitor, reduces the logistics guarantee burden and the safety risk of storage and transportation of a large amount of hydrate thermodynamic inhibitors on a deep sea operation platform, reduces environmental hazards, and is simpler and more convenient to prepare and maintain working fluid.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The present invention provides a hydrate inhibitor comprising at least 50 wt% of a dimethylaminoalkyl acrylamide.
According to a preferred embodiment of the present invention, in order to further enhance the hydrate inhibition effect, the inhibitor comprises 60 to 90 wt% of dimethylaminoalkylacrylamide.
According to a preferred embodiment of the present invention, in order to further improve the hydrate inhibition effect, the alkyl group of the dimethylaminoalkylacrylamide is a chain alkyl group, preferably a chain alkyl group having C1 to C5.
According to a preferred embodiment of the present invention, in order to further improve the hydrate inhibition effect, the dimethylaminoalkylacrylamide is at least two of dimethylaminopropyl methacrylamide, N- (2-dimethylaminoethyl) acrylamide and dimethylaminopropyl acrylamide.
According to a preferred embodiment of the present invention, in order to further improve the hydrate inhibition effect, the dimethylaminoalkyl acrylamide is a mixture of dimethylaminopropyl methacrylamide and N- (2-dimethylaminoethyl) acrylamide, preferably in a mass ratio of 1-4: 1.
according to a preferred embodiment of the present invention, in order to further enhance the hydrate inhibition effect, the inhibitor further comprises epoxypropyldimethylalkylammonium chloride.
According to a preferred embodiment of the present invention, in order to further improve the hydrate inhibition effect, the epoxypropyldimethylammonium chloride content is 10 to 40 wt%.
According to a preferred embodiment of the present invention, in order to further improve the hydrate inhibition effect, the mass ratio of the dimethylaminoalkylacrylamide to the epoxypropyldimethylalkylammonium chloride is 4-7: 1.
According to a preferred embodiment of the present invention, the epoxypropyldimethylalkylammonium chloride has the formula I:
in order to further improve the hydrate inhibition effect, n is 4-12.
According to the invention, the epoxypropyl dimethyl alkyl ammonium chloride is N-2, 3-epoxypropyl dimethyl butyl ammonium chloride or N-2, 3-epoxypropyl dimethyl dodecyl ammonium chloride.
The invention provides an application of the inhibitor in oil and gas exploitation and gathering processes.
The hydrate inhibitor with the properties can effectively inhibit a large amount of generation and aggregation of hydrates at a low dosage (0.5-2.0%), avoid blockage, greatly reduce the dosage of the traditional thermodynamic inhibitor, reduce the burden of logistics support, and has the characteristics of low cost, safety and environmental protection.
The dimethylaminoalkylacrylamides having the aforementioned structure of the present invention can achieve the objects of the present invention without particular requirements on the method of preparation thereof, and the dimethylaminoalkylacrylamides used in the specific examples of the present invention are commercially available chemically pure reagents.
The epoxypropyl dimethyl alkyl ammonium chloride with the structure can achieve the purpose of the invention, has no special requirements on the preparation method, and aiming at the invention, the invention provides a preparation method of epoxypropyl dimethyl alkyl ammonium chloride, which comprises the following steps: the dimethyl alkylamine and the epichlorohydrin are mixed and reacted, and then the product is obtained by purification.
According to a preferred embodiment of the method of the invention, the mixing is carried out in the following manner: under the condition of water bath, dimethyl alkylamine is dripped into epichlorohydrin; preferably, the temperature of the water bath is 35-55 ℃; the time for finishing the dripping is within the range of 20-50 min; the reaction time is determined by the reaction temperature and, according to a preferred embodiment of the invention, is 7 to 8 hours. By the above technical means, the hydrate inhibition effect can be further improved.
According to the method of the present invention, in order to further improve the hydrate inhibition effect, the alkyl group in the dimethyl alkylamine is selected from linear alkyl groups of C4-C12.
According to a preferred embodiment of the process of the invention, the molar ratio of epichlorohydrin to dimethylalkylamine is: 0.4-2: 1; preferably 0.8-1.2: 1. By the above technical means, the hydrate inhibition effect can be further improved.
The invention is further illustrated by the following examples and comparative examples.
The hydrate inhibitor reagent provided by the invention is prepared by adopting a conventional preparation method.
The hydrate blockage inhibition effect of the embodiment of the invention is evaluated by adopting a natural gas hydrate inhibition evaluation experimental device of China university of Petroleum (east China). The experimental device consists of a high-pressure reaction kettle, a thermostatic water bath, a booster pump, a magnetic stirring system, a vacuum pump, a gas flowmeter, a temperature sensor, a pressure sensor, a torque sensor and a data acquisition system. In the experimental process, the temperature, the pressure and the torque in the reaction kettle are monitored and recorded in real time by a data acquisition system. The experimental gas was methane gas. In the experimental process, when a small amount of hydrate particles are generated in the reaction kettle, but the particles are in a dispersed state, the particles cannot be blocked, and the torque value monitored in real time shows that the torque slightly rises, but can be kept in a stable state. When a large amount of hydrate is generated and aggregated, the stirring resistance is increased, and the torque is greatly increased; when hydrate blockage is formed in the reaction kettle, the torque value reaches the peak value, and stirring cannot be continued. Therefore, the hydrate inhibition effect of the hydrate inhibitor is analyzed by the change rule of the torque along with the time. The experimental temperature is 4 ℃, the pressure is 15MPa, and the water depth condition of 1500m is simulated. The stirring rate was 200r/min, simulating wellbore fluid flow conditions. The experimental time is 10h, and hydrate blockage is formed in 10h, which shows that the inhibitor cannot effectively prevent and treat hydrate flow obstacle; and when the time exceeds 10 hours, the blockage is not formed, the stirring can still be normally carried out, and the inhibitor can effectively prevent and control the hydrate blockage within a safe operation time window, so that the wellbore fluid can be safely returned to the ground from the bottom of the well.
In the examples of the present invention, the dimethylaminoalkylacrylamides used are all commercially available chemically pure reagents.
Preparation example 1
Preparation of N-2, 3-epoxypropyl dimethyl butyl ammonium chloride: adding epoxy chloropropane into a three-neck flask, dropwise adding N, N-dimethyl N-butylamine under the condition of water bath at the temperature of 45 ℃, and finishing dropwise adding for 20 min; the molar mass ratio of the epichlorohydrin to the dimethyl n-butylamine is 1: 1.2. The reaction time was 7.5h, and as the reaction proceeded, the solution gradually changed from a transparent liquid to a pale yellow liquid and finally to a yellow gum. Cooling to room temperature, purifying with acetone, and vacuum drying to obtain the target product.
Preparation example 2
The preparation method of the N-2, 3-epoxypropyl dimethyl dodecyl ammonium chloride comprises the following steps: adding epoxy chloropropane into a three-neck flask, dropwise adding dodecyl dimethyl tertiary amine under the condition of 35 ℃ water bath, and finishing dropwise adding for 50 min; the molar mass ratio of the epichlorohydrin to the dodecyl dimethyl tertiary amine is 1: 1. The reaction time was 8h, and as the reaction proceeded, the solution gradually changed from a clear liquid to a yellow liquid and finally to a yellow gum. Cooling to room temperature, purifying with acetone, and vacuum drying to obtain the target product.
Example 1
The N-2, 3-epoxypropyldimethylbutylammonium chloride obtained in preparation example 1 and N- (2-dimethylaminoethyl) acrylamide were mixed in a mass ratio of 1: 3 to obtain hydrate inhibitor a.
100 parts of water and 1.5 parts of hydrate inhibitor a were mixed to obtain a sample solution 1.
Hydrate blockage evaluation experimental results: hydrate blockage is not formed in 10 hours, the maximum torque is 9.0N cm, the flow resistance of fluid in the reaction kettle is small, and no flow obstacle is formed.
Example 2
The N-2, 3-epoxypropyldimethyldodecylammonium chloride obtained in preparation example 2 was mixed with dimethylaminopropylmethacrylamide and dimethylaminopropylacrylamide in a mass ratio of 1: 1 to obtain hydrate inhibitor b.
100 parts of water and 1.5 parts of hydrate inhibitor b were mixed to obtain a sample solution 2.
Hydrate blockage evaluation experimental results: hydrate blockage is not formed in 10 hours, the maximum torque is 8.7N cm, the flow resistance of fluid in the reaction kettle is small, and no flow obstacle is formed.
Example 3
The dimethylamino propyl methacrylamide and the N- (2-dimethylamino ethyl) acrylamide are matched according to the mass ratio of 4: 1 to obtain the hydrate inhibitor c.
100 parts of water and 1.5 parts of hydrate inhibitor c were mixed to obtain a sample solution 3.
Hydrate blockage evaluation experimental results: hydrate blockage is not formed in 10 hours, the maximum torque is 8.9N cm, the flow resistance of fluid in the reaction kettle is small, and no flow obstacle is formed.
Example 4
N-2, 3-epoxypropyldimethyldodecylammonium chloride obtained in preparation example 2 was mixed with dimethylaminopropylmethacrylamide and N- (2-dimethylaminoethyl) acrylamide in a mass ratio of 1: 1 to obtain hydrate inhibitor d.
100 parts of water and 1.5 parts of hydrate inhibitor d are mixed to obtain a sample solution 4.
Hydrate blockage evaluation experimental results: hydrate blockage is not formed in 10 hours, the maximum torque is 8.5N cm, the flow resistance of fluid in the reaction kettle is small, and no flow obstacle is formed.
Example 5
N-2, 3-epoxypropyldimethyldodecylammonium chloride obtained in preparation example 2 was mixed with dimethylaminopropylmethacrylamide and N- (2-dimethylaminoethyl) acrylamide in a mass ratio of 1: 4: 1 to obtain hydrate inhibitor e.
100 parts of water and 1.5 parts of hydrate inhibitor e are mixed to obtain a sample solution 5.
Hydrate blockage evaluation experimental results: hydrate blockage is not formed in 10 hours, the maximum torque is 8.1N cm, the flow resistance of fluid in the reaction kettle is small, and no flow obstacle is formed.
Example 6
The N-2, 3-epoxypropyldimethylbutylammonium chloride obtained in preparation example 1 was mixed with dimethylaminopropylmethacrylamide and N- (2-dimethylaminoethyl) acrylamide in a mass ratio of 1: 2: 1 to obtain a hydrate inhibitor f.
100 parts of water and 1.5 parts of hydrate inhibitor f are mixed to obtain a sample solution 6.
Hydrate blockage evaluation experimental results: hydrate blockage is not formed in 10 hours, the maximum torque is 8.4N cm, the flow resistance of fluid in the reaction kettle is small, and no flow obstacle is formed.
Example 7
N-2, 3-epoxypropyldimethyldodecylammonium chloride obtained in preparation example 2 was mixed with dimethylaminopropylmethacrylamide and N- (2-dimethylaminoethyl) acrylamide in a mass ratio of 1: 4 to obtain a hydrate inhibitor g.
100 parts of water and 1.5 parts of hydrate inhibitor g are mixed to obtain a sample solution 7.
Hydrate blockage evaluation experimental results: hydrate blockage is not formed in 10 hours, the maximum torque is 9.5N cm, the flow resistance of fluid in the reaction kettle is small, and no flow obstacle is formed.
Comparative example 1
The same as in example 2, except that the hydrate inhibitor is water.
Hydrate blockage evaluation experimental results: a large amount of hydrates are formed in the reaction kettle within 0.89h, the torque reaches the peak value of 28.7N cm, the stirring cannot be continued, and the reaction kettle is completely blocked by the hydrates.
Comparative example 2
The same as in example 2, except that the hydrate inhibitor is polyvinylpyrrolidone (a typical hydrate kinetic inhibitor product).
Hydrate blockage evaluation experimental results: the torque reaches the peak value of 27.1N cm at 4.57h, and hydrate blockage is formed in the reaction kettle.
Comparative example 3
The same as in example 2, except that the hydrate inhibitor is 1.5 parts ethylene glycol (a typical hydrate thermodynamic inhibitor product).
Hydrate blockage evaluation experimental results: the torque reaches the peak value of 28.6N cm at 0.94h, and hydrate blockage is formed in the reaction kettle.
Comparative example 4
The N-2, 3-epoxypropyldimethylbutylammonium chloride obtained in preparation example 1 and N- (2-dimethylaminoethyl) acrylamide were mixed in a mass ratio of 2: 1 to obtain a hydrate inhibitor h.
100 parts of water and 1.5 parts of hydrate inhibitor are mixed to obtain a test solution 8.
Hydrate blockage evaluation experimental results: the torque reaches the peak value of 27.7N cm at 2.02h, and hydrate blockage is formed in the reaction kettle.
The experimental results show that the hydrate inhibitor can effectively prevent and treat hydrate blockage under the conditions of deep water, low temperature, high pressure and low dosage.
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, numerous simple modifications can be made to the technical solution of the invention, including combinations of the individual specific technical features in any suitable way. The invention is not described in detail in order to avoid unnecessary repetition. Such simple modifications and combinations should be considered within the scope of the present disclosure as well.
Claims (10)
1. A hydrate inhibitor, characterized in that the inhibitor comprises at least 50 wt% of a dimethylaminoalkylacrylamide.
2. The inhibitor according to claim 1, wherein the inhibitor comprises 60-90 wt% of a dimethylaminoalkylacrylamide.
3. The inhibitor according to claim 1 or 2, wherein the alkyl group of the dimethylaminoalkylacrylamide is a chain alkyl group, preferably a chain alkyl group of C1-C5.
4. The inhibitor according to any one of claims 1 to 3, wherein the dimethylaminoalkyl acrylamide is at least two of dimethylaminopropyl methacrylamide, N- (2-dimethylaminoethyl) acrylamide and dimethylaminopropyl acrylamide.
5. Inhibitor according to claim 4, wherein the dimethylaminoalkyl acrylamide is a mixture of dimethylaminopropyl methacrylamide and N- (2-dimethylaminoethyl) acrylamide, preferably in a mass ratio of 1-4: 1.
6. the inhibitor according to any one of claims 1 to 5, wherein the inhibitor further comprises epoxypropyldimethylalkylammonium chloride.
7. The inhibitor according to claim 6, wherein the epoxypropyldimethylalkylammonium chloride content is 10-40 wt%.
8. The inhibitor according to claim 6 or 7, wherein the mass ratio of the dimethylaminoalkylacrylamide to the epoxypropyldimethylalkylammonium chloride is 2-7: 1.
9. The inhibitor according to any one of claims 1 to 8, wherein the epoxypropyldimethylammonium chloride has the formula I:
wherein n is 4-12.
10. Use of the inhibitor of any one of claims 1-9 in oil and gas production and gathering processes.
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Cited By (1)
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| CN115141312A (en) * | 2022-07-20 | 2022-10-04 | 西南石油大学 | Hydrate inhibitor based on vinyl pyrrolidone and preparation method thereof |
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| NL2032283A (en) | 2023-01-03 |
| CN113583645B (en) | 2022-08-02 |
| NL2032283B1 (en) | 2023-02-08 |
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