CN113292980B - Water-soluble thickened oil viscosity reducer and preparation method and application thereof - Google Patents
Water-soluble thickened oil viscosity reducer and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a water-soluble thickened oil viscosity reducer and a preparation method and application thereof, and belongs to the technical field of thickened oil viscosity reduction exploitation. The water-soluble thickened oil viscosity reducer comprises 5-10 wt% of free aza-carbene, 1-2wt% of cobalt dodecyl benzene sulfonate, 15-30 wt% of an oxidant, 1-5 wt% of a hydrogen donor, 1-2wt% of alkali, 0.5-1 wt% of an emulsifier and the balance of a solvent, wherein the total amount is 100%. The invention also provides a preparation method of the water-soluble thickened oil viscosity reducer, which comprises the following steps: mixing cobalt dodecylbenzene sulfonate with a solvent, then adding an oxidant and a hydrogen donor for mixing, then continuously adding alkali and an emulsifier for mixing, and then adding free aza-carbene for mixing to obtain the water-soluble thickened oil viscosity reducer. In addition, the invention also provides application of the water-soluble thickened oil viscosity reducer in treating thickened oil. The viscosity reducer can effectively improve the viscosity reducing rate of thick oil and accelerate the viscosity reducing speed.
Description
Technical Field
The invention relates to the technical field of thickened oil viscosity reduction exploitation, and particularly relates to a water-soluble thickened oil viscosity reducer and a preparation method and application thereof.
Background
The sulfoxide and the sulfone have higher application value in the pesticide and medicine field, and can be obtained by catalytic oxidation desulfurization and sulfur-based impurity removal of crude oil as an intermediate in the desulfurization process. The oxidation of thioethers to polysulfone-based organic compounds is well established. In the research of the field of viscosity reduction of thickened oil, a water-soluble catalytic oxidation system for underground in-situ modification of thickened oil is designed, the viscosity reduction reaction of thickened oil is carried out in a stratum oil reservoir through low-temperature catalytic oxidation, and products of sulfoxide and sulfone are obtained underground in situ, so that high-efficiency viscosity reduction is realized.
The viscous oil has the characteristics of high viscosity, high condensation point, poor fluidity in stratum and the like, so that the viscous oil is difficult to effectively exploit by adopting a conventional method. At present, heavy oil recovery technologies mainly comprise cold recovery technologies, hot recovery technologies and composite recovery technologies combining cold recovery and hot recovery. Among these mining techniques, the thermal mining technique mainly based on steam injection is most widely used.
In order to ensure the safety in the air injection oil extraction process and improve the economy of the oil extraction process, the southwest university of petroleum group in 2002 proposes a heavy oil reservoir air injection low-temperature catalytic oxidation oil extraction technology, which is characterized in that in the process of injecting air to extract heavy oil under the oil reservoir condition, a proper catalyst is injected to improve the low-temperature oxidation rate of crude oil, so that the oxygen consumption is increased and heat is released, and simultaneously flue gas or nitrogen is formed to assist in externally injecting high-dryness steam to improve the recovery rate of the heavy oil. However, the safety problem of the low-temperature catalytic oxidation technology for injecting air into thick oil has been the focus of academic attention, especially the safety of a production well, and the O in the produced gas must be ensured when the air breaks through 2 Is below the explosion safety threshold (5%). For this reason, the current trend is to oxidize the source O 2 By replacement with organic hydrogen peroxide compounds, H 2 O 2 、KIO 4 、NaIO 4 And the viscosity is reduced by adding a catalyst under the condition of adding or not adding a solvent. The problem of low viscosity reduction rate and long viscosity reduction time still exists.
Disclosure of Invention
The invention aims to overcome the technical defects, provides a water-soluble thickened oil viscosity reducer as well as a preparation method and application thereof, and solves the technical problem that the viscosity reducing rate is low and the viscosity reducing time is long in the prior art.
In order to achieve the technical purpose, the technical scheme of the invention provides a water-soluble thickened oil viscosity reducer and a preparation method and application thereof.
The invention provides a water-soluble thickened oil viscosity reducer, which comprises, by mass, 5-10 wt% of free aza-carbene, 1-2wt% of cobalt dodecyl benzene sulfonate, 15-30 wt% of an oxidant, 1-5 wt% of a hydrogen donor, 1-2wt% of an alkali, 0.5-1 wt% of an emulsifier, and the balance of a solvent, wherein the total amount is 100%.
Further, the oxidizing agent is tert-butyl hydroperoxide.
Further, the hydrogen donor is methanol.
Further, the base is sodium hydroxide.
Further, the solvent is benzene.
Further, the emulsifier is one or two of tween 20 and span 20.
Further, 1-5% of sodium dihydrogen phosphate is also included.
The invention also provides a preparation method of the water-soluble thickened oil viscosity reducer, which comprises the following steps: mixing cobalt dodecyl benzene sulfonate with a solvent, then adding an oxidant and a hydrogen donor for mixing, then continuously adding alkali and an emulsifier for mixing, and then adding free aza-carbene for mixing to obtain the water-soluble thickened oil viscosity reducer.
Further, the cobalt dodecylbenzene sulfonate is mixed with the solvent at 25-40 ℃.
In addition, the invention also provides an application of the water-soluble thickened oil viscosity reducer or the water-soluble thickened oil viscosity reducer prepared by the preparation method in treating thickened oil.
Compared with the prior art, the invention has the beneficial effects that: a small amount of emulsifier can realize that the partial degradation of viscous crude separates out metal ion, a small amount of dodecylbenzene sulfonic acid cobalt has surface active group, can effectively strengthen the mutual repulsion effect between the asphaltene particle, improve repulsion force and anti-agglomeration force between the asphaltene particle, improve the mobility of viscous crude, and then be favorable to free aza carbene to get into in the viscous crude and the metal ion complex in the viscous crude, can effectively improve the viscidity rate of viscous crude and accelerated the viscidity rate under the cooperation of other components, viscidity 12h falls, viscidity rate reaches more than 90%.
Drawings
FIG. 1 is a chemical structure identification NMR chart of free azacarbene of the present invention;
FIG. 2 is a FT-IR spectrum of thick oil before and after visbreaking in an example of the present invention.
Detailed Description
The specific embodiment provides a water-soluble thickened oil viscosity reducer, which comprises, by mass, 5-10 wt% of free aza-carbene, 1-2wt% of cobalt dodecyl benzene sulfonate, 15-30 wt% of an oxidant, 1-5 wt% of a hydrogen donor, 1-2wt% of an alkali, 0.5-1 wt% of an emulsifier, and the balance of a solvent, wherein the total amount is 100%.
Further, in this embodiment, the oxidant is tert-butyl hydroperoxide, the hydrogen donor is methanol, the alkali is sodium hydroxide, the solvent is benzene, and the emulsifier is one or two of tween 20 and span 20.
In certain preferred embodiments, the water-soluble thickened oil viscosity reducer further comprises 1-5 wt% of sodium dihydrogen phosphate. Sodium dihydrogen phosphate can provide proton, and the steady progress that falls is glued to improve and fall and glue the effect.
The specific embodiment further comprises a preparation method of the water-soluble thickened oil viscosity reducer, which comprises the following steps: mixing cobalt dodecyl benzene sulfonate with a solvent at 25-40 ℃, then adding an oxidant and a hydrogen donor for mixing, then continuing adding alkali and an emulsifier for mixing, and then adding free nitrogen carbene for mixing to obtain the water-soluble thickened oil viscosity reducer.
The specific embodiment further comprises an application of the water-soluble thickened oil viscosity reducer or the water-soluble thickened oil viscosity reducer prepared by the preparation method in thickened oil treatment.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
It is noted that the free azacarbenes in the following examples were prepared by the following steps:
adding 2, 6-diisopropylaniline, 40% glyoxal and formic acid into absolute ethyl alcohol for reaction for 2d, filtering, and washing with cold methanol to obtain the diaza-butadiene; wherein the molar ratio of the 2, 6-diisopropylaniline to the glyoxal is 2: 1; the yield of diazabetadine was 89.2%;
stirring paraformaldehyde and HCl (4M in dioxane) at 30 ℃ for 12 hours, then adding a mixture of diazadiene and THF, continuously stirring at room temperature for reacting for 4 hours, and filtering and washing to obtain the 1, 3-bis (2, 6-diisopropyl-1-phenyl) imidazolium chloride; the molar ratio of the diazabetadine, the paraformaldehyde, and the HCl is 1:1: 1; the yield of 1, 3-bis (2, 6-diisopropyl-1-phenyl) imidazolium chloride was 88.4%;
mixing 1, 3-bis (2, 6-diisopropyl-1-phenyl) imidazolium chloride and potassium tert-butoxide according to a molar ratio of 1:1, adding into a first organic solvent THF, stirring at room temperature for reaction for 4h, extracting with ethyl acetate, drying and purifying to obtain the free azacarbene; the yield of free azacarbene is 66.7%; in FIG. 1, the free azacarbene 1H-NMR (400MHz, C6D6) is D1.13 (D, J ═ 9.2Hz,12H, CH (CH) 3 ) 2 ),1.23(d,J＝9.2Hz,12H,CH(CH 3 ) 2 ),2.91(sep,J＝9.2Hz,4H,CH(CH 3 ) 2 ),6.57(s,2H,NCH),7.11(m,4H,m-C 6 H 3 ),7.22(m,2H,p-C 6 H 3 )。
The structural formula of the free azacarbene is as follows:
example 1
The embodiment provides a water-soluble thickened oil viscosity reducer, which comprises, by mass, 5 wt% of free azacarbene, 2wt% of cobalt dodecylbenzene sulfonate, 30 wt% of tert-butyl hydroperoxide as an oxidant, 3 wt% of methanol as a hydrogen donor, 1 wt% of sodium hydroxide as an alkali, 201 wt% of tween as an emulsifier, and the balance of benzene as a solvent, wherein the total amount is 100%.
The water-soluble thickened oil viscosity reducer of the embodiment is prepared by the following steps:
mixing cobalt dodecyl benzene sulfonate with a solvent at 25 ℃, then adding an oxidant and a hydrogen donor for mixing, then continuously adding alkali and an emulsifier for mixing, and then adding free aza-carbene for mixing to obtain the water-soluble thickened oil viscosity reducer.
Example 2
This example provides a water-soluble thickened oil viscosity reducer, which includes, by mass, 8 wt% of free azacarbene, 1 wt% of cobalt dodecylbenzenesulfonate, 20 wt% of tert-butyl hydroperoxide as an oxidant, 5 wt% of methanol as a hydrogen donor, 2wt% of an alkali, 200.5 wt% of span as an emulsifier, and the balance of benzene as a solvent, and the total is 100%.
The water-soluble thickened oil viscosity reducer of the embodiment is prepared by the following steps:
mixing cobalt dodecyl benzene sulfonate with a solvent at 30 ℃, then adding an oxidant and a hydrogen donor for mixing, then continuously adding alkali and an emulsifier for mixing, and then adding free nitrogen carbene for mixing to obtain the water-soluble thickened oil viscosity reducer.
Example 3
This example provides a water-soluble heavy oil viscosity-reducing agent, which includes, by mass, 10 wt% of free azacarbene, 1 wt% of cobalt dodecylbenzenesulfonate, 15 wt% of tert-butyl hydroperoxide as an oxidant, 1 wt% of methanol as a hydrogen donor, 1.5 wt% of sodium hydroxide as an alkali, 200.8 wt% of tween as an emulsifier, and the balance being solvent benzene, and the total is 100%.
The water-soluble thickened oil viscosity reducer of the embodiment is prepared by the following steps:
mixing cobalt dodecyl benzene sulfonate with a solvent at 30 ℃, then adding an oxidant and a hydrogen donor for mixing, then continuously adding alkali and an emulsifier for mixing, and then adding free aza-carbene for mixing to obtain the water-soluble thickened oil viscosity reducer.
Example 4
This example provides a water-soluble thickened oil viscosity reducer, which comprises, by mass, 6 wt% of free azacarbene, 1.5 wt% of cobalt dodecylbenzenesulfonate, 20 wt% of tert-butyl hydroperoxide as an oxidant, 3 wt% of methanol as a hydrogen donor, 1.5 wt% of alkali sodium hydroxide, 200.8 wt% of span as an emulsifier, and the balance being solvent benzene, and the total is 100%.
The water-soluble thickened oil viscosity reducer of the embodiment is prepared by the following steps:
mixing cobalt dodecyl benzene sulfonate with a solvent at 40 ℃, then adding an oxidant and a hydrogen donor for mixing, then continuously adding alkali and an emulsifier for mixing, and then adding free nitrogen carbene for mixing to obtain the water-soluble thickened oil viscosity reducer.
Example 5
The embodiment provides a water-soluble thickened oil viscosity reducer, which comprises, by mass, 5 wt% of free azacarbene, 2wt% of cobalt dodecylbenzene sulfonate, 30 wt% of tert-butyl hydroperoxide as an oxidant, 3 wt% of methanol as a hydrogen donor, 1 wt% of sodium hydroxide as an alkali, 201 wt% of tween as an emulsifier, 3 wt% of sodium dihydrogen phosphate, and the balance of benzene as a solvent, and the total amount is 100%.
The water-soluble thickened oil viscosity reducer of the embodiment is prepared by the following steps:
mixing cobalt dodecyl benzene sulfonate with a solvent at 25 ℃, then adding an oxidant and a hydrogen donor for mixing, then continuously adding alkali and an emulsifier for mixing, and then adding free nitrogen carbene for mixing to obtain the water-soluble thickened oil viscosity reducer.
Example 6
The embodiment provides a water-soluble thickened oil viscosity reducer, which comprises, by mass, 8 wt% of free azacarbene, 1 wt% of cobalt dodecylbenzene sulfonate, 20 wt% of tert-butyl hydroperoxide as an oxidant, 5 wt% of methanol as a hydrogen donor, 2wt% of sodium hydroxide as an alkali, 200.5 wt% of tween as an emulsifier, 1 wt% of sodium dihydrogen phosphate, and the balance of benzene as a solvent, wherein the total amount is 100%.
The water-soluble thickened oil viscosity reducer of the embodiment is prepared by the following steps:
mixing cobalt dodecyl benzene sulfonate with a solvent at 25 ℃, then adding an oxidant and a hydrogen donor for mixing, then continuously adding alkali and an emulsifier for mixing, and then adding free nitrogen carbene for mixing to obtain the water-soluble thickened oil viscosity reducer.
Example 7
The embodiment provides a water-soluble thickened oil viscosity reducer, which comprises, by mass, 10 wt% of free azacarbene, 1 wt% of cobalt dodecylbenzene sulfonate, 15 wt% of tert-butyl hydroperoxide as an oxidant, 3 wt% of methanol as a hydrogen donor, 1 wt% of sodium hydroxide as an alkali, 201 wt% of tween as an emulsifier, 5 wt% of sodium dihydrogen phosphate, and the balance of benzene as a solvent, and the total amount is 100%.
The water-soluble thickened oil viscosity reducer of the embodiment is prepared by the following steps:
mixing cobalt dodecyl benzene sulfonate with a solvent at 25 ℃, then adding an oxidant and a hydrogen donor for mixing, then continuously adding alkali and an emulsifier for mixing, and then adding free nitrogen carbene for mixing to obtain the water-soluble thickened oil viscosity reducer.
Comparative example 1
The water-soluble thickened oil viscosity reducer of the comparative example is different from that of example 1 in that: the catalyst does not contain free azacarbene, and specifically comprises 2wt% of cobalt dodecyl benzene sulfonate, 30 wt% of oxidant tert-butyl hydroperoxide, 3 wt% of hydrogen donor methanol, 1 wt% of alkali sodium hydroxide, 201 wt% of emulsifier Tween and the balance of solvent benzene, wherein the total amount is 100%.
Comparative example 2
The water-soluble thickened oil viscosity reducer of the comparative example is different from that of example 1 in that: the catalyst does not contain cobalt dodecyl benzene sulfonate, and specifically comprises 5 wt% of free azacarbene, 30 wt% of oxidant tert-butyl hydroperoxide, 3 wt% of hydrogen donor methanol, 1 wt% of alkali sodium hydroxide, 201 wt% of emulsifier Tween and the balance of solvent benzene, wherein the total amount is 100%.
Comparative example 3
The water-soluble thickened oil viscosity reducer of the comparative example is different from that of example 5 in that: the composition does not contain free azacarbene, and specifically comprises 2wt% of cobalt dodecyl benzene sulfonate, 30 wt% of tert-butyl hydroperoxide as an oxidant, 3 wt% of methanol as a hydrogen donor, 1 wt% of alkali sodium hydroxide, 201 wt% of Tween as an emulsifier, 3 wt% of sodium dihydrogen phosphate and the balance of benzene as a solvent, wherein the total amount is 100%.
Application example
The water-soluble thickened oil viscosity reducing agent disclosed in examples 1-7 and comparative examples 1-3 is used for treating thickened oil extracted from Touha as a reactant (the viscosity is 95650mPa & s at 50 ℃); specifically, the thickened oil and water are mixed according to the mass ratio of 7:3, then the water-soluble thickened oil viscosity reducer is added into the thickened oil according to the addition amount of the water-soluble thickened oil viscosity reducer being 1.0% of the mass of the thickened oil, viscosity reduction is carried out at the temperature of 60 ℃, and the viscosity reduction rates of 6h, 9h and 12h are detected and obtained.
The viscosity value of the thick oil was measured to evaluate the catalytic performance of the catalyst. The viscosity reduction rate is calculated as Δ η (%) ═ η ((η) 0 -η)/η 0 )×100％，η 0 And eta respectively represents the viscosity of the oil sample before and after the reaction, and the unit is mPa & s; the results of reducing caking are shown in table 1.
TABLE 1 reduced cohesiveness fruits for thickened oils at different times in examples 1-7 and comparative examples 1-3
As can be seen from Table 1, after 12h of viscosity reduction, the viscosity reduction rate of the examples 1-7 is as high as more than 90%, in addition, the viscosity reduction effect of the examples 5-7 added with sodium dihydrogen phosphate is slightly good, the viscosity reduction rate of the comparative example 1 is lower because free azacarbene is absent, the viscosity reduction rate of the comparative example 2 is also obviously lower because cobalt dodecylbenzenesulfonate is absent, the comparative example 3 has more sodium dihydrogen phosphate than the comparative example 1, and the viscosity reduction effect is slightly better than the comparative example 1, which indicates that the viscosity reduction effect of the water-soluble viscous oil viscosity reducer in the application is realized by matching of all components.
In addition, the heavy oil after catalytic oxidation viscosity reduction can be detected and characterized by combining with figure 2, and the heavy oil after viscosity reduction is carried out at the temperature of 925-1135cm -1 Has a broad absorption peak, specifically 1165 and 1120cm -1 The peak at (A) is attributed to SO in sulfone 2 Extension vibration, 1072, 1032cm -1 The peak is attributed to S ═ O stretching vibration of sulfoxide, which shows that the sulfoxide and the sulfone are obtained by viscosity reduction, and the viscosity reduction effect is obvious.
The above-described embodiments of the present invention should not be construed as limiting the scope of the present invention. Any other corresponding changes and modifications made according to the technical idea of the present invention should be included in the protection scope of the claims of the present invention.
Claims (8)
1. The water-soluble thickened oil viscosity reducer is characterized by comprising, by mass, 5-10% of free aza-carbene, 1-2% of cobalt dodecyl benzene sulfonate, 15-30% of an oxidant, 1-5% of a hydrogen donor, 1-2% of an alkali, 0.5-1% of an emulsifier, and the balance of a solvent, wherein the total amount is 100%; wherein the oxidant is tert-butyl hydroperoxide, the hydrogen donor is methanol, and the structural formula of the free aza-carbene is as follows:
2. the water-soluble heavy oil viscosity reducer according to claim 1, wherein the base is sodium hydroxide.
3. The water-soluble heavy oil viscosity reducer according to claim 1, wherein the solvent is benzene.
4. The water-soluble heavy oil viscosity reducer according to claim 1, wherein the emulsifier is one or both of tween 20 and span 20.
5. The water-soluble thickened oil viscosity reducer according to claim 1, further comprising 1-5% of sodium dihydrogen phosphate.
6. The preparation method of the water-soluble thickened oil viscosity reducer according to any one of claims 1 to 4, characterized by comprising the following steps: mixing cobalt dodecyl benzene sulfonate with a solvent, then adding an oxidant and a hydrogen donor for mixing, then continuously adding alkali and an emulsifier for mixing, and then adding free aza-carbene for mixing to obtain the water-soluble thickened oil viscosity reducer.
7. The method according to claim 6, wherein the cobalt dodecylbenzenesulfonate is mixed with the solvent at 25 to 40 ℃.
8. Use of the water-soluble thickened oil viscosity reducer of any one of claims 1 to 5 or the water-soluble thickened oil viscosity reducer prepared by the preparation method of any one of claims 6 to 7 in treating thickened oil.
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