CN116143639A - High-temperature-resistant clay stabilizer for deep anti-swelling of thickened oil thermal recovery and preparation method thereof - Google Patents

High-temperature-resistant clay stabilizer for deep anti-swelling of thickened oil thermal recovery and preparation method thereof Download PDF

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CN116143639A
CN116143639A CN202111384292.XA CN202111384292A CN116143639A CN 116143639 A CN116143639 A CN 116143639A CN 202111384292 A CN202111384292 A CN 202111384292A CN 116143639 A CN116143639 A CN 116143639A
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temperature
clay stabilizer
tertiary amine
propylene oxide
resistant clay
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江洋洋
王康
魏开轩
逯贵广
黄冬
杨阳
曾志强
王玉
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China Petroleum and Chemical Corp
Sinopec Nanjing Chemical Industry Corp
Research Institute of Sinopec Nanjing Chemical Industry Co Ltd
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China Petroleum and Chemical Corp
Sinopec Nanjing Chemical Industry Corp
Research Institute of Sinopec Nanjing Chemical Industry Co Ltd
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    • C07—ORGANIC CHEMISTRY
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    • C07C217/00—Compounds containing amino and etherified hydroxy groups bound to the same carbon skeleton
    • C07C217/02—Compounds containing amino and etherified hydroxy groups bound to the same carbon skeleton having etherified hydroxy groups and amino groups bound to acyclic carbon atoms of the same carbon skeleton
    • C07C217/04—Compounds containing amino and etherified hydroxy groups bound to the same carbon skeleton having etherified hydroxy groups and amino groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being acyclic and saturated
    • C07C217/06—Compounds containing amino and etherified hydroxy groups bound to the same carbon skeleton having etherified hydroxy groups and amino groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being acyclic and saturated having only one etherified hydroxy group and one amino group bound to the carbon skeleton, which is not further substituted
    • C07C217/08—Compounds containing amino and etherified hydroxy groups bound to the same carbon skeleton having etherified hydroxy groups and amino groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being acyclic and saturated having only one etherified hydroxy group and one amino group bound to the carbon skeleton, which is not further substituted the oxygen atom of the etherified hydroxy group being further bound to an acyclic carbon atom
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    • C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/02—Well-drilling compositions
    • C09K8/03—Specific additives for general use in well-drilling compositions
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    • C09K8/00—Compositions for drilling of boreholes or wells; Compositions for treating boreholes or wells, e.g. for completion or for remedial operations
    • C09K8/50—Compositions for plastering borehole walls, i.e. compositions for temporary consolidation of borehole walls
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    • C09K8/607—Compositions for stimulating production by acting on the underground formation specially adapted for clay formations
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    • C09K2208/00—Aspects relating to compositions of drilling or well treatment fluids
    • C09K2208/12—Swell inhibition, i.e. using additives to drilling or well treatment fluids for inhibiting clay or shale swelling or disintegrating

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Abstract

The invention provides a high-temperature-resistant clay stabilizer for deep anti-swelling of thickened oil thermal recovery and a preparation method thereof, wherein a plurality of ammonium ions, epoxypropane hydrophobic chain segments and a temperature-resistant benzene ring structure exist in the structure, and the high-temperature-resistant clay stabilizer has the advantages of strong adsorptivity, obvious hydrophobic effect, good temperature resistance, no chromatographic separation and the like. The high-temperature-resistant clay stabilizer provided by the invention has the anti-swelling rate reaching more than 90%, the temperature resistance reaching 300 ℃, the water washing resistance reaching 100%, and the core permeability retention value reaching more than 90%, and can be used for the deep anti-swelling of thick oil thermal recovery, and can be used for the swelling treatment of an oil well and the anti-swelling treatment of the oil well.

Description

High-temperature-resistant clay stabilizer for deep anti-swelling of thickened oil thermal recovery and preparation method thereof
Technical Field
The invention relates to a high-temperature-resistant clay stabilizer, a preparation method and application thereof in thick oil heat utilization.
Background
Clay minerals are widely present in oil layers, and 97% of the world's oil layers contain clay minerals to varying degrees. Typically, when the reservoir contains 5% to 20% clay, it is considered to be the higher clay content reservoir. If improper measures are taken during the development process, clay minerals can be caused to expand, disperse and migrate, thereby blocking the throat of the pore structure of the stratum, reducing the permeability of the stratum and generating stratum damage. During expansion, the clay absorbs water into the crystal structure, resulting in an increase in the volume of the clay, thereby blocking the formation pore channels; during migration, clay materials are dispersed by extraneous fluids or carried by the produced fluids, forming bridging or choking points at the pore throat of the capillaries, which can easily lead to a decrease in formation permeability. Therefore, in any technological measures such as drilling, well cementation, water injection, fracturing, acidification, well repair and well killing, and the like, water-sensitive injuries can be possibly caused as long as water-based working fluid invades in a reservoir with high clay content and strong water sensitivity, and the most common method for solving the water-sensitive injuries is to add a clay stabilizer into injected water, so that the research and development and use of a high-quality and high-efficiency anti-swelling agent are important measures for guaranteeing stable production of oil fields.
The medium petrochemical industry has ascertained that the thick oil resource accounts for about 102 hundred million tons and accounts for 38 percent of the medium petrochemical oil resource, and is mainly distributed in oil fields such as victory, northwest, henan and the like, thereby being a main battlefield for increasing the storage and the production in China in the future. In the thick oil thermal recovery process, high-temperature steam needs to be injected, the temperature reaches 300 ℃, and therefore, higher requirements are put on the temperature resistance of the clay stabilizer. At present, a clay stabilizer is commonly used for protecting stratum permeability in a shallow layer area, the temperature resistance is generally below 200 ℃, and two possibilities exist mainly in analysis of insufficient temperature resistance, namely, the heat stability of the treating agent is insufficient, decomposition occurs in a high-temperature state, and the swelling prevention effect cannot be achieved; secondly, the adsorptivity of the treating agent with clay is weakened at high temperature, and effective adsorption cannot be formed in the clay, so that the action effect is deteriorated. The method of compounding and using several treating agents can improve the temperature resistance, but the chromatographic separation phenomenon in the pore canal of the reservoir also exists, so that the field use effect is not satisfactory, and the deep expansion prevention effect cannot be achieved.
Disclosure of Invention
The invention provides a high-temperature-resistant clay stabilizer for deep anti-swelling of thickened oil thermal recovery and a preparation method thereof, wherein a plurality of ammonium ions, epoxypropane hydrophobic chain segments and a temperature-resistant benzene ring structure exist in the structure, and the high-temperature-resistant clay stabilizer has the advantages of strong adsorptivity, obvious hydrophobic effect, good temperature resistance, no chromatographic separation and the like.
The technical scheme adopted by the invention is as follows: a high-temperature-resistant clay stabilizer for thick oil thermal recovery depth expansion prevention is characterized in that: the molecular structure of the high temperature resistant clay stabilizer contains a propylene oxide hydrophobic chain, a high temperature resistant benzene ring structure and ammonium ions which can be strongly adsorbed in a stratum, and the structural general formula is as follows:
Figure 261610DEST_PATH_IMAGE001
wherein m is 1-10; r is methyl, ethyl, propyl or butyl; x is halogen.
The invention also provides a preparation method of the high-temperature-resistant clay stabilizer for deep thermal recovery of thickened oil, which is prepared by reacting tertiary amine containing propylene oxide hydrophobic chain in a molecular structure with benzyl halide, wherein the molecular structural general formula of the tertiary amine containing propylene oxide hydrophobic chain is as follows:
Figure 690187DEST_PATH_IMAGE002
wherein m is 1-10; r is methyl, ethyl, propyl or butyl.
The reaction conditions of the tertiary amine containing the propylene oxide hydrophobic chain and the benzyl halide are as follows: the reaction temperature is 80-90 ℃, the reaction time is 2-6h, the mass ratio of tertiary amine to halogenated benzyl substance is 1:2-1:3, preferably 1:2-1:2.3, and the halogenated benzyl is preferably benzyl chloride.
The tertiary amine containing the propylene oxide hydrophobic chain is prepared by directly reacting polyether alcohol with dialkylamine in the presence of a catalyst and hydrogen, and the molecular structural general formula of the polyether alcohol is as follows:
Figure 965310DEST_PATH_IMAGE003
wherein m is 1-10.
The reaction condition of polyether alcohol and dialkyl amine is that the catalyst dosage is 0.1-5%, preferably 0.5-1%; the reaction temperature is 185-245 ℃, the hydrogen partial pressure is 2.5-4.5MPa, and the reaction time is 3-6h.
The catalyst used for the reaction of the polyether alcohol and the dialkyl amine is a Ni/Al catalyst, wherein the Ni content is 25-40%.
The dialkylamine is dimethylamine, diethylamine, dipropylamine or dibutylamine.
The high-temperature-resistant clay stabilizer has the temperature resistance not lower than 300 ℃, can be used for thermal recovery of thick oil to prevent swelling, and can be used for oil well swelling treatment and swelling prevention treatment.
The invention provides a high-temperature resistant clay stabilizer for deep anti-swelling of thickened oil thermal recovery, which comprises two ammonium ions in the structure, wherein the adsorption force of the ammonium ions to stratum is far stronger than the lone pair electron effect on amino nitrogen, the adsorption force of the ammonium ions to stratum is firm, the two ammonium ions can form a plurality of effects of adsorption to clay, the adsorption is favorably enhanced, the ammonium ions can still be adsorbed in the clay under the high-temperature condition, and the anti-swelling effect is achieved; secondly, the structure of the clay contains a hydrophobic epoxypropane chain segment, and after the hydrophobic epoxypropane chain segment is adsorbed in the clay, the hydrophobic property of the epoxypropane chain not only can drive away water molecules in the clay, but also can prevent the water molecules from entering the clay; thirdly, a benzene ring structure is introduced into a side chain of the molecular structure, so that the thermal stability of the structure is improved, the steric hindrance effect is increased, and the entering opportunity of water molecules is further weakened; fourth, as a single substance with various properties, the chromatographic separation phenomenon in the reservoir during injection is avoided, the stability of the properties is maintained, and the deep anti-swelling effect can be achieved.
The temperature-resistant clay stabilizer provided by the invention has better anti-swelling property, temperature resistance and water washing resistance, the anti-swelling rate reaches more than 90%, the temperature resistance reaches 300 ℃, the water washing resistance reaches 100%, and the core permeability retention value reaches more than 90%.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1
(1) Preparation of tertiary amines containing propylene oxide hydrophobic chains
The molecular structure of the polyether alcohol is selected as follows:
Figure 546464DEST_PATH_IMAGE003
wherein m is 5.
Ni/Al catalyst with Ni content of 30% is selected, the dosage is 1%, dimethylamine is selected as dialkylamine, the amination reaction temperature is 245 ℃, the hydrogen partial pressure is 2.5MPa, and the reaction time is 4 hours, so that tertiary amine containing propylene oxide hydrophobic chain is prepared.
(2) Preparation of high temperature resistant clay stabilizer
And (3) reacting the tertiary amine containing the propylene oxide hydrophobic chain prepared in the step (1) with benzyl chloride at a reaction temperature of 90 ℃, wherein the amount of the tertiary amine and the benzyl chloride is 1:2, and the reaction time is 4 hours, so as to prepare the high-temperature-resistant clay stabilizer.
Example 2
(1) Preparation of tertiary amines containing propylene oxide hydrophobic chains
The molecular structure of the polyether alcohol is selected as follows:
Figure 881631DEST_PATH_IMAGE003
wherein m is 1.
Ni/Al catalyst with Ni content of 40% is selected, the dosage is 0.1%, diethylamine is selected as dialkylamine, the amination reaction temperature is 215 ℃, the hydrogen partial pressure is 4.5MPa, and the reaction time is 6 hours, so that tertiary amine containing propylene oxide hydrophobic chain is prepared.
(2) Preparation of high temperature resistant clay stabilizer
And (3) reacting the tertiary amine containing the propylene oxide hydrophobic chain prepared in the step (1) with benzyl bromide at a reaction temperature of 80 ℃, wherein the amount of the tertiary amine and benzyl chloride substances is 1:3, and the reaction time is 6 hours, so as to prepare the high-temperature-resistant clay stabilizer.
Example 3
(1) Preparation of tertiary amines containing propylene oxide hydrophobic chains
The molecular structure of the polyether alcohol is selected as follows:
Figure 797503DEST_PATH_IMAGE003
wherein m is 10.
Ni/Al catalyst with Ni content of 25% is selected, the dosage is 5%, dipropylamine is selected as dialkylamine, the amination reaction temperature is 185 ℃, the hydrogen partial pressure is 3.0MPa, and the reaction time is 3 hours, so that tertiary amine containing propylene oxide hydrophobic chain is prepared.
(2) Preparation of high temperature resistant clay stabilizer
And (3) reacting the tertiary amine containing the propylene oxide hydrophobic chain prepared in the step (1) with benzyl chloride at a reaction temperature of 85 ℃, wherein the amount of the tertiary amine and the benzyl chloride is 1:2.3, and the reaction time is 3 hours, so as to prepare the high-temperature-resistant clay stabilizer.
Example 4
(1) Preparation of tertiary amines containing propylene oxide hydrophobic chains
The molecular structure of the polyether alcohol is selected as follows:
Figure 876317DEST_PATH_IMAGE003
wherein m is 2.
Ni/Al catalyst with Ni content of 35% is selected, the dosage is 0.5%, dibutylamine is selected as dialkylamine, the amination reaction temperature is 235 ℃, the hydrogen partial pressure is 3.5MPa, and the reaction time is 5 hours, so that tertiary amine containing propylene oxide hydrophobic chain is prepared.
(2) Preparation of high temperature resistant clay stabilizer
And (3) reacting the tertiary amine containing the propylene oxide hydrophobic chain prepared in the step (1) with benzyl chloride at a reaction temperature of 90 ℃, wherein the amount of the tertiary amine and the benzyl chloride is 1:2.5, and the reaction time is 2 hours, so as to prepare the high-temperature-resistant clay stabilizer.
Example 5
(1) Preparation of tertiary amines containing propylene oxide hydrophobic chains
The molecular structure of the polyether alcohol is selected as follows:
Figure 374295DEST_PATH_IMAGE003
wherein m is 8.
Ni/Al catalyst with Ni content of 30% is selected, the dosage is 4%, dimethylamine is selected as dialkylamine, the amination reaction temperature is 225 ℃, the hydrogen partial pressure is 4.0MPa, and the reaction time is 4.5 hours, so that tertiary amine containing propylene oxide hydrophobic chain is prepared.
(2) Preparation of high temperature resistant clay stabilizer
And (3) reacting the tertiary amine containing the propylene oxide hydrophobic chain prepared in the step (1) with benzyl chloride at a reaction temperature of 85 ℃, wherein the amount of the tertiary amine and the benzyl chloride is 1:2.2, and the reaction time is 4 hours, so as to prepare the high-temperature-resistant clay stabilizer.
Example 6
(1) Preparation of tertiary amines containing propylene oxide hydrophobic chains
The molecular structure of the polyether alcohol is selected as follows:
Figure 801734DEST_PATH_IMAGE003
wherein m is 4.
Ni/Al catalyst with Ni content of 35% is selected, the dosage is 2.5%, dimethylamine is selected as dialkylamine, the amination reaction temperature is 205 ℃, the hydrogen partial pressure is 4.0MPa, and the reaction time is 3.5h, so that tertiary amine containing propylene oxide hydrophobic chain is prepared.
(2) Preparation of high temperature resistant clay stabilizer
And (3) reacting the tertiary amine containing the propylene oxide hydrophobic chain prepared in the step (1) with benzyl chloride at a reaction temperature of 85 ℃, wherein the amount of the tertiary amine and the benzyl chloride is 1:2.1, and the reaction time is 3.5h, so as to prepare the high-temperature-resistant clay stabilizer.
Example 7
(1) Preparation of tertiary amines containing propylene oxide hydrophobic chains
The molecular structure of the polyether alcohol is selected as follows:
Figure 486793DEST_PATH_IMAGE003
wherein m is 6.
Ni/Al catalyst with Ni content of 35% is selected, the dosage is 0.7%, dimethylamine is selected as dialkylamine, the amination reaction temperature is 195 ℃, the hydrogen partial pressure is 4.0MPa, and the reaction time is 4 hours, so that tertiary amine containing propylene oxide hydrophobic chain is prepared.
(2) Preparation of high temperature resistant clay stabilizer
And (3) reacting the tertiary amine containing the propylene oxide hydrophobic chain prepared in the step (1) with benzyl chloride at the reaction temperature of 88 ℃, wherein the amount of the tertiary amine and benzyl chloride is 1:2.2, and the reaction time is 4.5h, so as to prepare the high-temperature-resistant clay stabilizer.
Example 8
(1) Preparation of tertiary amines containing propylene oxide hydrophobic chains
The molecular structure of the polyether alcohol is selected as follows:
Figure 838140DEST_PATH_IMAGE003
wherein m is 3.
Ni/Al catalyst with Ni content of 30% is selected, the dosage is 0.8%, dimethylamine is selected as dialkylamine, the amination reaction temperature is 210 ℃, the hydrogen partial pressure is 4.0MPa, and the reaction time is 4 hours, so that tertiary amine containing propylene oxide hydrophobic chain is prepared.
(2) Preparation of high temperature resistant clay stabilizer
And (3) reacting the tertiary amine containing the propylene oxide hydrophobic chain prepared in the step (1) with benzyl chloride at 83 ℃, wherein the amount of the tertiary amine and benzyl chloride is 1:2.3, and the reaction time is 4h, so as to prepare the high-temperature-resistant clay stabilizer.
Comparative example 1
The tertiary amine obtained in example 4 was directly used as a clay stabilizer.
Comparative example 2
The tertiary amine and potassium chloride prepared in the example 4 are compounded according to the mass ratio of 6:1 to be used as clay stabilizer.
Comparative example 3
The tertiary amine prepared in the example 4 and common cationic quaternary ammonium salt hexadecyl trimethyl ammonium chloride are compounded according to the mass ratio of 2:1 to be used as a clay stabilizer
Comparative example 4
The tertiary amine prepared in the example 4 is compounded with common cationic quaternary ammonium salt hexadecyl trimethyl ammonium chloride and potassium chloride according to the mass ratio of 6:3:1 to be used as a clay stabilizer.
Test example 1
The anti-swelling rate test is carried out according to SY/T5971-2016 clay stabilizer for water injection performance evaluation method, and the steps are as follows: weighing 0.5g of sodium bentonite, adding into a 10mL centrifuge tube, adding deionized water to a 10mL scale, shaking fully, standing at room temperature for 2h, loading into a centrifuge, centrifuging at a rotating speed of 1500r/min for 15min, and reading the volume V2 of the sodium bentonite in water. The same procedure was used to measure the volume V1 of the centrifuged soil by replacing the clear water with a clay stabilizer aqueous solution of a certain concentration. The volume V0 of the soil was measured with kerosene instead of water.
Figure 190624DEST_PATH_IMAGE004
Wherein: η -anti-swelling rate,%; v (V) 0 -volume of sodium bentonite in kerosene, mL; v (V) 1 -volume of sodium bentonite in clay stabiliser, mL; v (V) 2 -volume of sodium bentonite in clear water, mL.
Test example 2
The anti-swelling rate test procedure after aging at 300 ℃ is as follows:
(1) Weighing 3.00g of bentonite powder to 0.01g accurately, and filling the bentonite powder into a high-temperature high-pressure closed reactor;
(2) Adding 60mL of clay stabilizer solution with the concentration of 4%, fully shaking and uniformly mixing, putting into a baking oven with the temperature of 300+/-2 ℃ for 24 hours, and cooling to room temperature;
(3) Transferring all clay mixed liquid in the high-temperature high-pressure sealed reactor into a 100mL beaker, fully shaking uniformly, rapidly taking out 10mL, adding into a glass centrifuge tube, loading into a centrifuge with an automatic balancing function, centrifuging for 15min at 1500r/min, and reading the expansion volume V1 of bentonite. The calculation formula of the anti-swelling rate is as follows:
Figure 133172DEST_PATH_IMAGE006
wherein: v (V) 0 Is the expansion volume of bentonite in kerosene; v (V) 1 Is the expansion volume of bentonite in clay stabilizer aqueous solution; v (V) 2 Is the expansion volume of bentonite in clear water;
test example 3
The washing resistance test steps are as follows:
pouring out supernatant in the centrifuge tube after centrifuging in the test example 2, adding deionized water to 10mL, stirring thoroughly, standing for 2h, and rotating at 1500r/min in the centrifugeQuick centrifugation is carried out for 15min, and finally the final volume V of the bentonite in the centrifuge tube is read out 1’ 。
The water resistance rate calculation formula:
Figure 758057DEST_PATH_IMAGE007
wherein: v (V) 1 The swelling volume of bentonite in the clay stabilizer aqueous solution is mL;
V 1’ the volume of the bentonite is the expansion volume of the bentonite after washing with water, and the volume is mL; v (V) 2 Is the expansion volume of bentonite in clear water, mL.
Test example 4
Testing the permeability K of an original rock core by adopting a rock core displacement test 0 Then the core is saturated with simulated formation water, then a clay stabilizer solution system is injected into a core tube at 300 ℃, then high-temperature steam at 300 ℃ is injected, and finally the permeability K of the core after the experiment is tested 1 ，K 1 /K 0 And the core permeability retention value is obtained.
Table 1 sample evaluation results
Figure DEST_PATH_IMAGE008
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Claims (10)

1. A high-temperature-resistant clay stabilizer for thick oil thermal recovery depth expansion prevention is characterized in that: the molecular structure of the high temperature resistant clay stabilizer contains a propylene oxide hydrophobic chain, a high temperature resistant benzene ring structure and ammonium ions which can be strongly adsorbed in a stratum, and the structural general formula is as follows:
Figure 838844DEST_PATH_IMAGE001
wherein m is 1-10; r is methyl, ethyl, propyl or butyl; x is halogen.
2. The method for preparing the high-temperature-resistant clay stabilizer for deep thermal recovery expansion prevention of thick oil according to claim 1, wherein the high-temperature-resistant clay stabilizer is prepared by reacting tertiary amine containing propylene oxide hydrophobic chain in molecular structure with benzyl halide, and the molecular structural general formula of the tertiary amine containing propylene oxide hydrophobic chain is as follows:
Figure 680898DEST_PATH_IMAGE002
wherein m is 1-10; r is methyl, ethyl, propyl or butyl.
3. The preparation method according to claim 2, wherein the reaction conditions of the tertiary amine containing a hydrophobic chain of propylene oxide and benzyl halide are as follows: the reaction temperature is 80-90 ℃, the reaction time is 2-6h, and the amount ratio of tertiary amine to halogenated benzyl substance is 1:2-1:3, preferably 1:2-1:2.3.
4. A process according to claim 2 or 3, characterized in that the benzyl halide is benzyl chloride.
5. A process according to claim 2 or 3, characterized in that the tertiary amine containing a hydrophobic chain of propylene oxide is obtained by direct reaction of a polyether alcohol with a dialkylamine in the presence of a catalyst, hydrogen, said polyether alcohol having the general molecular structure:
Figure 76107DEST_PATH_IMAGE003
wherein m is 1-10.
6. The process according to claim 5, wherein the reaction conditions of the polyether alcohol with the dialkylamine are: the catalyst consumption is 0.1-5%, the reaction temperature is 185-245 ℃, the hydrogen partial pressure is 2.5-4.5MPa, and the reaction time is 3-6h.
7. The process according to claim 6, wherein the catalyst is used in an amount of 0.5 to 1% by weight of the polyether alcohol to be reacted with the dialkylamine.
8. The process according to claim 5, wherein the catalyst used for the reaction of the polyether alcohol with the dialkylamine is a Ni/Al catalyst, wherein the Ni content is 25 to 40%.
9. The preparation method according to claim 5, wherein the dialkylamine is dimethylamine, diethylamine, dipropylamine or dibutylamine.
10. The high-temperature-resistant clay stabilizer for deep thermal recovery of thickened oil, which is disclosed in claim 1, is characterized in that the high-temperature-resistant clay stabilizer has a temperature resistance of not lower than 300 ℃ and is used for thermal recovery expansion treatment and expansion prevention treatment of thickened oil.
CN202111384292.XA 2021-11-22 2021-11-22 High-temperature-resistant clay stabilizer for deep anti-swelling of thickened oil thermal recovery and preparation method thereof Pending CN116143639A (en)

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