CN107312507B - Clay stabilizer and application thereof - Google Patents
Clay stabilizer and application thereof Download PDFInfo
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- CN107312507B CN107312507B CN201610269047.7A CN201610269047A CN107312507B CN 107312507 B CN107312507 B CN 107312507B CN 201610269047 A CN201610269047 A CN 201610269047A CN 107312507 B CN107312507 B CN 107312507B
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- 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
- C09K8/02—Well-drilling compositions
- C09K8/03—Specific additives for general use in well-drilling compositions
- C09K8/035—Organic additives
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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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/607—Compositions for stimulating production by acting on the underground formation specially adapted for clay formations
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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
- C09K8/60—Compositions for stimulating production by acting on the underground formation
- C09K8/62—Compositions for forming crevices or fractures
- C09K8/66—Compositions based on water or polar solvents
- C09K8/68—Compositions based on water or polar solvents containing organic compounds
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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 relates to a preparation method of a clay stabilizer for a low-permeability stratum, which sequentially comprises the following steps: adding epoxy chloropropane into aqueous solution of monohydric aliphatic amine, and reacting for a certain time; adding epoxy chloropropane, heating and reacting; and then adding polyamine and epoxy chloropropane, then reacting and drying to obtain the clay stabilizer.
Description
Technical Field
The invention relates to the field of auxiliaries used in oil and gas exploitation, and particularly relates to a preparation method and application of a clay stabilizer.
Background
The oil and gas reservoirs in China all contain a certain amount of clay minerals, when the clay content in the reservoirs is high (for example, the average clay content of shale gas reservoirs in Fuling areas of Chundong south of China is 32%, the clay content of Tshan areas reaches 40% -60%, and the clay content of Twen areas reaches 20% -50%), when water-based working fluids such as well drilling, well cementing, water injection, fracturing, acidizing, well workover and the like invade, the clay minerals are easy to expand, disperse and migrate, the throats of stratum pore structures can be blocked, the permeability of the stratum is reduced, the yield of oil wells is reduced, and the oil and gas layers are damaged, so a clay stabilizer is required to be added.
Clay stabilizers go through inorganic salt, inorganic polynuclear polymers, cationic surfactants, organic cationic polymer stages. Among them, organic cationic polymer clay stabilizers have become the popular research direction, for example, CN101921366 synthesizes triple-branched cationic polymers from diallylammonium chloride and triallylammonium chloride, and is used for stabilizing clay in the oil extraction process. However, studies show that high molecular weight cationic polymers are not suitable for low permeability formations and are easy to form plugs in pore passages of the formations, thereby blocking the formations; meanwhile, the polymer contains a large number of cationic groups due to the long molecular chain, and is easy to react with a treating agent containing anionic groups, so that the effect of the treating agent is greatly influenced. Therefore, there is a need to develop clay stabilizers with relatively low molecular mass, which protect the formation from damage, and which are well compatible with other treatments.
In field application, the dosage is very strictly controlled in some construction processes (such as drag reduction and water fracturing, and the dosage of the clay stabilizer is required to be extremely low to be 0.1-0.5%). However, in a large number of patents and documents, the anti-swelling effect of 1% to 2% is often emphasized, the anti-swelling effect of 0.3% to 1% is evaluated less, and a higher amount is often selected in application, and the clay stabilizer of the type currently has the problems of excellent anti-swelling effect (1% to 2% or more) when the amount is high, and poor anti-swelling effect when the amount is low (< 0.5%), such as small molecular polyamine stabilizer EM (chemical and biological engineering, 2010, 27(12)), wherein the anti-swelling rate reaches 72% to 86% when the amount is 1% to 2%, but the anti-swelling rate is only 43% when the amount is 0.5%.
Disclosure of Invention
The invention provides a preparation method of a clay stabilizer, aiming at the problems that the existing clay stabilizer is large in dosage, low in anti-swelling rate and large in molecular weight of a polymer clay stabilizer and is easy to cause stratum damage. The multi-component clay stabilizer prepared according to the invention has relatively low molecular weight, and can effectively inhibit hydration swelling and dispersion migration of clay even at an extremely low dosage. The clay stabilizer of the invention can be applied to low-permeability stratum. The invention also provides application of the clay stabilizer.
According to one aspect of the present invention, there is provided a method of preparing a clay stabilizer for a hypotonic subterranean formation, comprising the steps of, in order:
a, adding epoxy chloropropane into aqueous solution of monohydric aliphatic amine, and then reacting for a certain time;
b, adding epoxy chloropropane into the solution reacted in the step a, and then heating for reaction;
and c, adding polyamine into the solution reacted in the step b, adding epoxy chloropropane, reacting, and drying to obtain the clay stabilizer.
According to the method provided by the invention, the clay stabilizer can be prepared with high conversion rate. The obtained clay stabilizer forms a molecular structure with coexisting linear chains and a net structure through the reaction of monoamine fatty amine, epichlorohydrin and polyamine, and simultaneously acts on negatively charged clay particles in multiple points, so that the adsorption degree is high, and the aim of high anti-swelling rate at low addition is fulfilled.
According to a particular embodiment of the process provided by the present invention, the mono-aliphatic amine is selected from at least one of dimethylamine, trimethylamine, diethylamine and triethylamine. The polyamine is a compound containing at least two amine groups. In a specific embodiment, the polyamine is triethylenetetramine and/or tetraethylenepentamine. In another specific embodiment, the polyamine is a mixture of triethylene tetramine and tetraethylene pentamine. And in a preferred embodiment, the molar ratio of triethylene tetramine to tetraethylene pentamine is from 1:1 to 1: 5.
According to another embodiment of the process provided by the present invention, the molar ratio of the monohydric aliphatic amine, the total epichlorohydrin and the polyamine is 1 (0.9-1.5) to (0.2-1).
According to another embodiment of the process provided by the present invention, the molar ratio of epichlorohydrin in step a, epichlorohydrin in step b and epichlorohydrin in step c is 1 (1-1.2): 0.2-1.5. The epichlorohydrin is added in a plurality of times, so that the reaction conversion degree can be improved. In a specific example, the epichlorohydrin used in steps a, b and c is added dropwise. The dropping can control the temperature of the system and the adding speed.
According to another embodiment of the method provided by the present invention, said step a is controlled to be performed at a temperature below 20 ℃. In a specific example, the certain time in step a is 0.5-2h, such as 0.5-1h or 1-2 h. In another specific example, the molar ratio of the mono-aliphatic amine to water in the aqueous solution of the mono-aliphatic amine is 1 (20-30).
According to another embodiment of the method provided by the invention, in the step b, the temperature is increased to 80-95 ℃, and/or the reaction time is 2-4 h. In the step c, the reaction temperature is 60-85 ℃, and/or the reaction time is 1-4 h. The clay stabilizer obtained was in the form of a dry powder.
According to a specific embodiment of the present invention, the method comprises the following steps. Respectively weighing aliphatic monoamine, epichlorohydrin, polyamine and distilled water according to the molar ratio of 1 (0.9-1.5) to (0.2-1) to (10-30). Putting measured aliphatic monoamine and distilled water into a reactor, starting stirring, dropwise adding a certain amount of epoxy chloropropane by using a constant-pressure dropping funnel, controlling the low temperature and the dropping acceleration, and keeping the temperature for a certain reaction time, such as 1 hour after dropwise adding; and then dropwise adding a certain amount of epoxy chloropropane, gradually heating to 80-95 ℃, and reacting for 2-4 h. And adding metered polyamine into the obtained product, dropwise adding the residual epoxy chloropropane, gradually heating to 60-85 ℃, reacting for 1-4h, and vacuum drying the product to obtain the dry powdery clay stabilizer.
According to a specific embodiment of the present invention, the clay stabilizer is suitable for use in a low permeability formation, and the method is a method for preparing a clay stabilizer suitable for use in a low permeability formation.
According to the method provided by the invention, the reaction conversion degree is improved by feeding the reaction raw materials in several times; a large number of cationic groups are introduced into a molecular chain by sequentially adding monoamine and polyamine to form a multi-component stabilizer with a linear chain structure and a net structure, and simultaneously, the multi-component stabilizer acts on negatively charged clay particles in multiple points, so that the adsorption degree is high, the aim of high anti-swelling rate at low addition is fulfilled, and the anti-swelling rate can reach 73% at 0.3%.
The clay stabilizer has low relative molecular mass (for example, the number average molecular weight is about 250-5000, the main component is 250-1300, and accounts for about 55-87 percent), is solid dry powder, and is convenient to transport and store; the pore canal of the stratum is not easy to be blocked; the method is particularly suitable for low-permeability stratum without causing stratum damage; the product is used in operations such as well drilling, well cementing, water injection, acidification and the like, and has good compatibility with common treating agents; also has good anti-swelling property and stabilizer at low addition amount.
According to another aspect of the present invention, there is also provided a clay stabilizer for use in oil and gas production, comprising: the clay stabilizer is prepared by the method and then used for oil and gas exploitation. The clay stabilizer prepared by the method is used for oil and gas exploitation, is beneficial to improving the yield of an oil well and avoids or reduces the damage of an oil-gas layer.
Drawings
FIG. 1 is an IR spectrum of a stabilizer product according to one embodiment of the present invention.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the invention in any way.
Infrared characterization: the synthesized product is mixed with potassium bromide according to the proportion of 1:100, and then tabletting is carried out after grinding, and the spectrogram is measured by an infrared spectrometer.
Determination of molecular weight: the measurement was carried out by gel permeation chromatography.
Example 1:
adding 1.2mol of trimethylamine into a three-neck flask, adding 10mol of distilled water under the stirring condition, slowly dropwise adding 0.5mol of epoxy chloropropane by using a constant-pressure dropping funnel, controlling the accelerated temperature to be lower than 20 ℃, and preserving the heat for 1h after the dropwise adding is finished; then, adding 0.5mol of epoxy chloropropane, gradually heating to 90-95 ℃, and reacting for 2 h; and then 0.4mol of triethylene tetramine is added, 0.5mol of epoxy chloropropane is added dropwise, the temperature is increased to 65-70 ℃ for reaction for 2 hours, and the product is dried in vacuum to obtain the clay stabilizer.
The clay stabilizer was characterized by infrared, 1250cm, as can be seen from FIG. 1-1、980cm-1Is a C-N characteristic absorption peak of 2900-3000 cm-1Is a C-H stretching vibration peak in methyl and methylene, and no N-H absorption peak is in the figure, 3330cm-1The peak of hydroxyl group is a characteristic peak of water after potassium bromide tablet absorbs moisture, so that the stabilizer contains quaternary ammonium group.
The number average molecular weight range is about 250-5000, wherein 87% of the number average molecular weight range is about 250-1300.
Example 2:
adding 1.2mol of dimethylamine into a three-neck flask, adding 10mol of distilled water under the stirring condition, slowly dropwise adding 0.4mol of epichlorohydrin by using a constant-pressure dropping funnel, controlling the accelerated temperature to be lower than 20 ℃, and preserving the heat for 1h after the dropwise adding is finished; then, adding 0.4mol of epoxy chloropropane, gradually heating to 80-85 ℃ and reacting for 2 h; and then 0.4mol of triethylene tetramine is added, 0.4mol of epoxy chloropropane is added dropwise, the temperature is increased to 65-70 ℃ for reaction for 2 hours, and the product is dried in vacuum to obtain the clay stabilizer.
The stabilizer contains quaternary ammonium groups through tests. The number average molecular weight is about 250 to 5000, wherein 85% of the number average molecular weight is about 250 to 1300.
Example 3:
adding 1.5mol of dimethylamine into a three-neck flask, adding 15mol of distilled water under the stirring condition, slowly dropwise adding 0.7mol of epichlorohydrin by using a constant-pressure dropping funnel, controlling the accelerated temperature to be lower than 20 ℃, and preserving the heat for 1h after the dropwise adding is finished; then, adding 0.8mol of epoxy chloropropane, gradually heating to 80-85 ℃ and reacting for 2 h; and then 0.4mol of triethylene tetramine is added, 0.2mol of epoxy chloropropane is added dropwise, the temperature is increased to 65-70 ℃ for reaction for 2 hours, and the product is dried in vacuum to obtain the clay stabilizer.
The stabilizer contains quaternary ammonium groups through tests. The number average molecular weight is about 250 to 5000, wherein 55% of the number average molecular weight is about 250 to 1300.
Example 4:
adding 1.5mol of trimethylamine into a three-neck flask, adding 20mol of distilled water under the stirring condition, slowly dropwise adding 0.9mol of epoxy chloropropane by using a constant-pressure dropping funnel, controlling the accelerated temperature to be lower than 20 ℃, and preserving the heat for 1h after the dropwise adding is finished; then, adding 0.9mol of epoxy chloropropane, gradually heating to 90-85 ℃ and reacting for 2 h; and then 0.3mol of triethylene tetramine is added, 0.2mol of epoxy chloropropane is added dropwise, the temperature is increased to 65-70 ℃ for reaction for 4 hours, and the product is dried in vacuum to obtain the clay stabilizer.
The stabilizer contains quaternary ammonium groups through tests. The number average molecular weight is about 250 to 5000, wherein 59% of the number average molecular weight is about 250 to 1300.
Example 5:
adding 1.2mol of trimethylamine into a three-neck flask, adding 20mol of distilled water under the stirring condition, slowly dropwise adding 0.4mol of epoxy chloropropane by using a constant-pressure dropping funnel, controlling the accelerated temperature to be lower than 20 ℃, and preserving the heat for 1h after the dropwise adding is finished; then, adding 0.4mol of epoxy chloropropane, gradually heating to 90-85 ℃ and reacting for 2 h; and then adding a mixture of 0.3mol of triethylene tetramine and 0.3mol of tetraethylenepentamine, dropwise adding 0.6mol of epoxy chloropropane, heating to 65-70 ℃, reacting for 2 hours, and vacuum drying the product to obtain the clay stabilizer.
The stabilizer contains quaternary ammonium groups through tests. The number average molecular weight is about 250 to 5000, wherein the number average molecular weight is 87% of about 250 to 1300.
Characterization and comparison of clay stabilizers:
1. clay stabilizers of the invention are compared with other stabilizers
The anti-swelling rate is evaluated by measuring the volume expansion increment of the bentonite powder in a clay stabilizer solution and water according to a standard SY/T5971-94 performance evaluation method for clay stabilizers for water injection and a centrifugation method in Q/SH 0053-2010 technical requirement for clay stabilizers. Respectively measuring the anti-swelling rate of the clay stabilizer and other common clay stabilizers in clear water and the anti-drag hydraulic fracturing fluid under the addition of 0.3 wt% based on the weight of the fracturing fluid; and selecting a clay stabilizer with higher anti-swelling rate, and measuring the water washing resistance rate of the clay stabilizer in clear water. The formula of the drag reduction hydraulic fracturing fluid comprises the following components: 0.1% by weight of an anionic polymer (acrylamide-acrylic acid copolymer, molecular weight greater than 500 ten thousand, brand 80A-51) + 0.1% by weight of a surfactant (cleanup additive for fracturing, brand FC-117) + clear water, the results are shown in Table 1.
TABLE 1 comparison of the results of the swelling prevention ratio and the washing resistance ratio
In table 1, CPCS series (development of low relative molecular mass polyquaternium clay anti-swelling agent of CPCS series, oilfield chemistry, vol 26, No. 3, 2009, prepared from monoamine and epichlorohydrin as raw materials);
XFP-2 (development and field application of a novel high-temperature clay stabilizer XFP-2, development of fine petrochemical industry, No. 7, No. 10, 2006, monoamine as a main raw material);
HAPEA and HFHEA (synthesis of organic amine anti-swelling agent and performance evaluation thereof, Sigan oil university, Master's academic paper, 2012), wherein HAPEA takes monoamine and epichlorohydrin as main raw materials, HFHEA takes polyamine and epichlorohydrin as main raw materials, and the anti-swelling rate of the HFHEA is measured by using clay stabilizer addition amount higher than 0.3% and the anti-swelling rate is between 53% and 71%.
As can be seen from Table 1, the clay stabilizers of the present invention have a swelling prevention rate of more than 65% and a maximum of 73.6% in the clear water fracturing fluid at an addition of 0.3 wt%; the anti-swelling rate in the drag reduction hydraulic fracturing fluid is higher than 60 percent.
In the other clay stabilizers of the control, the swelling prevention rate at 0.3 wt% addition was less than that of the present application. Among these, the clay stabilizers of CPCS series, XFP-2, HAPEA and HFHEA have an anti-swelling rate much lower than that of the stabilizers of the present application even if added in an amount higher than that of the present application, not to mention that the anti-swelling rate is inevitably much lower than that of the stabilizers of the present application when added in the same amount as that of the present application.
By contrast, the clay stabilizer of the invention has the advantage of anti-swelling. Because the drag reducer in the drag reduction water is an anionic polymer and has certain influence on the inhibition effect of the cationic clay stabilizer, the anti-swelling rate in the drag reduction water is lower than that of clear water. The clay stabilizers of examples 1, 2 and 5, which had high anti-swelling rates, all had a water washing resistance higher than 90% and higher than XFP-2 and HY-200.
2. Influence of clay stabilizer addition on anti-swelling rate
The clay stabilizers of example 1 were measured for their anti-swelling rate at different addition levels in clean water, and the results are shown in Table 2.
TABLE 2 Effect of Clay stabilizer addition on anti-swelling Rate
3. Viscosity test experiment
Examples 1, 2, 5 of the present invention and high molecular weight cationic polymers were formulated into 10% solutions and their viscosities were measured using a Fann six speed rotational viscometer to characterize the relative molecular mass, with some comparison to the same product conditions, and the results are shown in table 3.
TABLE 3 viscosity comparison of clay stabilizer solutions
As can be seen from table 3, the clay stabilizers of the present invention have a lower viscosity in solution than the same addition of high molecular polymer clay stabilizers due to their low relative molecular mass.
4. Compatibility test
The compatibility of the clay stabilizers of example 1, example 2 and example 5 with conventional drilling fluid and fracturing fluid common treating agents was observed, and the results are shown in table 4:
TABLE 4 compatibility test results for Clay stabilizers
As can be seen from Table 4, the clay stabilizer of the present invention has no delamination, sedimentation and suspension when mixed with a conventional treating agent, and has good compatibility.
Any numerical value mentioned in this specification, if there is only a two unit interval between any lowest value and any highest value, includes all values from the lowest value to the highest value incremented by one unit at a time. For example, if it is stated that the amount of a component, or a value of a process variable such as temperature, pressure, time, etc., is 50 to 90, it is meant in this specification that values of 51 to 89, 52 to 88 … …, and 69 to 71, and 70 to 71, etc., are specifically enumerated. For non-integer values, units of 0.1, 0.01, 0.001, or 0.0001 may be considered as appropriate. These are only some specifically named examples. In a similar manner, all possible combinations of numerical values between the lowest value and the highest value enumerated are to be considered to be disclosed in this application.
It should be noted that the above-mentioned embodiments are only for explaining the present invention, and do not constitute any limitation to the present invention. The present invention has been described with reference to exemplary embodiments, but the words which have been used herein are words of description and illustration, rather than words of limitation. The invention can be modified, as prescribed, within the scope of the claims and without departing from the scope and spirit of the invention. Although the invention has been described herein with reference to particular means, materials and embodiments, the invention is not intended to be limited to the particulars disclosed herein, but rather extends to all other methods and applications having the same functionality.
Claims (9)
1. A preparation method of a clay stabilizer sequentially comprises the following steps:
a, adding epoxy chloropropane into aqueous solution of monohydric aliphatic amine, and then reacting for a certain time, wherein the certain time is 0.5-2 h;
b, adding epoxy chloropropane into the solution reacted in the step a, heating to 80-95 ℃, and reacting for 2-4 h;
c, adding polyamine and epoxy chloropropane into the solution reacted in the step b, then reacting, and drying to obtain the clay stabilizer, wherein the reaction temperature is 60-85 ℃, and the reaction time is 1-4 h;
the step a is controlled to be carried out below 20 ℃;
the mol ratio of the epoxy chloropropane in the step a, the epoxy chloropropane in the step b and the epoxy chloropropane in the step c is 1 (1-1.2) to (0.2-1.5);
the molar ratio of the monohydric aliphatic amine to the total epichlorohydrin to the polyamine is 1 (0.9-1.5) to (0.2-1);
the polyamine is triethylene tetramine and/or tetraethylene pentamine.
2. The method according to claim 1, wherein the mono-aliphatic amine is selected from at least one of dimethylamine, trimethylamine, diethylamine and triethylamine.
3. The method of claim 1, wherein the polyamine is a mixture of triethylene tetramine and tetraethylene pentamine.
4. The method of claim 3, wherein the molar ratio of triethylene tetramine to tetraethylene pentamine is from 1:1 to 1: 5.
5. The method according to any one of claims 1 to 4, wherein the molar ratio of the aliphatic monoamine to the water in the aqueous solution of the aliphatic monoamine is 1 (20-30).
6. Process according to any one of claims 1 to 4, characterized in that the epichlorohydrin used in steps a, b and c is added dropwise.
7. The method according to any one of claims 1 to 4, wherein the certain time in step a is 0.5 to 1 hour.
8. The method of any one of claims 1-4, wherein the clay stabilizer is in a dry powder form.
9. Use of a clay stabilizer in oil and gas production comprising: the clay stabilizer is prepared by the method of any one of claims 1-8 and then used in oil and gas recovery.
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| CN108179023B (en) * | 2017-12-07 | 2020-02-18 | 中海油天津化工研究设计院有限公司 | Heavy oil produced liquid reverse demulsifier and preparation method thereof |
| CN108329902A (en) * | 2018-01-23 | 2018-07-27 | 中国石油天然气股份有限公司 | A kind of salt tolerant clay stabilizer and preparation method thereof of oil field water outlet preparing fracturing fluid |
| CN108485633B (en) * | 2018-03-31 | 2021-10-08 | 青岛大学 | Preparation method of shale anti-swelling agent for net-shaped polyquaternary amine oil and gas well |
| CN109097006B (en) * | 2018-09-14 | 2020-09-29 | 中国石油集团渤海钻探工程有限公司 | Borehole wall anti-sloughing agent for drilling fluid and preparation method thereof |
| CN110452375B (en) * | 2019-07-12 | 2022-06-03 | 东北石油大学 | High-cationic-degree clay stabilizer and preparation method thereof |
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